CN106221215A - Cyanate ester resin composite material preparation method - Google Patents

Cyanate ester resin composite material preparation method Download PDF

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Publication number
CN106221215A
CN106221215A CN201610700498.1A CN201610700498A CN106221215A CN 106221215 A CN106221215 A CN 106221215A CN 201610700498 A CN201610700498 A CN 201610700498A CN 106221215 A CN106221215 A CN 106221215A
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CN
China
Prior art keywords
cyanate ester
ester resin
composite material
resin composite
material preparation
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201610700498.1A
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Chinese (zh)
Inventor
王大伟
寇静
段成金
于雅男
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Weihai Guangwei Composites Co Ltd
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Weihai Guangwei Composites Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
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Publication date
Application filed by Weihai Guangwei Composites Co Ltd filed Critical Weihai Guangwei Composites Co Ltd
Priority to CN201610700498.1A priority Critical patent/CN106221215A/en
Publication of CN106221215A publication Critical patent/CN106221215A/en
Pending legal-status Critical Current

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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L79/00Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen with or without oxygen or carbon only, not provided for in groups C08L61/00 - C08L77/00
    • C08L79/04Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00Specific properties of additives
    • C08K2201/002Physical properties
    • C08K2201/003Additives being defined by their diameter
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00Specific properties of additives
    • C08K2201/011Nanostructured additives
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00Polymer mixtures characterised by other features
    • C08L2205/02Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
    • C08L2205/025Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00Polymer mixtures characterised by other features
    • C08L2205/03Polymer mixtures characterised by other features containing three or more polymers in a blend

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Macromolecular Compounds Obtained By Forming Nitrogen-Containing Linkages In General (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

The present invention relates to polymeric material field, specifically a kind of cyanate ester resin composite material preparation method, it is characterized in that comprising the steps: in parts by mass, by 50~100 parts of cyanate ester resins, 1~100 part of benzoxazine resins, stir at 50~200 DEG C, melt transparent after, add 1~20 part of nano-ceramic powder, 0.1~10 part of thixotropic agent, it is uniformly dispersed, obtains cyanate ester resin composite material.The present invention uses cyanate ester resin and benzoxazine resins, nano-ceramic powder, thixotropic agent, the method that blending and modifying one step completes, production technology is simple, and the cyanate ester resin composite material of gained has good dielectric properties, mechanical property, wearability, hardness performance.

Description

Cyanate ester resin composite material preparation method
Technical field
The present invention relates to a kind of compositions of thermosetting resin field, specifically a kind of cyanate ester resin composite material system Preparation Method.
Background technology
It is known that cyanate ester resin has good mechanical property, dielectric properties, heat resistance etc., it and phenolic aldehyde tree Fat, epoxy resin, bimaleimide resin collectively forms four big high performance matrix of polymeric composites.Because of the dielectricity that it is prominent Can, dielectric constant (2.8-3.2), dielectric loss (0.002-0.008), may be used for structural material, electromagnetic wave transparent material, dielectric function Materials etc., are applied to the field such as Aero-Space, electronic information.But, current cyanate ester resin exists that manufacturability is poor, poor toughness, Working life and the storage phase is short, difference of hardness, the deficiency such as wear no resistance.
Summary of the invention
The purpose of the present invention is contemplated to overcome above-mentioned existing technical deficiency, it is provided that a kind of cyanate ester resin composite material Preparation method, the combination property such as the dielectric properties of composite, mechanical property, wearability, hardness significantly improves.
The present invention solves above-mentioned technical problem and the technical scheme is that a kind of cyanate ester resin composite material preparation side Method, it is characterised in that comprise the steps: in parts by mass, by 50~100 parts of cyanate ester resins, 1~100 part of benzimidazole dihydrochloride tree Fat, stirs at 50~200 DEG C, melt transparent after, adds 1~20 part of nano-ceramic powder, 0.1~10 part of thixotropic agent, dispersion is equal Even, obtain cyanate ester resin composite material.
Described cyanate ester resin is bisphenol A cyanate ester resin, bisphenol E-type cyanate resin, bisphenol-f type cyanate resin A kind of or the mixture of its arbitrary proportion in fat, bis-phenol M type cyanate ester resin, dicyclopentadiene type ethylene rhodanate resin.
Described benzoxazine resins is the one in bisphenol type benzimidazole dihydrochloride, diamine type benzimidazole dihydrochloride or its arbitrary proportion Mixture.
Described nano-ceramic powder be particle diameter be the nano-ceramic powder of 5~10nm.
Described thixotropic agent is the one in aerosil, organobentonite, castor oil hydrogenated, polyamide wax or several Kind.
The invention has the beneficial effects as follows, the cyanate ester resin composite material dielectric properties that produced, mechanical property, wear-resisting The combination properties such as property, hardness significantly improve.
Detailed description of the invention
Below by embodiment, the present invention is described in further details.
Embodiment 1:
Get the raw materials ready by following formula:
Bisphenol A cyanate ester resin 70 mass parts,
Bisphenol type benzoxazine resins 30 mass parts,
Nano-ceramic powder 6 mass parts,
Aerosil 2 mass parts.
By 70 parts of bisphenol A cyanate ester resins, 30 parts of bisphenol type benzoxazine resins, stir at 100 DEG C, melt transparent After, add the nano-ceramic powder that 6 parts of particle diameters are 5~10nm, 2 parts of aerosils, be uniformly dispersed, by straight for the resin mixed Connect in the mould pouring preheating into, put in the vacuum drying oven of 80 DEG C, remove bubble, take out mould, put into blast dry oven and enter Row elevated cure, curing process is 160 DEG C/1h, 210 DEG C/3h, then natural cooling, and the demoulding obtains a kind of exceptional hardness cyanate The composite of resin.After tested, the hardness of composite reaches 7H.
Embodiment 2:
Get the raw materials ready by following formula:
Bisphenol E-type cyanate resin 80 mass parts,
Diamine type benzoxazine resins 20 mass parts,
Nano-ceramic powder 8 mass parts,
Organobentonite 1 mass parts.
By 80 parts of bisphenol E-type cyanate resins, 20 parts of diamine type benzoxazine resins, stir at 130 DEG C, wait to melt thoroughly After bright, add 1 part of organobentonite, 8 parts of particle diameters be 5~10nm nano-ceramic powder, wait to be uniformly dispersed, the resin that will have mixed Directly pour in the mould of preheating, put in the vacuum drying oven of 100 DEG C, remove bubble, take out mould, put into blast dry oven Carrying out elevated cure, curing process is 160 DEG C/1h, 210 DEG C/3h, then natural cooling, the demoulding, obtains a kind of exceptional hardness cyanic acid The composite of ester resin.After tested, the hardness of composite reaches 7H.
Embodiment 3:
Get the raw materials ready by following formula:
Bisphenol-f type cyanate ester resin 65 mass parts,
Bisphenol type benzoxazine resins 40 mass parts,
Nano-ceramic powder 3 mass parts,
Polyamide wax 3 mass parts.
By 65 parts of bisphenol-f type cyanate ester resins, 40 parts of bisphenol type benzoxazine resins, stir at 120 DEG C, wait to melt thoroughly After bright, add 3 parts of polyamide waxes, 3 parts of nano-ceramic powders, wait to be uniformly dispersed, the resin mixed directly is poured into the mould of preheating In tool, put in the vacuum drying oven of 80 DEG C, remove bubble, take out mould, put into blast dry oven and carry out elevated cure, solidification Technique is 160 DEG C/1h, 210 DEG C/3h, then natural cooling, the demoulding, obtains the composite of a kind of exceptional hardness cyanate ester resin. After tested, the hardness of composite reaches 7H.
Embodiment 4:
Get the raw materials ready by following formula:
Bisphenol A cyanate ester resin 50 mass parts,
Diamine type benzoxazine resins 70 mass parts,
Nano-ceramic powder 10 mass parts,
Aerosil 3 mass parts.
By 50 parts of bisphenol A cyanate ester resins, 70 parts of diamine type benzoxazine resins, stir at 110 DEG C, wait to melt thoroughly After bright, add 3 parts of aerosils, 10 parts of nano-ceramic powders, wait to be uniformly dispersed, directly pour the resin mixed into preheating Mould in, put in the vacuum drying oven of 90 DEG C, remove bubble, take out mould, put into blast dry oven and carry out elevated cure, Curing process is 160 DEG C/1h, 210 DEG C/3h, then natural cooling, the demoulding, obtains the compound of a kind of exceptional hardness cyanate ester resin Material.After tested, the hardness of composite reaches 7H.

