CN112537808A - Method for synthesizing rhodium nitrate solution by using rhodium-containing waste - Google Patents
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Abstract
The invention discloses a method for synthesizing rhodium nitrate solution by utilizing rhodium-containing waste, which comprises the following steps: adjusting the acid concentration in the rhodium-containing waste leaching solution to 4-5 mol/L, and then heating and refluxing to obtain a rhodium acid solution; adding a precipitator into the rhodium acidic solution, heating to 100-110 ℃, refluxing for 12-24 h to obtain a mixture containing brownish black precipitates, cooling, filtering, dissolving, filtering, washing and dissolving to obtain a rhodium-containing solution; exchanging the rhodium-containing solution through hydrogen type cation resin, adding the rhodium-containing solution with trace impurities removed into a potassium hydroxide solution for precipitation reaction, and then washing and drying to obtain high-purity rhodium hydroxide solid; and adding the high-purity rhodium hydroxide solid into a nitric acid solution for dissolving reaction, and filtering to obtain a rhodium nitrate solution. The method has the advantages of strong process applicability, simple operation, low cost, high purity of the synthesized rhodium nitrate product and good stability.
Description
Technical Field
The invention relates to the field of precious metal chemical synthesis, in particular to a method for synthesizing a rhodium nitrate solution by utilizing rhodium-containing waste.
Background
Rhodium is an important precious metal in the platinum group and has irreplaceable effects in many key fields. The world's 90% rhodium is mainly used as an automobile exhaust catalyst, it is also commonly used as a hydrogenation catalyst, a thermocouple, a platinum rhodium alloy, etc., it is also commonly plated on searchlights and reflectors, as a polishing agent for precious stones and electrical contact parts, and rhodium is also used as a plating film for other metals. In recent years, the market demand of rhodium catalysts is huge, the demand of precursor rhodium nitrate solution for synthesizing the rhodium catalysts is directly driven, and the direct synthesis of rhodium nitrate from rhodium-containing waste materials is inevitable in the face of the huge market demand.
The traditional synthesis process of rhodium nitrate comprises the following steps: the rhodium powder is sequentially subjected to the working procedures of oxidation, leaching, filtration, hydrolysis, washing, filtration, acid dissolution and the like to obtain the gloriol. The yield of rhodium nitrate synthesized by the process is about 70%, the working procedures are long, the product purity is low, and particularly, chloride ions in the product are difficult to remove, so that the catalyst is poisoned, and the service life of the catalyst is seriously influenced.
At present, the direct synthesis of rhodium nitrate from rhodium-containing waste is mainly limited by a rhodium recovery method, and the recovery and purification methods of rhodium in the waste mainly comprise a precipitation separation method, an electrolysis method, a solvent extraction method, a resin separation method, an adsorption method, a metal replacement method and the like. The traditional precipitation purification method refers to a sodium nitrite complexing method, an ammoniation method, an ammonium sulfite method and the like. Sodium nitrite complexation method for generating stable soluble sodium nitrite complex Na by using sodium nitrite and rhodium3Rh(NO2)6And the base metal is hydrolyzed to form hydroxide precipitate, which is then reacted with rhodiumBut other platinum group metal liquid in the solution is also complexed into a similar soluble sodium nitrite complex by adopting the method, and cannot be completely separated from rhodium. The ammoniation method adopts the reaction of ammonia hexachlororhodate and ammonia water to generate [ Rh (NH)3)5Cl]Cl2Precipitation, but the operation process is complicated and the recovery rate is low. CN1414125A method for recovering rhodium from waste rhodium catalyst in oxo-synthesis reaction, burning and ashing the waste catalyst residual liquid, melting the residue with acid sulfate to generate soluble rhodium salt, and separating rhodium by electrolysis technology to obtain rhodium metal, wherein the once-through recovery rate of rhodium powder is more than 96%, and the purity is 99.95%. However, the rhodium plating layer obtained by the electrolytic method is inconvenient for rhodium powder conversion, which is a great limitation influencing the application of the rhodium plating layer.
