CN1051683A - The recovery method of waste copper-series catylist - Google Patents
The recovery method of waste copper-series catylist Download PDFInfo
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- CN1051683A CN1051683A CN 89108629 CN89108629A CN1051683A CN 1051683 A CN1051683 A CN 1051683A CN 89108629 CN89108629 CN 89108629 CN 89108629 A CN89108629 A CN 89108629A CN 1051683 A CN1051683 A CN 1051683A
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- copper
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Abstract
Waste copper-series catylist, particularly contain CuOZnOAl
2O
3The recovery method of waste copper-series catylist, this method comprises waste copper-series catylist is immersed in the aqueous solution of ammonia and carbon dioxide, the rich solution and the residue that leach carry out Separation of Solid and Liquid, and the rich solution heating evaporation after the separation is when being settled out now, with one times of rich solution dilution, and solution temperature remained on 45 ℃～55 ℃, being neutralized to pH with nitric acid is 6.0～6.2, is incubated 10～15 minutes then, discard mother liquor, its precipitation is the mixture of slaine and metal oxide.The technological process of this waste copper-series catylist recovery method is short, and the rate of recovery of metallic copper zinc reaches 93%, and what obtain is the intermediate products of Cu-series catalyst, has eliminated the operation of changing metal, has reduced environmental pollution.
Description
The present invention relates to a kind of waste copper-series catylist, particularly contain CuOZnOAl
2O
3The recovery method of waste copper-series catylist.
Low temperature conversion catalyst, low change protective agent and low pressure methanol synthesis catalyst all contain CuOZnOAl
2O
3, the recovery of this dead catalyst is general to separate Al with the acid alkali treatment earlier
2O
3After, again with chloride volatility process or smelting process recovering copper and zinc.Chloride volatility process is to handle dead catalyst under the high temperature chlorine atmosphere, separates and recovery copper and zinc with chloride form.Smelting process is dead catalyst to be added slag former etc. make pelletizing, melting in special smelting furnace, and zinc captures with the silicon magnesia brick in gas phase, obtains redistilled zinc after distillation; Copper forms matte, is smelted into blister copper earlier in converter, is electrolyzed to produce high pure electrolytic copper again.Above-mentioned recovery method equipment investment is big, complex process, reclaims the copper, the zinc metal that obtain and is separated from each other.If, copper, zinc metal need be made metal oxide, thereby consume the more chemical substance and the energy again during controlling catalyst with the copper that reclaims, zinc metal, make controlling catalyst cost up again.
The purpose of this utility model is to provide that a kind of technology is simple, equipment investment is little, reclaim what directly obtain is again the recovery method of waste copper-series catylist of the intermediate products metal oxide of controlling catalyst.
Waste copper-series catylist, particularly contain CuOZnOAl
2O
3The recovery method of waste copper-series catylist, this method comprises waste copper-series catylist is immersed in the aqueous solution of ammonia and carbon dioxide, make waste copper-series catylist copper, zinc oxide soak stripping, the rich solution and the residue that leach carry out Separation of Solid and Liquid, rich solution heating evaporation after the separation, when being settled out now, with one times of rich solution dilution, and solution temperature remained on 45 ℃～55 ℃, being neutralized to PH with nitric acid is 6.0～6.2, be incubated 10～15 minutes then, discard the mixture that its precipitation of mother liquor is slaine and metal oxide.
The leachate that ammonia, carbon dioxide and water are formed, its ammonia concentration 5～6M, gas concentration lwevel 1.8～2.2M, leach 50 ℃～60 ℃ of reaction temperatures, solid-to-liquid ratio 1: 8, the reaction time is no less than 2 hours, leaching process carries out mechanical agitation, and mixing speed is not less than 200 rev/mins.
Separation of Solid and Liquid adopts heavy heat-clearing method, and once heavy precipitation after clear adds the leaching of leaching agent secondary, and heavy again sorting was from solid-liquid after secondary leached, and the heavy precipitation after clear of secondary adds water washing, and washing lotion is made leaching agent and used.
Now with B
202Low temperature conversion catalyst is the recovery method of example explanation waste copper-series catylist.
