CN114134335A - Method for recovering rhodium in rhodium-containing nitrite wastewater - Google Patents
Method for recovering rhodium in rhodium-containing nitrite wastewater Download PDFInfo
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- CN114134335A CN114134335A CN202111211394.1A CN202111211394A CN114134335A CN 114134335 A CN114134335 A CN 114134335A CN 202111211394 A CN202111211394 A CN 202111211394A CN 114134335 A CN114134335 A CN 114134335A
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- rhodium
- nitrite
- wastewater
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- noble metal
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- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium atom Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 title claims abstract description 52
- 239000002351 wastewater Substances 0.000 title claims abstract description 49
- IOVCWXUNBOPUCH-UHFFFAOYSA-M Nitrite anion Chemical compound [O-]N=O IOVCWXUNBOPUCH-UHFFFAOYSA-M 0.000 title claims abstract description 43
- 229910052703 rhodium Inorganic materials 0.000 title claims abstract description 34
- 239000010948 rhodium Substances 0.000 title claims abstract description 34
- 238000000034 method Methods 0.000 title claims abstract description 29
- 229910000510 noble metal Inorganic materials 0.000 claims abstract description 26
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 24
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 24
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical group [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000002253 acid Substances 0.000 claims abstract description 13
- 239000000706 filtrate Substances 0.000 claims abstract description 12
- 239000001257 hydrogen Substances 0.000 claims abstract description 12
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 12
- 239000012279 sodium borohydride Substances 0.000 claims abstract description 11
- 229910000033 sodium borohydride Inorganic materials 0.000 claims abstract description 11
- 230000002378 acidificating effect Effects 0.000 claims abstract description 10
- 238000001914 filtration Methods 0.000 claims abstract description 10
- 239000012535 impurity Substances 0.000 claims abstract description 9
- QZPSXPBJTPJTSZ-UHFFFAOYSA-N aqua regia Chemical compound Cl.O[N+]([O-])=O QZPSXPBJTPJTSZ-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000010970 precious metal Substances 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 5
- 239000012065 filter cake Substances 0.000 claims abstract description 5
- 238000003756 stirring Methods 0.000 claims abstract description 5
- 238000005406 washing Methods 0.000 claims abstract description 5
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 11
- 230000035484 reaction time Effects 0.000 claims description 9
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims description 8
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 6
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims description 6
- 238000006722 reduction reaction Methods 0.000 claims description 6
- 235000010323 ascorbic acid Nutrition 0.000 claims description 4
- 229960005070 ascorbic acid Drugs 0.000 claims description 4
- 239000011668 ascorbic acid Substances 0.000 claims description 4
- QDWYPRSFEZRKDK-UHFFFAOYSA-M sodium;sulfamate Chemical compound [Na+].NS([O-])(=O)=O QDWYPRSFEZRKDK-UHFFFAOYSA-M 0.000 claims description 4
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims description 3
- 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 3
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 3
- NKZXQZGFOHGPDL-UHFFFAOYSA-K [Rh+3].[O-]N=O.[O-]N=O.[O-]N=O Chemical compound [Rh+3].[O-]N=O.[O-]N=O.[O-]N=O NKZXQZGFOHGPDL-UHFFFAOYSA-K 0.000 claims description 3
- 238000006243 chemical reaction Methods 0.000 claims description 3
- 235000019253 formic acid Nutrition 0.000 claims description 3
- QWPPOHNGKGFGJK-UHFFFAOYSA-N hypochlorous acid Chemical compound ClO QWPPOHNGKGFGJK-UHFFFAOYSA-N 0.000 claims description 3
- LNOPIUAQISRISI-UHFFFAOYSA-N n'-hydroxy-2-propan-2-ylsulfonylethanimidamide Chemical compound CC(C)S(=O)(=O)CC(N)=NO LNOPIUAQISRISI-UHFFFAOYSA-N 0.000 claims description 3
- 229910052708 sodium Inorganic materials 0.000 claims description 3
- 239000011734 sodium Substances 0.000 claims description 3
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 claims description 3
- 239000011701 zinc Substances 0.000 claims description 3
- 229910052725 zinc Inorganic materials 0.000 claims description 3
- 235000016804 zinc Nutrition 0.000 claims description 3
- 229910052751 metal Inorganic materials 0.000 abstract description 10
- 239000002184 metal Substances 0.000 abstract description 10
- 238000011084 recovery Methods 0.000 abstract description 9
- 230000000694 effects Effects 0.000 abstract description 4
- 125000004435 hydrogen atom Chemical class [H]* 0.000 abstract 1
- 238000000746 purification Methods 0.000 description 4
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 2
- -1 metal compound nitrogen oxide Chemical class 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- MWUXSHHQAYIFBG-UHFFFAOYSA-N nitrogen oxide Inorganic materials O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 2
- 229910052697 platinum Inorganic materials 0.000 description 2
