CN1660735A - Method for preparing hyperpure isopropyl alcohol - Google Patents
Method for preparing hyperpure isopropyl alcohol Download PDFInfo
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- CN1660735A CN1660735A CN 200410016616 CN200410016616A CN1660735A CN 1660735 A CN1660735 A CN 1660735A CN 200410016616 CN200410016616 CN 200410016616 CN 200410016616 A CN200410016616 A CN 200410016616A CN 1660735 A CN1660735 A CN 1660735A
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Abstract
A process for preparing superpure isopropanol from industrial isopropanol includes regulating pH value by carbonate, adding dewatering agent, reflux reaction, rectifying, distilling, and membrane filtering.
Description
Technical field
The present invention relates to a kind of preparation method of ultrapure Virahol.
Background technology
The development of information industry, various novel materials, new technology, novel process are had higher requirement to the use of associated materials, require the purity that reaches more and more higher as semi-conductor, large-scale integrated circuit to employed Virahol, develop into ultrapure Virahol (content of metal ion is the ppb level) by high-purity isopropanol (content of metal ion is the ppm level).Ultrapure Virahol is as a kind of important microelectronics chemistry product, be widely used in aspects such as cleaning in the assembling of semi-conductor, large-scale integrated circuit and the course of processing, drying, every index request reaches 12 grades-SEMI of the chemical material part C12 standard (hereinafter to be referred as SEMI C12 standard) of semiconductor equipment and material structure formulation, be that main content is greater than 99.80%, water-content is lower than 50ppm, cations is lower than 0.1ppb, and anion-content is lower than 50ppb.
In the prior art, Pure and applied Chemistry 1986, (10), 1412-1418 discloses a kind of preparation method of high-purity isopropanol, with the Virahol is raw material, adds a kind of backflow the in calcium oxide or the magnesium powder (making promoting agent with iodine), and fractional column is rectifying repeatedly, the isopropanol content that obtains is 99.94%, water-content 600ppm.The product water content height that this method obtains, if dewater with molecular sieve, foreign matter content obviously rises, and does not reach requirement.
Japanese patent laid-open 10-109948 discloses a kind of process for purification of Virahol.Add entry in the Virahol that contains the impurity element, utilize the azeotropic characteristic to add thermal distillation, remove foreign ion, Virahol is 80% in the product of distillation, and water is 20%.Because water-content is too high, the cost height that dewaters, aftertreatment difficulty.
Summary of the invention
The technical problem that the present invention solves provides a kind of preparation method of ultrapure Virahol, and is higher with the water-content and the foreign matter content that overcome product in the prior art, cost height, the deficiency of aftertreatment difficulty.
Technical conceive of the present invention is such:
The present invention is raw material with the industrial isopropanol, regulates pH value with carbonate, adds dewatering agent, carries out back flow reaction, through rectifying, distillation, membrane filtration, obtains target product of the present invention.
Technical scheme of the present invention:
Industrial isopropanol is regulated pH value with carbonate, add dewatering agent, reflux state keeps reaction 1-4 hour down, and through multistage serialization rectifying, distillation, membrane filtration, the granule number of control filtered solution is collected target product in purifying box.
According to the present invention, industrial isopropanol is regulated pH value to 5.5-7.5 with anhydrous sodium carbonate.
The said dewatering agent of the present invention is a hydrolith, and the add-on of dewatering agent is an industrial isopropanol: dewatering agent=100: 2.0-5.0 (weight ratio).
Ultrapure Virahol preparation method of the present invention adopts rectifier unit 2-4 level serialization rectifying, collects 82.0-83.0 ℃ middle runnings, filling φ 3 * 25mm glass spring filler in the rectifying column in the rectifier unit.
Ultrapure Virahol preparation method of the present invention adopts quartzy fractionation plant to distill, and collects 81.8-82.2 ℃ cut.
The present invention is that 0.1-0.2 μ m PVDF membrane (hereinafter to be referred as pvdf membrane) filters with the aperture, during filtration the aperture greater than the granule number of 0.5 μ m be controlled at 20 and below, the aperture greater than the granule number of 0.2 μ m be controlled at 200 and below.
The present invention collects finished product and carries out in charging into the purifying box that nitrogen protects.
