CN1465556A - Process for preparing 1,2-hexandiol - Google Patents
Process for preparing 1,2-hexandiol Download PDFInfo
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- CN1465556A CN1465556A CNA021131716A CN02113171A CN1465556A CN 1465556 A CN1465556 A CN 1465556A CN A021131716 A CNA021131716 A CN A021131716A CN 02113171 A CN02113171 A CN 02113171A CN 1465556 A CN1465556 A CN 1465556A
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Abstract
The preparation method of 1,2-hexandiol with higher purity which can be up to above 99% of characterized by that it uses 1-hexene as raw material, in the system using organic acid as solvent, uses peroxide as oxidation agent, utilizes oxidation reaction to remove organic acid, adds alkali to neutralize basicity, then adds acid to regulate it to neutrality, and adopts the processes of extraction, drying and distillation so as to can obtain the invented product.
Description
Technical field: the invention belongs to the Chemicals technology of preparing, particularly a kind of 1, the preparation method of 2-hexylene glycol.
Background technology: 1, the 2-hexylene glycol is a kind of important fine chemical product, and is extensive in sector applications such as pharmacy, weaving, agricultural chemicals, makeup, senior printing ink and macromolecular materials.But, find by retrieval, 1 of present use, the purity of 2-hexylene glycol is lower, influences its result of use.
Summary of the invention: technical problem to be solved by this invention is: provide a kind of purity higher, and purity can reach 1 more than 99%, the preparation method of 2-hexylene glycol.Its preparation method is:
(1), in 1: the ratio of 6-15 is added to oxygenant in the organic acid system, stirs the 1-hexene that is incubated and slowly drips organic acid consumption 1/9-15 (mol ratio) when being warming up to 30-60 ℃;
(2), slough organic acid behind the stirring reaction 10-32 hour, adding the alkali neutralization, to make pH value be 10-14, and adjusting back to pH value with acid again is 6-8;
(3), slough organic solvent after adding organic solvent extraction, rectifying promptly.
Described oxygenant is hydrogen peroxide or calcium peroxide.
Described organic acid is formic acid or acetate or propionic acid.
Described organic solvent is vinyl acetic monomer or ritalin.
Its technique effect is: through 1 of this preparation method preparation, and the 2-hexylene glycol, its purity is greater than 99%.
Embodiment:
With 23.9g, 0.21mol hydrogen peroxide and 94.2g, 2.0mol formic acid once put in the 250ml four-hole reaction flask that stirring, condenser, thermometer are housed, stir also and slowly be warming up to 40 ℃, beginning slowly drips 12.56g, 0.15mol the 1-hexene, dropping temperature remains between 40-45 ℃, the dropping time is 3.5 hours.Stirring reaction 24 hours at room temperature then drips concentration after sloughing formic acid again under high vacuum and is 30% sodium hydroxide, and the PH that makes solution is 12-13, at room temperature stirs after 12 hours hydrochloric acid with 3N pH value=7 that neutralize, and neutral temperature is less than 20 ℃.With 55ml ethyl acetate extraction organic phase, use the saturated salt water washing organic phase of 50ml then, with sulfuric acid drying, filtration.Organic phase elder generation normal pressure is sloughed vinyl acetic monomer, and decompression steams 1, the 2-hexylene glycol under 10mmHg then.Greater than 99%, moisture content is less than 0.1% with the content of gas-chromatography monitoring cut, and yield is greater than 75%, and its reaction equation is as follows:
Claims (4)
1, a kind of preparation method of 1,2 hexylene glycol is characterized in that:
(1), in 1: the ratio of 6-15 is added to oxygenant in the organic acid system, stirs the 1-hexene that is incubated and slowly drips organic acid consumption 1/9-15 (mol ratio) when being warming up to 30-60 ℃;
(2), slough organic acid behind the stirring reaction 10-32 hour, adding the alkali neutralization, to make pH value be 10-14, and adjusting back to pH value with acid again is 6-8;
(3), slough organic solvent after adding organic solvent extraction, rectifying promptly.
