CN115700286A - Waste Pd/Al 2 O 3 Method for recovering Pd in catalyst - Google Patents
Waste Pd/Al 2 O 3 Method for recovering Pd in catalyst Download PDFInfo
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- CN115700286A CN115700286A CN202110831564.XA CN202110831564A CN115700286A CN 115700286 A CN115700286 A CN 115700286A CN 202110831564 A CN202110831564 A CN 202110831564A CN 115700286 A CN115700286 A CN 115700286A
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- 238000000034 method Methods 0.000 title claims abstract description 41
- 239000003054 catalyst Substances 0.000 title claims abstract description 35
- 239000002699 waste material Substances 0.000 title claims abstract description 26
- 229910018072 Al 2 O 3 Inorganic materials 0.000 title claims abstract description 19
- KDLHZDBZIXYQEI-UHFFFAOYSA-N palladium Substances [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims abstract description 105
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 60
- 239000000843 powder Substances 0.000 claims abstract description 31
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 28
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 28
- 239000000460 chlorine Substances 0.000 claims abstract description 21
- 239000000706 filtrate Substances 0.000 claims abstract description 15
- 238000001914 filtration Methods 0.000 claims abstract description 13
- 239000001257 hydrogen Substances 0.000 claims abstract description 12
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 12
- 238000010438 heat treatment Methods 0.000 claims abstract description 10
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229910052801 chlorine Inorganic materials 0.000 claims abstract description 9
- 238000002386 leaching Methods 0.000 claims abstract description 9
- 229910052763 palladium Inorganic materials 0.000 claims abstract description 7
- 239000007788 liquid Substances 0.000 claims description 10
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 9
- 238000001354 calcination Methods 0.000 claims description 7
- 239000007787 solid Substances 0.000 claims description 7
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 5
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 5
- 230000035484 reaction time Effects 0.000 claims description 5
- 150000002431 hydrogen Chemical class 0.000 claims description 2
- 238000011084 recovery Methods 0.000 abstract description 11
- 238000007670 refining Methods 0.000 abstract description 4
- 125000004435 hydrogen atom Chemical class [H]* 0.000 abstract 1
- 238000006243 chemical reaction Methods 0.000 description 10
- 239000000463 material Substances 0.000 description 6
- 238000001816 cooling Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000007873 sieving Methods 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- IKHGUXGNUITLKF-UHFFFAOYSA-N Acetaldehyde Chemical compound CC=O IKHGUXGNUITLKF-UHFFFAOYSA-N 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 229910000510 noble metal Inorganic materials 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- 238000010298 pulverizing process Methods 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 1
- 239000005977 Ethylene Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000004517 catalytic hydrocracking Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000009858 dingxin Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
The invention provides a method for preparing waste Pd/Al 2 O 3 A process for the recovery of Pd from a catalyst, the process comprising: 1) Waste Pd/Al 2 O 3 Reducing the catalyst with hydrogen, adding hydrochloric acid and nitric acid, heating to dissolve, leaching, and taking filtrate; 2) And (2) filtering the filtrate obtained in the step 1) in a chlorine atmosphere, and adding Fe powder to prepare coarse Pd powder. The method finally recovers 99.95 percent of sponge palladium by leaching hydrochloric acid and nitric acid, filtering chlorine, controlling acidity, increasing temperature, prolonging time and controlling replacement conditions. The sponge Pd prepared by the method does not need to be repeatedly purified, the purity can reach 99.95 percent by one step, and the purity can reach 99.99 percent by refining and purifying once.
Description
Technical Field
The invention belongs to the technical field of catalyst recovery, and particularly relates to waste Pd/Al 2 O 3 A method for recovering Pd in the catalyst.
Background
In the petrochemical industry, pd catalysts are used for the oxidation of ethylene to produce acetaldehyde. Pd/Al for hydrocracking in petrochemical refinery 2 O 3 The catalyst has better economic effect. The development of Pd catalysts is still vigorous for many years, new varieties are continuously developed, and the Pd catalysts continuously play a remarkable role in new application fields.
