CN106277022A - A kind of production method of electronic-grade sulfuric acid cerium ammonium - Google Patents
A kind of production method of electronic-grade sulfuric acid cerium ammonium Download PDFInfo
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- CN106277022A CN106277022A CN201610606175.6A CN201610606175A CN106277022A CN 106277022 A CN106277022 A CN 106277022A CN 201610606175 A CN201610606175 A CN 201610606175A CN 106277022 A CN106277022 A CN 106277022A
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- mixed liquor
- sulfuric acid
- electronic
- filtrate
- production method
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F17/00—Compounds of rare earth metals
- C01F17/20—Compounds containing only rare earth metals as the metal element
- C01F17/206—Compounds containing only rare earth metals as the metal element oxide or hydroxide being the only anion
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Abstract
The invention discloses the production method of a kind of electronic-grade sulfuric acid cerium ammonium, step is as follows: (1), cerous carbonate is added to the water formation mixed liquor；(2) mixed liquor, by step (1) obtained adds concentrated nitric acid dissolve, and with ammonia adjustment pH value to 1.5 2, after heating, then adjust pH to 4 4.5 with cerous carbonate, obtain acid solution；(3), the acid solution obtained in step (2) is filtrated to get filtrate；(4), in the filtrate that step (3) obtains, it is sequentially added into hydrogen peroxide and ammonia formation mixed liquor, the pH value of mixed liquor is regulated to 7, stands the mixed liquor formed containing precipitating；(5), the mixed liquor containing precipitation that rapid heating step (4) obtains is to micro-boiling；(6), the precipitation after pure water step (5) processes, plate-and-frame filtration are added；(7) precipitation, by sulfuric acid dissolution step (6) filtered, solution filters；(8), the filtrate obtained to step (7) adds ammonium sulfate, negative pressure condensing crystallizing, centrifuge dehydration acquisition electronic-grade sulfuric acid cerium ammonium.In cerium carbonate product prepared by the method for the present invention, the metal impurities ion concentration of non-rare earth is the lowest, Fe, Ca, Na, K, Pb, Zn, Mn, Al, Cu, Ni, Co, Cr ＜ 0.00005%.
Description
Technical field
The invention belongs to rare earth field, be specifically related to the production method of a kind of electronic-grade sulfuric acid cerium ammonium.
Background technology
The preparation method of Cericammoniumsulfate mainly uses cerous carbonate nitric acid to dissolve at present, adjusts pH value remove impurity, filtration, filtrate
Adding ammonia precipitation process after adding hydrogen peroxide oxidation, the tetravalence cerium hydroxide of generation, through the tetravalence cerium hydroxide use of plate-and-frame filtration
Sulfuric acid dissolution generate tetravalence cerous sulfate, through filter, filtrate add ammonium sulfate evaporating, concentrating and crystallizing, centrifuge dehydration, washing,
Packaging.It has a following weak point: non-rare earth metal impurity ion content high (Fe, Ca, Na, K, Pb, Zn, Mn, Al, Cu,
Ni, Co, Cr ＜ 0.0005%)；The uneven color of finished product.
Summary of the invention
It is an object of the present invention to provide the production method of a kind of electronic-grade sulfuric acid cerium ammonium, solve the sulphuric acid that existing method produces
The problem that cerium ammonium non-rare earth ion impurity content is high.
The technical scheme is that the production method of a kind of electronic-grade sulfuric acid cerium ammonium, step is as follows:
(1), cerous carbonate is added to the water formation mixed liquor；
(2) mixed liquor, by step (1) obtained adds concentrated nitric acid dissolve, and with ammonia adjustment pH value to 1.5-2, add
After heat, then adjust pH to 4-4.5 with cerous carbonate, obtain acid solution；
(3), the acid solution obtained in step (2) is filtrated to get filtrate；
(4) in the filtrate that step (3) obtains, it is sequentially added into hydrogen peroxide and ammonia forms mixed liquor, by the pH of mixed liquor
Value regulation, to 7, stands the mixed liquor formed containing precipitation；
(5), the mixed liquor containing precipitation that rapid heating step (4) obtains is to micro-boiling；
(6), the precipitation after pure water step (5) processes, plate-and-frame filtration are added；
(7) precipitation, by sulfuric acid dissolution step (6) filtered, solution filters；
(8), the filtrate obtained to step (7) adds ammonium sulfate, negative pressure condensing crystallizing, centrifuge dehydration acquisition electronic-grade sulfuric acid
Cerium ammonium.
Further, in step (1), cerous carbonate is 1 1.5 with the weight ratio of water.
Further, in step (2), the method for heating is: be heated to boiling, keeps more than 30min.
Further, in step (3), the method for filtration is: first with 200 mesh filter-cloth filterings, then the micropore with aperture 1-5um
Filter filters.
Further, in step (5), quickly heating refers to be heated to micro-boiling within 10min.
Further, in step (8), the condition of negative pressure condensing crystallizing is: temperature is 120-130 DEG C, [H]+Concentration is
8mol/L, pressure are-0.02MPa.
