CN109911858A - The production equipment of One-step production super-clean high-purity microelectronics grade hydrogen peroxide - Google Patents
The production equipment of One-step production super-clean high-purity microelectronics grade hydrogen peroxide Download PDFInfo
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- CN109911858A CN109911858A CN201910333224.7A CN201910333224A CN109911858A CN 109911858 A CN109911858 A CN 109911858A CN 201910333224 A CN201910333224 A CN 201910333224A CN 109911858 A CN109911858 A CN 109911858A
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- Prior art keywords
- resin tower
- purity
- hydrogen peroxide
- storage tank
- clean high
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- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- 238000004519 manufacturing process Methods 0.000 title claims abstract description 53
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 title claims abstract description 25
- 238000004377 microelectronic Methods 0.000 title claims abstract description 16
- 239000011347 resin Substances 0.000 claims abstract description 75
- 229920005989 resin Polymers 0.000 claims abstract description 75
- 239000002994 raw material Substances 0.000 claims abstract description 19
- 238000000926 separation method Methods 0.000 claims abstract description 14
- 239000000463 material Substances 0.000 claims description 9
- 239000012535 impurity Substances 0.000 claims description 8
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims description 2
- 229910052731 fluorine Inorganic materials 0.000 claims description 2
- 239000011737 fluorine Substances 0.000 claims description 2
- 239000011521 glass Substances 0.000 claims description 2
- 230000008676 import Effects 0.000 claims description 2
- 230000003647 oxidation Effects 0.000 claims description 2
- 238000007254 oxidation reaction Methods 0.000 claims description 2
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 claims 1
- 239000005977 Ethylene Substances 0.000 claims 1
- 229910001220 stainless steel Inorganic materials 0.000 claims 1
- 239000010935 stainless steel Substances 0.000 claims 1
- 238000010521 absorption reaction Methods 0.000 abstract description 5
- 238000000034 method Methods 0.000 description 13
- 238000005516 engineering process Methods 0.000 description 9
- 239000007864 aqueous solution Substances 0.000 description 5
- 239000008187 granular material Substances 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
- 239000012528 membrane Substances 0.000 description 4
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 4
- 239000004810 polytetrafluoroethylene Substances 0.000 description 4
- 238000000746 purification Methods 0.000 description 4
- 238000005342 ion exchange Methods 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- PYKYMHQGRFAEBM-UHFFFAOYSA-N anthraquinone Natural products CCC(=O)c1c(O)c2C(=O)C3C(C=CC=C3O)C(=O)c2cc1CC(=O)OC PYKYMHQGRFAEBM-UHFFFAOYSA-N 0.000 description 2
- 150000004056 anthraquinones Chemical class 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 238000004821 distillation Methods 0.000 description 2
- -1 polytetrafluoroethylene Polymers 0.000 description 2
- 238000001223 reverse osmosis Methods 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- YEVQZPWSVWZAOB-UHFFFAOYSA-N 2-(bromomethyl)-1-iodo-4-(trifluoromethyl)benzene Chemical compound FC(F)(F)C1=CC=C(I)C(CBr)=C1 YEVQZPWSVWZAOB-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 125000002091 cationic group Chemical group 0.000 description 1
- 230000019771 cognition Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 238000010237 hybrid technique Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 239000012224 working solution Substances 0.000 description 1
Landscapes
- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The present invention relates to a kind of production equipments of One-step production super-clean high-purity microelectronics grade hydrogen peroxide, storage tank is received including raw material storage tank, power transfer pump, hybrid resin tower purifying system, film separation system and finished product, it is sequentially connected by pipeline, pipeline is equipped with control valve.Wherein, raw material storage tank is connected with power transfer pump, then be connected with hybrid resin tower purifying system, film separation system and finished product receive storage tank and are connected.The present invention skimmed absorption, yin, yang and mixing cumbersome production equipment, it is simple and practical and output can be improved.
Description
Technical field
The invention belongs to electronic information chemical industry material manufacturing field, product purpose is to remove chip, silicon wafer using the product
Piece, large-scale integrated circuit, various display panels and trace impurity and tiny dust granules on solar panel, in particular to
A kind of One-step production super-clean high-purity microelectronics grade hydrogen peroxide (H2O2) production equipment.
Background technique
Super-clean high-purity microelectronics grade H2O2Usually with technical grade H2O2It is produced made of purifying for raw material, at present work
Industry grade H2O2Production technology is using anthraquinone production, therefore technical grade H2O2Product contains a large amount of organic matter, tens kinds of gold
Belong to ion and nonmetallic inclusion, anthraquinone derivative, such as 2- alkyl-anthraquinone, trioctyl phosphate etc..Therefore it needs to technical grade H2O2
Aqueous solution implements purifying and purification.
It is currently known purifying technical grade H2O2Method have, distillation under vacuum, film filters method of purification, absorption and ion
Exchange process etc..
1) H of distillation under vacuum purifying2O2Aqueous products purity can only achieve the pure product quality of chemistry, and
Raw material output capacity is very low, and yield rate only has 80% or so, if there is multiple towers carry out circulation purifying production, is produced into
This is very high, a large amount of electric power energy is not only consumed in production process, and safety is also excessively poor.
2) film filters method of purification, technical grade H2O2Pass through membrane reverse osmosis system purifying H2O2Product, product quality are reachable
To high-purity H2O2Requirement, but raw material output capacity only have 60% hereinafter, and membrane reverse osmosis equipment service life it is very short
Temporarily, only several shifts, so production cost is higher by 150% or so than the product that other methods are produced.
3) more advanced at present is exactly electron level H that resin ion exchange process purifying general in the world produces2O2
Production technology;Absorption, yin and yang resin ion-exchange, though the method can produce the higher product of purity, cost can also be with
It controls, single zwitterion can be accomplished to be less than 5ppb in product, but the production technology is comparatively laborious, uses the production technology
It is difficult to accomplish the production line of automation;Because such production process is by adsorption system, cationic systems, anion system,
Hybrid technique system, the composition such as membrane separation process system, system is more and the technique requirement data of each system are also different,
Therefore it is difficult to be integrated into automatic production line.
Because production process is extremely complex cumbersome, operator's slightly general idea will result in the resin of yin and yang resin column
Mistake is loaded, increases several times simultaneously using workload.This phenomenon is commonplace, and handling resin workload is as a result caused not only to increase
Greatly, water power consumption increases and artificial and energy waste happens occasionally, because faulty operation easily leads to the accident of efficiency lost resin
It is also frequent occurrence, not only waste of resource also damages production equipment.
Summary of the invention
In order to solve the above technical problems, the present invention provides a kind of One-step production super-clean high-purity microelectronics grade hydrogen peroxide
Production equipment, including raw material storage tank, power transfer pump, hybrid resin tower purifying system, film separation system and finished product connect
Store up tank;
Raw material storage tank outlet is connected with power transfer pump, then with hybrid resin tower purifying system, UF membrane system
System, finished product receive storage tank and are connected, they are sequentially connected by pipeline, and the pipeline of connection is equipped with control valve.
Preferable, the hybrid resin tower purifying system includes the more resin towers being sequentially connected, the resin
Tower includes tower bucket, feed inlet, discharge port.
Preferable, the hybrid resin tower purifying system includes the first resin tower, the second resin tower, third resin
Tower, the 4th resin tower.
Preferable, first to fourth resin tower is sequentially connected by pipeline, feed inlet, the discharge port of the resin tower
The pipeline of connection is equipped with control valve;
The control valve of the first resin tower feed inlet is connected with power transfer pump, the 4th resin tower discharge port
Control valve is connected with film separation system import.
It is preferable, the resin tower, power transfer pump and control valve using few dissolution impurity organic glass, no
Rust steel, polytetrafluoroethylene (PTFE), pp, pe, epdf material are made.
Preferable, the resin tower height degree is 500mm-4500mm, diameter 150mm-1650mm.
Preferable, the resin tower is provided with resistance to oxidation resistant fluorine zwitterion resin, and fluororesin fills tower height degree ratio
For 50%-95%, yin-yang fluororesin filling ratio is that 10%-30%-50%-95% is differed in the resin tower.
In 0.5-1.5Mpa, temperature is controlled at 3-42 DEG C for the operating pressure control of production equipment operational process of the invention,
Working solution flow control is in 400L/h-500L/h, the raw material H2O2The concentration of aqueous solution is 27.5%-35% concentration.It is described
Impure more raw material H2O2Aqueous solution is inputted in four concatenated resin towers by power transfer pump, carries out zwitterion friendship
Change the purifying with impurity.In the production equipment directly and H2O2Contact is using few fluororesin material for dissolving out impurity
Material, so that 0.5ppb or so quality is obtained, super-clean high-purity microelectronics grade H2O2Product.
Beneficial effects of the present invention: production equipment of the invention is simple and practical and can improve output, is set using this production
Standby absorption of having skimmed, yin, yang and the cumbersome production technology mixed.
Using hybrid production technique, the production of the hybrid resin tower purifying system of four resin towers of connecting, so that it may
To produce the super-clean high-purity microelectronics grade H of 0.5ppb or more2O2, eliminate absorption, positive and negative, three production technologies process mistake
The device not only can be integrated into the production line of automation by journey, but also can be avoided conventional production technology because loaded resin is made
At series of malpractice.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of production equipment of the present invention;
Fig. 2 is the structure chart of resin tower of the present invention;
Wherein 1- raw material storage tank, 2- power transfer pump, 3- film separation system, 4- finished product receive storage tank, 5- control valve, 6-
Pipeline, the first resin tower of 7-, the second resin tower of 8-, 9- third resin tower, the 4th resin tower of 10-, 11- tower bucket, 12- feed inlet,
13- discharge port.
Specific embodiment
The present invention is further illustrated with reference to the accompanying drawing:
Production equipment shown in FIG. 1 includes raw material storage tank 1, power transfer pump 2, hybrid resin tower purifying system, film
Separation system 3 and finished product receive storage tank 4, and hybrid resin tower purifying system includes four resin towers, respectively the first resin
Tower 7, the second resin tower 8, third resin tower 9, the 4th resin tower 10, resin tower include tower bucket 11, feed inlet 12 and discharge port 13,
Apparatus above is connected by pipeline 6, and pipeline 6 is equipped with control valve 5.
In embodiment, by more industrial raw material H impure in raw material storage tank 12O2Aqueous solution passes through power transmission
Pump 2 enters hybrid resin tower purifying system.
Industrial raw material H2O2Aqueous solution is entered in tower bucket 11 by control valve 5 from 7 feed inlet 12 of the first resin tower
Purifying is carried out, then the second resin tower 8 will be flowed by the raw material liq of the first resin tower 7, then by the second resin tower 8
Material liquid flows into third resin tower 9, then the material liquid of third resin tower 9 is flowed into the 4th resin tower 10 and carries out last procedure
Purifying after, the product of the 4th resin tower 10 after purifying is flowed into film separation system 3 and removes granule foreign
Finished product is flowed into afterwards receives storage tank 4.
In the present embodiment, the pressure of operation is controlled at 3 DEG C -42 DEG C, is produced per hour in 0.5Mpa-1.5Mpa, temperature
Amount control is in 400L-500L, by the purifying of four resin towers, the H flowed out out of this resin tower2O2It has obtained thoroughly
Purification, but H2O2Granule foreign in liquid not yet removes, in former cognition, H2O2Unstable factor be considered by
Caused by metal ion, light, heat, and it is unaware that granule foreign to H2O2Harm.Due to the huge surface of granule foreign
Product makes H2O2Decomposing phenomenon is generated, and is not suitable for long-distance transportation and storage.
The separation accuracy of film separation system 3 is 0.2 μm in Fig. 1.Microelectronics grade H at this time2O2Solution obtain comprehensively purify and
After separation, less than 20, stability is greatly improved for every milliliter of graininess greater than 0.2 μm, can be entered finished product and be received
Storage tank 4 carries out product packaging using baling line.
In the present embodiment, raw material H2O2Utilization rate be greater than 99%, above-mentioned used resin tower, power transfer pump 2 and control
Valve 5 processed is made of polytetrafluoroethylene (PTFE), pp, pe, epdf material of few dissolution impurity.
Table 1 is different content H2O2Raw material various impurity contents after production technology of the invention and old technique purifying
Comparison, production technology embodiment 1-3 of the invention can compare old technique as seen from Table 1, various impurity contents have obtained very
Big reduction, substantially increases H2O2Purity.
Table 1: examining report, unit: ppb
Finally, it should be noted that the above embodiments are merely illustrative of the technical solutions of the present invention, rather than its limitations, although
Present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that, still may be used
To modify the technical solutions described in the foregoing embodiments or equivalent replacement of some of the technical features,
And these are modified or replaceed, technical solution of various embodiments of the present invention that it does not separate the essence of the corresponding technical solution spirit and
Range.
Claims (7)
1. the production equipment of One-step production super-clean high-purity microelectronics grade hydrogen peroxide, which is characterized in that including raw material storage tank, move
Power delivery pump, hybrid resin tower purifying system, film separation system and finished product receive storage tank;
Raw material storage tank outlet is connected with power transfer pump, then with hybrid resin tower purifying system, film separation system, at
Product receive storage tank and are connected, they are sequentially connected by pipeline, and the pipeline of connection is equipped with control valve.
2. the production equipment of One-step production super-clean high-purity microelectronics grade hydrogen peroxide according to claim 1, feature
Be, the hybrid resin tower purifying system includes the more resin towers being sequentially connected, the resin tower include tower bucket, into
Material mouth, discharge port.