However, the Pd catalyst is deteriorated in catalytic activity after long-term use, so that it loses activity and becomes a spent catalyst. However, the palladium content in the palladium/alumina catalyst is high, and the catalyst has important recovery value. Currently, there is still a lack of more efficient methods for recovering Pd.
Disclosure of Invention
In order to improve the technical problem, the invention provides the waste Pd/Al 2 O 3 A process for the recovery of Pd from a catalyst, the process comprising:
1) Waste Pd/Al 2 O 3 Reducing the catalyst by hydrogen, adding hydrochloric acid and nitric acid, heating for dissolving, leaching, and taking filtrate;
2) And (2) filtering the filtrate obtained in the step 1) in a chlorine atmosphere, and adding Fe powder to prepare coarse Pd powder.
According to the invention, the method further comprises the steps of:
3) And (3) post-treatment: dissolving the crude Pd powder obtained in the step 2) by adopting hydrochloric acid and nitric acid, and purifying by adopting a dichlorodiamine palladium complex method to obtain refined Pd powder.
According to the invention, the method further comprises the steps of:
4) Leaching the filter residue obtained in the leaching step in the step 1) at least once (namely dissolving the filter residue by adopting hydrochloric acid and nitric acid solution), and recovering the solid to obtain Al 2 O 3 。
According to the invention, the method further comprises the steps of:
5) Concentrating the waste liquid obtained after the solid is recovered in the step 4), namely FeCl 3 。
According to the invention, in step 1), the waste Pd/Al 2 O 3 The catalyst is calcined at 600-700 ℃ and then reduced by hydrogen.
According to the invention, in step 1), the time for hydrogen reduction is 1 to 4 hours, preferably 2 hours.
According to the invention, in step 1), the scrap Pd/Al 2 O 3 The Pd content in the catalyst is 0.18wt% -0.35 wt%.
According to the invention, in step 1), the concentration of the hydrochloric acid is 2 to 4M, preferably 3M.
According to the present invention, the heating temperature in step 1) is 85 to 100 ℃, for example, 85 ℃, 90 ℃, 95 ℃, 100 ℃.
According to the invention, in the step 1), the heating reaction time is 30-160 min, for example, 30min, 40min, 50min, 60min, 70min, 80min, 100min, 120min, 140min and 160min.
According to the present invention, in step 2), the filtered filtrate is combined with the filtrate in step 1) in order to improve the recovery efficiency.
According to the invention, in step 2), fe powder and waste Pd/Al are mixed 2 O 3 The mass ratio of the Pd content in the catalyst is 4-6, preferably 5.
According to the invention, in the step 3), the obtained refined Pd powder is sponge palladium powder.
The dichlorodiamine palladium-supported method in step 3) of the invention is a known method, and can be specifically referred to "precious metal extraction and refining", published by south China university of industry, li Dingxin Main ed, changsha, 1991.
According to the invention, step 3) comprises in particular: dissolving the crude Pd powder in the step 2) by using hydrochloric acid and nitric acid, adding ammonia water, and filtering to obtain Pd (NH) 3 ) 4 Cl 2 Adding hydrochloric acid into the solution to generate Pd (NH) 3 ) 2 Cl 2 And after calcination, introducing hydrogen for reduction to obtain sponge palladium powder.
Advantageous effects
1. In the method for recovering Pd, hydrochloric acid, nitric acid and chlorine (Cl) are adopted 2 ) The Pd is leached, the recovery period is short, the recovery rate is high, and the environmental pollution can be reduced.
2. In the method for recovering Pd, the material consumption is low, and the recovery rate is improved by 3-5 percent compared with the conventional treatment method.
3. The invention is leached by hydrochloric acid and nitric acid, and chlorine (Cl) 2 ) Filtering, controlling acidity (for example, using hydrochloric acid of 3MOL 10%), raising temperature, prolonging time, controlling replacement conditions, and finally recovering sponge palladium with purity of at least 99.95%.