The present invention compared with prior art has the advantage that
1, in the present invention, under certain temperature, pH and pressure, carry out condensing crystallizing, evaporate knot in such a situa-tion
Crystalline substance, makes Cericammoniumsulfate crystal particle diameter increase, and specific surface area will reduce, and the absorption to other ion is lowered, and more can get rid of other
Impurity metal ion, centrifuge dehydration obtains the Cericammoniumsulfate of electron level.
2, in cerium carbonate product prepared by the method for the present invention, the metal impurities ion concentration of non-rare earth is the lowest, Fe,
Ca, Na, K, Pb, Zn, Mn, Al, Cu, Ni, Co, Cr ＜ 0.00005%.
Detailed description of the invention
Embodiment 1
(1), 1 part of cerous carbonate is joined formation mixed liquor in 1.5 parts of pure water
(2) mixed liquor, by step (1) obtained adds concentrated nitric acid dissolve, and adjust back pH to 1.8 with ammonia, heat 30
After minute, then with cerous carbonate readjustment pH to 4.4 to acid solution.
(3) it is, that 200 mesh filter clothes carry out being filtrated to get filtrate by the acid solution obtained in step (2) by aperture；
(4), the filtrate that step (3) obtains is carried out microfilter (aperture 3um) and be filtrated to get filtrate；
(5) filtrate, in step (4) is sequentially added into hydrogen peroxide and ammonia forms mixed liquor, by the pH regulator of mixed liquor
To 7, stand the mixed liquor formed containing precipitation for 0.2 hour；
(6) mixed liquor containing precipitation, in rapid heating step (5), to micro-boiling, improves cerium oxygenation efficiency, and allows residual
Hydrogen peroxide decomposes；
(7) pure water, plate-and-frame filtration, are added；
(8), the high-quality sulfuric acid dissolution of the cerium hydroxide of tetravalence, solution filter；
(9), filtrate add refined ammonium sulfate, temperature be 125 DEG C, [H]+Concentration is 8mol/L, pressure for-
Under conditions of 0.02MPa, tiny structure condensing crystallizing, centrifuge dehydration obtains electronic-grade sulfuric acid cerium ammonium.
Embodiment 2
(1), 1 part of cerous carbonate is joined formation mixed liquor in 2 parts of pure water
(2) mixed liquor, by step (1) obtained adds concentrated nitric acid dissolve, and adjust back pH to 2 with ammonia, heat 30 points
Zhong Hou, then with cerous carbonate readjustment pH to 4 to acid solution.
(3) it is, that 200 mesh filter clothes carry out being filtrated to get filtrate by the acid solution obtained in step (2) by aperture；
(4), the filtrate that step (3) obtains is carried out microfilter (aperture 5um) and be filtrated to get filtrate；
(5) filtrate, in step (4) is sequentially added into hydrogen peroxide and ammonia forms mixed liquor, by the pH regulator of mixed liquor
To 7, stand the mixed liquor formed containing precipitation for 0.4 hour；
(6) mixed liquor containing precipitation, in rapid heating step (5), to micro-boiling, improves cerium oxygenation efficiency, and allows residual
Hydrogen peroxide decomposes；
(7) pure water, plate-and-frame filtration, are added；
(8), the high-quality sulfuric acid dissolution of the cerium hydroxide of tetravalence, solution filter；
(9), filtrate add refined ammonium sulfate, temperature be 120 DEG C, [H]+Concentration is 8mol/L, pressure for-
Under conditions of 0.02MPa, tiny structure condensing crystallizing, centrifuge dehydration obtains electronic-grade sulfuric acid cerium ammonium.
Embodiment 3
(1), 1 part of cerous carbonate is joined formation mixed liquor in 1.5 parts of pure water
(2) mixed liquor, by step (1) obtained adds concentrated nitric acid dissolve, and adjust back pH to 1.5 with ammonia, heat 30
After minute, then with cerous carbonate readjustment pH to 4.5 to acid solution.
(3) it is, that 200 mesh filter clothes carry out being filtrated to get filtrate by the acid solution obtained in step (2) by aperture；
(4), the filtrate that step (3) obtains is carried out microfilter (aperture 1um) and be filtrated to get filtrate；
(5) filtrate, in step (4) is sequentially added into hydrogen peroxide and ammonia forms mixed liquor, by the pH regulator of mixed liquor
To 7, stand the mixed liquor formed containing precipitation for 0.3 hour；
(6) mixed liquor containing precipitation, in rapid heating step (5), to micro-boiling, improves cerium oxygenation efficiency, and allows residual
Hydrogen peroxide decomposes；
(7) pure water, plate-and-frame filtration, are added；
(8), the high-quality sulfuric acid dissolution of the cerium hydroxide of tetravalence, solution filter；
(9), filtrate add refined ammonium sulfate, temperature be 130 DEG C, [H]+Concentration is 8mol/L, pressure for-
Under conditions of 0.02MPa, tiny structure condensing crystallizing, centrifuge dehydration obtains electronic-grade sulfuric acid cerium ammonium.
