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Synthesis method of fatty acid monoethanal acid amide

A technology of monoethanolamide and monoethanolamine, which is applied in the preparation of carboxylic acid amides, chemical instruments and methods, preparation of organic compounds, etc. Enhanced quality and performance, simple process, reduced oxidation effect

Inactive Publication Date: 2011-06-15
ZHEJIANG HUANGMA TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The product of this method has high purity, but the technical process is relatively complicated, and methanol needs to be used in the reaction process, and labor protection, fire prevention, and explosion-proof conditions are strict; the second is to directly react with fatty acid and monoethanolamine to prepare alcohol amides. The advantage is that the process is simple, but In addition to the formation of monoethanolamide, more by-products, such as amino esters, amide esters, etc.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] In a 1000mL four-neck flask equipped with a reflux condenser, a water separator, a stirrer, a thermometer, and a constant pressure dropping device, the molar ratio of oleic acid to monoethanolamine was fixed at 1:1.05. Add 650 parts of oleic acid, blow nitrogen, stir and heat up to 150°C, start to drop 90 parts of monoethanolamine (acid-alcohol molar ratio 1:0.65) at a constant speed with a constant pressure peristaltic pump, and reflux at 160°C. During the reaction process, take samples at regular intervals to measure the acid value, and stop the reaction when the acid value is less than 2 mgKOH / g (about 5 hours). The temperature was lowered to below 80°C, and the remaining 55 parts of monoethanolamine and 1.2 parts of potassium hydroxide (the mass of potassium hydroxide was 0.1% of the total mass of fatty acid and monoethanolamine) were added to carry out amination reaction. Stirring under nitrogen conditions, keeping the reaction at 70°C, the amine value of the react...

Embodiment 2

[0028] In a 1000mL four-neck flask equipped with a reflux condenser, a water separator, a stirrer, a thermometer, and a constant pressure dropping device, the molar ratio of oleic acid to monoethanolamine was fixed at 1:1.2. Add 650 parts of oleic acid, blow nitrogen, stir and heat up to 150°C, start to drop 110 parts of monoethanolamine (acid-alcohol molar ratio 1:0.80) at a constant speed with a constant pressure peristaltic pump, and reflux at 150-160°C. During the water separation process of the reaction, stop when the acid value is less than 2 (mgKOH / g) by taking samples at regular intervals (reaction is about 3 hours). The temperature was lowered to below 75° C., and the remaining 56 parts of monoethanolamine and 4 parts of potassium hydroxide (the mass of potassium hydroxide was 0.5% of the total mass of fatty acid and monoethanolamine) were added to carry out amination reaction. Stir under nitrogen, keep the reaction at 80°C until the amine value of the reactant no lon...

Embodiment 3

[0030] In a 1000mL four-necked flask equipped with a reflux condenser, a water separator, a stirrer, a thermometer, and a constant pressure dropping device, the molar ratio of oleic acid to monoethanolamine was fixed at 1:1.3. Add 650 parts of oleic acid, blow nitrogen, stir and heat up to 145°C, start to drop 138 parts of monoethanolamine (acid-alcohol molar ratio 1:1) at a constant speed with a constant pressure peristaltic pump, and wait for a certain period of time during the reflux reaction and water separation process at 160°C Stop the reaction when the acid value of the sample is less than 2 (mgKOH / g). The reaction takes about 3.5 hours. The temperature was lowered to below 75° C., and the remaining 42 parts of monoethanolamine and 8 parts of potassium hydroxide (the mass of potassium hydroxide was 1.0% of the total mass of fatty acid and monoethanolamine) were added to carry out amination reaction. Stirring under nitrogen, keeping the reaction at 90°C until the amine ...

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PUM

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Abstract

The invention discloses a synthesis method of fatty acid monoethanal acid amide. In the method, fatty acid and monoethanal amide are used as raw materials, wherein the molar ratio of the fatty acid to the monoethanal amide is 1:(1.05-1.30). The method is characterized by comprising the following steps of: (A) amidation reaction: slowly dripping monoethanol amine which is 44-77 percent of the total quantity of the raw materials to fatty acid under nitrogen environment for reacting at 130-160 DEG C; sampling, measuring the acid value, and stopping reacting when the acid value is smaller than 2 (mgKOH / g) to generate amide ester; and (B) amine decomposition reaction of the amide ester: adding residual monoethanol amine to the amide ester obtained in the step (A), and reacting for 1-3 hours at 70-90 DEG C in the presence of a potassium hydroxide catalyst to obtain the fatty acid monoethanal acid amide. Compared with the prior art, the method disclosed by the invention has the characteristics of high purity of the prepared product, stable product quality, and the like and the advantages of environmental friendliness and simple process.

Description

technical field [0001] The invention relates to a method for synthesizing fatty acid monoethanolamide, which belongs to the technical field of synthesizing nonionic surfactant amide compounds in organic chemistry. Background technique [0002] Fatty acid monoethanolamide, as an oil-soluble nonionic surfactant, differs from other surfactants in that it has no cloud point, has good chemical stability, excellent dispersion, solubilization, emulsification, thickening and lubrication It has good synergistic thickening effect and foam stabilization effect in liquid detergent, and the microbial degradation rate can reach more than 98%. Fatty acid ethanolamides include monoethanolamide and diethanolamide, with the latter having a larger yield. Liu Youcai. Toxicity of diethanolamide and its substitutes [J]. Daily Chemical Science, 1999 (1): 30-31. Studies have shown that fatty acid diethanolamide containing a small amount of diethanolamine has obvious carcinogenic effect on rodents....

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C231/02C07C233/18C07C233/20B01F17/22B01F17/38C09K23/22C09K23/38
Inventor 王伟松王胜利张月江金一丰万庆梅
Owner ZHEJIANG HUANGMA TECH
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