CN1285560C - Method for preparing hyperpure acetic acid and equipment - Google Patents
Method for preparing hyperpure acetic acid and equipment Download PDFInfo
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- CN1285560C CN1285560C CN 200310109477 CN200310109477A CN1285560C CN 1285560 C CN1285560 C CN 1285560C CN 200310109477 CN200310109477 CN 200310109477 CN 200310109477 A CN200310109477 A CN 200310109477A CN 1285560 C CN1285560 C CN 1285560C
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- Prior art keywords
- acetic acid
- preparation
- rectifying tower
- stage
- ultrapure
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- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 title claims abstract description 111
- 238000000034 method Methods 0.000 title claims description 17
- 238000002360 preparation method Methods 0.000 claims abstract description 14
- 239000012535 impurity Substances 0.000 claims abstract description 11
- 238000000746 purification Methods 0.000 claims abstract description 8
- 239000000126 substance Substances 0.000 claims abstract description 8
- 230000003647 oxidation Effects 0.000 claims abstract description 6
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 6
- 229920006395 saturated elastomer Polymers 0.000 claims abstract description 4
- 125000002485 formyl group Chemical class [H]C(*)=O 0.000 claims abstract 6
- 238000001914 filtration Methods 0.000 claims abstract 3
- 239000003795 chemical substances by application Substances 0.000 claims description 7
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 6
- 239000012528 membrane Substances 0.000 claims description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 5
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 claims description 4
- 239000000463 material Substances 0.000 claims description 4
- 238000010992 reflux Methods 0.000 claims description 4
- WGLPBDUCMAPZCE-UHFFFAOYSA-N Trioxochromium Chemical compound O=[Cr](=O)=O WGLPBDUCMAPZCE-UHFFFAOYSA-N 0.000 claims description 3
- QYKIQEUNHZKYBP-UHFFFAOYSA-N Vinyl ether Chemical compound C=COC=C QYKIQEUNHZKYBP-UHFFFAOYSA-N 0.000 claims description 3
- BCQZXOMGPXTTIC-UHFFFAOYSA-N halothane Chemical compound FC(F)(F)C(Cl)Br BCQZXOMGPXTTIC-UHFFFAOYSA-N 0.000 claims description 3
- 229960003132 halothane Drugs 0.000 claims description 3
- 239000012286 potassium permanganate Substances 0.000 claims description 3
- 239000000741 silica gel Substances 0.000 claims description 3
- 229910002027 silica gel Inorganic materials 0.000 claims description 3
- 150000008065 acid anhydrides Chemical class 0.000 claims description 2
- 229910000365 copper sulfate Inorganic materials 0.000 claims description 2
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 claims description 2
- 239000002808 molecular sieve Substances 0.000 claims description 2
- 238000012856 packing Methods 0.000 claims description 2
- 239000010453 quartz Substances 0.000 claims description 2
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims description 2
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical group FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 claims description 2
- 238000005516 engineering process Methods 0.000 abstract description 3
- 229910052751 metal Inorganic materials 0.000 abstract description 3
- 239000002184 metal Substances 0.000 abstract description 3
- 235000011054 acetic acid Nutrition 0.000 abstract 4
- 150000001243 acetic acids Chemical class 0.000 abstract 3
- 239000002245 particle Substances 0.000 abstract 2
- 239000012982 microporous membrane Substances 0.000 abstract 1
- 150000001299 aldehydes Chemical class 0.000 description 8
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 6
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 6
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 5
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- 238000009835 boiling Methods 0.000 description 4
- 238000004821 distillation Methods 0.000 description 4
- 238000004377 microelectronic Methods 0.000 description 4
- WFDIJRYMOXRFFG-UHFFFAOYSA-N Acetic anhydride Chemical compound CC(=O)OC(C)=O WFDIJRYMOXRFFG-UHFFFAOYSA-N 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 229960002050 hydrofluoric acid Drugs 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 241000282326 Felis catus Species 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 230000006315 carbonylation Effects 0.000 description 2
- 238000005810 carbonylation reaction Methods 0.000 description 2
- 239000008187 granular material Substances 0.000 description 2
- 229910017604 nitric acid Inorganic materials 0.000 description 2
- IQGZCSXWIRBTRW-ZZXKWVIFSA-N (2E)-2-ethyl-2-butenal Chemical compound CC\C(=C/C)C=O IQGZCSXWIRBTRW-ZZXKWVIFSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- MLUCVPSAIODCQM-NSCUHMNNSA-N crotonaldehyde Chemical compound C\C=C\C=O MLUCVPSAIODCQM-NSCUHMNNSA-N 0.000 description 1
- MLUCVPSAIODCQM-UHFFFAOYSA-N crotonaldehyde Natural products CC=CC=O MLUCVPSAIODCQM-UHFFFAOYSA-N 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000010295 mobile communication Methods 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention relates to a preparation method of hyperpure acetic acids and a device thereof. The technology combining chemical pretreatment, two-stage rectification and ultraclean filtration is used. The device mainly comprises a pretreater, a two-stage rectifying tower and an ultraclean filter. The preparation method comprises the steps: firstly, saturated aldehyde and unsaturated aldehyde are oxidized, and excessive moisture is removed; then, aldehyde oxidation products and metal impurities in acetic acids are removed; finally, under the purification environment, a microporous membrane filter is used for filtration. By adopting the present invention, the acetic acid content in the prepared acetic acids is more than 99.9%, the content of reducing impurities is reduced to less than 5 ppm, the content of single metal impurities is reduced to less than 10 ppb, and the content of particles with the particle diameters of more than 0.5 mu m is reduced to less than 25 per ml.
