CN100427406C - Waste molybdenum nickel cobalt catalyst utilization method for environmental protection - Google Patents
Waste molybdenum nickel cobalt catalyst utilization method for environmental protection Download PDFInfo
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- CN100427406C CN100427406C CNB2006100971487A CN200610097148A CN100427406C CN 100427406 C CN100427406 C CN 100427406C CN B2006100971487 A CNB2006100971487 A CN B2006100971487A CN 200610097148 A CN200610097148 A CN 200610097148A CN 100427406 C CN100427406 C CN 100427406C
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Abstract
The invention discloses an environment protective utilizing method of waste Mo-Ni-Co catalyst, which comprises the following step: adding different reacting materials into raw material; separating different products according to different chemical properties of metal salt and different conditions step by step; making the product.
Description
Technical field
The present invention relates to the method that the scrap metal environmental protection is reclaimed, the environmental protection of particularly a kind of waste molybdenum nickel cobalt catalyst molybdenum that is used for the petrochemical industry catalyzer, nickel, cobalt utilizes method.
Background technology
Molybdenum accounts for 16-30% in the molybdenum nickel cobalt catalyst of petrochemical industry widespread use, nickel accounts for 6-8%, cobalt accounts for about 4%, their forms with oxide compound in catalyzer exist, other is mainly the organic impurity of a spot of Si oxide and absorption, after cancelling, catalyzer can cause bigger pollution to environment, if can effective recycling, and its environmental protection and economy is worth considerable.But the recoverying and utilizing method that not only has the value of environmental protection but also better economic benefit can be arranged is not arranged also at present.
Summary of the invention
Purpose of the present invention provides a kind of method of utilizing that has waste molybdenum nickel cobalt catalyst that environmental protection and economy is worth concurrently.The technical scheme that realizes above-mentioned purpose is as follows:
Waste molybdenum nickel cobalt catalyst utilize method, comprise the steps:
A, the molybdenum nickel that will give up estimate catalyzer after organic impurity is removed in the roasting of 500-600 degree, make feed particles through wet-milling;
B adds sodium hydroxide and react the generation sodium molybdate solution under 75-90 degree condition in feed particles, filter;
C adds sulfuric acid and the pH value is transferred to 4-5 in the filtrate after the b step, the precipitation oven dry after the filtration obtains the molybdenum oxide product;
D, add sulfuric acid in the filter residue after in the b step, filtering, regulate pH to 1-1.5, generate single nickel salt and cobalt sulfate solution, filter out and in filtrate, add yellow soda ash behind the impurity and make pH value of solution transfer to alkalescence, generate cobaltous carbonate and nickelous carbonate precipitation, solution is heated to the above also bubbling air bubbling of 60 degree, make the cobaltous carbonate precipitation of generation change into the cobaltous dihydroxycarbonate precipitation again, solution is filtered;
E adds dilute acetic acid in the filter residue after the last filtration of d step, and reaction generates nickel acetate solution, mixed solution is filtered, and filtrate is nickel acetate, gets the nickel acetate product after routine is handled, filter residue is the cobaltous dihydroxycarbonate precipitation, is sintered into the cobalt oxide product at the 500-600 degree after drying.
Further, in the described a step after the wet-milling again after 300 purpose screen clothes are selected materials as feed particles.
Can also be to after generating single nickel salt and cobalt sulfate solution in the described d step, add sodium hydroxide again the pH value of solution value is transferred to 4, add hydrogen peroxide again and a spot of low price iron ion in the solution is oxidized to the high price precipitation of iron ions and filters to remove the impurity iron in the solution; Described filtering out adds yellow soda ash behind the impurity and makes the pH value of solution transfer to 8; Described Heating temperature is 80 degree.
In addition, in described e step, make the nickel acetate product after, Dichlorodiphenyl Acetate nickel product carries out roasting can get the nickel oxide product.
