A method for preparing 2,2,4-trimethyl-1,3-pentanediol diisobutyrate

A technology of pentanediol diisobutyrate and pentanediol monoisobutyrate, which is applied in the preparation of carboxylate, chemical instruments and methods, preparation of organic compounds, etc., can solve the problem of solid waste and waste water polluting the environment , complex process, low production efficiency and other problems, to achieve good economic and environmental benefits, simple operation, and reduced production costs

Inactive Publication Date: 2011-12-07
江苏天音化工有限公司 +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The problem of the above method is that after the reaction, the catalyst used needs to be removed by alkali neutralization, and the method has many side reactions, strong corrosion, complex process, low production efficiency, and produces a large amount of solid waste and waste water to pollute the environment.

Method used

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  • A method for preparing 2,2,4-trimethyl-1,3-pentanediol diisobutyrate
  • A method for preparing 2,2,4-trimethyl-1,3-pentanediol diisobutyrate

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Embodiment 1

[0024] process such as figure 1 As shown, the raw materials 2,2,4-trimethyl-1,3-pentanediol monoisobutyrate and isobutyric acid, which were preheated to 110°C, were mixed in a molar ratio of 1:1 at a flow rate of 15 L / h Continuously input the first fixed-bed reactor 1 equipped with 5 L of solid acid catalyst, the esterification reaction temperature is 110 °C, and the space velocity is 3 h -1 . The material reacted in the first fixed-bed reactor 1 enters the distillation tower 3. In the distillation tower 3, the water generated by the esterification reaction forms an azeotrope at 68-71 °C in the presence of water-carrying agent benzene and is continuously absorbed. separate. The material that has been dehydrated is continuously extracted with a flow rate of 30 L / h in the stripping section of the distillation tower 3 and delivered to the second stage fixed-bed reactor 2 equipped with 5 L of solid acid catalyst to continue the esterification reaction. The temperature is 120°C ...

Embodiment 2

[0026] process such as figure 1 As shown, the raw materials 2,2,4-trimethyl-1,3-pentanediol monoisobutyrate and isobutyric acid preheated to 95°C were mixed at a molar ratio of 1.5:1 at a flow rate of 20 L / h Continuously input the first fixed-bed reactor 1 equipped with 5 L of solid acid catalyst, the esterification reaction temperature is 95 ° C, and the space velocity is 4 h -1 . The material reacted in the first fixed-bed reactor 1 enters the distillation tower 3, and in the distillation tower 3, the water generated by the esterification reaction forms an azeotrope at 69-71 °C in the presence of cyclohexane water-carrying agent and continuously was separated. The esterification reaction material dehydrated is continuously drawn out with a flow rate of 40 L / h in the stripping section of the distillation tower 3 and delivered to the second stage fixed-bed reactor 2 equipped with 5 L of solid acid catalyst, and the esterification reaction temperature is 95°C, space velocity...

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Abstract

A process for preparing 2,2,4-trimethyl-1,3-pentanediol diisobutyrate by esterification, using 2,2,4-trimethyl-1,3-pentanediol monoisobutyrate Butyrate and isobutyric acid are used as raw materials, and a solid acid catalyst is used for a fixed-bed continuous esterification reaction. The esterification temperature is 70-150 ° C. The generated water is removed by azeotropic distillation; the esterification reaction product is rectified and removed. And recover unreacted 2,2,4-trimethyl-1,3-pentanediol monoisobutyrate and isobutyric acid to obtain 2,2,4-trimethyl-1,3-pentanediol Diisobutyrate. The method of the invention realizes the continuous production of 2,2,4-trimethyl-1,3-pentanediol diisobutyrate, has a simple operation mode, significantly improves production efficiency, reduces its production cost, and can reduce solid Pollutants and wastewater discharge, with excellent large-scale industrial application value.

Description

technical field [0001] The invention belongs to the field of fine chemicals, and relates to a method for preparing an aliphatic dibasic acid ester plasticizer, in particular to a method for preparing 2,2,4-trimethyl-1,3-pentanediol diisobutyric acid ester method. Background technique [0002] 2,2,4-Trimethyl-1,3-pentanediol diisobutyrate (TXIB) is a unique plasticizer with excellent performance. It has the characteristics of low viscosity, low density, low freezing point, hydrolysis resistance, colorless and transparent, high stability, safety and non-toxicity, etc. It is widely used in various PVC resin products, including PVC dipped gloves, toys, wallpaper, floor leather, artificial leather , Conveyor belts, etc. In addition, TXIB can also be applied to inks, pigments and EVA emulsions. [0003] There are few public reports about the preparation method of TXIB. US Patent No. 4110539A discloses a synthesis method of TXIB, which is prepared from 2,4-diisopropyl-5,5-dimeth...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/28C07C67/10
Inventor 秦怡生陈荣福朱红伟杨建国
Owner 江苏天音化工有限公司
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