Waste from the radio-electronic industry. Method for processing waste from the electronic and electrical industry. Study of the material composition of radio-electronic scrap

The invention relates to the metallurgy of precious metals and can be used at secondary metallurgy enterprises for processing radio-electronic scrap and when extracting gold or silver from waste of the electronic and electrochemical industry, in particular to a method for extracting precious metals from waste of the radio-electronic industry. The method involves obtaining copper-nickel anodes containing impurities of noble metals from waste, their electrolytic anodic dissolution with the deposition of copper on the cathode, producing a nickel solution and sludge with noble metals. In this case, anodic dissolution is carried out from an anode containing 6-10% iron, placing the cathode and anode in separate mesh diaphragms to create cathode and anode spaces with a chlorine-containing electrolyte located in them. The electrolyte obtained during the electrolysis process is directed from the cathode space to the anode space. The technical result of the invention is a significant increase in the rate of anode dissolution.

The invention relates to the metallurgy of precious metals and can be used at secondary metallurgy enterprises for processing radio-electronic scrap and for the extraction of gold or silver from waste of the electronic and electrochemical industries.

There are the following methods for electrorefining metals.

There is a known method that relates to the hydrometallurgy of precious metals, in particular to methods for extracting gold and silver from concentrates, waste from the electronic and jewelry industries. A method in which the recovery of gold and silver involves treatment with solutions of complexing salts and passing electric current with a density of 0.5-10 A/dm 2, solutions containing thiocyanate ions, ferric ions are used as solutions, and the pH of the solution is 0.5-4.0. The separation of gold and silver is carried out at the cathode, separated from the anode space by a filter membrane (RF Application No. 94005910, MPK S25S 1/20).

The disadvantages of this method are increased losses of precious metals in the sludge. The method requires additional treatment of concentrates with complexing salts.

An invention is known that relates to methods for the extraction of noble metals from spent catalysts, as well as to electrochemical processes with a fluidized or fixed bed. The processed material in the form of a backfill is placed in the interelectrode space of the electrolyzer, electrochemical leaching of noble metals based on their anodic dissolution is activated by pre-processing the material by reversing the polarity of the electrodes in static conditions, which turns it into a volumetric multipolar electrode, ensuring anodic dissolution of the metal in the entire volume of the material, and circulation of the electrolyte through the backfill from the anode to the cathode is provided at a speed determined from the condition of preventing hydrated anionic chloride complexes of noble metals formed during leaching in the volume of the backfill from reaching the cathode, while acidified water with a hydrochloric acid content of 0.3-4.0 is used as an electrolyte %. The method allows you to increase the productivity of the process and simplify it (RF Patent No. 2198947, IPC S25S 1/20).

The disadvantage of this method is the increased energy consumption.

A known method involves the electrochemical dissolution of gold and silver in an aqueous solution at a temperature of 10-70°C in the presence of a complexing agent. Sodium ethylenediaminetetraacetate is used as a complexing agent. EDTA Na concentration 5-150 g/l. Dissolution is carried out at pH 7-14. Current density 0.2-10 A/dm2. The use of the invention makes it possible to increase the rate of dissolution of gold and silver; reduce the copper content in the sludge sediment to 1.5-3.0% (RF Patent No. 2194801, IPC C25 C1/20).

The disadvantage of this method is that the dissolution rate is not high enough.

As a prototype of the present invention, a method was selected for the electrolytic refining of copper and nickel from copper-nickel alloys containing impurities of precious metals, which includes the electrochemical dissolution of anodes from a copper-nickel alloy, copper deposition to produce a nickel solution and slurry. The anodes are dissolved in the anode space separated by a diaphragm, in a suspended layer of sludge, which ensures a reduction in energy consumption (by 10%) and an increase in the concentration of gold content in the sludge. (RF Patent No. 2237750, IPC S25S 1/20, published 04/29/2003).

The disadvantages of this invention remain the loss of noble metals in the sludge and the dissolution rate being insufficiently high.

The technical result is the elimination of these shortcomings, i.e. reducing losses of precious metals in sludge, increasing the dissolution rate, reducing energy consumption.

The technical result is achieved by the fact that in the method of electrolytic sulfuric acid dissolution of copper-nickel anodes obtained from radio-electronic industry waste containing impurities of noble metals, including anodic dissolution, chemical dissolution and cathodic deposition of copper, producing a nickel solution and slurry with noble metals, According to the invention, the anode containing 6-10% iron and the cathode are placed in separate mesh diaphragms containing a chlorine-containing electrolyte, and the electrolyte obtained during the electrolysis process is directed from the cathode space to the anode space.

The method is implemented as follows.

In an electrolytic bath, the copper-nickel anode, containing 6-10% iron, impurities of noble metals, and the cathode are placed in separate mesh diaphragms with a chlorine-containing electrolyte, creating separate anode and cathode spaces. In the cathode space, the electrolyte is enriched with ferric iron FeCl 3, and then it is supplied to the anode space, for example, using a pump. The anode dissolution process is carried out at a current density of 2-10 A/dm 2, a temperature of 40-70 ° C and a voltage of 1.5-2.5 V. Under the influence of electric current and the oxidative effect of ferric iron, the anode dissolution process is significantly accelerated and the content of noble elements increases metals in sludge.

An electrolyte enriched in FeCl 2 is formed in the cathode space, which is sent to the anode space, where it is oxidized to FeCl 3, due to which the process of chemical dissolution of the anode begins.

Thanks to electrolytic and chemical exposure the anode dissolution rate increases significantly, the content of noble metals in the sludge increases, gold losses are reduced and the anode dissolution time is reduced.

When the iron concentration in the anode is less than 6%, a reduced content of FeCl 3 is observed in the electrolyte, which leads to an insufficient chemical effect of ferric iron FeCl 3 on the anode and, as a consequence, a low rate of dissolution of the anode.

An increase in the iron concentration in the anode by more than 10% does not further increase the rate of anode dissolution, but creates additional difficulties in processing the electrolyte.

This method is proven by the following examples.

A copper-nickel anode containing 7% Fe and weighing 119 g was placed in the anode space and dissolved at a voltage of 2.5 V, a temperature of 60°C and a current density of 1000 A/m 2 in an electrolyte of the following composition: CuSO 4 5H 2 O - 500 ml, H 2 SO 4 - 250 ml, FeSO 4 - 60 ml, HCl - 50 ml. In the absence of electrolyte circulation, the anode mass decreased by 0.9 g during the first hour of the process. Over two hours of electrolysis, the anode mass decreased by 1.8 g.

After the electrolyte began to move from the cathode space to the anode without changing the current density, the mass of the anode decreased by 4.25 g in the first hour of electrolysis, and by 8.5 g in two hours.

A copper-nickel anode containing 4% Fe and weighing 123 g was dissolved under the same conditions, and in the absence of electrolyte circulation, the anode mass decreased by 0.4 g in the first hour of the process, and in two hours of electrolysis, the anode mass decreased by 0.8 G.

Moving the electrolyte from the cathode space to the anode space, without changing the current density, made it possible to reduce the mass of this anode in the first hour of electrolysis by 1.15 g, and in two hours by 2.3 g.

Provided that the electrolyte moves from the cathode space to the anode, the anode mass decreased by 4.25 g in the first hour of electrolysis, and by 8.5 g in two hours.

Based on the data obtained, we can conclude that the iron content of 6-10% in the copper-nickel anode and the movement of the electrolyte enriched with FeCl 3 from the cathode space to the anode space can significantly increase the rate of anode dissolution.

Thanks to the proposed method the following effects are achieved:

1) increase in the content of noble metals in the sludge;

2) a significant increase in the rate of anode dissolution;

3) reduction of sludge volume.

CLAIM

A method for extracting noble metals from radio-electronic industry waste, including obtaining from them copper-nickel anodes containing impurities of noble metals, their electrolytic anodic dissolution with the deposition of copper on the cathode and obtaining a nickel solution and slurry with noble metals, characterized in that electrolytic anodic dissolution is carried out an anode containing 6-10% iron, when placing the cathode and anode in separate mesh diaphragms to create cathode and anode spaces with a chlorine-containing electrolyte located in them, and the electrolyte obtained during the electrolysis process is directed from the cathode space to the anode space.

As a manuscript

TELYAKOV Alexey Nailievich

DEVELOPMENT OF AN EFFECTIVE TECHNOLOGY FOR EXTRACTION OF NON-FERROUS AND NOBLE METALS FROM RADIO ENGINEERING INDUSTRY WASTE

Specialty 05.16.02– Metallurgy of ferrous and non-ferrous

and rare metals

A b r e f e r t

dissertations for an academic degree

candidate of technical sciences

SAINT PETERSBURG

The work was carried out in the state educational institution higher vocational education St. Petersburg State Mining Institute named after G.V. Plekhanov ( technical university)

Scientific director–

Doctor of Technical Sciences, Professor,

Honored Scientist of the Russian FederationV.M.Sizyakov

Official opponents:

Doctor of Technical Sciences, ProfessorI.N.Beloglazov

Candidate of Technical Sciences, Associate ProfessorA.Yu.Baymakov

Leading enterprise– Gipronickel Institute

The defense of the dissertation will take place on November 13, 2007 at 14:30 at a meeting of the dissertation council D 212.224.03 at the St. Petersburg State Mining Institute named after. G.V. Plekhanov (Technical University) at the address: 199106 St. Petersburg, 21st line, no. 2, room. 2205.

The dissertation can be found in the library of the St. Petersburg State Mining Institute.

SCIENTIFIC SECRETARY

dissertation council

Doctor of Technical Sciences, Associate ProfessorV.N.Brichkin

GENERAL DESCRIPTION OF WORK

Relevance of the work

Modern technology needs more and more precious metals. Currently, the extraction of the latter has sharply decreased and does not meet the demand, so it is necessary to use all opportunities to mobilize the resources of these metals, and, consequently, the role of secondary metallurgy of precious metals is increasing. In addition, the extraction of Au, Ag, Pt and Pd contained in waste is more profitable than from ores.

Changes in the economic mechanism of the country, including the military-industrial complex and the armed forces, necessitated the creation in certain regions of the country of factories for processing scrap radio-electronic industry containing precious metals. In this case, it is mandatory to maximize the extraction of precious metals from poor raw materials and reduce the mass of tailings. It is also important that, along with the extraction of precious metals, it is possible to additionally obtain non-ferrous metals, for example, copper, nickel, aluminum and others.

