CN108587060A - A kind of benzoxazine colophony constituent and its prepreg suitable for microwave curing process - Google Patents
A kind of benzoxazine colophony constituent and its prepreg suitable for microwave curing process Download PDFInfo
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- CN108587060A CN108587060A CN201810407900.6A CN201810407900A CN108587060A CN 108587060 A CN108587060 A CN 108587060A CN 201810407900 A CN201810407900 A CN 201810407900A CN 108587060 A CN108587060 A CN 108587060A
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- benzoxazine colophony
- constituent
- prepreg
- benzoxazine
- curing process
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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
- C08L61/00—Compositions of condensation polymers of aldehydes or ketones; Compositions of derivatives of such polymers
- C08L61/34—Condensation polymers of aldehydes or ketones with monomers covered by at least two of the groups C08L61/04, C08L61/18 and C08L61/20
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
Abstract
The present invention provides a kind of benzoxazine colophony constituents and its prepreg suitable for microwave curing process, and it is as follows that it includes components：A, at least one benzoxazine colophony；B, a kind of epoxy resin；C, at least one carbon nano-tube material.By resin combination and carbon fiber（Or carbon fibre fabric）Combined by hot melt, prepreg is made, after prepreg is laid in composite material mould surface according to Lay up design, periphery covers release cloth, isolation film, airfelt and vacuum bag and sealed with vacuum rubber belt successively；After vacuumizing, requires program mode to adjust microwave irradiation power size according to technological procedure, ensure the controllability of solidification process；Product curing molding after a certain period of time, cooling demoulding.The present invention is used for the manufacture of aviation rapid wear structural member, not only solve the problem that the deformation of traditional handicraft product is big, shrinking percentage is high, and product production efficiency is improved, manufacturing cost is reduced, the quick-replaceable maintenance levels to promoting China's aircraft equipment is of great significance.
Description
Technical field
The present invention relates to the preparations of a kind of benzoxazine colophony constituent and its prepreg, more particularly to one kind being suitable for boat
The preparation of empty rapid wear structural member manufacture microwave curing benzoxazine colophony constituent and its prepreg.
Background technology
Benzoxazine colophony is a kind of novel phenolic resins newly developed, and molecular polarity is almost nil after solidification, shrinking percentage
Extremely low, so there is extraordinary wet-hot aging performance, being used for a long time under moist hot environment can very well keep its excellent
Mechanical property and electric property.Again since the wetting property of benzoxazine colophony and a variety of reinforcements is very good, so it is multiple
The porosity of laminate article is relatively low, in addition benzoxazine colophony matrix hydroscopicity itself is low, is very suitable for military, industry
In some harsh environmental conditions purposes.But high, hardening time length etc. that there are solidification temperatures in benzoxazine colophony solidification process
Problem is higher to equipment, energy requirements.
Microwave has heating speed fast as a kind of completely new heat energy technology, and heat utilization rate is high, it can be achieved that quickly control
The advantages that.Microwave heating cure applications are in a kind of moulding process that the solidification of carbon fibre composite is new development in recent years, day
Benefit is paid attention to by constituent parts, but it is easy for aviation currently with microwave curing process to prepare benzoxazine colophony and its composite material
The manufacture of damage structure part has not been reported.
Therefore, the above problem is in the preparation method for prepare benzoxazine colophony and its composite material to microwave curing process
It should pay attention to and solve the problems, such as.
Invention content
The present invention provides a kind of benzoxazine tree suitable for microwave curing process for defect in the prior art is overcome
Fat composition and its prepreg
The technical scheme is that：Wherein it is suitable for the benzoxazine colophony constituent of microwave curing process, with organic solid
Object parts by weight meter, it includes component A, B, C, parts by weight are as follows：
A. at least one benzoxazine colophony, 50-70 parts；
B. epoxy resin, 20-50 parts；
C. at least one carbon nano-tube material, 1-10 parts.
A ingredients in the present invention, i.e. benzoxazine colophony are matrix resin component, play a leading role to material property, are wrapped
Dihydric phenol type benzoxazine is included, as shown in molecular formula 1：
1 dihydric phenol type benzoxazine monomer molecular formula of molecular formula
Naphthol type benzoxazine, as shown in molecular formula 2：
2 naphthol type benzoxazine molecular formula of molecular formula
Containing unsaturated bond type benzoxazine, as shown in molecular formula 3：
Molecular formula 3（1）The molecular formula of benzoxazine containing acetenyl
Molecular formula 3（2）The molecular formula of benzoxazine containing allyl
Diamin type benzoxazine, as shown in molecular formula 4：
4 diamin type benzoxazine molecular formula of molecular formula
B component in the present invention, i.e. epoxy resin, for adjusting resin system craftsmanship, to ensure that prepreg paving is good,
The specific trade mark is alicyclic trifunctional epoxy resin 4,5- 7-oxa-bicyclo[4.1.0-1,2- dicarboxylic acid diglycidyl esters.
