CN202063718U - Production device for ultrahigh-purity electronic-grade phosphoric acid - Google Patents
Production device for ultrahigh-purity electronic-grade phosphoric acid Download PDFInfo
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- CN202063718U CN202063718U CN2011201085422U CN201120108542U CN202063718U CN 202063718 U CN202063718 U CN 202063718U CN 2011201085422 U CN2011201085422 U CN 2011201085422U CN 201120108542 U CN201120108542 U CN 201120108542U CN 202063718 U CN202063718 U CN 202063718U
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- phosphoric acid
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Abstract
The utility model discloses a production device for ultrahigh-purity electronic-grade phosphoric acid, which comprises a phosphorus-oxychloride storing tank (23), a phosphorus-oxychloride steam generator (7), a vapor generator (6), a phosphoric-acid generator (1) with a liquid-collecting slot (8), a dechlorinating device (2), a phosphoric-acid storing slot (9), a vacuum pump (22), a hydrochloric-acid liquid collector (3) with a mother-liquid slot (11), a hydrochloric-acid evaporator (10), a hydrochloric-acid absorber (4) with a circulating slot (16), a heat exchanger (17), a circulating pump (18), a hydrochloric-acid storing slot (13), a tail-gas draught fan (24), a tail-gas tower (5) and connecting pipelines. The production device for the ultrahigh-purity electronic-grade phosphoric acid has the advantages that: 1. a system is closed, and an environment has no influence on the purity of a product; 2. the proportion of vapor and phosphorus-oxychloride steam is effectively controlled, the concentration of phosphoric acid is regulated, and the consumed energy for high-purity phosphoric-acid concentration is reduced; 3. the hydrochloric-acid content in the phosphoric acid and the phosphoric-acid content in the hydrochloric acid are effectively inhibited, and the time and the energy consumption of phosphoric-acid dechlorinating and hydrochloric-acid dephosphorizing working procedures are saved; and 4. the effective contact surface of the vapor and the phosphorus-oxychloride steam in the phosphoric-acid generator is large. The production device for the ultrahigh-purity electronic-grade phosphoric acid is suitable for producing the ultrahigh-purity electronic-grade phosphoric acid by using high-purity phosphorus trichloride.
Description
Technical field
The utility model relates to phosphoric acid, specifically, relates to the production equipment of ultra-pure electron-level phosphoric acid.
Background technology
The required phosphoric acid purity requirement of production of general production of integrated circuits and TFT-LCD liquid-crystal display is not high, and nonmetallic ion content is not higher than 12 * 10
-6(being 12ppm), metal ion is no more than 1100 * 10
-9(being 1100ppb), quality product reach SEMI grade 2 standards and get final product.But making requires quality index must reach SEMI grade 3 for large-scale integrated circuit, and required phosphoric acid requires rank higher in high-end chip manufacturing and the phosphorus source doping, and its metals content impurity is no more than 10 * 10
-9(being 10ppb).The present domestic production technique of producing SEMI grade 2 super high pured phosphoric acids, most indexs progressively approach SEMI grade 3 standards, and metal ion content is no more than 250 * 10
-9(being 250ppb), its preparation method is to improve on wet phosphoric acid purifying method for refining, the thermal phosphoric acid method of purification, crystallization legal system pure phosphoric acid, electrolytic cleaning method and the methods such as ion-exchange and electroosmotic drainage and realizes, all can not satisfy the requirement of high-end microelectronics industry, especially can not satisfy super large-scale integration and chip manufacturing demand, more can not use as the Doping Phosphorus source.Also useful abroad phosphoric acid prepares the technology of super high pured phosphoric acid, but all adopts the method for multiple working procedure purification to carry out, and is not that direct production obtains.Japanese Patent (publication number: 2000-239008) on September 5th, 2000 disclose high-purity phosphorus oxychloride add make its hydrolysis in the pure water and concentrate its hydrolysate after, obtain metal ion content and be no more than 10 * 10
-9The high-purity phosphoric acid production method.But its method reaction is fierce, inconvenience control, and the water yield is excessive in the phosphoric acid, and hydrogen chloride content is higher, need deviate from a large amount of hydrogenchloride and water, and energy consumption is too high.
Summary of the invention
The purpose of this utility model is to provide a kind of production equipment of ultra-pure electron-level phosphoric acid, to solve the plant issue that ultra-pure electron-level phosphoric acid production needs.