The main chemical reactions equation that aforementioned techniques scheme and technical measures thereof relate to is as follows:
MoO
3+NaOH→Na
2MoO
4+H
2O
Na
2MoO
4+H
2SO
4→MoO
3↓+Na
2SO
4
NiO+H
2SO
4→NiSO
4+H
2O
CoO+H
2SO
4→CoSO
4+H
2O
NiSO
4+Na
2CO
3→NiCO
3↓+Na
2SO
CoSO
4+Na
2CO
3→CoCO
3↓+Na
2SO
CoCO
3+OH
-→Co(OH)CO
3↓
NiCO
3+HAc→Ni(Ac)
2
Advantage of the present invention is molybdenum nickel cobalt valuable in the waste molybdenum nickel cobalt catalyst can be recycled, and non-environmental-pollution in the production process, has higher society and economy benefit.
Embodiment
Below be the specific embodiment of the present invention:
The molybdenum nickel that will give up is estimated catalyzer after organic impurity is removed in 500 degree roastings (mainly producing) when being used for the catalysis of petrochemical industry reaction process, polishing is made after 300 purpose screen clothes are made feed particles after sieving through humidification; In feed particles, add sodium hydroxide and under 80 degree conditions, react the generation sodium molybdate solution, in filtrate filtered, add sulfuric acid and the pH value is transferred to 4, generate the molybdenum oxide precipitation, oven dry behind the sedimentation and filtration is obtained the molybdenum oxide product; In feed particles, add the filter residue of sodium hydroxide after reaction is filtered under the 80 degree conditions and add sulfuric acid, regulate pH to 1, generate single nickel salt and cobalt sulfate solution, add sodium hydroxide again the pH value of solution value is transferred to 4, add hydrogen peroxide again and a spot of low price iron ion in the solution is oxidized to the high price precipitation of iron ions and filters to remove the impurity iron in the solution; Filter out and in filtrate, add yellow soda ash behind the impurity and make pH value of solution transfer to 8, generate cobaltous carbonate and nickelous carbonate precipitation, solution is heated to 80 degree and bubbling air bubblings, make the cobaltous carbonate precipitation of generation change into cobaltous dihydroxycarbonate again and precipitate, solution is filtered; Add dilute acetic acid in filter residue, reaction generates nickel acetate solution, and mixed solution is filtered, and filtrate is nickel acetate, after routine is handled the nickel acetate product, but also Dichlorodiphenyl Acetate nickel product carries out roasting and obtains the nickel oxide product.Filter residue is the cobaltous dihydroxycarbonate precipitation, is sintered into the cobalt oxide product at 600 degree after drying.
Claims (4)
1, waste molybdenum nickel cobalt catalyst utilize method, it is characterized by: comprise the steps,
A, the molybdenum nickel that will give up estimate catalyzer after organic impurity is removed in the roasting of 500-600 degree, make feed particles through wet-milling;
B adds sodium hydroxide and react the generation sodium molybdate solution under 75-90 degree condition in feed particles, filter;
C adds sulfuric acid and the pH value is transferred to 4-5 in the filtrate after the b step, the precipitation oven dry after the filtration obtains the molybdenum oxide product;
D, add sulfuric acid in the filter residue after in the b step, filtering, regulate pH to 1-1.5, generate single nickel salt and cobalt sulfate solution, filter out and in filtrate, add yellow soda ash behind the impurity and make pH value of solution transfer to alkalescence, generate cobaltous carbonate and nickelous carbonate precipitation, solution is heated to the above also bubbling air bubbling of 60 degree, make the cobaltous carbonate precipitation of generation change into the cobaltous dihydroxycarbonate precipitation again, solution is filtered;
E adds dilute acetic acid in the filter residue after the last filtration of d step, and reaction generates nickel acetate solution, mixed solution is filtered, and filtrate is nickel acetate, gets the nickel acetate product after routine is handled, filter residue is the cobaltous dihydroxycarbonate precipitation, is sintered into the cobalt oxide product at the 500-600 degree after drying.
2, waste molybdenum nickel cobalt catalyst according to claim 1 utilize method, it is characterized in that: in the described a step after the wet-milling again after 300 purpose screen clothes are selected materials as feed particles.
3, waste molybdenum nickel cobalt catalyst according to claim 1 utilizes method, it is characterized in that: after generating single nickel salt and cobalt sulfate solution in the described d step, add sodium hydroxide again the pH value of solution value is transferred to 4, add hydrogen peroxide again and a spot of low price iron ion in the solution is oxidized to the high price precipitation of iron ions and filters to remove the impurity iron in the solution; Described filtering out adds yellow soda ash behind the impurity and makes the pH value of solution transfer to 8; Described Heating temperature is 80 degree.