B
202Catalyst is is active component, zinc oxide with the cupric oxide as interval body, the alundum (Al CuOZnOAl as carrier
2O
3Be low change catalyzer, its chemical composition is as follows:
CuO ＞29%
ZnO 41～45%
Al
2O
38.4～10%
Loss on ignition (900 ℃ 2 hours)＜more than the 15%(by weight percentage)
B
202Catalyst is owing to use for a long time, and hole is stopped up by carbon and dust, thereby loses activity, and has been difficult to recover with physical method.Therefore adopt chemical method to handle, make it recover active.
B will give up
202Catalyst immerses in the aqueous solution of ammonia and carbon dioxide, the concentration of leaching agent ammonia is that 5～6M, gas concentration lwevel are 1.8～2.2M, solid-to-liquid ratio is 1: 8, extraction temperature is controlled between 50 ℃～60 ℃, extraction time is no less than 2 hours, adopt mechanical agitation for accelerating leaching velocity, mixing speed is not less than 200 rev/mins.
Residue after the leaching accounts for about 25% of material, and wherein exhausted major part is an alundum (Al, and its particle is very thin, is attached with graphite and carbon, and is mixed with silt, and it is very difficult that the method that slip filters with vacuum is carried out Separation of Solid and Liquid.Thereby adopt heavy heat-clearing method to carry out Separation of Solid and Liquid, with slip heavy clear after, by upper strata sucking-off clear liquid, precipitation adds the leaching agent leaching again, and heavy again sorting is from clear liquid, and secondary precipitation adds the water secondary washing, its secondary cleaning water is made leaching agent then and is used as the absorbent of ammonia, and the precipitation residue is drained.
The rich solution heating evaporation (about 90 ℃ of boiling point) that leaches with secondary once, when being heated to precipitation when just having occurred (free ammonia concentration is 6%), to precipitate one times of dilution, and make solution temperature remain on 45 ℃～55 ℃, nitric acid neutralization with 10%, when being neutralized to PH and being 6.0～6.2, neutralization promptly comes to an end.Be incubated 10～15 minutes then, the precipitation that obtains then is the mixture of carbon formula copper carbonate, basic zinc carbonate and cupric oxide, zinc.Because have nitric acid ammonia to generate in the N-process, the existence of nitric acid ammonia produces salt effect, and carbon formula basic copper carbonate zinc carbonate is had certain dissolution, the metal that contains in the mother liquor is still very considerable, can adopt ion-exchange to reclaim copper and zinc from mother liquor for this reason.Carbon formula copper carbonate, basic zinc carbonate and the cupric oxide that obtains, the mixture precipitation of zinc are produces B
202The intermediate products of low temperature conversion catalyst, this precipitation is pressed B
202Production technology is proceeded, and makes new B202 low temperature conversion catalyst, and its every technical indicator all meets the requirements.
Adopt said method to reclaim waste copper-series catylist, technological process is short, and the rate of recovery of metallic copper zinc reaches 93%, and what obtain is the intermediate products of Cu-series catalyst, has eliminated the operation of changing metal, has reduced environmental pollution.
Claims (3)
1, a kind of waste copper-series catylist, particularly contain CuOZnOAl
2O
3The recovery method of waste copper-series catylist, this method comprises waste copper-series catylist is immersed in the aqueous solution of ammonia and carbon dioxide, the rich solution and the residue that leach carry out Separation of Solid and Liquid, and the rich solution heating evaporation after the separation is when being settled out now, with one times of rich solution dilution, and solution temperature remained on 45 ℃～55 ℃, being neutralized to PH with nitric acid is 6.0～6.2, is incubated 10～15 minutes then, discard mother liquor, its precipitation is the mixture of slaine and metal oxide.
2, the recovery method of waste copper-series catylist according to claim 1, it is characterized in that in the leachate of ammonia, carbon dioxide and water composition, ammonia concentration 5～6M, gas concentration lwevel 1.8～2.2M, leach 50 ℃～60 ℃ of reaction temperatures, solid-to-liquid ratio 1: 8, the reaction time is no less than 2 hours, leaching process carries out mechanical agitation, and mixing speed is not less than 200 rev/mins.