4. The sponge Pd prepared by the method does not need to be purified repeatedly, the purity can reach 99.95 percent only by one step, and the purity can reach 99.99 percent if the sponge Pd is refined and purified once again.
5. The waste residue of the invention can be used as crude Al 2 O 3 And the wastewater can reach the discharge standard, so that the environmental pollution is reduced.
Drawings
FIG. 1 is a process flow diagram for Pd recovery in example 1.
FIG. 2 is a process flow diagram for Pd recovery in example 2.
Detailed Description
The technical solution of the present invention will be further described in detail with reference to specific embodiments. It is to be understood that the following examples are only illustrative and explanatory of the present invention and should not be construed as limiting the scope of the present invention. All the technologies realized based on the above-mentioned contents of the present invention are covered in the protection scope of the present invention.
Unless otherwise indicated, the raw materials and reagents used in the following examples are all commercially available products or can be prepared by known methods.
Examples Pd/Al 2 O 3 The spent catalyst originated from petrochemical refinery, was unloaded from the apparatus and sampled for analysis of Pd content of 0.25%.
Example 1
1. 50kg of waste Pd/Al is weighed 2 O 3 Calcining the catalyst (wherein Pd content is 125 g) in a calcining furnace at 650 deg.C, introducing H 2 Reducing for 2h, cooling, sieving with a 80-mesh sieve, transferring the materials into a 500L reaction kettle, and solidifying: liquid =1, 4, 18% hydrochloric acid was added.
2. Starting stirring, heating to 80 ℃, slowly dropwise adding a prepared 30% nitric acid solution (60 drops per minute), stopping adding the nitric acid when the reaction temperature is raised to 95 ℃ for 2 hours, wherein the reaction is violent at the moment, and the reaction time in the process is 40 minutes, namely, adding the nitric acid and reacting at the same time. After the reaction is stopped, leaching, and taking filtrate;
3. after the filtrate obtained in the step 2 was filtered for about 40min in a chlorine atmosphere, 625g of fe powder was added to prepare a crude Pd powder (purity about 99.95%).
4. Oxidizing and dissolving the crude Pd powder in the step 3 by adopting 50L of 18% hydrochloric acid and 20L of 30% nitric acid, dissolving the solution by adopting 7.5L of ammonia water, and filtering to obtain Pd (NH) 3 ) 4 Cl 2 Then 10L 18% hydrochloric acid was added to the solution to produce Pd (NH) 3 ) 2 Cl 2 And after calcining at 650 ℃, introducing hydrogen to reduce for 2 hours to obtain spongy palladium powder.
5. And (2) dissolving the filter residue filtered in the step 1 in a hydrochloric acid and nitric acid solution (the volume ratio of the hydrochloric acid to the nitric acid is 5) 2 O 3 。
6. Concentrating the waste liquid obtained after the solid is recovered in the step 5 to obtain FeCl 3 。
Example 2
Example 2 differs from example 1 in that: in step 1, the waste Pd/Al 2 O 3 The mass of the catalyst (wherein the Pd content was 200 g) was 80kg. In step 3, the amount of Fe powder added was 1000g.
Example 3
Pd/Al 2 O 3 Method for recovering waste catalyst
1. Weighing 50kg of waste catalyst (wherein the Pd content is 125 g), sieving with a 80-mesh sieve, and passing through H 2 Reducing for 2h, collecting materials, feeding the materials into a 500L reaction kettle, and solidifying: liquid =1:4, 18% hydrochloric acid is added.
2. Starting stirring, heating to 80 ℃, slowly adding 30% nitric acid (60 drops per minute, 5ml per drop, 12L drop) dropwise, stopping adding the nitric acid when the temperature is raised to 95 ℃, and stopping adding the nitric acid for 2h, wherein the reaction is violent at the moment, and the reaction time is about 40 minutes;
3. after the reaction is finished, keeping the temperature for 2 hours, cooling, filtering and taking filtrate; after filtering the filtrate for 40min in a chlorine atmosphere, 625g of Fe powder is added for replacement, and crude Pd powder (the purity is about 99.95%) is produced.
