CN104017034B - A kind of method that alcohol ether glucoside is isolated and purified - Google Patents
A kind of method that alcohol ether glucoside is isolated and purified Download PDFInfo
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- CN104017034B CN104017034B CN201410242301.5A CN201410242301A CN104017034B CN 104017034 B CN104017034 B CN 104017034B CN 201410242301 A CN201410242301 A CN 201410242301A CN 104017034 B CN104017034 B CN 104017034B
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- organic solvent
- alcohol ether
- ether glucoside
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Abstract
The invention belongs to extract and separate field, carry out isolated and purified method particularly to the alcohol ether glucoside for extractant, fatty alcohol-polyoxyethylene ether and glucose response obtained with organic solvent.The present invention proposes to utilize alcohol ether glucoside and fatty alcohol-polyoxyethylene ether different solubility in organic solvent, realizes the separation of the two and the purification of product by the method for extraction.This isolation technics has that technique is simple, mild condition, energy consumption are low, product recovery rate is high, purity advantages of higher.
Description
Technical field:
The invention belongs to extract and separate field, particularly to organic solvent for extractant to fatty alcohol-polyoxyethylene ether and glucose
The alcohol ether glucoside that reaction obtains carries out isolated and purified method.
Background technology:
Alcohol ether glucoside (Alkyl Ethoxy Polyglycosides is called for short AEG) is anti-with glucose by fatty alcohol-polyoxyethylene ether
The product that should obtain, also known as alcohol ether glucoside, belongs to novel green surfactant.Alcohol ether glucoside series products is nontoxic, stingless
Swashing, be readily biodegradable, have preserving moisture and protecting skin effect, can significantly reduce the zest of integral formula, low-temperature water-soluble is good,
Resistance to hard water, has good thickening effect to formula system, can compound with all kinds of active matters, stable chemical nature, to human body and
Environmental security.The performances such as excellent hard water resistance performance, mildness, compound property and the thickening of alcohol ether glucoside, solubilising, emulsifying,
Can be widely applied to laundry detergent, functional liquid detergent, cosmetics and personal-care supplies, sterilization lotion, industry help
The fields such as agent, industry cleaning link, agricultural-chemical emulsion.
Alcohol ether glucoside is fatty alcohol-polyoxyethylene ether (glucose and the fatty alcohol-polyoxyethylene ether mol ratio by glucose with excess
For 1:4～6) reaction under certain conditions obtains.Owing to product containing a large amount of unreacted fatty alcohol-polyoxyethylene ether,
And fatty alcohol-polyoxyethylene ether can affect the performance of alcohol ether glucoside, therefore, it is necessary to by fatty alcohol polyoxy second unreacted in product
Alkene ether completely removes as far as possible.At present, the isolated and purified of alcohol ether glucoside is in high temperature, fine vacuum by falling film type film evaporator
The lower unreacted fatty alcohol-polyoxyethylene ether of removing.This separating technology there is problems in that 1) due to evaporating temperature typically at 180 DEG C
Left and right, production process energy consumption is the highest；2) alcohol ether glucoside ratio of viscosities is relatively big, the most easily occurs product to be charred, line clogging
Etc. problem, the most whole production process is difficult to；3) alcohol ether glucoside at high temperature easily coking, causes post processing to take off
Color difficulty, affects product appearance, and then affects product price.
For the problems referred to above, the present invention proposes to utilize alcohol ether glucoside and fatty alcohol-polyoxyethylene ether dissolubility in organic solvent not
With, realize the separation of the two and the purification of product by the method for extraction.This technique has that technique is simple, mild condition, energy consumption
Low, product recovery rate is high, purity advantages of higher.
Summary of the invention:
It is an object of the invention to overcome current separation process energy consumption height, product to be easily charred, block place after pipeline and product
The problems such as reason is complicated, the method proposing to utilize organic solvent extraction to separate alcohol ether glucoside fatty alcohol-polyoxyethylene ether system.Organic
Solvent energy dissolved fat polyoxyethylenated alcohol also, can be able to obtain by alcohol ether glucoside mutually through distillation with the characteristic of alcohol ether glucoside layering
To more than 99% alcohol ether glucoside；Simultaneously by organic solvent through rectification, fatty alcohol-polyoxyethylene ether and organic molten can be reclaimed
Agent, and repeatable utilization.
