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Preparation method of fluorine-containing cyanate monomer

A technology of fluorine-containing cyanate and monomer, which is applied in the field of preparation of fluorine-containing cyanate monomer, and can solve problems such as unsatisfactory mechanical properties and poor dielectric properties

Inactive Publication Date: 2019-03-26
THE RES INST FOR SPECIAL STRUCTURES OF AERONAUTICAL COMPOSITE AVIC
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Fluorine-containing modification is a common method to improve the dielectric properties of polymers, but research on fluorine-containing modified CE is relatively rare at home and abroad.
Zhang Danfeng et al. filled the modified CE with polytetrafluoroethylene (PTFE), and the obtained composite material had excellent dielectric properties, but the mechanical properties were not ideal.
Hou Defa used bisphenol AF epoxy resin to modify bisphenol A type cyanate resin to prepare a new type of fluorine-containing cyanate copolymer, although the dielectric constant and loss are compared with bisphenol A type epoxy modified is smaller, but its dielectric properties are still worse than pure bisphenol A cyanate

Method used

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  • Preparation method of fluorine-containing cyanate monomer
  • Preparation method of fluorine-containing cyanate monomer
  • Preparation method of fluorine-containing cyanate monomer

Examples

Experimental program
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Effect test

Embodiment 1

[0021] (1) Put a 3000mL four-necked bottle in an ice-salt bath, add 450mL of acetone and 65g of cyanogen chloride, and stir to completely dissolve the cyanogen chloride.

[0022] (2) Under vigorous stirring, slowly add the solution of 101g triethylamine and 156g bisphenol AF, pay attention to make the drop rate of triethylamine slightly slower than that of bisphenol AF, and control the reaction temperature at -20°C-0 ℃, about 4h after the dropwise addition is complete, and then continue to stir for 3h to stop the reaction.

[0023] (3) Filter after standing for 2 hours to obtain the crude product of bisphenol AF type cyanate resin with a yield of 95%.

[0024] (4) Dissolve the crude product with dichloromethane, filter and distill, wash and filter with 2% sodium hydroxide solution, and wash the obtained product three times with deionized water. Dissolve the resin with dichloromethane, let it stand for a week, and dry the precipitated crystals with magnesium sulfate to obtain ...

Embodiment 2

[0028] (1) Put a 3000mL four-necked bottle in an ice-salt bath, add 450mL of acetone and 116.6 cyanogen bromide, and stir to completely dissolve the cyanogen bromide.

[0029] (2) Under vigorous stirring, slowly drop a solution of 101g triethylamine and 168g bisphenol AF, pay attention to make the drop rate of triethylamine slightly slower than that of bisphenol AF, and control the reaction temperature at -20-0°C , After about 4h, the dropwise addition was completed, and then continued to stir for 3h to stop the reaction.

[0030] (3) Filter after standing for 2 hours to obtain the crude product of bisphenol AF type cyanate resin with a yield of 96%.

[0031] (4) Dissolve the crude product with dichloromethane, filter and distill, wash and filter with 2% sodium hydroxide solution, and wash the obtained product three times with deionized water. Dissolve the resin with dichloromethane, let it stand for a week, and dry the precipitated crystals with magnesium sulfate to obtain a...

Embodiment 3

[0035] (1) Put a 3000ml four-neck flask in an ice-salt bath, add 900mL of acetone and 222.6g of cyanogen bromide, and stir to completely dissolve the cyanogen bromide.

[0036] (2) Under vigorous stirring, slowly add a solution of 202g triethylamine and 336g 1,3-bis[2-(4-hydroxyphenyl)hexafluoroisopropyl]benzene, paying attention to the rate of addition of triethylamine Slightly slower than the drop rate of 1,3-bis[2-(4-hydroxyphenyl)hexafluoroisopropyl]benzene, control the reaction temperature at -20-0°C, complete the drop after about 6 hours, and then continue to stir for 3 hours , stop responding.

[0037] (3) After standing for 2 hours, it was filtered to obtain the crude product of 1,3-bis[2-(4-hydroxyphenyl)hexafluoroisopropyl]benzene-type cyanate resin with a yield of 90%.

[0038] (4) Dissolve the crude product with dichloromethane, filter and distill, wash and filter with 3% sodium hydroxide solution, and wash the obtained product three times with deionized water. D...

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Abstract

The invention belongs to the technical field of synthesis of cyanate type compounds and relates to a preparation method of a fluorine-containing cyanate monomer. The method comprises the following steps: step 1, adding a solvent and cyanogen halide; stirring to completely dissolve the cyanogen halide; step 2, under violent stirring, slowly dropwise adding triethylamine and a solution of a fluorine-containing bisphenol compound, wherein the dropwise adding speed of the triethylamine is slightly smaller than the dropwise adding speed of the fluorine-containing bisphenol compound; controlling thereaction temperature to be -20 to 0 DEG C; finishing dropwise adding after 2 to 10 h; then continually stirring for 1 to 3 h and stopping reaction; step 3, after standing for 1 to 5 h, filtering to obtain a fluorine-containing bisphenol cyanate resin crude product and then purifying. The invention provides the method for synthesizing the fluorine-containing cyanate monomer so that the preparationof the fluorine-containing cyanate monomer becomes possible.

Description

technical field [0001] The invention belongs to the technical field of synthesis of cyanate ester compounds, and relates to a preparation method of fluorine-containing cyanate ester monomers. Background technique [0002] Cyanate ester (CE) is a kind of resin with -OCN functional group at the end group. After being heated, it can be trimerized to form a triazine ring, and cross-linked to form a thermosetting resin. It has excellent heat resistance, dielectric properties, and adhesion. Performance, etc., cyanate resin is a widely used matrix resin for high temperature resistant and wave-transparent composite materials. Fluorine-containing modification is a common method to improve the dielectric properties of polymers, but research on fluorine-containing modified CE is relatively rare at home and abroad. Zhang Danfeng et al. filled the modified CE with polytetrafluoroethylene (PTFE), and the obtained composite material had excellent dielectric properties, but the mechanical ...

Claims

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Application Information

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IPC IPC(8): C07C261/02
CPCC07C261/02
Inventor 张明习周凯运王志强苏韬
Owner THE RES INST FOR SPECIAL STRUCTURES OF AERONAUTICAL COMPOSITE AVIC
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