Goal of the work. Increasing the efficiency of pyro-hydrometallurgical technology for processing scrap from the radio-electronic industry with deep extraction of gold, silver, platinum, palladium and non-ferrous metals.

Research methods. To solve the assigned problems, the main experimental studies were carried out on an original laboratory installation, including a furnace with radially located blast nozzles, which made it possible to ensure rotation of the molten metal with air without splashing and thereby greatly increase the supply of blast (in comparison with the supply of air to the molten metal through pipes). Analysis of enrichment, smelting, and electrolysis products was carried out using chemical methods. For the study, the method of X-ray spectral microanalysis (XMA) and X-ray phase analysis (XRF) was used.

Reliability of scientific statements, conclusions and recommendations are due to the use of modern and reliable research methods and are confirmed by the good convergence of theoretical and practical results.

Scientific novelty

The main qualitative and quantitative characteristics of radioelements containing non-ferrous and precious metals have been determined, making it possible to predict the possibility of chemical and metallurgical processing of radio-electronic scrap.

The passivating effect of lead oxide films during the electrolysis of copper-nickel anodes made from radioelectronic scrap has been established. The composition of the films was revealed and the technological conditions for the preparation of anodes were determined to ensure the absence of a passivation effect.

The possibility of oxidation of iron, zinc, nickel, cobalt, lead, and tin from copper-nickel anodes made from radio-electronic scrap was theoretically calculated and confirmed as a result of fire experiments on 75-kilogram melt samples, which ensures high technical and economic indicators of the precious metals recovery technology. The apparent activation energy values for the oxidation of lead in a copper alloy were determined to be 42.3 kJ/mol, tin – 63.1 kJ/mol, iron 76.2 kJ/mol, zinc – 106.4 kJ/mol, nickel – 185.8 kJ/mol.

Practical significance of the work

A technological line for testing radio-electronic scrap has been developed, including departments for disassembly, sorting and mechanical enrichment to obtain metal concentrates;

A technology has been developed for melting radio-electronic scrap in an induction furnace, combined with the effect of oxidizing radial-axial jets on the melt, providing intense mass and heat transfer in the metal melting zone;

A technological scheme for processing radio-electronic scrap and technological waste enterprises, providing individual processing and settlement with each REL supplier.

Novelty technical solutions confirmed by three patents of the Russian Federation: No. 2211420, 2003; No. 2231150, 2004; No. 2276196, 2006

Approbation of work. The materials of the dissertation work were presented at the International Conference “Metallurgical Technologies and Equipment”. April 2003 St. Petersburg; All-Russian scientific and practical conference "New technologies in metallurgy, chemistry, enrichment and ecology." October 2004 St. Petersburg; Annual scientific conference of young scientists “Russian mineral resources and their development” March 9 – April 10, 2004 St. Petersburg; Annual scientific conference of young scientists "Russian mineral resources and their development" March 13-29, 2006 St. Petersburg.

Publications. The main provisions of the dissertation were published in 4 printed works.

Structure and scope of the dissertation. The dissertation consists of an introduction, 6 chapters, 3 appendices, conclusions and a list of references. The work is presented on 176 pages of typewritten text, contains 38 tables, 28 figures. The bibliography includes 117 titles.

The introduction substantiates the relevance of the research and outlines the main provisions submitted for defense.

The first chapter is devoted to a review of literature and patents in the field of technology for processing waste from the radio-electronic industry and methods for processing products containing precious metals. Based on the analysis and synthesis of literature data, the goals and objectives of the research are formulated.

The second chapter provides data on the study of the quantitative and material composition of radio-electronic scrap.

The third chapter is devoted to the development of technology for homogenizing radioelectronic scrap and obtaining metal concentrates for enriching REL.

The fourth chapter presents data on the development of technology for producing metal concentrates of radio-electronic scrap with the extraction of precious metals.

The fifth chapter describes the results of semi-industrial tests on the smelting of metal concentrates of radio-electronic scrap with subsequent processing into cathode copper and noble metal slurry.

The sixth chapter discusses the possibility of improving the technical and economic indicators of processes developed and tested on a pilot scale.

BASIC PROTECTED PROVISIONS

1. Physico-chemical studies of many types of radio-electronic scrap justify the need for preliminary operations of disassembling and sorting waste with subsequent mechanical enrichment, which provides a rational technology for processing the resulting concentrates with the release of non-ferrous and precious metals.

Based on study scientific literature and preliminary studies, the following main operations for processing electronic scrap were considered and tested:

melting scrap in an electric furnace;
leaching of scrap in acid solutions;
roasting of scrap followed by electric smelting and electrolysis of semi-finished products, including non-ferrous and precious metals;
physical enrichment of scrap followed by electrical smelting into anodes and processing of anodes into cathode copper and precious metal slurry.

The first three methods were rejected due to environmental difficulties, which turn out to be insurmountable when using the head operations in question.

The method of physical enrichment was developed by us and consists in the fact that incoming raw materials are sent for preliminary disassembly. At this stage, components containing precious metals are removed from electronic computers and other electronic equipment (Tables 1, 2). Materials that do not contain precious metals are sent for the extraction of non-ferrous metals. Material containing precious metals (printed circuit boards, connectors, wires, etc.) is sorted to remove gold and silver wires, gold-plated PCB side connector pins, and other parts with high precious metal content. These parts can be recycled separately.

Table 1

Balance of electronic equipment at the 1st disassembly site

No.	Name of industrial product	Quantity, kg	Content, %
1	Arrived for recycling Racks of electronic devices, machines, switching equipment	24000,0	100
2 3	Received after recycling Electronic scrap in the form of circuit boards, connectors, etc. Scrap of non-ferrous and ferrous metals, not containing precious metals, plastic, organic glass Total:	4100,0 19900,0	17,08 82,92
2 3		24000,0	100

table 2

Balance of electronic scrap at the 2nd disassembly and sorting site

No.	Name of industrial product	Quantity, kg	Content, %
1	Received for recycling Electronic scrap in the form of (connectors and circuit boards)	4100,0	100
2 3 4 5	Received after manual disassembly and sorting department Connectors Radio components Boards without radio components and accessories (the soldered legs of the radio components and the base contain precious metals) Board latches, pins, board guides (elements that do not contain precious metals) Total:	395,0 1080,0 2015,0 610,0	9,63 26,34 49,15 14,88
2 3 4 5		4100,0	100

Parts such as connectors on a thermosetting and thermoplastic basis, connectors on boards, small boards made of foiled getinax or fiberglass with separate radio components and tracks, capacitors of variable and constant capacity, microcircuits on a plastic and ceramic basis, resistors, ceramic and plastic sockets of radio tubes, fuses , antennas, switches and switches, can be processed by enrichment techniques.

A hammer crusher MD 2x5, a jaw crusher (DShch 100x200) and a cone-inertial crusher (KID-300) were tested as the main unit for the crushing operation.

During the work, it turned out that the cone inertial crusher should only operate under a pile of material, i.e. when the receiving funnel is completely filled. For efficient work cone inertial crusher there is an upper limit on the size of the processed material. Pieces bigger size interfere with the normal operation of the crusher. These shortcomings, the main one of which is the need to mix materials from different suppliers, forced us to abandon the use of KID-300 as the main unit for grinding.

The use of a hammer crusher as a head crushing unit compared to a jaw crusher turned out to be more preferable due to its high productivity when crushing electronic scrap.

It has been established that crushing products include magnetic and non-magnetic metal fractions, which contain the main part of gold, silver, and palladium. To extract the magnetic metal part of the grinding product, a magnetic separator PBSTs 40/10 was tested. It has been established that the magnetic part mainly consists of nickel, cobalt, and iron (Table 3). The optimal productivity of the apparatus was determined, which was 3 kg/min with a gold recovery of 98.2%.

The non-magnetic metal part of the crushed product was separated using an electrostatic separator ZEB 32/50. It has been established that the metal part consists mainly of copper and zinc. Noble metals are represented by silver and palladium. The optimal productivity of the apparatus was determined, which was 3 kg/min with a silver recovery of 97.8%.

When sorting electronic scrap, it is possible to selectively isolate dry multilayer capacitors, which are characterized by a high content of platinum - 0.8% and palladium - 2.8% (Table 3).

Table 3

Composition of concentrates obtained from sorting and processing electronic scrap

N p/p	Content, %
N p/p	Cu	Ni	Co	Zn	Fe	Ag	Au	Pd	Pt	Others	Sum
1	2	3	4	5	6	7	8	9	10	11	12
Silver-palladium concentrates
1	64,7	0,02	sl.	21,4	0,1	2,4	sl.	0,3	0,006	11,8	100,0
Gold concentrates
2	77,3	0,7	0,03	4,5	0,7	0,3	1,3	0,5	0,01	19,16	100,0
Magnetic concentrates
3	sl.	21,8	21,5	0,02	36,3	sl.	0,6	0,05	0,01	19,72	100,0
Concentrates from capacitors
4	0,2	0,59	0,008	0,05	1,0	0,2	No	2,8	0,8	MgO-14.9 CaO-25.6 Sn-2.3 Pb-2.5 R2O3-49.5	100,0

2. The combination of the processes of smelting REL concentrates and electrolysis of the resulting copper-nickel anodes underlies the technology for concentrating noble metals in sludge suitable for processing using standard methods; To increase the efficiency of the method, at the melting stage, slagging of REL impurities is carried out in devices with radially located blow nozzles.

Physico-chemical analysis of radio-electronic scrap parts showed that the parts contain up to 32 chemical elements, while the ratio of copper to the sum of the remaining elements is 5060: 5040.

REL HNO3 concentrates

Solution Precipitate (Au, Sn, Ag, Cu, Ni)

for Au production

Ag to alkaline

Melting solution

recycling

Cu+2, Ni+2, Zn+2, Pd-2

Fig.2. Precious metal extraction scheme

with concentrate leaching

Since most of the concentrates obtained during sorting and enrichment are presented in metallic form, an extraction scheme with leaching in acid solutions was tested. The circuit shown in Figure 2 was tested to produce 99.99% pure gold and 99.99% silver. Gold and silver recovery was 98.5% and 93.8%, respectively. To extract palladium from solutions, the sorption process on synthetic ion-exchange fiber AMPAN H/SO4 was studied.

The sorption results are presented in Figure 3. The sorption capacity of the fiber was 6.09%.

Fig.3. Results of palladium sorption on synthetic fiber

High aggressiveness mineral acids, relatively low silver recovery and the need for recycling large quantity waste solutions narrows the possibilities of using this method to the processing of gold concentrates (the method is ineffective for processing the entire volume of radioelectronic scrap concentrates).

