CN112442600A - Method for recovering platinum group metal from waste three-way catalyst - Google Patents
Method for recovering platinum group metal from waste three-way catalyst Download PDFInfo
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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
- C22B11/048—Recovery of noble metals from waste materials from spent catalysts
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Abstract
The invention discloses a method for recovering platinum group metals from waste three-way catalysts. Under the condition of low acid, ferric chloride is used as an oxidant, sodium chloride is used as an additive, palladium in the waste three-way catalyst is selectively leached efficiently to obtain leachate rich in palladium, the phenomenon of palladium peroxidation is avoided, and then primary leaching residue is subjected to oxidative leaching in a hydrochloric acid system to obtain leachate rich in platinum and rhodium. The method has high leaching efficiency, wherein the recovery rates of the platinum, the palladium and the rhodium are respectively more than 97%, more than 99% and more than 99.5%.
Description
Technical Field
The invention relates to the technical field of waste three-way catalyst recovery, in particular to a method for recovering platinum group metals from waste three-way catalysts.
Background
According to the prediction of the Ministry of industry and belief, the automobile keeping amount of China will break through 2 hundred million in 2020, and the strict automobile exhaust emission standard highlights the key role of the automobile exhaust catalyst in solving the problem of automobile exhaust emission. About 70% of current automobile exhaust catalysts are three-way catalysts. The three-way catalyst has certain safe life, and after the service life is exceeded, the catalyst is not used after being failed or the catalytic efficiency is reduced, and the catalyst is called as a waste three-way catalyst. The platinum group metal in the waste three-way catalyst has high recovery value. The three-way catalyst contains 0.08-0.12% of platinum, 0.017-0.04% of palladium and 0.007-0.014% of rhodium, and the total amount is 1000-1500 g/t. At present, the total consumption of platinum group metals in the ternary waste catalyst containing platinum, palladium and rhodium is between 90 and 100 tons, compared with primary energy, the content of noble metals is high, the composition is relatively single, and the catalyst is an important secondary resource of the platinum group metals.
Chinese patent CN 1385545A introduces a method for recovering metals such as platinum, palladium, rhodium and the like from automobile exhaust waste catalyst, which comprises crushing the waste catalyst under the process conditions of a solid-liquid ratio of 1:4, a weight ratio of a solvent to the waste catalyst of 3.5-4.5:1, solvent components of HCl 3-4 mol/L and H2SO410-14 mol/L, the initial reaction temperature is 110-120 ℃, the solution is dissolved in 2 hours of reaction time, and 300g of sodium chlorate is prepared into solution to be added in the later stage of dissolution. The leaching rate of the obtained palladium is 98.7 percent, the leaching rate of the platinum is 98.4 percent and the leaching rate of the rhodium is 97.6 percent, and then the comprehensive recovery rate of the palladium is obtained by ammoniating and separating the platinum, ion exchanging and complexing to extract the palladium and replacing the rhodium with copper powder>97 percent, 96 percent of comprehensive recovery rate of platinum and 90 percent of comprehensive recovery rate of rhodium, the leaching temperature of the patent is more than 100 ℃, and the requirements on equipment and the process are high.
Chinese patent CN 108265180A introduces a method for leaching platinum, palladium and rhodium from a waste three-way catalyst, the waste three-way catalyst is roasted and pretreated for 2-8 h at 300-900 ℃, then crushed and ground, the granularity is controlled to be 10-200 meshes, then reduction treatment is carried out for 3h at 60-90 ℃, noble metal in an oxidation state is reduced to a simple substance state, then the reaction is carried out for 2-4 h at more than 40% sulfuric acid as a leaching agent at the temperature of more than 90-110 ℃ and the liquid-solid ratio of 5:1, the alumina matrix of the waste three-way catalyst is dissolved, the dissolution later stage is enhanced and dissolution is carried out, the undissolved alumina is completely dissolved to destroy the matrix structure, finally hydrochloric acid is used as a second-stage leaching agent and added as an oxidant, solid-liquid separation is carried out to obtain a leaching solution rich in platinum, palladium and rhodium, the final leaching rate of platinum is 96.5%, and the sodium chlorate rate of palladium can reach 98.1%, The leaching rate of rhodium was 91.1%. The method aims at solving the problems that the waste three-way catalyst adopts a digestion matrix method, and has high reagent consumption, complex process and high energy consumption due to pretreatment although the method can reach higher leaching rate.
