阅读说明：本技术 一种高纯度柠檬酸甜菜碱的制备方法 (Preparation method of high-purity citric acid betaine ) 是由 俞臻泽 芮丹 陈刚 邹益东 陈冠雄 张高彬 于 2020-12-22 设计创作，主要内容包括：本发明公开了一种高纯度柠檬酸甜菜碱的制备方法,属于甜菜碱制备技术领域,其技术方案要点是包括以下步骤：S1、将氯乙酸和蒸馏水加入到反应釜中；S2、在反应釜中分批投入碳酸钠；S3、将三甲胺溶液加入反应釜中；S4、将乙醇和柠檬酸加入反应釜中；S5、将溶液从反应釜转移浓缩釜中进行一次浓缩；S6、取一次浓缩液转移到另一个浓缩釜中进行二次浓缩；S7、将二次浓缩液转移到结晶釜中结晶,本发明的优点在于制备的柠檬酸甜菜碱纯度更高,提高制备效率。(The invention discloses a preparation method of high-purity citric acid betaine, belonging to the technical field of betaine preparation, and the technical scheme is characterized by comprising the following steps: s1, adding chloroacetic acid and distilled water into a reaction kettle; s2, adding sodium carbonate into the reaction kettle in batches; s3, adding the trimethylamine solution into a reaction kettle; s4, adding ethanol and citric acid into the reaction kettle; s5, transferring the solution from the reaction kettle to a concentration kettle for primary concentration; s6, transferring the primary concentrated solution to another concentration kettle for secondary concentration; s7, transferring the secondary concentrated solution to a crystallization kettle for crystallization, and the method has the advantages that the purity of the prepared citric acid betaine is higher, and the preparation efficiency is improved.)

1. A preparation method of high-purity citric betaine is characterized by comprising the following steps: s1, adding chloroacetic acid and distilled water into a reaction kettle; s2, adding sodium carbonate into the reaction kettle in batches; s3, adding the trimethylamine solution into a reaction kettle; s4, adding ethanol and citric acid into the reaction kettle; s5, transferring the solution from the reaction kettle to a concentration kettle for primary concentration; s6, transferring the primary concentrated solution to another concentration kettle for secondary concentration; and S7, transferring the secondary concentrated solution to a crystallization kettle for crystallization.

2. The method for preparing high-purity citric betaine according to claim 1, wherein the method comprises the following steps: in step S1, the ratio of chloroacetic acid to distilled water is: 1kg corresponds to 0.76-1.2L of distilled water.

3. The method for preparing high-purity citric betaine according to claim 1, wherein the method comprises the following steps: in step S2, sodium carbonate is added into the reaction kettle for 4 hours, and the pH value in the reaction kettle is adjusted to be between 6.8 and 7.2.

4. The method for preparing high-purity citric betaine according to claim 1, wherein the method comprises the following steps: in step S3, a trimethylamine solution with a mass fraction of 35% is used.

5. The method for preparing high-purity citric betaine according to claim 1, wherein the method comprises the following steps: in step S3, the internal temperature of the reaction vessel is controlled to 40 to 50 ℃ and the internal pressure of the reaction vessel is controlled to 20 to 135 kpa.

6. The method for preparing high-purity citric betaine according to claim 1, wherein the method comprises the following steps: in step S4, the ethanol and citric acid are mixed to obtain a mixed solution, and the mixed solution is added into a reaction kettle, wherein the pH in the kettle is controlled to be 1.2-3.9.

7. The method for preparing high-purity citric betaine according to claim 1, wherein the method comprises the following steps: in step S5, the temperature in the concentration tank is controlled at 50 ℃ and the pressure is controlled at 150 kPa.

8. The method for preparing high-purity citric betaine according to claim 1, wherein the method comprises the following steps: in step S6, the temperature in the concentration tank is controlled at 55 ℃ and the pressure is controlled at 101 kPa.

9. The method for preparing high-purity citric betaine according to claim 1, wherein the method comprises the following steps: and in step S7, crystallizing at room temperature for 9-12h, and after the crystallization is finished, sending the white crystals into a dryer for drying.

10. The method for preparing high-purity citric betaine according to claim 9, wherein: in step S7, the drying temperature is set at 80 ℃ and the drying time is 2 h.

Technical Field

The invention relates to the technical field of betaine preparation, and particularly relates to a preparation method of high-purity citric acid betaine.

Background

Betaine (Betaine) was first discovered in europe and since the 19 th century, it was originally used for the extraction of sucrose as sugar cane, and it is mainly present in molasses of beet sugar and hence its name, but its efficacy was not gradually recognized until the seventies of the twentieth century. Betaine is ubiquitous in animals and plants, is an intermediate product of animal metabolism, and plays an important role in the metabolism of nutrients. Is a secondary product of metabolism, is a very important osmotic adjusting substance and is very important for enhancing the stress resistance of plants, such as salt and alkali resistance and drought tolerance.

The current mainstream method for producing the citric acid betaine is to simply and mechanically mix anhydrous betaine or betaine hydrochloride and citric acid, the betaine hydrochloride is generally taken as a raw material, ethanol is adopted for purification, separation and drying to obtain the corresponding anhydrous betaine, and the prepared citric acid betaine has limited purity and low preparation efficiency.

Disclosure of Invention

The invention aims to provide a preparation method of high-purity citric acid betaine, which has the advantages of higher purity of the prepared citric acid betaine and higher preparation efficiency.