The method for synthesizing rhodium nitrate by using rhodium-containing waste materials is greatly influenced by impurities, a rhodium recovery solution generally contains a large amount of sodium, potassium, aluminum, iron, nickel, copper, calcium and other impurities, and also contains other platinum group metals, the separation and purification of the platinum group metals are difficult due to similar chemical properties, the recovery and purification method has harsh process conditions, large environmental pollution and low recovery purity, and how to recover and purify the waste materials to synthesize rhodium compounds becomes a problem to be solved for synthesizing rhodium nitrate.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides the method for synthesizing the rhodium nitrate solution by utilizing the rhodium-containing waste, which has the advantages of simple process, controllable process, high purity of the rhodium hydroxide intermediate product, capability of avoiding the poisoning of rhodium nitrate, improvement on the stability of rhodium nitrate and prolonging the service life of rhodium nitrate.
The invention adopts the following technical scheme:
a method for synthesizing a rhodium nitrate solution by using rhodium-containing waste is characterized by comprising the following steps:
(1) adjusting the acid concentration in the rhodium-containing waste leachate to 4-5 mol/L, and heating and refluxing until the rhodium concentration in the rhodium-containing waste leachate is 50-70 g/L to obtain a rhodium acid solution;
(2) adding a precipitant into the rhodium acidic solution, heating to 100-110 ℃, refluxing for 12-24 h to obtain a mixture containing brownish black precipitates, cooling and filtering the mixture containing the brownish black precipitates, dissolving the mixture in ethanol at 40-50 ℃ for 5-6 h, filtering and washing to obtain rhodium salt precipitates, and dissolving the rhodium salt precipitates to obtain a rhodium-containing solution;
(3) exchanging the rhodium-containing solution through hydrogen type cation resin to obtain the rhodium-containing solution with trace impurities removed;
(4) adding the rhodium-containing solution with trace impurities removed into a potassium hydroxide solution for precipitation reaction, and then washing and drying to obtain a high-purity rhodium hydroxide solid; the process conditions of the precipitation reaction are as follows: the pH value of the reaction is 8-9, the reaction temperature is 50-60 ℃, and the reaction time is 2-3 h;
(5) adding high-purity rhodium hydroxide solid into a nitric acid solution for dissolution reaction, and filtering to obtain a rhodium nitrate solution; the process conditions of the dissolution reaction are as follows: the dissolving temperature is 40-50 ℃, and the dissolving time is 2-3 h.
The method for synthesizing the rhodium nitrate solution by using the rhodium-containing waste is characterized in that in the step (1), the acid concentration in the rhodium-containing waste leachate is adjusted to 4-5 mol/L, and then the rhodium-containing waste leachate is heated and refluxed for 18-24 h.
The method for synthesizing the rhodium nitrate solution by using the rhodium-containing waste is characterized in that the precipitator in the step (2) is benzyltriethylammonium bromide, and the mass ratio of the precipitator to the rhodium acid solution is (5-7): 1.
The method for synthesizing the rhodium nitrate solution by using the rhodium-containing waste is characterized in that the mixture containing the brownish black precipitate is cooled, filtered, dissolved and filtered in the step (2), and then is washed by using a mixed solution formed by ethanol and methanol.
The method for synthesizing the rhodium nitrate solution by using the rhodium-containing waste is characterized in that the mass percentage concentration of the potassium hydroxide solution in the step (4) is 16% -20%, and after precipitation reaction, pure water and ethanol are adopted for washing and drying, so that high-purity rhodium hydroxide solid is obtained.
The method for synthesizing the rhodium nitrate solution by using the rhodium-containing waste is characterized in that the mass percentage concentration of the nitric acid solution in the step (5) is 50% -60%, and the high-purity rhodium hydroxide solid is added into the nitric acid solution for dissolution reaction and then filtered by a Buchner funnel.