2, as weighing 1 described a kind of method, it is characterized in that: described oxygenant is hydrogen peroxide or calcium peroxide.
3, as weighing 1 described a kind of method, it is characterized in that: described organic acid is formic acid or acetate or propionic acid.
4, as weighing 1 described a kind of method, it is characterized in that: described organic solvent is vinyl acetic monomer or ritalin.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB021131716A CN1228294C (en) | 2002-06-12 | 2002-06-12 | Process for preparing 1,2-hexandiol |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB021131716A CN1228294C (en) | 2002-06-12 | 2002-06-12 | Process for preparing 1,2-hexandiol |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1465556A true CN1465556A (en) | 2004-01-07 |
| CN1228294C CN1228294C (en) | 2005-11-23 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB021131716A Expired - Fee Related CN1228294C (en) | 2002-06-12 | 2002-06-12 | Process for preparing 1,2-hexandiol |
Country Status (1)
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| CN (1) | CN1228294C (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103570493A (en) * | 2013-10-31 | 2014-02-12 | 江苏紫奇化工科技有限公司 | Method for synthesizing 1,2-orthodiol through immobilized type heteropolyacid phase-transfer catalytic oxidation |
| CN106316783A (en) * | 2016-08-23 | 2017-01-11 | 张英 | Gas-liquid pipeline type preparation method of 1,2-hexanediol |
| CN107903146A (en) * | 2017-11-23 | 2018-04-13 | 大连理工大学 | A kind of method that 1 hexene of catalysis oxidation prepares 1,2 hexylene glycols |
| CN111704527A (en) * | 2020-06-24 | 2020-09-25 | 福州大学 | Method and device system for producing 1, 2-hexanediol |
| CN112778085A (en) * | 2021-01-20 | 2021-05-11 | 上海博璞诺科技发展有限公司 | 1, 2-hexanediol and purification method and application thereof |
-
2002
- 2002-06-12 CN CNB021131716A patent/CN1228294C/en not_active Expired - Fee Related
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103570493A (en) * | 2013-10-31 | 2014-02-12 | 江苏紫奇化工科技有限公司 | Method for synthesizing 1,2-orthodiol through immobilized type heteropolyacid phase-transfer catalytic oxidation |
| CN106316783A (en) * | 2016-08-23 | 2017-01-11 | 张英 | Gas-liquid pipeline type preparation method of 1,2-hexanediol |
| CN107903146A (en) * | 2017-11-23 | 2018-04-13 | 大连理工大学 | A kind of method that 1 hexene of catalysis oxidation prepares 1,2 hexylene glycols |
| CN111704527A (en) * | 2020-06-24 | 2020-09-25 | 福州大学 | Method and device system for producing 1, 2-hexanediol |
| CN111704527B (en) * | 2020-06-24 | 2021-08-31 | 福州大学 | Method and device system for producing 1, 2-hexanediol |
| CN112778085A (en) * | 2021-01-20 | 2021-05-11 | 上海博璞诺科技发展有限公司 | 1, 2-hexanediol and purification method and application thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1228294C (en) | 2005-11-23 |
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Owner name: ANHUI FENGLE CHEMICAL TECHNOLOGY CO., LTD. Free format text: FORMER OWNER: HEFEI FENGLE SCIENCE AND TECHNOLOGY CO., LTD. Effective date: 20100419 |
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Free format text: CORRECT: ADDRESS; FROM: 230031 NO.8, WEST QILITANG FENGLE AVENUE, HEFEI CITY, ANHUI PROVINCE TO: 247260 XIANGYU CHEMICAL PARK, DONGZHI COUNTY, ANHUI PROVINCE |
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Effective date of registration: 20100419 Address after: 247260 Xiang chemical garden, Dongzhi County, Anhui Province Patentee after: Anhui fengle Chemical Technology Co Ltd Address before: 8 No. 230031 Anhui province Hefei City West seven Avenue in Tang Feng Patentee before: Hefei Fengle Science and Technology Co., Ltd. |
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