Since copper-based concentrates quantitatively predominate in concentrates (up to 85% of total mass) and the copper content in these concentrates is 50-70%, the possibility of processing the concentrate based on smelting into copper-nickel anodes with their subsequent dissolution was tested in laboratory conditions.

Fig.4. Scheme of extraction of precious metals with smelting

on copper-nickel anodes and electrolysis

The smelting of the concentrates was carried out in the Tammana furnace in graphite-chamotte crucibles. The mass of the melt was 200 g. Copper-based concentrates were melted without complications. Their melting point is in the range of 1200-1250°C. Iron-nickel based concentrates require a temperature of 1300-1350°C to melt. Industrial smelting, carried out at a temperature of 1300°C in an induction furnace with a 100 kg crucible, confirmed the possibility of melting concentrates when the bulk composition of enriched concentrates is fed to the smelting.

The gross content during smelting of radioelectronic scrap enrichment products is characterized by an increased copper content - above 50%, gold, silver and palladium 0.15; 3.4; 1.4%, the total content of nickel, zinc and iron is up to 30%. The anodes are subjected to electrochemical dissolution at a temperature of 400C and a cathodic current density of 200.0 A/m2. The initial electrolyte contains 40 g/l copper, 35 g/l H2SO4. Chemical composition electrolyte, sludge and cathode deposit are given in table 4.

As a result of tests, it was established that during the electrolysis of anodes made from metallized fractions of an electronic scrap alloy, the electrolyte used in the electrolysis bath is depleted in copper, and nickel, zinc, iron, and tin accumulate in it as impurities.

It has been established that palladium under electrolysis conditions is divided into all electrolysis products; Thus, the palladium content in the electrolyte is up to 500 mg/l, the concentration at the cathode reaches 1.4%. A smaller portion of the palladium ends up in the sludge. Tin accumulates in the sludge, which makes it difficult to further process without first removing the tin. Lead goes into sludge and also makes it difficult to recycle. Passivation of the anode is observed. X-ray diffraction and chemical analysis of the top part of the passivated anodes showed that the cause of the observed phenomenon is lead oxide.

Since the lead present in the anode is in metallic form, the following processes occur at the anode:

2OH 2e = H2O + 0.5O2

SO4-2 2e = SO3 + 0.5O2

When the concentration of lead ions in the sulfate electrolyte is insignificant, its normal potential is the most negative, therefore lead sulfate is formed at the anode, which reduces the anode area, as a result of which the anodic current density increases, which promotes the oxidation of divalent lead into tetravalent ions

As a result of hydrolysis, PbO2 is formed according to the reaction:

Pb(SO4)2 + 2H2O = PbO2 + 2H2SO4.

Table 4

Anode dissolution results

Item no.	Product name	Content, %, g/l
Item no.	Product name	Cu	Ni	Co	Zn	Fe	W	Mo	Pd	Au	Ag	Pb	Sn
1	Anode, %	51,2	11,9	1,12	14,4	12,4	0,5	0,03	0,6	0,15	3,4	2,0	2,3
2	Cathode deposit, %	97,3	0,2	0,03	0,24	0,4	No	sl.	1,4	0,03	0,4	No	No
3	Electrolyte, g/l	25,5	6,0	0,4	9,3	8,8	0,9	sl	0,5	0,001	0,5	No	2,9
4	Sludge, %	31,1	0,3	sl	0,5	0,2	2,5	sl.	0,7	1,1	27,5	32,0	4,1

Lead oxide creates a protective layer on the anode, which prevents further dissolution of the anode. The electrochemical potential of the anode was 0.7 V, which leads to the transfer of palladium ions into the electrolyte and its subsequent discharge at the cathode.

The addition of chlorine ion to the electrolyte made it possible to avoid the phenomenon of passivation, but this did not solve the issue of recycling the electrolyte and did not ensure the use of standard sludge processing technology.

The results obtained showed that the technology ensures the processing of radio-electronic scrap, but it can be significantly improved provided that the impurities of the group of metals (nickel, zinc, iron, tin, lead) of the radio-electronic scrap are oxidized and slagged during the smelting of the concentrate.

Thermodynamic calculations, carried out on the assumption that air oxygen enters the furnace bath unlimitedly, showed that impurities such as Fe, Zn, Al, Sn and Pb can be oxidized in copper. Thermodynamic complications during oxidation occur with nickel. Residual nickel concentrations are 9.37% when the copper content in the melt is 1.5% Cu2O and 0.94% when the copper content in the melt is 12.0% Cu2O.

Experimental testing was carried out on a laboratory furnace with a crucible weight of 10 kg for copper with radially located blast nozzles (Table 5), which allows for rotation of the molten metal with air without splashing and thereby greatly increases the blast supply (in comparison with the supply of air into the molten metal through pipes ).

Laboratory studies have established that the composition of the slag plays an important role in the oxidation of metal concentrate. When melting with fluxing, quartz does not transfer tin into slag and the transition of lead is difficult. When using a combined flux consisting of 50% quartz sand and 50% soda, all impurities are transferred to the slag.

Table 5

Results of smelting of metal concentrate from radio-electronic scrap

with radially arranged blow nozzles

depending on purge time

Item no.	Product name	Compound, %
Item no.	Product name	Cu	Ni	Fe	Zn	W	Pb	Sn	Ag	Au	Pd	Others	Total
1	Initial alloy	60,8	8,5	11,0	9,5	0,1	3,0	2,5	4,3	0,10	0,2	0,0	100,0
2	Alloy after 15-minute purging	69,3	6,7	3,5	6,5	0,07	0,4	0,8	4,9	0,11	0,22	7,5	100,0
3	Alloy after 30-minute purging	75,1	5,1	0,1	4,7	0,06	0,3	0,4	5,0	0,12	0,25	8,87	100,0
4	Alloy after 60-minute purging	77,6	3,9	0,05	2,6	0,03	0,2	0,09	5,2	0,13	0,28	9,12	100,0
5	Alloy after 120-minute purging	81,2	2,5	0,02	1,1	0,01	0,1	0,02	5,4	0,15	0,30	9,2	100,0

The results of the melts show that 15 minutes of blowing through the blow nozzles is sufficient to remove a significant part of the impurities. The apparent activation energy for the oxidation reaction in a copper alloy was determined to be 42.3 kJ/mol for lead, 63.1 kJ/mol for tin, 76.2 kJ/mol for iron, 106.4 kJ/mol for zinc, and 185.8 kJ/mol for nickel. mole.

Studies on the anodic dissolution of smelting products have shown that there is no passivation of the anode during electrolysis of the alloy in a sulfuric acid electrolyte after a 15-minute purge. The electrolyte is not depleted in copper and is not enriched with impurities that turned into sludge during melting, which ensures its repeated use. There is no lead or tin in the sludge, which allows the use of standard sludge processing technology according to the following scheme: sludge depuration, alkaline smelting into gold-silver alloy.

Based on the research results, furnace units with radially located blowing nozzles were developed, operating in a periodic mode at 0.1 kg, 10 kg, 100 kg copper, ensuring the processing of batches of electronic scrap of various sizes. At the same time, the entire processing line extracts precious metals without combining batches from various suppliers, which ensures accurate financial payment for the delivered metals. Based on the test results, initial data were developed for the construction of a plant for processing REL with a capacity of 500 kg of gold per year. The enterprise project has been completed. The payback period for capital investments is 7-8 months.

Conclusions

1. The theoretical foundations of a method for processing waste from the radio-electronic industry with deep extraction of noble and non-ferrous metals have been developed.

1.1. Thermodynamic characteristics of the main oxidation processes of metals in a copper alloy have been determined, making it possible to predict the behavior of the mentioned metals and impurities.

1.2. The values of the apparent activation energy of oxidation in a copper alloy were determined to be 185.8 kJ/mol for nickel, 106.4 kJ/mol for zinc, 76.2 kJ/mol for iron, 63.1 kJ/mol for tin, and 42.3 kJ/mol for lead. mole.

2. A pyrometallurgical technology has been developed for processing waste from the radio-electronic industry to produce a gold-silver alloy (Dore metal) and platinum-palladium concentrate.

2.1. Technological parameters have been established (crushing time, productivity of magnetic and electrostatic separation, degree of metal extraction) for the physical enrichment of REL according to the scheme grinding magnetic separation electrostatic separation, which makes it possible to obtain concentrates of noble metals with a predictable quantitative and qualitative composition.

2.2. The technological parameters (melting temperature, air flow, degree of transition of impurities into the slag, composition of the refining slag) of the oxidative smelting of concentrates in an induction furnace with air supplied to the melt by radial-axial tuyeres have been determined; Units with radial-axial lances of various capacities have been developed and tested.

3. Based on the research, a pilot plant for processing radio-electronic scrap was manufactured and put into production, including a grinding section (MD 25 crusher), magnetic and electrostatic separation (PBSTs 40/10 and 3EB 32/50), melting in an induction furnace ( PI 50/10) with a generator SCHG 1-60/10 and a melting unit with radial-axial lances, electrochemical dissolution of anodes and processing of precious metal sludge; the effect of anode “passivation” was studied; The existence of a sharply extreme dependence of the lead content in a copper-nickel anode made from radio-electronic scrap has been established, which should be taken into account when controlling the process of oxidative radial-axial melting.

4. As a result of semi-industrial testing of technology for processing radio-electronic scrap, initial data for the construction of a waste processing plant was developed radio engineering industry.

5. The expected economic effect from the implementation of the dissertation developments based on a gold production capacity of 500 kg/year is ~50 million rubles. with a payback period of 7-8 months.

1. Telyakov A.N. Recycling of waste from electrical engineering enterprises / A.N.Telyakov, D.V.Gorlenkov, E.Yu.Stepanova // Abstracts of the Intern. conf. "Metallurgical technologies and ecology." 2003.

2. Telyakov A.N. Results of tests of technology for processing radio-electronic scrap / A.N.Telyakov, L.V.Ikonin // Notes of the Mining Institute. T. 179. 2006.

3. Telyakov A.N. Research on the oxidation of impurities in radioelectronic scrap metal concentrate // Notes of the Mining Institute. T. 179. 2006.

4. Telyakov A.N. Technology for processing waste from the radio-electronic industry / A.N.Telyakov, D.V.Gorlenkov, E.Yu.Georgieva // Non-ferrous metals. No. 6. 2007.

