CN112725627A - Method for separating and recovering iridium and rhenium from iridium and rhenium waste material - Google Patents
Method for separating and recovering iridium and rhenium from iridium and rhenium waste material Download PDFInfo
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- CN112725627A CN112725627A CN202011596512.0A CN202011596512A CN112725627A CN 112725627 A CN112725627 A CN 112725627A CN 202011596512 A CN202011596512 A CN 202011596512A CN 112725627 A CN112725627 A CN 112725627A
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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
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/006—Wet processes
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
- C01C1/00—Ammonia; Compounds thereof
- C01C1/16—Halides of ammonium
- C01C1/164—Ammonium chloride
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G47/00—Compounds of rhenium
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G55/00—Compounds of ruthenium, rhodium, palladium, osmium, iridium, or platinum
- C01G55/002—Compounds containing, besides ruthenium, rhodium, palladium, osmium, iridium, or platinum, two or more other elements, with the exception of oxygen or hydrogen
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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
- C22B11/00—Obtaining noble metals
- C22B11/04—Obtaining noble metals by wet processes
- C22B11/042—Recovery of noble metals from waste materials
- C22B11/046—Recovery of noble metals from waste materials from manufactured products, e.g. from printed circuit boards, from photographic films, paper or baths
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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
- C22B11/00—Obtaining noble metals
- C22B11/06—Chloridising
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Abstract
The invention provides a method for separating and recovering iridium and rhenium from iridium and rhenium waste materials, and belongs to the field of separation and recovery of rare and precious metals. The method comprises the steps of carrying out heating reaction on iridium-rhenium waste and oxidizing gas to separate iridium from rhenium, absorbing tail gas by water or alkali solution, and purifying to realize recovery of rhenium; dissolving the residual solid metal after the heating reaction in acid liquor in the presence of an oxidant, adding a precipitator for precipitation, and collecting the precipitate to realize the recovery of iridium. The method does not adopt a repeated roasting and leaching process for purification, reduces the dispersion loss of noble metal iridium, has small equipment corrosivity, low investment cost and short flow, can ensure that the iridium recovery rate reaches over 95.8 percent, the purity of the obtained iridium salt reaches over 99.95 percent, and the purity of the obtained rhenium salt reaches over 99.9 percent.
Description
Technical Field
The invention belongs to the field of rare and precious metal separation and recovery, and particularly relates to a method for separating and recovering iridium rhenium from iridium rhenium waste.
Background
Iridium and its alloys are mainly used as catalysts in the petrochemical industry and in the electronic and electrical industry for the manufacture of resistance wires, thermocouples, iridium cathode filaments, relays, electrical contacts, printed circuits, etc. The iridium-platinum alloy with high hardness is commonly used for manufacturing gyroscope conducting rings, pen points, clocks, instrument bearings and the like, and the iridium can also be used for preparing high-temperature reaction crucibles. Currently, in the industry, the method for recovering iridium from solid waste mainly comprises: the iridium-containing material is treated by an induction melting method, incineration, roasting, microwave, a reduction method, metal fragmentation and the like, then subjected to alkali fusion and acid leaching to prepare a liquid, and then purified by extraction, ion exchange and other methods. However, the above methods all require high-temperature treatment or alkali fusion, have high requirements on equipment, cause iridium loss due to high-temperature treatment, and have complex subsequent processes, large consumption of chemical reagents and high equipment investment.
Rhenium is very hard, corrosion-resistant, wear-resistant and has good ductility, particularly because of its close-packed hexagonal crystal structure, can maintain hardness and ductility at low temperature, and maintain high strength and good creep resistance under high temperature and temperature shock conditions, and rhenium-containing alloys can maintain their strength, ductility and hardness at high temperature, so rhenium has wide application, and can be used as platinum-rhenium catalyst for platinum reforming device for producing high octane gasoline, synthetic chemical catalyst, solid propulsion thermosensitive element, hydrocarbon combustion device, oxidation-resistant coating, ultrasonic instrument, turbine blade of aircraft engine, electronic tube structure material and superconductor, etc.
