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Efficient trimellitate tri C8-C10 preparation method

A technology of C8-C10 and trimellitic acid, which is applied in the direction of carboxylate preparation, organic compound preparation, separation/purification of carboxylate, etc., can solve unfavorable economic benefits, difficulty in reducing costs, low production efficiency, etc. Problems, to achieve the effect of reducing production costs, avoiding investment, and convenient operation

Inactive Publication Date: 2017-03-22
TIANJIN CHEM REAGENT RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

trimellitic acid tri-C 8 -C 10 The usual production method of ester is direct esterification reaction, the color of the product obtained is yellow, difficult to sell as a product, must be further refined, that is, carry out a decompression refining treatment step, the problems of this type of preparation method: 1, due to decompression refining An expensive high-vacuum pump is required for the processing steps, so this method has many production facilities and high costs, making it difficult to reduce costs
2. Since the vacuum refining treatment step is to produce trimellitic acid tris-C 8 -C 10 It is an essential and time-consuming production step in the ester process. Therefore, this method has the problems of long production time and low production efficiency, which is not conducive to the improvement of economic benefits of enterprises.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] trimellitic acid tris C 8 -C 10 The preparation method of ester comprises the following steps:

[0028] 1. Esterification reaction steps

[0029] In a 500 liter reactor with heating device, electric stirring, thermometer water circulation condenser and oil-water separator, drop into 100 kilograms of trimellitic acid successively, C 8 -C 10 256 kilograms of alcohol, 0.3 kilograms of concentrated sulfuric acid, under stirring, micro-vacuum, heating to boiling reaction at the same time, keep boiling reflux state, continuously separate water from the oil-water separator, until no water is generated, stop heating, esterification reaction termination.

[0030] 2. Washing step

[0031] Add 250 kilograms of water to the mixed solution obtained after the esterification reaction, stir evenly, leave to stand to separate layers, and remove the water layer therein.

[0032] 3. Dealcoholization step

[0033] The mixture after washing with water is dealcoholized to obtain the c...

Embodiment 2

[0039] The preparation method of this tri-n-hexyl trimellitate comprises the following steps:

[0040] 1. Esterification reaction steps

[0041] In a 500 liter reactor with heating device, electric stirring, thermometer water circulation condenser and oil-water separator, drop into 100 kilograms of trimellitic acid successively, C 8 -C 10 256 kilograms of alcohol, 0.3 kilograms of concentrated sulfuric acid, under stirring, micro-vacuum, heating to boiling reaction at the same time, keep boiling reflux state, continuously separate water from the oil-water separator, until no water is generated, stop heating, esterification reaction termination.

[0042] 2. Washing step

[0043] Add 250 kilograms of water to the mixed solution obtained after the esterification reaction, stir evenly, leave to stand to separate layers, and remove the water layer therein.

[0044] 3. Dealcoholization step

[0045] The mixture after washing with water is dealcoholized to obtain the crude produ...

Embodiment 3

[0051] The preparation method of this tri-n-hexyl trimellitate comprises the following steps:

[0052] 1. Esterification reaction steps

[0053] In a 500 liter reactor with heating device, electric stirring, thermometer water circulation condenser and oil-water separator, drop into 100 kilograms of trimellitic acid successively, C 8 -C 10 Alcohol 256 kg, concentrated sulfuric acid 0.3 kg, under stirring, micro-vacuum, while heating to boiling reaction, keep boiling reflux state, continuously separate water from the oil-water separator, until no water is generated, stop heating, esterification The reaction was terminated.

[0054] 2. Washing step

[0055] Add 250 kilograms of water to the mixed solution obtained after the esterification reaction, stir evenly, leave to stand to separate layers, and remove the water layer therein.

[0056] 3. Dealcoholization step

[0057] The mixture after washing with water is dealcoholized to obtain the crude product, trimellitic acid tri...

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PUM

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Abstract

The invention relates to an efficient trimellitate tri C8-C10 preparation method, which comprises: (1) an esterifying reaction, wherein trimellitic acid, C8-C10 alcohol and concentrated sulfuric acid are poured into a reaction kettle, stirring is performed, heating is performed until a boiling state is achieved, a reaction is performed, the boiling reflux state is maintained, and the water is separated; (2) water washing; (3) alcohol removing; (4) refining; and (5) filtering, wherein the refined mixing liquid is filtered to obtain the trimellitate tri C8-C10 product. According to the present invention, the trimellitate tri C8-C10 preparation method has characteristics of convenient operation, simpleness, easy performing and production efficiency improving, and is suitable for industrial production.

Description

technical field [0001] The invention belongs to the field of preparation of organic compounds, in particular to a high-efficiency tris-C trimellitic acid 8 -C 10 Esters are simple and effective preparation methods. Background technique [0002] In industrial production, plastic industry and military production, trimellitic acid tri-C 8 -C 10 Esters, as an important organic compound and heat-resistant, high-temperature-resistant plasticizer, have good electrical properties and are more and more widely used. trimellitic acid tri-C 8 -C 10 The usual production method of ester is direct esterification reaction, the color of the product obtained is yellow, difficult to sell as a product, must be further refined, that is, carry out a decompression refining treatment step, the problems of this type of preparation method: 1, due to decompression refining An expensive high-vacuum pump is required for the processing step, so this method has the problems of a large number of prod...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/76C07C67/08C07C67/48C07C67/56
CPCC07C67/08C07C67/48C07C67/56C07C69/76
Inventor 张富强
Owner TIANJIN CHEM REAGENT RES INST
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