CN1410408A - Refining method of carbon 11-18 long chain diacid - Google Patents
Refining method of carbon 11-18 long chain diacid Download PDFInfo
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- CN1410408A CN1410408A CN 01142806 CN01142806A CN1410408A CN 1410408 A CN1410408 A CN 1410408A CN 01142806 CN01142806 CN 01142806 CN 01142806 A CN01142806 A CN 01142806A CN 1410408 A CN1410408 A CN 1410408A
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Abstract
A process for refining (or purifying) C11-18 long-chain dibasic acid includes such steps as dissolving the said long-chain dibasic acid prepared by fermenting petroleum in organic solvent, filtering, cooling the filtrate, crystallizing and drying. Its advantages are high purity and output rate, and low cost.
Description
Technical field
The present invention relates to a kind of carbon 11-18 long-chain biatomic acid process for purification, belong to the refining purification techniques of long-chain biatomic acid.
Background technology
The method of producing long-chain biatomic acid at present both at home and abroad mainly contains two kinds, and a kind of is chemical synthesis, is raw material with the divinyl, produces long-chain biatomic acid by high pressure polymerisation, purity height, but complex process, and dangerous big, yield is low, and raw material is expensive, the cost height; Another kind method is a biological fermentation process, utilize the special oxidation capacity of microorganism, two terminal methyls of oxidation normal paraffin, and produce the diprotic acid identical with the matrix carbochain, technology is simple, safety is easy to operate, the yield height, and cost of material is low, but foreign matter content height, purity is low, and is of poor quality, seriously restricted its range of application.
Summary of the invention
Technical problem to be solved by this invention is: a kind of carbon 11-18 long-chain biatomic acid process for purification is provided, and operational path is short, and safety is easy to operate, and cost is low, the yield height, and the product purity height, quality is good.
Carbon 11-18 long-chain biatomic acid process for purification of the present invention, the long-chain biatomic acid that petroleum fermentation is produced is dissolved in the organic solvent, removes by filter impurity, with filtrate cool, crystallization separates out diprotic acid, must make with extra care diprotic acid after the drying again.
Petroleum fermentation is produced long-chain biatomic acid, adjusts extracting method, combines with purification techniques again, can obtain purity height, the measured product of matter, and the yield height.
The extracting method of the long-chain biatomic acid that petroleum fermentation is produced is:
To ferment stop buffer under 30～90 ℃ of temperature, in alkaline environment, PH10～14, standing demix, take out fermentation clear liquid and thalline respectively and add gac 50～90 ℃ of decolourings, remove thalline, the clear liquid acidifying of will decolouring again, control PH3～4,50～95 ℃ of following crystallizations, filter, wash again diprotic acid crystallization filter cake, final drying gets diprotic acid dry powder.
Washing is to removing impurity, improving product purity and have very great help.
The organic solvent of dissolving long-chain biatomic acid is that ketone, alcoholic solvent are better, is the best with preferred acetone, methyl alcohol, ethanol.
Consumption of organic solvent is: the mass ratio of diprotic acid dry powder and solvent is 1: 1～8.
It is best to add gac in the refining batching, and proportion scale is:
The mass ratio of diprotic acid dry powder, gac, organic solvent is 1: 0.01～0.1: 1～8.
The dissolving controlled temperature is: 30～80 ℃, generally with the boiling point decision of organic solvent, dissolution process will constantly stir.
Not specified (NS) part of the present invention, operational requirement gets final product routinely.
Process for purification operational path of the present invention is short, and safety is easy to operate, and cost is low, the yield height, and the product purity height, quality is good, and total acid reaches more than 99.5%.Be convenient to realize large-scale industrial production.
Embodiment
The invention will be further described below in conjunction with embodiment.
