CN113118449A - Physical separation method and device for multi-component metal substance - Google Patents
Physical separation method and device for multi-component metal substance Download PDFInfo
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- CN113118449A CN113118449A CN201911412033.6A CN201911412033A CN113118449A CN 113118449 A CN113118449 A CN 113118449A CN 201911412033 A CN201911412033 A CN 201911412033A CN 113118449 A CN113118449 A CN 113118449A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/14—Making metallic powder or suspensions thereof using physical processes using electric discharge
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/12—Making metallic powder or suspensions thereof using physical processes starting from gaseous material
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B9/00—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals
- C22B9/16—Remelting metals
- C22B9/22—Remelting metals with heating by wave energy or particle radiation
- C22B9/228—Remelting metals with heating by wave energy or particle radiation by particle radiation, e.g. electron beams
Abstract
The invention relates to a physical separation method and a physical separation device for multi-component metal substances, and belongs to the field of material separation science. Adding a raw material containing multi-component metal and intermetallic compounds into a crucible in a vacuum electron beam furnace, and vacuumizing; heating by adopting an electron beam melting method, and vaporizing metal particles to form metal steam; ionizing the formed metal steam by using a continuous radio frequency hollow cathode discharge method to form low-temperature plasma; applying orthogonal magnetic fields around the plasma, wherein different metal ions have different mass-to-charge ratios, and different paths are formed in the same orthogonal magnetic field so as to separate different metals; and arranging a metal ion receiving plate around the crucible, and collecting metal powder formed after different types of metal ions fly out. The whole process is a physical separation process, is environment-friendly and is easy to realize automatic industrial production.
Description
Technical Field
The invention relates to a novel method and a novel device for separating metals, in particular to a physical separation method and a physical separation device for multi-component metal substances.
Background
With the widespread application of household appliances and electronic devices, the problem of disposing of electronic waste has become an increasingly serious environmental problem to be solved urgently. The electrical and electronic equipment has various types and complex manufacturing processes, contains a large amount of metals, plastics, glass and other compounds, wherein the toxic and harmful elements comprise a plurality of chlorofluorocarbons, halogen flame retardants, mercury, selenium, nickel, cadmium, lead, chromium and the like, can cause serious pollution to the environment if the treatment is improper, has high requirements on treatment technology and process, and simultaneously, electronic waste is an important renewable resource, so the exploration on the separation and recovery technology is generated, and a new research field of separation science is formed.
Research on the recovery of metals from electronic waste dates back to the end of the 60's 20 th century. At that time, the U.S. Ministry of mining attempted to recover precious metals from scrap military equipment and built pilot plants with a throughput of up to 0.23 t/h. Because the electronic waste is various in types and complex in components, the processing of the electronic waste relates to the fields of environmental science, chemistry, mineral processing, metallurgy, electronic power, machinery and the like, and the processing difficulty is very high, the U.S. national mining agency organizes and develops new processes for processing the electronic waste and recovering precious metals in 1986, and the new processes comprise technologies of manual disassembly, mechanical processing, pyrometallurgy, hydrometallurgy and the like. Meanwhile, research work in this field is actively conducted in other developed countries such as sweden, japan, germany, and the like, and great progress is made in process technology, but these technologies mainly recover precious metals. With the continuous decrease of the content of noble metals, the gradual increase of the content of basic metals and the increasing shortage of resources in electronic products, the development direction of recycling technology has started to turn to rare noble metals and basic metals.