The technical purpose of the invention is realized by the following technical scheme:

a preparation method of high-purity citric betaine comprises the following steps: s1, adding chloroacetic acid and distilled water into a reaction kettle; s2, adding sodium carbonate into the reaction kettle in batches; s3, adding the trimethylamine solution into a reaction kettle; s4, adding ethanol and citric acid into the reaction kettle; s5, transferring the solution from the reaction kettle to a concentration kettle for primary concentration; s6, transferring the primary concentrated solution to another concentration kettle for secondary concentration; and S7, transferring the secondary concentrated solution to a crystallization kettle for crystallization.

Further, in step S1, the ratio of chloroacetic acid to distilled water is: 1kg corresponds to 0.76-1.2L of distilled water.

Further, in step S2, sodium carbonate is added into the reaction kettle for 4 hours, and the pH value in the reaction kettle is adjusted to be between 6.8 and 7.2.

Further, in step S3, a trimethylamine solution having a mass fraction of 35% is used.

Further, in step S3, the internal temperature of the reaction vessel is controlled to 40 to 50 ℃ and the internal pressure of the reaction vessel is controlled to 20 to 135 kpa.

Further, in step S4, the ethanol and the citric acid are mixed to obtain a mixed solution, and the mixed solution is added into a reaction kettle, wherein the pH in the kettle is controlled to be 1.2-3.9.

Further, in step S5, the temperature in the concentration tank is controlled at 50 ℃ and the pressure is controlled at 150 kPa.

Further, in step S6, the temperature in the concentration tank is controlled to 55 ℃ and the pressure is controlled to 101 kPa.

Further, in step S7, crystallizing at room temperature for 9-12h, and after the crystallization is completed, drying the white crystal in a dryer.

Further, in step S7, the drying temperature is set at 80 ℃ and the drying time is 2 h.

In conclusion, the invention has the following beneficial effects:

1. the purity of the citric acid betaine prepared by the method is more than 99.5 percent, and the product quality is high;

2. the method has low requirement on equipment, is simple and easy to master, and is suitable for large-scale industrial production.

Drawings

FIG. 1 is a schematic view of the steps of a process for preparing high purity citric betaine.

Detailed Description

The present invention will be described in further detail with reference to the accompanying drawings.

Example 1: a method for preparing high-purity citric betaine is shown in figure 1, and comprises the following steps:

s1, adding chloroacetic acid and distilled water into the reaction kettle, wherein the proportion of the chloroacetic acid to the distilled water is as follows: 1kg corresponds to 0.76-1.2L of distilled water. In this example, 200kg of chloroacetic acid and 200L of distilled water were prepared.

S2, adding sodium carbonate into the reaction kettle in batches. Specifically, sodium carbonate is put into a reaction kettle in batches within 4 hours, and the interval of each batch is at least 15min until the pH value inside the reaction kettle is adjusted to be 6.8-7.2.

S3, adding the trimethylamine solution into the reaction kettle. The staff prepares trimethylamine solution 356L with mass fraction of 35% and adds the solution into the reaction kettle, the temperature in the reaction kettle is controlled between 40 and 50 ℃, and the pressure in the reaction kettle is controlled between 20 and 135 kpa.

S4, adding ethanol and citric acid into the reaction kettle. Specifically, the used ethanol and citric acid are mixed to obtain a mixed solution, and the mixed solution is added into a reaction kettle, wherein the pH value in the kettle is controlled to be 1.2-3.9.

And S5, transferring the solution from the reaction kettle to a concentration kettle for primary concentration. The temperature in the concentration kettle is controlled at 50 ℃, the pressure is controlled at 150kPa, and the concentration time is set to be 2 h.

And S6, transferring the solution from the reaction kettle to a concentration kettle for secondary concentration. The temperature in the concentration kettle is controlled at 55 ℃, the pressure is controlled at 101kPa, and the concentration time is set to be 1.5 h.

And S7, transferring the secondary concentrated solution to a crystallization kettle for crystallization. The drying temperature is set at 80 ℃ and the drying time is 2 h. Ensuring the complete volatilization of the ethanol and improving the crystallization degree of the solid.

And (3) crystal detection: the purity of the citric acid betaine crystal is 99.53%, and the yield is 92.14%.

Example 2: a method for preparing high-purity citric betaine, which comprises the same steps as example 1, and is different from example 1 in that:

s1, in this example, 250kg of chloroacetic acid and 300L of distilled water were prepared, and both were added to the monkey.

S3, preparing trimethylamine solution 451L with the mass fraction of 35% by workers, and adding the trimethylamine solution into a reaction kettle, wherein the internal temperature of the reaction kettle is controlled to be 40-50 ℃, and the internal pressure of the reaction kettle is controlled to be 20-135 kpa.

And (3) crystal detection: the purity of the citric acid betaine crystal is 99.74%, and the yield is 92.66%.

Example 3: a method for preparing high-purity citric betaine, which comprises the same steps as example 1, and is different from example 1 in that:

s1, in this example, 300kg of chloroacetic acid and 360L of distilled water were prepared, and both were added to the monkey.

S3, adding a trimethylamine solution 517L with the mass fraction of 35% prepared by workers into a reaction kettle, controlling the internal temperature of the reaction kettle to be 40-50 ℃ and the internal pressure of the reaction kettle to be 20-135 kpa.

And (3) crystal detection: the purity of the citric acid betaine crystal is 99.32%, and the yield is 94.57%.

The present embodiment is only for explaining the present invention, and it is not limited to the present invention, and those skilled in the art can make modifications of the present embodiment without inventive contribution as needed after reading the present specification, but all of them are protected by patent law within the scope of the claims of the present invention.