- LPXPTNMVRIOKMN-UHFFFAOYSA-M sodium nitrite Chemical compound [Na+].[O-]N=O LPXPTNMVRIOKMN-UHFFFAOYSA-M 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 239000000543 intermediate Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- KIDPOJWGQRZHFM-UHFFFAOYSA-N platinum;hydrate Chemical group O.[Pt] KIDPOJWGQRZHFM-UHFFFAOYSA-N 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 235000010288 sodium nitrite Nutrition 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
Classifications
-
- 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
-
- 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
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Manufacturing & Machinery (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Treatment Of Water By Oxidation Or Reduction (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention relates to a method for recovering rhodium in rhodium-containing nitrite wastewater, which comprises the following steps: 1: adding the water treatment agent into the waste water containing the nitrite and the platinum group, and fully stirring until no bubbles are generated; 2: adding the obtained strong acid solution into an acidic reducing agent, standing, and filtering to remove other noble metal impurities; 3: adjusting the pH value of the filtrate to be more than 7 by using sodium hydroxide, adding sodium borohydride, standing and filtering to obtain rhodium black; 4: and washing the filter cake with aqua regia, drying, introducing hydrogen, and obtaining rhodium powder meeting the purity requirement from the wastewater. The invention has the advantages that: the water treatment agent is used for efficiently removing nitrite, simultaneously, the coordination effect of the nitrite and the platinum group metal is broken through, the reduction effect of the noble metal impurities under different reducing agents is adopted, the noble metal impurities are removed in the process of recovering the platinum group metal in the wastewater, and finally, the rhodium powder meeting the requirement of 99.9 percent of purity is obtained. The treatment process has mild conditions, high nitrite removal efficiency, high precious metal rhodium recovery efficiency, high yield and high purity.
Description
Technical Field
The invention relates to a method for recovering rhodium in waste water containing rhodium nitrite, in particular to a method for treating waste water containing sodium nitrite and platinum group metal purification, belonging to the technical field of precious metal purification waste water treatment and precious metal recovery in waste water.
Background
Noble metals are widely used in high-tech fields such as metal catalysis, medical treatment, petrochemical industry, new energy and the like due to unique physicochemical properties of the noble metals. At present, nitrite is used as a coordination agent in the synthesis of noble metal compound nitrogen oxide intermediates and wet chemical purification in a platinum group purification process.
The process products can generate a large amount of high-concentration nitrite noble metal wastewater in the production process. Due to the special coordination property of nitrite and platinum group metal, if the reducing agent is directly used for wastewater reduction, the difficulties of great reduction difficulty, low recovery rate, high noble metal residue and the like in wastewater exist.
In the prior art, a solution concentration incineration method is generally adopted for high-concentration nitrite precious metal wastewater, and the method has the problems of high energy consumption, long concentration time, low treatment efficiency, complicated steps, high pollution in an incineration process, difficult platinum group metal recovery, low recovery rate and the like.
Disclosure of Invention
The invention provides a method for recovering rhodium in rhodium-containing nitrite wastewater, which aims to overcome the defects in the prior art, realize mild treatment process conditions and high nitrite removal efficiency, and simultaneously has the characteristics of high recovery efficiency, high yield, high purity and the like of noble metal rhodium.
The technical solution of the invention is as follows: a method for recovering rhodium in rhodium-containing nitrite wastewater comprises the following steps:
step 1: adding a water treatment agent into the waste water containing the nitrite and the platinum group, and fully stirring until no bubbles are generated so as to remove the nitrite and finally form strong acid waste water with the pH value less than 1;
step 2: adding the strong acid solution obtained in the step 1 into an acid reducing agent, standing, and filtering to remove other noble metal impurities;
and step 3: adjusting the pH value of the filtrate obtained in the step 2 to be more than 7 by using sodium hydroxide, adding an alkaline reducing agent sodium borohydride, standing, and filtering to obtain rhodium black, wherein the content of noble metal in the filtrate is less than 0.005 per thousand;
and 4, step 4: and (4) washing the filter cake obtained in the step (3) by using aqua regia, drying, and introducing hydrogen to obtain rhodium powder meeting the purity requirement from the wastewater.
Preferably, in the step 1, the initial pH of the waste water containing the platinum group nitrite is 6-8, the initial temperature is room temperature, the mass fraction of the precious metal containing the platinum group is 0.1-2 per mill, and the mass fraction of the nitrite is 5-15%.
