CN103896231B - The device of electron-level phosphoric acid is produced in a kind of tubulation crystallization - Google Patents
The device of electron-level phosphoric acid is produced in a kind of tubulation crystallization Download PDFInfo
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- CN103896231B CN103896231B CN201310744583.4A CN201310744583A CN103896231B CN 103896231 B CN103896231 B CN 103896231B CN 201310744583 A CN201310744583 A CN 201310744583A CN 103896231 B CN103896231 B CN 103896231B
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- acid
- pipeline
- phosphoric acid
- vertical array
- crystallizer tank
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- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 title claims abstract description 68
- 229910000147 aluminium phosphate Inorganic materials 0.000 title claims abstract description 34
- 238000002425 crystallisation Methods 0.000 title claims abstract description 18
- 230000008025 crystallization Effects 0.000 title claims abstract description 18
- 239000007921 spray Substances 0.000 claims abstract description 28
- 238000004519 manufacturing process Methods 0.000 claims abstract description 12
- 239000002253 acid Substances 0.000 claims description 40
- 230000008676 import Effects 0.000 claims description 17
- 239000013078 crystal Substances 0.000 claims description 8
- 229910001220 stainless steel Inorganic materials 0.000 claims description 8
- 239000010935 stainless steel Substances 0.000 claims description 8
- 239000000463 material Substances 0.000 claims description 5
- 238000013022 venting Methods 0.000 claims description 5
- 239000011521 glass Substances 0.000 claims description 4
- 239000012267 brine Substances 0.000 claims description 3
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 238000000034 method Methods 0.000 abstract description 10
- 230000008901 benefit Effects 0.000 abstract description 5
- 239000007791 liquid phase Substances 0.000 abstract description 5
- 239000007788 liquid Substances 0.000 abstract description 4
- 238000000746 purification Methods 0.000 abstract description 4
- 239000000126 substance Substances 0.000 abstract description 4
- 239000012071 phase Substances 0.000 abstract description 3
- 238000000926 separation method Methods 0.000 abstract 1
- OBSZRRSYVTXPNB-UHFFFAOYSA-N tetraphosphorus Chemical compound P12P3P1P32 OBSZRRSYVTXPNB-UHFFFAOYSA-N 0.000 description 5
- GNTDGMZSJNCJKK-UHFFFAOYSA-N divanadium pentaoxide Chemical compound O=[V](=O)O[V](=O)=O GNTDGMZSJNCJKK-UHFFFAOYSA-N 0.000 description 4
- 238000004140 cleaning Methods 0.000 description 3
- 229910021645 metal ion Inorganic materials 0.000 description 3
- 238000005265 energy consumption 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
- 239000007787 solid Substances 0.000 description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000003749 cleanliness Effects 0.000 description 1
- 238000005049 combustion synthesis Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 230000035900 sweating Effects 0.000 description 1
- 229910021642 ultra pure water Inorganic materials 0.000 description 1
- 239000012498 ultrapure water Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses the device that electron-level phosphoric acid is produced in a kind of tubulation crystallization, comprise crystallizer tank, go out sour pump, acid-regulating tank and recycle pump, connected successively by pipeline between them, and pipeline is equipped with valve; This device also comprises spray thrower, the vertical array tubular of infrared lamp and more than four; Spray thrower is arranged on the top of crystallizer tank; Infrared lamp is evenly distributed in crystallizer tank; Vertical array tubular Vertical Uniform is distributed in crystallizer tank, and vertical array tubular is in parallel and be provided with heat-eliminating medium entrance and heat-eliminating medium outlet.The present invention makes crystalline carrier by adopting vertical array tubular, xln is made to be suspended on vertical array tubular, the high liquid phase of foreign matter content can be made thoroughly to discharge when crystalline substance, liquid two-phase laminated flow, solve the crystalline substance of the existence of straight tube crystallization in the past, liquid separation does not thoroughly cause quality product not high, the problem that purification efficiency is lower.The present invention is simple and reasonable, simple to operation, simplifies technical process, reduces production cost, and energy suitability for industrialized production electron-level phosphoric acid, has good economic benefit.
