CN104030261A - A production method of high-purity electronic grade phosphoric acid - Google Patents
A production method of high-purity electronic grade phosphoric acid Download PDFInfo
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- CN104030261A CN104030261A CN201310744485.0A CN201310744485A CN104030261A CN 104030261 A CN104030261 A CN 104030261A CN 201310744485 A CN201310744485 A CN 201310744485A CN 104030261 A CN104030261 A CN 104030261A
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- phosphoric acid
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- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 title claims abstract description 187
- 229910000147 aluminium phosphate Inorganic materials 0.000 title claims abstract description 93
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 33
- 239000002253 acid Substances 0.000 claims abstract description 52
- 239000013078 crystal Substances 0.000 claims abstract description 49
- 239000002994 raw material Substances 0.000 claims abstract description 30
- 238000002425 crystallisation Methods 0.000 claims abstract description 28
- 239000007791 liquid phase Substances 0.000 claims abstract description 24
- 230000008025 crystallization Effects 0.000 claims abstract description 23
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 23
- 238000005406 washing Methods 0.000 claims abstract description 15
- 238000002844 melting Methods 0.000 claims abstract description 14
- 230000008018 melting Effects 0.000 claims abstract description 14
- 239000000126 substance Substances 0.000 claims abstract description 12
- 239000012071 phase Substances 0.000 claims abstract description 11
- 238000001914 filtration Methods 0.000 claims abstract description 10
- 239000012452 mother liquor Substances 0.000 claims description 17
- 238000001095 inductively coupled plasma mass spectrometry Methods 0.000 claims description 15
- 239000012535 impurity Substances 0.000 claims description 13
- 239000007788 liquid Substances 0.000 claims description 11
- 239000007921 spray Substances 0.000 claims description 9
- 239000012267 brine Substances 0.000 claims description 8
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 claims description 8
- 239000004576 sand Substances 0.000 claims description 6
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 6
- 239000012498 ultrapure water Substances 0.000 claims description 6
- 238000001514 detection method Methods 0.000 claims description 4
- 238000003828 vacuum filtration Methods 0.000 claims description 4
- 230000002950 deficient Effects 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 15
- 238000003756 stirring Methods 0.000 abstract description 5
- 230000008901 benefit Effects 0.000 abstract description 4
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 abstract description 3
- 238000000926 separation method Methods 0.000 abstract description 2
- 239000002826 coolant Substances 0.000 abstract 1
- 238000010438 heat treatment Methods 0.000 abstract 1
- 229910052698 phosphorus Inorganic materials 0.000 abstract 1
- 239000011574 phosphorus Substances 0.000 abstract 1
- 238000001816 cooling Methods 0.000 description 7
- 230000001105 regulatory effect Effects 0.000 description 4
- 238000004140 cleaning Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000005265 energy consumption Methods 0.000 description 3
- 229910021645 metal ion Inorganic materials 0.000 description 3
- RAHZWNYVWXNFOC-UHFFFAOYSA-N Sulphur dioxide Chemical compound O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000005530 etching Methods 0.000 description 2
- 239000004973 liquid crystal related substance Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 230000035900 sweating Effects 0.000 description 2
- 229910052785 arsenic Inorganic materials 0.000 description 1
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 description 1
- 230000003749 cleanliness Effects 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000005457 ice water Substances 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 239000010413 mother solution Substances 0.000 description 1
- 230000036470 plasma concentration Effects 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 235000010269 sulphur dioxide Nutrition 0.000 description 1
- 239000004291 sulphur dioxide Substances 0.000 description 1
- OBSZRRSYVTXPNB-UHFFFAOYSA-N tetraphosphorus Chemical compound P12P3P1P32 OBSZRRSYVTXPNB-UHFFFAOYSA-N 0.000 description 1
- 238000007669 thermal treatment Methods 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
- 239000002918 waste heat Substances 0.000 description 1
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a production method of high-purity electronic grade phosphoric acid, and belongs to the technical field of phosphoric acid production in the phosphorus chemical industry. The method includes steps of: adding a raw material acid into an agitated crystallizer, adding seeds, stirring and crystallizing until the crystallization ratio is 30-60%, vacuumizing and filtering to completely separate the crystal phase from the liquid phase, washing the crystal phase, heating the crystals with hot water in a jacket and stirring to melt the crystals, and adjusting the acid to obtain a product. By adoption of a stirring crystallization manner, the phosphoric acid is prepared into sandy crystals, the heat exchange rate between the phosphoric acid and a cooling medium is increased, and the crystallization speed is accelerated. Separation of the crystal phase and the liquid phase is more complete and rapid by adoption of a vacuumizing and filtering manner. The speed of crystal melting is accelerated by stirring crystal melting. Therefore, the production period of the electronic grade phosphoric acid is largely shortened, the production efficiency is largely increased, and the production method has good economic benefit.