Preferably, in the step 1, the water treatment agent is one or more of sodium sulfonate, sodium sulfamate, hydrogen peroxide, hypochlorous acid and sulfamic acid, and the mass ratio of the water treatment agent to the wastewater is 5-20: 100.
preferably, in the step 1, the reaction time of the water treatment agent for removing the nitrite is 10-60 minutes.
Preferably, in the step 2, the acidic reducing agent is one or more of formic acid, ascorbic acid and zinc blocks, and the mass ratio of the acidic reducing agent to the noble metal in the wastewater is 50-500: 100.
preferably, in the step 2, the reduction reaction time of the acidic reducing agent is 1 to 8 hours.
Preferably, in the step 3, the pH is adjusted to 8-14 by sodium hydroxide, and the mass ratio of the basic reducing agent sodium borohydride to rhodium is 50-200: 10.
preferably, in the step 3, after the sodium borohydride is added, the reaction temperature is 40-90 ℃, the reaction time is 1-5 hours, and the content of the noble metal in the filtrate is 0.001-0.005 per thousand.
Preferably, in the step 4, the mass ratio of the aqua regia to the rhodium black is 10-100: 1.
preferably, in the step 4, the temperature of the hydrogen introducing furnace is controlled to be 600-750 ℃, the hydrogen introducing time is 4-10 hours, and the purity of the rhodium powder is 99.9 percent finally.
The invention has the advantages that: the method is reasonable in design, the coordination effect of the nitrite and the platinum group metal is broken through while the water treatment agent is used for efficiently removing the nitrite, the reduction effect of the noble metal impurities under different reducing agents is adopted, the noble metal impurities are removed in the process of recovering the waste water platinum group metal, and finally the rhodium powder meeting the requirement of 99.9% in purity is obtained. Solves the problems of low treatment efficiency and complex steps of the waste water containing high-concentration nitrite, difficult recovery of platinum group metals in the waste water containing high-concentration nitrite and low recovery rate in the prior art. The treatment process has mild conditions, high nitrite removal efficiency, and the characteristics of high recovery efficiency, high yield, high purity and the like of the noble metal rhodium.
Detailed Description
The present invention will be described in further detail with reference to examples and specific embodiments.
A method for recovering rhodium in rhodium-containing nitrite wastewater comprises the following steps:
step 1: adding a certain amount of water treatment agent into the waste water containing the nitrite and the platinum family, and fully stirring until no bubbles are generated so as to remove the nitrite and finally form strong acid waste water with the pH value less than 1;
step 2: adding a certain amount of acid reducing agent into the strong acid solution obtained in the step (1), standing for a period of time, and filtering to remove other noble metal impurities;
and step 3: adjusting the pH value of the filtrate obtained in the step 2 to be more than 7 by using sodium hydroxide, adding a certain amount of alkaline reducing agent sodium borohydride, standing for a period of time, and filtering to obtain rhodium black, wherein the content of noble metal in the filtrate is less than 0.005 per thousand;
and 4, step 4: and (4) washing the filter cake obtained in the step (3) by using aqua regia, drying, and introducing hydrogen to obtain rhodium powder meeting the purity requirement from the wastewater.
In the step 1, the initial pH value of the waste water containing the platinum group nitrite is 6-8, the initial temperature is room temperature, the mass fraction of the precious metal containing the platinum group is 0.1-2 per mill, and the mass fraction of the nitrite is 5-15%.
In the step 1, the used water treatment agent is preferably one or more of sodium sulfonate, sodium sulfamate, hydrogen peroxide, hypochlorous acid and sulfamic acid, and the mass ratio of the water treatment agent to the wastewater is 5-20: 100.
in step 1, the reaction time of the water treatment agent for removing nitrite is preferably 10 to 60 minutes.
In the step 2, the used acidic reducing agent is preferably one or more of formic acid, ascorbic acid and zinc blocks, and the mass ratio of the acidic reducing agent to the noble metal in the wastewater is 50-500: 100.
in step 2, the reduction reaction time of the acidic reducing agent is preferably 1 to 8 hours.
In the step 3, the pH value of sodium hydroxide is preferably adjusted to be 8-14, and the mass ratio of the alkaline reducing agent sodium borohydride to rhodium is 50-200: 10.
in the step 3, after the sodium borohydride is added, the reaction temperature is preferably 40-90 ℃, the reaction time is 1-5 hours, and the content of noble metal in the filtrate is 0.001-0.005 per mill.
In the step 4, the mass ratio of the aqua regia to the rhodium black is preferably 10-100: 1, controlling the temperature of a hydrogen introducing furnace at 600-750 ℃, and introducing hydrogen for 4-10 hours, wherein the purity of the final rhodium powder is 99.9%.