Description
Technical field
The present invention relates to a kind of preparation method and device thereof of acetic acid, particularly a kind of technical grade acetic acid of producing with the methanol carbonylation process of content 99.0% is the method for the ultrapure acetic acid of feedstock production, and the device that uses this method.
Background technology
Along with development of information industry, computer and mobile communication are more and more universal, and large-scale unicircuit (super large-scale integration microelectronic industry) has become the guide in the information industry.Ultrapure acetic acid is one of indispensable microelectronics chemistry product as the important solvent in the etching, and market outlook are very wide.Therefore, the development of ultrapure acetic acid can promote the development of China's information industry.
At present, being applied to the industrial method of microelectronics chemistry product mainly contains: Chemical Pretreatment method, distillation and rectification method, gas absorption method and sub-boiling distillation method etc.Wherein the gas absorption method is applicable to that mainly water absorbs gas to reach the material of purification purpose, example hydrochloric acid, hydrofluoric acid, sulfuric acid, nitric acid etc.In patent CN1204550A, CN1300634A, introduced the technology of multiple ultrapure chemical such as suitable production ultra-pure sulfuric acid, ultrapure hydrochloric acid, super-pure nitric acid, ultra-pure hydrogen fluoric acid; The sub-boiling distillation method is only applicable to volatile liquid, such as hydrochloric acid, hydrofluoric acid etc.This shows that above-mentioned two kinds of methods all are not suitable for purification acetic acid.
Rectification method is the important purification process of acetic acid.Usually, industrial acetic acid all adopts this method to purify.Owing to be applicable to the ultrapure acetic acid of microelectronics chemistry product industry, to negatively charged ion wherein, harshness is all compared in the requirement of granule number and metallic impurity, and single rectifying can not reach requirement.
Summary of the invention
Technical problem to be solved by this invention is: the preparation method and the device thereof that provide a kind of acetic acid content can reach ultrapure acetic acid more than 99.9%.
The present invention is achieved like this: a kind of preparation method of ultrapure acetic acid, and it may further comprise the steps:
A. the oxygenant that adds dewatering agent and oxidable saturated aldehyde and unsaturated aldehyde in technical grade acetic acid carries out Chemical Pretreatment under the condition of 20 ℃～150 ℃ of pressure 0.02～0.2Mpa, temperature, remove excessive moisture;
B. two stage rectification is removed aldehydes oxidation products and metallic impurity in the acetic acid, and wherein first step rectifying pressure is 0～0.3Mpa, and temperature is 100 ℃～160 ℃, and reflux ratio is 1.5～5; Rectifying pressure in the second stage is 0～0.3Mpa, and temperature is 100 ℃～160 ℃;
C. ultra-clean filters, and to the acetic acid behind the two stage rectification, under environment purification, filters with nuclepore membrane filter.
A kind of device that adopts the ultrapure acetic acid of method for preparing comprises pretreater, condenser, receiver, rectifying tower, and strainer.It is characterized in that: rectifying tower is the two stage rectification tower, the delivery port of first step rectifying tower links to each other with the input aperture of second stage rectifying tower by first condenser, first receiver successively, and the delivery port of second stage rectifying tower links to each other with the input aperture of nuclepore membrane filter by second condenser, second receiver successively.
After Chemical Pretreatment, two stage rectification and ultra-clean filtered, the content of reducing impurity can drop to that 5ppm is following, single metals content impurity can drop to below the 10ppb with industrial acetic acid in the present invention, greater than the granule content of 0.5 μ m can drop to 25/below the ml.