Description
Technical field
The invention belongs to phosphoric acid production technical field in sulphur dioxide of phosphor chemical industry, relate to a kind of production method of high purity electron-level phosphoric acid.
Background technology
Electron-level phosphoric acid belongs to high-purity phosphoric acid, be widely used in large-scale integrated circuit, the microelectronics industry such as film liquid crystal display (TFT-LCD), be mainly used in cleaning and the etching of chip, its purity and the cleanliness factor yield rate to electronic devices and components, conductivity and reliability have a significant impact, the cleaning of what purity was lower be mainly used in liquid crystal panel parts, cleaning and the etching of electronic wafer production process that what purity was higher be mainly used in, due to insoluble solid particle or metal ion all may be between fine circuits On current, make it short circuit, so electron-level phosphoric acid has harsh requirement to insoluble solid particle and most metal ion content.
Owing to requiring in electron-level phosphoric acid, impurity metal ion content is few, and separating difficulty is larger, conventionally prepares electron-level phosphoric acid taking the PHOSPHORIC ACID TECH.GRADE of food grade phosphoric acid or preliminary purification as raw material.At present, the purifying method of phosphoric acid one have: solvent extration, ion exchange method, electroosmose process, crystallization process etc.Compared with other several method, crystallization process has that energy consumption is low, equipment is simple, running cost is little, pollute little advantage, and product purity is high simultaneously, and colourity is good, is used as primary study method prepared by electron-level phosphoric acid always.
Chinese patent 200610013611.5 use preparing electronic-grade phosphoric acid via melting-crystallizations, at-45～-35 DEG C, wall built-up produces kind and is then warming up to-2～-10 DEG C, circulation adds raw material to make it grow to when thickness reaches 2～4cm and start to heat up at plane of crystal, get rid of when liquid mass is 10～40% and stop, productive rate is 12～20%.This method service temperature is extremely low, and energy consumption is large, and need to carry out pre-treatment to raw material and remove arsenic, and the operating time is long, and production cost is high, and productive rate is low.
Chinese patent 201010100473.0 use preparing highly-pure phosphoric acid by flow chromatographic crystallization method, adopt additional sound field to produce, to raw materials used purity requirement high (major impurity ionic concn is all less than 1.7mg/L, and needs micro-pore-film filtration processing), application difficulty is larger, is not easy to industrialization.
Chinese patent 201010104321.8 adopts liquid membrane crystal legal system for electron-level phosphoric acid, on the wall of 10～20 DEG C, add kind to start cooling simultaneously, by sparger, raw material phosphor acid solution body is added on wall, raw material is liquid film state and flows through kind, grow into epitaxial at wall, reach 5～10 DEG C, terminal of cooling and start the sweating that heats up after mother liquor is fully got rid of,, stop when the sweating to 15～29 DEG C.The method is a dynamic crystallization operation process, and crystalline mother solution is not discharged immediately.By disposable decrease temperature crystalline---constant temperature discharge opeing---intensification thermal treatment carrys out refined product.This method has been improved kind producing method, and service temperature is brought up to easy to reach interval, twice crystallization yields 20～30%.But, Na, Al, Mg, Cr plasma concentration higher (1.79mg/L, 0.94mg/L, 0.49mg/L, 0.37mg/L) in the electron-level phosphoric acid preparing by the method, can not meet the demand that user upgrades day by day, still need further improvement.
Summary of the invention
Of the present inventionly overcome the problem existing in existing phosphoric acid crystallization and purification technology, the separating effect of a kind of crystallization velocity that can improve phosphoric acid and crystalline substance, liquid two-phase is provided, and the production method of the low electron-level phosphoric acid that consumes energy.