Examples
A method for recovering rhodium in rhodium-containing nitrite wastewater comprises the following steps:
step 1: adding 10kg of water treatment agent sodium sulfamate into 200L of wastewater, wherein the wastewater contains 10 mass fractions of nitrite and 200g of platinum group metal, stirring and fully reacting for 40 minutes until no bubbles are generated, removing the nitrite, and finally forming strong acid wastewater with the pH value less than 1;
step 2: adding a certain amount of acid reducing agent ascorbic acid into the strong acid solution obtained in the step 1, standing for 5 hours, and filtering to remove impurities such as other noble metals, such as gold, palladium, platinum and the like;
and step 3: adjusting the pH value of the filtrate obtained in the step 2 to 10 by using sodium hydroxide, adding 1000g of alkaline reducing agent sodium borohydride, standing for 2 hours, and filtering to obtain rhodium black, wherein the content of noble metal in the filtrate is 0.003 thousandth;
and 4, step 4: and (3) washing the filter cake obtained in the step (3) by using aqua regia, drying, putting into a hydrogen furnace, controlling the temperature at 650 ℃, and introducing hydrogen for 5 hours, so that rhodium powder with the purity of 99.9 percent can be obtained from the wastewater.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various changes and modifications can be made without departing from the inventive concept of the present invention, and these changes and modifications are all within the scope of the present invention.
Claims (10)
1. A method for recovering rhodium in rhodium-containing nitrite wastewater is characterized by comprising the following steps:
step 1: adding a water treatment agent into the waste water containing the nitrite and the platinum group, and fully stirring until no bubbles are generated so as to remove the nitrite and finally form strong acid waste water with the pH value less than 1;
step 2: adding the strong acid solution obtained in the step 1 into an acid reducing agent, standing, and filtering to remove other noble metal impurities;
and step 3: adjusting the pH value of the filtrate obtained in the step 2 to be more than 7 by using sodium hydroxide, adding an alkaline reducing agent sodium borohydride, standing, and filtering to obtain rhodium black, wherein the content of noble metal in the filtrate is less than 0.005 per thousand;
and 4, step 4: and (4) washing the filter cake obtained in the step (3) by using aqua regia, drying, and introducing hydrogen to obtain rhodium powder meeting the purity requirement from the wastewater.
2. The method as claimed in claim 1, wherein in step 1, the initial pH of the waste water containing rhodium and nitrite is 6-8, the initial temperature is room temperature, the mass fraction of precious metals in platinum group is 0.1-2%, and the mass fraction of nitrite is 5-15%.
3. The method for recovering rhodium from the rhodium-containing nitrite wastewater as claimed in claim 2, wherein in the step 1, the water treatment agent is one or more of sodium sulfonate, sodium sulfamate, hydrogen peroxide, hypochlorous acid and sulfamic acid, and the mass ratio of the water treatment agent to the wastewater is 5-20: 100.
4. the method as claimed in claim 3, wherein in step 1, the reaction time of the water treatment agent for removing nitrite is 10-60 min.
5. The method for recovering rhodium from waste water containing rhodium nitrite as claimed in claim 4, wherein in said step 2, the acidic reducing agent is one or more of formic acid, ascorbic acid and zinc block, the mass ratio of the acidic reducing agent to noble metal in the waste water is 50-500: 100.
6. the method as claimed in claim 5, wherein in step 2, the reduction reaction time of the acidic reducing agent is 1-8 hours.
7. The method for recovering rhodium from rhodium-containing nitrite wastewater as set forth in claim 6, characterized in that in said step 3, pH is adjusted to 8-14 by sodium hydroxide, and mass ratio of alkaline reducing agent sodium borohydride to rhodium is 50-200: 10.
8. the method for recovering rhodium from rhodium-containing nitrite wastewater as set forth in claim 7, wherein in said step 3, after adding sodium borohydride, the reaction temperature is 40 ℃ to 90 ℃, the reaction time is 1 to 5 hours, and the content of noble metal in the filtrate is 0.001 to 0.005 ‰.
9. The method for recovering rhodium from the waste water containing rhodium nitrite as set forth in claim 8, characterized in that in the step 4, the mass ratio of aqua regia to rhodium black is 10-100: 1.
10. the method for recovering rhodium from rhodium-containing nitrite wastewater as set forth in claim 9, wherein in the step 4, the temperature of the hydrogen furnace is controlled at 600-750 ℃, the hydrogen introducing time is 4-10 hours, and the final purity of rhodium powder is up to 99.9%.
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