Description of drawings
Accompanying drawing prepares the process flow sheet of ultrapure acetic acid
Embodiment
With reference to the accompanying drawings, the purifying technique of ultrapure acetic acid mainly is made up of equipment such as pretreater, rectifying tower 1, condenser 1, receiver 1, rectifying tower 2, condenser 2, receiver 2 and ultra-clean strainers.The impurity that mainly contains in the technical grade acetic acid that methanol carbonylation process is produced is unsaturated aldehydes such as saturated aldehyde and unsaturated aldehyde, especially crotonic aldehyde, 2-ethyl crotonaldehyde.The boiling point of these impurity compounds and the boiling point of acetic acid are very approaching, are unfavorable for next step distillation operation.At these characteristics, adopted these aldehydes of oxygenant oxidation, utilize the product after its oxidation to be separated apart from bigger characteristics with the acetic acid boiling-point difference.In addition, the existence of moisture also influences the quality of ultrapure acetic acid, has added suitable dewatering agent for this reason.Here dewatering agent can be a kind of in the vitriol oil, molecular sieve, sal epsom, calcium sulfate, copper sulfate, acid anhydrides or the silica gel, and the scope of its weight percent is 0.02%～15%; Oxygenant can be a kind of in chromic oxide, potassium permanganate, ozone, the hydrogen peroxide, and the scope of its weight percent is 0.01%～10%.Pressure 0.02～the 0.2Mpa of pretreater, 20 ℃～150 ℃ of temperature.Dewatering agent, oxygenant and technical grade acetic acid enter rectifying tower 1 and carry out one-level rectifying after pretreater is handled, remove the aldehydes oxidation products in the acetic acid.Rectifying tower 1 can adopt tray column or packing tower, and the operation pressure range of cat head is 0～0.3Mpa, and temperature is 100 ℃～160 ℃, and the span of control of reflux ratio is 1.5～5.Acetic acid after the one-level rectifying, the content of its reducing substances can be reduced to 5ppm.Remove the two-stage rectification of metallic impurity again.The material of rectifying tower 2 can be selected any in tetrafluoroethylene, high purity quartz, the poly-high fluothane Vinyl Ether for use, and the operation pressure range of cat head is 0～0.3Mpa, and temperature is 100 ℃～160 ℃.After two-stage rectification, be to carry out ultra-clean through 0.2 μ m nuclepore membrane filter under 100 grades the environment purification to filter at the ultra-clean index.
Preferred 3 embodiment are referring to table 1
The processing step and the condition of the ultrapure acetic acid of table 1 preparation
| Process conditions | Example 1 | Example 2 | Example 3 | |
| (1) Chemical Pretreatment | ||||
| Oxygenant | Title | Potassium permanganate | Chromic oxide | Hydrogen peroxide |
| Weight percent | 5％ | 0.2％ | 1％ | |
| Dewatering agent | Title | The vitriol oil | Aceticanhydride | Silica gel |
| Weight percent | 5％ | 0.2％ | 14％ | |
| Operation pressure (Mpa) | 0.1 | 0.1 | 0.1 | |
| Temperature (℃) | 110 | 30 | 20 | |
| (2) one-level rectifying | ||||
| Operation pressure (Mpa) | 0.1 | 0.1 | 0.2 | |
| Tower top temperature (℃) | 118 | 118 | 142 | |
| Reflux ratio | 5 | 3 | 4 | |
| (3) two-stage rectification | ||||
| The rectifying column material | Silica glass | Tetrafluoroethylene | Poly-high fluothane Vinyl Ether | |
| Operation pressure (Mpa) | 0.1 | 0.1 | 0.2 | |
| Tower top temperature (℃) | 118 | 118 | 142 | |
Claims (8)
1, a kind of preparation method of ultrapure acetic acid, it may further comprise the steps:
A. the oxygenant that adds dewatering agent and oxidable saturated aldehyde and unsaturated aldehyde in technical grade acetic acid carries out Chemical Pretreatment under the condition of 20 ℃～150 ℃ of pressure 0.02～0.2Mpa, temperature, remove excessive moisture;
B. two stage rectification is removed aldehydes oxidation products and metallic impurity in the acetic acid, and wherein first step rectifying pressure is 0～0.3Mpa, and temperature is 100 ℃～160 ℃, and reflux ratio is 1.5～5; Rectifying pressure in the second stage is 0～0.3Mpa, and temperature is 100 ℃～160 ℃;
C. ultra-clean filters, and to the acetic acid behind the two stage rectification, under environment purification, filters with nuclepore membrane filter.
2, preparation method according to claim 1 is characterized in that: described oxygenant is chosen a kind of in chromic oxide, potassium permanganate, hydrogen peroxide, and its weight percent is 0.01%～10%.