480 rub. | 150 UAH | $7.5 ", MOUSEOFF, FGCOLOR, "#FFFFCC",BGCOLOR, "#393939");" onMouseOut="return nd();"> Dissertation - 480 RUR, delivery 10 minutes, around the clock, seven days a week and holidays

Telyakov Alexey Nailievich. Development effective technology extraction of non-ferrous and precious metals from waste of the radio engineering industry: dissertation... Candidate of Technical Sciences: 05.16.02 St. Petersburg, 2007 177 pp., Bibliography: p. 104-112 RSL OD, 61:07-5/4493

Introduction

Chapter 1. Literature Review 7

Chapter 2. Study of the material composition of radio-electronic scrap 18

Chapter 3. Development of technology for averaging radio-electronic scrap 27

3.1. Burning radio-electronic scrap 27

3.1.1. Information about plastics 27

3.1.2. Technological calculations for the utilization of roasting gases 29

3.1.3. Roasting radio-electronic scrap in a lack of air 32

3.1.4. Firing radio-electronic scrap in a tube furnace 34

3.2 Physical methods recycling electronic scrap 35

3.2.1. Description of processing area 36

3.2.2. Technological diagram of enrichment section 42

3.2.3. Development of enrichment technology on industrial units 43

3.2.4. Determination of the productivity of units of the enrichment site when processing radio-electronic scrap 50

3.3. Industrial tests of enrichment of radio-electronic scrap 54

3.4. Conclusions to Chapter 3 65

Chapter 4. Development of technology for processing radio-electronic scrap concentrates . 67

4.1. Research on the processing of REL concentrates in acid solutions... 67

4.2. Testing the technology for producing concentrated gold and silver 68

4.2.1. Testing the technology for producing concentrated gold 68

4.2.2. Testing the technology for producing concentrated silver... 68

4.3. Laboratory studies on the extraction of gold and silver REL by smelting and electrolysis 69

4.4. Development of technology for extracting palladium from sulfuric acid solutions. 70

4.5. Conclusions to Chapter 4 74

Chapter 5. Pilot tests on smelting and electrolysis of radio-electronic scrap concentrates 75

5.1. Smelting of metal concentrates REL 75

5.2. Electrolysis of smelting products REL 76

5.3. Conclusions to Chapter 5 81

Chapter 6. Study of oxidation of impurities during melting of radio-electronic scrap 83

6.1. Thermodynamic calculations of impurity oxidation REL 83

6.2. Study of the oxidation of impurities in REL 88 concentrates

6.2. Study of the oxidation of impurities in REL 89 concentrates

6.3. Pilot tests on oxidative smelting and electrolysis of REL 97 concentrates

6.4. Chapter 102 Conclusions

Conclusions on work 103

Literature 104

Introduction to the work

Relevance of the work

Modern technology requires more and more precious metals. Currently, the extraction of the latter has sharply decreased and does not meet the demand, so it is necessary to use all opportunities to mobilize the resources of these metals, and, consequently, the role of secondary metallurgy of precious metals is increasing. In addition, the extraction of Au, Ag, Pt and Pd contained in waste is more profitable than from ores.

Changes in the economic mechanism of the country, including the military-industrial complex and the armed forces, have necessitated the creation in certain regions of the country of complexes for processing radio-electronic industry scrap containing precious metals. In this case, it is mandatory to maximize the extraction of precious metals from poor raw materials and reduce the mass of tailings. It is also important that, along with the extraction of precious metals, it is possible to additionally obtain non-ferrous metals, for example, copper, nickel, aluminum and others.

The purpose of the work is the development of technology for the extraction of gold, silver, platinum, palladium and non-ferrous metals from scrap electronics industry and technological waste from enterprises.

Main provisions submitted for defense

Preliminary sorting of REL with subsequent mechanical enrichment ensures the production of metal alloys with increased extraction of precious metals.

Physico-chemical analysis of radio-electronic scrap parts showed that the parts are based on up to 32 chemical elements, while the ratio of copper to the sum of the remaining elements is 50-g60: 50-o.

The low dissolution potential of copper-nickel anodes obtained by melting electronic scrap makes it possible to obtain

5 precious metal sludge suitable for processing using standard technology.

Research methods. Laboratory, enlarged laboratory, industrial tests; analysis of enrichment, smelting, and electrolysis products was carried out using chemical methods. For the study, the method of X-ray spectral microanalysis (XMA) and X-ray phase analysis (XRF) was used using the DRON-06 installation.

Validity and reliability of scientific statements, conclusions and recommendations are due to the use of modern and reliable research methods and are confirmed by the good convergence of the results of complex studies performed in laboratory, large-scale laboratory and industrial conditions.

Scientific novelty

Practical significance of the work

A technological line for testing radio-electronic scrap has been developed, including departments for disassembly, sorting, mechanical

enrichment of smelting and analysis of noble and non-ferrous metals;

A technology has been developed for melting radio-electronic scrap in induction
oven, combined with the effect on the melt of oxidative radial
but-axial jets, providing intense mass and heat transfer in the zone
metal melting;

Developed and tested on a pilot scale
logical scheme for processing radio-electronic scrap and technological materials
progress of enterprises, providing individual processing and settlement with
each REL supplier.

Approbation of work. The dissertation materials were presented: at the International Conference “Metallurgical Technologies and Equipment”, April 2003, St. Petersburg; All-Russian scientific and practical conference “New technologies in metallurgy, chemistry, enrichment and ecology”, October 2004, St. Petersburg; annual scientific conference of young scientists “Minerals of Russia and their development” March 9 - April 10, 2004, St. Petersburg; annual scientific conference of young scientists "Russian mineral resources and their development" March 13-29, 2006, St. Petersburg.

Publications. The main provisions of the dissertation were published in 7 published works, including 3 patents for inventions.

The materials of this work present the results of laboratory studies and industrial processing of waste containing precious metals at the stages of disassembly, sorting and enrichment of radio-electronic scrap, smelting and electrolysis, carried out in the industrial conditions of the SKIF-3 enterprise at the sites of the Russian Scientific Center "Applied Chemistry" and a mechanical plant them. Karl Liebknecht.

Study of the material composition of radio-electronic scrap

Currently, there is no domestic technology for processing poor radio-electronic scrap. Purchasing a license from Western companies is impractical due to the dissimilarity of laws on precious metals. Western companies can buy electronic scrap from suppliers, store and accumulate the volume of scrap to a value that corresponds to the scale of the production line. The resulting precious metals are the property of the manufacturer.

In our country, according to the terms of monetary settlements with scrap suppliers, each batch of waste from each deliverer, regardless of its size, must undergo a full technological testing cycle, including opening of parcels, checking net and gross masses, averaging of raw materials by composition (mechanical, pyrometallurgical, chemical) and selection of head samples , sampling from by-products of averaging (slag, insoluble sediments, wash waters, etc.), encryption, analysis, decoding of samples and certification of analysis results, calculation of the amount of precious metals in a batch, their acceptance on the balance sheet of the enterprise and registration of all accounting and settlement documentation.

After receiving semi-products concentrated in precious metals (for example, Dore metal), the concentrates are delivered to a state refinery, where, after refining, the metals are sent to Gokhran, and payment for their cost is sent through the reverse financial chain up to the supplier. It becomes obvious that for processing enterprises to operate successfully, each batch from a supplier must go through the entire technological cycle separately from materials from other suppliers.

Analysis of the literature showed that one of possible ways averaging of radio-electronic scrap is its firing at a temperature that ensures the combustion of plastics included in the REL, after which it is possible to melt the sinter, obtain an anode, followed by electrolysis.

Synthetic resins are used to make plastics. Synthetic resins, depending on the reaction of their formation, are divided into polymerized and condensed. There are also thermoplastic and thermosetting resins.

Thermoplastic resins can melt repeatedly when reheated without losing their plastic properties, these include: polyvinylacetate, polystyrene, polyvinyl chloride, condensation products of glycol with dibasic carboxylic acids, etc.

Thermosetting resins - when heated, they form infusible products, these include phenol-aldehyde and urea-formaldehyde resins, condensation products of glycerol with polybasic acids, etc.

Many plastics consist only of polymer, these include: polyethylenes, polystyrenes, polyamide resins, etc. Most plastics (phenoplasts, amioplastics, wood plastics, etc.) in addition to the polymer (binder) may contain: fillers, plasticizers, binding hardening and coloring agents, stabilizers and other additives. The following plastics are used in electrical engineering and electronics: 1. Phenolic plastics - plastics based on phenolic resins. Phenoplasts include: a) cast phenoplasts - hardened resins of the resol type, for example bakelite, carbolite, neoleukorite, etc.; b) layered phenolics - for example, a pressed product made of fabric and resol resin, called textolite. Phenol-aldehyde resins are obtained by condensation of phenol, cresol, xylene, alkylphenol with formaldehyde, furfural. In the presence of basic catalysts, resol (thermosetting) resins are obtained, in the presence of acidic catalysts, novolac (thermoplastic resins) are obtained.

Technological calculations for the utilization of roasting gases

All plastics mainly consist of carbon, hydrogen and oxygen, with valency being replaced by additives of chlorine, nitrogen, and fluorine. Consider, as an example, the burning of textolite. Textolite is a highly flammable material and is one of the components of electronic scrap. It consists of pressed cotton fabric impregnated with artificial resole (formaldehyde) resins. Morphological composition of radio-technical textolite: - cotton fabric - 40-60% (average - 50%) - resol resin - 60-40% (average -50%) Gross formula of cotton cellulose [SbN702(OH)z]z, and resol resin - (Cg H702)-m, where m is the coefficient corresponding to the products of the degree of polymerization. According to literature data, with an ash content of textolite of 8%, the humidity will be 5%. The chemical composition of the textolite in terms of the working mass will be, %: Cp-55.4; Hp-5.8; OP-24.0; Sp-0.l; Np-I.7; Fp-8.0; Wp- 5.0.

