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Preparation method of diisooctyl adipate

A technology of diisooctyl adipate and adipic acid, which is applied in the field of preparation of diisooctyl adipate, can solve problems such as difficult cost reduction, unfavorable economic benefits, and many production equipments, so as to reduce production costs, The effect of saving investment and convenient operation

Inactive Publication Date: 2013-09-04
TIANJIN CHEM REAGENT RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The usual production method of diisooctyl adipate is direct esterification reaction, the color of the obtained product is yellow, it is difficult to sell as a product, and it 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 process of producing diisooctyl adipate, 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

[0029] A preparation method of diisooctyl adipate, the steps are as follows:

[0030] ⑴Esterification reaction steps

[0031] Put 100 kg of adipic acid, 220 kg of isooctyl alcohol, and 0.3 kg of concentrated sulfuric acid into a 500-liter reactor equipped with a heating device, electric stirring, thermometer water circulation condenser, and vacuum oil-water separator. (500~600mmHg), heat to boiling at the same time, keep boiling and reflux, and continuously separate water from the oil-water separator until no water is formed, then stop heating, the esterification reaction is terminated, and a mixed solution is obtained.

[0032] ⑵Washing steps

[0033] Add 50 kg of water to the mixed solution in step (1), stir evenly, let stand to separate layers, and remove the water layer therein to obtain the mixture.

[0034] ⑶ dealcoholization step

[0035] The mixture washed with water is dealcoholized to obtain the crude product of diisooctyl adipate.

[0036] ⑷ Refining steps

[0...

Embodiment 2

[0042] A preparation method of diisooctyl adipate, the steps are as follows:

[0043] ⑴Esterification reaction steps

[0044] 100 kg of adipic acid, 220 kg of isooctyl alcohol, and 0.3 kg of concentrated sulfuric acid were successively put into a 500-liter reactor with a heating device, electric stirring, thermometer water circulation condenser, and oil-water separator. Under stirring, a slight vacuum ( 500~600mmHg), while heating to boiling reaction, keep boiling reflux state, continuously separate water from the oil-water separator, until no water is formed, stop heating, and the esterification reaction is terminated.

[0045] ⑵Washing steps

[0046] Add 50 kg of water to the mixed solution obtained after the esterification reaction, stir evenly, let stand to separate layers, and remove the water layer to obtain the mixture.

[0047] ⑶ dealcoholization step

[0048] The mixture washed with water is dealcoholized to obtain the crude product of diisooctyl adipate.

[0049]...

Embodiment 3

[0055] A preparation method of diisooctyl adipate, the steps are as follows:

[0056] ⑴Esterification reaction steps

[0057] 100 kg of adipic acid, 220 kg of isooctyl alcohol, and 0.3 kg of concentrated sulfuric acid were successively put into a 500-liter reactor with a heating device, electric stirring, thermometer water circulation condenser, and oil-water separator. Under stirring, a slight vacuum ( 500~600mmHg), while heating to boiling reaction, keep the boiling reflux state, continuously separate the water from the oil-water separator, until no water is formed, stop heating, the esterification reaction is terminated, and the mixed solution is obtained.

[0058] ⑵Washing steps

[0059] Add 50 kg of water to the mixed solution in step (1), stir evenly, let stand to separate layers, and remove the water layer therein to obtain the mixture.

[0060] ⑶ dealcoholization step

[0061] The mixture washed with water is dealcoholized to obtain the crude product of diisooctyl a...

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Abstract

The invention relates to a preparation method of diisooctyl adipate. The preparation method comprises the following steps of: putting adipic acid, isooctanol and concentrated sulfuric acid into a reaction kettle, heating until the materials are boiled under the conditions of stirring and micro-vacuum (500-600mmHG), keeping a boiling reflux state, and separating water from the heated mixture till no water exists in the heated mixture; adding water to the mixture subjected to an esterification reaction, uniformly stirring, standing for layering, and removing a water layer to obtain a water-washed mixture; dealcoholizing the water-washed mixture to obtain a rough diisooctyl adipate product; adding a refining agent to the rough diisooctyl adipate product, stirring and refining; and filtering the refined mixture liquid to obtain the diisooctyl adipate. According to the preparation method, in the production process, the refining agent (a calcium oxide, magnesium oxide, activated carbon and silica mixture) is used, so that the product quality and the long-term storage stability are ensured; meanwhile, the preparation method has the characteristics of simpleness in implementation and convenience for operation and is convenient for industrial production; and the investment of production equipment is saved and the production efficiency is improved.

Description

technical field [0001] The invention belongs to the field of organic compound preparation, in particular to a method for preparing diisooctyl adipate. Background technique [0002] In industrial production, plastic industry and military production, di-isooctyl adipate is used more and more widely as an important organic compound and cold-resistant plasticizer. [0003] The usual production method of diisooctyl adipate is direct esterification reaction, the color of the obtained product is yellow, it is difficult to sell as a product, and it 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 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 ...

Claims

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Application Information

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