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
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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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