CN112226621B - Method for recovering noble metal from deactivated noble metal catalyst - Google Patents
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- 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 relates to a method for recovering noble metal from a deactivated noble metal catalyst, which comprises the following steps: dissolving the deactivated noble metal catalyst in a nonpolar solvent to obtain a first solution; adding an oxidant into the first solution to adjust the first solution into an alkaline solution, and fully reacting to obtain a second solution; and adding an aqueous solution of a reducing agent into the second solution, fully reacting, separating liquid, retaining an aqueous phase, and evaporating and crystallizing the aqueous phase to obtain the noble metal. The method for recovering the noble metal from the inactivated noble metal catalyst has simple process, does not need incineration treatment, and avoids organic complex sublimation of the noble metal caused by incineration in the traditional recovery method, thereby improving the recovery rate of the noble metal.
Description
Technical Field
The invention relates to the technical field of waste resource noble metal extraction, in particular to a method for recovering noble metals from an inactivated noble metal catalyst.
Background
With the advancement of science and technology and the increasing improvement of environmental regulations, noble metals have been used not only for the manufacture of ornaments and for their economic and financial purposes, but also in industrial processes. Noble metals can accept many different types of complexes to form special spatial structures, and thus have been widely used in the field of catalysts used in petrochemical processes.
The noble metals such as palladium, platinum and the like have important irreplaceable functions in various fields due to the special electrochemical performance and excellent catalytic performance. However, our country's precious metal resources are scarce and expensive, and the domestic demand is increasing year by year. Meanwhile, a large amount of waste containing precious metals is produced in our country every year. Therefore, the method has great significance for recycling the secondary resource of the precious metal.
The homogeneous noble metal catalyst is in phase with the product during use, the product is usually distilled off by distillation, and the remaining part forms tar-like substances with increasing number of distillations, i.e. deactivated noble metal catalyst. The traditional method for recovering noble metals from deactivated noble metal catalysts is as follows: the recovery is carried out by using an incineration method. However, the organic complex of the noble metal may be sublimated during incineration, resulting in a low recovery rate of the noble metal.
Disclosure of Invention
In view of this, it is necessary to provide a method for recovering a noble metal from a deactivated noble metal catalyst, in order to solve the problem of how to improve the recovery rate of the noble metal.
A process for recovering noble metals from a deactivated noble metal catalyst comprising the steps of:
dissolving the deactivated noble metal catalyst in a nonpolar solvent to obtain a first solution;
adding an oxidant into the first solution to adjust the first solution into an alkaline solution, and obtaining a second solution after full reaction; and
and adding an aqueous solution of a reducing agent into the second solution, fully reacting, separating liquid, retaining an aqueous phase, and evaporating and crystallizing the aqueous phase to obtain the noble metal.
The method for recovering the noble metal from the inactivated noble metal catalyst has simple process, does not need incineration treatment, and avoids organic complex sublimation of the noble metal caused by incineration in the traditional recovery method, thereby improving the recovery rate of the noble metal.
In one embodiment, the non-polar solvent is selected from at least one of an aromatic solvent, an aliphatic hydrocarbon solvent, and a halogenated aliphatic hydrocarbon solvent.
In one embodiment, the content of the noble metal in the deactivated noble metal catalyst in the first solution is 1g/L to 100 g/L.
In one embodiment, the oxidizing agent is selected from at least one of hypochlorite, chlorite, and ozone.
In one embodiment, the pH value of the alkaline solution is 7-10 and is not 7.
In one embodiment, the second solution is obtained after the reaction is carried out fully, the reaction temperature is maintained at 20-80 ℃ and the reaction time is maintained at 2-24 h.
In one embodiment, the reducing agent is selected from at least one of an alcohol reducing agent, an aldehyde reducing agent, and a fatty acid reducing agent.
In one embodiment, the reducing agent is ethanol.
In one embodiment, the reaction time is maintained between 0.5h and 48h in the operation of separating and retaining the aqueous phase after the full reaction.
