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Method for simultaneous synthesis of 2,2,4-trimethyl-1,3-pentanediol diisobutyrate and 2,2,4-trimethyl-1,3-pentanediol

A technology of pentylene glycol diisobutyrate and pentylene glycol monoisobutyrate, which is applied in the field of fine chemical industry, can solve problems such as unreported methods, and achieve a high conversion rate

Active Publication Date: 2016-03-16
SHANDONG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] At present, there are few bibliographic reports on the synthesis of 2,2,4-trimethyl-1,3-pentanediol diisobutyrate and 2,2,4-trimethyl-1,3-pentanediol. There is no report on the synthesis of 2,2,4-trimethyl-1,3-pentanediol diisobutyrate and 2,2,4-trimethyl-1,3-pentanediol

Method used

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  • Method for simultaneous synthesis of 2,2,4-trimethyl-1,3-pentanediol diisobutyrate and 2,2,4-trimethyl-1,3-pentanediol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Add 100 parts by weight of 2,2,4-trimethyl-1,3-pentanediol monoisobutyrate and 0.5 parts of H 3 PO 4 , Control the temperature at 150°C to carry out transesterification reaction to generate 2,2,4-trimethyl-1,3-pentanediol diisobutyrate and 2,2,4-trimethyl-1,3- Pentylene glycol, stop the reaction after 4h to obtain the reaction solution.

[0031] Add an appropriate amount of sodium hydroxide to the reaction solution to remove the acidic catalyst. Ordinary rectification at 165±5°C and pressure -0.08±0.005MPa to obtain 2,2,4-trimethyl-1,3-pentanediol diisobutyrate and 2,2,4-trimethyl -1,3-pentanediol.

[0032] Under these conditions, the conversion rate of 2,2,4-trimethyl-1,3-pentanediol monoisobutyrate was 48%, 2,2,4-trimethyl-1,3-pentanediol The yield of alcohol diisobutyrate was 46%.

Embodiment 2

[0034] Add 100 parts by weight of 2,2,4-trimethyl-1,3-pentanediol monoisobutyrate and 0.7 parts of HNO to a tank reactor with stirring and temperature control system 3 , Control the temperature at 170°C to carry out transesterification reaction to generate 2,2,4-trimethyl-1,3-pentanediol diisobutyrate and 2,2,4-trimethyl-1,3- Pentylene glycol, stop the reaction after 5h to obtain the reaction solution.

[0035] The reaction liquid is introduced into a reboiler, and reactive distillation is carried out at 155±5°C and a pressure of -0.09±0.005MPa. Obtain 2,2,4-trimethyl-1,3-pentanediol at the top of the rectification tower, keep the operating conditions unchanged, and continuously extract 2,2,4-trimethyl-1,3-pentanediol from the top of the tower Diol, 2,2,4-trimethyl-1,3-pentanediol monoisobutyrate in the kettle is continuously decomposed, and the final column is 2,2,4-trimethyl-1,3- Pentylene Glycol Diisobutyrate.

[0036] Under these conditions, the conversion rate of 2,2,4...

Embodiment 3

[0038] In the tank reactor with stirring and temperature control system, add 100 parts by weight of 2,2,4-trimethyl-1,3-pentanediol monoisobutyrate and 0.5 part of sulfuric acid to control the temperature Perform transesterification at 150°C to generate 2,2,4-trimethyl-1,3-pentanediol diisobutyrate and 2,2,4-trimethyl-1,3-pentanediol , After 5h, the reaction was stopped to obtain a reaction solution.

[0039] The reaction liquid is introduced into a reboiler, and reactive distillation is carried out at 175±5°C and a pressure of -0.08±0.005MPa. Obtain 2,2,4-trimethyl-1,3-pentanediol at the top of the rectification tower, keep the operating conditions unchanged, and continuously extract 2,2,4-trimethyl-1,3-pentanediol from the top of the tower Diol, 2,2,4-trimethyl-1,3-pentanediol monoisobutyrate in the kettle is continuously decomposed, and the final column is 2,2,4-trimethyl-1,3- Pentylene Glycol Diisobutyrate.

[0040] Under these conditions, the conversion rate of 2,2,4-t...

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Abstract

The present invention relates to the field of fine chemicals, and in particular relates to a method for simultaneous synthesis of 2,2,4-trimethyl-1,3-pentanediol diisobutyrate and 2,2,4-trimethyl-1,3-pentanediol. The 2,2,4-trimethyl-1,3-pentanediol diisobutyrate and the 2,2,4-trimethyl-1,3-pentanediol can be obtained by transesterification of 2,2,4-trimethyl-1,3-pentanediol monoisobutyrate under the effect of an acidic catalyst according to the method. A new method for synthesis of the 2,2,4-trimethyl-1,3-pentanediol diisobutyrate and the 2,2,4-trimethyl-1,3-pentanediol is provided, and according to the situation, product separation can be performed by ordinary distillation or reactive distillation. When the ordinary distillation is used for the product separation, 2,2,4-trimethyl-1,3-pentanediol monoisobutyrate conversion rate is 45 to 60%. When the reactive distillation is used for the product separation, the 2,2,4-trimethyl-1,3-pentanediol monoisobutyrate conversion rate is high and can reach 98 to 99%.

Description

technical field [0001] The invention relates to the field of fine chemical industry, in particular to a simultaneous synthesis of 2,2,4-trimethyl-1,3-pentanediol diisobutyrate and 2,2,4-trimethyl-1,3- Pentylene glycol method. Background technique [0002] 2,2,4-Trimethyl-1,3-pentanediol diisobutyrate is an excellent plasticizer. 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 an ideal substitute for the existing carcinogenic plasticizer phthalate diester. This plasticizer meets the highest standards required by current national regulations, and has low initial viscosity, excellent viscosity stability and processability. This plasticizer can meet the requirements of high-speed molding production efficiency and cycle cycle. This product is widely used in various PVC resin products, including PVC dipped gloves, toys, wallpapers, floor leather, ar...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C29/09C07C29/80C07C31/20C07C67/03C07C67/54C07C69/28
CPCC07C29/09C07C29/80C07C67/03C07C67/54C07C31/20C07C69/28Y02P20/10
Inventor 宋峰庄淑娟崔洪友刘然升李岩梅
Owner SHANDONG UNIV OF TECH
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