The ultrapure isopropanol content that obtains with preparation method of the present invention is greater than 99.80%, and water-content is lower than 50ppm, and cations is lower than 0.1ppb, and anion-content is lower than 50ppb, meets SEMI C12 standard.
Industrial isopropanol material purity 98% used in the present invention, positively charged ion is more than 10ppm, and negatively charged ion is about 3000-5000ppm.
The present invention compared with prior art, the product purity height, foreign matter content is low, and is simple to operate, steady quality meets SEMI C12 standard, is suitable for suitability for industrialized production.
Embodiment
The invention will be further described below by embodiment, but embodiment does not limit protection scope of the present invention.
Embodiment 1
In the there-necked flask of 5000ml, input is 5.5 98% industrial isopropanol 3000ml with anhydrous sodium carbonate adjusting pH value, hydrolith 5g, reflux 2 hours, through 2 grades of serialization rectifying of rectifier unit (φ 3 * 25mm glass spring filler is housed in the rectifying column), temperature is controlled at 82.0-83.0 ℃, collects middle runnings in the quartzy there-necked flask of 2000ml; Reflux 1.5 hours, in quartzy fractionation plant, collect 81.8-82.2 ℃ cut, with the aperture is that the pvdf membrane of 0.1 μ m carries out membrane filtration, during filtration the aperture greater than the granule number of 0.5 μ m be controlled at 20 and below, the aperture greater than the granule number of 0.2 μ m be controlled at 200 and below; In the purifying box that charges into nitrogen in advance, collect target product, obtain ultrapure Virahol 1800ml, sampling analysis, analytical data sees Table 1.
Embodiment 2
In the there-necked flask of 5000ml, input is 7.0 98% industrial isopropanol 3000ml with anhydrous sodium carbonate adjusting pH value, hydrolith 3g, reflux 3 hours, through 2 grades of serialization rectifying of rectifier unit (φ 3 * 25mm glass spring filler is housed in the rectifying column), temperature is controlled at 82.0-83.0 ℃, collects middle runnings in the quartzy there-necked flask of 2000ml; Reflux 1.5 hours, in quartzy fractionation plant, collect 81.8-82.2 ℃ cut, with the aperture is that the pvdf membrane of 0.1 μ m carries out membrane filtration, during filtration the aperture greater than the granule number of 0.5 μ m be controlled at 20 and below, the aperture greater than the granule number of 0.2 μ m be controlled at 200 and below; In the purifying box that charges into nitrogen in advance, collect target product, obtain ultrapure Virahol 1800ml, sampling analysis, analytical data sees Table 1.
Table 1
| Project | Unit | SEMI C12 standard | Embodiment 1 | Embodiment 2 |
| Colourity | ????APHA | ????10 | ????5 | ????5 |
| Isopropanol content | ????％ | ????＞99.80 | ????99.99 | ????99.98 |
| Water-content | ????ppm | ????＜50 | ????30 | ????0.004 |
| Residue on evaporation | ????ppm | ????＜1.0 | ????0.5 | ????0.5 |
| Muriate (Cl) | ????ppb | ????＜50 | Do not detect | Do not detect |
| Nitrate (NO 3) | ????ppb | ????＜50 | ????25 | ????25 |
| Phosphoric acid salt (PO 4) | ????ppb | ????＜50 | ????20 | ????25 |
| Vitriol (SO 4) | ????ppb | ????＜50 | ????25 | ????25 |
| Aluminium (Al) | ????ppb | ????＜0.1 | ????0.06 | ????0.08 |
| Arsenic (As) | ????ppb | ????＜0.1 | ????0.05 | ????0.09 |
| Barium (Ba) | ????ppb | ????＜0.1 | ????0.09 | ????0.10 |
| Boron (B) | ????ppb | ????＜0.1 | ????0.05 | ????0.05 |
| Calcium (Ca) | ????ppb | ????＜0.1 | ????0.10 | ????0.10 |
| Copper (Cu) | ????ppb | ????＜0.1 | ????0.05 | ????0.05 |
| Iron (Fe) | ????ppb | ????＜0.1 | ????0.10 | ????0.10 |
| Plumbous (Pb) | ????ppb | ????＜0.1 | ????0.05 | ????0.08 |
| Magnesium (Mg) | ????ppb | ????＜0.1 | ????0.05 | ????0.07 |
| Manganese (Mn) | ????ppb | ????＜0.1 | Do not detect | Do not detect |
| Nickel (Ni) | ????ppb | ????＜0.1 | Do not detect | Do not detect |
| Potassium (K) | ????ppb | ????＜0.1 | ????0.08 | ????0.10 |
| Sodium (Na) | ????ppb | ????＜0.1 | ????0.10 | ????0.10 |
| Tin (Sn) | ????ppb | ????＜0.1 | Do not detect | Do not detect |
| Titanium (Ti) | ????ppb | ????＜0.1 | Do not detect | Do not detect |
| Zinc (Zn) | ????ppb | ????＜0.1 | ????0.05 | ????0.07 |
Analytical procedure wherein, colourity is reference colour with platinum-cobalt reference liquid, analyze with visual colorimetry, isopropanol content adopts gas chromatographic analysis, water-content adopts the analysis of karl Fischer method, residue on evaporation weighting method analysis, positively charged ion adopts plasma mass spectrum (ICP-MS) analysis, and negatively charged ion adopts ion-exchange chromatogram analysis.
