CN109811138B - Method for recovering iridium from iridium-containing organic waste liquid - Google Patents
Method for recovering iridium from iridium-containing organic waste liquid Download PDFInfo
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- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical compound [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 title claims abstract description 96
- 229910052741 iridium Inorganic materials 0.000 title claims abstract description 87
- 239000007788 liquid Substances 0.000 title claims abstract description 50
- 239000010815 organic waste Substances 0.000 title claims abstract description 33
- 238000000034 method Methods 0.000 title claims abstract description 32
- 239000002699 waste material Substances 0.000 claims abstract description 21
- 238000011084 recovery Methods 0.000 claims abstract description 12
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 11
- 239000002244 precipitate Substances 0.000 claims abstract description 11
- 239000007787 solid Substances 0.000 claims abstract description 9
- 150000002504 iridium compounds Chemical class 0.000 claims abstract description 5
- 239000002518 antifoaming agent Substances 0.000 claims abstract description 4
- 238000001035 drying Methods 0.000 claims abstract description 4
- 238000005406 washing Methods 0.000 claims abstract description 4
- 238000001914 filtration Methods 0.000 claims abstract 2
- 238000006722 reduction reaction Methods 0.000 claims abstract 2
- 238000006243 chemical reaction Methods 0.000 claims description 17
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- STCOOQWBFONSKY-UHFFFAOYSA-N tributyl phosphate Chemical compound CCCCOP(=O)(OCCCC)OCCCC STCOOQWBFONSKY-UHFFFAOYSA-N 0.000 claims description 8
- 239000008367 deionised water Substances 0.000 claims description 7
- 229910021641 deionized water Inorganic materials 0.000 claims description 7
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 6
- 239000011591 potassium Substances 0.000 claims description 6
- 229910052700 potassium Inorganic materials 0.000 claims description 6
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 5
- ORBBTCHHNMWMCP-UHFFFAOYSA-K cycloocta-1,5-diene trichloroiridium Chemical class [Ir](Cl)(Cl)Cl.C1=CCCC=CCC1 ORBBTCHHNMWMCP-UHFFFAOYSA-K 0.000 claims description 5
- 239000000463 material Substances 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- 238000011085 pressure filtration Methods 0.000 claims description 5
- 239000011734 sodium Substances 0.000 claims description 5
- 229910052708 sodium Inorganic materials 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 239000012279 sodium borohydride Substances 0.000 claims description 4
- 229910000033 sodium borohydride Inorganic materials 0.000 claims description 4
- -1 carbonyl tris (triphenylphosphine) iridium chloride Chemical compound 0.000 claims description 2
- 229910001873 dinitrogen Inorganic materials 0.000 claims description 2
- 229910021638 Iridium(III) chloride Inorganic materials 0.000 claims 1
- XHLLCVASRCVJHB-UHFFFAOYSA-N carbon monoxide;iridium;pentane-2,4-dione Chemical compound [Ir].[O+]#[C-].[O+]#[C-].CC(=O)CC(C)=O XHLLCVASRCVJHB-UHFFFAOYSA-N 0.000 claims 1
- VSPLSJCNZPDHCN-UHFFFAOYSA-M carbon monoxide;iridium;triphenylphosphane;chloride Chemical compound [Cl-].[Ir].[O+]#[C-].C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1.C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1 VSPLSJCNZPDHCN-UHFFFAOYSA-M 0.000 claims 1
- 230000007935 neutral effect Effects 0.000 claims 1
- DANYXEHCMQHDNX-UHFFFAOYSA-K trichloroiridium Chemical compound Cl[Ir](Cl)Cl DANYXEHCMQHDNX-UHFFFAOYSA-K 0.000 claims 1
- 239000002994 raw material Substances 0.000 abstract description 2
- 230000003647 oxidation Effects 0.000 description 8