4. Refining the crude Pd powder, oxidizing and dissolving the crude Pd powder by 50L 18% hydrochloric acid and 20L 30% nitric acid, dissolving the crude Pd powder by 7.5L ammonia water, and filtering to obtain Pd (NH) 3 ) 4 Cl 2 Then, 10L 18% hydrochloric acid was added to the solution to produce Pd (NH) 3 ) 2 Cl 2 And after calcining at 650 ℃, introducing hydrogen to reduce for 2 hours to obtain spongy palladium powder.
5. And (3) dissolving the filter residue filtered in the step 1 in a hydrochloric acid and nitric acid solution (the volume ratio of the hydrochloric acid to the nitric acid is 5) 2 O 3 And (3) pulverizing.
6. Concentrating the waste liquid obtained after the solid is recovered in the step 5, detecting that the content of noble metal in the mother liquid after replacement is less than 0.0005%, and concentrating to obtain FeCl 3 。
Example 4
Pd/Al 2 O 3 Method for recovering waste catalyst
1. Weighing 80kg of waste catalyst (wherein the Pd content is 200 g), crushing, sieving with 80-mesh sieve, and introducing H 2 Reducing for 2h, collecting materials, feeding the materials into a 500L reaction kettle, and solidifying: liquid =1:4, 18% hydrochloric acid is added.
2. Starting stirring, heating to 80 ℃, slowly adding 30% nitric acid (60 drops per minute) dropwise, stopping adding the nitric acid when the temperature is heated to 95 ℃, wherein the adding amount is about 30L, the reaction is violent at the moment, and the reaction time is about 6h;
3. after the reaction is finished, keeping the temperature for 2 hours, cooling, filtering and taking filtrate; after the filtrate was filtered for 40min in a chlorine atmosphere, 1000g of Fe powder was added to the produced filtrate for substitution, yielding crude Pd powder (purity about 99.95%).
4. Refining the crude Pd powder, dissolving the crude Pd powder in 50L of 18% hydrochloric acid and 20L of 30% nitric acid by oxidation, dissolving with 7.5L of ammonia water, and filtering to obtain Pd (NH) 3 ) 4 Cl 2 Then 10L 18% hydrochloric acid was added to the solution to produce Pd (NH) 3 ) 2 Cl 2 And after calcining at 650 ℃, introducing hydrogen to reduce for 2 hours to obtain spongy palladium powder.
5. Dissolving the waste residue filtered in the step 1 in a hydrochloric acid and nitric acid solution (the volume ratio of the hydrochloric acid to the nitric acid is 5 2 O 3 And (3) pulverizing. Al (aluminum) 2 O 3 The Pd content in the powder is less than 0.0005 percent.
6. Concentrating the waste liquid obtained after the solid is recovered in the step 5, detecting that the content of noble metal in the mother liquid after replacement is less than 0.0005%, and concentrating to obtain FeCl 3 。
Table 1 shows the waste Pd/Al in examples 1 to 4 2 O 3 Catalyst and sponge palladium.
As can be seen from Table 1, the process of the present invention resulted in a spent catalyst treatment of at least 50kg and a Pd recovery of greater than 99%.
TABLE 1 spent Pd/Al in examples 1-4 2 O 3 Catalyst and sponge palladium indexes
In table 1, the Pd-containing amount means the Pd content in the spent catalyst; the yield metal amount refers to the content of Pd recovered.
The embodiments of the present invention have been described above. However, the present invention is not limited to the above embodiment. 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. Waste Pd/Al 2 O 3 A method for recovering Pd from a catalyst, comprising:
1) Waste Pd/Al 2 O 3 Reducing the catalyst by hydrogen, adding hydrochloric acid and nitric acid, heating for dissolving, leaching, and taking filtrate;
2) And (2) filtering the filtrate obtained in the step 1) in a chlorine atmosphere, and adding Fe powder to prepare coarse Pd powder.
2. The method of claim 1, further comprising:
3) Post-treatment: dissolving the crude Pd powder obtained in the step 2) by adopting hydrochloric acid and nitric acid, and purifying by adopting a dichlorodiamine palladium complex method to obtain refined Pd powder.