The electronic waste mainly contains a large amount of base metal copper and a large amount of rare noble metal. For example: gold is widely used in electrical contact materials and conductive materials (gold wires, gold foils, parts pressed with gold powder, alloys of gold, gold-clad alloy materials, etc.), gold-based solders, and electronic pastes; germanium is an important semiconductor material used in the fabrication of transistors and various electronic devices. Indium is mainly used for producing ITO targets (for producing liquid crystal displays and flat screens) because of its strong light permeability and electrical conductivity, accounting for 70% of the global indium consumption. Tantalum is an important noble metal (TaN in copper interconnection) in a Chip (CPU), can also be used as an electrode of a valve, a rectifier, an electrolyte and a capacitor, and half of the worldwide production of tantalum metal is used for producing tantalum capacitors. Gallium is used for manufacturing semiconductor doping elements of gallium nitride, gallium arsenide, gallium phosphide and germanium; gallium compounds, particularly gallium arsenide, have attracted increasing attention in the electronics industry. The electronic and electric appliances are the industries with the largest silver consumption, the application of the electronic and electric appliances is divided into electric contact materials, composite materials and welding materials, and rhodium, palladium and the like are obtained in the electronic and electric appliances. Meanwhile, noble metal coatings are increasingly used in the electronics industry. The reason for this is that: the copper-based alloy has the advantages of high chemical stability, good corrosion resistance, good weldability, strong binding force, small contact resistance, particularly good conductivity and the like. At present, the international noble metal electroplating technology is developed quickly, measures for reducing the electroplating cost are explored in an effort under the condition of improving the quality of a plating layer, the components of the plating layer are developed from a single metal to a diversification direction, and the multielement alloy with excellent comprehensive performance is obtained. For example: gold alloys (e.g., gold tin, gold bismuth, gold silver, gold cobalt … …), silver alloys (silver nickel, silver tin … …), and palladium alloy plating processes, minimizing the use of precious metals such as rhodium, platinum, and gold. Normally, this effect cannot be achieved with one coating layer, but with a plurality of intermediate coating layers.
Because the electronic waste is a multi-substance and multi-component mixed system, the electronic waste is firstly crushed to achieve the dissociation of all materials, and then the materials are directly separated by adopting physical separation methods such as gravity separation, magnetic separation, electric separation and the like according to the difference of physical properties of the materials. However, after pretreatment such as electronic waste disassembly and material separation by sorting and crushing technologies, various metal mixtures, such as rare and precious metals including copper, heavy metals, gold, silver and the like, are obtained. How to separate, extract and purify copper, heavy metals (lead, cadmium and the like) and rare and precious metals (gold, silver and the like) in a plurality of metal mixtures in an environment-friendly manner to enable the metals to become secondary resources with higher added values and avoid secondary pollution to the environment is an important problem which needs to be solved urgently at present but is not solved yet.
At present, the technology for recovering metals from electronic waste can be broadly divided into: mechanical treatment technology, heat treatment technology, hydrometallurgy technology, biological treatment technology and the like, but the above technologies can generate a large amount of waste gas and waste water in the process, require strict environmental protection facilities, have high energy consumption, and can not separate some high-melting-point metals such as tungsten, molybdenum and tantalum efficiently.
Disclosure of Invention
The invention aims to provide a high-efficiency physical separation method and device for separating a multi-component metal mixture and an intermetallic compound, wherein no waste water is generated in the separation process, toxic additives are not used, and the method and device are harmless to the environment.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for physically separating multicomponent metallic species, comprising the steps of:
(1) adding a raw material containing multi-component metal and intermetallic compounds into a crucible in a vacuum electron beam furnace, and vacuumizing;
(2) heating by adopting an electron beam melting method, wherein metal particles are vaporized due to rapid temperature rise and a vacuum environment to form metal steam, and the temperature and the pressure of the metal steam are determined by the types of metal elements;
(3) ionizing the formed metal steam by using a continuous radio frequency hollow cathode discharge method to form low-temperature plasma, wherein metal ions in the plasma obtain a small amount of initial velocity due to an electric field formed by an electron gun;
(4) applying orthogonal magnetic fields around the plasmas formed in the step (3), wherein the sizes of the orthogonal magnetic fields are determined according to metal elements, and different paths can be formed in the same orthogonal magnetic fields due to different mass-to-charge ratios of different metal ions, so that the purpose of separating different metals is achieved;
(5) and arranging a metal ion receiving plate around the crucible to collect metal powder formed after different types of metal ions fly out, and finishing the separation.
In the step (1), different crucibles can be selected according to different raw materials; such as copper water-cooled crucibles, graphite crucibles, etc. The vacuum degree of the vacuum pumping is 10-2~10-3pa。
In the step (2), heating is carried out by adopting an electron beam melting method, and the heating can be adjusted according to the types of metal elements.
In the step (3), the method for ionizing the metal vapor can be selected according to different metal elements, and the hollow cathode is only the most common example which is easy to realize. The device adopted in the radio frequency hollow cathode discharge method is a hollow cathode discharge gun.