When 1 t/hour of textolite is burned, 0.05 t/hour of moisture evaporation and 0.08 t/hour of ash are formed. At the same time, it is supplied for combustion, t/hour: C - 0.554; N - 0.058; 0-0.24; S-0.001, N-0.017. Composition of textolite ash grades A, B, R according to literature data,%: CaO -40.0; Na, K20 - 23.0; Mg O - 14.0; РпО10 - 9.0; Si02 - 8.0; Al 203 - 3.0; Fe203 -2.7; SO3 -0.3. To carry out the experiments, firing was chosen in a sealed chamber without air access; for this purpose, a box measuring 100x150x70 mm with a flange fastening of the lid was made of stainless steel 3 mm thick. The lid was attached to the box through an asbestos gasket with bolted connections. Fitting holes were made in the end surfaces of the box, through which the contents of the retort were purged with inert gas (N2) and gas products of the process were removed. The following samples were used as test samples: 1. Boards cleared of radioelements, sawn to dimensions of 20x20 mm. 2. Black microcircuits from boards (full size 6x12 mm) 3. Connectors made of textolite (sawed to sizes 20x20 mm) 4. Connectors made of thermosetting plastic (cut to sizes 20x20 mm) The experiment was carried out as follows: 100 g of the test sample was loaded into the retort , was closed with a lid and placed in a muffle. The contents were purged with nitrogen for 10 minutes at a flow rate of 0.05 l/min. Throughout the experiment, nitrogen flow was maintained at 20-30 cm3/min. The exhaust gases were neutralized with an alkaline solution. The muffle shaft was closed with brick and asbestos. The temperature rise was regulated within 10-15C per minute. Upon reaching 600C, an hour-long exposure was carried out, after which the furnace was turned off and the retort was removed. During cooling, the nitrogen flow rate increased to 0.2 l/min. The observation results are presented in Table 3.2.

The main negative factor of the process is a very strong, pungent, unpleasant odor, released both from the cinder itself and from the equipment, which was “saturated” with this odor after the first experiment.

For the study, a continuous tubular rotary kiln with indirect electric heating was used with a charge capacity of 0.5-3.0 kg/hour. The furnace consists of a metal casing (length 1040 mm, diameter 400 mm), lined with refractory bricks. The heaters are 6 silit rods with a working part length of 600 mm, powered by two RNO-250 voltage variators. The reactor (total length 1560 mm) is a stainless steel pipe with an outer diameter of 89 mm lined with a porcelain pipe with an inner diameter of 73 mm. The reactor rests on 4 rollers and is equipped with a drive consisting of an electric motor, gearbox and belt drive.

To control the temperature in the reaction zone, a thermocouple complete with a portable potentiometer installed inside the reactor is used. Previously, its readings were adjusted based on direct measurements of the temperature inside the reactor.

Radio-electronic scrap was manually loaded into the oven at the ratio: boards cleared of radio elements: black microcircuits: PCB connectors: thermoplastic resin connectors = 60:10:15:15.

This experiment was carried out on the assumption that the plastic would burn before it melted, which would release the metal contacts. This turned out to be unattainable, since the problem of a strong odor remains, and as soon as the connectors reached the temperature zone of 300C, the thermoplastic plastic connectors stuck to the inner surface of the rotary kiln and blocked the passage of the entire mass of electronic scrap. Forced air supply into the furnace and an increase in temperature in the sticking zone did not lead to the possibility of firing.

Thermosetting plastic is also characterized by high viscosity and strength. A characteristic of these properties is that when cooled in liquid nitrogen for 15 minutes, thermoset plastic connectors were broken on an anvil using a ten-kilogram hammer, and no destruction of the connectors occurred. Considering that the number of parts made from such plastics is small and they can be easily cut using a mechanical tool, it is advisable to disassemble them manually. For example, cutting or cutting connectors along the central axis results in the release of the metal contacts from the plastic base.

The range of electronic industry scrap supplied for processing covers all parts and assemblies of various units and devices in the manufacture of which precious metals are used.

The base of a product containing precious metals, and accordingly their scrap, can be made of plastic, ceramics, fiberglass, multilayer material (BaTiO3) and metal.

Raw materials arriving from supplying enterprises are sent for preliminary disassembly. At this stage, components containing precious metals are removed from electronic computers and other electronic equipment. They make up about 10-15% of the total mass of computers. Materials that do not contain precious metals are used for the extraction of non-ferrous and ferrous metals. Waste material containing precious metals (printed circuit boards, connectors, wires, etc.) is sorted to remove gold and silver wires, gold-plated PCB side connector pins, and other parts with a high precious metal content. Selected parts go directly to the precious metals refining site.

Testing the technology for producing concentrated gold and silver

A sample of golden sponge weighing 10.10 g was dissolved in aqua regia by evaporation with hydrochloric acid got rid of nitric acid and precipitated metallic gold with a saturated solution of iron (I) sulfate prepared from carbonyl iron dissolved in sulfuric acid. The precipitate was washed repeatedly by boiling with distilled HC1 (1:1) and water, and gold powder was dissolved in aqua regia, prepared from acids distilled in a quartz vessel. The precipitation and washing operation was repeated and a sample was taken for emission analysis, which showed a gold content of 99.99%.

To carry out a material balance, the remains of samples selected for analysis (1.39 g Au) and gold from burnt filters and electrodes (0.48 g) were combined and weighed; irrecoverable losses amounted to 0.15 g, or 1.5% of the processed material . Such a high percentage of losses is explained by the small amount of gold involved in processing and the costs of the latter in debugging analytical operations.

Ingots of silver isolated from the contacts were dissolved by heating in concentrated nitric acid, the solution was evaporated, cooled and drained from the precipitated salt crystals. The resulting nitrate precipitate was washed with distilled nitric acid, dissolved in water and the metal was precipitated in the form of chloride with hydrochloric acid. The decanted mother liquor was used to develop the technology for refining silver by electrolysis.

The silver chloride precipitate that had settled for 24 hours was washed with nitrogenous acid and water, dissolved in excess aqueous ammonia and filtered. The filtrate was treated with excess hydrochloric acid until the formation of precipitate ceased. The latter was washed with cooled water and alkaline smelting, metallic silver was isolated, which was etched with boiling HC1, washed with water and melted with boric acid. The resulting ingot was washed with hot HCI (1:1), water, dissolved in hot nitric acid, and the entire cycle of silver separation through chloride was repeated. After melting with flux and washing with hydrochloric acid, the ingot was remelted twice in a pyrographite crucible with intermediate operations to clean the surface with hot hydrochloric acid. After this, the ingot was rolled into a plate, its surface was etched with hot HC1 (1:1) and a flat cathode was made for purifying silver by electrolysis.

Metallic silver was dissolved in nitric acid, the acidity of the solution was adjusted to 1.3% in HNO3, and electrolysis of this solution was carried out with a silver cathode. The operation was repeated, and the resulting metal was fused in a pyrographite crucible into an ingot weighing 10.60 g. Analysis in three independent organizations showed that the mass fraction of silver in the ingot was at least 99.99%.

From a large number of works on the extraction of noble metals from intermediate products, we chose for testing the method of electrolysis in a solution of copper sulfate.

62 g of metal contacts from the connectors were alloyed with borax and a flat ingot weighing 58.53 g was cast. The mass fraction of gold and silver is 3.25% and 3.1%, respectively. A portion of the ingot (52.42 g) was electrolyzed as an anode in a solution of copper sulfate acidified with sulfuric acid, resulting in 49.72 g of anode material dissolving. The resulting sludge was separated from the electrolyte and after fractional dissolution in nitric acid and aqua regia, 1.50 g of gold and 1.52 g of silver were isolated. After burning the filters, 0.11 g of gold was obtained. The losses of this metal amounted to 0.6%; irreversible loss of silver - 1.2%. The phenomenon of the appearance of palladium in the solution (up to 120 mg/l) has been established.

During the electrolysis of copper anodes, the precious metals contained therein are concentrated in sludge, which falls to the bottom of the electrolysis bath. However, a significant (up to 50%) transition of palladium into the electrolyte solution is observed. To cover the beginning of palladium losses, this work was performed.

The difficulty of extracting palladium from electrolytes is due to their complex composition. There are known works on sorption-extraction processing of solutions. The goal of the work is to obtain pure palladium sulfates and return the purified electrolyte to the process. To solve this problem, we used the process of sorption of metals on synthetic ion-exchange fiber AMPAN H/SO4. Two solutions were used as initial solutions: No. 1 - containing (g/l): 0.755 palladium and 200 sulfuric acid; No. 2 - containing (g/l): palladium 0.4, copper 38.5, iron - 1.9 and 200 sulfuric acid. To prepare the sorption column, 1 gram of AMPAN fiber was weighed, placed in a column with a diameter of 10 mm, and the fiber was soaked in water for 24 hours.

Development of technology for extracting palladium from sulfuric acid solutions

The solution was supplied from below using a dosing pump. During the experiments, the volume of the passed solution was recorded. Samples taken at regular intervals were analyzed by the atomic adsorption method for palladium content.

The experimental results showed that palladium sorbed on the fiber is desorbed by a solution of sulfuric acid (200 g/l).

Based on the results obtained when studying the processes of sorption-desorption of palladium on solution No. 1, an experiment was carried out to study the behavior of copper and iron in quantities close to their content in the electrolyte during the sorption of palladium on the fiber. The experiments were carried out according to the scheme presented in Fig. 4.2 (Table 4.1-4.3), which includes the process of sorption of palladium from solution No. 2 on the fiber, washing of palladium from copper and iron with a solution of 0.5 M sulfuric acid, desorption of palladium with a solution of 200 g/ l sulfuric acid and washing the fiber with water (Fig. 4.3).

The beneficiation products obtained at the beneficiation site of the SKIF-3 enterprise were taken as the initial raw material for the melts. The melting was carried out in the Tammana furnace at a temperature of 1250-1450C in graphite-fireclay crucibles with a volume of 200 g (for copper). Table 5.1 presents the results of laboratory melts of various concentrates and their mixtures. The concentrates, the compositions of which are presented in Tables 3.14 and 3.16, melted without complications. Concentrates, the composition of which is presented in Table 3.15, require a temperature in the range of 1400-1450C for melting. mixtures of these materials L-4 and L-8 require a temperature of about 1300-1350C for melting.

Industrial smelting P-1, P-2, P-6, carried out in an induction furnace with a crucible with a volume of 75 kg for copper, confirmed the possibility of melting concentrates when the bulk composition of enriched concentrates was fed to the smelting.

During the research, it turned out that part of the electronic scrap is melted with large losses of platinum and palladium (concentrates from REL capacitors, Table 3.14). The loss mechanism was determined by adding contacts to the surface of a copper molten bath with surface sputtering of silver and palladium on them (palladium content in contacts 8.0-8.5%). In this case, the copper and silver were melted, leaving a palladium shell of the contacts on the surface of the bath. An attempt to mix palladium into the bath resulted in the destruction of the shell. Some of the palladium flew off the surface of the crucible before it had time to dissolve in the copper bath. Therefore, all subsequent melts were carried out with a synthetic cover slag (50% S1O2 + 50% soda).