Description
Technical field
The invention belongs to technical field of chemical, especially relate to the device that electron-level phosphoric acid is produced in a kind of tubulation crystallization.
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.The device that current most domestic produces the employing of electron-level phosphoric acid producer is purified by industrial yellow phosphorus to make high-purity yellow phosphorus, refining high-purity yellow phosphorus is utilized to generate gaseous state Vanadium Pentoxide in FLAKES at clean, dry combustion synthesis in air, again Vanadium Pentoxide in FLAKES is dissolved in ultrapure water, produces electron-level phosphoric acid.This method purifying yellow phosphorus makes the loss of phosphorus comparatively large, cost up; Simultaneous reactions needs at high temperature to carry out, and energy consumption is high, and pollute large, because yellow phosphorus has pyrophoricity, this device is higher to equipment material, production control and affected personnel requirement, and production control is more difficult.
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.
The patent No. is that 201120108876.X discloses a kind of device producing electron-level phosphoric acid, comprises phosphoric acid subsider, crystallizer A, crystallizer B and product groove; Phosphoric acid subsider is connected to crystallizer A by pipeline A, strainer A is connected with below crystallizer A, strainer A discharge port connects complex acid groove A, complex acid groove A is connected to crystallizer B by pipeline, filter B is connected with below crystallizer B, filter B discharge port connects complex acid groove B, and complex acid groove B is connected to product groove by pipeline B.This device Production Flow Chart is loaded down with trivial details, and equipment used is more, and floor space is large, and product yield is lower.
Summary of the invention
The present invention is in order to overcome the deficiencies in the prior art, and provide a kind of equipment simple, floor space is little, can guarantee that crystalline phase is thoroughly separated with liquid phase, and the device of electron-level phosphoric acid is produced in a kind of tubulation crystallization improving the purification efficiency of phosphoric acid.
Technical scheme of the present invention is as follows:
A device for electron-level phosphoric acid is produced in tubulation crystallization, and comprise crystallizer tank, go out sour pump, acid-regulating tank and recycle pump, connected successively by pipeline between them, and pipeline is equipped with valve; It also comprises spray thrower, the vertical array tubular of infrared lamp and more than four; Described spray thrower is arranged on the top of crystallizer tank; Described infrared lamp is evenly distributed in crystallizer tank; Described vertical array tubular Vertical Uniform is distributed in crystallizer tank, and vertical array tubular is in parallel and be provided with heat-eliminating medium entrance and heat-eliminating medium outlet.
The upper end of above-described crystallizer tank is provided with acid inlet and crystal seed adds mouth; The lower end of described crystallizer tank is provided with acid mouth; Described acid mouth is connected by pipeline with the import going out sour pump, and pipeline is provided with valve.
Be provided with opening for feed and recycle acid import above above-described acid-regulating tank, below is provided with recycle acid outlet and products export, and top is provided with water-in and venting port; Described opening for feed with go out sour pump outlet and be connected, be provided with lateral and phosphoric acid production equipment connection in the middle of it; Described recycle acid import is connected with the export and import of recycle pump respectively by pipeline with recycle acid outlet, and described circulation pump outlet is provided with lateral and is connected with acid inlet and spray thrower respectively, and pipeline is equipped with valve.
Above-described spray thrower comprises sour pump and more than two stainless steel tubes; Described stainless steel tube is provided with spray header, and spray header is uniformly distributed the middle and upper part of crystallizer tank.
Above-described vertical array tubular adopts high strength glass material to make, and passes into heat-eliminating medium in pipe; Described heat-eliminating medium is cool brine or frozen water.
Compared to prior art, the present invention has the following advantages and positively effect:
1, the present invention makes crystalline carrier by adopting vertical array tubular, xln is made to be suspended on vertical array tubular, the high liquid phase of foreign matter content can be made thoroughly to discharge when brilliant, liquid two-phase laminated flow, solve the crystalline substance, the liquid that existed in the past and be separated and thoroughly do not cause quality product not high, the problem that purification efficiency is lower.
2, the present invention arranges and washes brilliant device in crystallizer tank, to crystal column surface and the spray washing of the remaining liquid phase of crystallizer tank, avoids the higher liquid phase of foreign matter content and the miscible situation of clean crystals, improves quality product.
