Method for preparing 2,2,4-trimethyl-1,3-pentanediol diisobutyrate

A technology of pentanediol diisobutyrate and trimethyl is applied in the preparation of carboxylate, chemical instruments and methods, preparation of organic compounds, etc., and can solve the problems of high production cost, expensive monoisobutyrate and the like , to achieve the effect of simple operation and avoiding the need for a large amount of lye to neutralize the product

Inactive Publication Date: 2015-02-11
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But the raw material 2,2,4-trimethyl-1,3-pentanediol monoisobutyrate

Method used

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

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Experimental program
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Embodiment 1

[0022] a. Bubble the gas purging device with stirring, reflux condenser, water separator and sieve plate (the structure of the gas purging device is a two-way with a gas regulating valve: one end has a sand core sieve plate, extending The gas can be blown out evenly under the liquid surface; the other end is connected to the reactor with a gas flow meter), and 40 g of green leaf oxane (2,4-diisopropyl-5,5-dimethyl-1,3 -dioxane), add 0.6g PW 12 (12-phosphotungstic acid) / SiO 2 (weight 40wt%) load heteropoly acid, slowly add 42g isobutyric acid dropwise with stirring, and carry out the reaction at 150°C; the reaction time is 7h;

[0023] b. The interval is 1 to 2 hours. When small water droplets appear on the surface of the water separator, adjust the flow rate of the gas flow meter of the gas purging device to 12L / h, and control the gas flow rate to separate the isobutyraldehyde and water generated in the reaction;

[0024] c, after the reaction finishes, adjust the gas flow r...

Embodiment 2

[0027] a. Bubble the gas purging device with stirring, reflux condenser, water separator and sieve plate (the structure of the gas purging device is a two-way with a gas regulating valve: one end has a sand core sieve plate, extending The gas can be blown out evenly under the liquid surface; the other end is connected to the reactor with a gas flow meter), and 20g of green leaf oxane (2,4-diisopropyl-5,5-dimethyl-1,3 -dioxane), add 0.3g copper p-toluenesulfonate, slowly add 28g isobutyric acid dropwise with stirring, and carry out the reaction at 150°C; the reaction time is 7h;

[0028] b. The interval is 1 to 2 hours. When small water droplets appear on the surface of the water separator, adjust the flow rate of the gas flow meter of the gas purging device to 12L / h, and control the gas flow rate to separate the isobutyraldehyde and water generated in the reaction;

[0029] c, after the reaction finishes, adjust the gas flow rate of the gas purging device to be 24L / h, control ...

Embodiment 3-10

[0032] a. Bubble the gas purging device with stirring, reflux condenser, water separator and sieve plate (the structure of the gas purging device is a two-way with a gas regulating valve: one end has a sand core sieve plate, extending The gas can be blown out evenly under the liquid surface; the other end is connected to the reactor with a gas flow meter), and an appropriate amount of aoba oxane (2,4-diisopropyl-5,5-dimethyl-1,3 -dioxane) and p-toluenesulfonic acid, slowly add an appropriate amount of isobutyric acid dropwise with stirring, and carry out the reaction at 150-160 °C; the reaction time is 6-9h;

[0033] b. The interval time is 1min to 4h. When small water droplets appear on the surface of the water separator, adjust the flow rate of the gas flow meter of the gas purging device to 12L / h, and control the gas flow rate to separate the isobutyraldehyde and water generated in the reaction;

[0034] c, after the reaction finishes, adjust the gas flow rate of the gas pu...

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Abstract

The present invention discloses a method for preparing 2,2,4-trimethyl-1,3-pentanediol diisobutyrate. According to the method, green oxane(2,4-diisopropyl-5,5-dimethyl-1,3-dioxane) and isobutyric acid are subjected to the catalysis cracking and esterification reaction under the catalyst effect to synthesize the 2,2,4-trimethyl-1,3-pentanediol diisobutyrate, wherein the isobutyric acid is added in a dropwise manner, and a molar ratio of the (2,4-diisopropyl-5,5-dimethyl-1,3-dioxane) to the isobutyric acid is 1:2-1:5. The method has characteristics of simple process, clean process and high yield.

Description

technical field [0001] The invention belongs to the field of fine chemicals, and relates to a preparation method of aliphatic dibasic acid ester green plasticizer, in particular to a preparation method of 2,2,4-trimethyl-1,3-pentanediol bisisobutylene Synthesis of acid esters. Background technique [0002] 2,2,4-Trimethyl-1,3-pentanediol diisobutyrate (TXIB) is an important green, non-toxic and environmentally friendly plasticizer with low viscosity, low density, low freezing point, anti- Features such as hydrolysis, colorless transparency, high stability, safety and non-toxicity, this plasticizer meets the highest standards required by regulations, and its non-toxic properties reassure many toy manufacturers and consumers. The plasticizer does not require re-formulation, reducing the risk of costly product recalls and customer complaints due to re-formulation errors. Due to its low tack and excellent viscosity stability and processability, the plasticizer can meet high-sp...

Claims

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Application Information

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IPC IPC(8): C07C69/28C07C67/08
CPCC07C67/08C07C69/28
Inventor 高爽李国松李军吕迎
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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