Technical scheme of the present invention is as follows:
A production method for high purity electron-level phosphoric acid, it comprises into acid, adds kind, stirred crystallization, vacuum filtration, washes crystalline substance, the operation of molten crystalline substance and acid adjustment, concrete operation step is as follows:
(1) crystallization: raw material acid is delivered in the stirred type crystallizer with chuck, starts stirred type crystallizer, pass into heat-eliminating medium to chuck; Introduce half water phosphoric acid crystal as kind, it is thrown and spread to raw material acid by 5 ‰ of raw material acid weight～10 ‰, bring out crystallization, start to grow up to sand shape crystal;
(2) discharge opeing: continue to pass into heat-eliminating medium to chuck, until crystal area proportion while reaching 30～60%, stops passing into heat-eliminating medium, and discharges mother liquor, be delivered on phosphoric acid production line;
(3) vacuum filtration: after most of mother liquor drains substantially, open vacuum pump and carry out vacuumizing filtration, thoroughly separate crystalline phase and liquid phase;
(4) wash crystalline substance: open and wash brilliant device, with washing liquid phase remaining in brilliant liquid spray washing plane of crystal and stirred type crystallizer, liquid phase is drained;
(5) molten brilliant: in chuck, to pass into hot water, melt crystalline substance, obtain melting acid;
(6) acid adjustment: get melting acid sample and do ICP-MS detection, the phosphoric acid that detects each metallic impurity qualified through ICP-MS is delivered in acid-regulating tank, regulate temperature and the concentration of phosphoric acid to make finished product phosphoric acid; If defective, be delivered in stirred type crystallizer and start to carry out secondary crystal circulation from step (1).
Above-described raw material acid is phosphoric acid, and the mass concentration of phosphoric acid is 86～88%, and controlling temperature is 26～30 DEG C.
Above-described heat-eliminating medium is cool brine or frozen water; The temperature of described heat-eliminating medium is-15～0 DEG C.
It is above-described that to wash brilliant liquid be ultrapure water or diluted acid.
Above-described diluted acid is the finished product phosphoric acid that in step (6), acid adjustment makes.
Hot water control temperature in above-described step (5) is 40～80 DEG C.
In above-described step (6), the temperature of qualified phosphoric acid is adjusted to >=40 DEG C; Regulate phosphoric acid concentration by demand.
With respect to prior art, the present invention has following advantage and positively effect:
1, the present invention, by adopting the mode of stirred crystallization in stirred type crystallizer to make phosphoric acid form husky granular crystal, improves the exchange rate of phosphoric acid and heat-eliminating medium, accelerates the speed of crystallization; Stir the molten brilliant speed of also having accelerated molten crystalline substance, significantly shortened the production cycle of electron-level phosphoric acid, greatly improved production efficiency.
2, the present invention adopts the mode of vacuumizing filtration by more thorough, quick separation brilliant, liquid two-phase, improves the refining effect of crystallization.
3, the present invention adopts and washes brilliant device to liquid phase spray washing remaining in plane of crystal and stirred type crystallizer and get rid of, and has avoided the situation of liquid phase that foreign matter content is higher and the miscible quality product decline causing of pure crystal.
4, the hot water temperature that the present invention adopts is low, can effectively utilize yellow phosphorus burning waste heat, reduces the production energy consumption of electron-level phosphoric acid, has good economic benefit.
Brief description of the drawings
Fig. 1 is process flow diagram of the present invention.
Embodiment
Below in conjunction with the drawings and specific embodiments, the invention will be further described.