A physical separation device for multi-component metal substances comprises an electron beam melting device, a plasma generator (including radio frequency hollow cathode discharge), a magnetic field generator, an ion collecting plate and the like, wherein the plasma generator is arranged above a melting crucible of the electron beam melting device, the magnetic field generator is arranged on the periphery of the upper part of the electron beam melting device, and the ion collecting plate is arranged around the melting crucible.
The electron beam melting device is a vacuum electron beam melting furnace, wherein an electron gun is arranged above a crucible.
The plasma generator can be a hollow cathode discharge gun arranged above the electron beam melting device.
The magnetic field generator is arranged at the periphery of the upper part of the electron beam melting device, and an orthogonal magnetic field is formed above the plasma generator.
The invention is a new method and apparatus for realizing the physical separation of multi-component metal mixture and intermetallic compound, utilize the electron beam of high energy density to vaporize the metal raw materials, form the metal vapor; then, by utilizing a plasma technology, ionizing metal steam to form plasma; different metal ions are separated by using the dispersion effect of the magnetic field on different metal element ions. The whole process is a physical separation process, is environment-friendly and is easy to realize automatic industrial production.
The invention has the advantages that:
1. the invention only utilizes the difference of the physical properties of different metal elements to realize the separation, does not generate new toxic and harmful substances such as waste gas and waste water in the whole process, can well remove the non-metallic impurities in the raw materials, can collect the waste gas generated by the raw materials, can carry out uniform harmless treatment, has simple required environmental protection measures, and can realize zero pollution and zero emission.
2. In the whole process of the invention, no consumable is needed to be added, and only the hot cathode material adopted by the electron gun needs to be replaced regularly.
3. The invention has higher utilization ratio of raw materials and higher purity of the obtained final product.
4. The method can realize the simultaneous separation of a plurality of metal elements from the multi-component metal raw material, has relatively simple process, and is easy to realize automatic control and sustainable industrial production.
Drawings
FIG. 1 is a schematic illustration of the principle of the separation process of the present invention.
Description of the main reference numerals:
1 crucible 2 Electron Beam
3 hollow cathode discharge gun 4 magnetic field
5 ion trajectory 6 ion collecting plate
7 raw materials
Detailed Description
As shown in fig. 1, the physical separation device of multi-component metal substances of the present invention comprises an electron beam melting device, a hollow cathode discharge gun 3, a magnetic field generator, an ion collecting plate, etc., wherein the hollow cathode discharge gun 3 is arranged above a melting crucible 1 of the electron beam melting device, the magnetic field generator is arranged at the periphery of the upper part of the electron beam melting device, and an orthogonal magnetic field is formed above a plasma generator; the ion collecting plate is arranged around the melting crucible 1. The electron beam melting device is a vacuum electron beam melting furnace in which an electron gun is disposed above the crucible 1.
The implementation method of the invention comprises the following steps:
(1) gold is mixed with multiple componentsAdding intermetallic compound raw material 7 into copper water-cooling crucible 1 in vacuum electron beam furnace, vacuumizing to vacuum degree of 10-2~10-3pa;
(2) Heating the raw material in the step (1) by adopting an electron beam melting method, scanning and melting the raw material 7 in a crucible by using an electron beam 2, wherein metal particles can be vaporized to form metal steam due to the sharp temperature rise and the vacuum environment, and the temperature and the pressure of the metal steam are determined by the types of metal elements;
(3) the metal steam formed by ionization by using a continuous radio frequency hollow cathode discharge method is formed into low-temperature plasma by using the hollow cathode discharge gun 3, and metal ions in the plasma obtain a small amount of initial velocity due to an electric field formed by the discharge gun;
(4) applying an orthogonal magnetic field 4 around the plasma formed in the step (3), wherein the size of the orthogonal magnetic field is determined by metal elements, and different ion tracks 5 can be formed in the same orthogonal magnetic field due to different mass-to-charge ratios of different metal ions, so as to achieve the purpose of separating different metals;
(5) and a metal ion collector, namely an ion collecting plate 6, is arranged around the crucible to collect metal powder formed after different types of metal ions fly out, and the separation is finished.
The above embodiments are only used for illustrating but not limiting the technical solutions of the present invention, and although the above embodiments describe the present invention in detail, those skilled in the art should understand that: all changes which come within the meaning and range of equivalency of the specification are to be embraced within their scope, either directly or indirectly.