In one embodiment, the method further comprises the following steps:
and (3) after the aqueous phase is evaporated and crystallized, adding sulfuric acid or hydrochloric acid, and fully reacting to obtain the sulfate of the noble metal or the hydrochloride of the noble metal.
Detailed Description
The present invention will be described in detail with reference to the following embodiments in order to make the aforementioned objects, features and advantages of the invention more comprehensible. In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
An embodiment of a method for recovering noble metals from a deactivated noble metal catalyst comprises the steps of:
s10, dissolving the deactivated noble metal catalyst in a nonpolar solvent to obtain a first solution.
The deactivated noble metal catalyst is waste liquid produced after the homogeneous noble metal catalyst is used, and the waste liquid is tar containing noble metal formed after distillation products are used for many times. For example, tetrakis (triphenylphosphine) palladium (0) catalyst tar, bis (dibenzylideneacetone) palladium (0) catalyst tar, trimethyl (methylcyclopentadienyl) platinum (IV) catalyst tar, [1,1' -bis (diphenylphosphino) ferrocene ] platinum (II) chloride catalyst tar, diiodo (p-cymene) ruthenium (II) dimer catalyst tar, chloro (pentamethylcyclopentadienyl) (cyclooctadiene) ruthenium (II) catalyst tar, tris (2-phenylpyridine) iridium (II) catalyst tar, methoxy (cyclooctadiene) iridium (II) dimer catalyst tar, rhodium hydroformylation catalyst tar, rhodium octanoate catalyst tar, or the like may be mentioned.
The noble metal in the deactivated noble metal catalyst may be platinum, palladium, ruthenium, rhodium, iridium, gold, or osmium.
In one embodiment, the non-polar solvent is selected from at least one of an aromatic solvent, an aliphatic hydrocarbon solvent, and a halogenated aliphatic hydrocarbon solvent. These kinds of nonpolar solvents can sufficiently dissolve the above deactivated noble metal catalyst. Preferably, the non-polar solvent is dichloromethane.
In one embodiment, the content of the noble metal in the deactivated noble metal catalyst in the first solution is 1g/L to 100 g/L. Is beneficial to the subsequent reaction.
Preferably, the content of the noble metal in the deactivated noble metal catalyst in the first solution is 10g/L to 20 g/L.
And S20, adding an oxidizing agent into the first solution to adjust the first solution into an alkaline solution, and fully reacting to obtain a second solution.
On one hand, the oxidizing agent can adjust the pH value of the solution and adjust the solution into an alkaline solution; on the other hand, it is also possible to provide an oxidizing atmosphere, which acts to oxidize the noble metal in the deactivated noble metal catalyst.
In one embodiment, the oxidizing agent is selected from at least one of chlorate, hypochlorite, chlorite, and ozone. These oxidizing agents are used in combination with the reducing agent in step S30, and can form a stable dynamic oxidation and reduction process in the solution, which is advantageous for the recovery of precious metals.
Preferably, the oxidizing agent is selected from at least one of sodium chlorate, sodium hypochlorite and sodium chlorite.
In one embodiment, the pH value of the alkaline solution is 7-10 and is not 7. The alkaline solution can stabilize the oxidant, and is beneficial to the oxidation reaction of the oxidant on the noble metal.
In one embodiment, the second solution is obtained after the reaction is carried out fully, the reaction temperature is maintained at 20-80 ℃ and the reaction time is maintained at 2-24 h. In this case, the oxidizing agent can be sufficiently reacted with the deactivated noble metal catalyst. In order to sufficiently progress the reaction, a method of continuously stirring during the reaction may be employed.
And S30, adding an aqueous solution of a reducing agent into the second solution, fully reacting, separating liquid, retaining an aqueous phase, and evaporating and crystallizing the aqueous phase to obtain the noble metal.
Wherein the reducing agent is used for reducing the noble metal obtained in step S20, and can be combined with the oxidizing agent to form a stable dynamic oxidation and reduction process in the solution. The reducing agent may be mixed with water in any proportion.