3. the production equipment of One-step production super-clean high-purity microelectronics grade hydrogen peroxide according to claim 2, feature
It is, the hybrid resin tower purifying system includes the first resin tower, the second resin tower, third resin tower, the 4th resin
Tower.
4. the production equipment of One-step production super-clean high-purity microelectronics grade hydrogen peroxide according to claim 3, feature
It is, first to fourth resin tower is sequentially connected by pipeline, on the feed inlet of the resin tower, the pipeline of discharge port connection
Equipped with control valve;
The control valve of the first resin tower feed inlet is connected with power transfer pump, the control of the 4th resin tower discharge port
Valve is connected with film separation system import.
5. the production equipment of One-step production super-clean high-purity microelectronics grade hydrogen peroxide according to claim 2, feature
It is, the resin tower, power transfer pump and control valve are using few organic glass, stainless steel, polytetrafluoro for dissolving out impurity
Ethylene, pp, pe, epdf material are made.
6. the production equipment of One-step production super-clean high-purity microelectronics grade hydrogen peroxide according to claim 2, feature
It is, the resin tower height degree is 500mm-4500mm, diameter 150mm-1650mm.
7. the production equipment of One-step production super-clean high-purity microelectronics grade hydrogen peroxide according to claim 2, feature
It is, the resin tower is provided with resistance to oxidation resistant fluorine zwitterion resin, and it is 50%-95% that fluororesin, which fills tower height degree ratio,
Yin-yang fluororesin filling ratio is that 10%-30%-50%-95% is differed in the resin tower.
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CN201910333224.7A CN109911858A (en) | 2019-04-24 | 2019-04-24 | The production equipment of One-step production super-clean high-purity microelectronics grade hydrogen peroxide |
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CN201910333224.7A CN109911858A (en) | 2019-04-24 | 2019-04-24 | The production equipment of One-step production super-clean high-purity microelectronics grade hydrogen peroxide |
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Citations (6)
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CN1285311A (en) * | 2000-09-21 | 2001-02-28 | 上海哈勃化工有限公司 | Process and equipment for preparation of ultrapure hydrogen peroxide |
CN101804969A (en) * | 2010-04-02 | 2010-08-18 | 赫格雷(大连)制药有限公司 | Low-carbon environment friendly production method for extra high-purity H2O2 |
CN101817511A (en) * | 2010-04-02 | 2010-09-01 | 赫格雷(大连)制药有限公司 | Device for producing low-carbon environment-friendly super clean high-purity H2O2 |
CN201770477U (en) * | 2010-04-02 | 2011-03-23 | 赫格雷(大连)制药有限公司 | Production device for low-carbon environmentally-friendly super-clean high-purity H2O2 |
US20120148482A1 (en) * | 2010-12-08 | 2012-06-14 | Shanghai Huayi Microelectronic Material Co., Ltd. | Method for producing ultra-pure aqueous hydrogen peroxide solution |
CN209974301U (en) * | 2019-04-24 | 2020-01-21 | 广州市天夫美新材料科技有限公司 | Production equipment for producing ultra-clean high-purity microelectronic hydrogen peroxide by one-step method |
-
2019
- 2019-04-24 CN CN201910333224.7A patent/CN109911858A/en active Pending
Patent Citations (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1285311A (en) * | 2000-09-21 | 2001-02-28 | 上海哈勃化工有限公司 | Process and equipment for preparation of ultrapure hydrogen peroxide |
CN101804969A (en) * | 2010-04-02 | 2010-08-18 | 赫格雷(大连)制药有限公司 | Low-carbon environment friendly production method for extra high-purity H2O2 |
CN101817511A (en) * | 2010-04-02 | 2010-09-01 | 赫格雷(大连)制药有限公司 | Device for producing low-carbon environment-friendly super clean high-purity H2O2 |
CN201770477U (en) * | 2010-04-02 | 2011-03-23 | 赫格雷(大连)制药有限公司 | Production device for low-carbon environmentally-friendly super-clean high-purity H2O2 |
US20120148482A1 (en) * | 2010-12-08 | 2012-06-14 | Shanghai Huayi Microelectronic Material Co., Ltd. | Method for producing ultra-pure aqueous hydrogen peroxide solution |
CN102556976A (en) * | 2010-12-08 | 2012-07-11 | 上海华谊微电子材料有限公司 | Method for continuous production of ultrapure hydrogen peroxide |
CN209974301U (en) * | 2019-04-24 | 2020-01-21 | 广州市天夫美新材料科技有限公司 | Production equipment for producing ultra-clean high-purity microelectronic hydrogen peroxide by one-step method |
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