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A kind of cyanate ester resin and its preparation method, composite material

A cyanate ester resin and cyanate esterification technology, applied in the field of cyanate resin, can solve the problems of low glass transition temperature, large dielectric loss, poor thermal performance, etc., and achieve high glass transition temperature and thermal weight loss Effects of improved temperature, processability and heat resistance, and excellent dielectric properties

Active Publication Date: 2020-05-19
CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] However, although cyanate ester resins such as bisphenol A type, bisphenol F type, and bisphenol E type have excellent dielectric properties, their thermal properties are poor, and the glass transition temperature is low, and none of them exceeds 300. ℃, which limits its application to some extent
[0004] The U.S. began to study the phenolic cyanate ester in the 1980s, and Japan also disclosed the preparation method of the phenolic cyanate resin in the 1980s (the patent No. is JP592149918 and JP58234822), and the phenolic cyanate resin It has the advantages of high heat resistance, flame retardancy, and high carbon residue rate of phenolic resin, but phenolic cyanate resin itself has many disadvantages, such as high melting point and high melt viscosity, and it needs to be prepared by adding a solvent Prepregs have a high curing temperature and poor manufacturability; at the same time, the dielectric constant of the phenolic cyanate cured product is high, and the dielectric loss is too large, which affects its application

Method used

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  • A kind of cyanate ester resin and its preparation method, composite material
  • A kind of cyanate ester resin and its preparation method, composite material
  • A kind of cyanate ester resin and its preparation method, composite material

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preparation example Construction

[0055] The invention provides a kind of preparation method of cyanate ester resin, comprises the following steps:

[0056] A) Cyanate ester resin obtained by subjecting trifluoromethyl-containing bisphenol to cyanate esterification reaction.

[0057] In the present invention, the selection and composition of raw materials and products in the preparation method of the above-mentioned cyanate resin, and the corresponding optimization principles, can correspond to the selection and composition of the corresponding structure in the aforementioned cyanate resin, and the corresponding optimization principles. , which will not be repeated here.

[0058] The present invention has no particular limitation on the specific selection of the trifluoromethyl-containing bisphenol, and the structure of the trifluoromethyl-containing bisphenol well known to those skilled in the art will suffice. The specific requirements, performance requirements or specific properties of the composite materi...

Embodiment 1

[0092] Slowly dissolve 3.2023 grams of 2,2'-bis(trifluoromethyl)-4,4'-diaminobiphenyl in 5ml of concentrated sulfuric acid, stir until clear and transparent, and dissolve 170g NaNO 2 Add it to concentrated sulfuric acid at low temperature (0-5°C), then stir and mix the two, place the mixture in a low-temperature tank, control the temperature at -5°C, stir for 10 minutes, and let stand for 2 hours.

[0093] Then the mixed solution was slowly added to a three-necked flask for hydrolysis, heated to reflux for 3 hours, cooled to room temperature naturally, a solid mixture was precipitated, the supernatant was removed, and the solid mixture was washed three times with water; then 0.2L CHCl3 was added, heated to reflux until completely dissolved, Then add 5g of anhydrous MgSO4 to remove water, let it stand for 2h. The mixture was filtered and rotary evaporated, and the product was filtered again and dried to obtain 2,2'-bis(trifluoromethyl)-4,4'-dihydroxybiphenyl.

[0094] Then it ...

Embodiment 2

[0107] Slowly dissolve 3.3426 grams of 2,2'-bis(trifluoromethyl)-4,4'-diaminodiphenyl ether in 5ml of concentrated sulfuric acid, stir until clear and transparent, and dissolve 170g of NaNO 2 Add it into concentrated sulfuric acid at low temperature (0-5°C), then stir and mix the two, place the mixture in a low-temperature tank, control the temperature at -5°C, stir for 10 minutes, and let stand for 2 hours.

[0108] Then the mixed solution was slowly added to a three-necked flask for hydrolysis, heated to reflux for 3h, cooled to room temperature naturally, a solid mixture was precipitated, the supernatant was removed, and the solid mixture was washed three times with water; then 0.2L CHCl was added 3 , heated to reflux until completely dissolved, then added 5 g of anhydrous MgSO 4 Remove moisture and let stand for 2h. The mixture was filtered and rotary evaporated, and the product was filtered again and dried to obtain 2,2'-bis(trifluoromethyl)-4,4'-dihydroxydiphenyl ether....

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Abstract

The present invention provides a kind of cyanate resin, and described cyanate resin has the structure shown in formula (I): NCO-R-OCN (I). The invention provides a new type of cyanate resin, which is obtained by cyanate esterification of trifluoromethyl-containing bisphenols. Because the cyanate resin contains trifluoromethyl groups, the new type of cyanate The cured ester resin has excellent dielectric properties. Because the structure also contains rigid structures such as benzene rings and biphenyl rings, the new cured cyanate resin has a high glass transition temperature and thermal weight loss temperature. The melting point of the resin is below 150°C, and the manufacturability and heat resistance are greatly improved. The results show that the cured product of the novel cyanate resin provided by the present invention has good mechanical properties, dielectric properties and thermal properties, its compressive strength can reach more than 190 MPa, the 5% thermal weight loss temperature can reach 440 ° C, and the glass transition The temperature can reach above 350°C.

Description

technical field [0001] The invention belongs to the technical field of cyanate resin and relates to a cyanate resin and a preparation method thereof, in particular to a novel cyanate resin and a preparation method thereof, a cyanate resin cured product and a composite material. Background technique [0002] Cyanate resin, also known as triazine A resin, is a thermosetting resin containing two or more cyanate resin functional groups in its molecular structure. The English name is Triazine A resin, TA resin or Cyanate resin, abbreviated as CE. There are many types of cyanate ester resins, and different structures have different properties, but after curing, they form a network polymer with a triazine ring structure, so they have common characteristics and are widely used in multi-layer printing. Circuit boards, high-speed substrates for optoelectronic devices, radomes, high-gain antennas, stealth aircraft, and structural composite materials. Especially in the aerospace indust...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G73/06C08L79/04C08K7/14C08K7/10C08K7/06
CPCC08G73/0644C08G73/065C08K7/06C08K7/10C08K7/14C08L2201/08C08L79/04
Inventor 刘敬峰阎敬灵王震崔磊
Owner CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI