CN104030261B - A kind of production method of high purity electron-level phosphoric acid - Google Patents
A kind of production method of high purity electron-level phosphoric acid Download PDFInfo
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- CN104030261B CN104030261B CN201310744485.0A CN201310744485A CN104030261B CN 104030261 B CN104030261 B CN 104030261B CN 201310744485 A CN201310744485 A CN 201310744485A CN 104030261 B CN104030261 B CN 104030261B
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- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 title claims abstract description 188
- 229910000147 aluminium phosphate Inorganic materials 0.000 title claims abstract description 93
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 32
- 239000013078 crystal Substances 0.000 claims abstract description 52
- 239000002253 acid Substances 0.000 claims abstract description 51
- 239000002994 raw material Substances 0.000 claims abstract description 30
- 238000002425 crystallisation Methods 0.000 claims abstract description 28
- 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 17
- 239000007788 liquid Substances 0.000 claims abstract description 14
- 239000000126 substance Substances 0.000 claims abstract description 14
- 238000001914 filtration Methods 0.000 claims abstract description 9
- 239000007791 liquid phase Substances 0.000 claims description 22
- 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
- 238000002844 melting Methods 0.000 claims description 12
- 230000008018 melting Effects 0.000 claims description 12
- 239000007921 spray Substances 0.000 claims description 9
- 239000012267 brine Substances 0.000 claims description 8
- 239000012071 phase 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
- 230000001105 regulatory effect Effects 0.000 claims description 2
- RAHZWNYVWXNFOC-UHFFFAOYSA-N Sulphur dioxide Chemical compound O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 abstract description 4
- 230000008901 benefit Effects 0.000 abstract description 4
- 238000003756 stirring Methods 0.000 abstract description 3
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 abstract description 2
- 238000000926 separation method Methods 0.000 abstract description 2
- 235000010269 sulphur dioxide Nutrition 0.000 abstract description 2
- 239000004291 sulphur dioxide Substances 0.000 abstract description 2
- 230000004927 fusion Effects 0.000 abstract 1
- 238000010438 heat treatment Methods 0.000 abstract 1
- 238000000034 method Methods 0.000 description 14
- 238000001816 cooling Methods 0.000 description 7
- 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
- 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
- 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
- 239000002904 solvent 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
Abstract
The invention discloses a kind of production method of high purity electron-level phosphoric acid, belong to phosphoric acid production technical field in sulphur dioxide of phosphor chemical industry.The present invention includes and add raw material acid to stirred type crystallizer, add crystal seed, stirred crystallization to 30 ~ 60%, vacuumizing filtration makes crystalline substance, liquid two-phase carries out washing crystalline substance after being thoroughly separated, stir molten brilliant with chuck hot water heating, the operation of product is made in last acid adjustment.The present invention adopts the mode of stirred crystallization to make phosphoric acid form husky granular crystal, improves the exchange rate of phosphoric acid and heat-eliminating medium, accelerates the speed of crystallization; Employing vacuumizes the mode being pumped through filter makes the separation of crystalline substance, liquid two-phase more thoroughly, fast, stir the molten brilliant speed also accelerating crystalline fusion, therefore significantly shorten the production cycle of electron-level phosphoric acid, substantially increase production efficiency, there is 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 cleanliness factor are to the yield rate of 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 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 impurity metal ion content few in electron-level phosphoric acid, separating difficulty is comparatively large, usually with the PHOSPHORIC ACID TECH.GRADE of food grade phosphoric acid or preliminary purification for electron-level phosphoric acid prepared by raw material.At present, the purifying method of phosphoric acid generally has: 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, always by the primary study method prepared as electron-level phosphoric acid.
Chinese patent 200610013611.5 preparing electronic-grade phosphoric acid via melting-crystallization, at-45 ~-35 DEG C, wall built-up produces crystal seed and is then warming up to-2 ~-10 DEG C, circulation adds raw material to be made it grow at plane of crystal to start when thickness reaches 2 ~ 4cm to heat up, eliminating liquid mass stops when being 10 ~ 40%, and productive rate is 12 ~ 20%.This method service temperature is extremely low, and energy consumption is large, and needs to carry out pre-treatment removing arsenic to raw material, and the operating time is long, and production cost is high, and productive rate is low.
Chinese patent 201010100473.0 preparing highly-pure phosphoric acid by flow chromatographic crystallization method, additional sound field is adopted to go out crystalline substance, to raw materials used purity requirement high (major impurity ionic concn is all less than 1.7mg/L, and needs micro-pore-film filtration process), application difficulty is comparatively large, is not easy to industrialization.
