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Preparation method of 2,2,4-trimethyl-3-hydroxyvaleric acid methyl ester, steel structure water-based industrial paint and preparation method thereof

A technology of methyl hydroxyvalerate and hydroxyvaleric acid is applied in the field of organic compound synthesis and application, which can solve the problems of high odor, low VOC content and high VOC content of water-based industrial paint for steel structures, and achieves low production cost and simplified production. The effect of high process and reaction rate

Active Publication Date: 2022-05-03
RUNTAI CHEM TAIXING CO LTD +1
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  • Claims
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Problems solved by technology

[0002] Steel is an important structural material in modern buildings. Many large-scale convention and exhibition centers, stadiums, airport terminals, and TV towers have adopted steel structures as the main structural form. Steel structures are mainly used in the coating design of steel structure buildings. Anticorrosion with water-based industrial paints; however, the coalescents used in the existing water-based industrial paints for steel structures are mainly dodecyl alcohol esters (2,2,4-trimethyl-1,3-pentanediol-monoiso Butyrate) and benzyl alcohol, ethylene glycol butyl ether composition, wherein dodecyl alcohol ester mainly plays a film-forming role, and benzyl alcohol and ethylene glycol butyl ether mainly play the role of helping volatilization, which is mainly due to ten The volatilization rate of dicarbonyl alcohol ester is relatively slow, and benzyl alcohol and butyl glycol ether need to be used to increase the volatilization rate. However, due to the relatively strong smell of benzyl alcohol and butyl glycol ether, the film-forming efficiency is low, which leads to the steel structure Water-based industrial paint has a relatively strong smell and high VOC content. Therefore, it is necessary to develop a film-forming aid with low VOC content, high film-forming efficiency and fast volatilization speed. At the same time, it is necessary to develop a steel film-forming aid containing this film-forming aid Structural water-based industrial paint

Method used

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  • Preparation method of 2,2,4-trimethyl-3-hydroxyvaleric acid methyl ester, steel structure water-based industrial paint and preparation method thereof
  • Preparation method of 2,2,4-trimethyl-3-hydroxyvaleric acid methyl ester, steel structure water-based industrial paint and preparation method thereof
  • Preparation method of 2,2,4-trimethyl-3-hydroxyvaleric acid methyl ester, steel structure water-based industrial paint and preparation method thereof

Examples

Experimental program
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preparation example Construction

[0031] A preparation method of 2,2,4-trimethyl-3 hydroxyvaleric acid methyl ester, comprising 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 2Oxidation reaction occurs to obtain 2,2,4-trimethyl-3 hydroxypentanoic acid, the reaction formula is as follows:

[0036]

[0037] 2) Preparation of 2,2,4-trimethyl-3-hydroxypentanoic acid methyl ester

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

[0039]

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

Embodiment 1

[0048] The preparation method of the 2,2,4-trimethyl-3 hydroxyvaleric acid methyl ester of the present embodiment comprises the following steps:

[0049] 1) Preparation of 2,2,4-trimethyl-3-hydroxypentanoic acid

[0050] 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.

[0051] 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 th...

Embodiment 2

[0057] The preparation method of the 2,2,4-trimethyl-3 hydroxyvaleric acid methyl ester of the present embodiment comprises the following steps:

[0058] 1) Preparation of 2,2,4-trimethyl-3-hydroxypentanoic acid

[0059] 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.

[0060] 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 synthesis and application of organic compounds, in particular to a preparation method of methyl 2,2,4-trimethyl-3-hydroxyvalerate, a water-based industrial paint for steel structures and a preparation method thereof. The preparation method of 2,2,4-trimethyl-3 hydroxyvaleric acid methyl ester 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 occurs to obtain 2,2,4-trimethyl-3 hydroxyvaleric acid; 2 ) reacting the 2,2,4-trimethyl-3 hydroxyvaleric acid and methanol prepared in step 1) under the action of a strong acid catalyst to obtain methyl 2,2,4-trimethyl-3 hydroxyvaleric acid. The preparation method of 2,2,4-trimethyl-3 hydroxyvaleric acid methyl ester of the present invention, the reaction product is single, does not need to carry out multi-step separation, and is simple to operate, and the present invention also provides a kind of containing above-mentioned 2,2, A water-based industrial paint for steel structures of 4-trimethyl-3-hydroxyvaleric acid methyl ester and a preparation method thereof.

Description

technical field [0001] The invention relates to the technical field of synthesis and application of organic compounds, in particular to a method for preparing 2,2,4-trimethyl-3-hydroxypentanoic acid methyl ester, a A water-based industrial paint for steel structures based on methyl ester and a preparation method thereof. Background technique [0002] Steel is an important structural material in modern buildings. Many large-scale convention and exhibition centers, stadiums, airport terminals, and TV towers have adopted steel structures as the main structural form. Steel structures are mainly used in the coating design of steel structure buildings. Anticorrosion with water-based industrial paints; however, the coalescents used in the existing water-based industrial paints for steel structures are mainly dodecyl alcohol esters (2,2,4-trimethyl-1,3-pentanediol-monoiso Butyrate) and benzyl alcohol, ethylene glycol butyl ether composition, wherein dodecyl alcohol ester mainly pla...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C67/08C07C69/675C09D133/04C09D5/08C09D5/02C09D7/63
CPCC07C67/08C07C51/285C07C45/72C09D133/04C09D5/08C09D5/024C07C69/675C07C59/01C07C47/19C08K13/02C08K5/101
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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