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Method for refining diisobutyl adipate

A technology of diisobutyl adipate and a refining method, which is applied to the preparation of carboxylic acid esters, chemical instruments and methods, and the preparation of organic compounds, and can solve problems such as difficulty in reducing costs, unfavorable economic benefits, and low production efficiency. Achieve the effect of reducing production cost, saving investment and convenient operation

Inactive Publication Date: 2013-02-20
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 diisobutyl adipate is direct esterification reaction, and the color of the product obtained 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, the method has the problems of many production equipment and high costs, so it is difficult to reduce the cost; 2. Since the decompression refining treatment step is to produce a 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

[0028] A method for refining diisobutyl adipate, the steps are as follows:

[0029] ⑴Esterification reaction steps

[0030] Add 100 kg of adipic acid, 300 kg of isobutanol, and 0.3 kg of concentrated sulfuric acid into a 500-liter reactor with a heating device, electric stirring, thermometer water circulation condenser and oil-water separator, and heat to Boiling reaction, keep the boiling reflux state, continuously separate the water from the oil-water separator, until no water is generated, stop heating, and the esterification reaction is terminated.

[0031] ⑵Washing steps

[0032] Add 50 kg of water to the mixed solution obtained after the esterification reaction, stir evenly, leave to stand and separate the layers, and remove the water layer therein.

[0033] ⑶ dealcoholization step

[0034] The mixture washed with water was dealcoholized to obtain the crude product, diisobutyl adipate.

[0035] ⑷ Refining steps

[0036] Add 0.5 kg of refined preparation (a mixture o...

Embodiment 2

[0040] A method for refining diisobutyl adipate, the steps are as follows:

[0041] ⑴Esterification reaction steps

[0042] Put 100 kg of adipic acid, 300 kg of isobutyl alcohol, and 0.3 kg of concentrated sulfuric acid into a 500-liter reactor with a heating device, electric stirring, thermometer, water circulation condenser, and oil-water separator, and heat simultaneously under stirring. Until the boiling reaction, keep the boiling reflux state, continuously separate the water from the oil-water separator, until no water is generated, stop heating, and the esterification reaction is terminated.

[0043] ⑵Washing steps

[0044] Add 50 kg of water to the mixed solution obtained after the esterification reaction, stir evenly, leave to stand and separate the layers, and remove the water layer therein.

[0045] ⑶ dealcoholization step

[0046] The mixture washed with water was dealcoholized to obtain the crude product, diisobutyl adipate.

[0047] ⑷ Refining steps

[0048] ...

Embodiment 3

[0052] A method for refining diisobutyl adipate, the steps are as follows:

[0053] ⑴Esterification reaction steps

[0054] Add 100 kilograms of adipic acid, 300 kilograms of isobutyl alcohol, and 0.3 kilograms of concentrated sulfuric acid to a 500-liter reaction kettle with a heating device, electric stirring, thermometer water circulation condenser and oil-water separator. Heating to boiling reaction, maintaining the boiling reflux state, continuously separating water from the oil-water separator, until no water is generated, stop heating, and the esterification reaction is terminated.

[0055] ⑵Washing steps

[0056] Add 50 kg of water to the mixed solution obtained after the esterification reaction, stir evenly, leave to stand and separate the layers, and remove the water layer therein.

[0057] ⑶ dealcoholization step

[0058] The mixture washed with water was dealcoholized to obtain the crude product, diisobutyl adipate.

[0059] ⑷ Refining steps

[0060] Add 0.7 k...

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Abstract

The invention relates to a method for refining diisobutyl adipate. The method includes the following steps of an esterification reaction step, a washing step, a dealcoholization step, a refining step and a filtering step, wherein the refining step includes that a refining agent is added to a dealcoholized crude product, the refining agent and the dealcoholized crude product are stirred and refined for one hour, and the refining agent is formed by mixing sodium carbonate, magnesium carbonate, activated carbon and magnesium sulfate according to the weight ratio of 1: 1: 2: 1.5; and the filtering step includes filtering a refined mixed solution to obtain the diisobutyl adipate. According to the method for refining the diisobutyl adipate, in the refining step, the color of a product obtained by using the refining agent is lighter, the product can be sold without being subjected to high vacuum refining treatment, and the prepared product fully meets requirements of technical indexes. According to the preparation method, a high vacuum refining step is omitted during production, and input of high vacuum pump devices is avoided, so that device investment is saved, production costs are reduced, and market competitiveness of the product is improved.

Description

technical field [0001] The invention belongs to the field of organic compound preparation, in particular to a simple and effective preparation method of diisobutyl adipate. Background technique [0002] In industrial production, plastic industry and military production, diisobutyl adipate, as an important organic compound and cold-resistant plasticizer, has been widely used. The usual production method of diisobutyl adipate is direct esterification reaction, and the color of the product obtained 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, the method has the problems of many production equipment and high costs, so it is difficult to reduce the cost; 2. Since the decompression refining treatment step is to produce a Therefore, this ...

Claims

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Application Information

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IPC IPC(8): C07C69/44C07C67/08C07C67/56
Inventor 张富强
Owner TIANJIN CHEM REAGENT RES INST
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