Embodiment described above only have expressed the detailed description of the invention of the application, and it describes more concrete and detailed, but also
Therefore the restriction to the application protection domain can not be interpreted as.It should be pointed out that, for those of ordinary skill in the art
For, on the premise of conceiving without departing from technical scheme, it is also possible to make some deformation and improvement, these broadly fall into this
The protection domain of application.
Claims (6)
1. the production method of an electronic-grade sulfuric acid cerium ammonium, it is characterised in that step is as follows:
(1), cerous carbonate is added to the water formation mixed liquor；
(2) mixed liquor, by step (1) obtained adds concentrated nitric acid dissolve, and with ammonia adjustment pH value to 1.5-2, after heating,
Adjust pH to 4-4.5 with cerous carbonate again, obtain acid solution；
(3), the acid solution obtained in step (2) is filtrated to get filtrate；
(4), in the filtrate that step (3) obtains, it is sequentially added into hydrogen peroxide and ammonia forms mixed liquor, by the pH value tune of mixed liquor
Joint, to 7, stands the mixed liquor formed containing precipitation；
(5), the mixed liquor containing precipitation that rapid heating step (4) obtains is to micro-boiling；
(6), the precipitation after pure water step (5) processes, plate-and-frame filtration are added；
(7) precipitation, by sulfuric acid dissolution step (6) filtered, solution filters；
(8), the filtrate obtained to step (7) adds ammonium sulfate, negative pressure condensing crystallizing, centrifuge dehydration acquisition electronic-grade sulfuric acid cerium
Ammonium.
The production method of a kind of electronic-grade sulfuric acid cerium ammonium the most according to claim 1, it is characterised in that in step (1), carbon
Acid cerium is 1 1.5 with the weight ratio of water.
The production method of a kind of electronic-grade sulfuric acid cerium ammonium the most according to claim 1, it is characterised in that in step (2), add
The method of heat is: be heated to boiling, keeps more than 30min.
The production method of a kind of electronic-grade sulfuric acid cerium ammonium the most according to claim 1, it is characterised in that in step (3), mistake
The method of filter is: first with 200 mesh filter-cloth filterings, then filters with the microfilter of aperture 1-5um.
The production method of a kind of electronic-grade sulfuric acid cerium ammonium the most according to claim 1, it is characterised in that in step (5), soon
Speed heating refers to be heated to micro-boiling within 10min.
The production method of a kind of electronic-grade sulfuric acid cerium ammonium the most according to claim 1, it is characterised in that in step (8), negative
The condition of pressure condensing crystallizing is: temperature is 120-130 DEG C, [H]+Concentration is 8mol/L, pressure is-0.02MPa.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610606175.6A CN106277022A (en) | 2016-07-28 | 2016-07-28 | A kind of production method of electronic-grade sulfuric acid cerium ammonium |
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| CN201610606175.6A CN106277022A (en) | 2016-07-28 | 2016-07-28 | A kind of production method of electronic-grade sulfuric acid cerium ammonium |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113023763A (en) * | 2021-03-08 | 2021-06-25 | 益阳鸿源稀土有限责任公司 | Preparation method of high-purity cerium ammonium sulfate |
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| CN1847154A (en) * | 2006-03-21 | 2006-10-18 | 江苏大学 | Prepn process of ammonium-cerium nitrate double salt |
| CN101891235A (en) * | 2010-07-17 | 2010-11-24 | 天津市化学试剂研究所 | Method for preparing high-grade pure ceric sulfate |
| CN101898781A (en) * | 2009-05-25 | 2010-12-01 | 甘肃稀土新材料股份有限公司 | Method for preparing ammonium cerium nitrate compound salt |
| CN103910373A (en) * | 2014-04-04 | 2014-07-09 | 江西稀有金属钨业控股集团有限公司 | Method and system for preparing cerium hydroxide |
| CN104961149A (en) * | 2015-07-01 | 2015-10-07 | 乐山沃耐稀电子材料有限公司 | Preparation method of electron-grade ceric ammonium nitrate |
| CN105016371A (en) * | 2015-07-01 | 2015-11-04 | 乐山沃耐稀电子材料有限公司 | Preparation method of electronic grade ceric sulfate |
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| CN1847154A (en) * | 2006-03-21 | 2006-10-18 | 江苏大学 | Prepn process of ammonium-cerium nitrate double salt |
| CN101898781A (en) * | 2009-05-25 | 2010-12-01 | 甘肃稀土新材料股份有限公司 | Method for preparing ammonium cerium nitrate compound salt |
| CN101891235A (en) * | 2010-07-17 | 2010-11-24 | 天津市化学试剂研究所 | Method for preparing high-grade pure ceric sulfate |
| CN103910373A (en) * | 2014-04-04 | 2014-07-09 | 江西稀有金属钨业控股集团有限公司 | Method and system for preparing cerium hydroxide |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113023763A (en) * | 2021-03-08 | 2021-06-25 | 益阳鸿源稀土有限责任公司 | Preparation method of high-purity cerium ammonium sulfate |
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Application publication date: 20170104 |