CN102634208A - Nanocomposite modification method applied to bismaleimide resin based composite - Google Patents
Nanocomposite modification method applied to bismaleimide resin based composite Download PDFInfo
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Abstract
The invention discloses a nanocomposite modification method applied to a bismaleimide resin based composite, belonging to the manufacturing field of advanced resin based composite. The method comprises the following steps of: adding N-(4-aminophenyl) bismaleimide modified phyllosilicate clay mineral to liquid O,O'-diallyl bisphenol A (DBA); performing intercalation pretreatment under the joint effect of mechanical stirring and ultrasonic dispersion; adding BDM (bismaleimide diphenylmethane) resin for pre-polymerization; cooling and adding acetone to prepare a resin solution with certain concentration; sufficiently steeping the continuous filament or fabric thereof in the resin solution, and heating to obtain prepreg; and finally preparing the hybrid multi-scale composite according to certain forming technology. By adopting the hybrid multi-scale composite obtained by the method disclosed by the invention, the synergistic effect of inorganic nanosheet layer and micron fiber can be effectively realized, and the comprehensive perforamnce of the bismaleimide resin based composite is further improved.
Description
Technical field: the present invention relates to a kind of method of modifying of matrix material, relate in particular to a kind of nano-compound modified method that is used for bimaleimide resin base composite material, belong to technical field of composite materials.
Background technology: bismaleimides (BMI) resin is as the main matrix resin of advanced composite material; Have good heat-resistant and mechanical property; And overcome the shortcoming that the epoxy resin thermotolerance is relatively low with fire resistant polyimide resin forming temperature is high, pressure is big, obtained in recent years developing rapidly and widespread use.But it is big that its main deficiency of unmodified BMI resin is self cured article fragility, must be through toughening modifying.
Use O, 4,4 of O '-diallyl bisphenol (DBA) modification '-dimaleoyl imino ditane (BDM) resin system obtained good toughening effect, the widespread use in engineering of its fibre composite.Yet; Though can significantly improve the toughness of resin with the BMI of DBA modification, but still can not reach the level of H.T. resin, and the existence of sec.-propyl has reduced its thermostability in the DBA molecule; At high temperature be prone to decompose, therefore limited the performance of its composite property to a certain extent.
Utilize layered silicate clay mineral pair resin matrix to carry out modification, under clay mineral addition situation seldom, the intensity of resin matrix, toughness and thermotolerance etc. all can be improved significantly.Just because of this, with lamella silicate modified bimaleimide resin base body and fiber composite, preparation hybrid multi-dimension matrix material, the synergy with performance inorganic nano lamella and micrometer fibers can further improve performance of composites.
Clay mineral is a large amount of mineral ions because of interlayer contains, and organic cpds is thin property, and processing need organise.Yet; Adopt common properties-correcting agent such as chain alkyl ammonium salt that clay is carried out finishing; To itself have superior heat resistance can resin be disadvantageous because this type properties-correcting agent thermotolerance is relatively poor, and is difficult to take place chemical reaction with the functional group of matrix resin and generates covalent linkage; At high temperature can at first decompose the interface interaction power that has weakened between layered silicate and the resin, thereby influence the relevant performance of modified resin to a certain extent.
" nanometer composite double maleimide resin and preparation method thereof " (patent No. is 02123693.3) of Beijing Research Inst. of Aeronautic Material's application discloses a kind of nano combined bimaleimide resin that is applicable to; And in this bimaleimide resin, fill the nanometer composite technology of nano material and the preparation method of matrix material thereof; Methane type BMI monomer, diallyl bisphenol and chavicol are mixed by the ratio of component weighing; Add nanoparticle; Through technologies such as pressurization, intensification, heat preservation solidification, obtain the matrix material of nano-dispersed.The disclosed just preparation of this patent is applicable to and nanoparticle compound bimaleimide resin base body; Do not relate to special organic modifiers, do not relate to BMI resin matrix and fiber composite after the modification yet to the used layered silicate clay mineral of bimaleimide resin.
Summary of the invention
The present invention strengthens O in order further to improve continuous fibre or fabric; The mechanical property and the resistance toheat of O '-diallyl bisphenol (DBA) modified bismaleimide resin based composites, and the preparation method of organise layered silicate clay mineral and the common enhanced hybrid multi-dimension of the fiber matrix material that provide.
For realizing above-mentioned purpose; The technical scheme that the present invention adopts is: a kind of nano-compound modified method that is used for bimaleimide resin base composite material; Its step is following: the layered silicate clay mineral that organise of N-(4-aminophenyl) maleimide modification are joined O; In O '-diallyl bisphenol, under mechanical stirring and ultrasonication, carry out preparatory intercalation.Contain phenyl ring and maleimide ring in the properties-correcting agent of clay mineral, good heat resistance, and also maleimide ring wherein can have an effect with the allyl group among the DBA, helps clay mineral peeling off in resin.Add dimaleoyl imino ditane resin then and carry out pre-polymerization, after the stirring cooling, add acetone and be mixed with resin solution.Make continuous fibre or fabric again after this resin solution fully floods; Utilize drying plant to add the heat extraction solvent and obtain prepreg; Further be stripped from moulding process laminate silicate at last, be dispersed in the resin matrix, obtain the hybrid multi-dimension matrix material with nanoscale.