After full reaction, the noble metal ions are separated from the organic matters in the deactivated noble metal catalyst, and the noble metal ions enter the water phase to achieve the purpose of liquid separation.
In one embodiment, the reducing agent is selected from at least one of an alcohol reducing agent, an aldehyde reducing agent, and a fatty acid reducing agent. These types of reducing agents are used in combination with the oxidizing agent in step S20, and can form a stable dynamic oxidation and reduction process in the solution, which is advantageous for the recovery of precious metals.
In one embodiment, the reducing agent is ethanol. The carbon atoms of the ethanol are two, so that the reducibility is strong, and the efficiency of the reduction reaction is improved.
In one embodiment, the reaction time is maintained between 0.5h and 48h in the operation of separating and retaining the aqueous phase after the full reaction. In order to sufficiently progress the reaction, a method of continuously stirring during the reaction may be employed.
In one embodiment, the method further comprises the following steps:
and (3) after the water phase is evaporated and crystallized, adding sulfuric acid or hydrochloric acid, and fully reacting to obtain the sulfate of the noble metal or the hydrochloride of the noble metal. Thus, the catalyst can be directly used for preparing the catalyst.
The method for recovering the noble metal from the inactivated noble metal catalyst has simple process, does not need incineration treatment, and avoids organic complex sublimation of the noble metal caused by incineration in the traditional recovery method, thereby improving the recovery rate of the noble metal.
In order to make the technical solutions of the present application more specific, clear and easy to understand by referring to the above implementation contents, the technical solutions of the present application are exemplified, but it should be noted that the contents to be protected by the present application are not limited to the following examples 1 to 14.
Example 1
10 liters of tetrakis (triphenylphosphine) palladium (0) catalyst tar having a palladium content of 10 wt% was dissolved in methylene chloride to obtain a first solution. The content of palladium in the first solution was 10 g/L.
To the first solution was added 7.8kg of sodium hypochlorite, and the reaction temperature was maintained at 70 ℃ and stirred for 10 hours to obtain a second solution.
To the second solution was added 10L of an aqueous ethanol solution (mass fraction of ethanol: 1%), liquid was separated and the aqueous phase was retained after stirring for 2 hours, and the aqueous phase was subjected to evaporation crystallization, followed by addition of 20L of concentrated sulfuric acid (mass fraction of sulfuric acid: 98%) to give 2462 g of palladium sulfate with a recovery rate of 98%.
Example 2
10 liters of catalyst tar of bis (dibenzylideneacetone) palladium (0) having a palladium content of 10 wt% was dissolved in methylene chloride to obtain a first solution. The content of palladium in the first solution was 10 g/L.
To the first solution was added 8kg of sodium hypochlorite, and the reaction temperature was maintained at 80 ℃ and stirred for 2 hours to obtain a second solution.
10L of ethanol aqueous solution (the mass fraction of ethanol is 1%) is added into the second solution, liquid separation is carried out after 2 hours of stirring, the water phase is kept, evaporation crystallization is carried out on the water phase, 20L of concentrated sulfuric acid (the mass fraction of sulfuric acid is 98%) is added, 2448 g of palladium sulfate is obtained, and the recovery rate is 97%.
Example 3
10 liters of trimethyl (methylcyclopentadienyl) platinum (IV) catalyst tar having a platinum content of 10 wt% was dissolved by adding methylene chloride to obtain a first solution. The content of platinum in the first solution was 10 g/L.
To the first solution was added 7.8kg of sodium hypochlorite, and the reaction temperature was maintained at 70 ℃ and stirred for 10 hours to obtain a second solution.
To the second solution was added 10L of an aqueous ethanol solution (mass fraction of ethanol: 1%), liquid was separated and the aqueous phase was retained after stirring for 2 hours, and the aqueous phase was subjected to evaporation crystallization, followed by addition of 20L of concentrated sulfuric acid (mass fraction of sulfuric acid: 98%) to obtain 1861 g of platinum sulfate with a recovery rate of 98%.
