CN102219668A - Wet treatment process for oxalate - Google Patents
Wet treatment process for oxalate Download PDFInfo
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- CN102219668A CN102219668A CN2011100954497A CN201110095449A CN102219668A CN 102219668 A CN102219668 A CN 102219668A CN 2011100954497 A CN2011100954497 A CN 2011100954497A CN 201110095449 A CN201110095449 A CN 201110095449A CN 102219668 A CN102219668 A CN 102219668A
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- CN
- China
- Prior art keywords
- oxalate
- acid
- filtrate
- cobalt
- filter residue
- Prior art date
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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
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
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- Manufacture And Refinement Of Metals (AREA)
- Electrolytic Production Of Metals (AREA)
Abstract
The invention provides a wet treatment process for oxalate, comprising the following steps: A, adding water in oxalate for slurrying; B, mixing sheddings of a Pb anodic plate in electrodeposition process, waste oxalate and acid to react under the acidic condition to obtain a mixture; and C, filtering the mixture to obtain a filter residue and a filtrate, recovering lead salt from the filter residue, and recovering salt of the oxalate from the filtrate. The wet treatment process for oxalate provided by the invention has the advantages of without adding furnace, shortening the process, reducing dust pollution, reducing roasting and auxiliary material consumption, processing one more pollutant, saving energy, reducing discharge and protecting the environment, with good social benefit and economic benefit.
Description
Technical field
The present invention relates to technical field of chemistry, particularly a kind of technology of wet processing oxalate.
Background technology
Oxalate, particularly cobalt oxalate (or nickelous oxalate) etc. are to make Wimet, magneticsubstance, and indispensable starting material such as metal cobalt powder and cobalt/cobalt oxide are example with the cobalt oxalate: generally be by the cobalt salt solution after purifying with make after oxalate mixes.In process of production, unavoidably can produce some useless cobalt oxalates, generally its ratio can account for about the 2-5% of cobalt oxalate ultimate production.The treatment process of prior art generally is that pyrogenic process roasting-reduction is leached.But need come roasting with a rotary kiln or other stoves, need extra a kind of roasting apparatus that adds for hydrometallurgy enterprise, processing step of many simultaneously increases, and, in roasting process, also special dust collection device and dust guard pollution abatement equipment to be arranged because the particle of general cobalt oxalate is thinner.
Summary of the invention
The invention provides a kind of technology of wet processing oxalate, with simple, pollution-free, handle chloride plate cast and useless oxalate when cost is low.
To achieve these goals, the invention provides following technical scheme:
A kind of technology of wet processing oxalate, it comprises step:
A, the oxalate that will give up add water and carry out the pulp processing;
B, add acid with chloride plate cast in the electrolytic deposition process and useless oxalate and be blended under the acidic conditions reaction and obtain mixture;
C, described mixture filtered obtain filter residue and filtrate, from described filter residue, reclaim lead salt, from described filtrate, reclaim the salt in this oxalate.Promptly when oxalate is cobalt oxalate, reclaim cobalt salt; When oxalate is nickelous oxalate, reclaim nickel salt ...
Preferably, the pH value of described acidic conditions is 0.5-1.0.
Preferably, described acid is sulfuric acid, nitric acid, hydrochloric acid or perchloric acid.
Preferably, describedly add acid with chloride plate cast in the electrolytic deposition process and useless oxalate and be blended under the acidic conditions and temperature is 60-80 ℃ of down reaction, the reaction times is 1-3 hour.
Preferably, described oxalate is cobalt oxalate or nickelous oxalate.
By implementing above technical scheme, have following technique effect: the technology that the invention provides the wet processing oxalate does not need to increase stoving oven, has shortened technical process, has reduced dust pollution simultaneously.The chloride plate cast also is a kind of pollutent, need to handle, so when handling oxalate also handling the chloride plate cast, kill two birds with one stone.Reduced roasting and supplementary product onsumption, also handled another pollutent simultaneously, saved the energy greatly, reduced discharging, also protected environment, good social benefit and economic benefit have been arranged.
