CN102321238A - The preparation method of fatty amide Soxylat A 25-7 - Google Patents
The preparation method of fatty amide Soxylat A 25-7 Download PDFInfo
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- CN102321238A CN102321238A CN201110221451A CN201110221451A CN102321238A CN 102321238 A CN102321238 A CN 102321238A CN 201110221451 A CN201110221451 A CN 201110221451A CN 201110221451 A CN201110221451 A CN 201110221451A CN 102321238 A CN102321238 A CN 102321238A
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Abstract
The invention discloses a kind of preparation method of fatty amide Soxylat A 25-7, the expression formula of said fatty amide Soxylat A 25-7 is:
Description
Technical field
The present invention relates to a kind of preparation method of fatty amide Soxylat A 25-7.
Background technology
The fatty amide Soxylat A 25-7 has emulsification, thickening, steady bubble, foam enhancing, washing and performance such as antirust; Because of existing amido linkage to have strong anti-hydrolytic performance in its molecule; And toxicity is low, and biological degradability is good, the skin affinity is good, is applicable to shampoo, body wash, dish washing detergent, laundry detergent; LAS and inorganic salt are had good consistency and synergy, be applicable to heavy-dirty liquid-detergent.In textile industry, can be used as detergent, levelling agent; In metal processing, be used as metal cleaner, lubricant; In petroleum industry, be used as the raw material emulsion splitter; In chemical fertilizer industry, be used as chemical fertilizer anti-caking agent etc.
The general structure of fatty amide Soxylat A 25-7 is:
At present; Less about the synthetic report; Patent CN 101955584 A have introduced a kind of preparation method and application thereof of alkylolamide Soxylat A 25-7; Lipid acid and diethylolamine or monoethanolamine react under the effect of Pottasium Hydroxide, feed reacting ethylene oxide then and get alkylolamide T 46155 ether product.Lipid acid and diethylolamine reacted fatty acid diethanolamine have more by product such as monoesters amine, diester amine, amine soap and free diethylolamine simultaneously.Lipid acid and monoethanolamine reacted lipid acid monoethanolamine have by product amido ester, carboxylic acid amide esters simultaneously.The fatty acid diethanolamine and the lipid acid monoethanolamine that have more by product; Do not pass through purification processes, directly feed reacting ethylene oxide, when producing the alkylolamide Soxylat A 25-7; More by product products must be arranged; Make product molecular weight distribution wide, color and luster is dark, influences the application performance of product.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of fatty amide Soxylat A 25-7.It is simple that the present invention has technology, environmental protection, convenience operation.
In order to reach above-mentioned purpose, solution of the present invention is:
The preparation method of
a kind of fatty amide Soxylat A 25-7, the expression formula of said fatty amide Soxylat A 25-7 is:
In the formula: n=2～25; R is a chain alkyl; With fatty acid amide and oxyethane is raw material, high vacuum, and high temperature dehydration carries out polyreaction and makes in the presence of catalyzer.
Described catalyzer is any one or more than one the mixture in the methanol solution, Pottasium Hydroxide, sodium hydroxide of solid sodium methylate, sodium methylate.
Described catalyzer add-on is 0.05～0.3% of the fatty amide Soxylat A 25-7 weight percent that makes.
Described high vacuum, high temperature dehydration specifically vacuumize vacuum hydro-extraction 1h through feeding nitrogen
Described polymeric reaction temperature is 110～170 ℃.
Described polymerization reaction time is 2～10 hours.
Described fatty acid amide adopts a kind of in stearic amide and the amine hydroxybenzene.
Beneficial effect of the present invention is: it is initiator that the present invention adopts fatty amide, reacts with ethylene oxide polymerization.Because used initiator fatty amide purity high (>=95%), problem such as it is many to have solved prior art by product when preparation fatty amide Soxylat A 25-7, and product purity is not high, and MWD is wide.Compared with prior art, have following outstanding advantage and positively effect:
1. the fatty amide Soxylat A 25-7 by product of the method for the invention preparation is few, narrow molecular weight distribution, and distribution coefficient is less than 1.09, and polyethyleneglycol content is less than 0.5%.
2. the present invention the pool state the fatty amide Soxylat A 25-7 steady quality of method preparation, lighter color.