3, the present invention arranges infrared lamp as heating unit in crystallizer tank, temperature easily and reliably in crystallization control groove, can make crystal melting sweating step by step, thus can obtain the electron-level phosphoric acid product of multiple pureness specifications simultaneously, to meet the different demands in market, create good economic benefit.
4, the present invention is simple and reasonable, simple to operation, simplifies technical process, reduces production cost, and energy suitability for industrialized production electron-level phosphoric acid, has good economic benefit.
Accompanying drawing explanation
Fig. 1 is structural representation of the present invention.
Accompanying drawing identifies:
1-crystallizer tank, 11-acid inlet, 12-crystal seed adds mouth, 13-acid mouth, 2-spray thrower, 41-heat-eliminating medium entrance, 42-heat-eliminating medium exports, 3-infrared lamp, 4-vertical array tubular, 5-goes out sour pump, 6-recycle pump, 7-acid-regulating tank, 71-opening for feed, 72-water-in, 73-venting port, the import of 74-recycle acid, 75-recycle acid exports, 76-products export.
Embodiment
Below in conjunction with the drawings and specific embodiments, the invention will be further described.
Embodiment 1:
A device for electron-level phosphoric acid is produced in tubulation crystallization, and comprise crystallizer tank 1, go out sour pump 5, acid-regulating tank 7 and recycle pump 6, connected successively by pipeline between them, pipeline is equipped with valve.The upper end of described crystallizer tank 1 is provided with acid inlet 11 and crystal seed adds mouth 12; The lower end of described crystallizer tank 1 is provided with acid mouth 13; Described acid mouth 13 is connected by pipeline with the import going out sour pump 5, and pipeline is provided with valve.
This vertical array tubular crystallization apparatus also comprises spray thrower 2, the vertical array tubular 4 of infrared lamp 3 and four.Described spray thrower 2 is arranged on the top of crystallizer tank 1; Spray thrower 2 comprises sour pump and two stainless steel tubes; Described stainless steel tube is provided with spray header, and spray header is uniformly distributed the middle and upper part of crystallizer tank 1.Described infrared lamp 3 is evenly distributed in crystallizer tank 1; Described vertical array tubular 4 Vertical Uniform is distributed in crystallizer tank 1, and vertical array tubular 4 is in parallel and be provided with heat-eliminating medium entrance 41 and heat-eliminating medium outlet 42.Described vertical array tubular 4 adopts high strength glass material to make, and passes into cool brine as heat-eliminating medium in pipe.
Be provided with opening for feed 71 and recycle acid import 74 above described acid-regulating tank 7, below is provided with recycle acid outlet 75 and products export 76, and top is provided with water-in 72 and venting port 73; Described opening for feed 71 is connected with the outlet going out sour pump 5, is provided with lateral and phosphoric acid production equipment connection in the middle of it.Described recycle acid import 74 is connected respectively by the export and import of pipeline with recycle pump 6 with recycle acid outlet 75, and the outlet of described recycle pump 6 is provided with lateral and is connected with acid inlet 11 and spray thrower 2 respectively, and pipeline is equipped with valve.
Embodiment 2:
A device for electron-level phosphoric acid is produced in tubulation crystallization, and comprise crystallizer tank 1, go out sour pump 5, acid-regulating tank 7 and recycle pump 6, connected successively by pipeline between them, pipeline is equipped with valve.The upper end of described crystallizer tank 1 is provided with acid inlet 11 and crystal seed adds mouth 12; The lower end of described crystallizer tank 1 is provided with acid mouth 13; Described acid mouth 13 is connected by pipeline with the import going out sour pump 5, and pipeline is provided with valve.
This vertical array tubular crystallization apparatus also comprises spray thrower 2, the vertical array tubular 4 of infrared lamp 3 and eight.Described spray thrower 2 is arranged on the top of crystallizer tank 1; Spray thrower 2 comprises sour pump and four stainless steel tubes; Described stainless steel tube is provided with spray header, and spray header is uniformly distributed the middle and upper part of crystallizer tank 1.Described infrared lamp 3 is evenly distributed in crystallizer tank 1; Described vertical array tubular 4 Vertical Uniform is distributed in crystallizer tank 1, and vertical array tubular 4 is in parallel and be provided with heat-eliminating medium entrance 41 and heat-eliminating medium outlet 42.Described vertical array tubular 4 adopts high strength glass material to make, and passes into frozen water as heat-eliminating medium in pipe.