- 238000007254 oxidation reaction Methods 0.000 description 8
- 238000011978 dissolution method Methods 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 238000011282 treatment Methods 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- YRKCREAYFQTBPV-UHFFFAOYSA-N acetylacetone Chemical compound CC(=O)CC(C)=O YRKCREAYFQTBPV-UHFFFAOYSA-N 0.000 description 2
- 230000004913 activation Effects 0.000 description 2
- 238000005660 chlorination reaction Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 239000002815 homogeneous catalyst Substances 0.000 description 2
- KZLHPYLCKHJIMM-UHFFFAOYSA-K iridium(3+);triacetate Chemical compound [Ir+3].CC([O-])=O.CC([O-])=O.CC([O-])=O KZLHPYLCKHJIMM-UHFFFAOYSA-K 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000005416 organic matter Substances 0.000 description 2
- 239000012074 organic phase Substances 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- RWSOTUBLDIXVET-UHFFFAOYSA-O sulfonium Chemical compound [SH3+] RWSOTUBLDIXVET-UHFFFAOYSA-O 0.000 description 2
- 230000002194 synthesizing effect Effects 0.000 description 2
- 229910001868 water Inorganic materials 0.000 description 2
- WVQBLGZPHOPPFO-UHFFFAOYSA-N 2-chloro-N-(2-ethyl-6-methylphenyl)-N-(1-methoxypropan-2-yl)acetamide Chemical compound CCC1=CC=CC(C)=C1N(C(C)COC)C(=O)CCl WVQBLGZPHOPPFO-UHFFFAOYSA-N 0.000 description 1
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 1
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 229910000272 alkali metal oxide Inorganic materials 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- QZPSXPBJTPJTSZ-UHFFFAOYSA-N aqua regia Chemical compound Cl.O[N+]([O-])=O QZPSXPBJTPJTSZ-UHFFFAOYSA-N 0.000 description 1
- 239000010953 base metal Substances 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 238000005810 carbonylation reaction Methods 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 125000002091 cationic group Chemical group 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- HTXDPTMKBJXEOW-UHFFFAOYSA-N dioxoiridium Chemical compound O=[Ir]=O HTXDPTMKBJXEOW-UHFFFAOYSA-N 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 235000019441 ethanol Nutrition 0.000 description 1
- 239000012847 fine chemical Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- OZDHQOIPFFBDPL-UHFFFAOYSA-N iridium hydrochloride Chemical compound Cl.[Ir] OZDHQOIPFFBDPL-UHFFFAOYSA-N 0.000 description 1
- 229910000457 iridium oxide Inorganic materials 0.000 description 1
- FJSGOKUOWYASDX-UHFFFAOYSA-K iridium(3+) triphenylphosphane trichloride Chemical compound [Ir+3].[Cl-].C1(=CC=CC=C1)P(C1=CC=CC=C1)C1=CC=CC=C1.[Cl-].[Cl-] FJSGOKUOWYASDX-UHFFFAOYSA-K 0.000 description 1
- HLYTZTFNIRBLNA-LNTINUHCSA-K iridium(3+);(z)-4-oxopent-2-en-2-olate Chemical compound [Ir+3].C\C([O-])=C\C(C)=O.C\C([O-])=C\C(C)=O.C\C([O-])=C\C(C)=O HLYTZTFNIRBLNA-LNTINUHCSA-K 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000003832 thermite Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Landscapes
- Manufacture And Refinement Of Metals (AREA)
- Treatment Of Water By Oxidation Or Reduction (AREA)
Abstract
The invention discloses a method for recovering iridium from an iridium-containing organic waste liquid, which is characterized by adjusting the pH value of the iridium-containing organic waste liquid, adding a defoaming agent into the iridium-containing organic waste liquid, carrying out reduction reaction on the waste liquid and a solid reducing agent, reducing an iridium compound in the waste liquid into metallic iridium precipitate, filtering, washing and drying to obtain iridium powder. The method has the advantages of simple process, high recovery efficiency and strong adaptability to raw materials, and can treat various iridium-containing organic waste liquids.
