CN108314991A - Resistance to 180 DEG C of high temperature adhesives of one kind and preparation method thereof - Google Patents
Resistance to 180 DEG C of high temperature adhesives of one kind and preparation method thereof Download PDFInfo
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- CN108314991A CN108314991A CN201810144635.7A CN201810144635A CN108314991A CN 108314991 A CN108314991 A CN 108314991A CN 201810144635 A CN201810144635 A CN 201810144635A CN 108314991 A CN108314991 A CN 108314991A
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- resistance
- epoxy resin
- high temperature
- benzimidazole
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J187/00—Adhesives based on unspecified macromolecular compounds, obtained otherwise than by polymerisation reactions only involving unsaturated carbon-to-carbon bonds
- C09J187/005—Block or graft polymers not provided for in groups C09J101/00 - C09J185/04
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G81/00—Macromolecular compounds obtained by interreacting polymers in the absence of monomers, e.g. block polymers
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J163/00—Adhesives based on epoxy resins; Adhesives based on derivatives of epoxy resins
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J179/00—Adhesives based on 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 C09J161/00 - C09J177/00
- C09J179/04—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
- 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
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer 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
-
- 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
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Epoxy Resins (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
The invention discloses a kind of resistance to 180 DEG C of high temperature adhesives, include the component of following mass fraction：10~60 parts of bisphenol A cyanate ester resin；10~40 parts of epoxy resin；5~30 parts of benzimidazole resin；5~40 parts of reactive diluent.The adhesive has excellent heat resistance and toughness, it can be suitable for bonding and the sealing of high-temperature structural material or thermally protective materials, the high-tech areas such as Aeronautics and Astronautics, communications and transportation and microelectronics are can be applied to, invention additionally discloses a kind of preparation methods of resistance to 180 DEG C of high temperature adhesives.
Description
Technical field
The present invention relates to adhesive areas, and in particular to resistance to 180 DEG C of high temperature adhesives of one kind and preparation method thereof.
Background technology
In recent years, with the progress of science and technology, various high-tech sectors, especially in fields such as Aeronautics and Astronautics, electronics
Requirement to high-temperature resistance adhesive performance is continuously improved.The characteristics of cyanate ester adhesive is high temperature resistant, corrosion-resistant, radiation resistance, together
When have many advantages, such as excellent electrical insulating property, water resistance and weatherability, can bonded metal, plastics, rubber, glass, ceramics etc.,
Be widely used in space travel, aircraft manufacturing, electronics industry, mechanical processing, automobile making and building and medical treatment aspect
Bonding and sealing.Although organic adhesion agent has excellent adhesive strength degree and rigidity, in using for cyanate ester adhesive
Also some shortcomings, such as rigid big, poor toughness and poor in processability are exposed in journey, and due to the heat resistance of resin matrix
Limitation, temperature in use is generally below 100 DEG C, to limit its application range.
Invention content
In order to solve the above-mentioned technical problem, the present invention discloses a kind of resistance to 180 DEG C of high temperature adhesives, which has excellent
Heat resistance and toughness, bonding and the sealing of high-temperature structural material or thermally protective materials can be suitable for, can be applied to aviation, boat
It, the high-tech areas such as communications and transportation and microelectronics, invention additionally discloses a kind of preparation methods of resistance to 180 DEG C of high temperature adhesives.
The present invention is achieved through the following technical solutions：
A kind of resistance to 180 DEG C of high temperature adhesives, include the component of following mass fraction：
10~60 parts of bisphenol A cyanate ester resin；10~40 parts of epoxy resin；5~30 parts of benzimidazole resin；Activity is dilute
Release 5~40 parts of agent.
The benzimidazole resin is benzimidazole resin and/or diamines benzimidazole resin.
The epoxy resin is appointing in F-44 phenol aldehyde type epoxy resins, AG-80 epoxy resin and TDE-85 epoxy resin
It is a kind of.
The epoxy resin includes F-44 phenol aldehyde type epoxy resins, AG-80 epoxy resin and TDE-85 epoxy resin.
A kind of preparation method of resistance to 180 DEG C of high temperature adhesives, comprises the following steps that：
(1) 10~60 parts of bisphenol A cyanate ester resins are put into reactor, are melted simultaneously at a temperature of 100~180 DEG C
Then 10~40 parts of epoxy resin are added to copolymer-1 0min~100min in reactor by pre-polymerization 1min~30min, obtain
One copolymerization system, i.e. component A need to be stirred continuously in the whole process.
