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Refining method of dihexyl sebacate

A refining method and technology of sebacic acid are applied in the preparation of carboxylate, separation/purification of carboxylate, chemical instruments and methods, etc., and can solve the problems of unfavorable economic benefits, difficulty in cost reduction, and many production equipment, etc. Reduce production costs, achieve simple and easy-to-operate effects

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 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 refining 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

[0027] The refining method of this di-n-hexyl sebacate comprises the following steps:

[0028] 1. Esterification reaction steps

[0029] 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.

[0030] 2. Washing step

[0031] 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.

[0032] 3. Dealcoholization step

[0033] The mixture washed with water was dealcoholized to obtain the crude product, di-n-hexyl sebacate.

[0034] 4. Refining steps

[0035] Add 0.5 kg of refining age...

Embodiment 2

[0039] The refining method of this di-n-hexyl sebacate comprises the following steps:

[0040] 1. Esterification reaction steps

[0041] 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.

[0042] 2. Washing step

[0043] 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.

[0044] 3. Dealcoholization step

[0045] The mixture washed with water was dealcoholized to obtain the crude product, di-n-hexyl sebacate.

[0046] 4. Refining steps

[0047] Add 0.6 kg of refining age...

Embodiment 3

[0051] The refining method of this di-n-hexyl sebacate comprises the following steps:

[0052] 1. Esterification reaction steps

[0053] In a 300 liter reactor with heating device, electric stirring, thermometer water circulation condenser and oil-water separator, drop into 100 kilograms of sebacic acid successively, 160 kilograms of n-hexanol, 0.3 kilogram of vitriol oil, under stirring, slight vacuum, At the same time, heat to boiling reaction, keep the boiling reflux state, and continuously separate water from the oil-water separator until no water is generated, stop heating, and the esterification reaction is terminated.

[0054] 2. Washing step

[0055] 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.

[0056] 3. Dealcoholization step

[0057] The mixture washed with water was dealcoholized to obtain the crude product, di-n-hexyl sebacate.

[00...

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Abstract

The invention relates to a refining method of dihexyl sebacate. The method comprises the following steps: (1) esterification reaction: adding sebacic acid, hexyl alcohol and concentrated sulfuric acid into a reaction kettle, stirring, heating to realize boiling reaction, and keeping in a boiling reflux state to separate water from a mixture; (2) washing: adding water into the mixture prepared by the esterification reaction, stirring uniformly, standing and layering to remove a water layer from the mixture; (3) dealcoholization: dealcoholizing the washed mixture to obtain a crude product of dihexyl sebacate; (4) refining and filtering, thus obtaining a dihexyl sebacate product. A refining agent used in the refining method of the dihexyl sebacate is a mixture of calcium hydroxide, magnesium hydroxide, activated carbon and magnesium sulfate, and has the characteristics of low cost and easiness for purchasing.

Description

technical field [0001] The invention belongs to the field of organic compound preparation, in particular to a simple and effective method for refining 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 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 refining 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 i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/50C07C67/08C07C67/48C07C67/56
CPCC07C67/08C07C67/48C07C67/56C07C69/50
Inventor 张富强
Owner TIANJIN CHEM REAGENT RES INST
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