Preparation method of tripalmitin citrate

A technology of tris and palmitate citrate, applied in the preparation of carboxylic acid esters, the preparation of organic compounds, chemical instruments and methods, etc., can solve the problems of plasticizers not resistant to migration, unsuitable catalysts, and high economic costs, and achieve finished products. The effect of light color, good catalytic effect and low economic cost

Active Publication Date: 2012-08-22
山东万图高分子材料股份有限公司
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  • Abstract
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Problems solved by technology

[0004] The present invention aims to solve the disadvantages of the existing low-carbon alcohol ester plasticizers of citric acid, such as intolerant migration, high volatility and high economic cost, and that the existing catalysts for the esterification reaction of citric acid esters are not suitable for use. Technical problem, provide an efficient, economical and environmentally friendly preparation method of tripalmityl citrate

Method used

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  • Preparation method of tripalmitin citrate

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Experimental program
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Effect test

Embodiment 1

[0023] (1) The preparation method of the composite catalyst: Weigh 10 g of zinc acetate and 2 g of antimony trioxide in a 50 ml beaker, perform electromagnetic stirring at room temperature, mix evenly, and set aside.

[0024] (2) Esterification reaction: add 0.2mol citric acid, 0.6mol palmityl alcohol, 0.052mol hexanaphthene in the 500ml four-necked bottle that is equipped with temperature control oil bath, agitator, water separator, reflux condenser and heat to Stir at 30°C. After the citric acid is completely dissolved and mixed evenly with palmityl alcohol, take a sample to measure the initial acid value A of the reaction solution. 0 , and then add 0.19 g of the composite catalyst prepared in step (1), heat to 100° C., and stir to generate reflux. When the water produced by the reaction begins to separate from the water separator, it is counted as the start time of the esterification reaction. When completely anhydrous is separated from the water separator, the reaction is...

Embodiment 2

[0028] (1) The preparation method of the composite catalyst: Weigh 10 g of zinc acetate and 10 g of antimony trioxide in a 50 ml beaker, perform electromagnetic stirring at room temperature, mix well, and set aside.

[0029] (2) Esterification reaction: add 0.2mol citric acid, 1mol palmityl alcohol, 0.06mol cyclohexane to 90 ℃, stirring, after the citric acid is completely dissolved and mixed evenly with palmitic alcohol, take a sample to measure the initial acid value of the reaction solution A 0 , and then add 0.28 g of the composite catalyst prepared in step (1), heat to 120° C., and stir to generate reflux. When the water produced by the reaction begins to separate from the water separator, it is counted as the start time of the esterification reaction. When completely anhydrous is separated from the water separator, the reaction is considered to have reached the end (6h). Then take a sample and measure the terminal acid value A of the reaction mixture 1 , the test stan...

Embodiment 3

[0032] (1) The preparation method of the composite catalyst: Weigh 10 g of zinc acetate and 50 g of antimony trioxide in a 50 ml beaker, perform electromagnetic stirring at room temperature, mix evenly, and set aside.

[0033] (2) Esterification reaction: add 0.2mol citric acid, 1.2mol palmityl alcohol, 0.076mol hexanaphthene in the 500ml four-necked bottle that is equipped with temperature control oil bath, agitator, water trap, reflux condenser and heat to Stir at 250°C, after the citric acid is completely dissolved and mixed evenly with palmitic alcohol, take a sample to measure the initial acid value A 0 , and then add 0.34 g of the composite catalyst prepared in step (1), heat to 210° C., and stir to generate reflux. When the water produced by the reaction begins to separate from the water separator, it is counted as the start time of the esterification reaction. When completely anhydrous is separated from the water separator, the reaction is considered to have reached t...

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Abstract

The invention relates to a preparation method of tripalmitin citrate, aiming at overcoming the defects that the existing citric low-carbon alcohol ester plasticizer is not transference-resistant and is high in volatility and economic cost, and solving the technical problem that the catalyst of the existing citrate esterification is not suitable for use. The preparation method takes zinc acetate and antimonous oxide as compound catalyst and enables citric acid and palmitin to have esterification so as to prepare the tripalmitin citrate. The prepared finished product can be taken as the plasticizer for use.

Description

technical field [0001] The present invention relates to a kind of preparation method of citric acid ester, specifically a kind of preparation method of tripalmityl citrate. Background technique [0002] Citrate plasticizers are non-toxic and safe, and are one of the first-choice environmentally friendly plasticizers in the plastic industry at home and abroad. The main varieties include triethyl citrate (TEC), acetyl triethyl citrate (ATEC), citric acid Tri-n-butyl citrate (TBC), Acetyl tri-n-butyl citrate (ATBC), Trioctyl citrate (TOC), Acetyl trioctyl citrate (ATOC), Tri-n-hexyl citrate (THC), Acetyl citric acid Tri-n-hexyl ester (ATHC), tri-n-hexyl butyryl citrate, etc. Citrate plasticizer has an excellent plasticizing effect on PVC, and its plasticizing effect is equivalent to that of DOP and DINP, and can partially replace DOP. However, the currently developed citric acid ester plasticizers (mainly low-carbon alcohol esters of citric acid, low-carbon alcohol series str...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/704C07C67/08B01J31/26
Inventor 周昌林王春娥雷景新闫建强
Owner 山东万图高分子材料股份有限公司
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