Claims (10)
1. the preparation method of a ultrapure Virahol, it is characterized in that may further comprise the steps: industrial isopropanol is regulated pH value with carbonate, add dewatering agent, reflux state keeps reaction 1-4 hour down, through multistage serialization rectifying, distillation, membrane filtration, the granule number of control filtered solution is collected target product in purifying box.
2. preparation method according to claim 1 is characterized in that it is 5.5-7.5 that industrial isopropanol is regulated pH value with anhydrous sodium carbonate.
3. preparation method according to claim 1 is characterized in that dewatering agent is a hydrolith.
4. preparation method according to claim 1, the consumption that it is characterized in that dewatering agent is an industrial isopropanol: dewatering agent=100: 2.0-5.0 (weight ratio).
5. preparation method according to claim 1 is characterized in that adopting rectifier unit to carry out 2-4 level serialization rectifying, collects 82.0-83.0 ℃ middle runnings.
6. preparation method according to claim 1 is characterized in that filling φ 3 * 25mm glass spring filler in the rectifying column in the rectifier unit.
7. preparation method according to claim 1 is characterized in that adopting quartzy fractionation plant to distill, and collects 81.8-82.2 ℃ cut.
8. preparation method according to claim 1, it is characterized in that adopting the aperture is that 0.1-0.2 μ m poly(vinylidene fluoride) (PVDF) film carries out membrane filtration.
9. preparation method according to claim 1, the granule number span of control of filtered solution when it is characterized in that filtering: the aperture greater than the granule number of 0.5 μ m 20 and below, the aperture greater than the granule number of 0.2 μ m 200 and below.
10. preparation method according to claim 1 is characterized in that collecting finished product in charging into the purifying box that nitrogen protects.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004100166164A CN100398502C (en) | 2004-02-27 | 2004-02-27 | Method for preparing hyperpure isopropyl alcohol |
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|---|---|---|---|
| CNB2004100166164A CN100398502C (en) | 2004-02-27 | 2004-02-27 | Method for preparing hyperpure isopropyl alcohol |
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| CN1660735A true CN1660735A (en) | 2005-08-31 |
| CN100398502C CN100398502C (en) | 2008-07-02 |
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102060663A (en) * | 2009-11-18 | 2011-05-18 | 天津市康科德科技有限公司 | Method for preparing chromatographic pure isopropanol |
| CN101362675B (en) * | 2008-09-16 | 2011-05-25 | 江阴市润玛电子材料有限公司 | Method for preparing super-clean and high-purity isopropanol and apparatus thereof |
| CN102249964A (en) * | 2011-05-27 | 2011-11-23 | 连云港升南化学有限公司 | Process for preparing isooctyl thioglycolate |
| CN102399179A (en) * | 2010-09-17 | 2012-04-04 | 上海化学试剂研究所 | Production process for ultra-pure N-methylpyrrolidone |
| CN102755759A (en) * | 2012-07-27 | 2012-10-31 | 福州大学 | Continuous reaction rectification process and rectification equipment for synthesizing isopropyl alcohol |
| CN104744213A (en) * | 2013-12-31 | 2015-07-01 | 上海星可高纯溶剂有限公司 | Method for purifying chromatographic grade isopropanol |