The invention patent CN 102134647A introduces a method for extracting platinum group metals from waste automobile three-way catalysts, which is characterized in that the platinum group metals in the waste three-way catalysts are enriched into a lead ingot by using a traditional lead smelting and trapping method, and then lead and the platinum group metals are separated by heating to 900-1200 ℃ under the condition that the vacuum degree is 1-600 Pa, so that platinum group metal particles are obtained. The method can reduce the amount of platinum group metal in condensate to below 1 g/t.
With the development of the automobile industry, the number of waste automobile exhaust purifiers is increased day by day, and the waste three-way catalyst has high recycling value, but the existing method has the problems of complex process, harsh production conditions, high energy consumption, high process cost and the like. Therefore, it is necessary to develop a recycling method with simple process conditions, easily accessible conditions and lower cost, which is convenient for industrial application.
Disclosure of Invention
Aiming at the defects and shortcomings of the prior art, the invention aims to provide a method for recovering platinum group metals from waste three-way catalysts, which has the advantages of mild reaction conditions, simple process and suitability for industrial application.
In order to solve the technical problems, the technical scheme provided by the invention is as follows:
a method for recovering platinum group metals from a spent three-way catalyst, comprising the steps of:
(1) adding the waste three-way catalyst, sodium chloride and ferric chloride into a hydrochloric acid solution A, carrying out primary leaching reaction, and carrying out solid-liquid separation to obtain a leaching solution containing palladium and leaching residues containing platinum and rhodium;
(2) and (2) adding the leaching slag containing the platinum and the rhodium obtained in the step (1) and an oxidant into a hydrochloric acid solution B, and performing secondary leaching reaction to obtain a leaching solution containing the platinum and the rhodium.
According to the technical scheme, a two-step leaching method is adopted, palladium is leached under the condition of low acid, and then platinum and rhodium are further leached completely, so that the peroxidation of palladium can be avoided, and the recovery rate of platinum group metals is greatly improved.
In the first leaching process, sodium chloride is used as an additive, ferric chloride is used as an oxidant, and the sodium chloride and a hydrochloric acid solution are used for synergistically leaching the waste three-way catalyst palladium, wherein the leaching rate of the palladium is more than or equal to 99%.
The inventor finds that hydrochloric acid provides an acid environment and also provides chloride ions to be complexed with palladium in the first leaching process, and sodium chloride with low price is added as an additive, so that the hydrochloric acid not only can provide the chloride ions, but also can reduce the reduction potential, so that palladium forms water-soluble coordination complex ions, and the dual effects are realized to improve the leaching rate of the palladium.
In addition, the platinum group metal can be promoted to be dissolved out by adding the oxidant, and the platinum group metal enters the solution in a chlorine coordination form, and in the invention, the inventor surprisingly discovers that FeCl with weaker oxidizing capability than sodium hypochlorite and hydrogen peroxide is adopted3But also can obtain higher leaching efficiency, and because the main component of the three-way catalyst is cordierite which contains iron, and new impurities can not be introduced by using ferric chloride as an oxidant,
in the prior artIn general, NaClO and H are selected2O2As an oxidizing agent, with FeCl3In comparison, the standard redox potentials of the three are respectively 1.630V, 1.776V and 0.771V, which are all higher than the potential of Pd metal. The oxidizing power of the three is strongest, the sodium hypochlorite is second, and the ferric chloride is worst. However, in the experimental process, hydrogen peroxide and sodium hypochlorite are found to cause the palladium to be subjected to peroxidation phenomenon if used as the oxidizing agent for the first leaching of the invention, so that the leaching rate is reduced, and the optimal leaching efficiency can be obtained only by using sodium chloride as an additive and ferric chloride as an oxidizing agent in the synergistic leaching of hydrochloric acid solution.