How to effectively separate and recover iridium and rhenium from iridium and rhenium waste materials, reduce the loss of iridium, reduce the requirements on equipment, simplify the process and reduce the investment cost, and becomes a difficult problem to be solved urgently.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a method for separating and recovering iridium and rhenium from iridium and rhenium waste materials, so that the iridium loss is reduced, the requirements on equipment are reduced, the process is simplified and the investment cost is reduced while the iridium and rhenium are effectively separated and recovered.
In order to achieve the above object, the present invention provides a method for separating and recovering iridium rhenium from an iridium rhenium waste material, comprising the steps of:
(1) carrying out heating reaction on iridium-rhenium waste and oxidizing gas to separate iridium from rhenium, and absorbing tail gas by using water or alkali solution to obtain absorption liquid;
(2) dissolving the residual solid metal after the heating reaction in a chloride solution in the presence of an oxidant, then adding a precipitator for precipitation, and collecting the precipitate to obtain iridium salt;
(3) when water is adopted to absorb tail gas in the step (1), the absorption liquid reacts with alkali and then is purified to obtain rhenium salt; when the tail gas is absorbed by the alkali solution in the step (1), the absorption liquid is directly purified, or is purified after reacting with the alkali, so that the rhenium salt is obtained.
Preferably, in the step (1), the oxidizing gas is chlorine gas.
Preferably, in the step (1), the temperature for heating the reaction is 600-800 ℃.
Preferably, in the step (2), the dissolving temperature is 90-98 ℃.
Preferably, in the step (2), the oxidizing agent is at least one of nitric acid, chlorine and sodium chlorate, the chloride in the chloride solution is at least one of hydrogen chloride, sodium chloride and potassium chloride, and the mass concentration of the chloride solution is 25-35%.
Preferably, in the step (2), the precipitant is at least one of ammonia water and ammonium salt.
Preferably, in the step (2), ammonium chloroiridate is precipitated.
Preferably, in the step (3), the rhenium salt obtained after purification is at least one of ammonium rhenate, potassium rhenate and sodium rhenate.
Preferably, the step (3) is purified by concentration and crystallization.
Preferably, in the step (1), the iridium-rhenium waste material is iridium-rhenium target material waste material.
Compared with the prior art, the invention has the beneficial effects that: compared with the prior art for recovering the noble metal iridium, the method does not adopt a repeated roasting and leaching process for purification, reduces the dispersion loss of the noble metal iridium, has less equipment corrosivity, low investment cost, short process and high iridium recovery rate which can reach more than 95.8 percent, and can obtain iridium salt with the purity of more than 99.95 percent and rhenium metal with high efficiency, and the purity of the obtained rhenium salt can reach more than 99.9 percent.
Detailed Description
To better illustrate the objects, aspects and advantages of the present invention, the present invention will be further described with reference to specific examples.
In order to reduce the loss of iridium, reduce the requirement on equipment, simplify the process and reduce the investment cost while effectively separating and recovering iridium and rhenium, the method for separating and recovering iridium and rhenium from the iridium and rhenium waste material comprises the following steps:
(1) carrying out heating reaction on iridium-rhenium waste and oxidizing gas to separate iridium from rhenium, and absorbing tail gas by using water or alkali solution to obtain absorption liquid;
(2) dissolving the residual solid metal after the heating reaction in a chloride solution in the presence of an oxidant, then adding a precipitator for precipitation, and collecting the precipitate to obtain iridium salt;
(3) when water is adopted to absorb tail gas in the step (1), the obtained absorption liquid reacts with alkali and then is purified to obtain rhenium salt; when the tail gas is absorbed by the alkali solution in the step (1), the obtained absorption liquid is directly purified, or is purified after reacting with the alkali, so that the rhenium salt is obtained. According to the method, the effective separation of iridium and rhenium is realized by utilizing the difference of the reducing properties of iridium and rhenium and the property of rhenium easy to gasify after oxidation, and then the effective recovery of iridium and rhenium is realized through the steps (2) and (3). The method does not adopt a repeated roasting and leaching process for purification, reduces the dispersion loss of noble metal iridium, has small equipment corrosivity, low investment cost and short flow, can ensure that the recovery rate of iridium reaches more than 95.8 percent, the purity of the obtained iridium salt reaches more than 99.95 percent, and the purity of the obtained rhenium salt reaches more than 99.9 percent.