C ingredients in the present invention, i.e. carbon nano-tube material component, including single tube material and/or multi wall carbon are received
Nanotube material is used mainly as microwave absorption, while carbon nanotube component will be significantly in the case where additive amount is smaller
The viscosity of increase system is changed into diffusion control to make chemical reaction play leading cross-linking reaction.
In mixture, the parts by weight of benzoxazine colophony are 50-70, and the parts by weight of epoxy resin are 20-50, the two
Weight ratio is preferably（55-65）:（35-45）.Carbon nano-tube material composition weight number is 1-10, preferably 3-7.
Further improvement of the present invention is：The benzoxazine colophony is dihydric phenol type benzoxazine colophony, naphthol type
One or more of benzoxazine colophony, two amine type benzoxazine colophonies composition.
Further improvement of the present invention is：The epoxy resin is alicyclic trifunctional epoxy resin 4,5- epoxide rings
Hexane -1,2- dicarboxylic acid diglycidyl esters.
Further improvement of the present invention is：The carbon nano-tube material is single tube material or multi-wall carbon nano-tube
One or more of tube material composition.
Further improvement of the present invention is：A kind of benzoxazine colophony constituent suitable for microwave curing process is provided
Prepreg, including benzoxazine colophony constituent and carbon fiber（Or carbon fibre fabric）, the preparation of the prepreg is using hot melt
Melt method, after benzoxazine colophony constituent obtained is toasted half an hour at 50-80 DEG C first, is placed on film applicator and uniformly applies
Preparation impregnation glued membrane is covered, then by glued membrane obtained and carbon fiber on pre- dipping machine（Or carbon fibre fabric）80-100 DEG C,
It is combined under 0.1-0.5MPa, prepreg can be obtained by finally covering PE films.
Further improvement of the present invention is：The microwave curing of a kind of benzoxazine colophony constituent and its prepreg is provided
Technique is as follows：
（1）After prepreg is laid in composite material mould surface according to Lay up design, periphery successively cover release cloth, isolation film,
Airfelt and vacuum bag are simultaneously sealed with vacuum rubber belt；
（2）After vacuumizing, program mode is required to adjust microwave irradiation power size according to technological procedure, and place temperature on mold
Sensing, the temperature feedback of measurement are compared to control system with process curve, ensure the controllability of solidification process；
（3）Product curing molding after a certain period of time, cooling demoulding, hardening time is 10-30 minutes, if product is more than 5mm, Gu
Change time lengthening to 40 ~ 60 minutes.
Further improvement of the present invention is：The composite material mould is carbon fibre reinforced composite mold, glass
MOULD OF FIBER REINFORCED COMPOSITES, ceramic material mold, quartz material mold, high temperature resistant cement material molds or high temperature resistant gypsum
Material molds.
Further improvement of the present invention is：The temperature sensing device includes thermocouple, thermistor, infrared sensing
It is one or more in device, optical fiber fluorescent sensor and fiber-optic grating sensor.
The beneficial effects of the invention are as follows：It is mainly used for the manufacture of the aviations rapid wear structural member such as lid, radome fairing to the present invention,
The use of benzoxazine colophony solves the problems, such as that conventional epoxies solidification leads to that product deformation is big, shrinking percentage is high, and microwave
Curing process not only reduces benzoxazine colophony solidification temperature, shortens hardening time, it is often more important that improves product production
Efficiency reduces manufacturing cost.Benzoxazine colophony constituent provided by the present invention suitable for microwave curing process and its pre-
Leaching material has the following advantages that：（1）The benzoxazine colophony and its prepreg of the present invention, composite product porosity after solidification
It is low, it is shunk close to zero, stress is small, without micro-crack,（2）The benzoxazine prepreg of the present invention is especially suitable for microwave curing work
Skill can significantly reduce benzoxazine solidification temperature, shorten hardening time,（3）Microwave curing used in the present invention, Neng Gouti
High product production efficiency reduces manufacturing cost,（4）The benzoxazine colophony and its prepreg and microwave curing process phase of the present invention
In conjunction with suitable for the manufacture of the aviations rapid wear structural members such as lid, radome fairing, to promoting China's boat under current complicated international environment
The quick-replaceable maintenance levels of sky equipment is of great significance.