Preferably, in the step (1), the mass ratio of the sodium chloride to the waste three-way catalyst is 0.2-1: 1, and preferably 0.5-1: 1.
Preferably, in the step (1), the mass ratio of the ferric chloride to the waste three-way catalyst is 0.1-1: 1, and preferably 0.4-0.6: 1.
Preferably, in the step (1), the concentration of the dissolved HCl in the hydrochloric acid solution A is 0.5-5 mol/L, and preferably 1-3 mol/L.
Preferably, in the step (1), the liquid-solid volume mass ratio of the hydrochloric acid solution A to the waste three-way catalyst is 5-10 ml:1 g.
In a preferable scheme, in the step (1), the temperature of the first leaching reaction is less than 100 ℃, and is preferably 80-90 ℃.
Preferably, in the step (1), the time of the first leaching reaction is 0.5-6 hours, and preferably 0.5-1.5 hours.
Preferably, in the step (2), the oxidant is selected from hypochlorous acid or hydrogen peroxide;
preferably, in the step (2), the oxidant is hydrogen peroxide, and the mass ratio of the added amount of the hydrogen peroxide to the liquid-solid volume of the leaching residue containing platinum and rhodium is 0.1-2: 1; preferably 1-1.5: 1.
In a preferable scheme, in the step (2), the temperature of the second leaching reaction is 40-90 ℃; preferably 80 to 85 ℃.
In a preferable scheme, in the step (2), the time of the second leaching reaction is 0.5-4 hours, and preferably 1-3 hours.
Preferably, in the step (2), the concentration of the dissolved HCl in the hydrochloric acid solution B is 5-10 mol/L, and preferably 6-8 mol/L.
Principles and advantages
Aiming at the problems encountered by the waste three-way catalyst in the leaching process, the platinum, the palladium and the rhodium are leached and enriched by a scheme of leaching step by step, in the invention, the waste three-way catalyst does not need to be roasted and pretreated to improve the reduction activity of palladium oxide in order to improve the leaching rate of the palladium in the prior art, the industrial flow is greatly simplified, simultaneously, the leaching rate of the invention is high, and in the preferred scheme, the recovery rates of the platinum, the palladium and the rhodium are respectively as follows: more than 97%, more than 99% and more than 99.5%.
The invention adopts the full wet process under the conditions of normal pressure and less than 100 ℃, has easily obtained raw materials, simple equipment, low hardware requirement, simple operation and low investment cost, and has better industrial popularization prospect.
Detailed Description
In order to facilitate an understanding of the invention, the invention will now be described more fully and in detail with reference to the accompanying description and preferred embodiments, but the scope of the invention is not limited to the specific embodiments described below.
Unless otherwise defined, all terms of art used hereinafter have the same meaning as commonly understood by one of ordinary skill in the art. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to limit the scope of the present invention.
Unless otherwise specifically stated, various raw materials, reagents, instruments, equipment and the like used in the present invention are commercially available or can be prepared by existing methods.
The main components of the waste three-way catalyst in each embodiment and the comparative example of the invention are 245g/t Pt, 1480g/t Pd and 185.2g/t Rh.
Example 1:
10g of raw materials are placed in a reactor, 1mol/L hydrochloric acid leaching agent is added according to the liquid-solid ratio of 10:1, 6g of ferric chloride is added as an oxidizing agent, 10g of sodium chloride is added as an additive, the first leaching is carried out at 90 ℃, the solid-liquid separation is carried out after 1h, leaching solution rich in palladium and leaching residue containing platinum and rhodium are obtained, and the leaching rate of palladium is 99.45%, the leaching rate of platinum is 6.97% and the leaching rate of rhodium is 34.66% after analysis.
Using 6mol/L hydrochloric acid as a leaching agent, leaching for the second time according to the liquid-solid ratio of 10:1, adding 10ml hydrogen peroxide, reacting for 1h at the temperature of 80 ℃, and performing solid-liquid separation after the reaction to obtain a leaching solution rich in platinum and rhodium. Through analysis and calculation, the comprehensive leaching rate of platinum is 97.72%, the comprehensive leaching rate of palladium is 99.53%, and the comprehensive leaching rate of rhodium is 99.63%.