Embodiment
Fatty amide and oxyethane addition, this reaction generates monoethanolamine earlier, and the oxyethane of further addition is not on the nitrogen-atoms of secondary amine, but on hydroxyl, its reaction formula is following:
The sub product polyoxyethylene glycol of this reaction is mainly caused by micro-moisture in fatty amide or the catalyzer, wants high vacuum, high temperature dehydration before the feeding oxyethane, reduces polyethyleneglycol content, to obtain highly purified fatty amide T 46155 ether product.
The preparation of reaction kettle before implementing: with zero(ppm) water autoclave is washed several times earlier, till clean, the oven dry reaction kettle, subsequent use after being cooled to 60～90 ℃.
Embodiment 1
In reaction kettle, add 300 parts of stearic amides, stir and be warming up to after stearic amide melts fully, add 0.25 part of solid sodium hydroxide, feed nitrogen, vacuumize three times repeatedly.Be warmed up to 120 ℃, behind the vacuum hydro-extraction 1h, add 186 parts in oxyethane, behind 130 ℃ of reaction 2h, be cooled to 85 ℃, discharging gets addition product.The product weight-average molecular weight is 458, distribution coefficient 1.06, polyethyleneglycol content 0.32%.
Embodiment 2
In reaction kettle, add 300 parts of stearic amides, stir and be warming up to after stearic amide melts fully, add 0.61 part of solid potassium hydroxide, feed nitrogen, vacuumize three times repeatedly.Be warmed up to 120 ℃, behind the vacuum hydro-extraction 1h, add 373 parts in oxyethane, behind 140 ℃ of reaction 4h, be cooled to 90 ℃, discharging gets addition product.The product weight-average molecular weight is 633, distribution coefficient 1.05, polyethyleneglycol content 0.48%.
Embodiment 3
In reaction kettle, add 300 parts of amine hydroxybenzenes, stir and be warming up to after amine hydroxybenzene melts fully, add 1.34 parts of solid sodium methylates, feed nitrogen, vacuumize three times repeatedly.Be warmed up to 110 ℃, behind the vacuum hydro-extraction 1h, add 658 parts in oxyethane, behind 150 ℃ of reaction 7h, be cooled to 80 ℃, discharging gets addition product.The product weight-average molecular weight is 898, distribution coefficient 1.07, polyethyleneglycol content 0.25%.
Embodiment 4
In reaction kettle, add 300 parts of amine hydroxybenzenes, stir and be warming up to after amine hydroxybenzene melts fully, add (30%) 11.9 part of the methanol solution of sodium methylate, feed nitrogen, vacuumize three times repeatedly.Be warmed up to 110 ℃, behind the vacuum hydro-extraction 1h, add 1127 parts in oxyethane, behind 170 ℃ of reaction 10h, be cooled to 80 ℃, discharging gets addition product.The product weight-average molecular weight is 1335, distribution coefficient 1.08, polyethyleneglycol content 0.45%.
Claims (7)
1. the preparation method of a fatty amide Soxylat A 25-7, the expression formula of said fatty amide Soxylat A 25-7 is: in
formula: n=2～25; R is a chain alkyl; It is characterized in that with fatty acid amide and oxyethane be raw material, high vacuum, high temperature dehydration carries out polyreaction and makes in the presence of catalyzer.
2. the preparation method of a kind of fatty amide Soxylat A 25-7 as claimed in claim 1 is characterized in that: described catalyzer is any one or more than one the mixture in the methanol solution, Pottasium Hydroxide, sodium hydroxide of solid sodium methylate, sodium methylate.
3. the preparation method of a kind of fatty amide Soxylat A 25-7 as claimed in claim 1 is characterized in that: described catalyzer add-on is 0.05～0.3% of the fatty amide Soxylat A 25-7 weight percent that makes.
4. the preparation method of a kind of fatty amide Soxylat A 25-7 as claimed in claim 1 is characterized in that: described high vacuum, high temperature dehydration specifically vacuumize vacuum hydro-extraction 1h through feeding nitrogen.
5. the preparation method of a kind of fatty amide Soxylat A 25-7 as claimed in claim 1 is characterized in that: described polymeric reaction temperature is 110～170 ℃.
6. the preparation method of a kind of fatty amide Soxylat A 25-7 as claimed in claim 1 is characterized in that: described polymerization reaction time is 2～10 hours.