The production equipment of ultra-pure electron-level phosphoric acid that the designer provides is made up of salt absorber acid, interchanger, recycle pump, salt acid storage tank, tail gas induced draft fan, tail gas tower and the connecting tube of the hydrochloric acid liquid trap of the phosphoric acid producer of phosphorus oxychloride storage tank, phosphorus oxychloride steam generator, water vapour producer, band intercepting basin, chlorine purifier, phosphoric acid storage tank, vacuum pump, band mother liquor tank, hydrochloric acid vaporizer, band circulation groove; Wherein, phosphorus oxychloride storage tank, phosphorus oxychloride steam generator are successively by the middle part of pipe connection to the phosphoric acid producer; The water vapour producer is connected with the upper and lower of phosphoric acid producer respectively by pipeline; The intercepting basin of phosphoric acid producer has pipeline to be connected with chlorine purifier, and chlorine purifier is connected with phosphoric acid storage tank and vacuum pump respectively by pipeline again; Phosphoric acid producer top has pipeline to be connected with the hydrochloric acid liquid trap, and the mother liquor tank of hydrochloric acid liquid trap is connected with the salt absorber acid with the hydrochloric acid vaporizer respectively by pipeline again; The circulation groove of salt absorber acid has pipeline to connect interchanger, recycle pump successively again and gets back to the salt absorber acid, and the pipe connection tail gas induced draft fan of hydrochloric acid absorber overhead enters tail gas tower, and circulating-pump outlet has lateral to connect the salt acid storage tank.
The upper and lower of above-mentioned phosphoric acid producer has steam spray nozzle, middle part that the phosphorus oxychloride nozzle is arranged, and the fluoro-resin packing ring is arranged at top, and the top also has fluid-tight.
One steam coils is arranged in the above-mentioned chlorine purifier, be used for heating, concentrated phosphoric acid, and remove hydrogenchloride.
In the above-mentioned hydrochloric acid vaporizer steam coils is arranged, be used for adding hot mother liquor, steam hydrogen chloride gas.
The nozzle of circulation fluid is arranged at above-mentioned salt absorber acid top, and condenser is arranged at the top, and the salt acid condensation in the tail gas is got off.
Above-mentioned vacuum pump is a water-ring vacuum pump, is used for extracting the hydrogenchloride that chlorine purifier is deviate from.
Above-mentioned interchanger is a shell and tube heat exchanger, uses the cold water cooling circulation liquid.
The Production Flow Chart of the production equipment of ultra-pure electron-level phosphoric acid is: high-purity phosphorus trichloride enters the phosphorus oxychloride steam generator from storage tank, and the phosphorus oxychloride steam that steams enters the middle part of phosphoric acid producer, sprays by nozzle; Ultrapure water enters the water vapour producer, and water vapour by the nozzle ejection of the upper and lower of phosphoric acid producer, with phosphorus oxychloride steam generation hydrolysis reaction, generates super high pured phosphoric acid respectively; Super high pured phosphoric acid flows into chlorine purifier from intercepting basin, heats by steam coils to enter the phosphoric acid storage tank after deviating from hydrogenchloride, promptly obtains ultra-pure electron-level phosphoric acid; The hydrogenchloride of deviating from is extracted by vacuum pump and discharges; Reaction end gas enters the hydrochloric acid liquid trap from phosphoric acid producer top, and the mother liquor under the collection flows into the hydrochloric acid vaporizer from mother liquor tank, steams hydrogen chloride gas and sends into the salt absorber acid by heating; The hydrochloric acid that the salt absorber acid absorbs comes out to squeeze into the absorption that circulates in the resorber with recycle pump after the back reduces temperature by interchanger, absorbs to enter the hydrochloric acid storage tank after the concentration of hydrochloric acid that obtains reaches 36%, and its metallic impurity are less than 10 * 10
-9, as byproduct; Nonabsorbable tail gas is discharged by tail gas tower after removing the disacidify foam by condenser.