Claims (8)
1. A method for physically separating multicomponent metallic species, comprising the steps of:
(1) adding a raw material containing multi-component metal and intermetallic compounds into a crucible in a vacuum electron beam furnace, and vacuumizing;
(2) heating by adopting an electron beam melting method, and vaporizing metal particles to form metal steam;
(3) ionizing the formed metal steam by using a continuous radio frequency hollow cathode discharge method to form low-temperature plasma, wherein metal ions in the plasma obtain a small amount of initial velocity due to an electric field formed by an electron gun;
(4) applying orthogonal magnetic fields around the plasmas formed in the step (3), wherein different metal ions have different mass-to-charge ratios, and different paths are formed in the same orthogonal magnetic fields so as to separate different metals;
(5) and arranging a metal ion receiving plate around the crucible, and collecting metal powder formed after different types of metal ions fly out.
2. A method of physically separating multicomponent metallic substances according to claim 1, wherein: the crucible is a copper water-cooling crucible or a graphite crucible.
3. A method of physically separating multicomponent metallic substances according to claim 1, wherein: the vacuum electron beam furnace is vacuumized, and the vacuum degree is 10-2~10-3pa。
4. A method of physically separating multicomponent metallic substances according to claim 1, wherein: the device adopted in the radio frequency hollow cathode discharge method is a hollow cathode discharge gun.
5. A device for physically separating a multi-component metal substance, comprising: the device comprises an electron beam melting device, a plasma generator, a magnetic field generator and an ion collecting plate, wherein the plasma generator is arranged above a melting crucible of the electron beam melting device, the magnetic field generator is arranged on the periphery of the upper part of the electron beam melting device, and the ion collecting plate is arranged around the melting crucible.
6. The apparatus for physical separation of multicomponent metallic substances according to claim 5, wherein: the electron beam melting device is a vacuum electron beam melting furnace.
7. The apparatus for physical separation of multicomponent metallic substances according to claim 5, wherein: the plasma generator is a hollow cathode discharge gun.
8. The apparatus for physical separation of multicomponent metallic substances according to claim 5, wherein: the magnetic field generator is arranged at the periphery of the upper part of the electron beam melting device, and an orthogonal magnetic field is formed above the plasma generator.
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Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
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GB1440139A (en) * | 1973-02-02 | 1976-06-23 | Jersey Nuclear Avco Isotopes | Method and apparatus for the separation of isotopes |
US4124801A (en) * | 1976-09-24 | 1978-11-07 | Phrasor Technology Incorporated | Apparatus and process for separating materials |
CN1217671A (en) * | 1996-03-15 | 1999-05-26 | 英国核燃料公众有限公司 | Separation of isotopes by ionisation for processing of nuclear fuel materials |
CN1304784A (en) * | 1999-11-29 | 2001-07-25 | 伊莱克特罗希里波尔联合企业 | Method of separating palladium isotop by using ion source in electromagnetic separator |
CN106048231A (en) * | 2016-07-14 | 2016-10-26 | 上海交通大学 | Method for recovering tantalum, silver, nickel and iron from waste tantalum capacitor |
CN211939059U (en) * | 2019-12-31 | 2020-11-17 | 有研工程技术研究院有限公司 | Physical separation device for multi-component metal substances |
-
2019
- 2019-12-31 CN CN201911412033.6A patent/CN113118449A/en active Pending
Patent Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
GB1440139A (en) * | 1973-02-02 | 1976-06-23 | Jersey Nuclear Avco Isotopes | Method and apparatus for the separation of isotopes |
US4124801A (en) * | 1976-09-24 | 1978-11-07 | Phrasor Technology Incorporated | Apparatus and process for separating materials |
CN1217671A (en) * | 1996-03-15 | 1999-05-26 | 英国核燃料公众有限公司 | Separation of isotopes by ionisation for processing of nuclear fuel materials |
CN1304784A (en) * | 1999-11-29 | 2001-07-25 | 伊莱克特罗希里波尔联合企业 | Method of separating palladium isotop by using ion source in electromagnetic separator |
CN106048231A (en) * | 2016-07-14 | 2016-10-26 | 上海交通大学 | Method for recovering tantalum, silver, nickel and iron from waste tantalum capacitor |
CN211939059U (en) * | 2019-12-31 | 2020-11-17 | 有研工程技术研究院有限公司 | Physical separation device for multi-component metal substances |
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