Embodiment 1
Carbon 11-18 long-chain biatomic acid process for purification of the present invention utilizes petroleum fermentation to produce long-chain biatomic acid and goes on foot and carry out according to extraction, purification two:
(1) extracts
The stop buffer that will ferment is heated to 60～70 ℃, adds industrial sodium hydroxide alkali lye and adjusts solution PH 12, is warming up to 90 ℃ again, squeeze into the standing demix jar, standing demix 25 hours, (that is: the upper strata is an oil reservoir to be divided into upper, middle and lower-ranking, the middle layer is a supernatant liquid, lower floor is the thalline layer), oil reservoir is recycled, and clear liquid and lower floor's thalline are squeezed into bleacher respectively in the middle of taking out, and add entry and make acid content be controlled at 6%, the gac of adding 0.9% is warming up to 70～80 ℃, is pressed into the sheet frame decolouring.Treat that clear liquid is little when yellow, squeezes into crystallizer (can remove thalline in decolorization) with clear liquid, when the clear liquid that will decolour is warming up to 60～70 ℃, in crystallizer, add concentration at the vitriol oil more than 93%, be controlled at PH3～4, open motor simultaneously and stir, crystallization finishes and is warming up to 70～90 ℃ again, naturally after lowering the temperature 10 hours then, use cooling water temperature again, reduce to room temperature after, filter, the washing, with the crystallization filter cake dry up, dry long-chain biatomic acid dry powder.
(2) purify
Long-chain biatomic acid dry powder, gac, ethanol that petroleum fermentation is produced add in the molten sour still in 1: 0.06: 5 ratio of mass ratio, seal the material mouth, start molten sour still agitator motor, and slowly in chuck, feed steam and make molten sour still be warming up to 50～70 ℃, the steam off valve filters (filtrate should be as clear as crystal) to the diprotic acid saturated solution, filtrate is squeezed in the crystallization kettle cool, crystallization, take out the crystallization centrifuge dripping, dry refining diprotic acid.Total acid is 99.8%.
Embodiment 2
Carbon 11-18 long-chain biatomic acid process for purification of the present invention utilizes petroleum fermentation to produce long-chain biatomic acid and goes on foot and carry out according to extraction, purification two:
The stop buffer that will ferment is heated to 70～90 ℃, adds industrial sodium hydroxide alkali lye and adjusts solution PH 13, squeezes into the standing demix jar, and standing demix 30 hours is divided into upper, middle and lower-ranking.Clear liquid and lower floor's thalline are squeezed into bleacher respectively in the middle of taking out, and add entry and make acid content be controlled at 8%, add 1% gac, are warming up to 60～70 ℃, are pressed into the sheet frame decolouring.Treat that clear liquid is little when yellow, clear liquid is squeezed into crystallizer, and when the clear liquid that will decolour was warming up to 50～70 ℃, adding concentration was 93% the vitriol oil in crystallizer, be controlled at about PH3, open motor simultaneously and stir, crystallization finishes and is warming up to 80～90 ℃ again, lowers the temperature 12 hours naturally then, use cooling water temperature again, after reducing to room temperature, filter, wash, at last crystallization is dried up, dries long-chain biatomic acid dry powder.
(2) purify
Long-chain biatomic acid dry powder, gac, methyl alcohol that petroleum fermentation is produced add in the molten sour still in 1: 0.1: 4 ratio of mass ratio, seal the material mouth, start molten sour still agitator motor, and slowly in chuck, feed steam and make molten sour still be warming up to 40～60 ℃, close down steam, diprotic acid solution is filtered, filtrate squeezed in the crystallization kettle cool, crystallization, take out crystallization, behind the centrifuge dripping, dry refining diprotic acid.Total acid is 99.7%.
Embodiment 3
Carbon 11-18 long-chain biatomic acid process for purification of the present invention utilizes petroleum fermentation to produce long-chain biatomic acid and goes on foot and carry out according to extraction, purification two:
The stop buffer that will ferment is heated to 40～60 ℃, adds industrial sodium hydroxide alkali lye and adjusts solution PH 11, is warming up to 90 ℃ again, squeezes into a jar standing demix jar, and standing demix 20 hours is divided into upper, middle and lower-ranking.Clear liquid and lower floor's thalline are squeezed into bleacher respectively in the middle of taking out, and add entry and make acid content be controlled at 10%, add 1.1% gac, are warming up to 70～90 ℃, are pressed into the sheet frame decolouring.Treat that clear liquid is little when yellow, squeezes into crystallizer with clear liquid, when the clear liquid that will decolour is warming up to 60～80 ℃, adding concentration is 94% the vitriol oil in crystallizer, be controlled at about PH4, open motor simultaneously and stir, crystallization finishes and is warming up to 70～80 ℃ again, naturally after lowering the temperature 16 hours then, use cooling water temperature again, reduce to room temperature after, filter, the washing, with the crystallization filter cake dry up, dry long-chain biatomic acid dry powder.
