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Method for preparing anhydrous betaine crystals with ultra-uniform granularity

A technology of anhydrous betaine and crystals, which is applied in the field of preparation of food-grade cubic anhydrous betaine crystals, and can solve problems such as changing the crystal habit

Active Publication Date: 2020-07-24
TIANJIN UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the current method of preparing anhydrous betaine in ethanol still needs to solve technical problems such as changing crystal habit, controlling particle size and increasing yield. How to improve the loose bulk density of anhydrous betaine crystals and make the particle size distribution concentrated and improve production Efficiency is the current problem

Method used

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  • Method for preparing anhydrous betaine crystals with ultra-uniform granularity
  • Method for preparing anhydrous betaine crystals with ultra-uniform granularity
  • Method for preparing anhydrous betaine crystals with ultra-uniform granularity

Examples

Experimental program
Comparison scheme
Effect test

Embodiment example 1

[0043] Add 31.2g of anhydrous betaine powder and 120g of absolute ethanol in the crystallizer, the mass ratio of anhydrous betaine powder and solvent is 0.26:1. The stirring speed is set to 400r / min, and the temperature is raised at a heating rate of 7°C / min to dissolve the betaine powder, and the temperature of the solution reaches the boiling point of the crystallization system.

[0044] Cool down rapidly, the cooling rate is 0.5°C / min, when the solution temperature drops to 80.2°C, there are crystal nuclei in the solution, at this time, put 1.1g of anhydrous betaine powder into the solution, that is, the dosage is 0.009g / g solvent , crystal nuclei exploded immediately in the solution, and continued to cool down to room temperature at a cooling rate of 0.05°C / min.

[0045] When the temperature of the solution drops to 25°C, do not filter for the time being, and put 10g of anhydrous betaine powder into the crystallizer again, that is, the dosage is 0.08g / g solvent, and the ad...

Embodiment example 2

[0049] Add 31.1g of anhydrous betaine powder and 120g of absolute ethanol in the crystallizer, the mass ratio of anhydrous betaine powder and solvent is 0.26:1. The stirring speed is set to 400r / min, and the temperature is raised at a heating rate of 6°C / min to dissolve the betaine powder, and the temperature of the solution reaches the boiling point of the crystallization system.

[0050] Cool down rapidly, the cooling rate is 0.5°C / min, when the solution temperature drops to 80.1°C, there are crystal nuclei in the solution, at this time, put 0.5g of anhydrous betaine powder into the solution, that is, the dosage is 0.004g / g solvent , the crystal nuclei exploded immediately in the solution, and continued to cool down to room temperature at a cooling rate of 0.5°C / min.

[0051] When the temperature of the solution is lowered to 23°C, do not filter for the time being, and put 15g of anhydrous betaine powder into the crystallizer again, that is, the dosage is 0.12g / g solvent, an...

Embodiment example 3

[0055] Add 31.5g of anhydrous betaine powder and 120g of absolute ethanol in the crystallizer, the mass ratio of anhydrous betaine powder and solvent is 0.26:1. The stirring speed is set to 400r / min, and the temperature is raised at a heating rate of 5°C / min to dissolve the betaine powder, and the temperature of the solution reaches the boiling point of the crystallization system.

[0056] Cool down rapidly, the cooling rate is 0.5°C / min, when the solution temperature drops to 80.4°C, crystal nuclei are precipitated in the solution. At this time, 0.1g of anhydrous betaine powder is put into the solution, that is, the dosage is 0.0008g / g solvent , crystal nuclei were precipitated explosively in the solution immediately, and continued to cool down to room temperature at a cooling rate of 0.2°C / min.

[0057] When the temperature of the solution is lowered to 20°C, do not filter for the time being, and drop 14g of anhydrous betaine powder into the crystallizer again, that is, the ...

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Abstract

The invention relates to a method for preparing anhydrous betaine crystals with ultra-uniform granularity. An over-boiling explosion nucleation-cooling circulation method is adopted. The method comprises the steps: adding anhydrous betaine powder into a crystallizer, adding a solvent into the crystallizer, heating to completely dissolve the powder, and enabling the temperature of the solution to reach the boiling point of a crystallization system; rapidly cooling, and when crystal nucleuses are separated out of the crystallization system, adding a small amount of anhydrous betaine powder intothe crystallizer again to promote explosive separation of the crystal nucleuses from the crystallization system; continuously cooling the solution to room temperature; adding anhydrous betaine powderinto the crystallizer again, heating to dissolve the betaine powder until the temperature of the solution reaches the boiling point temperature of the crystallization system, and then cooling to roomtemperature; repeating the heating and cooling operations repeatedly until the mass of the crystal with 20-60 meshes is not lower than 99% of the total mass of the crystal; and cooling to the final temperature, filtering and washing the crystal, and drying to obtain the anhydrous betaine crystal product with ultra-uniform granularity.

Description

technical field [0001] The present application relates to a method for crystallizing anhydrous betaine, in particular to a method for preparing food-grade cubic anhydrous betaine crystals with high bulk density and super uniform particle size. 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. Therefore, betaine can be used as a food additive, which is ben...

Claims

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Application Information

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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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