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The preparation method of colorless fatty alkyl amphoteric sodium acetate

A technology of aliphatic alkyl and sodium acetate, which is used in the preparation of carboxylic acid amides, the preparation of organic compounds, preparations for skin care, etc. and other problems, to achieve the effect of less steps, low production cost and less equipment investment

Active Publication Date: 2017-09-29
ZHANGJIAGANG GREAT CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Most of the products obtained according to the above process have the following problems: too long high temperature time, high energy consumption, darker color, generally yellow to dark yellow, industry standard ≤ 3Garden, high impurity content, high content of by-product diamide It will lead to the inability to carry out the carboxyalkylation reaction, and in severe cases, the product will be turbid at room temperature, and some will be turbid or low-temperature turbid for a long time
Fatty alkyl amphoteric sodium acetate is a widely used amphoteric surfactant, and the existing product color ≤ 3Garden can no longer meet the needs of preparing colorless and transparent products

Method used

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  • The preparation method of colorless fatty alkyl amphoteric sodium acetate
  • The preparation method of colorless fatty alkyl amphoteric sodium acetate
  • The preparation method of colorless fatty alkyl amphoteric sodium acetate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] a) Amidation reaction: put in 100g (0.5mol) of lauric acid, slowly heat up to 80°C to melt the acid, after the acid melt is complete, turn on nitrogen at 40L / h, add 54.71g of hydroxyethylethylenediamine, and heat up to 150°C within 4h ℃, turn on the vacuum, control the vacuum degree from 0MPa to -0.08MPa within 2h, and keep the reaction at this temperature and vacuum degree for 5-6h;

[0025] b) Preparation of intermediate: cooling the prepared amide to 50°C, adding 300g of absolute ethanol, stirring to dissolve, stirring at 50r / min, keeping the cooling rate at 2-3°C / h to 4°C, and maintaining crystallization for 24h, Obvious crystals can be observed through a microscope, vacuum filtration to obtain 134.21g filter cake, and then the resulting filter cake is vacuum-dried at 80°C to obtain 128.84g intermediate, and the residual bisamide is determined to be 0.15% (wt, ion exchange method);

[0026] c) Preparation of colorless fatty alkyl amphoteric sodium acetate: add 175.1...

Embodiment 2

[0031] a) Amidation reaction: put in 100g (0.5mol) of lauric acid and 28.5g of myristic acid, slowly heat up to 80°C to melt the acid, after the acid melt is complete, turn on nitrogen at 60L / h, add 162.74g of hydroxyethylethylenediamine, Raise the temperature to 150°C within 3 hours, turn on the vacuum, and control the vacuum degree from -0.06MPa to -0.08MPa within 3 hours. At this temperature and vacuum degree, keep the reaction for 4 hours to obtain the amide;

[0032] b) Preparation of intermediate: cooling the prepared amide to 60°C, adding 1000g of isopropanol, stirring to dissolve, stirring at 50r / min, keeping the cooling rate at 2-3°C / h to 10°C, and maintaining crystallization for 48h, Obvious crystals can be observed through a microscope, and 183.55 g of filter cakes are obtained by vacuum suction filtration, and 170.35 g of intermediates are obtained by vacuum drying at 90° C., and the residual bisamide is determined to be 0.11% (wt, ion exchange method);

[0033] c)...

Embodiment 3

[0038] a) Amidation reaction: put in 110g (0.5mol) coconut oil, slowly heat up to 80°C to melt the acid, after the acid melt is complete, turn on nitrogen gas at 100L / h, add 156.20g of hydroxyethylethylenediamine, and heat up to 80°C within 6h 150°C, turn on the vacuum, control the vacuum degree from -0.04MPa to -0.08MPa within 2 hours, and keep the reaction for 3-4 hours at this temperature and vacuum degree to obtain the amide;

[0039] b) Preparation of intermediate: Cool the prepared amide to 55°C, add 500g of acetone, stir to dissolve, keep stirring at 50r / min, keep the cooling rate at 2-3°C / h to 4°C, keep crystallization for 6h, and pass through the microscope Obvious crystals can be observed, vacuum suction filtration to obtain 145.07g filter cake, vacuum drying at 80°C to obtain 142.17g intermediate, and the residual bisamide was determined to be 0.21% (wt, ion exchange method);

[0040] c) Preparation of colorless fatty alkyl amphoteric sodium acetate: add 191.13 g of...

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Abstract

The invention discloses a preparation method of colorless fatty alkyl amphoteric sodium acetate. The method comprises the following steps: a) amidation reaction: dehydration reaction of fatty acid and excess hydroxyethylethylenediamine to generate amides; b) preparation of intermediates: Cool the prepared amide to cool down, add solvent and stir to dissolve, stir and cool down to crystallize, after the crystallization is completed, separate the solution from solid to liquid by vacuum filtration or centrifugation to obtain a filter cake, and vacuum dry to obtain the intermediate; c) Preparation of colorless fat Sodium alkylamphoacetate: add deionized water to the prepared intermediate, heat up, stir and dissolve fully, then add sodium chloroacetate solution and 32% liquid caustic dropwise at the same time, then heat up to 80-100°C, and then stir at a low speed. The color of the product prepared by the present invention is ≤30 Hazen, the residue of chloroacetic acid is ≤30ppm, the purity is high, the temperature is low, no precipitation occurs for a long time, the quality is stable, the process is reasonable, the steps are few, the energy consumption is low, the equipment investment is small, the process is simple, easy to operate, and the production low cost.

Description

technical field [0001] The invention relates to a preparation method of colorless fatty alkyl amphoteric sodium acetate. Background technique [0002] Fatty alkyl amphoteric sodium acetate, which contains both anion and cation groups in its molecule, is an improved and balanced amphoteric surfactant; it has a wide pH range with anionic, cationic, and nonionic surfactants. Good compatibility; mild, low toxicity, low irritation, and can effectively reduce the irritation of other surfactants (AES, etc.); high foaming ability, fine and stable foam, light color, low odor. It can be widely used in personal cleansing products, especially for sensitive skin. It can be used as the main surfactant or co-surfactant to formulate very mild products, such as high foaming and low irritation shampoo and shower gel for children and adults. It can also be used in the production of Mild facial cleanser, hand soap, bubble bath, shaving cream and sunscreen. [0003] The preparation process of ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C233/36C07C231/02C07C231/12A61K8/42A61K8/44A61K8/46A61Q5/02A61Q19/10
Inventor 徐由江朱红军车芳丽王凤军
Owner ZHANGJIAGANG GREAT CHEM
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