Method for preparing cubic anhydrous betaine crystals

A technology of anhydrous betaine and cubic shape, which is applied in the field of preparation of cubic anhydrous betaine crystals, and can solve problems such as the concentration of anhydrous betaine crystals

Active Publication Date: 2020-07-17
TIANJIN UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there are still technical problems to be solved in the current method of preparing anhydrous betaine. How to increase the bulk density of anhydrous betaine crystals and make the particle size distribution concentrated is a difficult problem at present.

Method used

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  • Method for preparing cubic anhydrous betaine crystals
  • Method for preparing cubic anhydrous betaine crystals
  • Method for preparing cubic anhydrous betaine crystals

Examples

Experimental program
Comparison scheme
Effect test

Embodiment example 1

[0049] Add 91.9g of anhydrous betaine powder and 118g of anhydrous methanol to the crystallizer, and the ratio of anhydrous betaine powder to solvent is 0.78:1. Set the stirring speed to 400r / min, and raise the temperature at a heating rate of 7°C / min to dissolve the powder, and the temperature of the solution rises to 72.3°C, reaching the boiling point of the crystallization system.

[0050] Cool down rapidly, the cooling rate is 0.3°C / min, when the solution temperature drops to 71.9°C, crystal nuclei begin to precipitate, at this time no anhydrous betaine powder is added, that is, the dosage is 0g / g solvent, and the solution explodes crystal nucleus, and then continue to cool down to room temperature at a cooling rate of 0.05°C / min.

[0051] After the temperature of the solution drops to 20° C., first filter, then wash the crystals with an acetone-methanol solution with an acetone mass fraction of 60 wt %, and then wash the crystals with acetone, the washing process needs to b...

Embodiment example 2

[0053] Add 91.9g of anhydrous betaine powder and 118g of methanol into the crystallizer, and the mass ratio of anhydrous betaine powder to solvent is 0.78:1. Set the stirring speed to 400r / min, and raise the temperature at a heating rate of 6°C / min to dissolve the powder, and the temperature of the solution rises to 72.4°C, reaching the boiling point of the crystallization system.

[0054] Cool down rapidly at a cooling rate of 0.5°C / min. When the solution temperature drops to 72°C, crystal nuclei begin to precipitate. At this time, 1g of anhydrous betaine powder is added to the solution, that is, the dosage is 0.008g / g solvent, and the solution is Immediately, crystal nuclei were precipitated explosively, and then continued to cool down to room temperature at a cooling rate of 0.05°C / min.

[0055] When the temperature of the solution drops to 20° C., filter first, then quickly wash the crystals with an acetone-methanol solution with an acetone mass fraction of 60 wt%, and the...

Embodiment example 3

[0057] Add 92.5g of anhydrous betaine powder and 118g of methanol into the crystallizer, and the mass ratio of anhydrous betaine powder to solvent is 0.78:1. Set the stirring speed at 400r / min, and raise the temperature at a rate of 5°C / min to dissolve the powder, and the temperature of the solution rises to 73.2°C, reaching the boiling point of the crystallization system.

[0058] Cool down rapidly at a rate of 0.5°C / min. When the temperature of the solution drops to 73°C, crystal nuclei begin to precipitate. At this time, 0.5g of anhydrous betaine powder is added to the solution, that is, the dosage is 0.004g / g solvent. Crystal nuclei were precipitated explosively in the solution immediately, and then continued to cool down to room temperature at a cooling rate of 0.05°C / min.

[0059] When the temperature is lowered to 20° C., filter first, then quickly wash the crystals with an acetone-methanol solution with an acetone mass fraction of 60 wt%, and then immediately wash the ...

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Abstract

The invention discloses a method for preparing cubic anhydrous betaine crystals. An over-boiling explosion nucleation method is adopted. The method comprises the following steps: adding anhydrous betaine powder into a crystallizer, adding a solvent into the crystallizer, carrying out heating to completely dissolve the powder, and enabling the temperature of a solution to reach the boiling point ofa crystallization system; carrying out rapid cooling, and when crystal nucleuses are separated out of the crystallization system, adding a small amount of anhydrous betaine powder into the crystallizer again to promote explosive separation of the crystal nucleuses from the crystallization system; continuously cooling the solution to room temperature; and carrying out cooling to a final temperature, filtering and washing crystals, and carrying out drying to obtain a cubic anhydrous betaine crystal product. According to the crystallization method disclosed by the invention, the growth process of the crystals is controlled by controlling the explosive nucleation process and the cooling process during cooling, and the two important processes also form the crystallization method-overboiling explosive nucleation method disclosed by the invention. According to the method, the flaky crystal habit of the anhydrous betaine crystals is thoroughly changed, operation time is short, production efficiency is high, and therefore, industrial production is better facilitated.

Description

technical field [0001] The present application relates to a crystallization method of betaine, in particular to a method for preparing cubic anhydrous betaine crystals. Background technique [0002] Betaine is a compound with quaternary ammonium inner salt or ammonium onium structure, which is a derivative of glycine, and the molecular structure of natural betaine is the simplest. The chemical name of the substance is betaine, that is, three methyl groups replace three hydrogen atoms on the nitrogen atom of glycine, and the molecular formula is C 5 h 11 NO 2 , the molecular weight is 117.15, and the structural formula is as follows [0003] [0004] Betaine is a natural component that is commonly found in animals and plants. It is an intermediate product of animal metabolism and plays a very important role in the metabolic process. Betaine also has a cleansing effect, does not harm the skin, is very safe, and is an excellent zwitterionic surfactant, so it is often use...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C227/42C07C229/12
CPCC07C227/42C07B2200/13C07C229/12
Inventor 龚俊波秦春雷陈冠雄侯宝红吴送姑杜世超郭盛争刘生通
Owner TIANJIN UNIV
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