Embodiment
Technical scheme is for a better understanding of the present invention described embodiment provided by the invention below in detail.
Embodiment 1
Get 1 kilogram useless cobalt oxalate, cobalt contents 30.1% wherein adds the 5L tap water and stirs pulp in the glass reinforced plastic reactor of 10L, add 5 kilograms chloride plate cast, add concentration and be 98% industrial vitriol oil 0.65L, temperature of reaction is 65 ℃, 2 hours reaction times, terminal point pH=1.12, filtration obtains the filtrate of 5.3L and the filter residue of 5.7kg, the cobalt contents 54.3g/L in the filtrate wherein, lead content 0.07g/L, the cobalt contents 0.54% in the filter residue.The leaching yield 90.3% of cobalt.
Embodiment 2
Get 1 kilogram useless cobalt oxalate, cobalt contents 31.2% wherein adds the 4L tap water and stirs pulp in the glass reinforced plastic reactor of 10L, add 6 kilograms chloride plate cast, add concentration and be 98% industrial vitriol oil 0.75L, temperature of reaction is 80 ℃, 3 hours reaction times, terminal point pH=0.37, filtration obtains the filtrate of 4.4L and the filter residue of 6.9kg, the cobalt contents 69.8g/L in the filtrate wherein, lead content 0.09g/L, the cobalt contents 0.13% in the filter residue.The leaching yield 97.2% of cobalt.
Embodiment 3
Get 1 kilogram useless nickelous oxalate, nickel content 28.2% wherein adds the 6L tap water and stirs pulp in the glass reinforced plastic reactor of 10L, add 7 kilograms chloride plate cast, add concentration and be 98% industrial vitriol oil 0.70L, temperature of reaction is 70 ℃, 2 hours reaction times, terminal point pH=0.89, filtration obtains the filtrate of 6.4L and the filter residue of 7.7kg, the nickel content 43.1g/L in the filtrate wherein, lead content 0.08g/L, the nickel content 0.21% in the filter residue.The leaching yield 94.4% of nickel.
Embodiment 4
Get 1 kilogram useless cobalt oxalate, cobalt contents 29.8% wherein adds the 6L tap water and stirs pulp in the glass reinforced plastic reactor of 10L, add 7 kilograms chloride plate cast, add concentration and be 36.5% industrial concentrated hydrochloric acid 1.75L, temperature of reaction is 60 ℃, 2 hours reaction times, terminal point pH=1.01, filtration obtains the filtrate of 7.2L and the filter residue of 7.4kg, the cobalt contents 40.1g/L in the filtrate wherein, lead content 1.01g/L, the cobalt contents 0.29% in the filter residue.The leaching yield 93.1% of cobalt.
The embodiment of the invention provides a kind of technology of wet processing oxalate, its principle be since chloride plate in electrolytic deposition process, under electric current and voltage effect, chloride plate can form one deck PbO on the surface
2Film, in use owing to a variety of causes, it can slowly come off.Contain strong oxidizer PbO in the cast
2, under acidic conditions, its can oxidation oxalate in oxalate, thereby make salt become solubility.Wherein main chemical equation:
AC
2O
4+ 4H
++ PbO
2=2CO
2+ pb
2++ 2H
2O+A
2+(A is the metallic elements such as cobalt nickel of divalence)
Pb+2H
+＝pb
2++H
2
PbO+2H
+＝pb
2++H
2O
This technology comprises step:
A, the oxalate that will give up add water and carry out the pulp processing; In the present embodiment, described useless oxalate can also can be nickelous oxalate or other oxalate for useless cobalt oxalate.
B, add acid with chloride plate cast in the electrolytic deposition process and useless oxalate and be blended under the acidic conditions reaction and obtain mixture; Wherein, the pH value of described acidic conditions is 0.5-1.0.Preferably, described acid is other strong acid of sulfuric acid, nitric acid, hydrochloric acid or perchloric acid or the like.Preferably, the temperature of described reaction is 60-80 ℃, and the reaction times is 1-3 hour.
