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Method for refining adipate2-benzyl ethylhexyl and used refining agent thereof

A technology of ethylhexyl benzyl ester and adipic acid, applied in the field of organic compound preparation, can solve the problems of difficulty in cost reduction, unfavorable economic benefits, low production efficiency and the like, and achieve the effects of reducing production cost, improving production efficiency and being convenient to operate

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 2-ethylhexylbenzyl adipate is direct esterification reaction, the color of the obtained product is yellow, it is difficult to sell as a product, and further refining must be carried out, that is, the step of vacuum refining treatment, such preparation methods exist 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 2-ethylhexyl benzyl adipate, the method has the problems of long production time and low production efficiency, which is not conducive to 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 step: to one with heating unit, electric stirring, drop into 100 kilograms of adipic acid successively in 300 liters of reactors of thermometer water circulation condenser and vacuum oil-water separator, 140 kilograms of 2-ethylhexanols, 90 kilograms of benzyl 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 The reaction was terminated.

[0020] (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.

[0021] (3) Dealcoholization ste...

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: to one with heating unit, electric stirring, drop into 100 kilograms of adipic acid successively in 300 liters of reactors of thermometer water circulation condenser and vacuum oil-water separator, 140 kilograms of 2-ethylhexanols, 90 kilograms of benzyl 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 The reaction was terminated.

[0027] (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.

[0028] (3) Dealcoholization step: dealcoho...

Embodiment 3

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

[0033] (1) Esterification step: to one with heating unit, electric stirring, drop into 100 kilograms of adipic acid successively in 300 liters of reactors of thermometer water circulation condenser and vacuum oil-water separator, 140 kilograms of 2-ethylhexanols, 90 kilograms of benzyl 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 The 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: dealc...

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Abstract

The invention relates to a method for refining adipate2-benzyl ethylhexyl 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 adipate2-benzyl ethylhexyl comprises the following refining steps of: adopting the refining agent, adding the refining agent to a crude product of the adipate2-benzyl ethylhexyl with the mass ratio of the refining agent to adipate being 0.005-0.01:1, stirring and refining for one hour, and filtering refined mixed liquid to obtain a finished product of the adipate2-benzyl ethylhexyl. 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, and in particular relates to a method for refining 2-ethylhexylbenzyl adipate and the used refining agent. Background technique; [0002] In industrial production, plastics industry and military production, 2-ethylhexylbenzyl adipate is used more and more widely as an important organic compound and cold-resistant plasticizer. The usual production method of 2-ethylhexylbenzyl adipate is direct esterification reaction, the color of the obtained product is yellow, it is difficult to sell as a product, and further refining must be carried out, that is, the step of vacuum refining treatment, such preparation methods exist 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 ...

Claims

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Application Information

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IPC IPC(8): C07C69/44C07C67/56
Inventor 张富强
Owner TIANJIN CHEM REAGENT RES INST
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