Claims (5)

1. a cyanate ester resin composite material preparation method, it is characterised in that comprise the steps: in parts by mass, by 50~ 100 parts of cyanate ester resins, 1~100 part of benzoxazine resins, at 50~200 DEG C stir, melt transparent after, add 1~20 part Nano-ceramic powder, 0.1~10 part of thixotropic agent, it is uniformly dispersed, obtains cyanate ester resin composite material.
Cyanate ester resin composite material preparation method the most according to claim 1, it is characterised in that described cyanate ester resin For bisphenol A cyanate ester resin, bisphenol E-type cyanate resin, bisphenol-f type cyanate ester resin, bis-phenol M type cyanate ester resin, double The mixture of a kind of or its arbitrary proportion in Cyclopeutadiene type cyanate ester resin.
Cyanate ester resin composite material preparation method the most according to claim 1, it is characterised in that described benzimidazole dihydrochloride tree Fat is a kind of or mixture of its arbitrary proportion in bisphenol type benzimidazole dihydrochloride, diamine type benzimidazole dihydrochloride.
Cyanate ester resin composite material preparation method the most according to claim 1, it is characterised in that described nano-ceramic powder For the nano-ceramic powder that particle diameter is 5~10nm.
Cyanate ester resin composite material preparation method the most according to claim 1, it is characterised in that described thixotropic agent is gas One or more in aerosil, organobentonite, castor oil hydrogenated, polyamide wax.
CN201610700498.1A 2016-08-22 2016-08-22 Cyanate ester resin composite material preparation method Pending CN106221215A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201610700498.1A CN106221215A (en) 2016-08-22 2016-08-22 Cyanate ester resin composite material preparation method

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201610700498.1A CN106221215A (en) 2016-08-22 2016-08-22 Cyanate ester resin composite material preparation method

Publications (1)

Publication Number Publication Date
CN106221215A true CN106221215A (en) 2016-12-14

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107955371A (en) * 2017-12-14 2018-04-24 威海光威复合材料股份有限公司 The preparation method of bimaleimide resin epoxy resin composite material
CN107974042A (en) * 2017-12-21 2018-05-01 威海光威复合材料股份有限公司 The preparation method of benzoxazine colophony cyanate ester resin composite material
CN107974084A (en) * 2017-12-14 2018-05-01 威海光威复合材料股份有限公司 The preparation method of bimaleimide resin benzoxazine colophony composite material
CN110845845A (en) * 2019-11-13 2020-02-28 上海卫星装备研究所 Nano particle modification-based space-grade cyanate ester resin and preparation method thereof

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103074027A (en) * 2013-01-11 2013-05-01 西北工业大学 Phenolphthalein cyanate/benzoxazine resin adhesive resistant to 250 DEG C and preparation method
CN103980704A (en) * 2014-05-28 2014-08-13 苏州生益科技有限公司 Halogen-free resin composition for high-frequency and high-speed substrate as well as prepreg and laminated plate

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103074027A (en) * 2013-01-11 2013-05-01 西北工业大学 Phenolphthalein cyanate/benzoxazine resin adhesive resistant to 250 DEG C and preparation method
CN103980704A (en) * 2014-05-28 2014-08-13 苏州生益科技有限公司 Halogen-free resin composition for high-frequency and high-speed substrate as well as prepreg and laminated plate

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107955371A (en) * 2017-12-14 2018-04-24 威海光威复合材料股份有限公司 The preparation method of bimaleimide resin epoxy resin composite material
CN107974084A (en) * 2017-12-14 2018-05-01 威海光威复合材料股份有限公司 The preparation method of bimaleimide resin benzoxazine colophony composite material
CN107974042A (en) * 2017-12-21 2018-05-01 威海光威复合材料股份有限公司 The preparation method of benzoxazine colophony cyanate ester resin composite material
CN110845845A (en) * 2019-11-13 2020-02-28 上海卫星装备研究所 Nano particle modification-based space-grade cyanate ester resin and preparation method thereof
CN110845845B (en) * 2019-11-13 2022-11-11 上海卫星装备研究所 Nano particle modification-based space-grade cyanate ester resin and preparation method thereof

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