The invention has the beneficial technical effects that: the invention separates, purifies and synthesizes rhodium nitrate solution from rhodium-containing waste leachate and other precious metals and base metals. The invention adopts benzyl triethyl ammonium bromide as a precipitator, platinum (IV) and rhodium (III) acid solution and excess tetramethyl ammonium chloride can react to generate platinum salt and rhodium salt precipitate, palladium (II) and other base metals do not generate precipitate and are left in the solution, the platinum salt precipitate is dissolved in ethanol, so that rhodium is separated from other impurities, ion exchange resin is used for removing residual trace impurities, high-purity rhodium hydroxide is obtained through conversion, and rhodium nitrate is synthesized by dissolving rhodium hydroxide in nitric acid. The method utilizes a mode of combining a precipitation method and an ion exchange method to separate and purify rhodium, the obtained rhodium hydroxide has high purity, and the synthesized rhodium nitrate product has high purity and good stability, thereby avoiding the poisoning of rhodium nitrate, improving the stability of rhodium nitrate and prolonging the service life of rhodium nitrate. The method has the advantages of strong process applicability, simple operation, controllable process, low cost, zero emission and no environmental pollution.
Detailed Description
The invention discloses a method for synthesizing rhodium nitrate solution by utilizing rhodium-containing waste, which comprises the following steps:
(1) liquid preparation: adjusting the acid concentration in the rhodium-containing waste leaching solution to 4-5 mol/L, and then heating and refluxing for 18-24 h. On the one hand, due to RhCl6 3-Can be hydrated, hydroxylated, acid-dissociated of hydrated ions or chlorinated along with the changes of the acidity, the concentration of chloride ions, the temperature, the standing time and the like of the solution to generate a series of chlorine, hydrated complexes or chlorine, water and hydroxyl complexes [ RhCl ]6]3-、[RhCl5(H2O)]2-、[RhCl4(H2O)]-、[RhCl3(H2O)3]、[RhCl2(H2O)4]+、[RhCl2(H2O)5]+、[Rh(H2O)6]3+. The formation of these chloro-water complexes makes it difficult for rhodium to be separated off. Therefore, in order to improve the separation and extraction efficiency of rhodium, it is necessary to combine these componentsThe substance is converted into a complex with good separation performance [ RhCl ] as far as possible6]3-. On the other hand, refluxing may convert tetravalent palladium in solution to divalent palladium to facilitate separation of rhodium from palladium. Until the rhodium concentration in the rhodium-containing waste leachate is 50g/L-70g/L, obtaining a rhodium acid solution; the impurity content in the sample was measured by ICP.
(2) Precipitation and purification: adding a precipitant into the rhodium acidic solution, heating to 100-110 ℃, boiling, refluxing for 12-24 h until rhodium and platinum in the solution generate a large amount of brownish black precipitates to obtain a mixture containing the brownish black precipitates, cooling and filtering the mixture containing the brownish black precipitates, dissolving the mixture in ethanol at 40-50 ℃ for 5-6 h, filtering and washing to obtain brown rhodium salt precipitates, and dissolving the rhodium salt precipitates in a sufficient amount of boiled water to obtain a rhodium-containing solution. When rhodium is precipitated, the addition amount of the precipitator is greatly excessive, so that the concentration of the precipitator reaches saturation, the precipitator is benzyltriethylammonium bromide, the mass ratio of the precipitator to the rhodium acid solution is (5-7):1, and the addition amount of the precipitator is controlled to be 500-700 g/L. And cooling, filtering, dissolving and filtering the mixture containing the brownish black precipitate, washing the mixture by using a mixed solution formed by ethanol and methanol, and removing impurities and redundant precipitator in the precipitate.
(3) Ion exchange purification: exchanging the rhodium-containing solution through hydrogen type cation resin to remove residual trace impurities in the solution to obtain the rhodium-containing solution with trace impurities removed;
(4) preparing rhodium hydroxide: adding the rhodium-containing solution with trace impurities removed into a potassium hydroxide solution for precipitation reaction to completely precipitate rhodium, and then washing and drying to obtain a high-purity rhodium hydroxide solid; the process conditions of the precipitation reaction are as follows: the pH value of the reaction is 8-9, the reaction temperature is 50-60 ℃, and the reaction time is 2-3 h; the mass percent concentration of the potassium hydroxide solution is 16-20%, and pure water and ethanol are adopted for washing and drying after precipitation reaction, so that high-purity rhodium hydroxide solid is obtained. The high-purity rhodium hydroxide solid can be used as a raw material for preparing rhodium powder which meets GB/T1421-2004 standard.