The method that a kind of alcohol ether glucoside of the present invention is isolated and purified, its step and condition are as follows:
(1) it is made to mix homogeneously with the organic solvent stirring of its 1/2 volume alcohol ether glucoside fatty alcohol-polyoxyethylene ether system,
Operation temperature: 20～60 DEG C, pressure: 0.1～1MPa, mixing time: 5～15min, phase organic solvent phase in static formation
With lower phase alcohol ether glucoside phase.
(2) isolate biphase, by organic solvent by heating Distillation recovery organic solvent, and reusable edible, remaining be
Fatty alcohol-polyoxyethylene ether；Alcohol ether glucoside is communicated pervaporation and removes a small amount of organic solvent, remaining as alcohol ether glucoside.
(3) in the alcohol ether glucoside that step (2) evaporation obtains, organic solvent is added, the same step of its technical conditions (1) and (2),
Use multitple extraction, improve the purity of alcohol ether glucoside.
Organic solvent of the present invention be methanol, ethanol, propanol, butanol, ethylene glycol, Polyethylene Glycol, acetonitrile, propionitrile,
Butyronitrile, methyl acetate, ethyl acetate, methyl propionate, ethyl propionate, acetone, butanone, Ketocyclopentane, Ketohexamethylene, You Jirong
Agent can use one or more mixture above-mentioned.
Detailed description of the invention:
Present invention following example illustrate, but the present invention is not limited to following embodiment, at the model without departing from the most described objective
In enclosing, all amendments based on basic thought of the present invention and variation, broadly fall in the technical scope that the present invention is claimed.
Embodiment 1: ethanol extract and separate alcohol ether glucoside fatty alcohol-polyoxyethylene ether system
(1) it is made to mix homogeneously with the ethanol stirring of its 1/2 volume alcohol ether glucoside fatty alcohol-polyoxyethylene ether system, operation
Temperature: 40 DEG C, pressure: 0.15MPa, mixing time: 5min, phase ethanol phase and lower phase alcohol ether glucoside phase in static formation.
(2) isolate biphase, by ethanol by heating Distillation recovery ethanol, and reusable edible, remaining for poly alkyl alcohol
Oxygen vinyl Ether；Alcohol ether glucoside is communicated pervaporation and removes a small amount of ethanol, remaining as alcohol ether glucoside.
(3) ethanol can also be added in step (2) alcohol ether glucoside that obtains of evaporation, the same step of its technical conditions (1) and
(2), use multitple extraction, improve the purity of alcohol ether glucoside.
Utilizing the content of gas Chromatographic Determination ethanol phase and alcohol ether glucoside middle fatty alcohol-polyoxyethylene ether mutually, distribution ratio (β) is by public affairs
Formula (1) calculates, and in formula, x represents molar fraction, and 1 represents fatty alcohol-polyoxyethylene ether, I and II represents alcohol ether glucoside phase and ethanol phase,
Result is listed in table 1.
The distribution ratio of table 1 ethanol extract and separate alcohol ether glucoside fatty alcohol-polyoxyethylene ether system
| Alcohol ether glucoside (molar fraction) | Fatty alcohol-polyoxyethylene ether (molar fraction) | β |
| 0.24 | 0.76 | 5.26 |
| 0.65 | 0.35 | 7.38 |
| 0.89 | 0.11 | 10.81 |
From table 1, along with the minimizing of fatty alcohol-polyoxyethylene ether molar fraction, the distribution ratio of fatty alcohol-polyoxyethylene ether is gradually
Increasing, when the molar fraction of fatty alcohol-polyoxyethylene ether is 0.35, i.e. the purity of alcohol ether glucoside is 68%, utilizes ethanol to extract
After separation, the distribution ratio of fatty alcohol-polyoxyethylene ether is 7.38, by alcohol ether glucoside mutually through distillation, obtains alcohol ether glucoside purity and reaches
To 91%.Illustrating, can pass through multitple extraction technique, the purity of alcohol ether glucoside can reach more than 99% simultaneously.
Embodiment 2 acetonitrile extraction separation alcohol ether glucoside fatty alcohol-polyoxyethylene ether system
According to the method for embodiment 1, with acetonitrile as extractant, wherein operate temperature: 30 DEG C, pressure: 0.1MPa, during stirring
Between: 10min, the distribution ratio result of fatty alcohol-polyoxyethylene ether is listed in table 2.From table 2, along with fatty alcohol-polyoxyethylene ether
The minimizing of molar fraction, the distribution ratio of fatty alcohol-polyoxyethylene ether is gradually increased, when the molar fraction of fatty alcohol-polyoxyethylene ether is
When 0.14, after utilizing acetonitrile extraction to separate, the distribution ratio of fatty alcohol-polyoxyethylene ether is 9.56.
