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Preparation method of environment-friendly glycine betaine

A betaine and environment-friendly technology, applied in the field of preparation of environment-friendly betaine, can solve the problems of difficult control, poor fluidity, large investment and the like

Inactive Publication Date: 2020-08-11
刘长飞
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Chemical synthesis methods usually use chloroacetic acid, sodium hydroxide or sodium carbonate, and trimethylamine as raw materials for neutralization reaction, then quaternization reaction, use ion resin or membrane separation, and then dry to obtain betaine, or continue to prepare betaine hydrochloride Salt, because the sodium salt is easy to crystallize, it needs to be separated from betaine to obtain betaine with a certain purity, but the crystallized sodium salt will still be mixed into betaine or betaine hydrochloride, resulting in too high impurity content in the product, and the product Easy to agglomerate, poor fluidity
In short, the existing betaine and betaine hydrochloride process is not easy to control, easy to produce by-products, large investment and low product yield, and there is a large amount of waste water, which has huge environmental pressure

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] In a 2000ml four-necked flask equipped with a condensing reflux device, stirring, and a thermometer, add 1000 grams of ethanol, heat to 65°C in a water bath, and while adding dropwise 30% ammonium chloroacetate ethanol solution (372 grams), simultaneously A 30% trimethylamine solution (197 g) was added dropwise, and the temperature was controlled between 60°C and 70°C. The dropwise reaction time was 60 minutes. After the reaction was completed, the reaction was incubated for 60 minutes. The temperature was lowered to 50°C, solid ammonium chloride was separated by suction filtration, and 45.3 g of ammonium chloride was obtained after drying.

[0031] The ethanol filtrate was evaporated and concentrated by a rotary evaporator, and 672 grams of ethanol was recovered by distillation. The temperature of the remaining liquid was cooled to 20° C., and after suction filtration and drying, 62.5 grams of crude betaine was obtained. After analysis, the content of betaine was 93....

Embodiment 2

[0033] Add 100 grams of methanol and 0.5 grams of 4-dimethylaminopyridine (DMAP) into a 2000ml four-necked flask equipped with a condensing reflux device, stirring and a thermometer, heat to 50°C in a water bath, and add chloroacetic acid in batches 111.5 grams of ammonium solids were added dropwise with a 30% methanol solution of trimethylamine (197 grams), and the temperature was controlled between 50°C and 60°C. The dropwise reaction time was 60 minutes. After the reaction was completed, the reaction was incubated for 30 minutes. The temperature was lowered to 40°C, solid ammonium chloride was separated by suction filtration, and 45.9 g of ammonium chloride was obtained after drying.

[0034] The methanol filtrate was evaporated and concentrated by a rotary evaporator, and 119 grams of methanol was recovered by distillation. The temperature of the remaining liquid was cooled to 20° C., and after suction filtration and drying, 55.36 grams of crude betaine was obtained. Aft...

Embodiment 3

[0036] Take the methanol solvent that filtered out the crude betaine in Example 2, add 75 grams of methanol, heat it to 50 ° C in a water bath, add 111.5 grams of ammonium chloroacetate solids in batches, and simultaneously add 30% trimethylamine dropwise Methanol solution (197 grams), the temperature is controlled between 50°C-60°C. The dropwise reaction time was 60 minutes. After the reaction was completed, the reaction was incubated for 30 minutes. The temperature was lowered to 10°C, solid ammonium chloride was separated by suction filtration, and 49.3 g of ammonium chloride was obtained after drying.

[0037] The methanol filtrate was evaporated and concentrated by a rotary evaporator, and 213 grams of methanol was recovered by distillation. The temperature of the remaining liquid was cooled to 20° C., and after suction filtration and drying, 121.5 grams of crude betaine was obtained. After analysis, the content of betaine was 96.4%.

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PUM

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Abstract

The invention provides a preparation method of environment-friendly high-quality glycine betaine. Agricultural ammonium chloride is co-produced while glycine betaine is produced. The method comprisesthe following steps: reacting chloroacetic acid with ammonia or ammonium bicarbonate to synthesize an ammonium chloroacetate solid intermediate, and carrying out quaternization reaction on the ammonium chloroacetate solid and trimethylamine in an ethanol or methanol solvent to synthesize glycine betaine (trimethylglycine) and ammonium chloride; ammonium chloroacetate and trimethylamine are subjected to quaternization reaction in an organic solvent, a catalyst 4-dimethylaminopyridine can be added, and potassium hydroxide can also be added to adjust the pH value of the solution.

Description

technical field [0001] The invention relates to a preparation method of environment-friendly betaine. Betaine is produced together with ammonium chloride, which belongs to the technical field of chemical production. Background technique [0002] Betaine, also known as betaine and trimethylglycine, has good physical and chemical properties, good stability and antioxidant capacity, high temperature and acid-base resistance; its chemical structure is similar to amino acids and choline, and has various biological functions. It is used in feed additives, pharmaceutical industry, agricultural and forestry production, food additives, daily chemicals and other fields. In terms of cosmetics, it has a moisturizing effect; in medicine, it has a liver-protecting effect. In terms of food, the US FDA has approved betaine as a safe food additive and dietary nutrition enhancer; betaine can improve the utilization of energy in food, improve the effective absorption of amino acids and Utiliz...

Claims

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Application Information

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IPC IPC(8): C07C229/12C07C227/08C05C3/00C01C1/16
CPCC01C1/164C05C3/00C07C227/08C07C229/12
Inventor 刘长飞李志伟王云鹤
Owner 刘长飞
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