Embodiment 1:
A production method for high purity electron-level phosphoric acid, is 86% by mass concentration, and temperature is that the phosphoric acid of 26 DEG C is delivered in the stirred type crystallizer with chuck as raw material acid, starts stirred type crystallizer, and passing into temperature to chuck is the cool brine of-15 DEG C; Introduce half water phosphoric acid crystal as kind, it is thrown and spread to raw material acid by 5 ‰ of raw material acid weight, bring out crystallization, start to grow up to sand shape crystal.Continue to pass into the cool brine of-15 DEG C to chuck, after crystallization 3h, when crystal area proportion reaches 30%, stop passing into cool brine, and discharge mother liquor, mother liquor is delivered on phosphoric acid production line; After most of mother liquor drains substantially, open vacuum pump and carry out vacuumizing filtration, thoroughly separate crystalline phase and liquid phase; Open and wash brilliant device, by liquid phase remaining in ultrapure water spray washing plane of crystal and stirred type crystallizer, liquid phase is drained; Be the hot water of 40 DEG C to passing into temperature in chuck, melt brilliantly, obtain melting acid; Get melting acid sample and do ICP-MS detection, the phosphoric acid that detects each metallic impurity qualified through ICP-MS is delivered in acid-regulating tank, regulate the temperature of phosphoric acid to be adjusted to 40 DEG C, regulating phosphoric acid concentration by demand is 75%, makes finished product electron-level phosphoric acid; To detect the underproof phosphoric acid modulation quality of each metallic impurity index concentration through ICP-MS is 86～88% as raw material acid, is delivered to and in stirred type crystallizer, starts to carry out secondary crystal circulation.
Embodiment 2:
A production method for high purity electron-level phosphoric acid, is 87% by mass concentration, and temperature is that the phosphoric acid of 28 DEG C is delivered in the stirred type crystallizer with chuck as raw material acid, starts stirred type crystallizer, and passing into temperature to chuck is the cool brine circulating cooling of-10 DEG C; Introduce half water phosphoric acid crystal as crystal seed, it is thrown and spread to raw material acid by 8 ‰ of raw material acid weight, bring out crystallization, start to grow up to sand shape crystal.Continue to pass into the cool brine of-10 DEG C to chuck, after crystallisation by cooling 4h, when crystal area proportion reaches 40%, stop passing into cool brine, and discharge mother liquor, mother liquor is delivered on phosphoric acid production line.After most of mother liquor drains substantially, open vacuum pump and carry out vacuumizing filtration, thoroughly separate crystalline phase and liquid phase; Open and wash brilliant device, by liquid phase remaining in ultrapure water spray washing plane of crystal and stirred type crystallizer, liquid phase is drained; Be the hot water of 60 DEG C to passing into temperature in chuck, melt brilliantly, obtain melting acid; Get melting acid sample and be ICP-MS and detect, the phosphoric acid that detects each metallic impurity qualified through ICP-MS is delivered in acid-regulating tank, regulate the temperature of phosphoric acid to be adjusted to 50 DEG C, regulating phosphoric acid quality concentration is 87% electron-level phosphoric acid that gets product.To detect the underproof phosphoric acid modulation quality of each metallic impurity index concentration through ICP-MS is 86 ~ 88% as raw material acid, is delivered to and in stirred type crystallizer, starts to carry out secondary crystal circulation.By underproof each part metallic impurity index phosphoric acid modulation diluted acid, as the brilliant liquid of washing in secondary crystal, the liquid phase of remnants in spray washing plane of crystal and stirred type crystallizer.
Embodiment 3:
A production method for high purity electron-level phosphoric acid, is 87% by mass concentration, and temperature is that the phosphoric acid of 29 DEG C is delivered in the stirred type crystallizer with chuck as raw material acid, starts stirred type crystallizer, and passing into temperature to chuck is that the ice water circulation of-5 DEG C is cooling; Introduce half water phosphoric acid crystal as kind, it is thrown and spread to raw material acid by 8 ‰ of raw material acid weight, bring out crystallization, start to grow up to sand shape crystal.Continue to pass into the frozen water of-5 DEG C to chuck, after crystallisation by cooling 4h, when crystal area proportion reaches 50%, stop passing into frozen water, and discharge mother liquor, mother liquor is delivered on phosphoric acid production line.After most of mother liquor drains substantially, open vacuum pump and carry out vacuumizing filtration, thoroughly separate crystalline phase and liquid phase; Open and wash brilliant device, by liquid phase remaining in ultrapure water spray washing plane of crystal and stirred type crystallizer, liquid phase is drained; Be the hot water of 70 DEG C to passing into temperature in chuck, melt brilliantly, obtain melting acid; Get melting acid sample and be ICP-MS and detect, the phosphoric acid that detects each metallic impurity qualified through ICP-MS is delivered in acid-regulating tank, regulate the temperature of phosphoric acid to be adjusted to 60 DEG C, regulating phosphoric acid quality concentration is 87% electron-level phosphoric acid that gets product.To detect the underproof phosphoric acid modulation quality of each metallic impurity index concentration through ICP-MS is 86～88% as raw material acid, is delivered to and in stirred type crystallizer, starts to carry out secondary crystal circulation.By underproof each part metallic impurity index phosphoric acid modulation diluted acid, as the brilliant liquid of washing in secondary crystal, the liquid phase of remnants in spray washing plane of crystal and stirred type crystallizer.