(2) reactor is taken out from heat source, is kept stirring, reduce the temperature of temperature to 80~130 DEG C, then again will
Reactor is put into heat source, maintains temperature in 80~130 DEG C of ranges, at this time by 5~30 parts of benzimidazole resins and 5~40 parts
Reactive diluent is added in the reactor of the component A of pre-polymerization, and melts copolymerization 5min~60min to get to resistance to 180 DEG C
The copolymerized system adhesive of bisphenol A cyanate ester/benzimidazole of high temperature, needs to be stirred continuously in the whole process.
Compared with prior art, the present invention having the following advantages and advantages：
A kind of resistance to 180 DEG C of high temperature adhesives of the invention, benzimidazole resin is added in bisphenol A cyanate ester resin,
So that the double bond in imidazoles is reacted with the double bond in bisphenol A cyanate ester and epoxy resin copolymerization system, network cross-linked is increased
Density improves the heat resistance of adhesive, while the introducing of benzimidazole reduces bisphenol A cyanate ester/epoxy-resin systems
Solidification temperature increases processing performance, and the composite adhesive of preparation can use at a high temperature of 180 DEG C for a long time, and with compared with
High tensile shear strength.
Specific implementation mode
To make the objectives, technical solutions, and advantages of the present invention clearer, with reference to embodiment, the present invention is made
Further to be described in detail, exemplary embodiment of the invention and its explanation are only used for explaining the present invention, are not intended as to this
The restriction of invention.
Embodiment 1
A kind of resistance to 180 DEG C of high temperature adhesives of the invention, are prepared by the following method：
It weighs 60 parts of bisphenol A cyanate ester resins to be put into reactor, melting and pre-polymerization 30min at a temperature of 100 DEG C,
Then 40 parts of epoxy resin heating stirrings are added to copolymerization 60min in reactor and obtain component A；Then by reactor from heat source
It takes out, is kept stirring, reduce temperature to 80 DEG C of temperature, then reactor is put into heat source again, maintain temperature at 80 DEG C,
In the reactor for the component A that 5 parts of benzimidazole resins and 40 portions of reactive diluents are added to pre-polymerization at this time, and melt altogether
Poly- 50min is to get to the copolymerized system adhesive of bisphenol A cyanate ester/benzimidazole of resistance to 180 DEG C of high temperature, in entire mistake
It needs to be stirred continuously in journey, resolidification reaction finally post-processes 190 DEG C/3h.
Shear strength is tested by national standard, test result is：Room temperature tensile shear strength 29.8MPa, 180 DEG C of stretchings are cut
Shearing stress 16.5MPa.
Embodiment 2
A kind of resistance to 180 DEG C of high temperature adhesives of the invention, are prepared by the following method：
It weighs 50 parts of bisphenol A cyanate ester resins to be put into reactor, melting and pre-polymerization 20min at a temperature of 120 DEG C,
Then 25 parts of epoxy resin heating stirrings are added to copolymerization 40min in reactor and obtain component A；Then by reactor from heat source
It takes out, is kept stirring, reduce temperature to 90 DEG C of temperature, then reactor is put into heat source again, maintain temperature at 90 DEG C,
In the reactor for the component A that 15 parts of benzimidazole resins and 35 portions of reactive diluents are added to pre-polymerization at this time, and melt
40min is copolymerized to get to the copolymerized system adhesive of bisphenol A cyanate ester/benzimidazole of resistance to 180 DEG C of high temperature, entire
It needs to be stirred continuously in the process, resolidification reaction finally post-processes 190 DEG C/3h.
Shear strength is tested by national standard, test result is：Room temperature tensile shear strength 28.1MPa, 180 DEG C of stretchings are cut
Shearing stress 15.9MPa.
Embodiment 3
A kind of resistance to 180 DEG C of high temperature adhesives of the invention, are prepared by the following method：
It weighs 40 parts of bisphenol A cyanate ester resins to be put into reactor, melting and pre-polymerization 15min at a temperature of 140 DEG C,
Then 10 parts of epoxy resin heating stirrings are added to copolymerization 30min in reactor and obtain component A；Then by reactor from heat source
It takes out, is kept stirring, reduce temperature to 100 DEG C of temperature, then reactor is put into heat source again, maintain temperature 100
DEG C, in the reactor for the component A that 20 parts of benzimidazole resins and 30 portions of reactive diluents are added to pre-polymerization at this time, and melt
Melt copolymerization 30min to get to the copolymerized system adhesive of bisphenol A cyanate ester/benzimidazole of resistance to 180 DEG C of high temperature, whole
It needs to be stirred continuously during a, resolidification reaction finally post-processes 190 DEG C/3h.
Shear strength is tested by national standard, test result is：Room temperature tensile shear strength 28.7MPa, 180 DEG C of stretchings are cut
Shearing stress 14.4MPa.