(5) Synthesis of rhodium nitrate: adding high-purity rhodium hydroxide solid into a nitric acid solution for dissolution reaction, and filtering by using a Buchner funnel to remove insoluble impurities to obtain a rhodium nitrate solution. The process conditions of the dissolution reaction are as follows: stirring and reacting for 2-3 h at 40-50 ℃. The mass percentage concentration of the nitric acid solution is 50-60%. The pH value of the rhodium solution purified and dissolved by the precipitation method is 2-4, the acidity of the solution is low, and the rhodium solution is easier to adsorb impurity ions on the resin through hydrogen type cationic resin, so trace impurity ions are easier to remove.
The present invention is further illustrated by the following examples, which are intended to be illustrative of the invention and are not to be construed as limiting the invention.
Example 1
Adjusting the acid concentration in the rhodium-containing waste leaching solution to 4mol/L, and then heating and refluxing for 24h to obtain a rhodium acid solution. The rhodium concentration in the rhodium acid solution was determined to be 55.51g/L, the impurity content Pt was 0.37g/L, Pd was 0.85g/L, Al was 0.53g/L, Fe was 0.29g/L, Ca was 0.33g/L, Mg was 0.26g/L, Cu was 0.41g/L, Ni was 0.33g/L, and Si was 0.18 g/L.
500mL of rhodium acid solution is measured and put into a flask, 250g of benzyltriethylammonium bromide is added, the temperature is raised to 100 ℃ to boil and reflux the solution for 12h until platinum and rhodium in the solution generate brownish black precipitates, and a mixture containing the brownish black precipitates is obtained. Cooling the mixture containing the brownish black precipitate to room temperature, filtering, adding the mixture containing the brownish black precipitate into 100mL of ethanol, heating to 50 ℃ to dissolve for 6 hours, cooling to room temperature, filtering, washing with ethanol and methanol, performing suction filtration to dryness, and dissolving the obtained rhodium precipitate in a sufficient amount of boiled water to obtain a rhodium-containing solution.
And (3) exchanging the rhodium-containing solution through hydrogen type cation resin to obtain the rhodium-containing solution with trace impurities removed. Adding the rhodium-containing solution with trace impurities removed into a potassium hydroxide solution with the mass percent concentration of 20% to perform precipitation reaction to obtain faint yellow rhodium hydroxide, wherein the process conditions of the precipitation reaction are as follows: the pH value of the reaction is 8, and the reaction is stirred at 50 ℃ for 2 hours; and after precipitation, fully washing the precipitate with water and ethanol, and drying the precipitate. The faint yellow rhodium hydroxide is transferred into 100mL nitric acid solution with the mass percentage concentration of 60%, the mixture is heated to 40 ℃, stirred and reacted for 2 hours, so that rhodium hydroxide precipitate is completely dissolved, insoluble impurities are removed through filtration by a Buchner funnel, 166.71 g of rhodium nitrate solution is obtained, the content of rhodium is 16.33% through ICP detection, and the purification rate of the rhodium is 98.11%.
Example 2
Adjusting the acid concentration in the rhodium-containing waste leaching solution to 4.5mol/L, and then heating and refluxing for 24h to obtain a rhodium acid solution. The rhodium concentration in the rhodium acid solution was measured to be 60.61g/L, the impurity content Pt was 0.38g/L, Pd was 0.82g/L, Al was 0.51g/L, Fe was 0.23g/L, Ca was 0.31g/L, Mg was 0.27g/L, Cu was 0.38g/L, Ni was 0.31g/L, and Si was 0.15 g/L.
