CN101062469A - Preparation method of methylglucoside polyether series product - Google Patents
Preparation method of methylglucoside polyether series product Download PDFInfo
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- CN101062469A CN101062469A CN200610050633.9A CN200610050633A CN101062469A CN 101062469 A CN101062469 A CN 101062469A CN 200610050633 A CN200610050633 A CN 200610050633A CN 101062469 A CN101062469 A CN 101062469A
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- methylglucoside
- polyether
- methyl glucoside
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Abstract
The invention relates to the making of surface activator methylglucoside polymer series product, starting with the methylglucoside, adding basic catalyst and moving catalyst, putting into epoxyethane or epoxypropane, reacting within 50deg.C-150deg.C, controlling temperature and pressure to zero through heat transfer rate, controlling temperature within 50deg.C- 200deg.C for 30-120 minutes to get methylglucoside, which is neutralized to PH 5-9, adding alcohol or water as the dilute, using active carbon decoloriation for 2-12 hours in the temperature of 90deg.C- 120deg.C. Under 80deg.C-100deg.C, it is filtered by bergmeal in the speed of 200-300Kg/hour to get the final product.
Description
Technical field
The present invention relates to a kind of preparation method of surfactant, especially relate to a kind of preparation method of methylglucoside polyether series product.
Background technology
Be that the surfactant produced of raw material is natural with the methyl glucoside, gentleness is easy to biodegradation, can be composite with plurality of raw materials, be used widely in industries such as daily use chemicals, food.With methyl glucoside polyoxyethylene (20) ether is the NMF of example, and its remarkable advantage is the character gentleness, and excitant is little, and can regulate the viscosity of shampoo system and do not reduce the special effect of active princlple content.Be usually used in personal-care supplies, as shampoo, in shower cream and the perfumed soap etc.Domestic performance does not reach application requirements at methylglucoside polyether series derivative manufacture view, and the quality instability is used in marketing and product, all is very limited.
Summary of the invention
The present invention solves existing existing product quality of methylglucoside polyether series product manufacturing technology and poor stability, the technical problem of application performance limitation etc.
Above-mentioned technical problem of the present invention is mainly solved by following technical proposals:
The preparation process of methylglucoside polyether series product divided for two steps---polymerisation and post processing; First step reaction is to be initiation material with the methyl glucoside, adds base catalyst and phase transfer catalysis (PTC) auxiliary agent, adds oxirane or expoxy propane, and initiation reaction in 50 ℃~150 ℃ scopes finishes by control temperature to initiation reaction, and pressure is to zero; Control reaction temperature again at 50 ℃~200 ℃, continue reaction 30~120 minutes, obtain the methylglucoside polyether crude product; The second step post processing is that the crude product with methylglucoside polyether neutralizes pH value after 5~9 scopes with acid, adds ethanol or water as diluent, uses activated carbon decolorizing, and bleaching time is 2~12 hours, and bleaching temperature is 90 ℃~120 ℃; Under 80 ℃~100 ℃ conditions, use super-cell to filter, filtering material is filter paper, filter cloth, the rate of filtration can obtain methylglucoside polyether at 200~300Kg/ hour.
The base catalyst that uses in the first step polymerisation can be a sodium methoxide, also can be NaOH, and perhaps other alkali compounds, or several mixture of alkaline compounds are 0.1%~3.0% with its consumption of weight percent meter of methyl glucoside; Phase transfer catalyst can be any one or any several mixture of modified glycerol, glycerine or crown ether, is 0.1%~2.0% with its consumption of weight percent meter of methyl glucoside.
Second goes on foot the neutralizing acid that uses in the last handling process, is any one of oxalic acid, acetate or sulfuric acid; Diatomite is as filter aid, and its order number is 0.1~3.0% with its consumption of weight percent meter of methyl glucoside between 600~2000 orders; High efficiency active carbon, order number are 200~2000 orders, are 0.1~3.0% with its consumption of weight percent meter of methyl glucoside; The filtering material that uses is cotton filter cloth or filter paper.
As preferably, the reaction temperature of the described first step is preferably in 110 ℃~140 ℃, and is unstable, easy to change under alkaline environment because of methyl glucoside, influences product quality, selects such reaction temperature to react, and can guarantee product quality.
As preferably, base catalyst consumption in the described first step reaction is preferably between 0.1~2.0%, though because the increase of catalytic amount can be shortened the initiation time, for the influence that is distributed with of molecular weight, also can make in the follow-up N-process salify more, influence the rate of filtration; And catalyst is very few, can cause that reaction speed is slow, reaction is incomplete etc.
As preferably, in the described second step post processing and the acid of using, preferably oxalic acid or acetate, they can form oarse-grained salt, thereby remove by filter easily, make the product low salinity that obtains, and the transparency is good; Use the cotton filtering material can make the rate of filtration reach 200~300KG/ hour during filtration.
Therefore, it is simple and easy that the present invention has preparation process, and production cost is low, characteristics such as the methylglucoside polyether series product good product performance that obtains, quality stability are good.
The specific embodiment
Below by embodiment, technical scheme of the present invention is described in further detail.
Embodiment: with the methyl glucoside is initiation material, adds catalyst sodium methoxide and phase transfer catalysis (PTC) additive modification glycerine, adds oxirane or expoxy propane, 120 ℃ of initiation reactions, by control reaction temperature until pressure to other; Reaction temperature is controlled at 150 ℃, added reacting ethylene oxide continuously 90 minutes, obtain the methylglucoside polyether crude product; The crude product of methylglucoside polyether is neutralized behind the PH=6.0 with oxalic acid, add ethanol as solvent, use activated carbon decolorizing, bleaching time is 6 hours, and bleaching temperature is 110 ℃; Under 110 ℃ of conditions, use super-cell, use the cotton filter cloth, filter paper is as filtering material, the rate of filtration is reached and kept 250Kg/ hour, can obtain the methylglucoside polyether product.
