阅读说明：本技术 一种椰油酰基甘安酸盐制备方法 (Preparation method of cocoyl glycinate ) 是由 吴运东 佘远斌 陈肖虎 舒华 胡洋 聂明莉 袁绿军 陈文绪 于 2019-10-23 设计创作，主要内容包括：本发明公开了一种椰油酰基甘安酸盐制备方法,原材料为月桂酰基谷氨酸、氢氧化钠、水和无水乙醇,通过高精度称重仪精准的称取月桂酰基谷氨酸、无水乙醇的摩尔比为1:1,制作氢氧化钠水,制作比例为0.122：0.12,溶解釜中加入月桂酰基谷氨酸和无水乙醇,搅拌升温到60℃到65℃,保温60℃到65℃,搅拌30分钟,充分溶解,趁热过滤,去除不溶杂质,控温60到65℃,搅拌20分钟到30分钟,溶液中无固体,缓慢滴加配置好的氢氧化钠/水溶液,约30分钟滴加,控制温度在70℃以内,滴加完毕,保温60℃-65℃搅拌30分钟；本发明具有优秀的发泡性能、温和的清洁效果、温和的滋润效果、解性能优异、使用安全、对环境无负面影响的优点。(The invention discloses a preparation method of cocoyl glycinate, which comprises the following steps of taking lauroyl glutamic acid, sodium hydroxide, water and absolute ethyl alcohol as raw materials, accurately weighing the lauroyl glutamic acid and the absolute ethyl alcohol by a high-precision weighing instrument, wherein the molar ratio of the lauroyl glutamic acid to the absolute ethyl alcohol is 1:1, and preparing the sodium hydroxide, wherein the preparation ratio is 0.122: 0.12, adding lauroyl glutamic acid and absolute ethyl alcohol into a dissolving kettle, stirring and heating to 60-65 ℃, keeping the temperature at 60-65 ℃, stirring for 30 minutes, fully dissolving, filtering while the solution is hot, removing insoluble impurities, controlling the temperature at 60-65 ℃, stirring for 20-30 minutes, slowly dropwise adding the prepared sodium hydroxide/water solution, dropwise adding for about 30 minutes, controlling the temperature within 70 ℃, keeping the temperature at 60-65 ℃ and stirring for 30 minutes; the invention has the advantages of excellent foaming performance, mild cleaning effect, mild moistening effect, excellent degradation performance, safe use and no negative influence on the environment.)

1. A preparation method of cocoyl glycinate is characterized in that: the raw materials are lauroyl glutamic acid, sodium hydroxide, water and absolute ethyl alcohol, the mole ratio of lauroyl glutamic acid to absolute ethyl alcohol is accurately weighed by a high-precision weighing instrument to be 1:1, sodium hydroxide is prepared, and the preparation ratio is 0.122: 0.12.

2. a method of preparing cocoyl glycinate according to claim 1, characterized in that: the preparation method comprises the following steps:

(1) adding lauroyl glutamic acid and absolute ethyl alcohol into a dissolving kettle, stirring and heating to 60-65 ℃;

(2) keeping the temperature of the (1) at 60-65 ℃, stirring for 30 minutes, fully dissolving, filtering while hot, and removing insoluble impurities;

(3) controlling the temperature of the (2) to be 60-65 ℃, and stirring for 20-30 minutes until the solution has no solid;

(4) slowly dripping the prepared sodium hydroxide/water solution in the step (3) for about 30 minutes, and controlling the temperature within 70 ℃;

(5) after the dropwise addition of the step (4), keeping the temperature at 60-65 ℃ and stirring for 30 minutes;

(6) discharging the reaction solution in the step (5), filling the reaction solution into a plastic barrel, cooling the reaction solution to room temperature by using cooling water, placing the reaction solution in a refrigeration house (the temperature is-13 ℃), and freezing and crystallizing the reaction solution for about 12 hours;

(7) centrifuging the step (6) until no liquid flows out;

(8) and (3) drying the material (7), controlling the temperature to be about 55 +/-2 ℃ by using a water bath at the beginning of drying for 4 hours, then heating for 60 two hours, then heating for 70 hours to dry (requiring sampling to detect the moisture content), recording the temperature of the material to be dried every 30 minutes, and finally obtaining the white crystalline sodium N-lauroyl glutamate.

3. A method of preparing cocoyl glycinate according to claim 1, characterized in that: the lauroyl glutamic acid, sodium hydroxide, absolute ethyl alcohol and the like are industrial reagents.

4. A method of preparing cocoyl glycinate according to claim 1, characterized in that: the water must be filtered.

5. A method of preparing cocoyl glycinate according to claim 2, characterized in that: the adopted instruments are as follows: 200L reaction kettle, 300L reaction kettle, 100L liquid caustic soda elevated tank, vacuum pump, vacuum drying oven, thermometer, centrifuge, filter press, pH meter.