| CN105085184A (en) * | 2014-05-16 | 2015-11-25 | 上海星可高纯溶剂有限公司 | Purification method of isopropyl alcohol for liquid chromatography-mass spectrometer |
| CN105085183A (en) * | 2014-05-16 | 2015-11-25 | 上海星可高纯溶剂有限公司 | Purification method of chromatographic-grade isopropanol |
| CN107382668A (en) * | 2017-08-29 | 2017-11-24 | 湖北工程学院 | Chromatographic pure isopropanol and preparation method thereof, production system |
| CN108250040A (en) * | 2018-01-11 | 2018-07-06 | 福建华夏蓝新材料科技有限公司 | A kind of method that alcohol solution separates and recovers in high purity aluminium oxide production |
| CN112723994A (en) * | 2020-12-30 | 2021-04-30 | 镇江润晶高纯化工科技股份有限公司 | Purification method of semiconductor grade isopropanol |
| CN112771016A (en) * | 2018-10-03 | 2021-05-07 | 株式会社德山 | High-purity isopropyl alcohol and method for producing same |
| CN115322074A (en) * | 2022-07-06 | 2022-11-11 | 晶瑞(湖北)微电子材料有限公司 | Purification method of isopropanol |
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| CN102398895B (en) * | 2010-09-16 | 2014-09-24 | 上海化学试剂研究所 | Production method of ultra-pure electronic grade chemical reagent |
-
2004
- 2004-02-27 CN CNB2004100166164A patent/CN100398502C/en not_active Expired - Fee Related
Cited By (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101362675B (en) * | 2008-09-16 | 2011-05-25 | 江阴市润玛电子材料有限公司 | Method for preparing super-clean and high-purity isopropanol and apparatus thereof |
| CN102060663A (en) * | 2009-11-18 | 2011-05-18 | 天津市康科德科技有限公司 | Method for preparing chromatographic pure isopropanol |
| CN102399179A (en) * | 2010-09-17 | 2012-04-04 | 上海化学试剂研究所 | Production process for ultra-pure N-methylpyrrolidone |
| CN102399179B (en) * | 2010-09-17 | 2014-06-18 | 上海化学试剂研究所 | Production process for ultra-pure N-methylpyrrolidone |
| CN102249964A (en) * | 2011-05-27 | 2011-11-23 | 连云港升南化学有限公司 | Process for preparing isooctyl thioglycolate |
| CN102755759A (en) * | 2012-07-27 | 2012-10-31 | 福州大学 | Continuous reaction rectification process and rectification equipment for synthesizing isopropyl alcohol |
| CN102755759B (en) * | 2012-07-27 | 2014-08-06 | 福州大学 | Continuous reaction rectification process and rectification equipment for synthesizing isopropyl alcohol |
| CN104744213A (en) * | 2013-12-31 | 2015-07-01 | 上海星可高纯溶剂有限公司 | Method for purifying chromatographic grade isopropanol |
| CN105085184A (en) * | 2014-05-16 | 2015-11-25 | 上海星可高纯溶剂有限公司 | Purification method of isopropyl alcohol for liquid chromatography-mass spectrometer |
| CN105085183A (en) * | 2014-05-16 | 2015-11-25 | 上海星可高纯溶剂有限公司 | Purification method of chromatographic-grade isopropanol |
| CN107382668A (en) * | 2017-08-29 | 2017-11-24 | 湖北工程学院 | Chromatographic pure isopropanol and preparation method thereof, production system |
| CN108250040A (en) * | 2018-01-11 | 2018-07-06 | 福建华夏蓝新材料科技有限公司 | A kind of method that alcohol solution separates and recovers in high purity aluminium oxide production |
| CN112771016A (en) * | 2018-10-03 | 2021-05-07 | 株式会社德山 | High-purity isopropyl alcohol and method for producing same |
| CN112723994A (en) * | 2020-12-30 | 2021-04-30 | 镇江润晶高纯化工科技股份有限公司 | Purification method of semiconductor grade isopropanol |
| CN115322074A (en) * | 2022-07-06 | 2022-11-11 | 晶瑞(湖北)微电子材料有限公司 | Purification method of isopropanol |
| CN115322074B (en) * | 2022-07-06 | 2024-02-20 | 晶瑞(湖北)微电子材料有限公司 | Purification method of isopropanol |
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