500mL of rhodium acid solution is measured and put into a flask, 300g of benzyltriethylammonium bromide is added, the temperature is raised to 105 ℃, the solution is boiled and refluxed for 18h until platinum and rhodium in the solution generate brownish black precipitates, and a mixture containing the brownish black precipitates is obtained. Cooling the mixture containing the brownish black precipitate to room temperature, filtering, adding the mixture containing the brownish black precipitate into 100mL of ethanol, heating to 50 ℃ to dissolve for 6 hours, cooling to room temperature, filtering, washing with ethanol and methanol, performing suction filtration to dryness, and dissolving the obtained rhodium precipitate in a sufficient amount of boiled water to obtain a rhodium-containing solution.
And (3) exchanging the rhodium-containing solution through hydrogen type cation resin to obtain the rhodium-containing solution with trace impurities removed. Adding the rhodium-containing solution with trace impurities removed into a potassium hydroxide solution with the mass percent concentration of 20% to perform precipitation reaction to obtain faint yellow rhodium hydroxide, wherein the process conditions of the precipitation reaction are as follows: the pH value of the reaction is 8.5, and the reaction is stirred at 55 ℃ for 2.5 h; and after precipitation, fully washing the precipitate with water and ethanol, and drying the precipitate. The faint yellow rhodium hydroxide is transferred into 100mL nitric acid solution with the mass percentage concentration of 60%, heated to 45 ℃, stirred and reacted for 2.5 hours to ensure that rhodium hydroxide precipitate is completely dissolved, insoluble impurities are removed by filtration through a Buchner funnel to obtain 169.82 g of rhodium nitrate solution, the content of rhodium is 17.56% by ICP detection, and the purification rate of the rhodium is 98.38%.
Example 3
Adjusting the acid concentration in the rhodium-containing waste leaching solution to 4.5mol/L, and then heating and refluxing for 24h to obtain a rhodium acid solution. The rhodium concentration in the rhodium acid solution was determined to be 70.16g/L, the impurity content Pt was 0.33g/L, Pd was 0.84g/L, Al was 0.49g/L, Fe was 0.26g/L, Ca was 0.36g/L, Mg was 0.23g/L, Cu was 0.34g/L, Ni was 0.35g/L, and Si was 0.12 g/L.
500mL of rhodium acid solution is measured and put into a flask, 350g of benzyltriethylammonium bromide is added, the temperature is raised to 110 ℃, the solution is boiled and refluxed for 24h until platinum and rhodium in the solution generate brownish black precipitates, and a mixture containing the brownish black precipitates is obtained. Cooling the mixture containing the brownish black precipitate to room temperature, filtering, adding the mixture containing the brownish black precipitate into 100mL of ethanol, heating to 50 ℃ to dissolve for 6 hours, cooling to room temperature, filtering, washing with ethanol and methanol, performing suction filtration to dryness, and dissolving the obtained rhodium precipitate in a sufficient amount of boiled water to obtain a rhodium-containing solution.
And (3) exchanging the rhodium-containing solution through hydrogen type cation resin to obtain the rhodium-containing solution with trace impurities removed. Adding the rhodium-containing solution with trace impurities removed into a potassium hydroxide solution with the mass percent concentration of 20% to perform precipitation reaction to obtain faint yellow rhodium hydroxide, wherein the process conditions of the precipitation reaction are as follows: the pH value of the reaction is 9, and the reaction is carried out for 3 hours under the stirring at 60 ℃; and after precipitation, fully washing the precipitate with water and ethanol, and drying the precipitate. Transferring the light yellow rhodium hydroxide into 100mL of nitric acid solution with the mass percentage concentration of 60%, heating to 50 ℃, stirring for reaction for 3h to ensure that rhodium hydroxide precipitates are completely dissolved, filtering by using a Buchner funnel to remove insoluble impurities to obtain 182.15 g of rhodium nitrate solution, wherein the content of rhodium is 19.03% by ICP detection, and the purification rate of the rhodium is 98.82%.
