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Catalytic synthesis method of tri-octyl tri-meta-benzoate

A technique for the synthesis of trioctyl trimellitate and its method, which is applied in the field of catalytic synthesis of trioctyl trimellitate, can solve the problems that do not meet the industrial policy requirements of energy saving and emission reduction in the chemical industry, environmental pollution, etc., and achieve the catalytic effect Good, simplified post-treatment process, high volume resistivity effect

Active Publication Date: 2013-02-13
JIANGSU ZHENGDAN CHEM IND CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the synthesis method of trioctyl trimellitate in the prior art generally uses Lewis acid as a catalyst, such as sulfuric acid, tetrabutyl titanate, etc., so that the synthesis process needs to be neutralized and washed to remove the contained in the product. Acid or hydrolysis removes titanate, resulting in a large amount of waste water in the production process, which pollutes the environment and does not meet the national industrial policy requirements for energy conservation and emission reduction in the chemical industry

Method used

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Effect test

Embodiment 1

[0016] A catalytic synthesis method of trioctyl trimellitate, the method steps are as follows: trimellitic anhydride, octanol and SnO are added to an esterification reaction kettle, the reaction temperature is controlled at 160° C., stirring and reflux reaction is carried out for 4 hours, and metasalate is synthesized through esterification reaction. Trioctyl trimellitate, trimellitic anhydride: octanol molar ratio is 1: 3.5, catalyst consumption is 0.1% of the total mass of reaction raw materials, the binary azeotrope formed by water and excess octanol formed in the esterification process is removed Esterification reaction system, so that the esterification reaction is continuously carried out in the direction of positive reaction. When the conversion rate of trimellitic anhydride is higher than 99.5%, and the acid value of the neutralization titration measurement system is 0.05mgKOH / g, the esterification reaction is completed, and the SnO is removed by filtration. Octanol is ...

Embodiment 2

[0018] A kind of catalytic synthesis method of trioctyl trimellitate, method step is as follows: trimellitic anhydride, octanol and ZrO 2 Add it into the esterification reaction kettle, control the reaction temperature at 180°C, stir and reflux for 3 hours, and synthesize trioctyl trimellitate through esterification reaction. The molar ratio of trimellitic anhydride to octanol is 1:3.9, and the amount of catalyst used is the total amount of reaction raw materials. 0.15% of the mass, the binary azeotrope formed by the water generated in the esterification process and excessive octanol is removed from the esterification reaction system, so that the esterification reaction continues to the positive reaction direction, when the conversion rate of trimellitic anhydride is higher than 99.5 %, neutralization titration measurement system acid value is 0.04mgKOH / g when the end of the esterification reaction, filter to remove ZrO 2 , remove octanol from the esterification product under ...

Embodiment 3

[0020] A catalytic synthesis method of trioctyl trimellitate, the method steps are as follows: trimellitic acid, octanol, TiO 2 Add ZnO and ZnO into the esterification reaction kettle, control the reaction temperature at 200 ° C, stir and reflux for 8 hours, and synthesize trioctyl trimellitate through esterification reaction. The molar ratio of trimellitic acid: octanol is 1: 4.0, and the catalyst The amount used is 0.2% of the total mass of the reaction raw materials, and the binary azeotrope formed by the water generated in the esterification process and excessive octanol is removed from the esterification reaction system, so that the esterification reaction is continuously carried out in the direction of the positive reaction. The conversion rate of the triacid is higher than 99.5%, and the esterification reaction is completed when the acid value of the neutralization titration measurement system is 0.03mgKOH / g, and the TiO is removed by filtration. 2 and ZnO, remove octan...

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Abstract

The invention discloses a catalytic synthesis method of tri-octyl tri-meta-benzoate. A solid oxide is adopted as a catalyst and has a better catalysis effect; the catalytic synthesis method is an innovative novel catalytic synthesis process; the catalyst can be recycled; and the obtained tri-octyl tri-meta-benzoate is light in color and has high mass resistivity. Non-acid catalysis is adopted, and operations of neutralization and water washing are not needed in a production process, therefore, an aftertreatment procedure is simplified, and no wastewater is discharged in a production process; and the catalytic synthesis method is a cleaner production process, and accords with the requirement of relevant industrial policies for encouraging energy saving and emission reduction in the chemical engineering industry in China.

Description

technical field [0001] The invention relates to a catalytic synthesis method of trioctyl trimellitate, which belongs to the technical field of plasticizer synthesis. Background technique [0002] Trioctyl trimellitate is a plasticizer with excellent performance. Compared with phthalate plasticizers, it has the advantages of high flash point, low volatility, resistance to solvent extraction, small migration, and large molecular weight. At the same time, due to the high volume resistivity of trioctyl trimellitate and its excellent compatibility with polymers, especially polyvinyl chloride materials, it can not only be used as a general-purpose plasticizer, but also widely used in 105°C cables Materials, 125 ℃ cable materials, automotive interior materials, medical devices and polyvinyl chloride and other materials, so it has broad application prospects. However, the synthesis method of trioctyl trimellitate in the prior art generally uses Lewis acid as a catalyst, such as sul...

Claims

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Application Information

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IPC IPC(8): C07C69/76C07C67/08
CPCY02P20/584
Inventor 曹正国潘鹤林荆晓平任伟
Owner JIANGSU ZHENGDAN CHEM IND CO LTD
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