Specific implementation mode
In order to deepen the understanding of the present invention, the present invention is described in further detail below in conjunction with embodiment, the reality
It applies example to be only used for explaining the present invention, protection scope of the present invention is not constituted and is limited.
Embodiment 1：
The technical solution of the present embodiment is：At 80 DEG C, by 55 parts of benzoxazine colophony AIBZ483 of component A（Shanghai is auspicious
Instrument Chemical Industry Science Co., Ltd）, 45 parts of epoxy resin 4,5- 7-oxa-bicyclo[4.1.0-1,2- dicarboxylic acid diglycidyl esters of B component（Extensively
Zhou Taiji new materials Co., Ltd）With 5 parts of single tube material WJST of component C（Anhui micro crystal material Science and Technology Ltd.）
It is uniformly mixed under high velocity agitation；
By above-mentioned resin compound be placed in film applicator be made glued membrane after and unidirectional carbon HF10-12K（The permanent refreshing share in Jiangsu
Co., Ltd）Interlayer structure is formed, benzoxazine colophony unidirectional carbon prepreg is prepared by hot pressing mode；
After above-mentioned prepreg is laid in composite material mould surface according to 0 ° of laying, periphery covers release cloth, isolation successively
Film, airfelt and vacuum bag are simultaneously sealed with vacuum rubber belt；After vacuumizing, program mode is required to adjust microwave spoke according to technological procedure
Watt level is penetrated, after twenty minutes product curing molding, cooling demoulding.
Benzoxazine unidirectional laminate bending strength is 1401MPa, interlaminar shear strength 102MPa, property in the embodiment
It can substantially equivalent solidification of hot-press tank.Other performance data are shown in Table one.
Embodiment 2
At 80 DEG C, by 70 parts of benzoxazine colophony AIBZ483 of component A（Shanghai Rui Yi Chemical Industry Science Co., Ltd）, B component
30 parts of epoxy resin 4,5- 7-oxa-bicyclo[4.1.0-1,2- dicarboxylic acid diglycidyl esters（Guangzhou Tai Ji new materials Co., Ltd）And C
5 parts of single tube material WJST of component（Anhui micro crystal material Science and Technology Ltd.）It is uniformly mixed under high velocity agitation；
By above-mentioned resin compound be placed in film applicator be made glued membrane after and unidirectional carbon HF10-12K（The permanent refreshing share in Jiangsu
Co., Ltd）Interlayer structure is formed, benzoxazine colophony unidirectional carbon prepreg is prepared by hot pressing mode；
After above-mentioned prepreg is laid in composite material mould surface according to 0 ° of laying, periphery covers release cloth, isolation successively
Film, airfelt and vacuum bag are simultaneously sealed with vacuum rubber belt；After vacuumizing, program mode is required to adjust microwave spoke according to technological procedure
Watt level is penetrated, after twenty minutes product curing molding, cooling demoulding.
Benzoxazine unidirectional laminate bending strength is 1287MPa, interlaminar shear strength 95MPa, property in the embodiment
It can substantially equivalent solidification of hot-press tank.Other performance data are shown in Table one.
Embodiment 3
At 80 DEG C, by 55 parts of benzoxazine colophony AIBZ483 of component A（Shanghai Rui Yi Chemical Industry Science Co., Ltd）, B component
45 parts of epoxy resin 4,5- 7-oxa-bicyclo[4.1.0-1,2- dicarboxylic acid diglycidyl esters（Guangzhou Tai Ji new materials Co., Ltd）And C
8 parts of single tube material WJST of component（Anhui micro crystal material Science and Technology Ltd.）It is uniformly mixed under high velocity agitation；
By above-mentioned resin compound be placed in film applicator be made glued membrane after and unidirectional carbon HF10-12K（The permanent refreshing share in Jiangsu
Co., Ltd）Interlayer structure is formed, benzoxazine colophony unidirectional carbon prepreg is prepared by hot pressing mode；
After above-mentioned prepreg is laid in composite material mould surface according to 0 ° of laying, periphery covers release cloth, isolation successively
Film, airfelt and vacuum bag are simultaneously sealed with vacuum rubber belt；After vacuumizing, program mode is required to adjust microwave spoke according to technological procedure
Watt level is penetrated, after ten minutes product curing molding, cooling demoulding.
