CN108395860A - The preparation method of low-temperature setting structural film adhesive - Google Patents
The preparation method of low-temperature setting structural film adhesive Download PDFInfo
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- CN108395860A CN108395860A CN201810325967.5A CN201810325967A CN108395860A CN 108395860 A CN108395860 A CN 108395860A CN 201810325967 A CN201810325967 A CN 201810325967A CN 108395860 A CN108395860 A CN 108395860A
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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
- C09J163/00—Adhesives based on epoxy resins; Adhesives based on derivatives of epoxy resins
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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
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
-
- 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
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/06—Non-macromolecular additives organic
-
- 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
- C09J7/00—Adhesives in the form of films or foils
- C09J7/20—Adhesives in the form of films or foils characterised by their carriers
- C09J7/21—Paper; Textile fabrics
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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
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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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
- C08L2203/00—Applications
- C08L2203/16—Applications used for films
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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
- 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
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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
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
The present invention provides a kind of preparation method of low-temperature setting structural film adhesive, this kind of low-temperature setting structural film adhesive, in terms of parts by weight, include the F components of the D components of the component A of 25~50 parts by weight, the B component of 25~50 parts by weight, the component C of 10~25 parts by weight, 5~40 parts by weight, the component E of 10~25 parts by weight and 1~25 parts by weight；Wherein, component A is selected from least one of polyfunctional epoxy resin；B component is one or more in bisphenol-type epoxy resin；Above A~F each components are obtained into resin combination after mixing, obtained resin combination is prepared into 100~400g/m through hot melt2Low-temperature setting structural film adhesive.The present invention easy tos produce internal stress during capable of effectively reducing heating cure, and low-temperature setting structural film adhesive obtained has excellent adhesive property, can be widely used in plate plate in metal or composite material, plate core splicing, have good bonding effect.
Description
Technical field
The present invention relates to a kind of preparation methods of low-temperature setting structural film adhesive.
Background technology
In aerospace field, the splicing of metal or composite material structural member is avoided that the stress concentration of mechanical connection, carries
The integrality and rigidity of high structure improve its anti-fatigue performance, while can also mitigate architecture quality, reduce manufacturing cost.
To reduce the manufacturing cost of Advanced Resin-based Composites, promote it in Aeronautics and Astronautics, weapons, ship and electronics
Equal fields are widely used, it is desirable that solidification temperature reduces as possible, to reduce the energy consumption of solidification process.But membranaceous epoxy glue is general
Need medium temperature or hot setting.120 DEG C of even higher temperature are heated to be cured.This just needs to use hot-press equipment,
The efficiency of industrialized mass production, and the difference of the coefficient of thermal expansion due to different materials are not only influenced, in heating cure
Internal stress is easy tod produce in journey.
Invention content
The object of the present invention is to provide a kind of solution of the preparation method of low-temperature setting structural film adhesive is existing in the prior art
Membranaceous epoxy glue generally requires medium temperature or hot setting, that is, is heated to 120 DEG C of even higher temperature and is cured.This is just needed
Using hot-press equipment, the efficiency of industrialized mass production, and the difference of the coefficient of thermal expansion due to different materials are not only influenced,
The problem of internal stress being easy tod produce during heating cure.
Technical solution of the invention is：
A kind of preparation method of low-temperature setting structural film adhesive, this kind of low-temperature setting structural film adhesive, in terms of parts by weight, including 25~
The component A of 50 parts by weight, the B component of 25~50 parts by weight, the component C of 10~25 parts by weight, the D components of 5~40 parts by weight, 10
The F components of the component E of~25 parts by weight and 1~25 parts by weight；Wherein, component A in polyfunctional epoxy resin at least
It is a kind of；B component is one or more in bisphenol-type epoxy resin；Component C is polyetheramine, imidazoles, dicyandiamide and its spreads out
Two or more in biological species and microcapsules class latent curing agent system；D groups are divided into activeness and quietness system；Component E is
Two or more in substituted urea, 2- benzylimidazolines, DMP-30；F groups are divided into auxiliary agent；Above A~F each components are uniformly mixed
After obtain resin combination, obtained resin combination is prepared into 100~400g/m through hot melt2Low-temperature setting structure glue
Film.
Further, one kind in TDE-85, AG-80, AFG-90 multi-functional epoxy of polyfunctional epoxy resin or
It is a variety of.
Further, bisphenol-type epoxy resin is selected from bisphenol A type epoxy resin, bisphenol f type epoxy resin and bisphenol S type
It is one or more in epoxy resin.
Further, activeness and quietness system is CTBN rubber, ETBN rubber, core shell rubbers, the modifies ring of elastic polyurethane
It is one or more in oxygen resin.
Further, auxiliary agent includes one or more in thixotropic agent, reinforcing agent, coupling agent.