The sequence of the step (2) and the step (3) is not sequential, and the step (2) and the step (3) can be carried out simultaneously, or the step (3) and the step (2) can be carried out firstly.
In some embodiments, the iridium rhenium waste in step (1) is a powder to achieve effective iridium rhenium separation. For example, the iridium-rhenium waste material can be selected to be powder with 100-200 meshes.
In some embodiments, the iridium rhenium scrap in step (1) is scrap of an iridium rhenium target. If the iridium-rhenium waste material can be selected as at least one of the iridium-rhenium target residual target, the cutting material and the leftover material.
In some embodiments, the oxidizing gas in step (1) is chlorine. Rhenium in the iridium-rhenium waste material reacts with chlorine to generate rhenium pentachloride, the rhenium pentachloride has a low boiling point and can be absorbed by water or an aqueous solution along with oxidizing gas, and iridium does not react with the chlorine, so that the separation of iridium and rhenium is realized.
In some preferred embodiments, the temperature of the heating reaction in step (1) is 600-800 ℃.
The tail gas of the heating reaction in the step (1) can be absorbed by water or an alkali solution. The alkali solution can be selected from ammonia water, potassium hydroxide solution, sodium hydroxide solution, or mixture of two or more of them. When absorbing tail gas with alkali solution, the purification can be directly carried out in the step (3) without adding alkali for reaction, and if the alkali of the alkali solution is insufficient, alkali can be added for continuous reaction. When absorbing the tail gas with water, alkali is added for reaction in the step (3), and then purification is carried out. The rhenium salt purified in the step (3) can be ammonium rhenate, potassium rhenate, sodium rhenate or others. The purification can be realized by adopting a concentration crystallization mode in the step (3), and other purification modes can be selected.
The dissolution in step (2) usually requires heating. In some embodiments, the dissolution temperature is 90-98 ℃. Preferably, the dissolution temperature is 95 ℃. The dissolution time is as appropriate. In some embodiments, the dissolution time in step (2) is 8-12 h.
In some preferred embodiments, the oxidizing agent in step (2) is at least one of nitric acid, chlorine gas, and sodium chlorate.
In some preferred embodiments, the chloride in the chloride solution in step (2) is at least one of hydrogen chloride, sodium chloride, and potassium chloride. Preferably, the mass concentration of the chloride solution is 25-35%.
The iridium salt (i.e. precipitate) obtained in step (2) may be selected from ammonium chloroiridate and the like. When the iridium salt obtained in the step (2) is ammonium chloroiridate, the precipitating agent can be selected to be at least one of ammonia water and ammonium salt. The ammonium salt can be selected from ammonium chloride, etc.
In some preferred embodiments, the precipitate is collected in step (2) and then washed. The washing solution can adopt ammonia water, ammonium chloride solution and the like.
Example 1
The embodiment provides a method for separating and recovering iridium and rhenium from iridium and rhenium waste materials, which comprises the following steps:
(1) weighing 500g of 100-mesh iridium-rhenium target material waste, putting the 100-mesh iridium-rhenium target material waste into a tubular furnace, heating to 600 ℃, slowly introducing chlorine gas to react at 600 ℃, and absorbing tail gas by pure water to obtain an absorption liquid;
(2) adding the residual powder in the tubular furnace into hydrochloric acid with the mass concentration of 35%, introducing chlorine gas at 90 ℃ for oxidation and dissolution, wherein the dissolution time is 8h, adding ammonium chloride into the obtained liquid (namely the leaching solution) for precipitation, collecting the precipitate, washing the precipitate by using an ammonium chloride dilute solution to obtain ammonium chloroiridate with the purity of 99.95%, and the iridium recovery rate is 95.8%;
(3) and (2) adding ammonia water into the absorption liquid obtained in the step (1) to generate ammonium rhenate, and then concentrating and crystallizing for 1 time to obtain the ammonium rhenate with the purity of 99.9%.