Be provided with opening for feed 71 and recycle acid import 74 above described acid-regulating tank 7, below is provided with recycle acid outlet 75 and products export 76, and top is provided with water-in 72 and venting port 73; Described opening for feed 71 is connected with the outlet going out sour pump 5, is provided with lateral and phosphoric acid production equipment connection in the middle of it.Described recycle acid import 74 is connected respectively by the export and import of pipeline with recycle pump 6 with recycle acid outlet 75, and the outlet of described recycle pump 6 is provided with lateral and is connected with acid inlet 11 and spray thrower 2 respectively, and pipeline is equipped with valve.
Claims (4)
1. a device for electron-level phosphoric acid is produced in tubulation crystallization, and comprise crystallizer tank (1), go out sour pump (5), acid-regulating tank (7) and recycle pump (6), connected successively by pipeline between them, pipeline is equipped with valve; It is characterized in that: it also comprises spray thrower (2), the vertical array tubular (4) of infrared lamp (3) and more than four; Described spray thrower (2) is arranged on the top of crystallizer tank (1); Described infrared lamp (3) is evenly distributed in crystallizer tank (1); Described vertical array tubular (4) Vertical Uniform is distributed in crystallizer tank (1), and vertical array tubular (4) is in parallel and be provided with heat-eliminating medium entrance (41) and heat-eliminating medium exports (42);
Described acid-regulating tank (7) top is provided with opening for feed (71) and recycle acid import (74), and below is provided with recycle acid outlet (75) and products export (76), and top is provided with water-in (72) and venting port (73); Described opening for feed (71) is connected with the outlet going out sour pump (5), is provided with lateral and phosphoric acid production equipment connection in the middle of it; Described recycle acid import (74) is connected respectively by the export and import of pipeline with recycle pump (6) with recycle acid outlet (75), the outlet of described recycle pump (6) is provided with lateral and is connected with acid inlet (11) and spray thrower (2) respectively, and pipeline is equipped with valve.
2. the device of electron-level phosphoric acid is produced in a kind of tubulation crystallization according to claim 1, it is characterized in that: the upper end of described crystallizer tank (1) is provided with acid inlet (11) and crystal seed adds mouth (12); The lower end of described crystallizer tank (1) is provided with acid mouth (13); Described acid mouth (13) is connected by pipeline with the import going out sour pump (5), and pipeline is provided with valve.
3. the device of electron-level phosphoric acid is produced in a kind of tubulation crystallization according to claim 1, it is characterized in that: described spray thrower (2) comprises sour pump and more than two stainless steel tubes; Described stainless steel tube is provided with spray header, and spray header is uniformly distributed the middle and upper part of crystallizer tank (1).
4. the device of electron-level phosphoric acid is produced in a kind of tubulation crystallization according to claim 1, it is characterized in that: described vertical array tubular (4) adopts high strength glass material to make, and passes into heat-eliminating medium in pipe; Described heat-eliminating medium is cool brine or frozen water.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310744583.4A CN103896231B (en) | 2013-12-30 | 2013-12-30 | The device of electron-level phosphoric acid is produced in a kind of tubulation crystallization |
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|---|---|---|---|
| CN201310744583.4A CN103896231B (en) | 2013-12-30 | 2013-12-30 | The device of electron-level phosphoric acid is produced in a kind of tubulation crystallization |
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| CN103896231A CN103896231A (en) | 2014-07-02 |
| CN103896231B true CN103896231B (en) | 2016-03-02 |
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102795609A (en) * | 2011-05-23 | 2012-11-28 | 杨志勇 | Apparatus for producing high purity electronic grade phosphoric acid |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102795609A (en) * | 2011-05-23 | 2012-11-28 | 杨志勇 | Apparatus for producing high purity electronic grade phosphoric acid |
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