CN105366656A - Purification method of capacitor grade phosphoric acid - Google Patents
Purification method of capacitor grade phosphoric acid Download PDFInfo
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- CN105366656A CN105366656A CN201510915838.8A CN201510915838A CN105366656A CN 105366656 A CN105366656 A CN 105366656A CN 201510915838 A CN201510915838 A CN 201510915838A CN 105366656 A CN105366656 A CN 105366656A
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- phosphoric acid
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- stage phosphoric
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Abstract
The invention belongs to the field of preparation of phosphoric acid and specifically relates to a purification method of capacitor grade phosphoric acid. The technical problem to be solved in the invention is that content of iron ion in existing capacitor grade phosphoric acid is high. In order to solve the above technical problem, the invention provides a purification method of capacitor grade phosphoric acid. The purification method comprises the following steps: a, cooling a capacitor grade phosphoric acid solution to 0-10 DEG C, adding seed crystal and crystallizing for 45-60 min; b, filtering out crystals after the crystallization, and washing the crystals with the capacitor grade phosphoric acid stock solution; c, adding high purity water into the crystals, and heating until the crystals are dissolved, so as to obtain purified capacitor grade phosphoric acid. The method provided by the invention has short industrial flow and is easy to control. By the method, investment cost is reduced and energy consumption is low.
Description
Technical field
The invention belongs to phosphoric acid preparation field, be specifically related to the purification process of capacitor stage phosphoric acid.
Background technology
In the capacitor stage phosphoric acid of current production, iron ion content is 2ppm, can only meet the demand of small portion ELECTRICAL MATERIALS manufacturing enterprise.And more high-end electronic raw material production enterprise, substantially all require iron ion content≤1ppm, to improve the performance and used life of product.
For meeting the specification of quality of high-end electronic enterprise to capacitor stage phosphoric acid, need the method researched and developed and reduce iron ion content in capacitor stage phosphoric acid badly.
Summary of the invention
The technical problem to be solved in the present invention is that in the capacitor stage phosphoric acid produced at present, iron ion content is higher.
Invent the purification process that the scheme solved the problems of the technologies described above is to provide a kind of capacitor stage phosphoric acid, comprise the following steps:
A, capacitor stage phosphoric acid solution is cooled to 0 ~ 10 DEG C, adds seeded crystallization 45 ~ 60 minutes;
After b, crystallization terminate, filter out crystal, with capacitor stage phosphoric acid stoste washing crystal;
C, in crystal, add high purity water, heating makes crystal dissolve, and obtains the capacitor stage phosphoric acid of purifying.
In the purification process of above-mentioned capacitor stage phosphoric acid, described in step a, the mass percentage of capacitor stage phosphoric acid solution is 84.0 ~ 85.0%; Wherein, the mass percentage of Fe ion is 0.0002 ~ 0.0003%.
In the purification process of above-mentioned capacitor stage phosphoric acid, the add-on of crystal seed described in step a is 1 ~ 3g/t phosphoric acid.
In the purification process of above-mentioned capacitor stage phosphoric acid, the cultural method of crystal seed described in step a is: capacitor stage phosphoric acid is cooled to 0 ~ 10 DEG C and makes phosphoric acid crystallization, purified by periodic crystallisation, the crystal seed prepared.The iron ion content of described crystal seed is lower than 1ppm.The purity of described crystal seed is (containing H
3pO
4) be 97.50%.
In the purification process of above-mentioned capacitor stage phosphoric acid, temperature when filtering described in step c is 0 ~ 10 DEG C.
In the purification process of above-mentioned capacitor stage phosphoric acid, the capacitor stage phosphoric acid stoste described in step c to be mass concentration be 79 ~ 82% capacitor stage phosphoric acid high purity water solution.
In the purification process of above-mentioned capacitor stage phosphoric acid, temperature when washing described in step c is 0 ~ 10 DEG C.
In the purification process of above-mentioned capacitor stage phosphoric acid, temperature when dissolving described in step c is 60 ~ 80 DEG C.
In the purification process of above-mentioned capacitor stage phosphoric acid, the add-on of high purity water described in step c is the mass percentage of phosphoric acid in the purifying capacitor stage phosphoric acid making to obtain is 79 ~ 82%.
Method industrial flow provided by the invention is short, is easy to control, and investment cost reduces, and energy consumption is low.Adopt the product that method purifying provided by the invention obtains, the content of its ion is reduced to≤1ppm from 2ppm, and its index, higher than former capacitor stage phosphoric acid company standard, realizes product up-gradation.
