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Preparation method of adipic acid-di-n-propyl ester

A technology of di-n-propyl adipate and adipic acid, applied in the field of preparation of di-n-propyl adipate, can solve the problems of unfavorable economic benefits, difficulty in cost reduction, low production efficiency, etc. The effect of production cost and convenient operation

Inactive Publication Date: 2010-12-29
TIANJIN CHEM REAGENT RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The problems that this preparation method exists are: 1, because need to use expensive high-vacuum pump to realize in the decompression refining treatment step, therefore, this method exists the problem of many production equipments, high cost, thus is difficult to reduce cost; 2, because The decompression refining treatment step is an indispensable and time-consuming production step in the production process of di-n-propyl adipate. Therefore, this method has the problems of long production time and low production efficiency, which is not conducive to the improvement of economic benefits of enterprises.

Method used

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Examples

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preparation example Construction

[0018] A preparation method of di-n-propyl adipate, comprising the following steps:

[0019] (1) Esterification step: drop into 100 kilograms of adipic acid, 85 kilograms of n-propanols, 0.3 kilograms of concentrated sulfuric acid successively in a 300-liter reactor with heating device, electric stirring, thermometer water circulation condenser and oil-water separator , heated to boiling reaction while stirring, kept boiling reflux state, continuously separated water from the oil-water separator, until no water was generated, stopped heating, and the esterification reaction was terminated.

[0020] (2) Water washing step: add 50 kilograms of water to the mixed solution obtained after the esterification reaction, stir evenly, leave to stand for stratification, and remove the water layer therein.

[0021] (3) Refining step: add 0.5 kg of refining agent (calcium hydroxide, magnesium hydroxide, activated carbon, magnesium sulfate mixture, its weight ratio 1:1:2:1.5) to the mixed s...

Embodiment 2

[0024] A preparation method of di-n-propyl adipate, comprising the following steps:

[0025] (1) Esterification step: drop into 100 kilograms of adipic acid, 85 kilograms of n-propanols, 0.3 kilograms of concentrated sulfuric acid successively in a 300-liter reactor with heating device, electric stirring, thermometer water circulation condenser and oil-water separator , heated to boiling reaction while stirring, kept boiling reflux state, continuously separated water from the oil-water separator, until no water was generated, stopped heating, and the esterification reaction was terminated.

[0026] (2) Water washing step: add 50 kilograms of water to the mixed solution obtained after the esterification reaction, stir evenly, leave to stand for stratification, and remove the water layer therein.

[0027] (3) Refining step: add 0.6 kg of refining agent (calcium hydroxide, magnesium hydroxide, gac, magnesium sulfate mixture, its weight ratio 1:1:2:1.5) to the mixed solution after...

Embodiment 3

[0030] A preparation method of di-n-propyl adipate, comprising the following steps:

[0031] (1) Esterification step: drop into 100 kilograms of adipic acid, 85 kilograms of n-propanols, 0.3 kilograms of concentrated sulfuric acid successively in a 300-liter reactor with heating device, electric stirring, thermometer water circulation condenser and oil-water separator , heated to boiling reaction while stirring, kept boiling reflux state, continuously separated water from the oil-water separator, until no water was generated, stopped heating, and the esterification reaction was terminated.

[0032] (2) Water washing step: add 50 kilograms of water to the mixed solution obtained after the esterification reaction, stir evenly, leave to stand for stratification, and remove the water layer therein.

[0033] (3) Refining step: add 0.7 kg of refining agent (calcium hydroxide, magnesium hydroxide, activated carbon, magnesium sulfate mixture, its weight ratio 1:1:2:1.5) to the mixed s...

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Abstract

The invention relates to a preparation method of adipic acid-di-n-propyl ester, comprising the following steps: (1) esterification reaction: putting adipic acid, normal propyl alcohol and concentrated sulphuric acid into a kettle, stirring, heating to boiling reaction, and keeping the boiling backflow state to separate water therein; (2) washing: adding water in mixture which finishes the esterification reaction, stirring evenly, standing, layering and removing an aqueous layer therein; (3) refining: adding refining agent into the washed mixture, and stirring and reining for one hour; and (4) filtering: filtering refined mixed liquor to obtain the adipic acid-di-n-propyl ester product. The preparation method of the invention saves the step of high-vacuum refining during production and avoids operation of high-vacuum pump equipment, thus saving equipment investment, lowering production cost and improving the market competitiveness of products.

Description

technical field [0001] The invention belongs to the field of organic compound preparation, in particular to a preparation method of di-n-propyl adipate. Background technique [0002] In industrial production and military production, di-n-propyl adipate is used more and more widely as an important organic compound. The usual production method of di-n-propyl adipate 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 that this preparation method exists are: 1, because need to use expensive high-vacuum pump to realize in the decompression refining treatment step, therefore, this method exists the problem of many production equipments, high cost, thus is difficult to reduce cost; 2, because The decompression refining treatment step is an indispensable and time-consuming production step in the production process ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/44C07C67/56C07C67/08
Inventor 张富强
Owner TIANJIN CHEM REAGENT RES INST
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