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Method of synthesizing dehydro sodium acetate

A technology of sodium dehydroacetate and dehydroacetic acid, which is applied in organic chemistry and other fields, can solve the problems of excessive labor, large plant area occupation, and high production cost, and achieve the effects of simple production process, less equipment investment, and small plant occupation

Inactive Publication Date: 2007-04-18
BEIJING UNIV OF AGRI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The above-mentioned process mainly has the following defects: (1), waste water and waste residue are produced in the production process; (2), waste gas will be produced if the organic solvent is used as the reaction medium, and even safety problems are arranged; (3), a large amount of waste water is required in the synthesis process energy; (4), high production cost; (5) large investment, large workshop area and labor

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Take 5kg of dehydroacetic acid, put it into a vertical ball mill, adjust the speed to 200 rpm, add 0.4kg of NaOH, use water cooling to keep the temperature between -2°C and 10°C, and control the pressure between 0.002Mpa and 0.1Mpa . After 420 minutes, add 0.4kg NaOH and continue grinding for 240 minutes. During this period, if the temperature rise is difficult to control, intermittent grinding can be carried out. Add 10g calcium oxide, add 0.38kgNaOH and 10g microcrystalline cellulose at the same time, and grind for 120 minutes to end. Dissolution test and purity test were carried out.

Embodiment 2

[0022] Take 5kg dehydroacetic acid, 0.2kgNaOH and 0.35kgNa 2 CO 3 , put it into a vertical ball mill, adjust the speed to 220 rpm, use water cooling to keep the temperature below 40°C, grind for 260 minutes, and then add 0.67kgNa 2 CO 3 , continue to grind for 120 minutes, during this period, if the temperature rises, stop grinding, add 22g of modified starch, and add 0.22kg of NaOH at the same time, grind and keep the pressure at 0.005Mpa ~ 0.12Mpa. 180 minutes over. Dissolution test and purity test were carried out.

Embodiment 3

[0024] Take 20kg dehydroacetic acid, add 0.5kgNa 2 CO 3 10H 2 O, put it into a vertical ball mill, adjust the speed to 100 rpm, and after grinding for 10 minutes, add 0.8kgNaOH and 1.5kgNa 2 CO 3 , the temperature is controlled below 90°C, grind for 30 minutes, and then add 2kg Na 2 CO 3 , continue to grind for 40 minutes, during this period, if the temperature rises, you can stop grinding, add 180g of modified starch, and add 0.6kgNaOH and 0.77kgNa at the same time 2 CO 3 , Grinding ends in 50 minutes. Dissolution test and purity test were carried out.

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Abstract

The present invention relates to a method for synthesizing sodium dehydroacetate. It uses dehydroacetic acid and sodium hydroxide and / or sodium carbonate as raw material and makes them undergo the processes of mixing, grinding and reaction so as to obtain the invented synthetic sodium dehydroacetate. Its reaction temperature is-2 deg.C-90 deg.C and reaction pressure is 0.01MPa-0.2MPa.

Description

technical field [0001] The invention relates to a method for synthesizing sodium dehydroacetate (also known as sodium dehydroacetate), in particular to a method for grinding and synthesizing sodium dehydroacetate by using dehydroacetic acid, sodium hydroxide and / or sodium carbonate in a solid state. Background technique [0002] There are two main methods in the current production of sodium dehydroacetate. One is to use water as the medium to react solid dehydroacetic acid with sodium hydroxide or sodium carbonate in an aqueous solution, and then filter, decolorize, concentrate, vacuum Dry or spray dry to obtain sodium dehydroacetate; the second is to use ethanol as a medium, heat to dissolve dehydroacetic acid in ethanol, then react with sodium ethoxide, centrifuge, dry, pulverize, and recover ethanol to obtain sodium dehydroacetate. The above-mentioned process mainly has the following defects: (1), waste water and waste residue are produced in the production process; (2), ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D309/36
Inventor 仝其根于同泉周敏路苹白云起苏亮李树臣黄漫青王晓东
Owner BEIJING UNIV OF AGRI
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