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Synthesis method of high-purity fatty acid monoethanolamine

A technology of monoethanolamide and synthesis method, which is applied in the preparation of carboxylic acid amide, chemical instruments and methods, and the preparation of organic compounds, etc. It can solve the problems of inability to remove impurities, high ester content, heavy amine odor, etc., and achieve amine value low odor, low odor, and high reaction efficiency

Inactive Publication Date: 2012-06-27
广州花语精细化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the simple post-treatment after standing and stratifying cannot remove the soap, glycerin and other water-soluble impurities in the product. The product will contain a certain amount of fatty acid soap and about 0.5-2% of glycerin residue
In addition, the ester content of the produced products is too high, mostly between 2% and 7%.
The amine value of the product is too high, mostly between 5 and 20mgKOH / g, which is about 0.6 to 2.2% when converted to free amine, which leads to a strong amine smell in the product

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Mix 400g of palm kernel oil with 100g of anhydrous methanol, add 2g of potassium hydroxide, heat and stir at 70°C for 4 hours, and after standing for 2 hours, separate the lower layer of glycerol to obtain the upper layer of crude palm kernel oil methyl ester. The excess methanol in the crude product was distilled off, then washed twice at 60°C with 200g of 5% dilute brine, and once with 200g of water, then heated to 100°C and distilled under reduced pressure for 1 hour to obtain 395.0g of palm kernel oil methyl ester. Add 104.0g of monoethanolamine and 0.2g of sodium methoxide, and react in vacuum at 100°C for 2h, and the vacuum degree is -0.095Mpa. High-purity palm kernel oleic acid monoethanolamide was obtained, with a purity of 98.3%, an amine value of 1.1 (0.12% converted to free amine), and an ester content of 1.58%.

Embodiment 2

[0039] Mix 400g of palm kernel oil with 150g of anhydrous methanol, add 2g of potassium hydroxide, heat and stir at 70°C for 2 hours, and after standing for 1 hour, separate the lower layer of glycerol to obtain the upper layer of crude palm kernel oil methyl ester. The excess methanol in the crude product was distilled off, then washed twice at 60°C with 200g of 5% dilute brine, and once with 200g of water, and then heated to 100°C for 1 hour of vacuum distillation to obtain 397.2g of palm kernel oil methyl ester. Add 107.2g of monoethanolamine and 0.2g of sodium methoxide, and react in vacuum at 100°C for 2h, and the vacuum degree is -0.095Mpa. High-purity palm kernel oleic acid monoethanolamide was obtained, with a purity of 98.5%, an amine value of 1.2 (0.13% converted to free amine), and an ester content of 1.36%.

Embodiment 3

[0041] Mix 400g of coconut oil with 120g of anhydrous methanol, add 1g of sodium methoxide, heat and stir at 70°C for 3 hours, and let stand for 1 hour to separate the lower layer of glycerin to obtain the upper layer of crude palm coconut oil methyl ester. Distill the excess methanol out of the crude product, then wash twice with 200g of 5% dilute brine at 60°C, and wash once with 200g of water, then heat up to 100°C and distill under reduced pressure for 1 hour to obtain 397.1g of methyl coconut oleate. Add 110.1g of monoethanolamine and 0.2g of sodium methoxide, and react in vacuum at 100°C for 2h, and the vacuum degree is -0.095Mpa. High-purity coconut oleic acid monoethanolamide was obtained, with a purity of 98.3%, an amine value of 1.8 (0.12% converted to free amine), and an ester content of 1.63%.

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Abstract

The invention belongs to the technical field of synthesis of a surfactant in organic chemistry, and particularly relates to a synthesis method of a high-purity fatty acid monoethanolamine, which comprises the following steps of: 1) preparation of a fatty acid methyl ester; 2) post-treatment refining of the fatty acid methyl ester; and 3) amidation reaction. The fatty acid monoethanolamine prepared by the method has the advantages of high purity, light odor, low amine value, light color and the like.

Description

[0001] technical field [0002] The invention belongs to the technical field of surfactant synthesis in organic chemistry, and in particular relates to a synthesis method of high-purity fatty acid monoethanolamide. [0003] Background technique [0004] Fatty acid monoethanolamide is a nonionic surfactant. Due to the presence of amide bonds in its molecule, it has good chemical stability in a wide pH range, excellent dispersion, solubilization, emulsification, thickening and lubricating properties. In the daily chemical industry, fatty acid monoethanolamide is often used as a thickener in liquid detergents to thicken and stabilize foam. At present, the most widely used thickener in liquid detergents is fatty acid diethanolamide, but studies have shown that free diethanolamine contained in fatty acid diethanolamide series surfactants has obvious carcinogenic activity. Fatty acid monoethanolamide is expected to be a substitute of fatty acid diethanolamide surfactant. ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C231/02C07C233/17C07C233/18
Inventor 余照权张涌刘机灵
Owner 广州花语精细化工有限公司
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