3, the recovery method of waste copper-series catylist according to claim 1 and 2, it is characterized in that Separation of Solid and Liquid adopts heavy heat-clearing method, precipitation after once sinking clearly adds the leaching of leaching agent secondary, heavy again sorting was from solid-liquid after secondary leached, precipitation after secondary sinks clearly adds water washing, and washing lotion is made leaching agent and used.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 89108629 CN1051683A (en) | 1989-11-16 | 1989-11-16 | The recovery method of waste copper-series catylist |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 89108629 CN1051683A (en) | 1989-11-16 | 1989-11-16 | The recovery method of waste copper-series catylist |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1051683A true CN1051683A (en) | 1991-05-29 |
Family
ID=4857651
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 89108629 Pending CN1051683A (en) | 1989-11-16 | 1989-11-16 | The recovery method of waste copper-series catylist |
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| CN (1) | CN1051683A (en) |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1048920C (en) * | 1995-10-27 | 2000-02-02 | 中国石油化工集团公司北京化工研究院 | Catalyst regenerating method for synthesizing 1,4-butynediol from formaldehyde and acetylene by slurry-bed reaction |
| CN1048919C (en) * | 1995-10-27 | 2000-02-02 | 中国石油化工集团公司北京化工研究院 | Regenerating method of catalyst for 1,4-butine-glycol synthetized by formaldehyde and acetylene reacted in slurry bed |
| CN1081085C (en) * | 1996-11-15 | 2002-03-20 | 李宽义 | Method for applying regenerated circulation of fluid-bed catalytic hydrogenation catalyst |
| CN102125851A (en) * | 2010-12-29 | 2011-07-20 | 西南化工研究设计院 | Application method of waste copper based catalyst to preparing catalyst for preparing hydrogen from methanol |
| CN103274951A (en) * | 2013-03-26 | 2013-09-04 | 南通市海圣药业有限公司 | Method for recovering copper-containing mother liquid in 4-aminotrifluorotoluene production technology |
| CN105478001A (en) * | 2015-12-30 | 2016-04-13 | 北京三聚环保新材料股份有限公司 | Method for preparing desulfurizing agent from copper-zinc dead catalyst |
| CN113104881A (en) * | 2019-12-12 | 2021-07-13 | 林齐坤 | Treatment method of washing liquid in condensation section of reduced olive green B-B imine |
-
1989
- 1989-11-16 CN CN 89108629 patent/CN1051683A/en active Pending
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1048920C (en) * | 1995-10-27 | 2000-02-02 | 中国石油化工集团公司北京化工研究院 | Catalyst regenerating method for synthesizing 1,4-butynediol from formaldehyde and acetylene by slurry-bed reaction |
| CN1048919C (en) * | 1995-10-27 | 2000-02-02 | 中国石油化工集团公司北京化工研究院 | Regenerating method of catalyst for 1,4-butine-glycol synthetized by formaldehyde and acetylene reacted in slurry bed |
| CN1081085C (en) * | 1996-11-15 | 2002-03-20 | 李宽义 | Method for applying regenerated circulation of fluid-bed catalytic hydrogenation catalyst |
| CN102125851A (en) * | 2010-12-29 | 2011-07-20 | 西南化工研究设计院 | Application method of waste copper based catalyst to preparing catalyst for preparing hydrogen from methanol |
| CN102125851B (en) * | 2010-12-29 | 2012-11-21 | 西南化工研究设计院 | Application method of waste copper based catalyst to preparing catalyst for preparing hydrogen from methanol |
| CN103274951A (en) * | 2013-03-26 | 2013-09-04 | 南通市海圣药业有限公司 | Method for recovering copper-containing mother liquid in 4-aminotrifluorotoluene production technology |
| CN103274951B (en) * | 2013-03-26 | 2015-01-14 | 南通市海圣药业有限公司 | Method for recovering copper-containing mother liquid in 4-aminotrifluorotoluene production technology |
| CN105478001A (en) * | 2015-12-30 | 2016-04-13 | 北京三聚环保新材料股份有限公司 | Method for preparing desulfurizing agent from copper-zinc dead catalyst |
| CN113104881A (en) * | 2019-12-12 | 2021-07-13 | 林齐坤 | Treatment method of washing liquid in condensation section of reduced olive green B-B imine |
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