(2) purify
Long-chain biatomic acid dry powder, gac, acetone that petroleum fermentation is produced add in the molten sour still in 1: 0.012: 4 ratio of mass ratio, seal the material mouth, start molten sour still agitator motor, and slowly in chuck, feed steam and make molten sour still be warming up to 50～55 ℃, stop steam, diprotic acid solution is filtered, filtrate squeezed in the crystallization kettle cool, crystallization, take out crystallization, behind the centrifuge dripping, dry refining diprotic acid.Total acid is 99.8%.
Claims (11)
1, a kind of carbon 11-18 long-chain biatomic acid process for purification is characterized in that the long-chain biatomic acid that petroleum fermentation is produced is dissolved in the organic solvent, removes by filter impurity, with filtrate cool, crystallization separates out diprotic acid, must make with extra care diprotic acid after the drying.
2, process for purification according to claim 1, the organic solvent that it is characterized in that dissolving long-chain biatomic acid is alcohols, organic solvent of ketone.
3, process for purification according to claim 1 is characterized in that organic solvent is acetone, methyl alcohol, ethanol.
4, process for purification according to claim 3, it is characterized in that consumption of organic solvent is: the mass ratio of diprotic acid dry powder and solvent is 1: 1～8.
5, process for purification according to claim 4 is characterized in that being added with gac in the refining batching.
6, process for purification according to claim 5 is characterized in that proportion scale is:
The mass ratio of diprotic acid dry powder, gac, organic solvent is 1: 0.01～0.1: 1～8.
6, process for purification according to claim 2 is characterized in that dissolving controlled temperature and is: 30～80 ℃.
7, process for purification according to claim 2 is characterized in that dissolution process will constantly stir.
8, process for purification according to claim 1, the extracting method that it is characterized in that the long-chain biatomic acid that petroleum fermentation is produced is: will ferment stop buffer under 30～90 ℃ of temperature, standing demix in alkaline environment takes out fermentation clear liquid and thalline respectively and adds activated carbon decolorizing, removes thalline simultaneously, the clear liquid acidifying of will decolouring again, PH is 3～4 in control, and crystallization is filtered, wash again diprotic acid crystallization filter cake, final drying gets diprotic acid dry powder.
9, process for purification according to claim 8 is characterized in that Tc is controlled to be 50～95 ℃.
10, process for purification according to claim 8 is characterized in that the alkaline environment requirement is PH10～14.
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| Application Number | Priority Date | Filing Date | Title |
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| CN 01142806 CN1410408A (en) | 2001-12-21 | 2001-12-21 | Refining method of carbon 11-18 long chain diacid |
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| CN 01142806 CN1410408A (en) | 2001-12-21 | 2001-12-21 | Refining method of carbon 11-18 long chain diacid |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101985416A (en) * | 2010-04-30 | 2011-03-16 | 山东瀚霖生物技术有限公司 | Refining technology for producing long carbon chain dicarboxylic acid by using biological fermentation process |
| CN102503800A (en) * | 2011-10-12 | 2012-06-20 | 江南大学 | Refining method of C11-C18 long-chain diacid |
| CN101698859B (en) * | 2009-09-11 | 2012-07-18 | 淄博广通化工有限责任公司 | Production method of n-hexadecyl dibasic acid |
| CN102795989A (en) * | 2012-08-28 | 2012-11-28 | 淄博广通化工有限责任公司 | Method for refining dodecanedioic acid |