The low-temperature setting structural film adhesive that the present invention obtains has excellent adhesive strength, suitable for metal or composite material
Board-to-board, plate-core rubber connect, and have good bonding effect.The low-temperature setting structural film adhesive that the present invention obtains, can be with metal or multiple
Condensation material carries out the splicing of the materials such as board-to-board, plate-core or structural member, has excellent adhesive shear strength.
In the present invention, condition of cure is to cure 4~5h, 0.1~0.3 MPa of solidifying pressure at 85 DEG C.What the present invention obtained
Low-temperature setting structural film adhesive, after 85 DEG C of solidifications, metal list lap shear strength is at room temperature up to 35.5 MPa, 82 DEG C
Down cut intensity still has 28.0 MPa, shows that the low-temperature setting structural film adhesive has excellent adhesive property.
The beneficial effects of the invention are as follows：The preparation method of this kind of low-temperature setting structural film adhesive, it is active to differential responses solid
Agent is used in compounding, and the addition of low temperature curing agent is conducive to that reaction is promoted to carry out at low temperature, is put in LOTES process
The heat gone out is conducive to further promote the progress of pyroreaction.The extent of reaction is carried out by controlling low temperature curing agent usage amount
Control, makes reaction be unlikely to excessively to carry out.The addition of high-temperature curing agent can effectively improve membranaceous epoxy glue in high temperature side simultaneously
Performance under test ring border.Accelerator package, accelerator package is selected to be made of two or more different accelerating agent,
Using the mutual supplement with each other's advantages of all kinds of accelerating agent performances, reach best using effect, different accelerating agents promotes different solidifications
Agent reacts.Final obtained membranaceous epoxy glue can at 85 DEG C completion of cure, can effectively reduce and hold during heating cure
It is also easy to produce internal stress.Low-temperature setting structural film adhesive produced by the present invention has excellent adhesive property, can be widely used in gold
Board-to-board, plate-core rubber connect in category or composite material, have good bonding effect.
Specific implementation mode
The following detailed description of the preferred embodiment of the present invention.
Embodiment
A kind of low-temperature setting structural film adhesive, in terms of parts by weight, composition is as follows：
Component A：30 parts of TDE-85 epoxy resin, 25 parts of AG-80 epoxy resin；
B component：45 parts of Bisphenol F epoxies；
Component C：5 parts of polyetheramines, 6 parts of dicyandiamides；
D components：15 parts of core shell rubbers（MX-157）, 15 parts of thermoplastic resins；
Component E：3 parts of substituted ureas, 1 part of DMP-30；
F components：2 parts of titanate esters, 2 parts of aerosils.
The preparation method of this kind of low-temperature setting structural film adhesive is as follows：
Component A, B component and D components are added in mixing apparatus, being warming up to 120 DEG C of 60 min of insulated and stirred keeps D components abundant
It dissolves and is uniformly mixed, F components are added, in 90 DEG C of 30 min of insulated and stirred, component C and component E are added after being cooled to 45 DEG C,
20 min of insulated and stirred makes system be uniformly mixed, obtains resin combination.
Above-mentioned resin combination is film-made on adhesive film machine and obtains 300 ± 25 g/m of weight per unit area2Resin film simultaneously
With the compound obtained low-temperature setting structural film adhesive of nylon gauze carrier.
Performance test：
1, using 2024-T3 aluminiums, HBZ197 is pressed in aluminium material surface processing《Structural adhesive bonding aluminium alloy phosphoric acid technological specification》
It carries out, prepares metal list lap shear strength sample, solidification temperature condition is 85 DEG C of heat preservations 4h, 0.3 MPa of pressure.
2, it is tested into row metal list lap shear strength according to ASTM D1002, data are as shown in table 1 below.
1 low-temperature setting structural film adhesive performance data of table
As it can be seen from table 1 the low-temperature setting structural film adhesive not only has preferable shear strength at room temperature, at 82 DEG C
Shear strength still up to 28.0 MPa, has preferable heat resistance.
Comparative example
A kind of low-temperature setting structural film adhesive, in terms of parts by weight, composition is as follows：
Component A：30 parts of TDE-85 epoxy resin, 25 parts of AG-80 epoxy resin；
B component：45 parts of Bisphenol F epoxies；
Component C：5 parts of polyetheramines, 6 parts of dicyandiamides；
D components：15 parts of thermoplastic resins；
Component E：3 parts of substituted ureas, 1 part of DMP-30；
F components：2 parts of titanate esters, 2 parts of aerosils.