Example 2:
10g of raw materials are placed in a reactor, 2mol/L hydrochloric acid leaching agent is added according to the liquid-solid ratio of 5:1, 10g of ferric chloride is added as an oxidizing agent, 5g of sodium chloride is added as a reducing agent, primary leaching is carried out at 85 ℃, solid-liquid separation is carried out after 1.5h, leaching solution rich in palladium and primary leaching residue containing platinum and rhodium are obtained, and the leaching rate of palladium is 98.92%, the leaching rate of platinum is 6.37% and the leaching rate of rhodium is 34.89% through analysis.
Using 5mol/L hydrochloric acid as a leaching agent, leaching for the second time according to the liquid-solid ratio of 10:1, adding 15ml hydrogen peroxide, reacting for 1h at 85 ℃, and performing solid-liquid separation after the reaction to obtain a leaching solution rich in platinum and rhodium. Through analysis and calculation, the comprehensive leaching rate of platinum is 97.21%, the comprehensive leaching rate of palladium is 99.05%, and the comprehensive leaching rate of rhodium is 99.76%.
Example 3:
10g of raw materials are placed in a reactor, 0.5mol/L hydrochloric acid leaching agent is added according to the liquid-solid ratio of 10:1, 10g of ferric chloride is added as an oxidizing agent, 10g of sodium chloride is added as a reducing agent, the first leaching is carried out at 90 ℃, the solid-liquid separation is carried out after 2.5h, leaching solution rich in palladium and leaching residue containing platinum and rhodium are obtained, and the leaching rate of palladium, the leaching rate of platinum and the leaching rate of rhodium are obtained through analysis and are 98.42%, 5.85% and 30.02%, respectively.
Using 8mol/L hydrochloric acid as a leaching agent, leaching for the second time according to the liquid-solid ratio of 6:1, adding 15ml hydrogen peroxide, reacting for 1h at 85 ℃, and performing solid-liquid separation after the reaction to obtain a leaching solution rich in platinum and rhodium. Through analysis and calculation, the comprehensive leaching rate of platinum is 97.48%, the comprehensive leaching rate of palladium is 98.94%, and the comprehensive leaching rate of rhodium is 99.46%.
Example 4:
10g of raw materials are placed in a reactor, 3mol/L hydrochloric acid leaching agent is added according to the liquid-solid ratio of 10:1, 5g of ferric chloride is added as an oxidizing agent, 2g of sodium chloride is added as a reducing agent, the first leaching is carried out at 90 ℃, the solid-liquid separation is carried out after 2h, leaching solution rich in palladium and leaching residue containing platinum and rhodium are obtained, and the leaching rate of palladium is 99.16%, the leaching rate of platinum is 6.45% and the leaching rate of rhodium is 33.62% through analysis.
Using 10mol/L hydrochloric acid as a leaching agent, leaching for the second time according to the liquid-solid ratio of 5:1, adding 12ml hydrogen peroxide, reacting for 1.5h at 85 ℃, and performing solid-liquid separation after the reaction to obtain a leaching solution rich in platinum and rhodium. Through analysis and calculation, the comprehensive leaching rate of platinum is 98.12%, the comprehensive leaching rate of palladium is 99.36%, and the comprehensive leaching rate of rhodium is 99.56%.
Example 5:
10g of raw materials are placed in a reactor, 3mol/L hydrochloric acid leaching agent is added according to the liquid-solid ratio of 6:1, 5g of ferric chloride is added as an oxidizing agent, 10g of sodium chloride is added as a reducing agent, the first leaching is carried out at 85 ℃, solid-liquid separation is carried out after 2h, leaching solution rich in palladium and leaching residue containing platinum and rhodium are obtained, and the leaching rate of palladium is 99.32%, the leaching rate of platinum is 6.74% and the leaching rate of rhodium is 35.43% through analysis.
Using 7mol/L hydrochloric acid as a leaching agent, leaching for the second time according to the liquid-solid ratio of 6:1, adding 10ml hydrogen peroxide, reacting for 3 hours at 85 ℃, and performing solid-liquid separation after the reaction is finished to obtain a leaching solution rich in platinum and rhodium. Through analysis and calculation, the comprehensive leaching rate of platinum is 96.88%, the comprehensive leaching rate of palladium is 99.44%, and the comprehensive leaching rate of rhodium is 98.17%.
