Method for directly synthesizing 2,2,4-trimethyl-1,3-pentanediol diisobutyrate from isobutyraldehyde

A technology of pentylene glycol diisobutyrate and pentylene glycol monoisobutyrate, which is applied to the preparation of carboxylic acid esters, chemical instruments and methods, and the preparation of organic compounds, and can solve the high cost of separation and purification and potential safety hazards and other problems, to achieve the effect of low price, simplified operation process, and cheap and easy-to-obtain raw materials

Active Publication Date: 2016-05-04
SHANDONG UNIV OF TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although both 2,2,4-trimethyl-1,3-pentanediol monoisobutyrate and isobutyric acid can be obtained by converting isobutyraldehyde, the cost of separation and purification is high
Moreover, there is a potential safety hazard in the process of isobutyraldehyde oxidation to isobutyric acid

Method used

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  • Method for directly synthesizing 2,2,4-trimethyl-1,3-pentanediol diisobutyrate from isobutyraldehyde
  • Method for directly synthesizing 2,2,4-trimethyl-1,3-pentanediol diisobutyrate from isobutyraldehyde
  • Method for directly synthesizing 2,2,4-trimethyl-1,3-pentanediol diisobutyrate from isobutyraldehyde

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Embodiment 1

[0031] The method for directly synthesizing 2,2,4-trimethyl-1,3-pentanediol diisobutyrate by isobutyraldehyde, the steps are as follows:

[0032] (1) In the tank reactor with stirring and temperature control system, add 1 part by weight of basic catalyst NaOH, and slowly add 50 parts by weight of isobutyraldehyde dropwise under stirring conditions, and control the temperature at 40 ° C Carry out aldol condensation reaction and disproportionation into ester reaction to obtain a reaction solution of 2,2,4-trimethyl-1,3-pentanediol monoisobutyrate and unreacted isobutyraldehyde; the reaction time is 5 hours , the conversion rate of isobutyraldehyde in aldol condensation reaction and disproportionation into ester reaction is controlled at 62.1%.

[0033] (2) NaOH in the reaction solution is filtered out, and the oxidation catalyst MnO is added to the reactor 2 Afterwards, the oxidant air is passed into the reaction kettle, and the temperature is controlled at 60° C., and the reac...

Embodiment 2

[0037] The method for directly synthesizing 2,2,4-trimethyl-1,3-pentanediol diisobutyrate by isobutyraldehyde, the steps are as follows:

[0038] (1) In the tank reactor with stirring, temperature control system, add the basic catalyst Ca(OH) of 4 parts by weight 2 , under stirring conditions, slowly add 200 parts by weight of isobutyraldehyde dropwise, and control the temperature at 80°C for aldol condensation reaction and disproportionation into ester reaction to obtain 2,2,4-trimethyl-1,3-pentane The reaction solution of diol monoisobutyrate and unreacted isobutyraldehyde; the reaction time is 3 hours, and the conversion rate of isobutyraldehyde in aldol condensation reaction and disproportionation into ester reaction is controlled to be 63.6%.

[0039] (2) Ca(OH) in the reaction solution 2 Filter out, and add oxidation catalyst MnO to the reactor 2 After that, add the oxidant hydrogen peroxide to the reaction kettle, control the temperature at 60°C, and react for 5 hours...

Embodiment 3

[0043] The method for directly synthesizing 2,2,4-trimethyl-1,3-pentanediol diisobutyrate by isobutyraldehyde, the steps are as follows:

[0044] (1) In the tank reactor with stirring and temperature control system, add 2 parts by weight of basic catalyst Na 2 O, under stirring conditions, slowly add 200 parts by weight of isobutyraldehyde dropwise, and control the temperature to carry out aldol condensation reaction and disproportionation into ester reaction at 60°C to obtain 2,2,4-trimethyl-1,3- The reaction solution of pentanediol monoisobutyrate and unreacted isobutyraldehyde; the reaction time is 2 hours, and the conversion rate of isobutyraldehyde in aldol condensation reaction and disproportionation into ester reaction is controlled to be 67.3%.

[0045] (2) Na in the reaction liquid 2 O is filtered out and the oxidation catalyst Fe is added to the reactor 2 o 3 Afterwards, feed oxidant oxygen into the reactor, control the temperature at 100°C, and react for 7 hours ...

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Abstract

The invention belongs to the field of fine chemical engineering, and particularly relates to a method for directly synthesizing 2,2,4-trimethyl-1,3-pentanediol diisobutyrate from isobutyraldehyde. According to the method, isobutyraldehyde, as a by-product of an industrial butanol-octanol production process, is taken as a raw material, and 2,2,4-trimethyl-1,3-pentanediol diisobutyrate is directly synthesized. The method comprises the following steps: firstly, conducting aldol condensation and disproportionation-esterification on part of isobutyraldehyde to obtain 2,2,4-trimethyl-1,3-pentanediol isobutyrate; then, conducting oxidization on the remaining unreacted isobutyraldehyde to generate isobutyric acid, wherein separation and purification are not needed; finally, carrying out an esterification reaction to obtain 2,2,4-trimethyl-1,3-pentanediol diisobutyrate. The method has the following advantages: the raw material is cheap and easy to obtain, and can be recycled for several times; the intermediate product needs not be separated and can be directly synthesized into the final product, so as to simplify the technical operation process for generation of the final product; and the raw material conversion rate is high, that is, the isobutyraldehyde conversion rate exceeds 92%.

Description

technical field [0001] The invention belongs to the field of fine chemicals, and in particular relates to a method for directly synthesizing 2,2,4-trimethyl-1,3-pentanediol diisobutyrate from isobutyraldehyde. Background technique [0002] 2,2,4-Trimethyl-1,3-pentanediol diisobutyrate is an excellent plasticizer with low viscosity, low density, low freezing point, hydrolysis resistance, colorless and transparent, It is characterized by high stability, safety and non-toxicity, and is an ideal substitute for phthalate diester plasticizers widely used in industry. Because of its extremely low toxicity and good safety in use, the plasticizer fully complies with the requirements of current domestic and foreign regulations on green and safe plasticizers. Due to its low initial tack, excellent viscosity stability and processability, this plasticizer can meet the requirements of high-speed molding, shorten cycle time and improve production efficiency. The plasticizer can be widely...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C45/74C07C47/263C07C67/00C07C69/28C07C51/235C07C53/124C07C67/08
CPCC07C45/74C07C51/235C07C67/00C07C67/08C07C47/263C07C69/28C07C53/124
Inventor 宋峰庄淑娟崔洪友刘然升
Owner SHANDONG UNIV OF TECH
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