The described layered silicate clay mineral that organise are meant polynite, rectorite leng or sepiolite etc. through organic modification.
Described continuous fibre is meant thomel, spun glass, aramid fiber or pbo fiber, and fabric is the plain that forms of above-mentioned fibrage or drills etc.
Described moulding is meant compression molding, autoclave molding or method such as Wrapping formed.
The beneficial effect that the present invention reached is: strengthen O at continuous fibre or fabric; O '-diallyl bisphenol (DBA)/4; 4 '-dimaleoyl imino ditane (BDM) composite system in; After introducing N-(4-aminophenyl) maleimide modified layered silicate clay mineral, the flexural strength of matrix material and interlaminar shear strength improve 20-60% respectively, interlayer faults toughness (G
IC) improving 50-100%, heat decomposition temperature improves 10-20 ℃.The bimaleimide resin base hybrid multi-dimension matrix material that makes, excellent combination property has broad application prospects.
Embodiment
Embodiment 1
Under 80-140 ℃ oil bath condition, the organic montmorillonoid of N-(4-aminophenyl) maleimide modification is joined O, among the O '-diallyl bisphenol (DBA); Behind the mechanical stirring 0.5h; Carry out the supersound process of 1-1.5h, the power of supersound process is 100-800W, and frequency is 20-45Hz.Add dimaleoyl imino ditane (BDM) resin then and carry out the pre-polymerization of 0.5h; The amount of substance of DBA and BDM is than being 0.85-1.15: 1; The consumption of organic montmorillonoid is the 1-10% of resin quality; After the cooling, add acetone and be mixed with the resin solution that mass percent concentration is 10-35%.Then, make continuous carbon fibre or its fabric after this resin solution fully floods, heating obtains prepreg, after die press technology for forming prepares the hybrid multi-dimension matrix material.
The flexural strength of gained hybrid multi-dimension matrix material, interlaminar shear strength and interlayer faults toughness are respectively 1976MPa, 121MPa and 275J/m
2, compare the matrix material that does not add organo montmorillonite, flexural strength, interlaminar shear strength and interlayer faults toughness improve 26.2%, 32.5% and 81.5% respectively; Heat decomposition temperature is 437 ℃, improves 19 ℃.
Embodiment 2
The difference of present embodiment and embodiment 1 is: used layer silicate mineral is the rectorite leng that organises.
Embodiment 3
The difference of present embodiment and embodiment 1 is: used layer silicate mineral is the sepiolite that organises.
Embodiment 4
The difference of present embodiment and embodiment 1 is: used fiber is a spun glass.
Embodiment 5
The difference of present embodiment and embodiment 1 is: used fiber is an aramid fiber.
Embodiment 6
The difference of present embodiment and embodiment 1 is: used fiber is a pbo fiber.
Embodiment 7
The difference of present embodiment and embodiment 1 is: used forming method is an autoclave technology.
Embodiment 8
The difference of present embodiment and embodiment 1 is: used forming method is a winding process.
Claims (5)
1. nano-compound modified method that is used for bimaleimide resin base composite material; Its step is following: the layered silicate clay mineral that organise of N-(4-aminophenyl) maleimide modification are joined O; In O '-diallyl bisphenol, under mechanical stirring and ultrasonication, carry out preparatory intercalation; Add dimaleoyl imino ditane resin then and carry out pre-polymerization, after the stirring cooling, add acetone and be mixed with resin solution; Make continuous fibre or fabric again after this resin solution fully floods; Utilize drying plant to add the heat extraction solvent and obtain prepreg; Further be stripped from moulding process laminate silicate at last, be dispersed in the resin matrix, obtain the hybrid multi-dimension matrix material with nanoscale.
2. a kind of nano-compound modified method that is used for bimaleimide resin base composite material as claimed in claim 1 is characterized in that: the described layered silicate clay mineral that organise are meant polynite, rectorite leng or sepiolite through organic modification.
3. a kind of nano-compound modified method that is used for bimaleimide resin base composite material as claimed in claim 1; It is characterized in that: described continuous fibre is meant thomel, spun glass, aramid fiber or pbo fiber, and fabric is plain or the drills that above-mentioned fibrage forms.
4. a kind of nano-compound modified method that is used for bimaleimide resin base composite material as claimed in claim 1, it is characterized in that: described moulding is meant compression molding, autoclave molding or Wrapping formed.
