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Refining method of dinonyl adipate

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

Inactive Publication Date: 2013-02-06
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 , due to the need to use expensive high vacuum pumps in the decompression refining treatment step to realize, therefore, there are many production equipments and high cost problems in this method, so it is difficult to reduce the cost; 2, because 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

[0027] A method for refining dinonyl adipate, comprising the following steps:

[0028] ⑴Esterification reaction steps

[0029] 100 kilograms of adipic acid, 220 kilograms of nonanol, and 0.3 kilograms of concentrated sulfuric acid are successively dropped into a 500-liter reactor with a heating device, electric stirring, a thermometer water circulation condenser and a vacuum oil-water separator, and under stirring, a 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.

[0030] ⑵Washing steps

[0031] 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.

[0032] ⑶ dealcoholization step

[0033] The mixture washed with water was dealcoholized to obtain crude dinonyl adipa...

Embodiment 2

[0039] A method for refining dinonyl adipate, comprising the following steps:

[0040] ⑴Esterification reaction steps

[0041] 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.

[0042] ⑵Washing steps

[0043] 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.

[0044] ⑶ dealcoholization step

[0045] The mixture washed with water was dealcoholized to obtain the crude product, dinonyl adipate.

[0046] ⑷ Refining steps

[0047] Add 0.6 kg of refined preparat...

Embodiment 3

[0051] A method for refining dinonyl adipate, comprising the following steps:

[0052] ⑴Esterification reaction steps

[0053] 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.

[0054] ⑵Washing steps

[0055] 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.

[0056] ⑶ dealcoholization step

[0057] The mixture washed with water was dealcoholized to obtain the crude product, dinonyl adipate.

[0058] ⑷ Refining steps

[0059] Add 0.7 kg of refined preparat...

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Abstract

The invention relates to a refining method of dinonyl adipate. The method comprises the following steps: esterifying: putting adipic acid, nonyl alcohol and concentrated sulfuric acid in a reaction kettle, stirring, carrying out micro vacuumizing, heating to boil, reacting, and separating out water in the reaction under the condition that 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, the color of the product obtained by using the refining agent is light, the product can be sold without high-vacuumizing treatment, and the quality of the prepared product completely meets the technical index requirements. The high-vacuumizing refining step is omitted during production, and the investment of a high-vacuumizing pump is avoided, thus equipment investment is saved, production cost is reduced, and the market competitiveness of the product is improved.

Description

technical field [0001] The invention belongs to the field of organic compound preparation, in particular to a method for refining dinonyl adipate. Background technique [0002] In industrial production, plastics industry and military production, dinonyl adipate is used more and more widely as an important organic compound and cold-resistant plasticizer. 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 , due to the need to use expensive high vacuum pumps in the decompression refining treatment step to realize, therefore, there are many production equipments and high cost problems in this method, so it is difficult to reduce the cost; 2, because the decompression refining treatment step is to produce adipic acid It is an indisp...

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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