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Preparation method of diisobutyl sebacate

A technology of diisobutyl sebacate and sebacic acid, which is applied in the field of preparation of organic compounds, can solve the problems of unfavorable economic benefits, difficulty in reducing costs, and many production equipments, and achieve reduction of production costs, simple implementation, and convenient operation Effect

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 diisobutyl 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. 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 production of diisobutyl sebacate, 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

[0026] The preparation method of this diisobutyl sebacate comprises the following steps:

[0027] 1. Esterification reaction steps

[0028] Add 100 kg of sebacic acid, 115 kg of isobutanol, and 0.3 kg of concentrated sulfuric acid to a 300-liter reactor with a heating device, electric stirring, thermometer water circulation condenser and vacuum oil-water separator. , 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.

[0029] 2. Washing step

[0030] 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.

[0031] 3. Refining steps

[0032] Add 0.5 kg of refining agent (calcium oxide, magnesium oxide, activated carbon, silicon dioxide mixture) to the mixed solution after washing with water, and stir an...

Embodiment 2

[0036] The preparation method of this diisobutyl sebacate comprises the following steps:

[0037] 1. Esterification reaction steps

[0038] 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, 115 kilograms of isobutanol, 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.

[0039] 2. Washing step

[0040] 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.

[0041] 3. Refining steps

[0042] Add 0.6 kg of refining agent (calcium oxide, magnesium oxide, activated carbon, silicon dioxide mixture) to...

Embodiment 3

[0046] The preparation method of this diisobutyl sebacate comprises the following steps:

[0047] 1. Esterification reaction steps

[0048] 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, 115 kilograms of isobutanol, 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.

[0049] 2. Washing step

[0050] 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.

[0051] 3. Refining steps

[0052] Add 0.7 kg of refining agent (calcium oxide, magnesium oxide, activated carbon, silicon dioxide mixture) to...

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Abstract

The invention relates to a preparation method of diisobutyl sebacate. The method comprises the following steps: (1) an esterification reaction step: sebacic acid, isobutanol, and concentrated sulfuric acid are added into a reaction vessel, stirring is carried out in micro-vacuum, heating is carried out till a boiling reaction, boiling and backflow state are kept in order to separate moisture in the materials; (2) a washing step; (3) a refining step, (4) a filtering step: refined mixed liquor is filtered, and the diisobutyl sebacate product is obtained. A refining agent used in the preparation method of diisobutyl sebacate is a mixture of calcium oxide, magnesium oxide, active carbon, and silicon dioxide, and the method has the characteristics of low price and easy purchase.

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 sebacate. Background technique [0002] In industrial production, plastics industry and military production, diisobutyl sebacate is more and more widely used as an important organic compound and cold-resistant plasticizer. The usual production method of diisobutyl 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. Since an expensive high-vacuum pump needs to be used in the decompression refining treatment step, this method has the problems of a large number of production equipment and high costs, making it difficult to reduce the cost. 2. Since the decompression refining treatment step is an indispe...

Claims

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Application Information

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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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