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Preparation method for refining dibutyl adipate

A technology of di-n-butyl adipate and adipic acid, which is applied in the field of organic compound preparation, can solve the problems of difficult cost reduction, unfavorable economic benefits, low production efficiency, etc., and achieves production cost reduction, investment saving, and convenient operation Effect

Inactive Publication Date: 2017-03-22
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 di-n-butyl 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 pumps in the decompression refining treatment step, the method has the problems of many production equipment and high costs, so it is difficult to reduce the cost; 2. Since the decompression refining treatment step is to produce a 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 preparation method for refining di-n-butyl adipate, the steps are as follows:

[0029] ⑴Esterification reaction steps

[0030] Add 100 kg of adipic acid, 300 kg of n-butanol, and 0.3 kg of concentrated sulfuric acid to 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.

[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, di-n-butyl adipate.

[0035] ⑷ Refining steps

[0036] Add 0.5 kg of refining agent (a mixtu...

Embodiment 2

[0040] A preparation method for refining di-n-butyl adipate, the steps are as follows:

[0041] ⑴Esterification reaction steps

[0042] Put 100 kg of adipic acid, 300 kg of n-butyl alcohol, 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 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.

[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, di-n-butyl adipate.

[0047] ⑷ Refining steps ...

Embodiment 3

[0052] A preparation method for refining di-n-butyl adipate, the steps are as follows:

[0053] ⑴Esterification reaction steps

[0054] Add 100 kilograms of adipic acid, 300 kilograms of n-butyl alcohol, and 0.3 kilograms of concentrated sulfuric acid to 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.

[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, di-n-butyl adipate.

[0059] ⑷ Refining steps

[0060] Add 0....

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Abstract

The invention relates to a preparation method for refining dibutyl adipate. The preparation method comprises the following steps: (1) an esterification reaction step; (2) a washing step; (3) a dealcoholization step; (4) a refining step: adding a refining agent into a crude product obtained after dealcoholization and carrying out stirring and refining for one hour, wherein the refining agent is prepared by mixing calcium hydrate, magnesium hydroxide, active carbon and magnesium sulfate according to a weight ratio of 1: 1: 2: 1.5; and (5) a filtering step: filtering a refined mixed solution so as to obtain a dibutyl adipate product. In the refining step, the product obtained after treatment by the refining agent has a lighter color and can be sold without high-vacuum refining, and the quality of the prepared product completely meets requirements of technical indexes. The preparation method omits the step of high-vacuum refining, so a high-vacuum pump is not needed; thus, equipment investment is saved, production cost is lowered, 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 simple and effective preparation method of di-n-butyl adipate. Background technique [0002] In industrial production, plastic industry and military production, di-n-butyl adipate, as an important organic compound and cold-resistant plasticizer, has been widely used. The usual production method of di-n-butyl 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 pumps in the decompression refining treatment step, the method has the problems of many production equipment and high costs, so it is difficult to reduce the cost; 2. Since the decompression refining treatment step is to produce a Therefore, this ...

Claims

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Application Information

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IPC IPC(8): C07C67/08C07C67/48C07C69/44
CPCC07C67/08C07C67/48C07C69/44
Inventor 张富强
Owner TIANJIN CHEM REAGENT RES INST
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