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Method for preparing dinonyl adipate by utilizing refining agent

A dinonyl adipate and refined preparation technology, which is applied in the field of organic compound preparation, can solve the problems of difficulty in reducing costs, unfavorable economic benefits, and many production equipments, and achieve the effects of reducing production costs, saving investment, and convenient operation

Inactive Publication Date: 2013-02-06
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 dinonyl adipate is direct esterification reaction, and the color of the obtained product is yellow, which is difficult to sell as a product, and must be further refined, that is, a decompression refining treatment step. The problems in this type of preparation method: 1 .Because an expensive high-vacuum pump needs to be used in the decompression refining treatment step to realize, therefore, this method has the problems of many production equipments and high expenses, so it is difficult to reduce the cost; 2. Since the decompression refining treatment step is to produce adipic acid It is an indispensable and time-consuming production step in the dinonyl ester process. 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

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] A kind of method utilizing refined preparation to prepare dinonyl adipate comprises the following steps:

[0029] ⑴Esterification reaction steps

[0030] Add 100 kg of adipic acid, 220 kg of nonanol, and 0.3 kg of concentrated sulfuric acid successively into a 500-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.

[0031] ⑵Washing steps

[0032] 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.

[0033] ⑶ dealcoholization step

[0034] The mixture washed with water was dealcoholized to obtain the crude product, dinonyl adipate.

[0035] ⑷ Refining steps

[00...

Embodiment 2

[0040] A kind of method utilizing refined preparation to prepare dinonyl adipate comprises the following steps:

[0041] ⑴Esterification reaction steps

[0042] Add 100 kg of adipic acid, 220 kg of nonanol, and 0.3 kg of concentrated sulfuric acid successively into a 500-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.

[0043] ⑵Washing steps

[0044] 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.

[0045] ⑶ dealcoholization step

[0046] The mixture washed with water was dealcoholized to obtain the crude product, dinonyl adipate.

[0047] ⑷ Refining steps

[00...

Embodiment 3

[0052] A kind of method utilizing refined preparation to prepare dinonyl adipate comprises the following steps:

[0053] ⑴Esterification reaction steps

[0054] In a 500-liter reaction kettle with heating device, electric stirring, thermometer water circulation condenser and oil-water separator, drop into 100 kilograms of adipic acid successively, 220 kilograms of nonanol, 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.

[0055] ⑵Washing steps

[0056] 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.

[0057] ⑶ dealcoholization step

[0058] The mixture washed with water was dealcoholized to obtain the crude product, ...

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Abstract

The invention relates to a method for preparing dinonyl adipate by utilizing a refining agent. The method comprises the following steps: esterifying, namely, putting adipic acid, nonyl alcohol and concentrated sulfuric acid in a reaction kettle, stirring, carrying micro vacuumizing, heating to boil, reacting, and separating out water in the reaction under the condition that the boiling reflux state is maintained, wherein the weight ratio of adipic acid to nonyl alcohol to concentrated sulfuric acid is 1:2.2:(0.002-0.005); and then washing, dealcoholizing, refining and filtering. According to the refining method of dinonyl adipate, in the refining step, due to use of the refining agent, the color of the obtained product is light, the obtained product can be sold without high-vacuum refining treatment, and the quality of the prepared product completely meets the technical index requirements.

Description

technical field [0001] The invention belongs to the field of organic compound preparation, in particular to a method for preparing dinonyl adipate by using refined preparations. Background technique [0002] In industrial production, plastic industry and military production, dinonyl adipate, as an important organic compound and cold-resistant plasticizer, has been widely used. The usual production method of dinonyl adipate is direct esterification reaction, and the color of the obtained product is yellow, which is difficult to sell as a product, and must be further refined, that is, a decompression refining treatment step. The problems in this type of preparation method: 1 .Because an expensive high-vacuum pump needs to be used in the decompression refining treatment step to realize, therefore, this method has the problems of many production equipments and high expenses, so it is difficult to reduce the cost; 2. Since the decompression refining treatment step is to produce a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/44C07C67/08C07C67/48C07C67/56
Inventor 张富强
Owner TIANJIN CHEM REAGENT RES INST
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