Example 2
The embodiment provides a method for separating and recovering iridium and rhenium from iridium and rhenium waste materials, which comprises the following steps:
(1) weighing 500g of 100-mesh iridium-rhenium target material waste, putting the 100-mesh iridium-rhenium target material waste into a tubular furnace, heating the waste to 700 ℃, slowly introducing chlorine gas to react at 700 ℃, and absorbing tail gas by adopting a potassium hydroxide solution to obtain an absorption solution containing potassium rhenium precipitate;
(2) adding the residual powder in the tubular furnace into a sodium chloride solution with the mass concentration of 35%, adding nitric acid at the temperature of 92 ℃ for oxidation and dissolution, wherein the dissolution time is 12h, adding ammonium chloride into the obtained liquid (namely the leaching solution) for precipitation, collecting the precipitate, washing the precipitate by an ammonium chloride dilute solution to obtain ammonium chloroiridate with the purity of 99.99%, and the iridium recovery rate is 96%;
(3) concentrating and crystallizing the absorption liquid containing potassium rhenium precipitate obtained in the step (1) for 3 times to obtain the potassium rhenium with the purity of 99.99 percent.
Example 3
The embodiment provides a method for separating and recovering iridium and rhenium from iridium and rhenium waste materials, which comprises the following steps:
(1) weighing 500g of 200-mesh iridium-rhenium target material waste, putting the weighed material waste into a tube furnace, heating the material waste to 800 ℃, slowly introducing chlorine gas to react at 800 ℃, and absorbing tail gas by pure water to obtain an absorption liquid;
(2) adding the residual powder in the tubular furnace into a potassium chloride solution with the mass concentration of 35%, introducing chlorine gas at 95 ℃ for oxidation and dissolution, wherein the dissolution time is 10h, adding ammonium chloride into the obtained liquid (namely the leaching solution) for precipitation, collecting the precipitate, washing the precipitate by an ammonium chloride diluted solution to obtain ammonium chloroiridate with the purity of 99.99%, and the iridium recovery rate is 96%;
(3) and (2) adding ammonia water into the absorption liquid obtained in the step (1) to generate ammonium rhenate, and then concentrating and crystallizing for 3 times to obtain the ammonium rhenate with the purity of 99.999%.
Example 4
The embodiment provides a method for separating and recovering iridium and rhenium from iridium and rhenium waste materials, which comprises the following steps:
(1) weighing 500g of iridium-rhenium target material waste of 200 meshes, putting the iridium-rhenium target material waste into a tube furnace, heating to 750 ℃, slowly introducing chlorine gas to react at 750 ℃, and absorbing tail gas by adopting pure water to obtain absorption liquid;
(2) adding the residual powder in the tubular furnace into hydrochloric acid with the mass concentration of 35%, introducing chlorine gas at 95 ℃ for oxidation and dissolution, wherein the dissolution time is 12h, adding ammonium chloride into the obtained liquid (namely the leaching solution) for precipitation, collecting the precipitate, washing the precipitate by using an ammonium chloride dilute solution to obtain ammonium chloroiridate with the purity of 99.99%, and the iridium recovery rate is 96.2%;
(3) and (2) adding ammonia water into the absorption liquid obtained in the step (1) to generate ammonium rhenate, and then concentrating and crystallizing for 3 times to obtain the ammonium rhenate with the purity of 99.999%.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and not for limiting the protection scope of the present invention, and although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Claims (10)
1. A method for separating and recovering iridium rhenium from iridium rhenium waste materials, which is characterized by comprising the following steps:
(1) carrying out heating reaction on iridium-rhenium waste and oxidizing gas to separate iridium from rhenium, and absorbing tail gas by using water or alkali solution to obtain absorption liquid;
(2) dissolving the residual solid metal after the heating reaction in a chloride solution in the presence of an oxidant, then adding a precipitator for precipitation, and collecting the precipitate to obtain iridium salt;
(3) when water is adopted to absorb tail gas in the step (1), the absorption liquid reacts with alkali and then is purified to obtain rhenium salt; when the tail gas is absorbed by the alkali solution in the step (1), the absorption liquid is directly purified, or is purified after reacting with the alkali, so that the rhenium salt is obtained.
