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High consistency and high purity aqueous solutions of betaine preparation method

An alkaline aqueous solution, high-purity technology, applied in chemical instruments and methods, dissolution, organic chemistry, etc., can solve unsatisfactory problems, excessive residues of alkylamides and halogenated carboxylic acids, skin hazards, etc., and achieve improvement Effects of quaternization process, increased post-treatment process, and high active substance content

Active Publication Date: 2012-07-04
广州星业科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But some of the solid content of the betaine aqueous solution prepared by these methods can only be increased to 40%; and the product with solid content reaching or close to 50% is either very viscous, has poor fluidity, is inconvenient to use, or is added to the reaction system. Excessive viscosity regulators were added, such as nonionic surfactants (polyoxyethylene ethers, etc.), amphoteric glycinate, trimethylglycine, cyclodextrin, dextran, etc., but the addition of these substances reduced the sugar beet At the same time as the alkali viscosity, the viscosity of the formula system will be greatly reduced when the user uses it, which has a greater impact on the use of the product; there are also some methods that add organic solvents to the reaction system, and the presence of organic solvents will cause potential negative effects on the user's formula. The impact may be greater
Therefore, some methods that have been proposed so far are still unsatisfactory for solving this problem.
[0027] In addition, as far as betaines are commonly used at present, there are generally problems of excessive residues of alkylamides and halogenated carboxylic acids (mainly monochloroacetic acid and dichloroacetic acid)
However, alkylamides and halogenated carboxylic acids are highly irritating and toxic chemical substances. If they remain in various washing and care products and are in direct contact with the human body, they are bound to cause harm to human skin and even affect human health. good health

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0070] The steps are as follows:

[0071] i. Amidation

[0072] 1) The molar ratio of 1:3.0~5.0 prepares vegetable oil—600g lightened coconut oil and 310g of alkyl tertiary amine—N.N-dimethyl 1.3-propanediamine;

[0073] 2) Into a 1-liter four-necked flask equipped with a stirrer, a reflux tube, a thermometer and a nitrogen tube, first add 6.0 g of lightened coconut oil and the catalyst sodium methoxide to the flask, pass nitrogen protection, and then add NN-dimethyl 1.3-Propylenediamine, heated to 170°C, and refluxed at 170°C for 8 hours for amidation reaction;

[0074] 3) After the amidation reaction is completed, distill under reduced pressure at 170°C for 2 hours to minus 0.05-0.1Mpa, distill off the excess tertiary amine to obtain the intermediate product alkylamido tertiary amine—cocamidopropyl Dimethyl tertiary amine;

[0075] ii. Quaternization and post-treatment

[0076] 1) The molar ratio of 1:1.0~1.5 prepares 250 grams of cocamidopropyl dimethyl tertiary amine and halogenate...

Embodiment 2

[0089] 1. Amidation to prepare alkyl amide tertiary amine

[0090] Same example 1;

[0091] 2. Preparation of betaine aqueous solution by quaternization and post-treatment

[0092] First, add 250 grams of cocamidopropyl dimethyl tertiary amine prepared in step 1) and 250 grams of water into a 1-liter four-necked flask equipped with a reflux tube, thermometer, stirrer and dropping funnel, and stir and warm to 60°C; then 200g of 50% sodium monochloroacetate aqueous solution was added dropwise from the dropping funnel for 30 minutes, and then the reaction mixture was heated to 95°C, kept at this temperature and reacted for 8 hours. During the reaction, drip Add 50% sodium hydroxide aqueous solution to maintain the pH of the reaction system at 9-10; after the quaternization reaction is completed, add 3.64 g of sodium bisulfite and keep it for 4 hours; add 2.38 g of 50% hydrogen peroxide and keep it for 1 hour.

[0093] The technical index test results of the obtained betaine solution are...

Embodiment 3

[0100] 1. Amidation to prepare alkyl amide tertiary amine

[0101] Into a 1 liter four-necked flask equipped with a stirrer, reflux tube, thermometer and nitrogen tube, first add 600g of light coconut oil and catalyst 6.0g sodium hydroxide, pass nitrogen protection, and then add 310gN.N-dimethyl 1.3-propylene diamine, then heated to 170 ℃, and refluxed at 170 ℃ for 8 hours; finally reduced pressure to minus 0.08Mpa, distilled at 170 ℃ for 2 hours to remove excess NN-dimethyl 1.3-propylene amine;

[0102] 2. Preparation of betaine aqueous solution by quaternization and post-treatment

[0103] First, add 250 g of cocamidopropyl dimethyl tertiary amine prepared in step 1) and 278 g of water into a 1-liter four-necked flask equipped with a reflux tube, thermometer, stirrer and dropping funnel.

[0104] Stir and raise the temperature to 60°C, then add 200 g of 50% sodium monochloroacetate aqueous solution dropwise from the dropping funnel for 30 minutes, then heat the reaction mixture to ...

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Abstract

The invention relates to a method for preparing beet alkaline aqueous solution with high concentration and high pureness and good fluidity at relatively low temperature (2 DEG C), which is produced according to the steps that: firstly, vegetable oil is amidated with alkyl tertiary amine; then alkyl amido tertiary amine, the amidated product, is quaternized with halogenated carboxylic acid; wherein, during the quaternization period, the pH value of the reaction system is controlled to ensure that the quaternization is more complete and micelle thickener is added during the reaction; a further post-processing reaction is carried out after the quaternization, so that the residue of the halogenated carboxylic acid is less than 20ppm, thus meeting the requirements of high concentration and high pureness.

Description

Technical field [0001] The invention relates to a preparation method for preparing a high-concentration and high-purity betaine aqueous solution, the active content of which is as high as 37% by weight or more. Background technique [0002] Because betaine is a very mild co-surfactant, compatible with all surfactants, it has the characteristics of high foaming, excellent viscosity increasing, and detergency. At present, it has become a household product and cosmetics industry. A fixed ingredient in various washing care formulas. In addition, betaine also has good decontamination ability, low irritation, and does not cause any toxic side effects even on sensitive skin, especially various personal washing products used to clean hair and body. [0003] The existing preparation method of betaine aqueous solution usually involves the quaternization reaction of fatty amide containing tertiary amine nitrogen atom and halogenated carboxylic acid or its salt in water. [0004] The fatty ami...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C309/62B01F17/18C07C233/34C09K23/18
Inventor 叶建忠孟巨光
Owner 广州星业科技股份有限公司