Accompanying drawing explanation
Fig. 1 process flow sheet of the present invention.
Embodiment
The purification process of capacitor stage phosphoric acid, comprises the following steps:
A, capacitor stage phosphoric acid solution is cooled to 0 ~ 10 DEG C, adds seeded crystallization 45 ~ 60 minutes;
After b, crystallization terminate, filter out crystal, with capacitor stage phosphoric acid stoste washing crystal;
C, in crystal, add high purity water, heating makes crystal dissolve, and obtains the capacitor stage phosphoric acid of purifying.
In the purification process of above-mentioned capacitor stage phosphoric acid, described in step a, the mass percentage of capacitor stage phosphoric acid solution is 84.0 ~ 85.0%; Wherein, the mass percentage of Fe ion is 0.0002 ~ 0.0003%.
In the purification process of above-mentioned capacitor stage phosphoric acid, the add-on of crystal seed described in step a is 1 ~ 3g/t phosphoric acid.
In the purification process of above-mentioned capacitor stage phosphoric acid, the cultural method of crystal seed described in step a is: capacitor stage phosphoric acid is cooled to 0 ~ 10 DEG C and makes phosphoric acid crystallization, purified by periodic crystallisation, the crystal seed prepared.The iron ion content of described crystal seed is lower than 1ppm.The purity of described crystal seed is (containing H
3pO
4) be 97.50%.
In the purification process of above-mentioned capacitor stage phosphoric acid, temperature when filtering described in step c is 0 ~ 10 DEG C.
In the purification process of above-mentioned capacitor stage phosphoric acid, the capacitor stage phosphoric acid stoste described in step c to be mass concentration be 79 ~ 82% capacitor stage phosphoric acid high purity water solution.
In the purification process of above-mentioned capacitor stage phosphoric acid, temperature when washing described in step c is 0 ~ 10 DEG C.
In the purification process of above-mentioned capacitor stage phosphoric acid, temperature when dissolving described in step c is 60 ~ 80 DEG C.As, steam can be poured in crystallizer chuck, heat up and dissolve crystal.
In the purification process of above-mentioned capacitor stage phosphoric acid, the add-on of high purity water described in step c is the mass percentage of phosphoric acid in the purifying capacitor stage phosphoric acid making to obtain is 79 ~ 82%.
The preparation of embodiment 1 crystal seed
1) use pure high purity water, cooling reactor is cleaned up, in cooling reactor, add 9 ~ 10 tons of elementary capacitor stage phosphoric acid;
2) turn on agitator, opens ice maker, cools capacitor stage phosphoric acid elementary in reactor, after about 30 minutes, start in reactor to occur xln, continue cooling, until phosphoric acid Temperature reaches about 0 DEG C in reactor, after about 60 minutes, stop ice maker, and keep normal stirring;
3) open outlet valve, the phosphoric acid after crystallization is put into filter and filters, mother liquor after filtration stores and for the production of PHOSPHORIC ACID TECH.GRADE;
4) crystal (about 6.5 ~ 8t) after filtering, transfers to cooling reactor, adds 1 ~ 1.5t high purity water, and open jacket steam, melting of heating;
5) after crystal all melts, repeating step 2) ~ 3) operation, when after Fe≤0.0001% in sampling and measuring phosphoric acid, crystal is packaged as the crystal seed finished product of 25kg/ bag.
The purifying of embodiment 2 capacitor stage phosphoric acid
10t capacitor stage phosphoric acid solution is cooled to 0 DEG C, adds seeded crystallization 30g and continue 0 DEG C of standing crystallization about 60 minutes, then stop cooling, and keep normal stirring.
After crystallization terminates, get axonometry crystal with f and f e content, if below Fe≤0.0001%, filter out crystal, with a small amount of 79% capacitor stage phosphoric acid stoste washing crystal; If crystal with f and f e >=0.0001%, pure water is adopted to carry out rinsing to the crystal inside filter, until Fe≤0.0001%, after leaching crystal, with a small amount of 79% capacitor stage phosphoric acid stoste washing crystal.
Cooling reactor is transferred to the crystal leached (about 7.5t), adds 1t high purity water, reheat and make it dissolve, obtain the capacitor stage phosphoric acid of purifying.
The mass concentration of the capacitor stage phosphoric acid that the present embodiment purifying obtains is 79%, and wherein, Fe content is≤1ppm.