Description
Technical Field
The invention relates to a method for recovering iridium, in particular to a method for recovering iridium from an iridium-containing organic waste liquid.
Background
Organic compounds of iridium, such as iridium acetylacetonate, iridium bis (phenylphosphine) carbonyl chloride, iridium acetate and the like, are important precursor compounds for iridium phosphorescent molecular materials, homogeneous catalysts and metal organic chemical vapor deposition for OLEDs. In the organic phase of iridiumIn the process of preparing the compound, a considerable part of iridium by-products enter waste liquid containing a large amount of organic matters due to low product yield. 1, 5-cyclooctadiene iridium chloride homogeneous catalyst for synthesizing metolachlor in fine chemical industry and iridium acetate catalyst [ Ir ] for producing acetic acid by process of synthesizing Cativa acetate through methanol low-pressure carbonylation3(O2CCH3)6-μ3-O(H2O)3]O2CCH3After the organic waste liquid is invalid, a large amount of iridium-containing organic waste liquid is generated in the preparation process of the OLED iridium phosphorescent molecular material, and the iridium-containing organic waste liquid is generated in the preparation process of triphenylphosphine iridium chloride, wherein the organic waste liquid mainly comprises an organic phase, a water phase and the like.
Few reports are made on the method for recovering iridium in organic waste liquid. At present, two main methods of iridium in iridium-containing organic waste materials are a traditional incineration method and an oxidation dissolution method. The traditional incineration method is to remove organic matters through incineration to generate metal iridium or iridium oxide, then to convert iridium into solution through methods such as moderate temperature chlorination, alkali oxide melting or sulfonium capture-aluminothermic activation and the like, and then to purify the iridium. The oxidation dissolution method is to use a strong oxidant to destroy the stability of organic matters in the solution under specific conditions, oxidize or decompose the organic matters, transfer iridium into an inorganic phase, and recover and purify the iridium. For example, research is conducted on recovering iridium from an iridium-containing waste liquid containing organic matters such as acetylacetone and alcohol by means of oxidative dissolution, organic matters are firstly destroyed by means of aqua regia oxidation to realize transformation of a solution medium, the iridium is transformed into an iridium hydrochloric acid solution, nitric acid is added after oxidation is completed, residual organic matters and most of soluble salts can be removed through hydrolysis, base metal impurities such as aluminum, copper, iron, magnesium and calcium in the iridium solution are removed through exchange by means of strong acid type cationic resin, the iridium does not easily form hydrated cations, the iridium-containing solution is purified and then concentrated and crystallized to obtain chloroiridic acid, and the chloroiridic acid is directly calcined and reduced by hydrogen to produce iridium high-purity powder.
Because iridium in the iridium-containing organic waste exists in the form of an organic iridium compound, the conventional reducing agent is difficult to directly reduce and recover iridium from an organic system; meanwhile, volatile iridium compounds are contained in the organic waste liquid, and the loss of iridium can be caused by direct heating or calcination. When the method is used for treating the iridium-containing organic waste liquid, a relatively simple organic waste liquid system can be recovered by an oxidation dissolution method; however, the recovery of iridium in a complex system is difficult, the recovery of iridium can be realized only by a series of complicated process treatments such as incineration, moderate-temperature chlorination, alkali melting oxidation or sulfonium capture, thermite activation and the like, and the recovery rate of iridium is difficult to ensure.
Disclosure of Invention
The invention aims to provide a method for recovering iridium from an iridium-containing organic waste liquid, aiming at solving the problems of the existing method for recovering iridium from the organic waste liquid.