2. The method according to claim 1, wherein in the step (1), the oxidizing gas is chlorine gas.
3. The method as claimed in claim 1, wherein the temperature for heating reaction in step (1) is 600-800 ℃.
4. The method according to claim 1, wherein in the step (2), the dissolution temperature is 90-98 ℃.
5. The method according to claim 1, wherein in the step (2), the oxidizing agent is at least one of nitric acid, chlorine gas and sodium chlorate, the chloride in the chloride solution is at least one of hydrogen chloride, sodium chloride and potassium chloride, and the mass concentration of the chloride solution is 25-35%.
6. The method according to claim 1, wherein in the step (2), the precipitant is at least one of ammonia water and ammonium salt.
7. The process of claim 1, wherein in step (2), ammonium chloroiridate is precipitated.
8. The method as claimed in claim 1, wherein in the step (3), the rhenium salt obtained after purification is at least one of ammonium rhenate, potassium rhenate and sodium rhenate.
9. The method of claim 1, wherein the step (3) is performed by concentration and crystallization.
10. The method according to claim 1, wherein in step (1), the iridium-rhenium scrap is iridium-rhenium target scrap.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114196832A (en) * | 2021-12-16 | 2022-03-18 | 合肥工业大学 | Method for preparing rhenium powder by recycling tungsten-rhenium alloy waste |
| CN115011808A (en) * | 2022-06-22 | 2022-09-06 | 广东先导稀材股份有限公司 | Method for separating and recovering ruthenium and iridium from ruthenium and iridium-containing materials |
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| CN101985696A (en) * | 2010-12-01 | 2011-03-16 | 金川集团有限公司 | Method for extracting iridium from iridium containing materials |
| WO2019165560A1 (en) * | 2018-03-01 | 2019-09-06 | Aurum Integra Inc. | Method for selectively oxidizing metals of an alloy |
| CN110616330A (en) * | 2019-09-30 | 2019-12-27 | 江苏奇纳新材料科技有限公司 | Method for recovering rare and noble metals in rhenium-containing high-temperature alloy waste |
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Patent Citations (3)
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| CN101985696A (en) * | 2010-12-01 | 2011-03-16 | 金川集团有限公司 | Method for extracting iridium from iridium containing materials |
| WO2019165560A1 (en) * | 2018-03-01 | 2019-09-06 | Aurum Integra Inc. | Method for selectively oxidizing metals of an alloy |
| CN110616330A (en) * | 2019-09-30 | 2019-12-27 | 江苏奇纳新材料科技有限公司 | Method for recovering rare and noble metals in rhenium-containing high-temperature alloy waste |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114196832A (en) * | 2021-12-16 | 2022-03-18 | 合肥工业大学 | Method for preparing rhenium powder by recycling tungsten-rhenium alloy waste |
| CN114196832B (en) * | 2021-12-16 | 2024-06-07 | 合肥工业大学 | Method for preparing rhenium powder by recycling tungsten-rhenium alloy waste |
| CN115011808A (en) * | 2022-06-22 | 2022-09-06 | 广东先导稀材股份有限公司 | Method for separating and recovering ruthenium and iridium from ruthenium and iridium-containing materials |
| CN115011808B (en) * | 2022-06-22 | 2023-10-24 | 广东先导稀材股份有限公司 | Method for separating and recovering ruthenium and iridium from ruthenium and iridium-containing material |
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