CN103601624A - Preparation method for ultra pure acetone - Google Patents
Preparation method for ultra pure acetone Download PDFInfo
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- CN103601624A CN103601624A CN201310632156.7A CN201310632156A CN103601624A CN 103601624 A CN103601624 A CN 103601624A CN 201310632156 A CN201310632156 A CN 201310632156A CN 103601624 A CN103601624 A CN 103601624A
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- acetone
- preparation
- molecular sieve
- ultrapure
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
- C07C45/78—Separation; Purification; Stabilisation; Use of additives
- C07C45/79—Separation; Purification; Stabilisation; Use of additives by solid-liquid treatment; by chemisorption
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
- C07C45/78—Separation; Purification; Stabilisation; Use of additives
- C07C45/85—Separation; Purification; Stabilisation; Use of additives by treatment giving rise to a chemical modification
Abstract
The invention discloses a preparation method for ultra pure acetone. The preparation method comprises the following steps removing foreign ions in industrial acetone by using a disodium ethylene diamine tetraacetate surface modified mesoporous silica adsorbent; carrying out distillation in the presence of the oxidizing agent potassium permanganate so as to remove organic impurities; removing water by using a molecular sieve; and carrying out membrane filtration by using a cellulose acetate microporous membrane so as to prepare the target product ultra pure acetone. The ultra pure acetone prepared by using the method has purity of more than 99.5% and water content of less than 0.5%; according to detection results, the contents of foreign ions in the target product are all smaller than index values, and the number of granular impurities with a size of greater than 10 mu m is less than 10ml, according with the standard SEMI C1.2-96.
Description
Technical field
The present invention relates to a kind of preparation method of ultrapure acetone, the ultrapure acetone making can reach the chemical materials part SEMI C1.2-96 standard-required of semiconductor equipment and material structure formulation.
Background technology
Acetone is important organic synthesis raw material, for the production of epoxy resin, and polycarbonate, synthetic glass, medicine, agricultural chemicals etc.; Also be good solvent, for coating, cakingagent, steel cylinder acetylene etc.; Also be used as thinner, clean-out system, extraction agent; Still manufacture the important source material of aceticanhydride, Pyranton, chloroform, iodoform, epoxy resin, polyisoprene rubber, methyl methacrylate etc.
In microelectronics industry, semicon industry, the purity of acetone and cleanliness factor have very important impact to the yield rate of electronic product, electrical property and reliability.In recent years, high speed development along with semiconductor technology, supporting with it ultrapure acetone is had higher requirement, require particle and foreign matter content to be reduced to 1-3 the order of magnitude, reach the chemical materials part SEMI C1.2-96 standard that semiconductor equipment and material structure are formulated.
In prior art, the purifying of technical grade acetone adopts the method for absorption, rectifying to prepare conventionally, take industrial acetone as raw material, by steps such as resin anion(R.A), resin cation (R.C.)s, carries out adsorption treatment, through multistage rectification, obtains highly purified acetone.
The method of Chinese patent 201010102368.0 is removed impurity with the means of multistep extracting rectifying, this method complex operation, and the factor that is easily subject to environment in operating process affects quality product.
[the Zhou Shuzhen such as Zhou Shuzhen, Li Tao, Li Yu, Ren Baozeng, high pure acetone Study on Preparation, Henan chemical industry [J], 2010,27 (3): 33-34] take analytical pure acetone as raw material, adopt the method for two-stage sub-boiling distillation to prepare high pure acetone, but there is technology controlling and process difficulty in this method, production capacity is low, the high deficiency of energy consumption.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of ultrapure acetone, to overcome prior art, produce high pure acetone complex operation, production capacity is low, the deficiency that energy consumption is higher.