Kozyrev, Vladimir Vasilievich

Abstract of the dissertation on the topic "Development of an effective technology for the extraction of non-ferrous and precious metals from waste from the radio engineering industry"

As a manuscript

TELYAKOV Alexey Nailievich

DEVELOPMENT OF EFFECTIVE TECHNOLOGY

EXTRACTION OF NON-FERROUS AND NOBLE METALS FROM RADIO ENGINEERING INDUSTRY WASTES

Specialty 05.16.02 - Ferrous and non-ferrous metallurgy

SAINT PETERSBURG 2007

The work was carried out at the state educational institution of higher professional education, St. Petersburg State Mining Institute named after G.V. Plekhanov (Technical University).

Scientific supervisor - Doctor of Technical Sciences, Professor, Honored Scientist of the Russian Federation

The leading enterprise is the Gipronickel Institute.

The defense of the dissertation will take place on November 13, 2007 at 14:30 at a meeting of the dissertation council D 212.224.03 at the St. Petersburg State Mining Institute named after G.V. Plekhanov (Technical University) at the address: 199106 St. Petersburg, 21st line , building 2, room. 2205.

The dissertation can be found in the library of the St. Petersburg State Mining Institute.

Sizyakov V.M.

Official opponents: Doctor of Technical Sciences, Professor

Belogazoe I.N.

Candidate of Technical Sciences, Associate Professor

Baymakov A.Yu.

SCIENTIFIC SECRETARY

Dissertation Council Doctor of Technical Sciences, Associate Professor

V.N.BRICHKIN

GENERAL DESCRIPTION OF WORK

Relevance of the work

Modern technology requires an increasing amount of noble metals. Currently, the extraction of the latter has sharply decreased and does not meet the demand, so it is necessary to use all opportunities to mobilize the resources of these metals, and, consequently, the role of secondary metallurgy of noble metals is increasing. In addition, the extraction of Au, Ag, Р1 and Рс1 contained in waste are more profitable than from ores

Changes in the economic mechanism of the country, including the military-industrial complex and the armed forces, have necessitated the creation in certain regions of the country of factories for processing radio-electronic industry scrap containing precious metals. At the same time, the maximum extraction of precious metals from poor raw materials and reducing the mass of tailings is also essential. the fact that, along with the extraction of precious metals, it is possible to additionally obtain non-ferrous metals, for example, copper, nickel, aluminum and others

Goal of the work. Increasing the efficiency of pyro-hydrometallurgical technology for processing scrap from the radio-electronic industry with deep extraction of gold, silver, platinum, palladium and non-ferrous metals

Research methods. To solve the assigned problems, the main experimental studies were carried out on an original laboratory installation, including a furnace with radially located blast nozzles, which made it possible to ensure rotation of the molten metal with air without splashing and thereby greatly increase the supply of blast (in comparison with the supply of air to the molten metal through pipes). Analysis of enrichment, smelting, and electrolysis products was carried out using chemical methods. The X-ray spectroscopic method was used for the study.

tral microanalysis (RSMA) and X-ray phase analysis (XRF).

The reliability of scientific statements, conclusions and recommendations is determined by the use of modern and reliable research methods and is confirmed by the good convergence of theoretical and practical results.

Scientific novelty

The possibility of oxidation of iron, zinc, nickel, cobalt, lead, tin from copper-nickel anodes made from radio-electronic scrap was theoretically calculated and confirmed as a result of fire experiments on 75-kg melt samples, which ensures high technical and economic indicators of the technology for the return of noble metals Defined values of apparent activation energy for oxidation in a copper alloy of lead - 42.3 kJ/mol, tin - 63.1 kJ/mol, iron 76.2 kJ/mol, zinc - 106.4 kJ/mol, nickel - 185.8 kJ /mol.

A technological line for testing radio-electronic scrap has been developed, including departments for disassembly, sorting and mechanical enrichment to obtain metal concentrates,

A technology has been developed for melting radio-electronic scrap in an induction furnace, combined with exposing the melt to oxide-

casting radial-axial jets, providing intense mass and heat transfer in the metal melting zone,

The novelty of technical solutions is confirmed by three RF patents No. 2211420, 2003; No. 2231150, 2004, No. 2276196, 2006

Approbation of the work The materials of the dissertation work were presented at the International Conference “Metallurgical Technologies and Equipment”. April 2003 St. Petersburg, All-Russian scientific and practical conference “New technologies in metallurgy, chemistry, enrichment and ecology” October 2004 St. Petersburg; Annual scientific conference of young scientists "Russian mineral resources and their development" March 9 - April 10, 2004 St. Petersburg, Annual scientific conference of young scientists "Russian mineral resources and their development" March 13-29, 2006 St. Petersburg

Publications. The main provisions of the dissertation were published in 4 printed works

Structure and scope of the dissertation. The dissertation consists of an introduction, 6 chapters, 3 appendices, conclusions and a list of references. The work is presented on 176 pages of typewritten text, contains 38 tables, 28 figures. Bibliography includes 117 titles

The introduction substantiates the relevance of the research and outlines the main provisions put forward for defense.

The second chapter provides data on the study of the quantitative and material composition of radio-electronic scrap

The third chapter is devoted to the development of technology for homogenizing radioelectronic scrap and obtaining metal concentrates for enriching REL.

The fourth chapter presents data on the development of technology for obtaining metal concentrates of radio-electronic scrap with the extraction of precious metals

The fifth chapter describes the results of semi-industrial tests on the smelting of metal concentrates of radio-electronic scrap with subsequent processing into cathode copper and noble metal slurry

The sixth chapter discusses the possibility of improving the technical and economic indicators of processes developed and tested on a pilot scale.

BASIC PROTECTED PROVISIONS

1. Physico-chemical studies of many types of radio-electronic scrap justify the need for preliminary operations of disassembly and sorting of waste followed by mechanical enrichment, which provides a rational technology for processing the resulting concentrates with the release of non-ferrous and precious metals.

Based on the study of scientific literature and preliminary research, the following main operations for processing radio-electronic scrap-1 were considered and tested. melting scrap in an electric furnace,

2 leaching of scrap in acid solutions;

3 roasting of scrap followed by electric smelting and electrolysis of semi-finished products, including non-ferrous and precious metals,

4 physical enrichment of scrap followed by electrical smelting into anodes and processing of anodes into cathode copper and precious metal slurry.

The first three methods were rejected due to environmental difficulties, which turn out to be insurmountable when using the head operations in question.

The method of physical enrichment was developed by us and consists in the fact that the incoming raw materials are sent for preliminary disassembly. At this stage, components containing precious metals are removed from electronic computers and other electronic equipment (Tables 1, 2). Materials that do not contain precious metals are sent for extraction non-ferrous metals Material containing precious metals (printed circuit boards, connectors, wires, etc.) is sorted to remove gold and silver wires, gold-plated PCB side connector pins and other parts with a high precious metal content. These parts can be recycled separately.

Table 1

Balance of electronic equipment at the 1st disassembly site

No. Name of industrial product Quantity, kg Content, %

1 Received for recycling Racks of electronic devices, machines, switching equipment 24000.0 100

2 3 Received after processing Electronic scrap in the form of circuit boards, connectors, etc. Scrap of non-ferrous and ferrous metals, not containing precious metals, plastic, organic glass Total 4100.0 19900.0 17.08 82.92

table 2

Balance of electronic scrap at the 2nd disassembly and sorting site

p/n Name of industrial product Quantity- Contents-

value, kg, %

Received for processing

1 Electronic scrap in the form of (connectors and boards) 4100.0 100

Received after manual separation

disassembly and sorting

2 Connectors 395.0 9.63

3 Radio components 1080.0 26.34

4 Boards without radio components and accessories (at VPA- 2015.0 49.15

on the legs of radio components and on the floor

noble metals hold)

Board latches, pins, board guides (electronic

5 ments not containing noble metals) 610.0 14.88

Total 4100.0 100

Parts such as connectors on thermosetting and thermoplastic bases, connectors on boards, small boards made of fabricated getinax or fiberglass with separate radio components and tracks, capacitors of variable and constant capacitance, microcircuits on plastic and ceramic bases, resistors, ceramic and plastic sockets of radio tubes , fuses, antennas, switches and switches can be processed by enrichment techniques.

A hammer crusher MD 2x5, a jaw crusher (DShch 100x200) and a cone-inertia crusher (KID-300) were tested as the main unit for the crushing operation.

During the work, it turned out that the cone inertial crusher should only operate under a pile of material, that is, when the receiving funnel is completely filled. For a cone inertia crusher to operate efficiently, there is an upper limit to the size of the processed material. Larger pieces interfere with the normal operation of the crusher. These disadvantages, the main one of which is the need to mix materials of different

suppliers were forced to abandon the use of KID-300 as the main unit for grinding.

The use of a hammer crusher as a head crushing unit compared to a jaw crusher turned out to be more preferable due to its high productivity when crushing electronic scrap

It has been established that crushing products include magnetic and non-magnetic metal fractions, which contain the main part of gold, silver, and palladium. To extract the magnetic metal part of the grinding product, a magnetic separator PBSTS 40/10 was tested. It was found that the magnetic part mainly consists of nickel, cobalt, and iron (Table 3). The optimal performance of the apparatus was determined, which was 3 kg/min when extracting gold 98.2 %

The non-magnetic metal part of the crushed product was separated using an electrostatic separator ZEB 32/50. It was established that the metal part consists mainly of copper and zinc. Noble metals are represented by silver and palladium. The optimal productivity of the apparatus was determined, which was 3 kg/min with a silver recovery of 97.8%.

When sorting electronic scrap, it is possible to selectively isolate dry multilayer capacitors, which are characterized by a high content of platinum - 0.8% and palladium - 2.8% (Table 3)

Table 3

Composition of concentrates obtained from sorting and processing electronic scrap

Si No. Co 1xx Re AN Ai Rc1 14 Other Amount

1 2 3 4 5 6 7 8 9 10 11 12

Silver-palladium concentrates

1 64.7 0.02 cl 21.4 od 2.4 cl 0.3 0.006 11.8 100.0

2 77,3 0,7 0,03 4,5 0,7 0,3 1,3 0,5 0,01 19,16 100,0

Magnetic concentrates

3 lines 21.8 21.5 0.02 36.3 lines 0.6 0.05 0.01 19.72 100.0

Concentrates from capacitors

4 0.2 0.59 0.008 0.05 1.0 0.2 no 2.8 0.8 M£0-14.9 CaO-25.6 8n-2.3 Pb-2.5 11203-49, 5 100.0

Fig. 1 Agcharature-technological scheme for enrichment of radio-electronic scrap

1- hammer crusher MD- 2x5; 2-tooth-roll crusher 210 DR, 3-vibrating screen VG-50, 4-high separator PBSTs-40/Yu; 5- electrostatic separator ZEB-32/50

2. The combination of the processes of smelting REL concentrates and electrolysis of the resulting copper-nickel anodes underlies the technology for concentrating noble metals in slurries suitable for processing using standard methods; To increase the efficiency of the method, at the melting stage, slagging of REL impurities is carried out in devices with radially located blow nozzles.