Example 4
10 liters of [1,1' -bis (diphenylphosphino) ferrocene ] platinum (II) chloride catalyst tar having a platinum content of 10 wt% was dissolved in methylene chloride to obtain a first solution. The content of platinum in the first solution was 10 g/L.
To the first solution was added 8kg of sodium hypochlorite, the reaction temperature was maintained at 80 ℃ and stirred for 2 hours to obtain a second solution.
To the second solution was added 10L of an aqueous ethanol solution (mass fraction of ethanol: 1%), liquid was separated and the aqueous phase was retained after stirring for 2 hours, and the aqueous phase was subjected to evaporative crystallization, followed by addition of 20L of concentrated sulfuric acid (mass fraction of sulfuric acid: 98%) to obtain 1848 g of platinum sulfate with a recovery rate of 97%.
Example 5
10 liters of diiodo (p-cymene) ruthenium (II) dimer catalyst tar having a ruthenium content of 10 wt% was dissolved in methylene chloride to obtain a first solution. The ruthenium content in the first solution was 10 g/L.
To the first solution was added 7.8kg of sodium hypochlorite, and the reaction temperature was maintained at 70 ℃ and stirred for 10 hours to obtain a second solution.
10L of ethanol aqueous solution (the mass fraction of ethanol is 1%) was added to the second solution, the mixture was stirred for 2 hours, then liquid separation was carried out and the aqueous phase was retained, and evaporation crystallization was carried out on the aqueous phase, followed by addition of 20L of concentrated sulfuric acid (the mass fraction of sulfuric acid is 98%) to obtain 2391 g of ruthenium sulfate, the recovery rate of which was 98%.
Example 6
10 liters of chloro (pentamethylcyclopentadienyl) (cyclooctadiene) ruthenium (II) catalyst tar having a ruthenium content of 10 wt% was dissolved by adding methylene chloride to obtain a first solution. The ruthenium content in the first solution was 10 g/L.
To the first solution was added 8kg of sodium hypochlorite, and the reaction temperature was maintained at 80 ℃ and stirred for 2 hours to obtain a second solution.
To the second solution was added 10L of an aqueous ethanol solution (mass fraction of ethanol: 1%), and after stirring for 2 hours, liquid separation was performed while retaining the aqueous phase, and the aqueous phase was subjected to evaporative crystallization, followed by addition of 20L of concentrated sulfuric acid (mass fraction of sulfuric acid: 98%) to obtain 2347 g of ruthenium sulfate with a recovery rate of 97%.
Example 7
10 liters of tris (2-phenylpyridine) iridium catalyst tar having an iridium content of 10 wt% was dissolved in methylene chloride to obtain a first solution. The iridium content in the first solution was 10 g/L.
To the first solution was added 7.8kg of sodium hypochlorite, and the reaction temperature was maintained at 70 ℃ and stirred for 10 hours to obtain a second solution.
To the second solution was added 10L of an aqueous ethanol solution (mass fraction of ethanol: 1%), liquid was separated and the aqueous phase was retained after stirring for 2 hours, and the aqueous phase was subjected to evaporative crystallization, followed by addition of 20L of concentrated sulfuric acid (mass fraction of sulfuric acid: 98%) to obtain 2492 g of iridium sulfate with a recovery rate of 98%.
Example 8
10 liters of methoxy (cyclooctadiene) iridium dimer catalyst tar having an iridium content of 10 wt% was dissolved by adding methylene chloride to obtain a first solution. The iridium content in the first solution was 10 g/L.
To the first solution was added 8kg of sodium hypochlorite, and the reaction temperature was maintained at 80 ℃ and stirred for 2 hours to obtain a second solution.
To the second solution was added 10L of an aqueous ethanol solution (mass fraction of ethanol: 1%), liquid was separated and the aqueous phase was retained after stirring for 2 hours, and the aqueous phase was subjected to evaporative crystallization, followed by addition of 20L of concentrated sulfuric acid (mass fraction of sulfuric acid: 98%) to give 2271 g of iridium sulfate with a recovery rate of 97%.