For achieving the above object, the present invention mainly adopts following technical scheme:
A preparation method for ultrapure acetone, is characterized in that, comprises the steps:
1) will be through Na
2the mesoporous silicon oxide sorbent material of EDTA finishing adds in industrial acetone, under the condition of 20-30 ℃, stirs 6-8 hour, and suction filtration is removed sorbent material, collects filtrate;
2) filtrate of collection is proceeded to rectifier unit, add solid potassium permanganate, total reflux 2-4 hour, then collects the cut of 56.0-56.5 ℃;
3) by adding the standing 8-12 hour of molecular sieve in the cut of collection, remove by filter molecular sieve, collect filtrate;
4) filtrate of collection is carried out to membrane filtration by acetyl cellulose micropore filtering film, obtain target product ultrapure acetone.
Further, the industrial acetone described in step 1) with through Na
2the mass ratio of the mesoporous silicon oxide sorbent material of EDTA finishing is 1:0.1-0.3, g/g.
And, step 2) in potassium permanganate and step 1) the mass ratio of industrial acetone be 1:10-30, g/g.
Again, step 2), reflux ratio is 1:0.5-3.
Again, in the molecular sieve described in step 3) and step 1), the mass ratio of industrial acetone is 1:3-5.
Described molecular sieve is a kind of in 3A molecular sieve, 4A molecular sieve or 5A molecular sieve.Molecular sieve is preferably 4A molecular sieve.
Further, the aperture of the acetyl cellulose micropore filtering film described in step 4) is 0.10-0.22 μ m.
Used in the present invention through disodium ethylene diamine tetraacetate (Na
2eDTA) the mesoporous silicon oxide sorbent material of finishing can prepare according to the method for Nankai University's Ph D dissertation " mild conditions of mesoporous silicon oxide is synthetic " report.
Compared with prior art, beneficial effect of the present invention is:
(1) use through disodium ethylene diamine tetraacetate (Na
2eDTA) the mesoporous silicon oxide sorbent material of finishing, 4A molecular sieve all can regenerations, can effectively reduce the impact on environment, meet the requirement of environmental protection, the target product ultrapure acetone steady quality obtaining, good impurity removing effect, easy and simple to handle, be suitable for suitability for industrialized production.
(2) through disodium ethylene diamine tetraacetate (Na
2eDTA) the mesoporous silicon oxide sorbent material pore distribution of finishing is uniform and stable, is six side's ordered arrangement and aperture adjustable, and the mesoporous material surface after activation has abundant silicon hydroxyl, and the inorganic salts foreign ion in acetone is had to desirable adsorption effect.
(3) in rectifying, adding potassium permanganate, can be that high boiling component is able to by rectifying it and acetone separation by the oxidation of impurities in acetone, as being formic acid, acetic acid by methyl alcohol, oxidation of ethanol; The mass ratio that simultaneously can control itself and industrial acetone, limits its consumption, effectively raising rectification efficiency.
(4) the ultrapure acetone purity obtaining by the inventive method is more than 99.5%, water-content is below 0.5%, and after testing, the content of target product foreign ion is all lower than desired value, be greater than the number of 1.0 μ m granule foreigns lower than 10/ml, meet SEMI C1.2-96 standard.
Embodiment
Below by specific embodiment, the present invention is described further, but embodiment does not limit the scope of the invention.
Embodiment 1
By 100g through Na
2the mesoporous silicon oxide sorbent material of EDTA finishing joins in 1000g industrial acetone, the conditions of 25 ℃, stir 6 hours, remove by filter sorbent material, the filtrate of gained proceeds in rectifier unit, add 35g solid potassium permanganate, total reflux 2 hours, then under the condition that is 2:1 in reflux ratio, collect the cut of 56.0-56.5 ℃, obtain acetone 920g, add 100g4A molecular sieve, standing 12 hours, remove by filter molecular sieve, the acetyl cellulose micropore filtering film that filtrate is 0.22 μ m by aperture filters, and obtains target product ultrapure acetone 890g.
