Preparation method of diisobutyl adipate

A technology of diisobutyl adipate and adipic acid, which is applied in the field of organic compound preparation, can solve problems such as expensive vacuum degree, unfavorable economic benefits, and difficulty in reducing costs, and achieve low prices, reduce production costs, and avoid investment Effect

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 diisobutyl adipate is direct esterification reaction, and the color of the product obtained 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 in this type of preparation method: 1. Due to the need to use expensive, high-vacuum, and high-efficiency vacuum pumps in the decompression and refining treatment steps, this method has the problems of many production equipment and high costs, so it is difficult to reduce costs
2. Since the decompression refining treatment step is an indispensable and time-consuming production step in the production of diisobutyl 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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preparation example Construction

[0026] A preparation method of diisobutyl adipate, the method may further comprise the steps:

[0027] ⑴Esterification reaction steps

[0028] Put adipic acid, isobutanol, and concentrated sulfuric acid into the reaction kettle, stir, and heat to boiling reaction under slight vacuum, and keep the boiling reflux state to separate the water therein.

[0029] ⑵Washing steps

[0030] Water is added to the mixture after the esterification reaction, and after being stirred evenly, the mixture is left standing to separate layers, and the water layer is removed.

[0031] ⑶ dealcoholization step

[0032] The mixture washed with water was dealcoholized to obtain the crude product, diisobutyl adipate.

[0033] ⑷ Refining steps

[0034] Add the refining agent to the crude product after dealcoholization, stir and refine for one hour.

[0035] ⑸Filtration steps

[0036] Filter the refined mixed solution to obtain diisobutyl adipate product.

[0037] The refined preparation is prepare...

Embodiment 1

[0042] A preparation method for diisobutyl adipate, comprising the following steps:

[0043] ⑴Esterification reaction steps

[0044] Put 100 kg of adipic acid, 300 kg of isobutanol, 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, and heat simultaneously under stirring. Until the boiling reaction, keep the boiling reflux state, continuously separate the water from the oil-water separator, until no water is generated, 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, leave to stand and separate the layers, and remove the water layer therein.

[0047] ⑶ dealcoholization step

[0048] The mixture washed with water was dealcoholized to obtain the crude product, diisobutyl adipate.

[0049] ⑷ Refining...

Embodiment 2

[0054] A preparation method for diisobutyl adipate, comprising the following steps:

[0055] ⑴Esterification reaction steps

[0056] Add 100 kg of adipic acid, 300 kg of isobutanol, and 0.3 kg of concentrated sulfuric acid into a 500-liter reactor with a heating device, electric stirring, thermometer water circulation condenser and oil-water separator, and heat to Boiling reaction, keep the boiling reflux state, continuously separate the water from the oil-water separator, until no water is generated, stop heating, and the esterification reaction is terminated.

[0057] ⑵Washing steps

[0058] 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.

[0059] ⑶ dealcoholization step

[0060] The mixture washed with water was dealcoholized to obtain the crude product, diisobutyl adipate.

[0061] ⑷ Refining steps

[0062] Add 0.6 kg of refined preparation (ca...

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PUM

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Abstract

The invention relates to a preparation method of diisobutyl adipate. The method includes following steps of an esterification reaction step, a washing step, a dealcoholizing step, a refining step and a filtering step, wherein the dealcoholizing step is that refining agents are added to dealcoholized coarse products to be stirred and refined for one hour, and the filtering step is that refined mixed liquids are filtered to obtain a diisobutyl adipate product. According to the preparation method of the diisobutyl adipate, the refining agents are used in the refining step so that the color of the final obtained product is shallow, the product can be sold without high vacuum refining processing, and the quality of the prepared product completely fits with technical indicator requirements. According to the preparation method, a high vacuum refining step is omitted during production, investment for high vacuum pump devices is avoided, accordingly, device investment is saved, production costs are reduced, and market competition of the product is improved.

Description

technical field [0001] The invention belongs to the field of organic compound preparation, in particular to a simple and effective preparation method of diisobutyl adipate. Background technique [0002] In industrial production, plastics industry and military production, diisobutyl adipate is an important organic compound and cold-resistant plasticizer, which has more and more applications. The usual production method of diisobutyl adipate is direct esterification reaction, and the color of the product obtained 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 in this type of preparation method: 1. Due to the need to use expensive, high-vacuum, and high-efficiency vacuum pumps in the decompression refining treatment step, this method has the problems of many production equipment and high costs, so it is difficult to reduce the cost. 2. Since the decompression refining t...

Claims

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Application Information

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