Example 9
10 liters of rhodium hydroformylation catalyst tar having a rhodium content of 10 wt% was dissolved in methylene chloride to obtain a first solution. The content of rhodium in the first solution was 10 g/L.
To the first solution was added 7.8kg of sodium hypochlorite, and the reaction temperature was maintained at 70 ℃ and stirred for 10 hours to obtain a second solution.
10L of ethanol aqueous solution (the mass fraction of ethanol is 1%) is added into the second solution, liquid separation is carried out after 2 hours of stirring, the water phase is kept, evaporation crystallization is carried out on the water phase, 20L of concentrated sulfuric acid (the mass fraction of sulfuric acid is 98%) is added, 2261 g of rhodium sulfate is obtained, and the recovery rate is 98%.
Example 10
10 liters of rhodium octanoate catalyst tar having a rhodium content of 10 wt% was dissolved in methylene chloride to obtain a first solution. The content of rhodium in the first solution was 10 g/L.
To the first solution was added 8kg of sodium hypochlorite, and the reaction temperature was maintained at 80 ℃ and stirred for 2 hours to obtain a second solution.
10L of ethanol aqueous solution (the mass fraction of ethanol is 1%) is added into the second solution, liquid separation is carried out after 2 hours of stirring, the water phase is kept, evaporation crystallization is carried out on the water phase, and then 20L of concentrated sulfuric acid (the mass fraction of sulfuric acid is 98%) is added, so that 2248 g of rhodium sulfate is obtained, and the recovery rate is 97%.
All possible combinations of the technical features of the above embodiments may not be described for the sake of brevity, but should be considered as within the scope of the present disclosure as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (9)
1. A method for recovering a noble metal from a deactivated noble metal catalyst, comprising the steps of:
dissolving the deactivated noble metal catalyst in a nonpolar solvent to obtain a first solution, wherein the nonpolar solvent is selected from at least one of an aromatic solvent, an aliphatic hydrocarbon solvent and a halogenated aliphatic hydrocarbon solvent;
adding an oxidant into the first solution to adjust the first solution into an alkaline solution, and obtaining a second solution after sufficient reaction, wherein the oxidant is selected from at least one of chlorate, hypochlorite, chlorite and ozone; and
and adding an aqueous solution of a reducing agent into the second solution, fully reacting, separating liquid, retaining an aqueous phase, and evaporating and crystallizing the aqueous phase to obtain the noble metal, wherein the reducing agent is at least one selected from an alcohol reducing agent, an aldehyde reducing agent and a fatty acid reducing agent.
2. The method of recovering a noble metal from a deactivated noble metal catalyst of claim 1, wherein the noble metal in the deactivated noble metal catalyst is platinum, palladium, ruthenium, rhodium, iridium, gold, or osmium.
3. The method of claim 1, wherein the first solution contains from 1g/L to 100g/L of the noble metal in the deactivated noble metal catalyst.
4. The method of claim 1 wherein the oxidizing agent is selected from at least one of sodium chlorate, sodium hypochlorite and sodium chlorite.
5. The method for recovering noble metal from a deactivated noble metal catalyst according to claim 1, wherein the pH of the alkaline solution is 7 to 10 and is not 7.
6. The method for recovering noble metal from deactivated noble metal catalyst according to claim 1, wherein the reaction temperature is maintained at 20 to 80 ℃ and the reaction time is maintained at 2 to 24 hours in the operation of obtaining the second solution after the sufficient reaction.
7. The method of recovering a noble metal from a deactivated noble metal catalyst of claim 1, wherein the reducing agent is ethanol.
8. The method for recovering noble metal from a deactivated noble metal catalyst according to claim 1, wherein the reaction time is maintained for 0.5 to 48 hours in the operation of separating and retaining the aqueous phase after the sufficient reaction.
9. The method of recovering a noble metal from a deactivated noble metal catalyst of claim 1, further comprising the steps of:
and (3) after the aqueous phase is evaporated and crystallized, adding sulfuric acid or hydrochloric acid, and fully reacting to obtain the sulfate of the noble metal or the hydrochloride of the noble metal.
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