C, described mixture filtered obtain filter residue and filtrate, from described filter residue, reclaim lead salt, from described filtrate, reclaim the salt in this oxalate.
The technology that the foregoing description provides is owing to contain very a high proportion of strong oxidizer PbO in the chloride plate cast
2, it can the oxidation oxalate be CO
2Thereby, make oxalate, become the salt of solubility as the cobalt in the cobalt oxalate, can reclaim lead salt in the lump simultaneously.
Do not need to increase stoving oven, shortened technical process, reduced dust pollution simultaneously.The chloride plate cast also is a kind of pollutent, need to handle, so when handling oxalate also handling the chloride plate cast, kill two birds with one stone.Reduced roasting and supplementary product onsumption, also handled another pollutent simultaneously, saved the energy greatly, reduced discharging, also protected environment, good social benefit and economic benefit have been arranged.
More than the technology of a kind of wet processing oxalate that the embodiment of the invention provided is described in detail, for one of ordinary skill in the art, thought according to the embodiment of the invention, part in specific embodiments and applications all can change, in sum, this description should not be construed as limitation of the present invention.
Claims (5)
1. the technology of a wet processing oxalate is characterized in that, comprises step:
A, the oxalate that will give up add water and carry out the pulp processing;
B, add acid with chloride plate cast in the electrolytic deposition process and useless oxalate and be blended under the acidic conditions reaction and obtain mixture;
C, described mixture filtered obtain filter residue and filtrate, from described filter residue, reclaim lead salt, from described filtrate, reclaim the salt in this oxalate.
2. technology according to claim 1 is characterized in that the pH value of described acidic conditions is 0.5-1.0.
3. as technology as described in the claim 2, it is characterized in that described acid is sulfuric acid, nitric acid, hydrochloric acid or perchloric acid.
4. technology according to claim 1 is characterized in that, describedly adds acid with chloride plate cast in the electrolytic deposition process and useless oxalate and is blended under the acidic conditions and temperature is 60-80 ℃ of reaction down, and the reaction times is 1-3 hour.
5. technology according to claim 1 is characterized in that described oxalate is cobalt oxalate or nickelous oxalate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011100954497A CN102219668A (en) | 2011-04-15 | 2011-04-15 | Wet treatment process for oxalate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011100954497A CN102219668A (en) | 2011-04-15 | 2011-04-15 | Wet treatment process for oxalate |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102219668A true CN102219668A (en) | 2011-10-19 |
Family
ID=44776402
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2011100954497A Pending CN102219668A (en) | 2011-04-15 | 2011-04-15 | Wet treatment process for oxalate |
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| CN (1) | CN102219668A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104086406A (en) * | 2014-07-15 | 2014-10-08 | 中南大学 | Method for separating and recycling sodium oxalate from waste water containing oxalic acid |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4594230A (en) * | 1985-02-04 | 1986-06-10 | Gte Products Corporation | Recovery of cobalt |
| CN1995415A (en) * | 2006-12-22 | 2007-07-11 | 金川集团有限公司 | Process for treating secondary cobalt oxalate |
| CN101514395A (en) * | 2009-03-31 | 2009-08-26 | 大连物华天宝科技发展有限公司 | Method for recovering lead oxide by waste lead-acid storage battery |
-
2011
- 2011-04-15 CN CN2011100954497A patent/CN102219668A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4594230A (en) * | 1985-02-04 | 1986-06-10 | Gte Products Corporation | Recovery of cobalt |
| CN1995415A (en) * | 2006-12-22 | 2007-07-11 | 金川集团有限公司 | Process for treating secondary cobalt oxalate |
| CN101514395A (en) * | 2009-03-31 | 2009-08-26 | 大连物华天宝科技发展有限公司 | Method for recovering lead oxide by waste lead-acid storage battery |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104086406A (en) * | 2014-07-15 | 2014-10-08 | 中南大学 | Method for separating and recycling sodium oxalate from waste water containing oxalic acid |
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Application publication date: 20111019 |