Method for refining trioctyl trimellitate and refining agent used thereby

A technology of trimellitic acid tris and ethylhexyl esters, which is applied in the field of organic compound preparation, can solve the problems of difficulty in cost reduction, unfavorable economic benefits, long production time, etc. Effect

Inactive Publication Date: 2014-03-26
TIANJIN CHEM REAGENT RES INST
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The usual production method of tri-2-ethylhexyl trimellitate is a direct esterification reaction, and the color of the obtained product is yellow, which is difficult to sell as a product, and must be further refined, that is, to carry out a decompression refining treatment step. This type of preparation method Existing problems: 1. Since an expensive high vacuum pump needs to be used in the decompression refining treatment step, this method has the problems of many production equipment and high cost, so it is difficult to reduce the cost
2. Since the decompression refining treatment step is an indispensable and time-consuming production step in the process of producing tri-2-ethylhexyl trimellitate, the method has the problems of long production time and low production efficiency, which is not necessary Conducive to the improvement of economic benefits of enterprises

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Preparation of refined preparation: mix (100) g calcium oxide, (100) g magnesium oxide, (200) g activated carbon, and (100) g silicon dioxide evenly.

[0019] (1) Esterification reaction step: drop into successively 100 kilograms of trimellitic acid, 276 kilograms of 2-ethylhexanols in 500 liters of reactors that have heating device, electric stirring, thermometer water circulation condenser and vacuum oil-water separator , 0.3 kg of concentrated sulfuric acid, under stirring, under slight vacuum, heated to boiling reaction at the same time, kept boiling reflux state, continuously separated water from the oil-water separator, until no water was generated, stopped heating, and the esterification reaction was terminated.

[0020] (2) Water washing step: add 250 kilograms of water to the mixed solution obtained after the esterification reaction, stir evenly, leave to stand for stratification, and remove the water layer therein.

[0021] (3) Dealcoholization step: dealcohol...

Embodiment 2

[0025] Preparation of refined preparation: (120) g calcium oxide, (120) g magnesium oxide, (240) g gac, (120) g silicon dioxide are mixed evenly.

[0026] (1) Esterification reaction step: drop into successively 100 kilograms of trimellitic acid, 276 kilograms of 2-ethylhexanols in 500 liters of reactors that have heating device, electric stirring, thermometer water circulation condenser and vacuum oil-water separator , 0.3 kg of concentrated sulfuric acid, under stirring, under slight vacuum, heated to boiling reaction at the same time, kept boiling reflux state, continuously separated water from the oil-water separator, until no water was generated, stopped heating, and the esterification reaction was terminated.

[0027] (2) Water washing step: add 250 kilograms of water to the mixed solution obtained after the esterification reaction, stir evenly, leave to stand for stratification, and remove the water layer therein.

[0028] (3) Dealcoholization step: dealcoholizing the w...

Embodiment 3

[0032] Preparation of refined preparation: (140) g calcium oxide, (140) g magnesium oxide, (280) g gac, (140) g silicon dioxide are mixed evenly.

[0033] (1) Esterification reaction step: drop into successively 100 kilograms of trimellitic acid, 276 kilograms of 2-ethylhexanols in 500 liters of reactors that have heating device, electric stirring, thermometer water circulation condenser and vacuum oil-water separator , 0.3 kg of concentrated sulfuric acid, under stirring, under slight vacuum, heated to boiling reaction at the same time, kept boiling reflux state, continuously separated water from the oil-water separator, until no water was generated, stopped heating, and the esterification reaction was terminated.

[0034] (2) Water washing step: add 50 kilograms of water to the mixed solution obtained after the esterification reaction, stir evenly, leave to stand for stratification, and remove the water layer therein.

[0035] (3) Dealcoholization step: dealcoholizing the wa...

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PUM

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Abstract

The invention relates to a method for refining trioctyl trimellitate and a refining agent used thereby. The refining agent comprises components including calcium oxide, magnesium oxide, active carbon and silica in a mass ratio of 1:1:2:1. The refining agent is adopted in a refining step in the preparation of trioctyl trimellitate. The refining agent is added into coarse trioctyl trimellitate according to a refining agent to trioctyl trimellitate mass ratio of (0.05-0.1):1; the mixture is stirred and refined for 1 hour; the refined mixed solution is filtered; and thus, finished trioctyl trimellitate is obtained. In the preparation method, the need of a high-vacuum refining step and investment in high-vacuum pump equipment during production is obviated, so the equipment investment is saved, production cost is lowered and the market competitive power of the product is increased.

Description

technology field; [0001] The invention belongs to the field of organic compound preparation, in particular to a method for refining tri-2-ethylhexyl trimellitate and a used refining preparation thereof. Background technique; [0002] In industrial production, plastic industry and military production, tri-2-ethylhexyl trimellitate is used more and more widely as an important organic compound and heat-resistant, high-temperature-resistant plasticizer with good electrical properties. The usual production method of tri-2-ethylhexyl trimellitate is a direct esterification reaction, and the color of the obtained product is yellow, which is difficult to sell as a product, and must be further refined, that is, to carry out a decompression refining treatment step. This type of preparation method Existing problems: 1. Since an expensive high-vacuum pump needs to be used in the decompression refining treatment step, this method has the problems of many production equipment and high cos...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C69/76C07C67/56C07C67/08
Inventor 张富强
Owner TIANJIN CHEM REAGENT RES INST
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