Claims (10)
1. the purification process of capacitor stage phosphoric acid, comprises the following steps:
A, capacitor stage phosphoric acid solution is cooled to 0 ~ 10 DEG C, adds seeded crystallization 45 ~ 60 minutes;
After b, crystallization terminate, filter out crystal, with capacitor stage phosphoric acid stoste washing crystal;
C, in crystal, add high purity water, heating makes crystal dissolve, and obtains the capacitor stage phosphoric acid of purifying.
2. the purification process of capacitor stage phosphoric acid according to claim 1, is characterized in that: described in step a, the mass percentage of capacitor stage phosphoric acid solution is 84.0 ~ 85.0%; Wherein, the mass percentage of Fe ion is 0.0002 ~ 0.0003%.
3. the purification process of capacitor stage phosphoric acid according to claim 1, is characterized in that: the add-on of crystal seed described in step a is 1 ~ 3g/t phosphoric acid.
4. the purification process of capacitor stage phosphoric acid according to claim 1, is characterized in that: the cultural method of crystal seed described in step a is: capacitor stage phosphoric acid is cooled to 0 ~ 10 DEG C and makes phosphoric acid crystallization, purified by periodic crystallisation, the crystal seed prepared.
5. the purification process of capacitor stage phosphoric acid according to claim 1, is characterized in that: the iron ion content of crystal seed described in step a is lower than 1ppm.
6. the purification process of capacitor stage phosphoric acid according to claim 1, is characterized in that: temperature when filtering described in step c is 0 ~ 10 DEG C.
7. the purification process of capacitor stage phosphoric acid according to claim 1, is characterized in that: the capacitor stage phosphoric acid stoste described in step c to be mass concentration be 79 ~ 82% capacitor stage phosphoric acid high purity water solution.
8. the purification process of capacitor stage phosphoric acid according to claim 1, is characterized in that: temperature when washing described in step c is 0 ~ 10 DEG C.
9. the purification process of capacitor stage phosphoric acid according to claim 1, is characterized in that: temperature when dissolving described in step c is 60 ~ 80 DEG C.
10. the purification process of capacitor stage phosphoric acid according to claim 1, is characterized in that: the add-on of high purity water described in step c is the mass percentage of phosphoric acid in the purifying capacitor stage phosphoric acid making to obtain is 79 ~ 82%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510915838.8A CN105366656A (en) | 2015-12-10 | 2015-12-10 | Purification method of capacitor grade phosphoric acid |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510915838.8A CN105366656A (en) | 2015-12-10 | 2015-12-10 | Purification method of capacitor grade phosphoric acid |
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| CN105366656A true CN105366656A (en) | 2016-03-02 |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4657559A (en) * | 1985-05-08 | 1987-04-14 | Freeport Research And Engineering Company | Process for seed crystal preparation for phosphoric acid crystallization |
| CN101269804A (en) * | 2008-05-07 | 2008-09-24 | 瓮福（集团）有限责任公司 | Method for producing high-purity phosphoric acid crystal |
| CN101774555A (en) * | 2010-02-02 | 2010-07-14 | 天津大学 | Method for preparing electronic grade phosphoric acid through liquid membrane crystallization |
| CN104030261A (en) * | 2013-12-30 | 2014-09-10 | 广西明利化工有限公司 | A production method of high-purity electronic grade phosphoric acid |
-
2015
- 2015-12-10 CN CN201510915838.8A patent/CN105366656A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4657559A (en) * | 1985-05-08 | 1987-04-14 | Freeport Research And Engineering Company | Process for seed crystal preparation for phosphoric acid crystallization |
| CN101269804A (en) * | 2008-05-07 | 2008-09-24 | 瓮福（集团）有限责任公司 | Method for producing high-purity phosphoric acid crystal |
| CN101774555A (en) * | 2010-02-02 | 2010-07-14 | 天津大学 | Method for preparing electronic grade phosphoric acid through liquid membrane crystallization |
| CN104030261A (en) * | 2013-12-30 | 2014-09-10 | 广西明利化工有限公司 | A production method of high-purity electronic grade phosphoric acid |
Non-Patent Citations (3)
| Title |
|---|
| 中国国家标准化管理委员会: "电子级磷酸", 《中华人民共和国国家标准》 * |
| 欧阳平凯: "《生物分离原理及技术》", 28 February 1999 * |
| 肖立华: ""冷却结晶法制电子级磷酸的研究"", 《中国优秀硕士全文数据库 工程科技I辑》 * |
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Application publication date: 20160302 |