| CN102911036A (en) * | 2011-08-01 | 2013-02-06 | 中国石油化工股份有限公司 | Method for obtaining high pure dicarboxylic acid |
| CN103113209A (en) * | 2013-02-05 | 2013-05-22 | 徐杰 | Method for removing organic amine nitrogen impurities from long chain binary acid produced by using microbiological method |
| CN103804172A (en) * | 2012-11-08 | 2014-05-21 | 中国石油化工股份有限公司 | Method for improving organic acid product quality |
| CN104529741A (en) * | 2014-12-26 | 2015-04-22 | 淄博广通化工有限责任公司 | Purification method of long-carbon-chain dicarboxylic acid |
| CN108947809A (en) * | 2017-05-18 | 2018-12-07 | 中国石油化工股份有限公司 | A method of extracting simultaneously refining long-chain dicarboxylic acids from fermentation liquid |
| CN111099987A (en) * | 2018-10-26 | 2020-05-05 | 中国石油化工股份有限公司 | Refining method of long-chain dicarboxylic acid in fermentation liquor |
| CN115093319A (en) * | 2022-06-25 | 2022-09-23 | 宁夏中科生物新材料有限公司 | Novel method for decoloring activated carbon of long-carbon-chain dibasic acid fermentation liquor |
-
2001
- 2001-12-21 CN CN 01142806 patent/CN1410408A/en active Pending
Cited By (19)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101698859B (en) * | 2009-09-11 | 2012-07-18 | 淄博广通化工有限责任公司 | Production method of n-hexadecyl dibasic acid |
| CN101985416B (en) * | 2010-04-30 | 2016-11-09 | 上海凯赛生物技术研发中心有限公司 | Biological fermentation process produces the process for refining of long carbochain biatomic acid |
| CN101985416A (en) * | 2010-04-30 | 2011-03-16 | 山东瀚霖生物技术有限公司 | Refining technology for producing long carbon chain dicarboxylic acid by using biological fermentation process |
| CN102911036A (en) * | 2011-08-01 | 2013-02-06 | 中国石油化工股份有限公司 | Method for obtaining high pure dicarboxylic acid |
| CN102503800B (en) * | 2011-10-12 | 2014-06-18 | 江南大学 | Refining method of C11-C18 long-chain diacid |
| CN102503800A (en) * | 2011-10-12 | 2012-06-20 | 江南大学 | Refining method of C11-C18 long-chain diacid |
| CN102795989B (en) * | 2012-08-28 | 2014-07-09 | 淄博广通化工有限责任公司 | Method for refining dodecanedioic acid |
| CN102795989A (en) * | 2012-08-28 | 2012-11-28 | 淄博广通化工有限责任公司 | Method for refining dodecanedioic acid |
| CN103804172A (en) * | 2012-11-08 | 2014-05-21 | 中国石油化工股份有限公司 | Method for improving organic acid product quality |
| CN103804172B (en) * | 2012-11-08 | 2015-11-18 | 中国石油化工股份有限公司 | A kind of method improving organic acid production quality |
| CN103113209A (en) * | 2013-02-05 | 2013-05-22 | 徐杰 | Method for removing organic amine nitrogen impurities from long chain binary acid produced by using microbiological method |
| WO2014121427A1 (en) * | 2013-02-05 | 2014-08-14 | Xu Jie | Method for removing organic amine nitrogen impurities in long-chain binary acids produced by microbiological method |
| CN103113209B (en) * | 2013-02-05 | 2015-05-06 | 徐杰 | Method for removing organic amine nitrogen impurities from long chain binary acid produced by using microbiological method |
| CN104529741A (en) * | 2014-12-26 | 2015-04-22 | 淄博广通化工有限责任公司 | Purification method of long-carbon-chain dicarboxylic acid |
| CN104529741B (en) * | 2014-12-26 | 2016-03-30 | 淄博广通化工有限责任公司 | The method of purification of Long carbon chain di-carboxylic acid |
| CN108947809A (en) * | 2017-05-18 | 2018-12-07 | 中国石油化工股份有限公司 | A method of extracting simultaneously refining long-chain dicarboxylic acids from fermentation liquid |
| CN108947809B (en) * | 2017-05-18 | 2021-08-06 | 中国石油化工股份有限公司 | Method for extracting and refining long-chain dicarboxylic acid from fermentation liquor |
| CN111099987A (en) * | 2018-10-26 | 2020-05-05 | 中国石油化工股份有限公司 | Refining method of long-chain dicarboxylic acid in fermentation liquor |
| CN115093319A (en) * | 2022-06-25 | 2022-09-23 | 宁夏中科生物新材料有限公司 | Novel method for decoloring activated carbon of long-carbon-chain dibasic acid fermentation liquor |
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