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Flame-retardant vinyl ester resin, flame-retardant vinyl ester resin condensate and preparation method of flame-retardant vinyl ester resin condensate

A technology for flame retardant vinyl ester and vinyl ester resin, applied in the direction of organic chemistry, etc., can solve the problems of releasing a large amount, not completely improving the flame retardant performance of vinyl ester resin, and limited increase in oxygen index.

Active Publication Date: 2022-04-26
BEIJING INSTITUTE OF TECHNOLOGYGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Industrialized vinyl ester resin has excellent properties such as good fluidity, formability, chemical corrosion resistance and low curing temperature, but its oxygen index is low, and it will release a lot of smoke and heat when burning. limits its wide application
[0004] At present, the method to improve the flame retardancy of vinyl ester resin is mainly to add phosphorus-nitrogen flame retardants and silicon-containing flame retardants. However, the addition of flame retardants does not completely improve the flame retardancy of vinyl ester resins. It may also cause secondary pollution to the environment
For example: phosphorus-nitrogen flame retardants have a significant effect on improving the oxygen index of vinyl ester resins, but they increase the smoke release of the resin while improving the flame retardancy of the resin, which is likely to cause secondary pollution; while silicon-containing flame retardants It can significantly reduce the heat release and smoke release of vinyl ester resins, but it has a limited increase in the oxygen index, and cannot fully solve the problems existing in the burning of vinyl ester resins.
[0005] Moreover, in the prior art, there is little research on directly changing the structure of vinyl ester resin monomers to realize the intrinsic flame retardancy of vinyl resins.

Method used

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  • Flame-retardant vinyl ester resin, flame-retardant vinyl ester resin condensate and preparation method of flame-retardant vinyl ester resin condensate
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  • Flame-retardant vinyl ester resin, flame-retardant vinyl ester resin condensate and preparation method of flame-retardant vinyl ester resin condensate

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preparation example Construction

[0039] The present invention also provides a preparation method for the flame retardant vinyl ester resin monomer described in the above technical solution, comprising the following steps:

[0040] Mixing magnolol, vinyl acid chloride reactants, acid-binding agent and organic solvent, performing the first substitution reaction, then raising the temperature to perform the second substitution reaction, to obtain the flame retardant vinyl ester resin monomer;

[0041] The vinyl acid chloride reactants include acryloyl chloride or methacryloyl chloride.

[0042] In the present invention, unless otherwise specified, the raw materials used in the present invention are preferably commercially available products.

[0043] In the present invention, when the magnolol is reacted with vinyl acid chloride reactants, the obtained flame retardant vinyl ester resin monomer has the structure shown in formula I.

[0044] In the present invention, the acid-binding agent preferably includes one ...

Embodiment 1

[0090] (1) Dissolve 12 g of magnolol and 10 g of triethylamine in 100 mL of dichloromethane to obtain a magnolol solution.

[0091] (2) Disperse 10 g of methacryloyl chloride in 20 mL of dichloromethane to obtain a methacryloyl chloride solution.

[0092] (3) Under a nitrogen protective atmosphere, add the methacryloyl chloride solution dropwise to the magnolol solution at 2°C, and the dropping time is controlled at about 30 minutes. After the addition is completed, react at 2°C for 30 minutes, and then heat up to 30°C, react for 10h.

[0093] (4) Suction filtration is carried out to above-mentioned gained reaction solution, after removing the triethylamine hydrochloride that reaction produces, wash 1 time with the NaOH solution of 50mL 5wt%; Wash 3 times with 50mL deionized water respectively, then, add 15g of Anhydrous magnesium sulfate was used to dry the washed reaction solution.

[0094] (5) The dried reaction solution was vacuum rotary evaporated under the conditions o...

Embodiment 2

[0098] (1) Dissolve 12 g of magnolol and 10 g of triethylamine in 90 mL of chloroform to obtain a magnolol solution.

[0099] (2) Dissolve 8.5 g of acryloyl chloride in 10 mL of chloroform to obtain an acryloyl chloride solution.

[0100] (3) Under a nitrogen protective atmosphere, add the acryloyl chloride solution dropwise to the magnolol solution at 5°C, and the dropping time is controlled at about 15 minutes. After the addition is completed, react at 5°C for 30 minutes, and then heat up to 30 ℃ reaction 10h.

[0101] (4) Suction filter the reaction solution obtained above, remove the triethylamine hydrochloride produced by the reaction, wash once with 50mL 3wt% NaOH solution, then wash three times with 50mL deionized water, then add 20g anhydrous magnesium sulfate to dry the washed reaction solution.

[0102] (4) The dried reaction solution was vacuum rotary evaporated under the conditions of vacuum degree -0.06MPa, temperature 35°C, and 80r / min to obtain 13.4g of flame ...

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Abstract

The invention belongs to the technical field of flame-retardant materials, and particularly relates to flame-retardant vinyl ester resin, a flame-retardant vinyl ester resin condensate and a preparation method of the flame-retardant vinyl ester resin condensate. The flame-retardant vinyl ester resin comprises the following components in parts by weight: 65-80 parts of a flame-retardant vinyl ester resin monomer and 19-35 parts of a diluent, the diluent is prepared from one or more of styrene, alpha-methyl styrene and divinyl benzene; the flame-retardant vinyl ester resin monomer has a structure as shown in a formula I. The flame-retardant vinyl ester resin provided by the invention has the advantages of excellent intrinsic flame retardance, low heat release and low smoke release.

Description

[0001] The application date is April 19, 2021, the application number is 202110417229.5, and the title of the invention is "A Flame Retardant Vinyl Ester Resin Monomer and Its Preparation, Flame Retardant Vinyl Ester Resin, Cured Flame Retardant Vinyl Ester Resin" and preparation of a divisional application. technical field [0002] The invention belongs to the technical field of flame retardant materials, and in particular relates to a flame retardant vinyl ester resin, a cured product of the flame retardant vinyl ester resin and its preparation. Background technique [0003] Industrialized vinyl ester resin has excellent properties such as good fluidity, formability, chemical corrosion resistance and low curing temperature, but its oxygen index is low, and it will release a lot of smoke and heat when burning. limit its wide application. [0004] At present, the method to improve the flame retardancy of vinyl ester resin is mainly to add phosphorus-nitrogen flame retardant...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F222/26C08F212/08
CPCC08F222/102C08F212/08
Inventor 杨荣杰张鑫张文超
Owner BEIJING INSTITUTE OF TECHNOLOGYGY