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Preparation method of 2,2,4-trimethyl-3-hydroxypentanoic acid n-butyl ester, latex paint and preparation method thereof

A technology of n-butyl hydroxyvalerate and hydroxyvaleric acid, which is applied in the synthesis and application of organic compounds, can solve the problems of slow drying speed, low film forming efficiency, poor water whitening resistance, etc., and achieve less side reactions and high reaction rate , no by-product effects

Active Publication Date: 2022-05-03
RUNTAI CHEM TAIXING CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The coalescent of existing exterior wall latex paint generally adopts dodecyl alcohol ester (2,2,4-trimethyl-1,3 pentanediol-monoisobutyrate), but dodecyl alcohol ester The film-forming efficiency is relatively low, and the film-forming aid with high film-forming efficiency has a relatively high boiling point and slow volatilization, so it is not suitable for use on exterior walls, and the existing exterior wall latex paint made of dodecyl alcohol esters has The drying speed is slow at low temperature and the initial water whitening resistance is not good. Therefore, it is necessary to develop a film-forming aid that can improve the film-forming efficiency of latex paint and the drying speed at low temperature while solving the problem of early water whitening resistance of latex paint. At the same time, it is necessary to develop A kind of latex paint containing the coalescent

Method used

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  • Preparation method of 2,2,4-trimethyl-3-hydroxypentanoic acid n-butyl ester, latex paint and preparation method thereof
  • Preparation method of 2,2,4-trimethyl-3-hydroxypentanoic acid n-butyl ester, latex paint and preparation method thereof
  • Preparation method of 2,2,4-trimethyl-3-hydroxypentanoic acid n-butyl ester, latex paint and preparation method thereof

Examples

Experimental program
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Effect test

preparation example Construction

[0031] A kind of preparation method of 2,2,4-trimethyl-3 hydroxypentanoic acid n-butyl ester, comprises the following steps:

[0032] 1) Preparation of 2,2,4-trimethyl-3-hydroxypentanoic acid

[0033] Isobutyraldehyde undergoes an aldol condensation reaction under the action of a basic catalyst to generate 2,2,4-trimethyl-3-hydroxypentanal. The reaction formula is as follows:

[0034] 2

[0035] The 2,2,4-trimethyl-3-hydroxypentanal obtained above was mixed with H 2 o 2 Oxidation reaction occurs to obtain 2,2,4-trimethyl-3 hydroxypentanoic acid, the reaction formula is as follows:

[0036]

[0037] 2) Preparation of n-butyl 2,2,4-trimethyl-3 hydroxypentanoate

[0038] The 2,2,4-trimethyl-3 hydroxyvaleric acid and n-butanol obtained in step 1) are reacted under the action of a strong acid catalyst to obtain 2,2,4-trimethyl-3 hydroxyvaleric acid n-butyl, and the reaction The formula is as follows:

[0039]

[0040] In the step 1), the basic catalyst is NaOH, KOH, Ca(...

Embodiment 1

[0046] The preparation method of the 2,2,4-trimethyl-3 hydroxyvaleric acid n-butyl ester of the present embodiment comprises the following steps:

[0047] 1) Preparation of 2,2,4-trimethyl-3-hydroxypentanoic acid

[0048] With 600g isobutyraldehyde and 45 grams, mass fraction is 40% Ba(OH) 2 Add the solutions into the reaction kettle respectively, stir and raise the temperature to 55°C. After reacting for 7 hours, take samples for gas chromatography test at intervals of 30 minutes. When 2,2,4-trimethyl-3-hydroxypentanal Stop the reaction when the content of isobutyraldehyde no longer increases, then distill off the unreacted isobutyraldehyde at 70°C and -0.1MPa, then wash with water, separate the oil phase product, and obtain 520g of 2,2,4-trimethyl- 3-Hydroxypentanal.

[0049] Add the 2,2,4-trimethyl-3-hydroxyvaleraldehyde obtained above into the reaction kettle, raise the temperature to 80°C, and add hydrogen peroxide dropwise while reacting. 2 o 2 The mass fraction of t...

Embodiment 2

[0055] The preparation method of the 2,2,4-trimethyl-3 hydroxyvaleric acid n-butyl ester of the present embodiment comprises the following steps:

[0056] 1) Preparation of 2,2,4-trimethyl-3-hydroxypentanoic acid

[0057] Add 700g of isobutyraldehyde and 60g of KOH solution with a mass fraction of 35% into the reaction kettle respectively, stir and raise the temperature to 65°C, after reacting for 2 hours, take samples at 30-minute intervals for gas chromatography test, when two consecutive chromatographic tests Stop the reaction when the content of 2,2,4-trimethyl-3-hydroxypentanal no longer increases, then distill off the unreacted isobutyraldehyde at 65°C and -0.05MPa, then wash with water, and separate the oil phase product, 620g of 2,2,4-trimethyl-3-hydroxypentanal was obtained.

[0058] Add the 2,2,4-trimethyl-3-hydroxyvaleraldehyde obtained above into the reaction kettle, raise the temperature to 50°C, and add hydrogen peroxide dropwise while reacting. 2 o 2 The mass...

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Abstract

The invention relates to the technical field of organic compound synthesis and application, in particular to a preparation method of n-butyl 2,2,4-trimethyl-3 hydroxypentanoate, which contains 2,2,4-trimethyl-3 hydroxypentyl Latex paint of n-butyl ester and preparation method thereof. The preparation method of 2,2,4-trimethyl-3 hydroxy-n-butyl valerate of the present invention comprises the following steps: 1) isobutyraldehyde undergoes an aldol condensation reaction under the action of a basic catalyst to generate 2,2, 4-Trimethyl-3-hydroxypentanal; the 2,2,4-trimethyl-3-hydroxypentanal obtained above was mixed with H 2 o 2 Oxidation reaction to obtain 2,2,4-trimethyl-3 hydroxyvaleric acid; 2) 2,2,4-trimethyl-3 hydroxyvaleric acid and n-butanol prepared in step 1) under the action of a strong acid catalyst The reaction yields n-butyl 2,2,4-trimethyl-3-hydroxyvalerate.

Description

technical field [0001] The invention relates to the technical field of synthesis and application of organic compounds, in particular to a preparation method of n-butyl 2,2,4-trimethyl-3-hydroxypentanoate, which contains 2,2,4-trimethyl-3-hydroxypentanoic acid Latex paint of n-butyl ester and preparation method thereof. Background technique [0002] Latex paint is a type of paint with polymer emulsion as the film-forming substance, also known as synthetic resin emulsion paint. It generally uses water as the dispersion medium, and has the characteristics of simple preparation process, relatively environmental protection, and good color retention. The coalescent of existing exterior wall latex paint generally adopts dodecyl alcohol ester (2,2,4-trimethyl-1,3 pentanediol-monoisobutyrate), but dodecyl alcohol ester The film-forming efficiency is relatively low, and the film-forming aid with high film-forming efficiency has a relatively high boiling point and slow volatilization,...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C67/08C07C69/675C07C45/72C07C47/19C07C51/285C07C59/01C09D133/04C09D7/63C09D5/02
CPCC07C67/08C07C45/72C07C51/285C09D133/04C09D5/024C08K5/101C07C47/19C07C59/01C07C69/675
Inventor 卢小松张世元姜明秋王永成张润赟
Owner RUNTAI CHEM TAIXING CO LTD
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