Quick preparation method of di-n-hexyl sebacate

A technology of sebacic acid and n-hexyl ester, which is applied in the field of organic compound preparation, can solve the problems of difficulty in reducing costs, unfavorable economic benefits, and low production efficiency, and achieve the effects of reducing production costs, saving investment, and convenient operation

Inactive Publication Date: 2017-03-22
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 di-n-hexyl sebacate 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 , 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 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 di-n-hexyl sebacate, the method has the problems of long production time and low production efficiency, which is not conducive to the economic benefit of the enterprise improve

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] The preparation method of this di-n-hexyl sebacate comprises the following steps:

[0029] 1. Esterification reaction steps

[0030] To a heating device, electric stirring, thermometer, water circulation condenser and oil-water separation

[0031] 100 kilograms of sebacic acid, 160 kilograms of n-hexanol, and 0.3 kilograms of concentrated sulfuric acid were successively put into the 300-liter reactor of the reactor. The water is separated out, until no water is generated, the heating is stopped, and the esterification reaction is terminated.

[0032] 2. Washing step

[0033] 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.

[0034] 3. Dealcoholization step

[0035] The mixture washed with water was dealcoholized to obtain the crude product, di-n-hexyl sebacate.

[0036] 4. Refining steps

[0037] Add 0.5 kg of refining preparation (sodium ca...

Embodiment 2

[0041] The preparation method of this di-n-hexyl sebacate comprises the following steps:

[0042] 1. Esterification reaction steps

[0043] Add 100 kg of sebacic acid, 160 kg of n-hexanol, and 0.3 kg of concentrated sulfuric acid to a 300-liter reactor 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.

[0044] 2. Washing step

[0045] 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.

[0046] 3. Dealcoholization step

[0047] The mixture washed with water was dealcoholized to obtain the crude product, di-n-hexyl sebacate.

[0048] 4. Refining steps

[0049] Add 0.6 kg of refining ...

Embodiment 3

[0053] The preparation method of this di-n-hexyl sebacate comprises the following steps:

[0054] 1. Esterification reaction steps

[0055] To a heating device, electric stirring, thermometer, water circulation condenser and oil-water separation

[0056] 100 kg of sebacic acid, 160 kg of n-hexanol, and 0.3 kg of concentrated sulfuric acid were successively put into the 300-liter reactor of the reactor. Under stirring, a slight vacuum was heated to boiling reaction at the same time. The water is separated, and the heating is stopped until no water is generated, and the esterification reaction is terminated.

[0057] 2. Washing step

[0058] 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.

[0059] 3. Dealcoholization step

[0060] The mixture washed with water was dealcoholized to obtain the crude product, di-n-hexyl sebacate.

[0061] 4. Refining st...

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PUM

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Abstract

The invention relates to a quick preparation method of di-n-hexyl sebacate. The method includes the following steps: (1) an esterification reaction step: putting sebacic acid, n-hexyl alcohol and concentrated sulfuric acid into a reaction kettle, stirring, heating to carrying out boiling reaction, keeping a boiling reflux state, and separating water; (2) a water washing step: adding water into the mixture after the esterification reaction, stirring evenly, standing to layer, and removing an aqueous layer; (3) a dealcoholization step: dealcoholizing the mixture after the water washing, to obtain a crude product di-n-hexyl sebacate; and (4) a refining step and a filtration step to obtain the di-n-hexyl sebacate product. The preparation method of di-n-hexyl sebacate has the advantages of convenient operation, simple and feasible operation, and easy realization of industrialized production, and improves the production efficiency.

Description

technical field [0001] The invention belongs to the field of organic compound preparation, in particular to a quick preparation method of di-n-hexyl sebacate. Background technique [0002] In industrial production, plastic industry and military production, di-n-hexyl sebacate, as an important organic compound and cold-resistant plasticizer, has more and more applications. The usual production method of di-n-hexyl sebacate 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 , because it needs to use expensive high-vacuum pump to realize in the decompression refining treatment step, therefore, this method has the problems of many production equipments and high cost, thus it is difficult to reduce the cost. 2. Since the decompression refining treatment step is an indispensab...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/08C07C67/48C07C69/50
CPCC07C67/08C07C67/48C07C69/50
Inventor 张富强
Owner TIANJIN CHEM REAGENT RES INST
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