Physico-chemical analysis of radio-electronic scrap parts showed that the parts contain up to 32 chemical elements, while the ratio of copper to the sum of the remaining elements is 50-M50 50-40.

REL SHOya concentrates

U........................... . ■ .- ...I II." h

Leaching

xGpulpa

Filtration

I Solution I Precipitate (Au, VP, Ad, Cu, N1) --■ for the production of Au

Ag deposition

Filtration

Disposal solution^ Cu+2, M+2.2n+\PcG2

"TAd on alkaline ▼ pl

Fig. 2 Scheme of extraction of precious metals with concentrate leaching

The sorption results are presented in Figure 3. The sorption capacity of the fiber was 6.09%.

Fig.3. Results of palladium sorption on synthetic fiber

The high aggressiveness of mineral acids, relatively low silver recovery and the need to dispose of a large amount of waste solutions narrows the possibilities of using this method to the processing of gold concentrates (the method is ineffective for processing the entire volume of radioelectronic scrap concentrates).

Since the concentrates are quantitatively dominated by copper-based concentrates (up to 85% of the total mass) and the copper content in these concentrates is 50-70%, in laboratory tests

In this work, the possibility of processing the concentrate based on smelting into copper-nickel anodes with their subsequent dissolution was tested.

Radioelectronic scrap concentrates

Electrolyte I-\

-[ Electrolysis |

Sludge of noble cathode metals copper

Fig. 4 Scheme of extraction of noble metals with smelting for copper-nickel anodes and electrolysis

The melting of the concentrates was carried out in a Tammana furnace in graphite-chamotte crucibles. The mass of the melt was 200 g. Copper-based concentrates were melted without any complications. Their melting point is in the range of 1200-1250°C. Concentrates on an iron-nickel base require a temperature of 1300-1350°C for melting. Industrial smelting, carried out at a temperature of 1300°C in an induction furnace with a 100 kg crucible, confirmed the possibility of melting concentrates when the bulk composition of enriched concentrates is fed to the smelting.

contains 40 g/l copper, 35 g/l H2804. The chemical composition of the electrolyte, sludge and cathode deposit is given in Table 4

It has been established that palladium under electrolysis conditions is divided into all electrolysis products, so the palladium content in the electrolyte is up to 500 mg/l, the concentration at the cathode reaches 1.4%. A smaller part of the palladium goes into the sludge. Tin accumulates in the sludge, which complicates its further processing without first removing the tin. Lead goes into the sludge and also complicates its processing. Passivation of the anode is observed. X-ray diffraction and chemical analysis of the upper part of passivated anodes showed that the cause of the observed phenomenon is lead oxide.

Since the lead present in the anode is in metallic form, the following processes occur at the anode.

Pb - 2e = Pb2+

20Н - 2е = Н20 + 0.502 804 "2 - 2е = 8<Э3 + 0,502

When the concentration of fistula ions in the sulfuric acid electrolyte is insignificant, its normal potential is the most negative, therefore lead sulfate is formed on the anode, which reduces the anode area, as a result of which the anodic current density increases, which promotes the oxidation of divalent lead into tetravalent ions

Pb2+ - 2e = Pb4+

As a result of hydrolysis, the formation of PIO2 occurs according to the reaction.

Pb(804)2 + 2H20 = Pb02 + 2H2804

Table 4

Anode dissolution results

No. Product name Content, %, g/l

Si No. Co Xp Be Mo R<1 Аи РЬ Бп

1 Anode, % 51.2 11.9 1.12 14.4 12.4 0.5 0.03 0.6 0.15 3.4 2.0 2.3

2 Cathode deposit, % 97.3 0.2 0.03 0.24 0.4 no sl 1.4 0.03 0.4 no no

3 Electrolyte, g/l 25.5 6.0 0.4 9.3 8.8 0.9 sl 0.5 0.001 0.5 no 2.9

4 Sludge, % 31.1 0.3 cl 0.5 0.2 2.5 cl 0.7 1.1 27.5 32.0 4.1

Thermodynamic calculations, carried out on the assumption that air oxygen enters the furnace bath unlimitedly, have shown that impurities such as Fe, Chn, Al, Si and Pb can be oxidized in copper. Thermodynamic complications during oxidation arise with nickel. Residual concentrations of nickel - 9 .37% when the copper content in the melt is 1.5% Cu20 and 0.94% when the copper content in the melt is 12.0% Cu20.

Laboratory studies have established that an important role in the oxidation of metal concentrate belongs! all impurities

Table 5

Results of melting of metal concentrate from radio-electronic scrap with radially located blow nozzles depending on the blowing time

No. Product name Composition, %

Si No. Re gp Pb Bp Ad Ai M Other Total

1 Initial alloy 60.8 8.5 11.0 9.5 0.1 3.0 2.5 4.3 0.10 0.2 0.0 100.0

2 Alloy after 15-minute purging 69.3 6.7 3.5 6.5 0.07 0.4 0.8 4.9 0.11 0.22 7.5 100.0

3 Alloy after 30-minute purging 75.1 5.1 0.1 4.7 0.06 0.3 0.4 5.0 0.12 0.25 8.87 100.0

4 Alloy after 60-minute purging 77.6 3.9 0.05 2.6 0.03 0.2 0.09 5.2 0.13 0.28 9.12 100.0

5 Alloy after 120-minute purging 81.2 2.5 0.02 1.1 0.01 0.1 0.02 5.4 0.15 0.30 9.2 100.0

Studies on the anodic dissolution of smelting products have shown that there is no passivation of the anode during electrolysis of the alloy in a sulfuric acid electrolyte after a 15-minute purge. The electrolyte is not depleted in copper and is not enriched with impurities that passed into the sludge during melting, which ensures its repeated use. The sludge is free of lead and tin, which allows the use of standard sludge processing technology according to the sludge depuration scheme - "alkaline smelting for gold-silver alloy

Based on the research results, furnace units with radially located blowing nozzles were developed, operating in a periodic mode at 0.1 kg, 10 kg, 100 kg for copper, ensuring the processing of batches of radio-electronic scrap of various sizes. At the same time, the entire processing line extracts precious metals without combining batches from various suppliers, which ensures accurate financial calculations for the delivered metals. Based on the test results, initial data have been developed for the construction of a plant for processing REL with a productivity of 500 kg of gold per year. The enterprise project has been completed. The payback period for capital investments is 7-8 months.

1 The theoretical foundations of a method for processing waste from the radio-electronic industry with deep extraction of noble and non-ferrous metals have been developed.

1 1 The thermodynamic characteristics of the main processes of metal oxidation in a copper alloy have been determined, allowing one to predict the behavior of the mentioned metals and impurities

1 2 The values of the apparent activation energy of oxidation in a copper alloy of nickel - 185.8 kJ/mol, zinc - 106.4 kJ/mol, iron - 76.2 kJ/mol, tin 63.1 kJ/mol, lead 42.3 kJ/mol.

2 A pyrometallurgical technology has been developed for processing waste from the radio-electronic industry to produce a gold-silver alloy (Dore metal) and platinum-palladium concentrate.

2.1 Technological parameters have been established (crushing time, productivity of magnetic and electrostatic separation, degree of metal extraction) for the physical enrichment of REL according to the scheme grinding - "magnetic separation -" electrostatic separation, which makes it possible to obtain concentrates of precious metals with a predictable quantitative and qualitative composition

2 2 Technological parameters (melting temperature, air flow, degree of transition of impurities into slag, composition of refining slag) of oxidative smelting of concentrates in an induction furnace with air supplied to the melt by radial-axial lances have been determined; units with radial-axial lances of various capacities have been developed and tested

3 Based on the research, a pilot plant for processing radio-electronic scrap was manufactured and put into production, including a grinding section (MD2x5 crusher), magnetic and electrostatic separation (PBSTs 40/10 and ZEB 32/50), melting in an induction furnace (PI 50 /10) with an SCHG 1-60/10 generator and a melting unit with radial-axial tuyeres, electrochemical dissolution of anodes and processing of noble metal sludge, the effect of “passivation” of the anode was studied, the existence of a sharply extreme dependence of the lead content in the copper-nickel anode was established , made from radio-electronic scrap, which should be taken into account when controlling the process of oxidative radial-axial melting

4. As a result of semi-industrial testing of technology for processing radio-electronic scrap, initial data were developed

for the construction of a plant for processing waste from the radio engineering industry

5. The expected economic effect from the implementation of the dissertation developments based on a gold production capacity of 500 kg/year is ~50 million rubles. with a payback period of 7-8 months

1 Telyakov A.N. Recycling of waste from electrical enterprises / A.N. Telyakov, D.V. Gorlenkov, E.Yu. Stepanova // Abstracts of the report of the International. Conf "Metallurgical Technologies and Ecology" 2003

2 Telyakov A N. Results of tests of technology for processing radio-electronic scrap / AN Telyakov, L.V. Ikonin // Notes of the Mining Institute. T 179 2006

3 Telyakov A.N. Research on the oxidation of impurities in radio-electronic scrap metal concentrate // Notes of the Mining Institute T 179 2006

4 Telyakov A.N. Technology for processing waste from the radio-electronic industry / AN Telyakov, D. V. Gorlenkov, E. Yu Georgieva // Non-ferrous metals No. 6 2007.

RIC SPGGI 08 109 2007 3 424 T 100 copies 199106 St. Petersburg, 21st line, no. 2

INTRODUCTION

Chapter 1. LITERATURE REVIEW.

Chapter 2. STUDY OF SUBSTANTIAL COMPOSITION

RADIO ELECTRONIC SCRAP.

Chapter 3. DEVELOPMENT OF AVERAGING TECHNOLOGY

RADIO ELECTRONIC SCRAP.

3.1. Roasting of electronic scrap.

3.1.1. Information about plastics.

3.1.2. Technological calculations for the utilization of roasting gases.

3.1.3. Roasting radio-electronic scrap in a lack of air.

3.1.4. Firing radio-electronic scrap in a tube furnace.

3.2 Physical methods for processing radio-electronic scrap.

3.2.1. Description of the processing area.

3.2.2. Technological diagram of the enrichment section.

3.2.3. Development of enrichment technology on industrial units.

3.2.4. Determination of the productivity of the units of the enrichment site during the processing of radio-electronic scrap.