The method for recovering iridium from organic waste liquid comprises the following steps:
A. adjusting the pH value of the iridium-containing organic waste liquid to 7-10, and adding a defoaming agent tributyl phosphate into the waste liquid according to the mass ratio of 0.05-0.1%;
B. slowly adding the organic waste liquid obtained in the step A into a reactor containing solid sodium/potassium borohydride, stirring until no obvious bubbles are generated, and reducing an iridium compound in the waste liquid into a metallic state to precipitate out, wherein the molar ratio of the sodium/potassium borohydride to iridium in the organic waste liquid is 5-30;
C. and D, washing the iridium precipitate obtained in the step B by using absolute ethyl alcohol and deionized water at the temperature of 80 ℃, and drying in nitrogen gas flow at the temperature of 250-300 ℃ in a tubular furnace to obtain iridium powder.
The method has the advantages that the existing incineration method and the oxidation dissolution method both need to destroy organic matter systems, which cause the loss of iridium in the recovery process and destroy organic matters. According to the invention, the iridium-containing organic waste liquid is directly treated by using a strong reducing agent sodium/potassium borohydride, so that an iridium component is precipitated in a metal form, and the separated organic matter component can be subjected to other recovery treatments. According to the invention, incineration, oxidation and other treatment are not needed, the pH of the waste liquid is adjusted to 7-10, the stability of the reducing agent in the system is ensured, and the using amount of the reducing agent is reduced; the tributyl phosphate is added to effectively inhibit the generation of a large amount of bubbles in the reaction process, and the loss of iridium caused by overflowing of the tank can be avoided. The method has the advantages of simple process, high recovery efficiency and strong adaptability to raw materials, and can treat various iridium-containing organic waste liquids (the mass fraction of iridium is 0.01-3%).
Detailed Description
Example 1 taking 5000g of reaction waste liquid (iridium content 0.24%) generated in the process of preparing 1, 5-cyclooctadiene iridium chloride dimer, adjusting the pH value to 10, adding 5g of tributyl phosphate, slowly adding the waste liquid into a reactor containing 50g of solid reducing agent sodium borohydride, and fully stirring for reaction until no bubbles are generated; after the reaction is finished, iridium precipitate is separated by reduced pressure filtration, is fully washed by absolute ethyl alcohol and deionized water at the temperature of 80 ℃, is filtered, and is dried in a tubular furnace at the temperature of 300 ℃ under nitrogen flow to obtain 10.82g of iridium powder, wherein the recovery rate of iridium is 90.17%.
Example 2 taking 2000g of reaction waste liquid (iridium content is 0.08%) generated in the process of preparing acetylacetonatodicarbonyl iridium, adjusting the pH value to 10, adding 1.5g of tributyl phosphate, slowly adding the waste liquid into a reactor containing 25g of solid reducing agent potassium borohydride, and fully stirring for reaction until no bubbles are generated; after the reaction is finished, the iridium precipitate is separated by reduced pressure filtration, is fully washed by absolute ethyl alcohol and deionized water at the temperature of 80 ℃, is filtered, and is dried in a tubular furnace at the temperature of 300 ℃ under nitrogen flow to obtain 1.43g of iridium powder, wherein the recovery rate of the iridium is 89.37%.
Example 3 3000g (iridium content 2.19%) of a concentrated solution obtained by concentrating a reaction waste liquid generated in the process of preparing 1, 5-cyclooctadiene iridium chloride dimer through reduced pressure distillation is adjusted to have a pH value of 7, 3g of tributyl phosphate is added, the waste liquid is slowly added into a reactor containing 150g of solid reducing agent sodium borohydride, and the mixture is fully stirred for reaction until no bubbles are generated; after the reaction is finished, the iridium precipitate is separated by reduced pressure filtration, is fully washed by absolute ethyl alcohol and deionized water at the temperature of 80 ℃, is filtered, and is dried in a tubular furnace at the temperature of 300 ℃ under nitrogen flow to obtain 62.00g of iridium powder, wherein the recovery rate of the iridium is 94.36%.
