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Preparation method of 2,2,4-trimethyl-3-hydroxyvalerate methoxyethyl ester, water-based wood paint and preparation method thereof

A technology of methoxyethyl hydroxyvalerate and hydroxyvaleric acid is applied in the field of preparation of water-based wood lacquer, and can solve the problem that dodecyl alcohol ester is easy to have residue, dodecyl alcohol ester is not volatile, and wood products cannot overlap. and other problems, to achieve the effects of no by-products, high reaction rate and complete esterification

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 film-forming aid of existing waterborne woodware paint generally adopts the mixture of DPM (dipropylene glycol methyl ether) and DPNB (dipropylene glycol butyl ether), and DPM mainly plays the effect of helping volatilization, accelerates volatilization speed, and DPNB plays the effect of helping film formation, However, the film-forming efficiency of existing water-based wood paints is relatively low, and water-based wood paints use dodecyl alcohol ester (2,2,4-trimethyl-1,3-pentanediol-monoisobutyrate) as the forming material. Membrane additives have the problems that dodecyl alcohol ester is not easy to volatilize, dodecyl alcohol ester is easy to have residue, and the water-based wood paint is easy to stick back, so that wood products cannot be overlapped. Therefore, it is necessary to develop a kind of water-based wood paint. Film efficiency, at the same time the volatilization speed is fast, and the anti-adhesion effect is good. At the same time, it is necessary to develop a water-based wood paint containing this film-forming agent

Method used

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  • Preparation method of 2,2,4-trimethyl-3-hydroxyvalerate methoxyethyl ester, water-based wood paint and preparation method thereof
  • Preparation method of 2,2,4-trimethyl-3-hydroxyvalerate methoxyethyl ester, water-based wood paint and preparation method thereof
  • Preparation method of 2,2,4-trimethyl-3-hydroxyvalerate methoxyethyl ester, water-based wood paint and preparation method thereof

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Experimental program
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preparation example Construction

[0029] A preparation method of 2,2,4-trimethyl-3 hydroxyvaleric acid methoxyethyl ester, comprising the following steps:

[0030] 1) Preparation of 2,2,4-trimethyl-3-hydroxypentanoic acid

[0031] 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:

[0032]

[0033] 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:

[0034]

[0035] 2) Preparation of 2,2,4-trimethyl-3-hydroxypentanoic acid methoxyethyl ester

[0036] Reaction of 2,2,4-trimethyl-3 hydroxyvaleric acid and ethylene glycol methyl ether prepared in step 1) under the action of a strong acid catalyst to obtain 2,2,4-trimethyl-3 hydroxyvaleric acid methoxy Ethyl ester, the reaction formula is as follows:

[0037]

[0038] In the step 1), the basi...

Embodiment 1

[0044] The preparation method of the 2,2,4-trimethyl-3 hydroxypentanoic acid methoxyethyl ester of the present embodiment comprises the following steps:

[0045] 1) Preparation of 2,2,4-trimethyl-3-hydroxypentanoic acid

[0046] 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.

[0047] 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 fracti...

Embodiment 2

[0053] The preparation method of the 2,2,4-trimethyl-3 hydroxypentanoic acid methoxyethyl ester of the present embodiment comprises the following steps:

[0054] 1) Preparation of 2,2,4-trimethyl-3-hydroxypentanoic acid

[0055] 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.

[0056] 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 T...

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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 methoxyethyl 2,2,4-trimethyl-3-hydroxyvalerate, a water-based wood varnish and a preparation method thereof. The preparation method of 2,2,4-trimethyl-3 hydroxyvaleric acid methoxyethyl 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 above obtained 2,2,4-trimethyl-3-hydroxypentanal with H 2 o 2 Oxidation reaction occurs to obtain 2,2,4-trimethyl-3 hydroxyvaleric acid; 2) 2,2,4-trimethyl-3 hydroxyvaleric acid and ethylene glycol methyl ether prepared in step 1) in strong acid The reaction under the action of a catalyst gives 2,2,4-trimethyl-3 hydroxyvaleric acid methoxyethyl ester. The preparation method of 2,2,4-trimethyl-3 hydroxyvaleric acid methoxyethyl ester of the present invention has a single reaction product, does not need to be separated in multiple steps, and is simple to operate. At the same time, the present invention also provides a water-based woodenware Lacquer and its preparation method.

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 methoxyethyl ester and a compound containing 2,2,4-trimethyl-3-hydroxypentanoate The preparation method of the waterborne wood lacquer of methoxyethyl 3 hydroxyvalerate. Background technique [0002] Water-based wood paint is a special paint with water as the dispersion medium. Since it does not contain harmful substances such as benzene, xylene, and free TDI (toluene diisocyanate), it is an environmentally friendly, less volatile, non-flammable and non-explosive paint. Favored by consumers. The film-forming aid of existing waterborne woodware paint generally adopts the mixture of DPM (dipropylene glycol methyl ether) and DPNB (dipropylene glycol butyl ether), and DPM mainly plays the effect of helping volatilization, accelerates volatilization speed, and DPNB plays the effect o...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C67/08C07C69/675C09D7/63C09D175/04
CPCC07C45/72C07C51/285C07C67/08C09D7/63C09D175/04C08L2205/03C08L2205/025C08L23/06C08K13/02C08K5/101C07C47/19C07C59/01C07C69/675
Inventor 卢小松张世元姜明秋王永成张润赟
Owner RUNTAI CHEM TAIXING CO LTD