CN108219454A - A kind of preparation method of cyanate resin base glued membrane - Google Patents

A kind of preparation method of cyanate resin base glued membrane Download PDF

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Publication number
CN108219454A
CN108219454A CN201611161230.1A CN201611161230A CN108219454A CN 108219454 A CN108219454 A CN 108219454A CN 201611161230 A CN201611161230 A CN 201611161230A CN 108219454 A CN108219454 A CN 108219454A
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CN
China
Prior art keywords
resin
glued membrane
component
cyanate
preparation
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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
CN201611161230.1A
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Chinese (zh)
Inventor
狄成瑞
修志锋
王平
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AVIC Research Institute Special Structures Aeronautical Composites
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AVIC Research Institute Special Structures Aeronautical Composites
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Priority to CN201611161230.1A priority Critical patent/CN108219454A/en
Publication of CN108219454A publication Critical patent/CN108219454A/en
Pending legal-status Critical Current

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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L79/00—Compositions 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
    • C08L79/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
    • C08J5/18—Manufacture of films or sheets
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2379/00—Characterised by the use 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 C08J2361/00 - C08J2377/00
    • C08J2379/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2461/00—Characterised by the use of condensation polymers of aldehydes or ketones; Derivatives of such polymers
    • C08J2461/04—Condensation polymers of aldehydes or ketones with phenols only
    • C08J2461/16—Condensation polymers of aldehydes or ketones with phenols only of ketones with phenols
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2463/00—Characterised by the use of epoxy resins; Derivatives of epoxy resins
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2481/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing sulfur with or without nitrogen, oxygen, or carbon only; Polysulfones; Derivatives of such polymers
    • C08J2481/06—Polysulfones; Polyethersulfones
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00—Properties
    • C08L2201/08—Stabilised against heat, light or radiation or oxydation
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2203/00—Applications
    • C08L2203/16—Applications used for films
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00—Polymer mixtures characterised by other features
    • C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend

Abstract

The present invention relates to a kind of glue film manufacturing process, more particularly to a kind of preparation method of cyanate resin base glued membrane.Thermoplastic resin is heat-fused in the mixture of epoxy resin, reactive diluent or both and forms component A；Powdered thermoplastic resin forms B component with cyanate ester resin or with the cyanate resin lipoprotein mixture blended under agitation added with one or both of epoxy resin, reactive diluent；Component A and B component are blended to form sizing material；Sizing material is made by glued membrane using hot melt film applicator or film laminator.A kind of preparation method of cyanate resin base glued membrane for being easy to Project Realization is provided, solves glued membrane toughness, the technical issues of craftsmanship is unstable in the prior art.

