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Method for refining diisobutyl sebacate

A technology of diisobutyl sebacate and a refining method, which is applied in the direction of carboxylate preparation, carboxylate separation/purification, chemical instruments and methods, etc., and can solve the problem of difficulty in reducing costs, unfavorable economic benefits, and many production equipments and other issues, to achieve the effect 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 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

[0025] The preparation method of this diisobutyl sebacate comprises the following steps:

[0026] 1. Esterification reaction steps

[0027] 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.

[0028] 2. Washing step

[0029] 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.

[0030] 3. Refining steps

[0031] Add 0.5 kg of refining agent (calcium hydroxide, magnesium hydroxide, activated carbon, magnesium sulfate m...

Embodiment 2

[0035] The preparation method of this diisobutyl sebacate comprises the following steps:

[0036] 1. Esterification reaction steps

[0037] 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.

[0038] 2. Washing step

[0039] 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.

[0040] 3. Refining steps

[0041] Add 0.6 kg of refining agent (calcium hydroxide, magnesium hydroxide, activated carbon, magnesium sulfate m...

Embodiment 3

[0045] The preparation method of this diisobutyl sebacate comprises the following steps:

[0046] 1. Esterification reaction steps

[0047] 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 oil-water separator. , while heating to boiling reaction, keep the state of boiling reflux, and continuously separate the water from the oil-water separator, until no water is generated, stop heating, and the esterification reaction is terminated.

[0048] 2. Washing step

[0049] 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.

[0050] 3. Refining steps

[0051] Add 0.7 kg of refining agent (calcium hydroxide, magnesium hydroxide, activated carbon, magnesium sulfate mixture) to the mixed solution after washing wit...

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Abstract

The invention relates to a method for refining diisobutyl sebacate, and the method comprises the following steps: (1) an esterification step, to be more specific, pouring sebacic acid, isobutyl alcohol and concentrated sulfuric acid into a reaction kettle, stirring, and heating to boil for reaction, and keeping a boiling reflux state for separation of water in the reaction kettle; (2) a water washing process; (3) a refining step, to be more specific, adding a refining agent into a mixture after the water washing step, and stirring for refining for an hour; and (4) a filtering step, to be more specific, filtering a mixed solution filter after the refining step to obtain a diisobutyl sebacate product. The refining agent used in the method for preparation of the diisobutyl sebacate is a mixture of calcium hydroxide, magnesium hydroxide, activated carbon and magnesium sulfate, and has the advantages of low cost and easy purchase.

Description

technical field [0001] The invention belongs to the field of organic compound preparation, in particular to a simple and effective method for refining diisobutyl sebacate. Background technique [0002] In industrial production, plastics industry and military production, diisobutyl sebacate, as an important organic compound and cold-resistant plasticizer, has more and more applications. 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 indis...

Claims

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Application Information

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