5. a kind of nano-compound modified method that is used for bimaleimide resin base composite material as claimed in claim 1; It is characterized in that: under 80-140 ℃ oil bath condition, the organic montmorillonoid of N-(4-aminophenyl) maleimide modification is joined O, in O '-diallyl bisphenol; Behind the mechanical stirring 0.5h; Carry out the supersound process of 1-1.5h, the power of supersound process is 100-800W, and frequency is 20-45Hz; Add dimaleoyl imino ditane resin then and carry out the pre-polymerization of 0.5h, the amount of substance of DBA and BDM is than being 0.85-1.15: 1, and the consumption of organic montmorillonoid is the 1-10% of resin quality; After the cooling; Add acetone and be mixed with the resin solution that mass percent concentration is 10-35%, then, make continuous carbon fibre or its fabric after this resin solution fully floods; Heating obtains prepreg, after die press technology for forming prepares the hybrid multi-dimension matrix material.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103881379A (en) * | 2014-03-20 | 2014-06-25 | 西北工业大学 | Hydroxyl silicate/phosphorus-containing benzoxazine/bismaleimide resin composite material and preparation method thereof |
| CN103881297A (en) * | 2012-12-20 | 2014-06-25 | 南京理工大学 | Thermosetting resin-based composite material and preparation method thereof |
| CN103881298A (en) * | 2012-12-20 | 2014-06-25 | 南京理工大学 | Thermosetting resin composite material with electricity and heat conduction functions, and preparation method thereof |
| CN107057288A (en) * | 2017-05-22 | 2017-08-18 | 安徽三义和能源科技有限公司 | A kind of preparation method of Pressure-resistant fireproof plate |
| CN107325439A (en) * | 2017-07-03 | 2017-11-07 | 安徽真劲智能科技有限公司 | Ventilation dustproof additive is used in a kind of silica gel protected shell processing of smart electronicses product |
| CN109306148A (en) * | 2017-07-27 | 2019-02-05 | 宁德时代新能源科技股份有限公司 | Heat diffusion-proof resin composite material, preparation method thereof and battery module |
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| CN1467231A (en) * | 2002-07-09 | 2004-01-14 | 北京航空材料研究院 | Nanometer composite double maleimide resin and method for preparing the same |
| CN1978518A (en) * | 2005-11-29 | 2007-06-13 | 西北工业大学 | Carbon fiber reinforced bismalemide resin base composite material, and its preparing method |
| CN101532243A (en) * | 2009-04-20 | 2009-09-16 | 沈阳航空工业学院 | Shaping agent for nano composite reinforced fabric and application thereof |
| US20090229868A1 (en) * | 2008-03-12 | 2009-09-17 | Ibiden Co., Ltd. | Printed wiring board with reinforced insulation layer and manufacturing method thereof |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1467231A (en) * | 2002-07-09 | 2004-01-14 | 北京航空材料研究院 | Nanometer composite double maleimide resin and method for preparing the same |
| CN1978518A (en) * | 2005-11-29 | 2007-06-13 | 西北工业大学 | Carbon fiber reinforced bismalemide resin base composite material, and its preparing method |
| US20090229868A1 (en) * | 2008-03-12 | 2009-09-17 | Ibiden Co., Ltd. | Printed wiring board with reinforced insulation layer and manufacturing method thereof |
| CN101532243A (en) * | 2009-04-20 | 2009-09-16 | 沈阳航空工业学院 | Shaping agent for nano composite reinforced fabric and application thereof |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103881297A (en) * | 2012-12-20 | 2014-06-25 | 南京理工大学 | Thermosetting resin-based composite material and preparation method thereof |
| CN103881298A (en) * | 2012-12-20 | 2014-06-25 | 南京理工大学 | Thermosetting resin composite material with electricity and heat conduction functions, and preparation method thereof |
| CN103881379A (en) * | 2014-03-20 | 2014-06-25 | 西北工业大学 | Hydroxyl silicate/phosphorus-containing benzoxazine/bismaleimide resin composite material and preparation method thereof |
| CN103881379B (en) * | 2014-03-20 | 2016-05-18 | 西北工业大学 | Hydroxy silicate/phosphorous benzoxazine/bismaleimide resin composite material and preparation method thereof |
| CN107057288A (en) * | 2017-05-22 | 2017-08-18 | 安徽三义和能源科技有限公司 | A kind of preparation method of Pressure-resistant fireproof plate |
| CN107325439A (en) * | 2017-07-03 | 2017-11-07 | 安徽真劲智能科技有限公司 | Ventilation dustproof additive is used in a kind of silica gel protected shell processing of smart electronicses product |
| CN109306148A (en) * | 2017-07-27 | 2019-02-05 | 宁德时代新能源科技股份有限公司 | Heat diffusion-proof resin composite material, preparation method thereof and battery module |
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