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Production method of fluorine-containing cyanate ester resin

A fluorocyanate-containing resin technology is applied in the field of preparation of fluorocyanate-containing resins, which can solve the problems of lowering polymer rigidity, lowering rigidity, lowering flame retardant performance and thermal stability performance, etc., and improving high temperature resistance. The effect of improving flammability, improving flexibility and reducing rigidity

Active Publication Date: 2019-08-30
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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  • Production method of fluorine-containing cyanate ester resin
  • Production method of fluorine-containing cyanate ester resin
  • Production method of fluorine-containing cyanate ester resin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Add 350 g of methyl acrylate to 1 L of 50% hydrochloric acid solution, stir for 5-6 hours, add the obtained product to chloroform for extraction, and then carry out 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 soaked in ether therein, wherein the amount added is based on the mass of magnesium chips and 25g magnesium chips are added, and the solution boils slightly during the addition process. After the addition is complete, react until the solution does not boil, then keep stirring for 20-30 minutes, then filter to remove the unreacted magnesium powder, and carry out vacuum distillation on the filtrate to obtain the Grignard reagent with a yield of 87.6%.

Embodiment 2

[0031] A kind of preparation method of fluorine-containing cyanate ester resin, concrete preparation process is as follows:

[0032] The first step: Weigh a certain amount of p-methoxyacetophenone and dissolve it in ethanol to obtain a p-methoxyacetophenone solution with a concentration of 65%, and add 1L of p-methoxyacetophenone solution to the reaction kettle , stir and mix evenly, heat up to 60-70°C, then add 100g of sodium ethoxide and 510g of methyl chloroacrylate prepared in Example 1 into the reaction vessel, react at constant temperature for 15-18h, and then carry out vacuum distillation to obtain biscarbonyl unsaturated monomers;

[0033] In the second step, 1 kg of the dicarbonyl unsaturated monomer prepared in the first step is added in the dimethyl sulfoxide solution, and after stirring and dissolving, 0.705 kg of the Grignard reagent prepared in Example 1 is added thereto, and the stirring reaction at normal temperature is 5- 6h, then carry out vacuum distillatio...

Embodiment 3

[0039] A kind of preparation method of fluorine-containing cyanate ester resin, concrete preparation process is as follows:

[0040] The first step: Weigh a certain amount of p-methoxyacetophenone and dissolve it in ethanol to obtain a p-methoxyacetophenone solution with a concentration of 65%, and add 1L of p-methoxyacetophenone solution to the reaction kettle , stir and mix evenly, heat up to 60-70°C, then add 100g of sodium ethoxide and 510g of methyl chloroacrylate prepared in Example 1 into the reaction vessel, react at constant temperature for 15-18h, and then carry out vacuum distillation to obtain biscarbonyl unsaturated monomers;

[0041] In the second step, 1 kg of the dicarbonyl unsaturated monomer prepared in the first step is added in the dimethyl sulfoxide solution, and after stirring and dissolving, 0.705 kg of the Grignard reagent prepared in Example 1 is added thereto, and the stirring reaction at normal temperature is 5- 6h, then carry out vacuum distillatio...

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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 resin preparation and relates to a preparation method of fluorine-containing cyanate resin. Background technique [0002] Bisphenol A cyanate resin has the equivalent modulus and mechanical strength of bisphenol A epoxy resin, and has excellent dielectric properties, and through the modification of the bisphenol A matrix, a large amount of fluorine is introduced into the matrix , prepared into bis(phenyl cyanate) hexafluoropropane, the resin has high flame retardancy due to the effect of fluorine element, but the bisphenol A cyanate resin is a linear structure, resulting in the rigidity of the prepared resin after curing Larger and less resilient. [0003] In the curing process of the existing cyanate resin, the trimerization ring formation reaction forms a triazine ring structure, which makes the cured product stronger in rigidity, brittle in texture and poor in toughness. In order to improve the toughnes...

Claims

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Application Information

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Patent Type & Authority Applications(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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