Claims (6)
1. A method for synthesizing a rhodium nitrate solution by using rhodium-containing waste is characterized by comprising the following steps:
(1) adjusting the acid concentration in the rhodium-containing waste leachate to 4-5 mol/L, and heating and refluxing until the rhodium concentration in the rhodium-containing waste leachate is 50-70 g/L to obtain a rhodium acid solution;
(2) adding a precipitant into the rhodium acidic solution, heating to 100-110 ℃, refluxing for 12-24 h to obtain a mixture containing brownish black precipitates, cooling and filtering the mixture containing the brownish black precipitates, dissolving the mixture in ethanol at 40-50 ℃ for 5-6 h, filtering and washing to obtain rhodium salt precipitates, and dissolving the rhodium salt precipitates to obtain a rhodium-containing solution;
(3) exchanging the rhodium-containing solution through hydrogen type cation resin to obtain the rhodium-containing solution with trace impurities removed;
(4) adding the rhodium-containing solution with trace impurities removed into a potassium hydroxide solution for precipitation reaction, and then washing and drying to obtain a high-purity rhodium hydroxide solid; the process conditions of the precipitation reaction are as follows: the pH value of the reaction is 8-9, the reaction temperature is 50-60 ℃, and the reaction time is 2-3 h;
(5) adding high-purity rhodium hydroxide solid into a nitric acid solution for dissolution reaction, and filtering to obtain a rhodium nitrate solution; the process conditions of the dissolution reaction are as follows: the dissolving temperature is 40-50 ℃, and the dissolving time is 2-3 h.
2. The method for synthesizing the rhodium nitrate solution by using the rhodium-containing waste as claimed in claim 1, wherein the acid concentration in the rhodium-containing waste leachate is adjusted to 4mol/L-5mol/L in step (1), and then the rhodium-containing waste leachate is heated and refluxed for 18h-24 h.
3. The method for synthesizing the rhodium nitrate solution by using the rhodium-containing waste material as claimed in claim 2, wherein the precipitating agent in the step (2) is benzyltriethylammonium bromide, and the mass ratio of the precipitating agent to the rhodium acidic solution is (5-7): 1.
4. The method for synthesizing the rhodium nitrate solution by using the rhodium-containing waste material as claimed in claim 2, wherein the mixture containing the brownish black precipitate is cooled, filtered, dissolved and filtered in the step (2), and then is washed by using a mixed solution of ethanol and methanol.
5. The method for synthesizing the rhodium nitrate solution by using the rhodium-containing waste material according to claim 1, wherein the mass percentage concentration of the potassium hydroxide solution in the step (4) is 16% -20%, and after the precipitation reaction, pure water and ethanol are adopted for washing and then drying, so that a high-purity rhodium hydroxide solid is obtained.
6. The method for synthesizing the rhodium nitrate solution by using the rhodium-containing waste material as claimed in claim 5, wherein the mass percentage concentration of the nitric acid solution in the step (5) is 50% -60%, and the high-purity rhodium hydroxide solid is added into the nitric acid solution for dissolution reaction and then filtered by using a Buchner funnel.
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| CN115849586A (en) * | 2021-09-22 | 2023-03-28 | 中国石油化工股份有限公司 | Method for recovering rhodium from rhodium-containing wastewater and recovered rhodanate |
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| CN102212696A (en) * | 2010-07-23 | 2011-10-12 | 金属回收科技有限公司 | Process for recovery of precious metals |
| CN104860358A (en) * | 2015-04-23 | 2015-08-26 | 金川集团股份有限公司 | High purity rhodium recovery purification method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102212696A (en) * | 2010-07-23 | 2011-10-12 | 金属回收科技有限公司 | Process for recovery of precious metals |
| CN104860358A (en) * | 2015-04-23 | 2015-08-26 | 金川集团股份有限公司 | High purity rhodium recovery purification method |
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| 马世昌: "《基础化学反应》", 31 January 2003, 陕西科学技术出版社 * |
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| CN115849586A (en) * | 2021-09-22 | 2023-03-28 | 中国石油化工股份有限公司 | Method for recovering rhodium from rhodium-containing wastewater and recovered rhodanate |
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