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Method for refining tri-n-hexyl trimellitate and refining agent used in method

A technology of tri-n-hexyl trimellitate and trimellitic acid, which is applied in the field of organic compound preparation, can solve problems such as unfavorable economic benefits, difficulty in reducing costs, and low production efficiency, so as to reduce production costs, improve production efficiency, and operate convenient effect

Inactive Publication Date: 2011-11-23
TIANJIN CHEM REAGENT RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The usual production method of tri-n-hexyl trimellitate is direct esterification, 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. Since the decompression refining treatment step requires the use of expensive high vacuum pumps, this method has the problems of a large number of production equipment and high costs, making it difficult to reduce costs
2. Since the decompression refining treatment step is an indispensable and time-consuming production step in the process of producing tri-n-hexyl trimellitate, the method has the problems of long production time and low production efficiency, which is not conducive to the economic benefits of enterprises 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, (100) g gac, (150) g ​​magnesium sulfate mix homogeneously.

[0019] (1) Esterification step: drop into successively 100 kilograms of trimellitic acid, 256 kilograms of n-hexanols, 0.3 kilograms of concentrated sulfuric acid in a 500-liter reactor with a heating device, electric stirring, thermometer water circulation condenser and vacuum oil-water separator. Kilogram, under stirring, slight 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, 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 was...

Embodiment 2

[0025] Preparation of refined preparation: (60) g sodium carbonate, (120) g magnesium carbonate, (120) g gac, (180) g magnesium sulfate mix homogeneously.

[0026] (1) Esterification step: drop into successively 100 kilograms of trimellitic acid, 256 kilograms of n-hexanols, 0.3 kilograms of concentrated sulfuric acid in a 500-liter reactor with a heating device, electric stirring, thermometer water circulation condenser and vacuum oil-water separator. Kilogram, under stirring, slight 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, 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 ...

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, 256 kilograms of n-hexanols, 0.3 kilograms of concentrated sulfuric acid in a 500-liter reactor with a heating device, electric stirring, thermometer water circulation condenser and vacuum oil-water separator. Kilogram, under stirring, slight 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, 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 m...

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Abstract

The invention relates to a method for refining tri-n-hexyl trimellitate and a refining agent used in the method. The refining agent comprises the following components: sodium carbonate, magnesium carbonate, activated carbon and magnesium sulfate, wherein the mass ratio of sodium carbonate to magnesium carbonate to activated carbon to magnesium sulfate is 0.5:1:2:1.5. The method for preparing the tri-n-hexyl trimellitate comprises the following refining steps: adding the refining agent in a tri-n-hexyl trimellitate crude product, stirring and refining for 1 hour, wherein the mass ratio of refining agent to trimellitic acid is (0.05-0.1):1; and filtering a mixed liquid after refining so as to obtain the tri-n-hexyl trimellitate finished product. In the preparation method, a high vacuum refining step is omitted when in production, and the investment of high vacuum pump equipment is avoided, thus saving equipment investment, reducing production cost and improving the market competitiveness of a product.

Description

technology field; [0001] The invention belongs to the field of organic compound preparation, in particular to a method for refining tri-n-hexyl trimellitate and a used refining preparation thereof. Background technique; [0002] In industrial production, plastic industry and military production, tri-n-hexyl 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-hexyl trimellitate is direct esterification, 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. Since an expensive high-vacuum pump needs to be used in the decompression refining treatment step, this method has the problems of a large number of production equipment and high costs, making it di...

Claims

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Application Information

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IPC IPC(8): C07C69/76C07C67/56C07C67/08
Inventor 张富强
Owner TIANJIN CHEM REAGENT RES INST
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