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Preparation method of dinonyl adipate

A technology of dinonyl adipate and adipic acid, which is applied in the field of organic compound preparation, can solve problems such as difficult cost reduction, unfavorable economic benefits, and low production efficiency, and achieve the effects of reducing production costs, saving investment, and convenient operation

Inactive Publication Date: 2013-02-27
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 preparation method of 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

[0036] Add 0.5 kg of refined ...

Embodiment 2

[0040] A kind of preparation method of 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

[0048] Add 0.6 kg of refined ...

Embodiment 3

[0052] A kind of preparation method of 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, dinonyl adipate.

[0059]...

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Abstract

The invention relates to a preparation method of dinonyl adipate. The method comprises the following steps of: (1) performing an esterification reaction step, i.e., adding adipic acid, nonanol and concentrated sulfuric acid into a reaction kettle, stirring, treating under a micro-vacuum condition and heating to be boiled for reaction, and keeping in a boiling reflow state to separate moisture in the mixture, and the weight ratio of the adipic acid to the nonanol to the concentrated sulfuric acid is 1:2.2:0.002-0.005; and then washing, dealcoholizing, refining and filtering. The refining method of the dinonyl adipate is in the refining step; by using a refining agent, the color of an obtained product becomes light; the dinonyl adipate can be used as a product to be sold without high-vacuum refining treatment; the quality of the prepared product fully meets the technical index requirement.

Description

technical field [0001] The invention belongs to the field of organic compound preparation, in particular to a simple and effective preparation method of dinonyl adipate. 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 adipic ac...

Claims

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Application Information

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