Embodiment 2
By 300g through Na
2the mesoporous silicon oxide sorbent material of EDTA finishing joins in 1000g industrial acetone, the conditions of 30 ℃, stir 8 hours, remove by filter sorbent material, the filtrate of gained proceeds in rectifier unit, add 100g solid potassium permanganate, total reflux 4 hours, then under the condition that is 1:3 in reflux ratio, collect the cut of 56.0-56.5 ℃, obtain acetone 900g, add 180g4A molecular sieve, standing 8 hours, remove by filter molecular sieve, the acetyl cellulose micropore filtering film that filtrate is 0.22 μ m by aperture filters, and obtains target product ultrapure acetone 860g.
Ultrapure acetone purity detecting result prepared by embodiment is as follows, the instrument that wherein analytical procedure is used is as follows: water-content adopts karl Fischer moisture content tester, metal ion adopts plasma mass spectrograph (ICP-MS), and negatively charged ion adopts ionic liquid phase chromatographic instrument (IC):
The detected result of table 1 ultrapure acetone standard and analytical results embodiment
As shown in Table 1, the ultrapure acetone being made by preparation method provided by the invention, its impurity ion content is all far below the desired value in SEMI C1.2-96 standard, and preparation technology is simple, use through disodium ethylene diamine tetraacetate (Na
2eDTA) the mesoporous silicon oxide sorbent material of finishing, 4A molecular sieve all can regenerations, can effectively reduce the impact on environment, meet the requirement of environmental protection, the target product ultrapure acetone steady quality obtaining, good impurity removing effect, easy and simple to handle, be suitable for suitability for industrialized production.
It should be noted that, above embodiment is only unrestricted in order to technical scheme of the present invention to be described.Although the present invention is had been described in detail with reference to preferred embodiment, those of ordinary skill in the art is to be understood that, can modify or be equal to replacement the technical scheme of invention, and not depart from the scope of technical solution of the present invention, it all should be encompassed in claim scope of the present invention.
Claims (8)
1. a preparation method for ultrapure acetone, is characterized in that, comprises the steps:
1) will be through Na
2the mesoporous silicon oxide sorbent material of EDTA finishing adds in industrial acetone, under the condition of 20-30 ℃, stirs 6-8 hour, and suction filtration is removed sorbent material, collects filtrate;
2) filtrate of collection is proceeded to rectifier unit, add solid potassium permanganate, total reflux 2-4 hour, then collects the cut of 56.0-56.5 ℃;
3) by adding the standing 8-12 hour of molecular sieve in the cut of collection, remove by filter molecular sieve, collect filtrate;
4) filtrate of collection is carried out to membrane filtration by acetyl cellulose micropore filtering film, obtain target product ultrapure acetone.
2. the preparation method of a kind of ultrapure acetone according to claim 1, is characterized in that, the industrial acetone described in step 1) with through Na
2the mass ratio of the mesoporous silicon oxide sorbent material of EDTA finishing is 1:0.1-0.3, g/g.
3. the preparation method of a kind of ultrapure acetone according to claim 1, is characterized in that step 2) in potassium permanganate and step 1) the mass ratio of industrial acetone be 1:10-30, g/g.
4. the preparation method of a kind of ultrapure acetone according to claim 1, is characterized in that step 2) in reflux ratio be 1:0.5-3.
5. the preparation method of a kind of ultrapure acetone according to claim 1, is characterized in that, in the molecular sieve described in step 3) and step 1), the mass ratio of industrial acetone is 1:3-5.
6. a kind of preparation method of ultrapure acetone according to claim 1 or 5, is characterized in that, described molecular sieve is a kind of in 3A molecular sieve, 4A molecular sieve or 5A molecular sieve.
7. the preparation method of a kind of ultrapure acetone according to claim 6, is characterized in that, described molecular sieve is preferably 4A molecular sieve.
8. the preparation method of a kind of ultrapure acetone according to claim 1, is characterized in that, the aperture of the acetyl cellulose micropore filtering film described in step 4) is 0.10-0.22 μ m.
