阅读说明：本技术 一种椰油酰基谷氨酸成制备方法 (Preparation method of cocoyl glutamic acid ) 是由 吴运东 佘远斌 陈肖虎 舒华 邓成方 陈小峰 冯明友 胡小琴 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谷氨酸成制备方法,原材料为椰油酰氯、谷氨酸钠、氢氧化钠、盐酸、丙酮和蒸馏水,通过高精度称重仪精准的称取谷氨酸钠、椰油酰氯、丙酮的摩尔比为40：85：20,配制a比例氢氧化钠水,比例为6：85,配制b比例氢氧化钠水,比例为：12：53,配制盐酸水中,比例为：25:1200,加入谷氨酸钠,用氢氧化钠/水配置的氢氧化钠水溶液溶解谷氨酸钠,待降至20℃以下时,再加入丙酮,在充分搅拌下,同时向其中缓慢滴加氢氧化钠/水配置而成的氢氧化钠水溶液,使反应体系温度在25℃以内,pH值控制在8左右；具有生物降解性高、适合制成各种形态、合适的起泡力、合适的洗涤力、耐硬水性、弱酸性、无过敏性的优点。(The invention discloses a preparation method of cocoyl glutamic acid, which comprises the following steps of taking cocoyl chloride, sodium glutamate, sodium hydroxide, hydrochloric acid, acetone and distilled water as raw materials, and accurately weighing the sodium glutamate, the cocoyl chloride and the acetone by a high-precision weighing instrument according to a molar ratio of 40: 85: 20, preparing sodium hydroxide with the ratio of a to 6: 85, preparing sodium hydroxide with the proportion of b: 12: 53, preparing hydrochloric acid water according to the following proportion: 1200, adding sodium glutamate, dissolving the sodium glutamate by using a sodium hydroxide aqueous solution prepared from sodium hydroxide/water, adding acetone when the temperature is reduced to be below 20 ℃, and slowly dropwise adding the sodium hydroxide aqueous solution prepared from sodium hydroxide/water into the acetone under full stirring to ensure that the temperature of a reaction system is within 25 ℃ and the pH value is controlled to be about 8; has the advantages of high biodegradability, suitability for being made into various forms, appropriate foaming power, appropriate washing power, hard water resistance, weak acidity and no allergy.)

1. A preparation method of cocoyl glutamic acid is characterized in that: the raw materials are cocoyl chloride, sodium glutamate, sodium hydroxide, hydrochloric acid, acetone and distilled water, and the molar ratio of the sodium glutamate, the cocoyl chloride and the acetone is 40: 85: 20, preparing sodium hydroxide with the ratio of a to 6: 85, preparing sodium hydroxide with the proportion of b: 12: 53, preparing hydrochloric acid water according to the following proportion: 25:1200.

2. A method of preparing cocoyl glutamic acid according to claim 1, wherein: the preparation method comprises the following steps:

(1) adding sodium glutamate into a four-necked bottle provided with a mechanical stirrer and a reflux condenser, dissolving the sodium glutamate with a sodium hydroxide aqueous solution prepared from sodium hydroxide/water a, and cooling to below 20 ℃ to form a mixed material;

(2) adding acetone into the mixed material in the step (1), cooling while stirring, and carrying out the next step after the temperature is reduced to below 20 ℃;

(3) under the condition of fully stirring the above (2), slowly dropwise adding a sodium hydroxide aqueous solution prepared by sodium hydroxide/water b into the mixture, controlling the temperature of a reaction system within 25 ℃ and the pH value to be about 8, heating to 25 ℃, reacting for 3 hours, and preserving heat to finish the reaction;

(4) slowly adding the material in the step (3) into a prepared hydrochloric acid aqueous solution beaker while stirring, washing the beaker with distilled water, continuously stirring for about 30 minutes, and stopping when the pH is less than or equal to 3.0;

(5) and (3) standing the mixed material in the step (4) for about 30 minutes, performing suction filtration, washing with distilled water until the pH value is about 6, and drying the product in a forced air drying oven at 65 ℃ to obtain the cocoyl glutamic acid.

3. A method of preparing cocoyl glutamic acid according to claim 1, wherein: the cocoyl chloride must have a color of less than 50 and a content of greater than 99%.

4. A method of preparing cocoyl glutamic acid according to claim 1, wherein: the distilled water must be filtered.

5. A method of preparing cocoyl glutamic acid according to claim 2, characterized in that: the air-blast drying oven adopts a vacuum drying oven.

6. A method of preparing cocoyl glutamic acid according to claim 2, characterized in that: an electric stirrer is adopted during stirring.

Technical Field

The invention relates to the technical field of preparation of cocoyl glutamic acid, in particular to a preparation method of cocoyl glutamic acid.

Background

Because of the excellent properties of amino acid surfactants, they meet the requirements of people, and thus have attracted more and more attention. It is widely used in foreign countries in the formulation of daily chemicals such as skin care products, facial cleansers, hand lotions, bubble baths, body washes, shampoos, hair conditioners, face masks, detergents, toothpastes, and the like, and in the formulation of food additives, pesticides, metal cleaning processes, ore floatation, secondary petroleum extraction, dyeing and finishing of silk, leather treatment, corrosion inhibitors, lubricants, fuel additives, foaming agents, fiber cleaners, antistatic agents, and rust-proofing additives, and the like.

The current more influential amino acid type surfactant products are Hamposyl in the united states, Medialan in germany, Amisoft in japan, etc.; compared with developed countries, the research, development and application of amino acid surfactants in China have a considerable gap, and 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 a preparation method of cocoyl glutamic acid, has the advantages of high biodegradability, suitability for being prepared into various forms, appropriate foaming power, appropriate washing power, hard water resistance, weak acidity and no allergy, and solves the problems in the prior art.

In order to achieve the purpose, the invention provides the following technical scheme: the cocoyl glutamic acid preparation method comprises the following steps of taking cocoyl chloride, sodium glutamate, sodium hydroxide, hydrochloric acid, acetone and distilled water as raw materials, and accurately weighing the sodium glutamate, the cocoyl chloride and the acetone by a high-precision weighing instrument according to a molar ratio of 40: 85: 20, preparing sodium hydroxide with the ratio of a to 6: 85, preparing sodium hydroxide with the proportion of b: 12: 53, preparing hydrochloric acid water according to the following proportion: 25: 1200;

the preparation method comprises the following steps:

(1) adding sodium glutamate into a four-necked bottle provided with a mechanical stirrer and a reflux condenser, dissolving the sodium glutamate with a sodium hydroxide aqueous solution prepared from sodium hydroxide/water a, and cooling to below 20 ℃ to form a mixed material;

(2) adding acetone into the mixed material in the step (1), cooling while stirring, and carrying out the next step after the temperature is reduced to below 20 ℃;

(3) under the condition of fully stirring the above (2), slowly dropwise adding a sodium hydroxide aqueous solution prepared by sodium hydroxide/water b into the mixture, controlling the temperature of a reaction system within 25 ℃ and the pH value to be about 8, heating to 25 ℃, reacting for 3 hours, and preserving heat to finish the reaction;

(4) slowly adding the material in the step (3) into a prepared hydrochloric acid aqueous solution beaker while stirring, washing the beaker with distilled water, continuously stirring for about 30 minutes, and stopping when the pH is less than or equal to 3.0;

(5) and (3) standing the mixed material in the step (4) for about 30 minutes, performing suction filtration, washing with distilled water until the pH value is about 6, and drying the product in a forced air drying oven at 65 ℃ to obtain the cocoyl glutamic acid.

Preferably, the cocoyl chloride must have a color of less than 50 and a content of greater than 99%.

Preferably, the distilled water must be filtered.

Preferably, the forced air drying oven adopts a vacuum drying oven.

Preferably, an electric stirrer is used for stirring.

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 glutamic acid slowly drops sodium hydroxide water solution prepared by sodium hydroxide/water 2, makes the temperature of reaction system within 25 deg.C, pH value controlled at about 8, reduces acidity;

2: the preparation method of the cocoyl glutamic acid is characterized in that materials are slowly added into a prepared hydrochloric acid/water solution beaker while stirring, the beaker is washed by water, the stirring is continued for about 30 minutes, the measured pH value is less than or equal to 3.0, the beaker is kept standing for about 30 minutes, the filter is carried out, the beaker is washed by water until the pH value is about 6, the acidity is reduced again, the mildness of the product is ensured, the product is free of allergy, the biodegradability is high, and the cocoyl glutamic acid can be quickly decomposed in discharged water;

3: a method for preparing cocoyl glutamic acid comprises drying the product in 65 deg.C air-blast drying oven, which adopts vacuum drying oven to ensure cleanness, and drying to obtain solid, liquid and foam, which is convenient for processing.

Drawings

FIG. 1 is a preparation reaction formula of a preparation method of cocoyl glutamic acid.

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.