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

A technology of pentanediol monoisobutyrate and trimethyl, which is applied in the field of preparation 2, can solve the problems of high catalyst toxicity, under-mild reaction conditions, and equipment corrosion, and achieve environmentally friendly synthesis processes, mild reaction conditions, and equipment little corrosion effect

Inactive Publication Date: 2010-10-20
江苏天音化工有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, when sodium hydroxide is used as the catalyst for the Tishchenko reaction, the product yield is low, many by-products cause serious corrosion to equipment, the reaction conditions are not mild enough, and the amount of wastewater discharge is large
When barium hydroxide is used as the catalyst for the Tishchenko reaction, although the product yield can be increased, the catalyst is highly toxic, expensive, and has a large amount of waste water discharge
In 2004, EASTMAN Company reported the solid base for the synthesis of 2,2,4-trimethyl-1,3-pentanediol monoisobutyrate with sodium hydroxide modified soil montmorillonite, gelatinous clay and kaolin Catalyst, but the catalytic activity is low, and the reaction time is as long as 200h (US6794325)
Therefore, the synthesis of 2,2,4-trimethyl-1,3-pentanediol monoisobutyrate in the prior art cannot simultaneously achieve the goals of high yield per pass, few by-products, low cost, and environmental friendliness

Method used

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

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Experimental program
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Embodiment 1

[0023] Using isobutyraldehyde as raw material, 2,2,4-trimethyl-1,3-pentanediol monoisobutyrate is prepared through two steps of isobutyraldehyde condensation and Jishchenko reaction, in which isobutyraldehyde condensation product occurs The catalyst used in the Tishchenko reaction is layered magnesium-aluminum anion clay supported by tert-butoxy anion pillars.

[0024] Preparation of layered magnesium aluminum anion clay catalyst supported by tert-butoxy anion pillars:

[0025] (1) Magnesium aluminum anion clay (MgAl-HT-NO 3 ) preparation

[0026] In a reaction kettle with a thermometer, a stirrer and a dropping funnel, under nitrogen protection, 30.8g (0.12mol) Mg(NO 3 ) 2 6H20 and 15.0g (0.04mol) Al(NO 3 ) 3 9H 2 0 completely dissolved in 100mL of CO removal 2 deionized water; at room temperature and under stirring conditions, add 2M NaOH solution dropwise. During the dropping process, the pH value of the slurry is controlled at about 10, and the dropping time is kept...

Embodiment 2-4

[0038] Prepare 2,2,4-trimethyl-1,3-pentanediol monoisobutyrate according to the method of Example 1, and other conditions are the same as Example 1, except that the catalyst is reused 3 times, and The reaction results are shown in Table 1 below:

[0039] Table 1

[0040]

Embodiment 5-7

[0042] Prepare 2,2,4-trimethyl-1,3-pentanediol monoisobutyrate according to the method of Example 1, and other conditions are the same as in Example 1, except that the 2nd) reaction of step Jishchenko reaction The time is 5, 15, 20 hours respectively. Its reaction result is as shown in table 2 below:

[0043] Table 2

[0044]

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Abstract

The invention provides an environmental-friendly method for preparing 2,2,4-trimethyl-1,3-pentanediol monoisobutyrate, which comprises a condensation reaction and a Tishchenko reaction of isobutyraldehyde, wherein condensation products of the isobutyraldehyde are subjected to the Tishchenko reaction under the catalytic action of tert-butoxy anion-pillared layered magnesium-aluminum anionic clay to generate 2,2,4-trimethyl-1,3-pentanediol monoisobutyrate. The preparation method has the advantages of high single-pass yield, high selectivity of target products, a few by-products, mild reaction conditions, catalyst recycling and environmental-friendly synthetic process.

Description

technical field [0001] The invention belongs to the field of fine chemicals and relates to a method for preparing 2,2,4-trimethyl-1,3-pentanediol monoisobutyrate. Background technique [0002] 2,2,4-Trimethyl-1,3-pentanediol monoisobutyrate is a film-forming aid for water-based architectural coatings (usually latex paints), with excellent film-forming effect, non-toxic and harmless, etc. Advantages, suitable for vinyl acetate homopolymerization and copolymerization emulsion, acrylate homopolymerization and copolymerization emulsion, vinyl acetate / acrylate copolymerization emulsion, styrene / methacrylate copolymerization emulsion, vinyl acetate / vinyl carbonate copolymerization emulsion, styrene / Acrylic ester / methyl methacrylate / glycidyl methacrylate multi-copolymer emulsion and other coating systems. It can also be used as a film-forming aid for water-based inks. At present, my country's paint production ranks third in the world, second only to the United States and Japan, ...

Claims

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Application Information

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IPC IPC(8): C07C69/28C07C67/44B01J31/26
CPCY02P20/584
Inventor 秦怡生杨建国秦旭东陈荣福王伟哈健蒋大智张学军朱红伟段启伟
Owner 江苏天音化工有限公司
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