Preparation method of diisooctyl adipate

A technology of diisooctyl adipate and adipic acid, which is applied in the field of preparation of diisooctyl adipate, can solve the problems of difficult cost reduction, unfavorable economic benefits, long production time, etc., and achieve reduction of production cost, Saving investment and convenient operation

Inactive Publication Date: 2013-09-11
TIANJIN CHEM REAGENT RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The usual production method of diisooctyl adipate is direct esterification reaction, the color of the obtained product is yellow, it is difficult to sell as a product, and it 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 needs to use an expensive high-vacuum pump, 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 diisooctyl adipate, 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

[0030] A preparation method of diisooctyl adipate, the steps are as follows:

[0031] ⑴Esterification reaction steps

[0032] 100 kg of adipic acid, 220 kg of isooctyl alcohol, and 0.3 kg of concentrated sulfuric acid were successively put into a 500-liter reactor equipped with a heating device, electric stirring, thermometer, water circulation condenser, and oil-water separator. Under stirring, a slight vacuum ( 500~600mmHg), heat to boiling at the same time, keep boiling and reflux, and continuously separate water from the oil-water separator until no water is formed, then stop heating, the esterification reaction is terminated, and a mixed solution is obtained.

[0033] ⑵Washing steps

[0034] 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.

[0035] ⑶ dealcoholization step

[0036] The mixture washed with water was dealcoholized to obtain the crud...

Embodiment 2

[0043] A preparation method of diisooctyl adipate, the steps are as follows:

[0044] ⑴Esterification reaction steps

[0045] 100 kg of adipic acid, 220 kg of isooctyl alcohol, and 0.3 kg of concentrated sulfuric acid were successively put into a 500-liter reactor with a heating device, electric stirring, thermometer water circulation condenser, and oil-water separator. Under stirring, a slight vacuum ( 500~600mmHg), while heating to boiling reaction, keep boiling reflux state, continuously separate water from the oil-water separator, until no water is formed, stop heating, and the esterification reaction is terminated.

[0046] ⑵Washing steps

[0047] 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.

[0048] ⑶ dealcoholization step

[0049] The mixture washed with water was dealcoholized to obtain the crude product of diisooctyl adipate.

[0050] ⑷ ...

Embodiment 3

[0056] A preparation method of diisooctyl adipate, the steps are as follows:

[0057] ⑴Esterification reaction steps

[0058] Put 100 kg of adipic acid, 220 kg of isooctyl alcohol, and 0.3 kg of concentrated sulfuric acid into a 500-liter reactor equipped with a heating device, electric stirring, thermometer, water circulation condenser, and oil-water separator. (500 ~ 600mmHg), while heating to boiling reaction, 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.

[0059] ⑵Washing steps

[0060] Add 50 kilograms of water to the mixed solution obtained after the esterification reaction, stir evenly, let stand to separate layers, and remove the water layer therein.

[0061] ⑶ dealcoholization step

[0062] The mixture washed with water was dealcoholized to obtain the crude product of diisooctyl adipate.

[0063] ⑷ Refining steps

[0064] Add 0.7 kg of ...

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PUM

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Abstract

The invention relates to a preparation method of diisooctyl adipate. The preparation method comprises the following steps of: putting adipic acid, isooctanol and concentrated sulfuric acid into a reaction kettle; under stirring condition, heating for a boiling reaction in micro-vacuum (500-600 mmHg), keeping a boiling reflux state and separating out moisture from the mixture; adding water to a mixture subjected to esterification reaction, standing for layering after even stirring, and removing the moisture from the mixture; dealcoholizing the mixture subjected to water washing, thereby obtaining the crude product of diisooctyl adipate; adding a refining agent to the dealcoholized crude product and stirring and refining; and filtering the refined mixed liquid, thereby obtaining the diisooctyl adipate. According to the method provided by the invention, the refining agent (a mixture of sodium carbonate, magnesium carbonate, active carbon and magnesium sulfate) is used in the refining step, so that the color of the obtained diisooctyl adipate is lighter and the diisooctyl adipate can be sold out as a product without high-vacuum refining treatment; and the quality of the prepared diisooctyl adipate completely meets the requirements of technical indexes.

Description

technical field [0001] The invention belongs to the field of organic compound preparation, in particular to a method for preparing diisooctyl adipate. Background technique [0002] In industrial production, plastics industry and military production, di-isooctyl adipate, as an important organic compound and cold-resistant plasticizer, is more and more widely used. [0003] The usual production method of diisooctyl adipate is direct esterification reaction, the color of the obtained product is yellow, it is difficult to sell as a product, and it 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 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-consumi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/44C07C67/08C07C67/48
Inventor 张富强
Owner TIANJIN CHEM REAGENT RES INST
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