Benzoxazine unidirectional laminate bending strength is 1383MPa, interlaminar shear strength 100MPa, property in the embodiment
It can substantially equivalent solidification of hot-press tank.Other performance data are shown in Table one.
Embodiment 4
At 80 DEG C, by 55 parts of benzoxazine colophony Coryes-CB3 of component A（Chengdu KeYi polymer Science Co., Ltd）、B
45 parts of epoxy resin 4,5- 7-oxa-bicyclo[4.1.0-1,2- dicarboxylic acid diglycidyl esters of component（Guangzhou Tai Ji new materials Co., Ltd）
With 5 parts of single tube material WJST of component C（Anhui micro crystal material Science and Technology Ltd.）It is uniformly mixed under high velocity agitation；
By above-mentioned resin compound be placed in film applicator be made glued membrane after and unidirectional carbon HF10-12K（The permanent refreshing share in Jiangsu
Co., Ltd）Interlayer structure is formed, benzoxazine colophony unidirectional carbon prepreg is prepared by hot pressing mode；
After above-mentioned prepreg is laid in composite material mould surface according to 0 ° of laying, periphery covers release cloth, isolation successively
Film, airfelt and vacuum bag are simultaneously sealed with vacuum rubber belt；After vacuumizing, program mode is required to adjust microwave spoke according to technological procedure
Watt level is penetrated, after twenty minutes product curing molding, cooling demoulding.
Benzoxazine unidirectional laminate bending strength is 1408MPa, interlaminar shear strength 101MPa, property in the embodiment
It can substantially equivalent solidification of hot-press tank.Other performance data are shown in Table one.
Embodiment 5
At 80 DEG C, by 55 parts of benzoxazine colophony AIBZ483 of component A（Shanghai Rui Yi Chemical Industry Science Co., Ltd）, B component
45 parts of epoxy resin 4,5- 7-oxa-bicyclo[4.1.0-1,2- dicarboxylic acid diglycidyl esters（Guangzhou Tai Ji new materials Co., Ltd）And C
5 parts of single tube material WJST of component（Anhui micro crystal material Science and Technology Ltd.）It is uniformly mixed under high velocity agitation；
By above-mentioned resin compound be placed in film applicator be made glued membrane after and carbon fibre fabric HFW220T-A3（The permanent refreshing stock in Jiangsu
Part Co., Ltd）Interlayer structure is formed, benzoxazine colophony unidirectional carbon prepreg is prepared by hot pressing mode；
After above-mentioned prepreg is laid in composite material mould surface according to 0 ° of laying, periphery covers release cloth, isolation successively
Film, airfelt and vacuum bag are simultaneously sealed with vacuum rubber belt；After vacuumizing, program mode is required to adjust microwave spoke according to technological procedure
Watt level is penetrated, product curing molding after 30 minutes, cooling demoulding.
Benzoxazine unidirectional laminate bending strength is 866MPa, interlaminar shear strength 67MPa, performance in the embodiment
Substantially equivalent solidification of hot-press tank.Other performance data are shown in Table one.
The performance comparison of one each embodiment of table
| Performance | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 |
| Tensile strength, MPa | 1700 | 1663 | 1738 | 1802 | 886 |
| Stretch modulus, GPa | 137 | 140 | 141 | 139 | 60 |
| Compressive strength, MPa | 1204 | 1043 | 1168 | 1257 | 678 |
| Compression modulus, GPa | 129 | 125 | 130 | 128 | 61 |
| Bending strength, MPa | 1401 | 1287 | 1383 | 1408 | 866 |
| Bending modulus, GPa | 126 | 121 | 128 | 126 | 60 |
| Interlaminar shear strength, MPa | 102 | 95 | 100 | 101 | 67 |
In conclusion benzoxazine colophony constituent disclosed herein and its prepreg, especially suitable for microwave curing process,
It can show well balanced between a variety of physical properties after the solidification of such constituent, especially show faster solidification
Efficiency, can solve the high energy consumption occurred in current material manufacturing process, product deformation it is big the problems such as, can be used for lid, rectification
The manufacture of the aviations rapid wear structural members such as cover.
The technical staff of industry is it should be appreciated that the present invention is not limited to the above embodiments, above embodiments and description
Described in merely illustrate the principles of the invention, without departing from the spirit and scope of the present invention, the present invention also has respectively
Kind changes and improvements, these changes and improvements all fall within the protetion scope of the claimed invention.The claimed scope of the invention by
Appended claims and its equivalent thereof.