Compared with prior art, the utlity model has following advantage: 1. system is a closed-loop operation, and environment does not have influence to product purity; 2. can effectively control water vapour and phosphorus oxychloride vapor mixing ratio in the phosphoric acid producer, effectively adjust phosphoric acid concentration, reduce high-purity phosphoric acid and concentrate power consumption; 3. the phosphoric acid of phosphorus oxychloride hydrolysis generation and hydrogenchloride major part flow toward different directions respectively, phosphorus acid content in content of hydrochloric acid and the hydrochloric acid in effective inhibition phosphoric acid, and phosphoric acid liquid collecting under reaction heat influence, hydrochloric acid liquid collecting temperature are higher, thereby save phosphoric acid dechlorination and hydrochloric acid dephosphorization activity time and energy consumption; 4. steam and the effective contact surface of phosphorus oxychloride steam are big in the phosphoric acid producer, and on the phosphoric acid producer, phosphoric acid fluid-tight security device is set, and having overcome water and fed in phosphorus oxychloride or the phosphorus oxychloride feeding water, contact area is little, the local reaction fierceness, defective such as production security difference and efficient are low.Be applicable to high-purity phosphorus trichloride and produce ultra-pure electron-level phosphoric acid.
Description of drawings
Fig. 1 is an apparatus structure synoptic diagram of the present utility model.1 is the phosphoric acid producer among the figure, and 2 is chlorine purifier, and 3 is the hydrochloric acid liquid trap, 4 is the salt absorber acid, and 5 is tail gas tower, and 6 is the water vapour producer, 7 is the phosphorus oxychloride steam generator, and 8 is intercepting basin, and 9 is the phosphoric acid storage tank, 10 is the hydrochloric acid vaporizer, and 11 is mother liquor tank, and 12 is steam jet, 13 is the salt acid storage tank, 14 is phosphorus oxychloride steam nozzle, and 15 is the fluoro-resin packing ring, and 16 is circulation groove, 17 is interchanger, 18 is recycle pump, and 19 is the circulation fluid nozzle, and 20 is condenser, 21 are fluid-tight, 22 is vacuum pump, and 23 is the phosphorus oxychloride storage tank, and 24 is the tail gas induced draft fan.
Embodiment
As the production equipment of ultra-pure electron-level phosphoric acid of Fig. 1, form by salt absorber acid 4, interchanger 17, recycle pump 18, salt acid storage tank 13, tail gas induced draft fan 24, tail gas tower 5 and the connecting tube of the hydrochloric acid liquid trap 3 of the phosphoric acid producer 1 of phosphorus oxychloride storage tank 23, phosphorus oxychloride steam generator 7, water vapour producer 6, band intercepting basin 8, chlorine purifier 2, phosphoric acid storage tank 9, vacuum pump 22, band mother liquor tank 11, hydrochloric acid vaporizer 10, band circulation groove 16; Wherein, phosphorus oxychloride storage tank 23, phosphorus oxychloride steam generator 7 are successively by the middle part of pipe connection to phosphoric acid producer 1; Water vapour producer 6 is connected with the upper and lower of phosphoric acid producer 1 respectively by pipeline; The intercepting basin 8 of phosphoric acid producer 1 has pipeline to be connected with chlorine purifier 2, and chlorine purifier 2 is connected with phosphoric acid storage tank 9 and vacuum pump 22 respectively by pipeline again; Phosphoric acid producer 1 top has pipeline to be connected with hydrochloric acid liquid trap 3, and the mother liquor tank 11 of hydrochloric acid liquid trap 3 is connected with salt absorber acid 4 with hydrochloric acid vaporizer 10 respectively by pipeline again; The circulation groove 16 of salt absorber acid 4 has pipeline to connect interchanger 17, recycle pump 18 successively again and gets back to salt absorber acid 4, the pipe connection tail gas induced draft fan 24 at salt absorber acid 4 tops enters tail gas tower 5, and recycle pump 18 outlets have lateral to connect salt acid storage tank 13.The upper and lower of phosphoric acid producer 1 has steam spray nozzle 12, middle part that phosphorus oxychloride nozzle 14 is arranged, and fluoro-resin packing ring 15 is arranged at top, and the top also has fluid-tight 21.In the chlorine purifier 2 and in the hydrochloric acid vaporizer 10 steam coils is arranged respectively.Circulation fluid nozzle 19 is arranged at salt absorber acid 4 tops, and condenser 20 is arranged at the top.Vacuum pump 22 is water-ring vacuum pumps.Interchanger 17 is a shell and tube heat exchanger.