3.3. Industrial tests of enrichment of radio-electronic scrap.

3.4. Conclusions to Chapter 3.

Chapter 4. DEVELOPMENT OF TECHNOLOGY FOR PROCESSING RADIO ELECTRONIC SCRAP CONCENTRATES.

4.1. Research on the processing of REL concentrates in acid solutions.

4.2. Testing the technology for producing concentrated gold and silver.

4.2.1. Testing the technology for producing concentrated gold.

4.2.2. Testing the technology for producing concentrated silver.

4.3. Laboratory studies on the extraction of gold and silver REL by smelting and electrolysis.

4.4. Development of technology for extracting palladium from sulfuric acid solutions.

4.5. Conclusions to Chapter 4.

Chapter 5. SEMI-INDUSTRIAL TESTS FOR MELTING AND ELECTROLYSIS OF RADIO-ELECTRONIC SCRAP CONCENTRATES.

5.1. Smelting of REL metal concentrates.

5.2. Electrolysis of REL smelting products.

5.3. Conclusions to chapter 5.

Chapter 6. STUDY OF OXIDATION OF IMPURITIES DURING MELTING OF RADIO ELECTRONIC SCRAP.

6.1. Thermodynamic calculations of the oxidation of REL impurities.

6.2. Study of the oxidation of impurities in REL concentrates.

6.3. Pilot tests on oxidative smelting and electrolysis of REL concentrates.

6.4. Conclusions on the chapter.

Introduction 2007, dissertation on metallurgy, Telyakov, Alexey Nailievich

Relevance of the work

The goal of the work is to develop a technology for the extraction of gold, silver, platinum, palladium and non-ferrous metals from scrap electronics industry and industrial waste from enterprises.

Main provisions submitted for defense

1. Preliminary sorting of REL with subsequent mechanical enrichment ensures the production of metal alloys with increased extraction of precious metals.

2. Physico-chemical analysis of radio-electronic scrap parts showed that the parts are based on up to 32 chemical elements, while the ratio of copper to the sum of the remaining elements is 50-r60: 50-I0.

3. The low dissolution potential of copper-nickel anodes obtained by melting radio-electronic scrap makes it possible to obtain noble metal slurries suitable for processing using standard technology.

Research methods. Laboratory, enlarged laboratory, industrial tests; analysis of enrichment, smelting, and electrolysis products was carried out using chemical methods. For the study, the method of X-ray spectral microanalysis (XMA) and X-ray phase analysis (XRF) was used using the DRON-Ob installation.

The validity and reliability of scientific statements, conclusions and recommendations are determined by the use of modern and reliable research methods and are confirmed by the good convergence of the results of complex studies performed in laboratory, large-scale laboratory and industrial conditions.

Scientific novelty

Practical significance of the work

A technological line for testing radio-electronic scrap has been developed, including departments for disassembly, sorting, mechanical enrichment of smelting and analysis of precious and non-ferrous metals;

A technological scheme for processing radio-electronic scrap and technological waste from enterprises has been developed and tested on a pilot industrial scale, ensuring individual processing and settlement with each REL supplier.

Publications. The main provisions of the dissertation were published in 7 published works, including 3 patents for inventions.

Conclusion dissertation on the topic "Development of an effective technology for the extraction of non-ferrous and precious metals from waste from the radio engineering industry"

CONCLUSIONS ON THE WORK

1. Based on an analysis of literary sources and experiments, a promising method for processing electronic scrap has been identified, including sorting, mechanical enrichment, smelting and electrolysis of copper-nickel anodes.

2. A technology has been developed for testing radio-electronic scrap, which makes it possible to separately process each technological batch of the supplier with quantitative determination of metals.

3. Based on comparative tests of 3 head crushing devices (cone-inertia crusher, jaw crusher, hammer crusher), a hammer crusher is recommended for industrial implementation.

4. Based on the research carried out, a pilot plant for processing radio-electronic scrap was manufactured and put into production.

5. The effect of “passivation” of the anode was studied in laboratory and industrial experiments. The existence of a sharply extreme dependence of the lead content in a copper-nickel anode made from radio-electronic scrap has been established, which should be taken into account when controlling the process of oxidative radial-axial melting.

6. As a result of semi-industrial testing of technology for processing radio-electronic scrap, initial data were developed for the construction of a plant for processing waste from the radio-technical industry.

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Similar works

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As a manuscript

TELYAKOV Alexey Nailievich

DEVELOPMENT OF AN EFFECTIVE TECHNOLOGY FOR EXTRACTION OF NON-FERROUS AND NOBLE METALS FROM RADIO ENGINEERING INDUSTRY WASTE

Specialty 05.16.02– Metallurgy of ferrous and non-ferrous

and rare metals

A b r e f e r t

dissertations for an academic degree

candidate of technical sciences

SAINT PETERSBURG

The work was carried out at the state educational institution of higher professional education, St. Petersburg State Mining Institute named after G.V. Plekhanov (Technical University)

Scientific director–

Doctor of Technical Sciences, Professor,

Honored Scientist of the Russian FederationV.M.Sizyakov

Official opponents:

Doctor of Technical Sciences, ProfessorI.N.Beloglazov

Candidate of Technical Sciences, Associate ProfessorA.Yu.Baymakov

Leading enterprise– Gipronickel Institute

The dissertation can be found in the library of the St. Petersburg State Mining Institute.

SCIENTIFIC SECRETARY

dissertation council

Doctor of Technical Sciences, Associate ProfessorV.N.Brichkin

GENERAL DESCRIPTION OF WORK

Relevance of the work

Changes in the economic mechanism of the country, including the military-industrial complex and the armed forces, have necessitated the creation in certain regions of the country of plants for processing scrap electronics containing precious metals. In this case, it is mandatory to maximize the extraction of precious metals from poor raw materials and reduce the mass of tailings. It is also important that, along with the extraction of precious metals, it is possible to additionally obtain non-ferrous metals, for example, copper, nickel, aluminum and others.

Scientific novelty

Practical significance of the work

A technological line for testing radio-electronic scrap has been developed, including departments for disassembly, sorting and mechanical enrichment to obtain metal concentrates;

The novelty of technical solutions is confirmed by three patents of the Russian Federation: No. 2211420, 2003; No. 2231150, 2004; No. 2276196, 2006

Publications. The main provisions of the dissertation were published in 4 printed works.

The introduction substantiates the relevance of the research and outlines the main provisions submitted for defense.

The second chapter provides data on the study of the quantitative and material composition of radio-electronic scrap.

The third chapter is devoted to the development of technology for homogenizing radioelectronic scrap and obtaining metal concentrates for enriching REL.

The fourth chapter presents data on the development of technology for producing metal concentrates of radio-electronic scrap with the extraction of precious metals.

The fifth chapter describes the results of semi-industrial tests on the smelting of metal concentrates of radio-electronic scrap with subsequent processing into cathode copper and noble metal slurry.

The sixth chapter discusses the possibility of improving the technical and economic indicators of processes developed and tested on a pilot scale.

BASIC PROTECTED PROVISIONS

Based on the study of scientific literature and preliminary research, the following main operations for processing electronic scrap were considered and tested:

melting scrap in an electric furnace;
leaching of scrap in acid solutions;
roasting of scrap followed by electric smelting and electrolysis of semi-finished products, including non-ferrous and precious metals;
physical enrichment of scrap followed by electrical smelting into anodes and processing of anodes into cathode copper and precious metal slurry.

The first three methods were rejected due to environmental difficulties, which turn out to be insurmountable when using the head operations in question.

Table 1

Balance of electronic equipment at the 1st disassembly site

No.	Name of industrial product	Quantity, kg	Content, %
1	Arrived for recycling Racks of electronic devices, machines, switching equipment	24000,0	100
2 3	Received after recycling Electronic scrap in the form of circuit boards, connectors, etc. Scrap of non-ferrous and ferrous metals, not containing precious metals, plastic, organic glass Total:	4100,0 19900,0	17,08 82,92
2 3		24000,0	100

table 2

Balance of electronic scrap at the 2nd disassembly and sorting site

No.	Name of industrial product	Quantity, kg	Content, %
1	Received for recycling Electronic scrap in the form of (connectors and circuit boards)	4100,0	100
2 3 4 5	Received after manual disassembly and sorting department Connectors Radio components Boards without radio components and accessories (the soldered legs of the radio components and the base contain precious metals) Board latches, pins, board guides (elements that do not contain precious metals) Total:	395,0 1080,0 2015,0 610,0	9,63 26,34 49,15 14,88
2 3 4 5		4100,0	100

A hammer crusher MD 2x5, a jaw crusher (DShch 100x200) and a cone-inertial crusher (KID-300) were tested as the main unit for the crushing operation.

During the work, it turned out that the cone inertial crusher should only operate under a pile of material, i.e. when the receiving funnel is completely filled. For efficient operation of a cone inertial crusher, there is an upper limit on the size of the processed material. Larger pieces interfere with the normal operation of the crusher. These shortcomings, the main one of which is the need to mix materials from different suppliers, forced us to abandon the use of KID-300 as the main unit for grinding.

The use of a hammer crusher as a head crushing unit compared to a jaw crusher turned out to be more preferable due to its high productivity when crushing electronic scrap.

When sorting electronic scrap, it is possible to selectively isolate dry multilayer capacitors, which are characterized by a high content of platinum - 0.8% and palladium - 2.8% (Table 3).

Table 3

Composition of concentrates obtained from sorting and processing electronic scrap

N p/p	Content, %
N p/p	Cu	Ni	Co	Zn	Fe	Ag	Au	Pd	Pt	Others	Sum
1	2	3	4	5	6	7	8	9	10	11	12
Silver-palladium concentrates
1	64,7	0,02	sl.	21,4	0,1	2,4	sl.	0,3	0,006	11,8	100,0
Gold concentrates
2	77,3	0,7	0,03	4,5	0,7	0,3	1,3	0,5	0,01	19,16	100,0
Magnetic concentrates
3	sl.	21,8	21,5	0,02	36,3	sl.	0,6	0,05	0,01	19,72	100,0
Concentrates from capacitors
4	0,2	0,59	0,008	0,05	1,0	0,2	No	2,8	0,8	MgO-14.9 CaO-25.6 Sn-2.3 Pb-2.5 R2O3-49.5	100,0