Claims (8)
1. a kind of benzoxazine colophony constituent suitable for microwave curing process, it is characterised in that：The benzoxazine colophony
Constituent is it includes at least one benzoxazine colophony, and parts by weight are 50-70 parts, epoxy resin, parts by weight 20-50
Part, at least one carbon nano-tube material, parts by weight are 1-10 parts.
2. a kind of benzoxazine colophony constituent suitable for microwave curing process according to claim 1, feature exist
In：The benzoxazine colophony is dihydric phenol type benzoxazine colophony, naphthol type benzoxazine colophony, two amine type benzoxazine trees
One or more of fat composition.
3. a kind of benzoxazine colophony constituent suitable for microwave curing process according to claim 1, feature exist
In：The epoxy resin is alicyclic trifunctional epoxy resin 4,5- 7-oxa-bicyclo[4.1.0-1,2- dicarboxylic acid diglycidyl esters.
4. a kind of benzoxazine colophony constituent suitable for microwave curing process according to claim 1, feature exist
In：The carbon nano-tube material is one or more of single tube material or multi-wall carbon nano-tube tube material composition.
5. a kind of benzoxazine colophony constituent prepreg suitable for microwave curing process, it is characterised in that：It is wanted including right
Ask the benzoxazine colophony constituent and carbon fiber of any one of 1-4（Or carbon fibre fabric）, usual resin Composition accounts for preimpregnation
Expect that the percentage of weight is 30%-50%.
6. the preparation method of benzoxazine colophony constituent prepreg as claimed in claim 5, it is characterised in that：A. it will be made
Benzoxazine colophony constituent toast half an hour at 50-80 DEG C after, be placed on film applicator uniformly coating prepare impregnation glued membrane；
B. by glued membrane obtained and carbon fiber on pre- dipping machine（Or carbon fibre fabric）It is combined at 80-100 DEG C, 0.1-0.5MPa,
Prepreg can be obtained after covering PE films.
7. the microwave curing process of benzoxazine colophony constituent prepreg as claimed in claim 5, it is characterised in that：Specifically
Steps are as follows：
（1）After prepreg is laid in composite material mould surface according to Lay up design, periphery successively cover release cloth, isolation film,
Airfelt and vacuum bag are simultaneously sealed with vacuum rubber belt；
（2）After vacuumizing, program mode is required to adjust microwave irradiation power size according to technological procedure, and place temperature on mold
The temperature feedback of sensing device, measurement is compared to control system with process curve, ensures the controllability of solidification process；
（3）Product curing molding after a certain period of time, cooling demoulding.
8. the application of benzoxazine colophony constituent prepreg as claimed in claim 5, it is characterised in that：For aviation rapid wear
The manufacture of structural member.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810407900.6A CN108587060A (en) | 2018-05-02 | 2018-05-02 | A kind of benzoxazine colophony constituent and its prepreg suitable for microwave curing process |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810407900.6A CN108587060A (en) | 2018-05-02 | 2018-05-02 | A kind of benzoxazine colophony constituent and its prepreg suitable for microwave curing process |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113861362A (en) * | 2021-09-30 | 2021-12-31 | 中北大学 | Method for rapidly curing and simultaneously toughening benzoxazine resin |
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| CN105038224A (en) * | 2015-07-23 | 2015-11-11 | 江苏恒神股份有限公司 | Benzoxazine prepreg composite and preparation method |
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2018
- 2018-05-02 CN CN201810407900.6A patent/CN108587060A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105038224A (en) * | 2015-07-23 | 2015-11-11 | 江苏恒神股份有限公司 | Benzoxazine prepreg composite and preparation method |
Non-Patent Citations (3)
| Title |
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| 周其凤 等: "《跨世纪的高分子科学 高分子化学》", 31 October 2001, 化学工业出版社 * |
| 周冀: "《高分子材料基础》", 31 July 2007, 国防工业出版社 * |
| 张凯: "苯并噁嗪/环氧树脂基碳纳米管复合材料", 《中国优秀硕士学位论文全文数据库 工程科技I辑》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113861362A (en) * | 2021-09-30 | 2021-12-31 | 中北大学 | Method for rapidly curing and simultaneously toughening benzoxazine resin |
| CN113861362B (en) * | 2021-09-30 | 2024-01-23 | 中北大学 | Method for rapidly curing and toughening benzoxazine resin |
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Application publication date: 20180928 |