The diameter of phosphoric acid producer 1 is 200mm, highly is 2800mm; The diameter of hydrochloric acid liquid trap 3 is 100mm, highly is 1000mm, and the diameter of salt absorber acid 4 is 200mm, highly is 3000mm; The diameter of tail gas tower 5 is 300mm, highly is 6000mm.
Claims (5)
1. the production equipment of a ultra-pure electron-level phosphoric acid is characterized in that this device is made up of salt absorber acid (4), interchanger (17), recycle pump (18), salt acid storage tank (13), tail gas induced draft fan (24), tail gas tower (5) and the connecting tube of the hydrochloric acid liquid trap (3) of the phosphoric acid producer (1) of phosphorus oxychloride storage tank (23), phosphorus oxychloride steam generator (7), water vapour producer (6), band intercepting basin (8), chlorine purifier (2), phosphoric acid storage tank (9), vacuum pump (22), band mother liquor tank (11), hydrochloric acid vaporizer (10), band circulation groove (16); Wherein, phosphorus oxychloride storage tank (23), phosphorus oxychloride steam generator (7) arrive phosphoric acid producer (1) middle part by pipe connection; Water vapour producer (6) is connected with the upper and lower of phosphoric acid producer (1) respectively by pipeline; The intercepting basin (8) of phosphoric acid producer (1) has pipeline to be connected with chlorine purifier (2), and chlorine purifier (2) is connected with phosphoric acid storage tank (9) and vacuum pump (22) respectively by pipeline again; Phosphoric acid producer (1) top has pipeline to be connected with hydrochloric acid liquid trap (3), and the mother liquor tank (11) of hydrochloric acid liquid trap (3) is connected with salt absorber acid (4) with hydrochloric acid vaporizer (10) respectively by pipeline again; The circulation groove (16) of salt absorber acid (4) has pipeline to connect interchanger (17), recycle pump (18) successively again and gets back to salt absorber acid (4), salt absorber acid (4) top duct connects tail gas induced draft fan (24) and enters tail gas tower (5), and recycle pump (18) outlet has lateral to connect salt acid storage tank (13).
2. production equipment as claimed in claim 1 is characterized in that the upper and lower of described phosphoric acid producer (1) has steam spray nozzle (12), middle part that phosphorus oxychloride nozzle (14) is arranged, and fluoro-resin packing ring (15) is arranged at top, and the top also has fluid-tight (21).
3. production equipment as claimed in claim 1 is characterized in that in the described chlorine purifier (2) and in the hydrochloric acid vaporizer (10) steam coils being arranged respectively.
4. production equipment as claimed in claim 1 is characterized in that circulation fluid nozzle (19) is arranged at described salt absorber acid (4) top, and condenser (20) is arranged at the top.
5. production equipment as claimed in claim 1 is characterized in that described vacuum pump (22) is a water-ring vacuum pump; Described interchanger (17) is a shell and tube heat exchanger.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011201085422U CN202063718U (en) | 2011-04-14 | 2011-04-14 | Production device for ultrahigh-purity electronic-grade phosphoric acid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011201085422U CN202063718U (en) | 2011-04-14 | 2011-04-14 | Production device for ultrahigh-purity electronic-grade phosphoric acid |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN202063718U true CN202063718U (en) | 2011-12-07 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2011201085422U Expired - Fee Related CN202063718U (en) | 2011-04-14 | 2011-04-14 | Production device for ultrahigh-purity electronic-grade phosphoric acid |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105883738A (en) * | 2014-12-31 | 2016-08-24 | 杨志勇 | Semi-continuous multi-variety high-purity electronic-grade phosphoric acid production technology and device |
| CN113830744A (en) * | 2021-09-14 | 2021-12-24 | 成都市科隆化学品有限公司 | Method for efficiently concentrating and dechlorinating phosphoric acid |
-
2011
- 2011-04-14 CN CN2011201085422U patent/CN202063718U/en not_active Expired - Fee Related
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105883738A (en) * | 2014-12-31 | 2016-08-24 | 杨志勇 | Semi-continuous multi-variety high-purity electronic-grade phosphoric acid production technology and device |
| CN113830744A (en) * | 2021-09-14 | 2021-12-24 | 成都市科隆化学品有限公司 | Method for efficiently concentrating and dechlorinating phosphoric acid |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20111207 Termination date: 20160414 |