The distribution ratio of table 2 acetonitrile extraction separation alcohol ether glucoside fatty alcohol-polyoxyethylene ether system
| Alcohol ether glucoside (molar fraction) | Fatty alcohol-polyoxyethylene ether (molar fraction) | β |
| 0.20 | 0.80 | 5.10 |
| 0.53 | 0.47 | 7.08 |
| 0.86 | 0.14 | 9.56 |
Embodiment 3 acetone extract separation alcohol ether glucoside fatty alcohol-polyoxyethylene ether system
According to the method for embodiment 1, with acetone as extractant, wherein operate temperature: 20 DEG C, pressure: 1MPa, mixing time:
15min, the distribution ratio result of fatty alcohol-polyoxyethylene ether is listed in table 3.
The distribution ratio of table 3 acetone extract separation alcohol ether glucoside fatty alcohol-polyoxyethylene ether system
| Alcohol ether glucoside (molar fraction) | Fatty alcohol-polyoxyethylene ether (molar fraction) | β |
| 0.23 | 0.77 | 5.78 |
| 0.76 | 0.24 | 8.25 |
| 0.94 | 0.06 | 11.36 |
From table 3, along with the minimizing of fatty alcohol-polyoxyethylene ether molar fraction, the distribution ratio of fatty alcohol-polyoxyethylene ether is gradually
Increase, when the molar fraction of fatty alcohol-polyoxyethylene ether is 0.06, after utilizing acetone extract to separate, fatty alcohol-polyoxyethylene ether
Distribution ratio be 11.36.
Claims (2)
1. the method that an alcohol ether glucoside is isolated and purified, it is characterised in that described method comprises the steps:
(1) it is made to mix homogeneously with the organic solvent stirring of its 1/2 volume alcohol ether glucoside fatty alcohol-polyoxyethylene ether system,
Operation temperature: 20～60 DEG C, pressure: 0.1～1MPa, mixing time: 5～15min；Phase organic solvent phase in static formation
With lower phase alcohol ether glucoside phase；
(2) isolating biphase, by organic solvent by heating Distillation recovery organic solvent, and reusable edible, remaining as fat
Fat polyoxyethylenated alcohol；Alcohol ether glucoside is communicated pervaporation and removes organic solvent, remaining as alcohol ether glucoside；
Described organic solvent is ethanol, acetonitrile, acetone, and organic solvent can use one or more mixture above-mentioned.
The method that a kind of alcohol ether glucoside the most as claimed in claim 1 purifies, it is characterised in that use the mode of multitple extraction,
Also include step (3): in the alcohol ether glucoside that step (2) evaporation obtains, add organic solvent, the same step of its technical conditions (1)
(2).
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Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2016116618A1 (en) * | 2015-01-23 | 2016-07-28 | Basf Se | Desalination of polyaryl ethers by means of melt extraction |
| CN105669786B (en) * | 2015-12-29 | 2018-12-18 | 河北合佳医药科技集团有限公司 | The method of continuous production alcohol ether glucoside |
| CN106317404A (en) * | 2016-07-28 | 2017-01-11 | 中国科学院过程工程研究所 | High-purity powdery alcohol ether glucoside and production method and application thereof |
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| US4483979A (en) * | 1982-12-08 | 1984-11-20 | The Procter & Gamble Company | Polar solvent extraction of colored materials from alkylsaccharides under essentially anhydrous conditions |
| CN1651129A (en) * | 2004-11-30 | 2005-08-10 | 中国日用化学工业研究院 | Surface active agent alcohol ether glucoside and its preparation method |
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| US4483979A (en) * | 1982-12-08 | 1984-11-20 | The Procter & Gamble Company | Polar solvent extraction of colored materials from alkylsaccharides under essentially anhydrous conditions |
| CN1651129A (en) * | 2004-11-30 | 2005-08-10 | 中国日用化学工业研究院 | Surface active agent alcohol ether glucoside and its preparation method |
| CN1966513A (en) * | 2006-10-24 | 2007-05-23 | 中国日用化学工业研究院 | Process for preparing modified fatty alcohol polyethenoxy ether |
| CN101885745A (en) * | 2010-07-12 | 2010-11-17 | 中国日用化学工业研究院 | Process for preparing glucoside sulfosuccinate ester salt by solvent-free method |
| CN101948491A (en) * | 2010-09-17 | 2011-01-19 | 华宝食用香精香料（上海）有限公司 | Preparation method of polyol glucoside |
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