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Method for refining trioctyl trimellate and refining agent used in refining

A technology of tri-n-octyl trimellitate and refined preparations, which is applied in the field of organic compound preparation, can solve the problems of unfavorable economic benefits, difficulty in reducing costs, low production efficiency, etc., and achieves reduction of production costs, improvement of production efficiency, and convenient operation Effect

Inactive Publication Date: 2013-09-25
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: (50) g ​​sodium carbonate, (100) g magnesium carbonate, (200) g gac, (150) g ​​magnesium sulfate are mixed homogeneously.

[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 mixt...

Embodiment 2

[0025] Preparation of refined preparation: (60) g sodium carbonate, (60) g magnesium carbonate, (240) g gac, (180) g magnesium sulfate mix homogeneously.

[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 obta...

Embodiment 3

[0032] Preparation of refined preparation: (70) g sodium carbonate, (140) g magnesium carbonate, (280) g gac, (210) g magnesium sulfate mix homogeneously.

[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 obta...

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Abstract

The invention relates to a method for refining trioctyl trimellate and a refining agent used in the refining process. The refining agent comprises the following ingredients: 0.5 weight portions of sodium carbonate, 1 weight portion of magnesium carbonate, 2 weight portions of active carbon, and 1.5 weight portions of magnesium sulfate. The finished product of trioctyl trimellate is prepared by the following steps: adding the refining agent in the crude product of trioctyl trimellate with the weight ratio of the refining agent to trioctyl trimellate of 0.05-0.1:1, stirring for refining for 1 h, and filtering the refined mixed solution. The method omits the step of high vacuum refining, avoids the investment of high vavuum pump equipment, so that, the equipment investment is saved, the production cost is reduced, and the competition power of the product is increased.

Description

technical 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 expense...

Claims

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Application Information

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