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Preparation method of non-toxic and efficient plasticizer triethyl citrate

A technology of plasticizer citric acid and triethyl citrate, which is applied in the field of preparation of non-toxic and high-efficiency plasticizer triethyl citrate, can solve problems such as unbearable for users, high production cost, and no profit for manufacturers, and achieve Good pumping resistance and light resistance, strong anti-mildew effect, enhanced effect of pumping resistance

Inactive Publication Date: 2012-02-01
肖连朝
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] As early as the 1980s, countries such as the United States and the Soviet Union also carried out special research and development on this project product, but no practical progress has been made so far. The main reasons are: first, due to the limitation of raw material citric acid, the product The cost is high, which exceeds the double price of normal plasticizers, which is difficult for users to bear and difficult to promote in the market; second, the production process is complicated, the product yield is low, the production cost is high, and the manufacturer has no profit; the third is that the product is slightly soluble in water, and the reaction Unstable synthesis, resulting in unstable product quality

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] A. Put citric acid and ethanol into the reaction kettle at a weight ratio of 1:1.1, add mixed solid acid as a catalyst, stir and react at 75°C for 1.8 hours, complete the esterification reaction, and obtain monoester, diester, and triester Mixture; (monoester yield is about 60%)

[0018] B Add 0.5% ethyl titanate of the total weight of the above-mentioned materials to the product A, slowly heat up to 110°C while stirring, start to feed ethanol gas, the gas flow rate is 6 cubic meters / h, pass ethanol gas during the reaction Take out the water, carry out the polymerization reaction under the action of ethyl titanate, convert the mixed ester into a high-purity monoester, and quickly reach the end of the reaction. The reaction time is 1 hour, the conversion rate reaches more than 98%, and the yield reaches 94%. %above;

[0019] After the reaction of C and B is completed, add saturated lye for neutralization, extract with solvent oil and wash with water to make the material...

Embodiment 2

[0021] A. Put citric acid and ethanol into the reaction kettle in a weight ratio of 1:1.2, add mixed solid acid as a catalyst, stir and react at 80°C for 2.1 hours, complete the esterification reaction, and obtain monoester, diester, and triester Mixture; (monoester yield is about 60%)

[0022] B Add 0.5% ethyl titanate of the total weight of the above-mentioned materials to the product A, slowly heat up to 115°C while stirring, start to feed ethanol gas, the gas flow rate is 5 cubic meters / h, pass ethanol gas during the reaction process Take out the water, carry out the polymerization reaction under the action of ethyl titanate, convert the mixed ester into a high-purity monoester, and quickly reach the end of the reaction, the reaction time is 0.9 hours, the conversion rate reaches more than 98%, and the yield reaches 94% %above;

[0023] After the reaction of C and B is completed, add saturated lye for neutralization, extract with solvent oil and wash with water to make th...

Embodiment 3

[0025] A. Put citric acid and ethanol into the reaction kettle at a weight ratio of 1:1.3, add mixed solid acid as a catalyst, stir and react at 85°C for 2.2 hours, complete the esterification reaction, and obtain monoester, diester, and triester Mixture; (monoester yield is about 60%)

[0026] B. Add 0.5% ethyl titanate of the total weight of the above-mentioned materials to the product A, slowly raise the temperature to 105°C while stirring, and start to feed ethanol gas at a gas flow rate of 7 cubic meters / h. During the reaction, ethanol gas passes through Take out the water, carry out the polymerization reaction under the action of ethyl titanate, convert the mixed ester into a high-purity monoester, and quickly reach the end of the reaction, the reaction time is 1.3 hours, the conversion rate reaches more than 98%, and the yield reaches 94% %above;

[0027] After the reaction of C and B is completed, add saturated lye for neutralization, extract with solvent oil and wash...

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PUM

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Abstract

The invention relates to a preparation method of a non-toxic and efficient plasticizer triethyl citrate. The non-toxic and efficient plasticizer triethyl citrate is prepared via esterification, polymerization and neutralization of such raw materials as citric acid, ethanol, p-toluenesulfonic acid, phosphorous acid and tetraethyl titanate. The weight percentages of the raw materials are: 55-63 percent of citric acid; 56-63 percent of ethanol; 1.0-2.0 percent of p-toluenesulfonic acid, 0.2-0.8 percent of phosphorous acid and 0.2-0.8 percent of tetraethyl titanate. The preparation method needs a simple process, stable reaction and mild conditions, and the process can be easily controlled.

Description

technical field [0001] The present invention relates to a kind of preparation method of plasticizer, relate to a kind of preparation method of nontoxic high-efficiency plasticizer triethyl citrate more specifically. Background technique [0002] As early as the 1980s, countries such as the United States and the Soviet Union also carried out special research and development on this project product, but no practical progress has been made so far. The main reasons are: first, due to the limitation of raw material citric acid, the product The cost is high, which exceeds the double price of normal plasticizers, which is difficult for users to bear and difficult to promote in the market; second, the production process is complicated, the product yield is low, the production cost is high, and the manufacturer has no profit; the third is that the product is slightly soluble in water, and the reaction The synthesis is unstable, resulting in unstable product quality. According to the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/704C07C67/08
Inventor 肖连朝
Owner 肖连朝
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