Comparative example 1:
other conditions of this comparative example were the same as those of example 1 except that hydrogen peroxide was used as an oxidizing agent in step 1. Analysis shows that the leaching rate of palladium in the leaching solution in the step 1 is 88.45 percent.
Comparative example 2:
the other conditions of this comparative example were the same as example 1 except that no sodium chloride was added as an additive in step 1. Analysis shows that the leaching rate of palladium in the leaching solution in the step 1 is 84.45 percent.
Comparative example 3:
the other conditions of this comparative example were the same as example 1 except that 5g of sodium chloride was added as an additive in step 1. Analysis shows that the leaching rate of palladium in the leaching solution in the step 1 is 92.15%.
Comparative example 4:
the other conditions of this comparative example were the same as in example 1 except that ferric chloride was added as an oxidizing agent in step 2. Through analysis, the comprehensive leaching rate of platinum is 6.79 percent, and the leaching rate of rhodium is 45.42 percent.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A method for recovering platinum group metals from waste three-way catalysts is characterized by comprising the following steps:
(1) adding the waste three-way catalyst, sodium chloride and ferric chloride into a hydrochloric acid solution A, carrying out primary leaching reaction, and carrying out solid-liquid separation to obtain a leaching solution mainly containing palladium and leaching residues mainly containing platinum and rhodium;
(2) and (2) adding the leaching slag containing the platinum and the rhodium obtained in the step (1) and an oxidant into a hydrochloric acid solution B, and performing secondary leaching reaction to obtain a leaching solution containing the platinum and the rhodium.
2. The method for recovering platinum group metals from waste three-way catalysts according to claim 1, wherein in the step (1), the mass ratio of sodium chloride to the waste three-way catalysts is 0.2-1: 1.
3. The method for recovering platinum group metals from waste three-way catalysts according to claim 1, wherein in the step (1), the mass ratio of ferric chloride to the waste three-way catalysts is 0.1-1: 1.
4. The method for recovering platinum group metals from waste three-way catalysts according to claim 1, wherein in the step (1), the concentration of HCl dissolved in the hydrochloric acid solution A is 0.5-5 mol/L.
In the step (1), the liquid-solid volume mass ratio of the hydrochloric acid solution A to the waste three-way catalyst is 5-10 mL:1 g.
5. The method for recovering platinum group metals from waste three-way catalysts according to claim 1, wherein the temperature of the first leaching reaction in step (1) is less than 100 ℃.
6. The method for recovering platinum group metals from waste three-way catalysts according to claim 1, wherein the time of the first leaching reaction in step (1) is 0.5-6 h.
7. The method for recovering platinum group metals from waste three-way catalysts according to claim 1, characterized in that:
in the step (2), the oxidant is selected from hypochlorous acid or hydrogen peroxide.
8. The method for recovering platinum group metals from the waste three-way catalyst according to claim 7, wherein in the step (2), the oxidant is hydrogen peroxide, and the liquid-solid volume mass ratio of the added amount of hydrogen peroxide to the leaching residue containing platinum and rhodium is 0.1-2 mL:1 g.
9. The method for recovering platinum group metals from waste three-way catalysts according to claim 1, characterized in that:
in the step (2), the temperature of the second leaching reaction is 40-90 ℃;
in the step (2), the time of the second leaching reaction is 0.5-4 h.
10. The method for recovering platinum group metals from waste three-way catalysts according to claim 1, characterized in that:
in the step (2), the concentration of HCl dissolved in the hydrochloric acid solution B is 5-10 mol/L.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114737058A (en) * | 2022-03-22 | 2022-07-12 | 徐州浩通新材料科技股份有限公司 | Method for separating platinum, palladium, rhodium and iridium from solution |
| CN115717198A (en) * | 2022-11-18 | 2023-02-28 | 大连理工大学 | Method for leaching platinum group metals from waste catalyst by using ultraviolet visible light |
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Application publication date: 20210305 |