Example 4 a reaction waste solution 1000g (iridium content 0.52%) generated in the process of preparing the organic iridium phosphorescent molecular material complex is adjusted to have a pH value of 8, 1g of tributyl phosphate is added, the waste solution is slowly added into a reactor containing 30g of solid reducing agent sodium borohydride, and the mixture is fully stirred for reaction until no bubbles are generated; after the reaction is finished, the iridium precipitate is separated by reduced pressure filtration, is fully washed by absolute ethyl alcohol and deionized water at the temperature of 80 ℃, is filtered, and is dried in a tubular furnace at the temperature of 300 ℃ under nitrogen flow to obtain iridium powder of 4.70g, wherein the recovery rate of iridium is 90.38%.
Claims (2)
1. A method for recovering iridium from an iridium-containing organic waste liquid is characterized by comprising the following steps: adjusting the pH value of the iridium-containing organic waste liquid, adding a defoaming agent, carrying out reduction reaction on the waste liquid and a solid reducing agent, reducing an iridium compound in the waste liquid into metallic iridium precipitate, filtering, washing and drying to obtain iridium powder, wherein the method comprises the following specific steps:
A. adjusting the pH value of the iridium-containing organic waste liquid to 7-10, and adding 0.05-0.1 mass% of defoaming agent tributyl phosphate into the iridium-containing organic waste liquid;
B. slowly adding the organic waste liquid obtained in the step A into a reactor containing solid sodium/potassium borohydride, stirring until no obvious bubbles are generated, and reducing iridium in the waste liquid into a metallic state to precipitate, wherein the molar ratio of the sodium/potassium borohydride to iridium in the organic waste liquid is 5-30;
C. washing the iridium precipitate obtained in the step B by absolute ethyl alcohol and deionized water at the temperature of 80 ℃ respectively until the iridium precipitate is neutral, drying the iridium precipitate in a nitrogen gas flow at the temperature of 250-300 ℃ in a tubular furnace to obtain iridium powder,
the iridium-containing organic waste liquid treated by the method is any one or more of reaction waste liquids of 1, 5-cyclooctadiene iridium chloride dimer, acetylacetone dicarbonyl iridium, carbonyl tris (triphenylphosphine) iridium chloride, carbonyl bis (triphenylphosphine) iridium chloride and organic iridium phosphorescent molecular material complex prepared from hydrated iridium trichloride, wherein the content of iridium is 0.01-3%.
2. A method for recovering iridium from an iridium-containing organic waste liquid is characterized by comprising the following steps:
taking 5000g of reaction waste liquid generated in the process of preparing 1, 5-cyclooctadiene iridium chloride dimer, adjusting the pH value to 10, adding 5g of tributyl phosphate, slowly adding the waste liquid into a reactor containing 50g of solid reducing agent sodium borohydride, and fully stirring for reaction until no bubbles are generated; after the reaction is finished, iridium precipitate is separated by reduced pressure filtration, is fully washed by absolute ethyl alcohol and deionized water at the temperature of 80 ℃, is filtered, and is dried in a tubular furnace at the temperature of 300 ℃ under nitrogen flow to obtain 10.82g of iridium powder, wherein the recovery rate of iridium is 90.17%.
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| CN1105786C (en) * | 1999-05-07 | 2003-04-16 | 中国石油化工集团公司北京化工研究院 | Method for recovering metal rhodium from waste rhodium catalyst raffinate |
| CN101362207A (en) * | 2008-09-19 | 2009-02-11 | 浙江省冶金研究院有限公司 | Method for recovering rhodium from the organic waste liquor |
| CN102277499B (en) * | 2011-08-11 | 2012-12-26 | 杭州凯大催化金属材料有限公司 | Method for recovering rhodium from organic waste liquid produced in carbonyl synthesis reaction |
| CN102443707A (en) * | 2011-11-30 | 2012-05-09 | 徐州浩通新材料科技股份有限公司 | Method for recycling platinum from organic alcohol waste liquor |
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