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Method for refining tri-n-octyl trimellitate and used refining agent thereof

A technology of tri-n-octyl trimellitate and trimellitic acid, which is applied in the field of organic compound preparation, can solve the problems of difficult cost reduction, unfavorable economic benefits, and many production equipments, so as to reduce production costs, improve production efficiency, The effect of easy operation

Inactive Publication Date: 2012-01-18
TIANJIN CHEM REAGENT RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The usual production method of tri-n-octyl trimellitate is 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. The problems in this type of preparation method : 1, due to the need to use expensive high vacuum pumps in the decompression refining treatment step to realize, therefore, 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-n-octyl trimellitate, the method has the problems of long production time and low production efficiency, which is not conducive to the economics of enterprises Benefit improvement

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 step: drop into successively 100 kilograms of trimellitic acid, 276 kilograms of n-octanols, concentrated sulfuric acid in a 500 liters of reactors with a heating device, electric stirring, thermometer water circulation condenser and vacuum oil-water separator 0.3 kg, under stirring, under slight vacuum, heat to boiling reaction at the same time, keep boiling and reflux, continuously separate water from the oil-water separator, until no water is generated, stop heating, and the esterification reaction is 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: dealcoholizing the washed mixture to o...

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 step: drop into successively 100 kilograms of trimellitic acid, 276 kilograms of n-octanols, concentrated sulfuric acid in a 500 liters of reactors with a heating device, electric stirring, thermometer water circulation condenser and vacuum oil-water separator 0.3 kg, under stirring, under slight vacuum, heat to boiling reaction at the same time, keep boiling and reflux, continuously separate water from the oil-water separator, until no water is generated, stop heating, and the esterification reaction is 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 washed mixture to obtain crude...

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 step: drop into successively 100 kilograms of trimellitic acid, 276 kilograms of n-octanols, concentrated sulfuric acid in a 500 liters of reactors with a heating device, electric stirring, thermometer water circulation condenser and vacuum oil-water separator 0.3 kg, under stirring, under slight vacuum, heat to boiling reaction at the same time, keep boiling and reflux, continuously separate water from the oil-water separator, until no water is generated, stop heating, and the esterification reaction is 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 washed mixture to obtain crude ...

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Abstract

The invention relates to a method for refining tri-n-octyl trimellitate and a used refining agent thereof. The refining agent comprises the following components in the following mass ratio: calcium oxide: magnesia: active carbon: silicon dioxide=1:1:2:1. The method for preparing the tri-n-octyl trimellitate comprises the following refining steps of: adopting the refining agent, adding the refining agent to a crude product of the tri-n-octyl trimellitate with the mass ratio of the refining agent to trimellitic acid being 0.05-0.1:1, stirring and refining for one hour, and filtering refined mixed liquid to obtain a finished product of the tri-n-octyl trimellitate. A high-vacuum refining step is omitted in the preparation method during production, thereby the input of high-vacuum pump equipment is avoided, so that the investment of the equipment is saved, the production cost is lowered, and the market competitiveness of the product is improved.

Description

technology field; [0001] The invention belongs to the field of organic compound preparation, in particular to a method for refining tri-n-octyl trimellitate and a used refining preparation thereof. Background technique; [0002] In industrial production, plastic industry and military production, tri-n-octyl 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-n-octyl trimellitate is 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. The problems in this type of preparation method : 1, owing to need to use expensive high-vacuum pump to realize in the decompression refining treatment step, therefore, this method exists the problem of many production equipments, high expe...

Claims

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Application Information

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IPC IPC(8): C07C69/76C07C67/56
Inventor 张富强
Owner TIANJIN CHEM REAGENT RES INST
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