7. the preparation method of a kind of fatty amide Soxylat A 25-7 as claimed in claim 1 is characterized in that: described fatty acid amide adopts a kind of in stearic amide and the amine hydroxybenzene.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201110221451A CN102321238A (en) | 2011-08-04 | 2011-08-04 | The preparation method of fatty amide Soxylat A 25-7 |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103666431A (en) * | 2012-09-05 | 2014-03-26 | 中国石油化工股份有限公司 | Surfactant composition and preparation method thereof |
| CN109232296A (en) * | 2018-10-25 | 2019-01-18 | 江南大学 | Oleic monoethanolamide polyoxyethylene ether and its synthetic method |
| CN109597227A (en) * | 2018-12-26 | 2019-04-09 | 惠科股份有限公司 | A kind of display panel and its manufacturing method |
| CN110845716A (en) * | 2019-11-26 | 2020-02-28 | 上海东大化学有限公司 | Fatty acid monoethanolamide polyoxyethylene ether and preparation method thereof |
| CN114000367A (en) * | 2021-11-09 | 2022-02-01 | 苏州联胜化学有限公司 | Electrolyte-resistant emulsifying thickener and preparation method thereof |
| CN115536829A (en) * | 2022-10-20 | 2022-12-30 | 上海多纶化工有限公司 | Method for synthesizing fatty acid monoethanolamide polyoxyethylene ether |
| CN115678001A (en) * | 2022-11-24 | 2023-02-03 | 上海多纶化工有限公司 | Method for synthesizing fatty acid monoethanolamide polyoxyethylene ether |
| CN115536829B (en) * | 2022-10-20 | 2024-07-09 | 上海多纶化工有限公司 | Synthesis method of fatty acid monoethanolamide polyoxyethylene ether |
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| JPH07247258A (en) * | 1994-03-10 | 1995-09-26 | Kao Corp | Production of polyoxyethylene ether sulfate |
| CN101955584A (en) * | 2010-04-06 | 2011-01-26 | 孙安顺 | Preparation method of alkanolamide polyoxyethylene ether and application thereof |
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2011
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH07247258A (en) * | 1994-03-10 | 1995-09-26 | Kao Corp | Production of polyoxyethylene ether sulfate |
| CN101955584A (en) * | 2010-04-06 | 2011-01-26 | 孙安顺 | Preparation method of alkanolamide polyoxyethylene ether and application thereof |
Non-Patent Citations (1)
| Title |
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| 《表面活性剂工业》 19990515 孙惠章等 乳化剂FAEO的合成及性能研究 第21页右栏第2段到第22页左栏第4段 1-7 , * |
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103666431A (en) * | 2012-09-05 | 2014-03-26 | 中国石油化工股份有限公司 | Surfactant composition and preparation method thereof |
| CN103666431B (en) * | 2012-09-05 | 2016-02-10 | 中国石油化工股份有限公司 | Surfactant composition and preparation method thereof |
| CN109232296A (en) * | 2018-10-25 | 2019-01-18 | 江南大学 | Oleic monoethanolamide polyoxyethylene ether and its synthetic method |
| CN109597227A (en) * | 2018-12-26 | 2019-04-09 | 惠科股份有限公司 | A kind of display panel and its manufacturing method |
| CN109597227B (en) * | 2018-12-26 | 2022-02-18 | 惠科股份有限公司 | Display panel and manufacturing method thereof |
| CN110845716A (en) * | 2019-11-26 | 2020-02-28 | 上海东大化学有限公司 | Fatty acid monoethanolamide polyoxyethylene ether and preparation method thereof |
| CN114000367A (en) * | 2021-11-09 | 2022-02-01 | 苏州联胜化学有限公司 | Electrolyte-resistant emulsifying thickener and preparation method thereof |
| CN114000367B (en) * | 2021-11-09 | 2023-08-04 | 苏州联胜化学有限公司 | Electrolyte-resistant emulsifying thickener and preparation method thereof |
| CN115536829A (en) * | 2022-10-20 | 2022-12-30 | 上海多纶化工有限公司 | Method for synthesizing fatty acid monoethanolamide polyoxyethylene ether |
| CN115536829B (en) * | 2022-10-20 | 2024-07-09 | 上海多纶化工有限公司 | Synthesis method of fatty acid monoethanolamide polyoxyethylene ether |
| CN115678001A (en) * | 2022-11-24 | 2023-02-03 | 上海多纶化工有限公司 | Method for synthesizing fatty acid monoethanolamide polyoxyethylene ether |
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Application publication date: 20120118 |