Description

A kind of preparation method of cyanate resin base glued membrane
Technical field
The present invention relates to a kind of glue film manufacturing process, more particularly to a kind of preparation method of cyanate resin base glued membrane.
Background technology
Existing and common glued membrane method for toughening is that cyanate ester resin and polysulfones, polyether sulfone, polyether-ether-ketone, polyamides is sub- The thermoplastic resins toughening such as amine, polyphenylene oxide.To reach ideal toughening effect, need to add a large amount of thermoplastic resin, General more than 20% addition, often takes following three kinds of modes：One kind is using suitable by cyanate ester resin and thermoplastic resin Solvent dissolving blending, but the solvent boiling point for dissolving engineering plastics is higher, it is difficult to it removes, influences the performance of glued membrane；One kind is will be hot Plastic resin is heat-fused in cyanate ester resin prepares glued membrane using hot melt, but the fusing point of some thermoplastic resins is higher and be difficult to It is fused in cyanate ester resin, is sharply increased even if cyanate ester resin can be fused to and will also result in resin viscosity, the operation of melten gel process is tired Difficulty, the pre-polymerization degree difficulty or ease control of cyanate ester resin, causes glue film performance unstable；Another kind is that thermoplastic resin is made powder It is last to be blended, but it is scattered that sizing material be caused to do, and is not easy to form a film with cyanate ester resin, even if adding in a large amount of epoxy resin, activity dilution Agent improves glued membrane craftsmanship, but can cause the decline of glued membrane dielectric properties, heat resistance.
Invention content
The purpose of the present invention：A kind of preparation method of cyanate resin base glued membrane for being easy to Project Realization is provided, is solved existing There is the technical issues of glued membrane toughness in technology, craftsmanship is unstable.
Technical scheme of the present invention：A kind of preparation method of cyanate resin base glued membrane, it is characterised in that the method Including：
Thermoplastic resin is heat-fused in the mixture of epoxy resin, reactive diluent or both and forms component A；
Powdered thermoplastic resin and cyanate ester resin or with added with one or both of epoxy resin, reactive diluent Cyanate resin lipoprotein mixture blended under agitation formed B component；
Component A and B component are blended to form sizing material；
Sizing material is made by glued membrane using hot melt film applicator or film laminator.
Preferably, the grain size of powdered thermoplastic resin is 20 μm~100 μm.
Preferably, the glued membrane is compound by hot pressing and cloth of reinforcement fibers or reinforcing fiber net.
Beneficial effects of the present invention：Present invention eliminates the influence of solvent, while solve a large amount of thermoplastic resins are complete The mixture that portion is fused to cyanate ester resin, epoxy resin or both causes viscosity increased dramatically, it is difficult to operate, cyanate ester resin is pre- The problems such as poly- terminal is difficult to control, and glue film performance is unstable also solves exclusive use powder and is difficult to the technological problems to form a film, this Kind of method only needs a small amount of epoxy resin or reactive diluent with regard to that can improve viscosity, the craftsmanship of sizing material, it is easier to it production and uses, And do not influence the dielectric and heat resistance of glued membrane.
Specific embodiment
A kind of cyanate resin base glue film manufacturing process be by thermoplastic resin elder generation low-temperature grinding to powdered, then will be hot Plastic resin, which is heat-fused in the mixture of epoxy resin, reactive diluent or both, forms component A, and powdered thermoplastic resin is then With the mixture blended under agitation shape of cyanate ester resin or one or both of cyanate ester resin and epoxy resin, reactive diluent Into B component, finally component A, B component are blended to form sizing material, are made of hot melt film applicator, film laminator or other equivalent of the apparatus Glued membrane.
The method is realized by following steps：
Step 1：By thermoplastic resin in low-temperature grinding.
Step 2：Thermoplastic resin is heat-fused in the mixture of epoxy resin, reactive diluent or both and forms component A.
Step 3：Thermoplastic resin and cyanate ester resin or cyanate ester resin and epoxy resin or cyanogen after step 1 is crushed Acid ester resin and reactive diluent or cyanate ester resin and epoxy resin and reactive diluent are mixing uniformly to form B component.
Step 4：Component A and B component are formed to final sizing material after mixing.
Step 5：Glued membrane is made in the sizing material that step 4 obtains.
The thermoplastic resin is polysulfones, polyether sulfone, polyether-ether-ketone, polyimides etc., and low-temperature grinding temperature is -50 DEG C ~-150 DEG C, the grain size after crushing is 10 μm~200 μm, preferably 20 μm~100 μm.
Thermoplastic resin can be can also not crush after crushing in the step 2.
In the step 4 hybrid mode be manual mode or mechanical agitation, mechanical agitation speed for 50r/min~ 500r/min；Mixing can be that component A and B component manufacture last the two and be uniformly mixed respectively, can also directly add in component A Add the component of B component, be then uniformly mixed.
Glued membrane is prepares using hot melt in the step 5, i.e., using resin coating film machine, film laminator or other equivalent It is prepared by equipment；The glued membrane can only resiniferous resin film or include the resin film of carrier；The glue Film surface glue-line is uniform, mass area ratio 120g/m2~400g/m2。
Embodiment 1
Step 1：Bisphenol-a polysulfone is crushed using low temperature breaking equipment, it is -50 DEG C~-150 DEG C to crush temperature, is crushed Grain size afterwards is 50 μm~100 μm.
Step 2：By 10~50 parts of bisphenol-a polysulfones be heat-fused in 10~50 parts of bisphenol A type epoxy resins (E-51) and 10~ Component A is formed in 50 parts of neopentylglycol diglycidyl ether epoxide diluent mixtures, melting temperature is 100 DEG C~150 DEG C.
Step 3：By 50~100 parts of cyanate ester resins, 20~50 parts of bisphenol-a polysulfone powder using hand operated mixing or The churned mechanically mode of 50r/min~500r/min rotating speeds forms B component.
Step 4：Component A and B component are used into hand operated mixing or the churned mechanically side of 50r/min~500r/min rotating speeds Formula forms final sizing material after mixing.
Step 5：Sizing material is pressed by glued membrane using film laminator.
Embodiment 2
Step 1：Polyether-ether-ketone is crushed using low temperature breaking equipment, it is -50 DEG C~-150 DEG C to crush temperature, after crushing Grain size is 50 μm~100 μm.
Step 2：Weigh 60~100 parts of bisphenol E-type cyanate resins in parts by weight, 25~50 parts of polyether-ether-ketones, 15~ 45 parts of alicyclic type epoxy resins (TDE-85).
Step 3：5~10 parts of polyether-ether-ketones are heat-fused in shape in 15~25 parts of alicyclic type epoxy resin (TDE-85) mixtures Into component A, melting temperature is 100 DEG C~150 DEG C.
Step 4：60~100 parts of cyanate ester resins, 5~20 parts of polyether-ether-ketone powder are uniformly mixed, form B component.
Step 5：Component A and B component are used into hand operated mixing or the churned mechanically side of 50r/min~500r/min rotating speeds Formula is uniformly mixed.
Step 6：Using hot melt film applicator by sizing material the film on barrier paper, finally with quartz fiber cloth hot pressing complex Into carrier adhesive.

