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Preparation method of dioctyl 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 difficulty in cost reduction, unfavorable economic benefits, low production efficiency, etc., and achieves reduction in production cost, The effect of saving investment and convenient operation

Inactive Publication Date: 2015-12-30
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 diisooctyl 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 are as follows: 1. Due to the need to use expensive high-vacuum pumps in the decompression refining treatment step, this 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 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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preparation example Construction

[0026] A preparation method of diisooctyl adipate, the method may further comprise the steps:

[0027] 1. Esterification reaction steps

[0028] Add 100 kg of adipic acid, 220 kg of isooctyl alcohol, and 0.3 kg of concentrated sulfuric acid to a 500-liter reactor with a heating device, electric stirring, thermometer, water circulation condenser, and oil-water separator. Under stirring, a slight vacuum of 550mmHg Under the same conditions, heat to boiling reaction at the same time, keep the boiling reflux state, and continuously separate the water from the oil-water separator, until no water is generated, stop heating, and the esterification reaction is terminated.

[0029] 2. Washing steps

[0030] Add 50 kg of water to the mixed solution obtained after the esterification reaction, stir evenly, let stand to separate layers, and remove the water layer to obtain the washed mixture.

[0031] 3. Dealcoholization step

[0032] The mixture washed with water was dealcoholized to o...

Embodiment 2

[0038] A preparation method of diisooctyl adipate, the method may further comprise the steps:

[0039] 1. Esterification reaction steps

[0040] Add 100 kg of adipic acid, 220 kg of isooctyl alcohol, and 0.3 kg of concentrated sulfuric acid to a 500-liter reactor with a heating device, electric stirring, thermometer, water circulation condenser, and oil-water separator. Under stirring, a slight vacuum of 570mmHg Under the same conditions, heat to boiling reaction at the same time, keep the boiling reflux state, and continuously separate the water from the oil-water separator, until no water is generated, stop heating, and the esterification reaction is terminated.

[0041] 2. Washing steps

[0042] Add 50 kg of water to the mixed solution obtained after the esterification reaction, stir evenly, let stand to separate layers, and remove the water layer to obtain the washed mixture.

[0043] 3. Dealcoholization step

[0044] The mixture washed with water was dealcoholized to o...

Embodiment 3

[0050] A preparation method of diisooctyl adipate, the method may further comprise the steps:

[0051] 1. Esterification reaction steps

[0052] Add 100 kg of adipic acid, 220 kg of isooctyl 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. Under stirring, a slight vacuum of 590mmHg Under the same conditions, heat to boiling reaction at the same time, keep the boiling reflux state, and continuously separate the water from the oil-water separator, until no water is generated, stop heating, and the esterification reaction is terminated.

[0053] 2. Washing steps

[0054] Add 50 kg of water to the mixed solution obtained after the esterification reaction, stir evenly, let stand to separate layers, and remove the water layer to obtain the washed mixture.

[0055] 3. Dealcoholization step

[0056] The mixture washed with water was dealcoholized to...

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Abstract

The invention relates to a preparation method of dioctyl adipate. The preparation method includes the steps that 1, adipic acid, isooctyl alcohol and concentrated sulphuric acid are thrown into a reaction kettle, stirred and heated to a boiling reaction under the condition of micro-vacuum 550-590 mmHg, and a boiling reflux state is kept to separate water in the mixture; 2, water is added into a mixture after an esterification reaction, even stirring is performed, then standing layering is performed, and a water layer in the mixture is removed; 3, dealcoholization is performed on a rinsed mixture to obtain crude product dioctyl adipate; 4, a refining agent is added into the crude product after dealcoholization, stirring refining is performed for 1 hour, and mixed liquor is obtained and filtered; 5, the refined mixed liquor is filtered to obtain dioctyl adipate. In the refining step, the color intensity of the product obtained through using the refining agent becomes lower, and dioctyl adipate can serve as a product to be sold without high vacuum refining treatment. The quality of the prepared product completely meets technical index requirements, equipment investment is saved, the production cost is lowered, and the market competitiveness of the product is improved.

Description

technical field [0001] The invention belongs to the technical field of organic compound preparation, in particular to a simple and effective preparation method of diisooctyl adipate. Background technique [0002] In industrial production, plastic industry and military production, di-isooctyl adipate, as an important organic compound and cold-resistant plasticizer, has been widely used. The usual production method of diisooctyl 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 are as follows: 1. Due to needing to use expensive high vacuum pumps in the decompression refining treatment step, the method has the problems of many production equipments and high expenses, so it is difficult to reduce the cost. 2. Since the decompression refining treatment step is...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/44C07C67/08C07C67/48C07C67/62
Inventor 张富强
Owner TIANJIN CHEM REAGENT RES INST
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