3, preparation method according to claim 1 is characterized in that: described dewatering agent is chosen a kind of in the vitriol oil, molecular sieve, sal epsom, calcium sulfate, copper sulfate, acid anhydrides or silica gel, and its weight percent is 0.02%～15%.
4, preparation method according to claim 1 is characterized in that: described nuclepore membrane filter adopts 0.2 μ m millipore filtration.
5, according to claim 1 or 4 described preparation methods, it is characterized in that: the ultra-clean index of described environment purification is 100 grades.
6, a kind of device that adopts the described method of claim 1 to prepare ultrapure acetic acid, comprise pretreater, condenser, receiver, rectifying tower and strainer, it is characterized in that: rectifying tower is the two stage rectification tower, the delivery port of first step rectifying tower links to each other with the input aperture of second stage rectifying tower by first condenser, first receiver successively, and the delivery port of second stage rectifying tower links to each other with the input aperture of nuclepore membrane filter by second condenser, second receiver successively.
7, the device of the ultrapure acetic acid of preparation according to claim 6 is characterized in that: the material of described second stage rectifying tower is a kind of in tetrafluoroethylene, high purity quartz, the poly-high fluothane Vinyl Ether.
8, the device of the ultrapure acetic acid of preparation according to claim 6 is characterized in that: described first step rectifying tower is tray column or packing tower.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200310109477 CN1285560C (en) | 2003-12-16 | 2003-12-16 | Method for preparing hyperpure acetic acid and equipment |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200310109477 CN1285560C (en) | 2003-12-16 | 2003-12-16 | Method for preparing hyperpure acetic acid and equipment |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1562938A CN1562938A (en) | 2005-01-12 |
| CN1285560C true CN1285560C (en) | 2006-11-22 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN 200310109477 Expired - Lifetime CN1285560C (en) | 2003-12-16 | 2003-12-16 | Method for preparing hyperpure acetic acid and equipment |
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| Country | Link |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2012062299A (en) * | 2010-09-17 | 2012-03-29 | Shanghai Huayi Microelectric Material Co Ltd | Method for producing high-purity electronic grade acetic acid |
Families Citing this family (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101362683B (en) * | 2008-09-16 | 2011-07-20 | 江阴市润玛电子材料有限公司 | Method for preparing super-clean and high-purity acetic acid and apparatus thereof |
| CN101979370B (en) * | 2010-11-29 | 2014-07-16 | 上海化学试剂研究所 | Method for improving quality of technical grade acetic acid |
| CN102746137B (en) * | 2012-08-03 | 2014-10-22 | 天津长芦海晶集团有限公司 | Method for producing medical glacial acetic acids by using industrial glacial acetic acids |
| CN103449994A (en) * | 2013-09-09 | 2013-12-18 | 成都红胜科技发展有限公司 | Purifying process of cyclobutanone |
| CN104744233B (en) * | 2015-03-31 | 2016-08-24 | 太仓沪试试剂有限公司 | A kind of purification process of glacial acetic acid |
| US10793502B2 (en) | 2016-12-19 | 2020-10-06 | Sabic Global Technologies B.V. | Method of purifying acetic acid |
| CN107216247B (en) * | 2017-07-20 | 2018-04-03 | 台山市新宁制药有限公司 | A kind of preparation method of medicinal glacial acetic acid |
| CN107382711A (en) * | 2017-08-29 | 2017-11-24 | 湖北工程学院 | Chromatographically pure glacial acetic acid and preparation method thereof, production system |
| CN110589784B (en) * | 2019-10-08 | 2021-11-23 | 中国计量科学研究院 | Fine series purification system and purification method for laboratory-grade ultrapure nitric acid |
-
2003
- 2003-12-16 CN CN 200310109477 patent/CN1285560C/en not_active Expired - Lifetime
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2012062299A (en) * | 2010-09-17 | 2012-03-29 | Shanghai Huayi Microelectric Material Co Ltd | Method for producing high-purity electronic grade acetic acid |
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| CN1562938A (en) | 2005-01-12 |
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Owner name: SHANGHAI HUAYI ENERGY + CHEMICAL INDUSTRY CO., LTD Free format text: FORMER OWNER: WUJING CHEMICAL CO., LTD., SHANGHAI Effective date: 20150119 |
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Effective date of registration: 20150119 Address after: 200241 Minhang District, Wu Long Road, No. 4280, Shanghai Patentee after: SHANGHAI HUAYI ENERGY CHEMICAL CO.,LTD. Address before: 200241 No. 4600, Wu Long Road, Shanghai, Minhang District Patentee before: Shanghai Wujing Chemical Co.,Ltd. |
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