Embodiment 4:
A production method for high purity electron-level phosphoric acid, is 88% by mass concentration, and temperature is that the phosphoric acid of 30 DEG C is delivered in the stirred type crystallizer with chuck as raw material acid, starts stirred type crystallizer, and passing into temperature to chuck is the frozen water of 0 DEG C; Introduce half water phosphoric acid crystal as kind, it is thrown and spread to raw material acid by 10 ‰ of raw material acid weight, bring out crystallization, start to grow up to sand shape crystal.Continue to pass into the frozen water of-0 DEG C to chuck, after crystallisation by cooling 4h, when crystal area proportion reaches 60%, stop passing into frozen water, and discharge mother liquor, mother liquor is delivered on phosphoric acid production line; After most of mother liquor drains substantially, open vacuum pump and carry out vacuumizing filtration, thoroughly separate crystalline phase and liquid phase; Open and wash brilliant device, by liquid phase remaining in ultrapure water spray washing plane of crystal and stirred type crystallizer, liquid phase is drained; Be the hot water of 80 DEG C to passing into temperature in chuck, melt brilliantly, obtain melting acid; Get melting acid sample and do ICP-MS detection, the phosphoric acid that detects each metallic impurity qualified through ICP-MS is delivered in acid-regulating tank, regulate the temperature of phosphoric acid to be adjusted to 60 DEG C, regulating phosphoric acid concentration is 85%, makes finished product electron-level phosphoric acid.
Claims (7)
1. a production method for high purity electron-level phosphoric acid, is characterized in that: it comprises into acid, adds crystal seed, stirred crystallization, and vacuum filtration, washes crystalline substance, the operation of molten crystalline substance and acid adjustment, concrete operation step is as follows:
(1) crystallization: raw material acid is delivered in the stirred type crystallizer with chuck, starts stirred type crystallizer, pass into heat-eliminating medium to chuck; Introduce half water phosphoric acid crystal as crystal seed, throw and spread to raw material acid by 5 ‰ of raw material acid weight ~ 10 ‰, bring out crystallization, start to grow up to sand shape crystal;
(2) discharge opeing: continue to pass into heat-eliminating medium to chuck, until crystal area proportion while reaching 30 ~ 60%, stops passing into heat-eliminating medium, and discharges mother liquor, be delivered on phosphoric acid production line;
(3) vacuum filtration: after most of mother liquor drains substantially, open vacuum pump and carry out vacuumizing filtration, thoroughly separate crystalline phase and liquid phase;
(4) wash crystalline substance: open and wash brilliant device, with washing liquid phase remaining in brilliant liquid spray washing plane of crystal and stirred type crystallizer, liquid phase is drained;
(5) molten brilliant: in chuck, to pass into hot water, melt crystalline substance, obtain melting acid;
(6) acid adjustment: get melting acid sample and do ICP-MS detection, the phosphoric acid that detects each metallic impurity qualified through ICP-MS is delivered in acid-regulating tank, regulate temperature and the concentration of phosphoric acid to make finished product phosphoric acid; If defective, be delivered in stirred type crystallizer and start to carry out secondary crystal circulation from step (1).
2. the production method of a kind of high purity electron-level phosphoric acid according to claim 1, is characterized in that: described raw material acid is phosphoric acid, and the mass concentration of phosphoric acid is 86 ~ 88%, and controlling temperature is 26 ~ 30 DEG C.
3. the production method of a kind of high purity electron-level phosphoric acid according to claim 1, is characterized in that: described heat-eliminating medium is cool brine or frozen water; The temperature of described heat-eliminating medium is-15 ~ 0 DEG C.
4. the production method of a kind of high purity electron-level phosphoric acid according to claim 1, is characterized in that: the described brilliant liquid of washing is ultrapure water or diluted acid.
