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Method for preparing myrcenyl vinyl ester resin monomer

A technology of alkenyl vinyl ester and resin monomer, which is applied in the field of preparation of unsaturated resin monomer, can solve the problems of high content of toxic components, poor weather resistance, etc., and achieves good product stability, strong corrosion resistance, and synthetic process Environmentally friendly effect

Inactive Publication Date: 2014-10-08
INST OF CHEM IND OF FOREST PROD CHINESE ACAD OF FORESTRY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] Technical problem to be solved: In order to improve the shortcomings of traditional vinyl ester resins such as high content of toxic components and poor weather resistance, the present invention provides a bio-based myrcene Preparation method of vinyl ester resin monomer

Method used

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  • Method for preparing myrcenyl vinyl ester resin monomer
  • Method for preparing myrcenyl vinyl ester resin monomer

Examples

Experimental program
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Effect test

Embodiment 1

[0030] (1) Add maleic anhydride to a four-neck bottle, raise the temperature to 50°C to dissolve it completely, add dropwise myrcene with a molar ratio of 1.1:1 to maleic anhydride, and keep the temperature at 50~60°C during the dropping process ℃. After the dropwise addition, react at 70° C. for 5 h to obtain myrcene maleic anhydride.

[0031] (2) Put equimolar water and acid anhydride into the reactor, and add epichlorohydrin whose mole number is 10 times the number of acid anhydride moles, and stir at 100°C for two hours to fully hydrolyze the acid anhydride group. Then add benzyltriethylammonium chloride accounting for 1 wt% of the total mass of the reactants, and react at 100°C for 2h.

[0032] (3) Cool down to 60°C, add sodium hydroxide and calcium oxide with an equal molar number of carboxyl groups, and stir at 60°C for 3 hours. Spread filter paper and diatomaceous earth, and filter under reduced pressure at a vacuum degree of 0.1Mpa to obtain a filtrate. Rotary evap...

Embodiment 2

[0036] (1) Add acrylic acid to a four-necked bottle, raise the temperature to 50°C, add myrcene with a molar ratio of 1:1 to acrylic acid dropwise, and keep the temperature at 50-60°C during the dropwise addition. After the dropwise addition, react at 60° C. for 5 h to obtain myrcenyl acrylic acid.

[0037] (2) Add epichlorohydrin whose molar number is 10 times that of carboxylic acid, tetramethylammonium chloride accounting for 1 wt% of the total mass of reactants, and react at 100°C for 2 hours.

[0038] (3) Cool down to 60°C, add sodium hydroxide and calcium oxide with an equal molar number of carboxyl groups, and stir at 60°C for 3 hours. Spread filter paper and diatomaceous earth, and filter under reduced pressure at a vacuum degree of 0.1Mpa to obtain a filtrate. Rotary evaporation removes excess epichlorohydrin to obtain a myrcene-based epoxy resin intermediate.

[0039] (4) Add the myrcene-based epoxy resin intermediate and N,N-dimethylbenzylamine and 0.1wt% of the p...

Embodiment 3

[0042] (1) Add methacrylic acid to a four-neck flask, raise the temperature to 50°C, add myrcene with a molar ratio of 1.2:1 to methacrylic acid dropwise, and maintain the temperature at 50-60°C during the dropwise addition. After the dropwise addition, react at 70° C. for 5 h to obtain myrcenyl methacrylic acid.

[0043] (2) Add epichlorohydrin whose mole number is 10 times that of carboxylic acid, tetramethylammonium bromide accounting for 2.0 wt% of the total mass of reactants, and react at 100°C for 2 hours.

[0044] (3) Cool down to 60°C, add sodium hydroxide ion and calcium oxide having an equal molar number to the carboxyl group, and stir at 60°C for 3 hours. Spread filter paper and diatomaceous earth, and filter under reduced pressure at a vacuum degree of 0.1Mpa to obtain a filtrate. Rotary evaporation removes excess epichlorohydrin to obtain a myrcene-based epoxy resin intermediate.

[0045](4) Add the myrcene-based epoxy resin intermediate and N,N-dimethylbenzylam...

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Abstract

The invention discloses a method for preparing a myrcenyl vinyl ester resin monomer. The method comprises the following steps: adding unsaturated carboxylic acid or anhydride into a reactor, and dripping myrcene; reacting after dripping is ended, and thus obtaining myrcenyl carboxylic acid or myrcenyl anhydride; adding myrcenyl anhydride and water in an equal molar ratio into the reactor, adding epoxy chloropropane, and stirring, so that the anhydride group is fully hydrolyzed; adding a catalyst A for reacting, or adding the myrcenyl carboxylate or epoxy chloropropane into the reactor, and adding the catalyst A for reacting; reducing the temperature and adding sodium hydroxide and calcium oxide; spreading filter paper and diatomite, and performing reduced pressure suction filtration to obtain filtrate; performing rotary evaporation to remove excessive epoxy chloropropane, and thus obtaining a myrcenyl epoxy resin intermediate; adding the myrcenyl epoxy resin intermediate, a catalyst B and a polymerization inhibitor into the reactor, raising the temperature, dripping acrylic acid into the reactor, reacting after dripping is ended, and thus obtaining the myrcenyl vinyl ester resin monomer. The prepared vinyl ester resin is high in strength, high in corrosion resistance and high in weather resistance.

Description

[0001] technical field [0002] The invention relates to a preparation method of an unsaturated resin monomer, in particular to a preparation method of a myrcenyl vinyl ester resin monomer. [0003] Background technique [0004] Vinyl ester resin is a new type of resin developed in the 1960s. It is a kind of unsaturated polyester resin, such as acrylic resin, acrylic epoxy resin and vinyl ester. The basic vinyl ester resin with the largest amount is bisphenol A epoxy acrylate synthesized by ring-opening addition of bisphenol A epoxy resin and carboxyl-containing vinyl monomer. After the solid or semi-solid bisphenol A epoxy acrylate is diluted with about 40% styrene, the free radical copolymerization reaction of styrene and bisphenol A epoxy acrylate is initiated by the initiator, and the resin can be cured rapidly at room temperature. Linked into a network-shaped polymer material, its curing mechanism is similar to that of unsaturated polyester resin, and its chemical str...

Claims

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Application Information

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IPC IPC(8): C07C69/75C07C67/24
CPCC07C51/353C07C67/11C07C67/24C07C2601/16C07D317/46C07C69/75C07C62/30
Inventor 夏建陵杨雪娟李守海宋健黄坤李梅杨小华张燕
Owner INST OF CHEM IND OF FOREST PROD CHINESE ACAD OF FORESTRY
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