Chinese patent 201010104321.8 adopts liquid membrane crystal legal system for electron-level phosphoric acid, the wall of 10 ~ 20 DEG C adds crystal seed and starts cooling simultaneously, by sparger, raw material phosphoric acid liquid is added on wall, raw material is that liquid film state flows through crystal seed, epitaxial is grown at wall, reach cooling 5 ~ 10 DEG C, terminal and start the sweating that heats up after mother liquor is fully got rid of, stop during sweating to 15 ~ 29 DEG C.The method is a dynamic crystallization operation process, and non-crystalline mother solution is discharged immediately.By disposable decrease temperature crystalline---constant temperature discharge opeing---intensification thermal treatment carrys out refined product.This method improves crystal seed producing method, 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), can not meet the demand that user upgrades day by day, still need further improvement in the electron-level phosphoric acid prepared by the method.
Summary of the invention
Of the present inventionly overcome Problems existing in existing phosphoric acid crystallization and purification technology, provide a kind of can improve phosphoric acid crystallization velocity and crystalline substance, liquid two-phase separating effect, 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 crystal seed, stirred crystallization, and crystalline substance is washed in vacuum filtration, the operation of molten crystalline substance and acid adjustment, and concrete operation step is as follows:
(1) crystallization: raw material acid be delivered in the stirred type crystallizer with chuck, starts stirred type crystallizer, passes into heat-eliminating medium to chuck; Introduce half water phosphoric acid crystal as crystal seed, throw by 5 ‰ ~ 10 ‰ of raw material acid weight and spread in raw material acid, bring out crystallization, start to grow up to sand shape crystal;
(2) discharge opeing: continue to pass into heat-eliminating medium to chuck, until when crystal area proportion reaches 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, opens vacuum pump and carries out vacuumizing filtration, be thoroughly separated crystalline phase and liquid phase;
(4) washing 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 being drained;
(5) molten brilliant: in chuck, to pass into hot water, carry out molten brilliant, obtain melting acid;
(6) acid adjustment: get melting acid sample and do ICP-MS detection, the phosphoric acid detecting each metallic impurity qualified is delivered in acid-regulating tank, regulates the temperature and concentration of phosphoric acid to obtain finished product phosphoric acid through ICP-MS; If defective, be then delivered in stirred type crystallizer and 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 control 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 is obtained.
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; Phosphoric acid concentration is regulated by demand.
Relative to prior art, the present invention has following advantage and positively effect:
1, the present invention makes phosphoric acid form husky granular crystal by adopting the mode of stirred crystallization in stirred type crystallizer, improves the exchange rate of phosphoric acid and heat-eliminating medium, accelerates the speed of crystallization; Stir the molten brilliant speed also accelerating molten crystalline substance, significantly shorten the production cycle of electron-level phosphoric acid, substantially increase production efficiency.
2, the present invention adopts the mode of vacuumizing filtration by more thorough, quick for separation that is 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 avoids the situation that the higher liquid phase of foreign matter content and the miscible quality product caused of clean crystals decline.
4, the hot water temperature of the present invention's employing is low, can effectively utilize yellow phosphorus burning waste heat, reduces the production energy consumption of electron-level phosphoric acid, has good economic benefit.
Accompanying drawing explanation
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:
Mass concentration is 86% by a production method for high purity electron-level phosphoric acid, 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, passes into chuck the cool brine that temperature is-15 DEG C; Introduce half water phosphoric acid crystal as crystal seed, it is thrown by 5 ‰ of raw material acid weight and spreads in raw material acid, bring out crystallization, start to grow up to sand shape crystal.Continue the cool brine passing into-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, be thoroughly separated 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; In chuck, pass into the hot water that temperature is 40 DEG C, carry out molten brilliant, obtain melting acid; Get melting acid sample and do ICP-MS detection, the phosphoric acid detecting each metallic impurity qualified is delivered in acid-regulating tank, regulates the temperature of phosphoric acid to be adjusted to 40 DEG C, regulate phosphoric acid concentration to be 75% by demand, obtained completed electronic level phosphoric acid through ICP-MS; To detect each metallic impurity index underproof phosphoric acid modulation quality concentration through ICP-MS is 86 ~ 88% as raw material acid, is delivered in stirred type crystallizer and starts to carry out secondary crystal circulation.