At last, should be pointed out that above embodiment only is the more representational example of the present invention.Obviously, technical scheme of the present invention is not limited to the foregoing description, and many distortion can also be arranged.All distortion that those of ordinary skill in the art can directly derive or associate from content disclosed by the invention all should be thought protection scope of the present invention.
Claims (1)
1. the preparation method of a methylglucoside polyether series product is characterized in that preparation process in two steps: polymerisation and post processing.
A: first step polymerisation is to be initiation material with the methyl glucoside, adds base catalyst and phase transfer catalysis (PTC) auxiliary agent, adds oxirane or expoxy propane, initiation reaction in 50~150 ℃ of scopes, and the control reaction temperature reduces to zero until pressure; After causing section, reaction temperature is controlled at 50 ℃~200 ℃, add oxirane or expoxy propane, continue reaction 30~120 minutes, obtain the methylglucoside polyether crude product; The second step post processing neutralizes pH value with the crude product of methylglucoside polyether after 5~9 scopes with acid, adds ethanol or water as diluent, uses high-efficiency activated carbon decoloring, and bleaching time is 2~12 hours, and bleaching temperature is 90 ℃~120 ℃; Under 80 ℃~100 ℃ conditions, use diatomite to be filter aid, to filter, the rate of filtration can obtain the methylglucoside polyether product at 200~300Kg/ hour.
B: the base catalyst that uses in the described first step polymerisation, can be sodium methoxide, also can be NaOH, perhaps other alkali compounds, or several mixture of alkaline compounds, be 0.1%~3.0% with its consumption of weight percent meter of methyl glucoside.
C: the phase transfer catalyst that uses in the described first step polymerisation can be any one of modified glycerol, glycerine or crown ether, is 0.1%~2.0% with its consumption of weight percent meter of methyl glucoside.
D: described second goes on foot the neutralizing acid that uses in the last handling process, is any one of oxalic acid, acetate or sulfuric acid.
E: described second step uses diatomite to be filter aid in the last handling process, and its order number is 0.1~3.0% with its consumption of weight percent meter of methyl glucoside between 600~2000 orders.
F: second high efficiency active carbon of step described in the last handling process, the order number is 200~2000 orders, is 0.1~3.0% with its consumption of weight percent meter of methyl glucoside.
G: the filtering material that uses in the described second step last handling process is cotton filter cloth and filter paper.
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Cited By (6)
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CN104140454A (en) * | 2013-10-29 | 2014-11-12 | 中国石油化工股份有限公司 | Polyether amine based alkyl glycoside for drilling fluid and preparation method thereof |
CN104140525A (en) * | 2013-10-29 | 2014-11-12 | 中国石油化工股份有限公司 | Preparation method of alkyl glucoside polyether for drilling fluid |
CN105713052A (en) * | 2016-01-19 | 2016-06-29 | 威尔(福建)生物有限公司 | Polyether glucoside sulfonate, preparation method and application thereof and herbicide |
CN106700061A (en) * | 2017-01-22 | 2017-05-24 | 抚顺东科精细化工有限公司 | Synthesis method of green modified nonylphenol polyoxyethylene ether |
CN110894290A (en) * | 2019-12-02 | 2020-03-20 | 中国日用化学研究院有限公司 | Preparation method of alkyl glycoside polyoxypropylene ether |
CN113827510A (en) * | 2021-11-02 | 2021-12-24 | 广州市骄子日化有限公司 | Method for preparing emulsifier pair under guidance of reduction of oil-water interfacial tension |
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2006
- 2006-04-29 CN CN200610050633.9A patent/CN101062469A/en active Pending
Cited By (10)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN104140454A (en) * | 2013-10-29 | 2014-11-12 | 中国石油化工股份有限公司 | Polyether amine based alkyl glycoside for drilling fluid and preparation method thereof |
CN104140525A (en) * | 2013-10-29 | 2014-11-12 | 中国石油化工股份有限公司 | Preparation method of alkyl glucoside polyether for drilling fluid |
CN104140454B (en) * | 2013-10-29 | 2017-06-30 | 中国石油化工股份有限公司 | A kind of drilling fluid polyethers amido APG and preparation method thereof |
CN104140525B (en) * | 2013-10-29 | 2017-07-11 | 中国石油化工股份有限公司 | A kind of drilling fluid preparation method of APG polyethers |
CN105713052A (en) * | 2016-01-19 | 2016-06-29 | 威尔(福建)生物有限公司 | Polyether glucoside sulfonate, preparation method and application thereof and herbicide |
CN105713052B (en) * | 2016-01-19 | 2019-01-04 | 威尔(福建)生物有限公司 | A kind of polyether glucoside sulfonate and preparation method thereof, using and a kind of herbicide |
CN106700061A (en) * | 2017-01-22 | 2017-05-24 | 抚顺东科精细化工有限公司 | Synthesis method of green modified nonylphenol polyoxyethylene ether |
CN110894290A (en) * | 2019-12-02 | 2020-03-20 | 中国日用化学研究院有限公司 | Preparation method of alkyl glycoside polyoxypropylene ether |
CN110894290B (en) * | 2019-12-02 | 2022-07-12 | 中国日用化学研究院有限公司 | Preparation method of alkyl glycoside polyoxypropylene ether |
CN113827510A (en) * | 2021-11-02 | 2021-12-24 | 广州市骄子日化有限公司 | Method for preparing emulsifier pair under guidance of reduction of oil-water interfacial tension |
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