CN105523950A - Novel process for synthesizing coconut oil fatty acid monoethanol amide - Google Patents
Novel process for synthesizing coconut oil fatty acid monoethanol amide Download PDFInfo
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- CN105523950A CN105523950A CN201410517207.6A CN201410517207A CN105523950A CN 105523950 A CN105523950 A CN 105523950A CN 201410517207 A CN201410517207 A CN 201410517207A CN 105523950 A CN105523950 A CN 105523950A
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- monoethanol amide
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Abstract
The invention discloses a novel process for synthesizing coconut oil fatty acid monoethanol amide. The process is characterized by adopting the technical scheme which comprises the following steps of weighing a certain amount of monoethanolamine, sodium ethoxide and absolute ethyl alcohol in a reaction in which a stirrer and a distillation column measurement device are disposed, and conducting stirring at 60-70 DEG C until the materials are completely dissolved; dropwise adding coconut oil into the reaction system, and controlling the reaction temperature to be 60-90 DEG C; conducting a reflux reaction after dropwise adding is completed while recovering an ethanol fraction having a top temperature of 78.1 DEG C; conducting cooling after the reaction is conducted for 6-10 hours and is completed so as to obtain a solid crude product coconut oil fatty acid monoethanol amide; and recrystallizing the prepared crude product with ethanol to obtain a product which has a content of more than 98.2 percent and has a yield of 90 percent in terms of coconut oil. The method is mild in reaction conditions, simple and convenient to operate, high in conversion rate and low in cost, and is suitable for industrial production.
Description
Technical field
The present invention relates to a kind of new synthetic process of fatty monoethanol amide, belong to surfactant field.
Background technology
Coconut oil fatty acid monoethanolamide (coconutoilfattyacidmonoethanolamide), be called for short CMA or methyl esters, it is a kind of faint yellow thin slice, nontoxic, due to the existence of amido linkage in its molecule, make it in wider pH value range, have good chemical stability, the performances such as excellent dispersion, solubilising, emulsification, thickening and lubrication.Microbiological deterioration rate more than 98%.Research shows, on liquid washing agent, apply free diethanolamine contained in very wide diglycollic amide series of surfactants at present has obvious carcinogenic activity.Can become the surrogate of diglycollic amide series of surfactants as the CMA being both alkylolamide class nonionogenic tenside, and use with other surfactant compounds, its performance can surmount cocoanut fatty acid diethanolamide.Especially with the thickening property of its uniqueness, softness and being widely used in the formula of the products such as various washing composition and makeup.In addition, the processing of raw wool cleaning, POLYESTER YARNS in textile industry is also usually used in, the pretreated static inhibitor of fiber, lubricant, the clean-out system of metal cleaning and processing and rust-preventive agent etc.CMA also can be obtained by reacting other tensio-active agents further, has broad prospect of application.
The main synthesis technique of CMA has 3 kinds: 1. obtained by Oleum Cocois and monoethanolamine direct reaction, and this reaction is not easily complete, containing glycerine and higher free monoethanolamine in product; 2. synthesized obtained by coco-nut oil fatty acid and monoethanolamine, temperature of reaction is higher, and product color easily deepens, and has the by products such as amine ester to produce; 3. by reacting obtained after coconut oil methyl ester with monoethanolamine, reaction conversion ratio is high, cost is high, and there are the Hazard Factor such as methyl alcohol process.
Summary of the invention
Goal of the invention: the defect existed for prior art, the invention provides a kind of synthesis technique and simplify easy to operate, transformation efficiency is high, the new synthetic process of the fatty monoethanol amide that cost is low.
For achieving the above object, a kind of new synthetic process of fatty monoethanol amide, by the following technical solutions: be configured with agitator and surveying in the reaction of distillation tower device, take a certain amount of monoethanolamine, sodium ethylate, dehydrated alcohol, stir after making it to dissolve completely at 60 DEG C ~ 70 DEG C, Oleum Cocois is dripped in reaction system, control temperature of reaction 60 DEG C ~ 9O DEG C, dropwise, carry out back flow reaction, reclaim the ethanol fraction that top temperature is 78.1 DEG C simultaneously, reaction times 6h ~ 10h reacts end, cool, obtain solid crude product fatty monoethanol amide, gained crude product ethanol is carried out recrystallization, obtain the product that content is greater than 98.2%, yield counts 90% with cocounut oil.
The quality of described sodium ethylate is 0.1% ~ 1.0% of the quality of Oleum Cocois;
The mol ratio 1:1.2 of described Oleum Cocois and monoethanolamine;
The new synthetic process of a kind of fatty monoethanol amide provided by the invention, compared to existing technology, has following beneficial effect:
Method reaction temperature of the present invention and, easy and simple to handle, transformation efficiency is high, and cost is low, is suitable for suitability for industrialized production.