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| CN201310632156.7A CN103601624B (en) | 2013-12-02 | 2013-12-02 | A kind of preparation method of acetone |
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| CN201310632156.7A CN103601624B (en) | 2013-12-02 | 2013-12-02 | A kind of preparation method of acetone |
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| CN103601624A true CN103601624A (en) | 2014-02-26 |
| CN103601624B CN103601624B (en) | 2016-02-10 |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104030903A (en) * | 2014-06-25 | 2014-09-10 | 苏州晶瑞化学有限公司 | Continuous production method of ultra-clean high-purity acetone |
| CN104119216A (en) * | 2014-08-01 | 2014-10-29 | 苏州市晶协高新电子材料有限公司 | Production method of continuous acetone dehydration |
| CN105175236A (en) * | 2015-09-25 | 2015-12-23 | 江阴润玛电子材料股份有限公司 | Ultra-clean high-purity acetone production method |
| CN107410837A (en) * | 2017-04-13 | 2017-12-01 | 浙江省海洋水产研究所 | A kind of marine product dearsenification adsorbent and preparation method thereof |
| CN112378723A (en) * | 2020-11-19 | 2021-02-19 | 深圳市易瑞生物技术股份有限公司 | Sample pad for separating and concentrating target and application thereof |
| CN113735697A (en) * | 2021-08-25 | 2021-12-03 | 晶瑞电子材料股份有限公司 | Continuous production method of semiconductor grade acetone |
| CN115368227B (en) * | 2022-09-13 | 2023-09-19 | 黎明化工研究设计院有限责任公司 | Method for producing 2-ethyl anthraquinone |
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| CN101219818A (en) * | 2007-11-29 | 2008-07-16 | 复旦大学 | Process for processing and recovering acetone wastewater |
| WO2010077725A1 (en) * | 2008-12-09 | 2010-07-08 | Sabic Innovative Plastics Ip B.V. | Method for purifying acetone |
| CN101973859A (en) * | 2010-10-29 | 2011-02-16 | 上海化学试剂研究所 | Method and device for preparing ultrapure acetone |
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2013
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| CN101219818A (en) * | 2007-11-29 | 2008-07-16 | 复旦大学 | Process for processing and recovering acetone wastewater |
| WO2010077725A1 (en) * | 2008-12-09 | 2010-07-08 | Sabic Innovative Plastics Ip B.V. | Method for purifying acetone |
| CN101973859A (en) * | 2010-10-29 | 2011-02-16 | 上海化学试剂研究所 | Method and device for preparing ultrapure acetone |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104030903A (en) * | 2014-06-25 | 2014-09-10 | 苏州晶瑞化学有限公司 | Continuous production method of ultra-clean high-purity acetone |
| CN104119216A (en) * | 2014-08-01 | 2014-10-29 | 苏州市晶协高新电子材料有限公司 | Production method of continuous acetone dehydration |
| CN104119216B (en) * | 2014-08-01 | 2016-02-24 | 苏州市晶协高新电子材料有限公司 | A kind of production method of acetone serialization dehydration |
| CN105175236A (en) * | 2015-09-25 | 2015-12-23 | 江阴润玛电子材料股份有限公司 | Ultra-clean high-purity acetone production method |
| CN107410837A (en) * | 2017-04-13 | 2017-12-01 | 浙江省海洋水产研究所 | A kind of marine product dearsenification adsorbent and preparation method thereof |
| CN112378723A (en) * | 2020-11-19 | 2021-02-19 | 深圳市易瑞生物技术股份有限公司 | Sample pad for separating and concentrating target and application thereof |
| CN113735697A (en) * | 2021-08-25 | 2021-12-03 | 晶瑞电子材料股份有限公司 | Continuous production method of semiconductor grade acetone |
| CN113735697B (en) * | 2021-08-25 | 2023-12-29 | 晶瑞电子材料股份有限公司 | Continuous production method of semiconductor-grade acetone |
| CN115368227B (en) * | 2022-09-13 | 2023-09-19 | 黎明化工研究设计院有限责任公司 | Method for producing 2-ethyl anthraquinone |
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| CN103601624B (en) | 2016-02-10 |
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