4, waste molybdenum nickel cobalt catalyst according to claim 1 utilize method, it is characterized in that: after making the nickel acetate product in the described e step, Dichlorodiphenyl Acetate nickel product carries out roasting can get the nickel oxide product.
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| CNB2006100971487A CN100427406C (en) | 2006-10-25 | 2006-10-25 | Waste molybdenum nickel cobalt catalyst utilization method for environmental protection |
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| CNB2006100971487A CN100427406C (en) | 2006-10-25 | 2006-10-25 | Waste molybdenum nickel cobalt catalyst utilization method for environmental protection |
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| CN100427406C true CN100427406C (en) | 2008-10-22 |
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Families Citing this family (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101435027B (en) * | 2007-11-15 | 2010-06-02 | 中国石油化工股份有限公司 | Method for recycling high purity molybdenum from molybdenum-containing spent catalyst |
| CN101724758B (en) * | 2008-10-29 | 2011-04-06 | 中国石油化工股份有限公司抚顺石油化工研究院 | Method for recycling molybdenum of molybdenum-contained waste catalyst |
| MX349312B (en) * | 2011-08-26 | 2017-07-20 | Ecometales Ltd | Method for recovering technical-grade molybdenum from diluted acid leaching solutions (pls) that have a high arsenic concentration and originate from metallurgical waste. |
| CN103849772A (en) * | 2012-11-28 | 2014-06-11 | 大连东泰产业废弃物处理有限公司 | Method for recovering metal cobalt by N,N'-1,2-ethanediylbis-1-aspartic acid |
| CN103343232A (en) * | 2013-07-11 | 2013-10-09 | 岳阳鼎格云天环保科技有限公司 | Method for recycling Ni from waste FCC (Fluid Catalytic Cracking) catalyst |
| CN105603195B (en) * | 2016-02-03 | 2017-06-13 | 华东理工大学 | The method that molybdenum and nickel are extracted from acrylonitrile dead catalyst |
| CN107585789B (en) * | 2017-09-26 | 2019-08-23 | 河南科技大学 | A method of high-purity molybdenum trioxide is prepared using hydrometallurgy molybdenum concentrate |
| CN108728653B (en) * | 2018-06-11 | 2019-11-22 | 江苏北矿金属循环利用科技有限公司 | A method of extracting molybdenum from useless nickel molybdenum catalyst |
| CN110937991A (en) * | 2018-09-21 | 2020-03-31 | 荆门市格林美新材料有限公司 | Preparation method of green synthetic nickel acetate crystal |
| CN114763585B (en) * | 2021-01-14 | 2024-04-09 | 万华化学集团股份有限公司 | Method for preparing cobalt iso-octoate by using waste Raney cobalt catalyst |
Citations (3)
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|---|---|---|---|---|
| JPH09235628A (en) * | 1996-02-29 | 1997-09-09 | Catalysts & Chem Ind Co Ltd | Separation and recovery of useful metal from used desulfurization catalyst |
| CN1544666A (en) * | 2003-11-14 | 2004-11-10 | 沈阳嘉禾冶金炉料有限公司 | Method for recovering nickel and aluminum from waste aluminum based nickel-containing catalyst |
| CN1814827A (en) * | 2005-04-30 | 2006-08-09 | 李翔 | Method for separating and recovering cobalt and molybdic from waste cobalt-molybdic catalyst |
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2006
- 2006-10-25 CN CNB2006100971487A patent/CN100427406C/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH09235628A (en) * | 1996-02-29 | 1997-09-09 | Catalysts & Chem Ind Co Ltd | Separation and recovery of useful metal from used desulfurization catalyst |
| CN1544666A (en) * | 2003-11-14 | 2004-11-10 | 沈阳嘉禾冶金炉料有限公司 | Method for recovering nickel and aluminum from waste aluminum based nickel-containing catalyst |
| CN1814827A (en) * | 2005-04-30 | 2006-08-09 | 李翔 | Method for separating and recovering cobalt and molybdic from waste cobalt-molybdic catalyst |
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