Embodiment 2:
Mass concentration is 87% by a production method for high purity electron-level phosphoric acid, 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, passes into chuck the cool brine circulating cooling that temperature is-10 DEG C; Introduce half water phosphoric acid crystal as crystal seed, it is thrown by 8 ‰ of raw material acid weight and spreads in raw material acid, bring out crystallization, start to grow up to sand shape crystal.Continue the cool brine passing into-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, be thoroughly separated 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; In chuck, pass into the hot water that temperature is 60 DEG C, carry out molten brilliant, obtain melting acid; Get melting acid sample to be ICP-MS and to detect, the phosphoric acid detecting each metallic impurity qualified is delivered in acid-regulating tank, regulates the temperature of phosphoric acid to be adjusted to 50 DEG C through ICP-MS, regulate phosphoric acid quality concentration to be 87% to get product electron-level phosphoric acid.To detect each metallic impurity index underproof phosphoric acid modulation quality concentration through ICP-MS is 86 ~ 88% as raw material acid, is delivered in stirred type crystallizer and starts to carry out secondary crystal circulation.By underproof for each for part metallic impurity index phosphoric acid modulation diluted acid, as washing brilliant liquid in secondary crystal, liquid phase remaining in spray washing plane of crystal and stirred type crystallizer.
Embodiment 3:
Mass concentration is 87% by a production method for high purity electron-level phosphoric acid, 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, passes into chuck the ice water circulation cooling that temperature is-5 DEG C; Introduce half water phosphoric acid crystal as crystal seed, it is thrown by 8 ‰ of raw material acid weight and spreads in raw material acid, bring out crystallization, start to grow up to sand shape crystal.Continue the frozen water passing into-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, be thoroughly separated 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; In chuck, pass into the hot water that temperature is 70 DEG C, carry out molten brilliant, obtain melting acid; Get melting acid sample to be ICP-MS and to detect, the phosphoric acid detecting each metallic impurity qualified is delivered in acid-regulating tank, regulates the temperature of phosphoric acid to be adjusted to 60 DEG C through ICP-MS, regulate phosphoric acid quality concentration to be 87% to get product electron-level phosphoric acid.To detect each metallic impurity index underproof phosphoric acid modulation quality concentration through ICP-MS is 86 ~ 88% as raw material acid, is delivered in stirred type crystallizer and starts to carry out secondary crystal circulation.By underproof for each for part metallic impurity index phosphoric acid modulation diluted acid, as washing brilliant liquid in secondary crystal, liquid phase remaining in spray washing plane of crystal and stirred type crystallizer.
Embodiment 4:
Mass concentration is 88% by a production method for high purity electron-level phosphoric acid, 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, passes into chuck the frozen water that temperature is 0 DEG C; Introduce half water phosphoric acid crystal as crystal seed, it is thrown by 10 ‰ of raw material acid weight and spreads in raw material acid, bring out crystallization, start to grow up to sand shape crystal.Continue the frozen water passing into-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, be thoroughly separated 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; In chuck, pass into the hot water that temperature is 80 DEG C, carry out molten brilliant, obtain melting acid; Get melting acid sample and do ICP-MS detection, the phosphoric acid detecting each metallic impurity qualified is delivered in acid-regulating tank, regulates the temperature of phosphoric acid to be adjusted to 60 DEG C, regulate phosphoric acid concentration to be 85%, obtained completed electronic level phosphoric acid through ICP-MS.
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 crystalline substance is washed in vacuum filtration, the operation of molten crystalline substance and acid adjustment, and concrete operation step is as follows:
Crystallization: raw material acid be delivered in the stirred type crystallizer with chuck, starts stirred type crystallizer, passes into heat-eliminating medium to chuck; Introduce half water phosphoric acid crystal as crystal seed, throw by 5 ‰ ~ 10 ‰ of raw material acid weight and spread in raw material acid, bring out crystallization, start to grow up to sand shape crystal;
Discharge opeing: continue to pass into heat-eliminating medium to chuck, until when crystal area proportion reaches 30 ~ 60%, stops passing into heat-eliminating medium, and discharges mother liquor, be delivered on phosphoric acid production line;
Vacuum filtration: after most of mother liquor drains, opens vacuum pump and carries out vacuumizing filtration, be thoroughly separated crystalline phase and liquid phase;
Washing 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 being drained;
Molten brilliant: in chuck, to pass into hot water, carry out molten brilliant, obtain melting acid;
Acid adjustment: get melting acid sample and do ICP-MS detection, the phosphoric acid detecting each metallic impurity qualified is delivered in acid-regulating tank, regulates the temperature and concentration of phosphoric acid to obtain finished product phosphoric acid through ICP-MS; If defective, be then delivered in stirred type crystallizer and 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, the mass concentration of phosphoric acid is 86 ~ 88%, and control 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: 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 is obtained.
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; Phosphoric acid concentration is regulated by demand.
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| 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 |
| CN108275669B (en) * | 2018-01-16 | 2021-12-03 | 湖北兴福电子材料有限公司 | Method for removing irritant odor of electronic 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 |
| 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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| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
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2013
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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 |
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