3. The method according to any of claims 1-2, characterized in that the method further comprises the steps of:
4) Leaching the filter residue obtained in the leaching step in the step 1) at least once, and recovering solids to obtain Al 2 O 3 。
4. A method according to any of claims 1-3, characterized in that the method further comprises the steps of:
5) Concentrating the waste liquid obtained after the solid is recovered in the step 4), namely FeCl 3 。
5. The method according to any one of claims 1 to 4, wherein in step 1), the spent Pd/Al is 2 O 3 The catalyst is calcined at 600-700 ℃ and then reduced by hydrogen.
6. The process according to any one of claims 1 to 5, wherein the time for the hydrogen reduction in step 1) is from 1 to 4 hours, preferably 2 hours.
7. The method according to any one of claims 1 to 6, wherein in step 1), the spent Pd/Al is 2 O 3 The Pd content in the catalyst is 0.18wt% -0.35 wt%.
8. The method according to any one of claims 1 to 7, wherein in step 1), the heating temperature is 85 to 100 ℃; the heating reaction time is 30-160 min.
9. The method as claimed in any one of claims 1 to 8, wherein in the step 2), the Fe powder is mixed with the waste Pd/Al 2 O 3 The mass ratio of the Pd content in the catalyst is 4-6.
10. The method according to any one of claims 1 to 9, wherein in the step 3), the obtained refined Pd powder is sponge palladium powder.
Preferably, step 3) comprises: dissolving the crude Pd powder in the step 2) by using hydrochloric acid and nitric acid, adding ammonia water, and filtering to obtain Pd (NH) 3 ) 4 Cl 2 Adding hydrochloric acid into the solution to generate Pd (NH) 3 ) 2 Cl 2 And after calcination, introducing hydrogen to reduce to obtain refined Pd powder.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5981788A (en) * | 1997-11-03 | 1999-11-09 | General Electric Company | Method for recovering and recycling catalyst constituents |
| CN1448522A (en) * | 2002-04-04 | 2003-10-15 | 中国石油化工股份有限公司 | Method of recovering noble metal from spent catalyst containing noble metal |
| CN102242276A (en) * | 2011-06-13 | 2011-11-16 | 白银万山稀贵金属科技有限责任公司 | Process for extracting noble metal palladium from industrial solid wastes |
| CN104878208A (en) * | 2015-05-29 | 2015-09-02 | 宁波大地化工环保有限公司 | Recovery method for palladium and ruthenium in catalytic combustion catalyst Pd-Ru/alumina |
| CN104988319A (en) * | 2015-06-19 | 2015-10-21 | 徐州浩通新材料科技股份有限公司 | Method and system for treating load type palladium-contained dead catalyst |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5981788A (en) * | 1997-11-03 | 1999-11-09 | General Electric Company | Method for recovering and recycling catalyst constituents |
| CN1448522A (en) * | 2002-04-04 | 2003-10-15 | 中国石油化工股份有限公司 | Method of recovering noble metal from spent catalyst containing noble metal |
| CN102242276A (en) * | 2011-06-13 | 2011-11-16 | 白银万山稀贵金属科技有限责任公司 | Process for extracting noble metal palladium from industrial solid wastes |
| CN104878208A (en) * | 2015-05-29 | 2015-09-02 | 宁波大地化工环保有限公司 | Recovery method for palladium and ruthenium in catalytic combustion catalyst Pd-Ru/alumina |
| CN104988319A (en) * | 2015-06-19 | 2015-10-21 | 徐州浩通新材料科技股份有限公司 | Method and system for treating load type palladium-contained dead catalyst |
Non-Patent Citations (2)
| Title |
|---|
| 张永平;: "从废钯碳催化剂中回收钯的研究", 山西化工, vol. 30, no. 01, pages 20 - 22 * |
| 金佳敏;何兴娇;石能富;: "含钯废催化剂中钯回收研究进展", 浙江化工, vol. 45, no. 02, pages 18 - 22 * |
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