Claims (3)

1. a kind of preparation method of cyanate resin base glued membrane, it is characterised in that the method includes：
Thermoplastic resin is heat-fused in the mixture of epoxy resin, reactive diluent or both and forms component A；
Powdered thermoplastic resin and cyanate ester resin or with the cyanogen added with one or both of epoxy resin, reactive diluent Acid ester resin mixture blended under agitation forms B component；
Component A and B component are blended to form sizing material；
Sizing material is made by glued membrane using hot melt film applicator or film laminator.
2. a kind of preparation method of cyanate resin base glued membrane according to claim 1, it is characterized in that：Powdery thermoplastic The grain size of resin is 20 μm~100 μm.
3. a kind of preparation method of cyanate resin base glued membrane according to claim 1, it is characterized in that：The glued membrane leads to It crosses hot pressing and cloth of reinforcement fibers or reinforcing fiber net is compound.
CN201611161230.1A 2016-12-15 2016-12-15 A kind of preparation method of cyanate resin base glued membrane Pending CN108219454A (en)

Priority Applications (1)

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CN201611161230.1A CN108219454A (en) 2016-12-15 2016-12-15 A kind of preparation method of cyanate resin base glued membrane

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201611161230.1A CN108219454A (en) 2016-12-15 2016-12-15 A kind of preparation method of cyanate resin base glued membrane

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Publication Number Publication Date
CN108219454A true CN108219454A (en) 2018-06-29

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102876247A (en) * 2012-10-24 2013-01-16 黑龙江省科学院石油化学研究院 Modified cyanate adhesive film and preparation method thereof
CN102922855A (en) * 2012-10-24 2013-02-13 中国航空工业集团公司北京航空材料研究院 Method for preparing high-tenacity hot-melt prepreg by hot-melt resin matrix
CN105623546A (en) * 2015-12-22 2016-06-01 中国航空工业集团公司济南特种结构研究所 Preparation method of reinforced adhesive film

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102876247A (en) * 2012-10-24 2013-01-16 黑龙江省科学院石油化学研究院 Modified cyanate adhesive film and preparation method thereof
CN102922855A (en) * 2012-10-24 2013-02-13 中国航空工业集团公司北京航空材料研究院 Method for preparing high-tenacity hot-melt prepreg by hot-melt resin matrix
CN105623546A (en) * 2015-12-22 2016-06-01 中国航空工业集团公司济南特种结构研究所 Preparation method of reinforced adhesive film

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
乔海涛等: "高韧性氰酸酯基胶膜的研制", 《第17届全国复合材料学术会议论文》 *

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Application publication date: 20180629

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