5. the production method of a kind of high purity electron-level phosphoric acid according to claim 4, is characterized in that: described diluted acid is the finished product phosphoric acid that in step (6), acid adjustment makes.
6. the production method of a kind of high purity electron-level phosphoric acid according to claim 1, is characterized in that: the hot water control temperature in described step (5) is 40 ~ 80 DEG C.
7. the production method of a kind of high purity electron-level phosphoric acid according to claim 1, is characterized in that: in described step (6), the temperature of qualified phosphoric acid is adjusted to >=40 DEG C; Regulate phosphoric acid concentration by demand.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105366656A (en) * | 2015-12-10 | 2016-03-02 | 四川蓝海化工（集团）有限公司 | Purification method of capacitor grade phosphoric acid |
| CN108275669A (en) * | 2018-01-16 | 2018-07-13 | 湖北兴福电子材料有限公司 | A kind of method of electron-level phosphoric acid removing penetrating odor |
| CN110255519A (en) * | 2019-07-17 | 2019-09-20 | 南京化学试剂股份有限公司 | A kind of purification process of pharmaceutical grade phosphoric acid |
| CN111342097A (en) * | 2018-12-18 | 2020-06-26 | 中国科学院大连化学物理研究所 | Preparation method of electrolyte membrane with high conductivity and good mechanical property |
| CN116354321A (en) * | 2023-03-27 | 2023-06-30 | 湖北兴福电子材料股份有限公司 | Industrial method and device for purifying electronic grade phosphoric acid through crystallization |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4655790A (en) * | 1985-05-08 | 1987-04-07 | Freeport Research And Development Company | Phosphoric acid crystallization process |
| CN1843900A (en) * | 2006-05-08 | 2006-10-11 | 朱健 | Method for preparing electronic grade phosphoric acid by fusion crystallization method |
| CN1850590A (en) * | 2006-05-25 | 2006-10-25 | 贵州宏福实业开发有限总公司 | Method for producing electron-level phosphoric acid |
| CN102020255A (en) * | 2010-04-29 | 2011-04-20 | 杨志勇 | Semi-continuous and multi-variety high-purity electronic grade phosphoric acid production process and equipment |
| CN102730654A (en) * | 2011-04-14 | 2012-10-17 | 罗培华 | Production method of ultra-pure electronic grade phosphoric acid |
-
2013
- 2013-12-30 CN CN201310744485.0A patent/CN104030261B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4655790A (en) * | 1985-05-08 | 1987-04-07 | Freeport Research And Development Company | Phosphoric acid crystallization process |
| CN1843900A (en) * | 2006-05-08 | 2006-10-11 | 朱健 | Method for preparing electronic grade phosphoric acid by fusion crystallization method |
| CN1850590A (en) * | 2006-05-25 | 2006-10-25 | 贵州宏福实业开发有限总公司 | Method for producing electron-level phosphoric acid |
| CN102020255A (en) * | 2010-04-29 | 2011-04-20 | 杨志勇 | Semi-continuous and multi-variety high-purity electronic grade phosphoric acid production process and equipment |
| CN102730654A (en) * | 2011-04-14 | 2012-10-17 | 罗培华 | Production method of ultra-pure electronic grade phosphoric acid |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105366656A (en) * | 2015-12-10 | 2016-03-02 | 四川蓝海化工（集团）有限公司 | Purification method of capacitor grade phosphoric acid |
| CN108275669A (en) * | 2018-01-16 | 2018-07-13 | 湖北兴福电子材料有限公司 | A kind of method of electron-level phosphoric acid removing penetrating odor |
| CN111342097A (en) * | 2018-12-18 | 2020-06-26 | 中国科学院大连化学物理研究所 | Preparation method of electrolyte membrane with high conductivity and good mechanical property |
| CN110255519A (en) * | 2019-07-17 | 2019-09-20 | 南京化学试剂股份有限公司 | A kind of purification process of pharmaceutical grade phosphoric acid |
| CN116354321A (en) * | 2023-03-27 | 2023-06-30 | 湖北兴福电子材料股份有限公司 | Industrial method and device for purifying electronic grade phosphoric acid through crystallization |
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| CN104030261B (en) | 2016-01-27 |
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