Embodiment 4
A kind of resistance to 180 DEG C of high temperature adhesives of the invention, are prepared by the following method：
It weighs 30 parts of bisphenol A cyanate ester resins to be put into reactor, melting and pre-polymerization 10min at a temperature of 160 DEG C,
Then 40 parts of epoxy resin heating stirrings are added to copolymerization 20min in reactor and obtain component A；Then by reactor from heat source
It takes out, is kept stirring, reduce temperature to 120 DEG C of temperature, then reactor is put into heat source again, maintain temperature 120
DEG C, in the reactor for the component A that 25 parts of benzimidazole resins and 20 portions of reactive diluents are added to pre-polymerization at this time, and melt
Melt copolymerization 20min to get to the copolymerized system adhesive of bisphenol A cyanate ester/benzimidazole of resistance to 180 DEG C of high temperature, whole
It needs to be stirred continuously during a, resolidification reaction finally post-processes 190 DEG C/3h.
Shear strength is tested by national standard, test result is：Room temperature tensile shear strength 29.4MPa, 180 DEG C of stretchings are cut
Shearing stress 15.6MPa.
Above-described specific implementation mode has carried out further the purpose of the present invention, technical solution and advantageous effect
It is described in detail, it should be understood that the foregoing is merely the specific implementation mode of the present invention, is not intended to limit the present invention
Protection domain, all within the spirits and principles of the present invention, any modification, equivalent substitution, improvement and etc. done should all include
Within protection scope of the present invention.
Claims (5)
1. a kind of resistance to 180 DEG C of high temperature adhesives, which is characterized in that include the component of following mass fraction：
10~60 parts of bisphenol A cyanate ester resin；10~40 parts of epoxy resin；5~30 parts of benzimidazole resin；Reactive diluent
5~40 parts.
2. the resistance to 180 DEG C of high temperature adhesives of one kind according to claim 1, which is characterized in that the benzimidazole resin is
Benzimidazole resin and/or diamines benzimidazole resin.
3. the resistance to 180 DEG C of high temperature adhesives of one kind according to claim 1, which is characterized in that the epoxy resin is F-44
Any one of phenol aldehyde type epoxy resin, AG-80 epoxy resin and TDE-85 epoxy resin.
4. the resistance to 180 DEG C of high temperature adhesives of one kind according to claim 1, which is characterized in that the epoxy resin includes F-
44 phenol aldehyde type epoxy resins, AG-80 epoxy resin and TDE-85 epoxy resin.
5. a kind of preparation method of resistance to 180 DEG C of high temperature adhesives as described in any one of claim 1-4, which is characterized in that
It comprises the following steps that：
(1) 10~60 parts of bisphenol A cyanate ester resins are put into reactor, melting and pre-polymerization at a temperature of 100~180 DEG C
Then 10~40 parts of epoxy resin are added to copolymer-1 0min~100min in reactor, obtained uniform by 1min~30min
Copolymerization system, i.e. component A need to be stirred continuously in the whole process.
(2) reactor is taken out from heat source, is kept stirring, reduce the temperature of temperature to 80~130 DEG C, it then again will reaction
Device is put into heat source, maintains temperature in 80~130 DEG C of ranges, at this time by 5~30 parts of benzimidazole resins and 5~40 parts of activity
Diluent is added in the reactor of the component A of pre-polymerization, and melts copolymerization 5min~60min to get to resistance to 180 DEG C of high temperature
The copolymerized system adhesive of bisphenol A cyanate ester/benzimidazole, need to be stirred continuously in the whole process.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810144635.7A CN108314991A (en) | 2018-02-12 | 2018-02-12 | Resistance to 180 DEG C of high temperature adhesives of one kind and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810144635.7A CN108314991A (en) | 2018-02-12 | 2018-02-12 | Resistance to 180 DEG C of high temperature adhesives of one kind and preparation method thereof |
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| CN108314991A true CN108314991A (en) | 2018-07-24 |
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| CN201810144635.7A Pending CN108314991A (en) | 2018-02-12 | 2018-02-12 | Resistance to 180 DEG C of high temperature adhesives of one kind and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111925628A (en) * | 2020-06-30 | 2020-11-13 | 上海复合材料科技有限公司 | Solvent-free epoxy resin system for winding composite material pipe structure and preparation method thereof |
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2018
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111925628A (en) * | 2020-06-30 | 2020-11-13 | 上海复合材料科技有限公司 | Solvent-free epoxy resin system for winding composite material pipe structure and preparation method thereof |
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Application publication date: 20180724 |