Technical Field

The invention relates to the technical field of preparation of cocoyl glycinate, and particularly relates to a preparation method of cocoyl glycinate.

Background

With the rapid development of the glutamic acid industry. The development of secondary product research has attracted attention. The N-acyl glutamic acid series novel anionic surfactant has wide application prospect in the aspects of daily chemical industry, medicine and health, food processing and the like. Especially lauroyl glutamic acid is an excellent antibacterial surfactant.

Currently, the most influential amino acid type surfactant products are Hamposyl in the united states, Medialan in germany, Amisoft in japan, and the like. Compared with developed countries, the research, development and application of amino acid surfactants in China have a considerable gap, the demand for high-quality products is still imported, and the price is high. Therefore, it is necessary to develop the research in this aspect vigorously in our country, develop the production technology suitable for our country's situation and expand its application range to meet the increasingly expanding market demand in our country.

Disclosure of Invention

The invention aims to overcome the defects of the prior art, provides the preparation method of the cocoyl glycinate, has the advantages of excellent foaming performance, mild cleaning effect, mild moistening effect, excellent hydrolysis performance, safe use and no negative influence on the environment, and solves the problems in the prior art.

In order to achieve the purpose, the invention provides the following technical scheme: a preparation method of cocoyl glycinate comprises the steps of taking lauroyl glutamic acid, sodium hydroxide, water and absolute ethyl alcohol as raw materials, accurately weighing the lauroyl glutamic acid and the absolute ethyl alcohol by a high-precision weighing instrument, wherein the molar ratio of the lauroyl glutamic acid to the absolute ethyl alcohol is 1:1, and preparing the sodium hydroxide according to the preparation ratio of 0.122: 0.12;

the preparation method comprises the following steps:

(1) adding lauroyl glutamic acid and absolute ethyl alcohol into a dissolving kettle, stirring and heating to 60-65 ℃;

(2) keeping the temperature of the (1) at 60-65 ℃, stirring for 30 minutes, fully dissolving, filtering while hot, and removing insoluble impurities;

(3) controlling the temperature of the (2) to be 60-65 ℃, and stirring for 20-30 minutes until the solution has no solid;

(4) slowly dripping the prepared sodium hydroxide/water solution in the step (3) for about 30 minutes, and controlling the temperature within 70 ℃;

(5) after the dropwise addition of the step (4), keeping the temperature at 60-65 ℃ and stirring for 30 minutes;

(6) discharging the reaction solution in the step (5), filling the reaction solution into a plastic barrel, cooling the reaction solution to room temperature by using cooling water, placing the reaction solution in a refrigeration house (the temperature is-13 ℃), and freezing and crystallizing the reaction solution for about 12 hours;

(7) centrifuging the step (6) until no liquid flows out;

(8) and (3) drying the material (7), controlling the temperature to be about 55 +/-2 ℃ by using a water bath at the beginning of drying for 4 hours, then heating for 60 two hours, then heating for 70 hours to dry (requiring sampling to detect the moisture content), recording the temperature of the material to be dried every 30 minutes, and finally obtaining the white crystalline sodium N-lauroyl glutamate.

Preferably, the lauroyl glutamic acid, sodium hydroxide, absolute ethyl alcohol and the like are all industrial reagents.

Preferably, the water must be filtered.

Preferably, the adopted instruments are as follows: 200L reaction kettle, 300L reaction kettle, 100L liquid caustic soda elevated tank, vacuum pump, vacuum drying oven, thermometer, centrifuge, filter press, pH meter.

The parts not involved in the invention are the same as or can be realized by the prior art.

Compared with the prior art, the invention has the following beneficial effects:

1: a method for preparing cocoyl glycinate comprises adding 50g lauroyl glutamic acid and 50g anhydrous alcohol into a three-neck flask equipped with electric stirrer, dropping funnel and thermometer, and stirring to ensure stirring uniformity;

2: the preparation method of the cocoyl glycinate fully dissolves a solution, filters the solution while the solution is hot, slowly dropwise adds the prepared NaOH/water solution after the solution is dissolved to be free of solid impurities, dropwise adds the prepared NaOH/water solution for about 30 minutes, and removes the impurities by controlling the temperature within 70 ℃ so as to ensure the safety of the product;

3: a method for preparing cocoyl glycinate comprises cooling the product at room temperature, and freezing and crystallizing in refrigerator. And after suction filtration and press drying, and preparing layer by layer to ensure the performance of the product and achieve the effect of convenient processing after drying.

Drawings

FIG. 1 is a preparation reaction formula of a preparation method of cocoyl glycinate of the invention.

Detailed Description

The present invention will be further described with reference to specific embodiments, which will become apparent from the following description, but are intended to be exemplary only, and not limiting as to the scope of the invention, it will be understood by those skilled in the art that changes in detail and modifications of form and detail may be made therein without departing from the spirit and scope of the invention, and that such changes and modifications are within the scope of the invention.