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Method for preparing food-grade sodium dehydroacetate

The technology of sodium dehydroacetate and dehydroacetic acid is applied in the field of preparation of food-grade sodium dehydroacetate, and can solve the problems of low purity, unstable quality, inferior color of sodium dehydroacetate, and achieve white appearance, low cost, Easy-to-use effects

Inactive Publication Date: 2012-07-11
BENGBU BBCA MEDICINE SCI DEV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The existing method for synthesizing sodium dehydroacetate generally uses dehydroacetic acid and sodium hydroxide or sodium carbonate as raw materials, mixes and grinds the raw materials, and directly reacts them under solid-state conditions. It can be obtained for chemical grade, pharmaceutical grade Or food-grade sodium dehydroacetate, but the sodium dehydroacetate synthesized by existing methods has low purity, inferior color and unstable quality

Method used

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  • Method for preparing food-grade sodium dehydroacetate
  • Method for preparing food-grade sodium dehydroacetate
  • Method for preparing food-grade sodium dehydroacetate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Add 270mL of ethyl acetate, 30mL of acetic anhydride and 0.2g of anhydrous sodium acetate into a 1000mL three-necked flask, and heat to 75°C while stirring. Add 200 mL of diketene into the dropping funnel, and slowly add it dropwise to the above mixture, keeping the internal temperature at about 78°C-80°C. After the dropwise addition, the reaction was continued for 2 h.

[0022] The above-mentioned completely reacted solution was transferred to a beaker, cooled to room temperature under constant stirring, and then refrigerated at 0°C for 6 hours for crystallization. Suction filtration, the filter cake was washed twice with refrigerated ethyl acetate, and dried in an oven at 75°C. 70 g of light yellow solid was obtained.

[0023] Mix the obtained 70g of solid and 200mL of absolute ethanol in a single-necked flask, stir and reflux at 80°C until the solution is clear, continue to stir for 0.5h, then transfer to a beaker for cooling and crystallization. Suction filtratio...

Embodiment 2

[0026] Add 140mL of ethyl acetate, 15mL of acetic anhydride and 0.1g of anhydrous sodium acetate into a three-necked flask, and heat to 75°C while stirring. Add 100 mL of diketene into the dropping funnel, and slowly add it dropwise to the above mixture, keeping the internal temperature at about 80°C. After the dropwise addition, the reaction was continued for 2 h.

[0027] The above-mentioned completely reacted solution was transferred to a beaker, cooled to room temperature under constant stirring, and then refrigerated at 0°C for 6 hours for crystallization. Suction filtration, the filter cake was washed twice with cold ethyl acetate, and dried in an oven at 80°C. 53 g of light yellow solid was obtained.

[0028] Mix the obtained 53g of solid and 160mL of absolute ethanol in a single-necked flask, stir and reflux at 80°C until the solution is clear, continue to stir for 0.5h, then transfer to a beaker for cooling and crystallization. Suction filtration and drying at 80°C...

Embodiment 3

[0031] Add 140mL of anhydrous toluene, 15mL of acetic anhydride and 0.1g of triethylenediamine into a three-necked flask, and heat to 75°C while stirring. Add 100 mL of diketene into the dropping funnel, and slowly add it dropwise to the above mixture, keeping the internal temperature at about 80°C. After the dropwise addition, the reaction was continued for 2 h. The above-mentioned completely reacted solution was transferred to a beaker, cooled to room temperature under constant stirring, and then refrigerated at 0°C for 6 hours for crystallization.

[0032] Suction filtration, the filter cake was washed 3 times with refrigerated toluene, and dried in an oven at 75°C. Obtained 49.3 g of light yellow solid.

[0033] The resulting 49.3g solid and 160mL absolute ethanol were mixed in a single-necked flask, stirred and refluxed at 70°C until the solution was clear, and then continued to stir for 0.5h, then transferred to a beaker for cooling and crystallization. Suction filtra...

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Abstract

The invention provides a method for preparing food-grade sodium dehydroacetate. The method comprises the following steps of: (1) polymerizing diketene to obtain dehydroacetic acid; (2) crystallizing the dehydroacetic acid; (3) refining the dehydroacetic acid; and (4) performing neutralization reaction on the dehydroacetic acid obtained in step (3) and sodium hydroxide to obtain sodium dehydroacetate. The diketene is taken as a raw material, and a good catalytic polymerization effect can be obtained and a high polymer can be inhibited from being formed by dimerizing the diketene and using an excellent catalyst (sodium acetate anhydrous) and a water absorbent (acetic anhydride); and the quality of the sodium dehydroacetate is improved by the recrystallization by using absolute ethanol, so that the convenience is brought to the synthesis of a final product, namely the sodium dehydroacetate. The invention provides the method for preparing the food-grade sodium dehydroacetate. The method is easy to operate and low in cost. The product is pure white in appearance and has stable properties, and the quality can reach the national food-grade standard.

Description

technical field [0001] The invention belongs to the field of biochemical industry, in particular to a preparation method of food-grade sodium dehydroacetate. Background technique [0002] With the rapid development of my country's food industry and the continuous improvement of people's living standards, more and more food is put on the market, and the shelf life and quality of food have become the main issues that people care about. Therefore, various anti-corrosion and fresh-keeping measures must be taken to prolong the shelf life and shelf life and reduce the loss of nutrients. There are many specific methods, including canning, cold bulbing, drying, pickling, chemical preservation, and modern popular new technologies such as aseptic packaging, vacuum packaging, microwave sterilization, and radiation preservation. These methods have their own characteristics and scope of application. Among them, chemical antisepsis can effectively inhibit or kill the microorganisms that ...

Claims

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Application Information

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IPC IPC(8): C07D309/36
Inventor 王燕汪洪湖陈文婕孙建华杨廷韦亚锋方超
Owner BENGBU BBCA MEDICINE SCI DEV
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