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A kind of preparation method of fluorine-containing cyanate ester resin

A technology of fluorine-containing cyanate and resin, which is applied in the field of preparation of fluorine-containing cyanate resin, can solve the problems of reducing polymer rigidity, reducing rigidity, and large steric hindrance, so as to improve high temperature resistance and flame retardancy, improve Flexibility, the effect of improving toughness

Active Publication Date: 2020-04-21
YANGZHOU TECHIA MATERIAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The object of the present invention is to provide a kind of preparation method of fluorine-containing cyanate resin, the prepared fluorine-containing cyanate resin contains a plurality of cyanate groups, has more action sites, and a plurality of cyanate The groups are distributed in different directions, and the steric hindrance of a single monomer resin molecule is relatively large, which limits the formation of triazine rings during the curing process, thereby greatly improving the toughness of the resin, and the cyanate groups in different directions can be simultaneously Reaction in multiple directions, hyperbranched structure can be formed in different directions during the polymerization process, further reducing the rigidity of the polymer, and the hyperbranched structure forms a huge network structure, so that a large amount of fluorine and silicon are evenly distributed in the network structure Elements, because the introduction of a large number of Si-O bonds improves the flexibility of the polymer and further reduces its rigidity, so that the prepared resin monomer has higher toughness compared with bisphenol A cyanate resin, And compared with the resin modified by miscibility with rubber elastomer, its thermal property is higher, and then solves the problem that the existing bisphenol A cyanate resin is a straight chain structure, resulting in greater rigidity of the prepared resin after curing , the toughness is low, and when the existing bisphenol A type cyanate resin is modified, it is directly mixed with the rubber elastomer for modification, but the flame retardancy and thermal stability of the modified cyanate resin are both Reducing, and adding reinforcement additives during the melting process, because it is difficult to achieve complete blending of the reinforcement additives and the two, resulting in the problem of uneven thermal stability, flame retardancy and toughness of the modified resin

Method used

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  • A kind of preparation method of fluorine-containing cyanate ester resin
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  • A kind of preparation method of fluorine-containing cyanate ester resin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Add 350g of methyl acrylate to 1L of 50% hydrochloric acid solution, stir and react for 5-6h, add the resulting product to chloroform for extraction, and then perform vacuum distillation to obtain methyl chloroacrylate with a yield of 91.3% .

[0029] Add 143g of 4-chloroanisole and ether solution into the reflux reaction vessel, then slowly add magnesium chips immersed in ether to it, and add 25g of magnesium chips based on the mass of the magnesium chips. During the addition, the solution boils slightly. After the addition is complete, the reaction is maintained until the solution does not boil and the reaction is kept stirring for 20-30 minutes, and then the unreacted magnesium powder is removed after filtration, and the filtrate is distilled under reduced pressure to obtain Grignard reagent with a yield of 87.6%.

Embodiment 2

[0031] A preparation method of fluorocyanate ester resin, the specific preparation process is as follows:

[0032] The first step: Weigh a certain amount of p-methoxyacetophenone and dissolve it in ethanol to obtain a 65% p-methoxyacetophenone solution, and add 1L of p-methoxyacetophenone solution to the reactor After stirring and mixing uniformly, the temperature is raised to 60-70°C, and then 100g sodium ethoxide and 510g methyl chloroacrylate prepared in Example 1 are added to the reaction vessel, reacted at a constant temperature for 15-18h, and then subjected to vacuum distillation to obtain biscarbonyl Unsaturated monomer

[0033] In the second step, add 1 kg of the dicarbonyl unsaturated monomer prepared in the first step to the dimethyl sulfoxide solution, stir to dissolve and add 0.705 kg of the Grignard reagent prepared in Example 1 to it, and stir to react at room temperature. 5- 6h, then carry out vacuum distillation to obtain unsaturated alkenyl trimethoxyphenyl ether...

Embodiment 3

[0039] A preparation method of fluorocyanate ester resin, the specific preparation process is as follows:

[0040] The first step: Weigh a certain amount of p-methoxyacetophenone and dissolve it in ethanol to obtain a 65% p-methoxyacetophenone solution, and add 1L of p-methoxyacetophenone solution to the reactor After stirring and mixing uniformly, the temperature is raised to 60-70°C, and then 100g sodium ethoxide and 510g methyl chloroacrylate prepared in Example 1 are added to the reaction vessel, reacted at a constant temperature for 15-18h, and then subjected to vacuum distillation to obtain biscarbonyl Unsaturated monomer

[0041] In the second step, add 1 kg of the dicarbonyl unsaturated monomer prepared in the first step to the dimethyl sulfoxide solution, stir to dissolve and add 0.705 kg of the Grignard reagent prepared in Example 1 to it, and stir to react at room temperature. 5- 6h, then carry out vacuum distillation to obtain unsaturated alkenyl trimethoxyphenyl ether...

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Abstract

The invention discloses a production method of fluorine-containing cyanate ester resin. A specific production process comprises the following steps of firstly, producing a dicarbonyl unsaturated monomer, then making the dicarbonyl unsaturated monomer reacted with a Grignard reagent to produce unsaturated alkylene trimethoxy phenyl ether, then introducing silicon and fluorine onto a monomer, and conducting cross-linking by means of boric acid to produce the fluorine-containing cyanate ester resin. The fluorine-containing cyanate ester resin produced through the method contains multiple cyanateester groups, and has multiple acting sites, moreover, the multiple cyanate ester groups are distributed in different directions, the steric hindrance of a single monomer resin molecule is large, generation of a triazine ring in a curing process is limited, thus the tenacity of the resin is greatly improved, moreover, the cyanate ester groups in the different directions can be reacted at the sametime in the multiple directions, in a polymerization process, hyperbranched structures can be formed in the different directions, and the rigidity of a polymer is further reduced, so that compared with bisphenol A cyanate ester resin, a produced resin monomer has high tenacity.

Description

Technical field [0001] The invention belongs to the field of cyanate ester resin preparation, and relates to a preparation method of fluorine-containing cyanate ester resin. Background technique [0002] Bisphenol A cyanate ester resin possesses the equivalent modulus and mechanical strength of bisphenol A epoxy resin, and has excellent dielectric properties. It also modifies the bisphenol A matrix and introduces a large amount of fluorine on the matrix. , Prepared into bis(phenylcyanate) hexafluoropropane, the resin has high flame retardancy due to the effect of fluorine element, but the bisphenol A cyanate ester resin has a linear structure, resulting in the rigidity of the prepared resin after curing Larger, lower toughness. [0003] In the curing process of the existing cyanate ester resin, the trimerization reaction forms a triazine ring structure, which makes the cured product more rigid, brittle texture, and poorer toughness. In order to improve the toughness of the cyanate...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G73/06
CPCC08G73/0644C08G73/065
Inventor 范春晖金中宝王跃彪季静静
Owner YANGZHOU TECHIA MATERIAL CO LTD
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