The preparation method of this kind of low-temperature setting structural film adhesive is as follows：
Component A, B component and D components are added in mixing apparatus, being warming up to 120 DEG C of 60 min of insulated and stirred keeps D components abundant
It dissolves and is uniformly mixed, F components are added, in 90 DEG C of 30 min of insulated and stirred, component C and component E are added after being cooled to 45 DEG C,
20 min of insulated and stirred makes system be uniformly mixed, obtains resin combination.
Above-mentioned resin combination is film-made on adhesive film machine and obtains 300 ± 25 g/m of weight per unit area2Resin film simultaneously
With the compound obtained low-temperature setting structural film adhesive of nylon gauze carrier.
Performance test：
1, using 2024-T3 aluminiums, HBZ197 is pressed in aluminium material surface processing《Structural adhesive bonding aluminium alloy phosphoric acid technological specification》
It carries out, prepares metal list lap shear strength sample, solidification temperature condition is 85 DEG C of heat preservations 4h, 0.3 MPa of pressure.
2, it is tested into row metal list lap shear strength according to ASTM D1002, data are as shown in table 1 below.
2 low-temperature setting structural film adhesive performance data of table
From table 2 it can be seen that low-temperature setting structural film adhesive its room temperature list overlap joint and high temperature list overlap joint property after removing MX-157
It can decrease drastically.
Claims (5)
1. a kind of preparation method of low-temperature setting structural film adhesive, it is characterised in that：This kind of low-temperature setting structural film adhesive, with parts by weight
Number meter, including the component A of 25~50 parts by weight, the B component of 25~50 parts by weight, the component C of 10~25 parts by weight, 5~40 weights
Measure the D components, the F components of the component E of 10~25 parts by weight and 1~25 parts by weight of part；Wherein, component A is selected from polyfunctional group
At least one of epoxy resin；B component is one or more in bisphenol-type epoxy resin；Component C is polyetheramine, imidazoles
Two or more in class, dicyandiamide and its derivative species and microcapsules class latent curing agent system；D groups are divided into enhancing and increase
Tough system；Component E is two or more in substituted urea, 2- benzylimidazolines, DMP-30；F groups are divided into auxiliary agent；By above A~F
Each component obtains resin combination after mixing, and obtained resin combination is prepared into 100~400g/m through hot melt2It is low
Warm consolidated structures glued membrane.
2. the preparation method of low-temperature setting structural film adhesive as described in claim 1, it is characterised in that：Polyfunctional epoxy resin
It is one or more in TDE-85, AG-80, AFG-90 multi-functional epoxy.
3. the preparation method of low-temperature setting structural film adhesive as described in claim 1, it is characterised in that：Bisphenol-type epoxy resin selects
From one or more in bisphenol A type epoxy resin, bisphenol f type epoxy resin and bisphenol-s epoxy resin.
4. the preparation method of low-temperature setting structural film adhesive as described in any one of claims 1-3, it is characterised in that：Activeness and quietness
System is one or more in CTBN rubber, ETBN rubber, core shell rubbers, polyurethane elastomer modified epoxy.
5. the preparation method of low-temperature setting structural film adhesive as described in any one of claims 1-3, it is characterised in that：Auxiliary agent includes
It is one or more in thixotropic agent, reinforcing agent, coupling agent.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810325967.5A CN108395860A (en) | 2018-04-12 | 2018-04-12 | The preparation method of low-temperature setting structural film adhesive |
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| CN201810325967.5A CN108395860A (en) | 2018-04-12 | 2018-04-12 | The preparation method of low-temperature setting structural film adhesive |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109321186A (en) * | 2018-10-15 | 2019-02-12 | 航天材料及工艺研究所 | It a kind of semi-solid preparation epoxy jelly membrane and preparation method thereof and uses |
| CN112309703A (en) * | 2020-11-03 | 2021-02-02 | 安徽智磁新材料科技有限公司 | Solidification method of nanocrystalline magnetic core |
| CN114752314A (en) * | 2022-04-11 | 2022-07-15 | 中国航发北京航空材料研究院 | High-durability high-temperature curing epoxy structure adhesive film and preparation method thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109321186A (en) * | 2018-10-15 | 2019-02-12 | 航天材料及工艺研究所 | It a kind of semi-solid preparation epoxy jelly membrane and preparation method thereof and uses |
| CN112309703A (en) * | 2020-11-03 | 2021-02-02 | 安徽智磁新材料科技有限公司 | Solidification method of nanocrystalline magnetic core |
| CN114752314A (en) * | 2022-04-11 | 2022-07-15 | 中国航发北京航空材料研究院 | High-durability high-temperature curing epoxy structure adhesive film and preparation method thereof |
| CN114752314B (en) * | 2022-04-11 | 2024-02-13 | 中国航发北京航空材料研究院 | High-durability high-temperature cured epoxy structural adhesive film and preparation method thereof |
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Application publication date: 20180814 |