Specific embodiment
By the following examples the present invention is further explained:
Embodiment 1
Be configured with agitator and surveying in the reaction of distillation tower device, take 1.2mol monoethanolamine, 0.5g sodium ethylate, 80ml dehydrated alcohol, stir after making it to dissolve completely at 60 DEG C ~ 70 DEG C, 1mol Oleum Cocois is dripped in reaction system, control temperature of reaction 60 DEG C ~ 9O DEG C, dropwise, carry out back flow reaction, reclaim the ethanol fraction that top temperature is 78.1 DEG C simultaneously, reaction times 6h ~ 10h reacts end, cool, obtain solid crude product fatty monoethanol amide, gained crude product ethanol is carried out recrystallization, obtain the product of content 98.8%, yield counts 90% with cocounut oil.
Embodiment 2
Be configured with agitator and surveying in the reaction of distillation tower device, take 1.15mol monoethanolamine, 0.4g sodium ethylate, 80ml dehydrated alcohol, stir after making it to dissolve completely at 60 DEG C ~ 70 DEG C, 1mol Oleum Cocois is dripped in reaction system, control temperature of reaction 60 DEG C ~ 9O DEG C, dropwise, carry out back flow reaction, reclaim the ethanol fraction that top temperature is 78.1 DEG C simultaneously, reaction times 6h ~ 10h reacts end, cool, obtain solid crude product fatty monoethanol amide, gained crude product ethanol is carried out recrystallization, obtain the product that content is greater than 98.5%, yield counts 90.3% with cocounut oil.
Embodiment 3
Be configured with agitator and surveying in the reaction of distillation tower device, take 1.1mol monoethanolamine, 0.38g sodium ethylate, 80ml dehydrated alcohol, stir after making it to dissolve completely at 60 DEG C ~ 70 DEG C, 1mol Oleum Cocois is dripped in reaction system, control temperature of reaction 60 DEG C ~ 9O DEG C, dropwise, carry out back flow reaction, reclaim the ethanol fraction that top temperature is 78.1 DEG C simultaneously, reaction times 6h ~ 10h reacts end, cool, obtain solid crude product fatty monoethanol amide, gained crude product ethanol is carried out recrystallization, obtain the product that content is greater than 98.9%, yield counts 90.5% with cocounut oil.
The above is only the preferred embodiment of the present invention; be noted that for those skilled in the art; under the premise without departing from the principles of the invention, can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (3)
1. the new synthetic process of a fatty monoethanol amide, it is characterized in that, by the following technical solutions, be configured with agitator and surveying in the reaction of distillation tower device, take a certain amount of monoethanolamine, sodium ethylate, dehydrated alcohol, stir after making it to dissolve completely at 60 DEG C ~ 70 DEG C, Oleum Cocois is dripped in reaction system, control temperature of reaction 60 DEG C ~ 9O DEG C, dropwise, carry out back flow reaction, reclaim the ethanol fraction that top temperature is 78.1 DEG C simultaneously, reaction times 6h ~ 10h reacts end, cool, obtain solid crude product fatty monoethanol amide, gained crude product ethanol is carried out recrystallization, obtain the product that content is greater than 98.2%, yield counts 90% with cocounut oil.
2. the new synthetic process of a kind of fatty monoethanol amide as claimed in claim 1, is characterized in that the quality of sodium ethylate is 0.1% ~ 1.0% of the quality of Oleum Cocois.
3. the new synthetic process of a kind of fatty monoethanol amide as claimed in claim 1, is characterized in that the mol ratio of Oleum Cocois and monoethanolamine is 1:1.2.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410517207.6A CN105523950A (en) | 2014-09-30 | 2014-09-30 | Novel process for synthesizing coconut oil fatty acid monoethanol amide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410517207.6A CN105523950A (en) | 2014-09-30 | 2014-09-30 | Novel process for synthesizing coconut oil fatty acid monoethanol amide |
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| CN105523950A true CN105523950A (en) | 2016-04-27 |
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| CN201410517207.6A Pending CN105523950A (en) | 2014-09-30 | 2014-09-30 | Novel process for synthesizing coconut oil fatty acid monoethanol amide |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105624221A (en) * | 2015-10-28 | 2016-06-01 | 江南大学 | Enzymatic synthesis method for fatty acid monoethanol amide |
| CN112608249A (en) * | 2020-12-22 | 2021-04-06 | 赞宇科技集团股份有限公司 | Preparation method of fatty acid monoethanolamide |
-
2014
- 2014-09-30 CN CN201410517207.6A patent/CN105523950A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105624221A (en) * | 2015-10-28 | 2016-06-01 | 江南大学 | Enzymatic synthesis method for fatty acid monoethanol amide |
| CN105624221B (en) * | 2015-10-28 | 2020-11-03 | 江南大学 | Enzymatic synthesis method of fatty acid monoethanolamide |
| CN112608249A (en) * | 2020-12-22 | 2021-04-06 | 赞宇科技集团股份有限公司 | Preparation method of fatty acid monoethanolamide |
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Application publication date: 20160427 |
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| WD01 | Invention patent application deemed withdrawn after publication |