CN104893654A - Novel flame-retardant composite solid material - Google Patents
Novel flame-retardant composite solid material Download PDFInfo
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Abstract
The invention relates to a novel flame-retardant composite solid material which is reasonable in composition and high in compatibility among components; therefore, the prepared novel flame-retardant composite solid material is better in mechanical property, adhesive property and heat resistance, especially excellent in flame retardation, and can meet demands in development and application of novel flame-retardant composite solid material; a preparation method disclosed by the invention is wide in raw material sources, simple and controllable in preparation process; only normal operations are required, and industrialization can be achieved easily.
Description
Technical field
The invention belongs to advanced composite material technical field, be specifically related to a kind of novel flame-retardant composite solid material.
Background technology
First the development of solid glue stick starts from abroad, so far the history in existing more than 70 years.Initial solid glue stick development is the solidification of liquid-type tackiness agent, allows tackiness agent use in solid form exactly.Deepening continuously and developing along with research, also regenerates in continuous renewal as bonding tackiness agent.Through the development of decades, the investigation and application technology comparative maturity of external solid glue stick, some companies have the solid gums product-feed of the multiple trade mark.
so-called polymer is often referred to the macromolecular cpd connect with chemical bond by ten million micromolecular compound.Commodity polymer material is divided into the 5 large classes such as plastics, rubber, fiber, tackiness agent, coating.Matrix material is the heterogeneous material prepared through recombining process by two or more the material such as metallic substance, stupalith or macromolecular material, various material makes up for each other's deficiencies and learn from each other in performance, produce synergistic effect, make the over-all properties of matrix material be better than former composition material and meet various different requirement.Matrix material is by the matrix of external phase and formed by the phase reinforcement that matrix contains.The history that matrix material uses can trace back to ancient times.The straw continued to use from ancient times to the present or wheat straw strengthen clay and have used the Steel Concrete of a century to be composited by bi-material.The development of modern high technology be unable to do without matrix material, and matrix material, to the development of modern science and technology, has very important effect.The depth of investigation and speed and the scale of applying range and production development thereof of matrix material, become one of important symbol of a measurement national science advanced technology level.
Matrix material mainly can be divided into structural composite material and the large class of functional composite material two.Functional composite material is generally made up of functive constituent element and matrix constituent element, and matrix not only plays integrant effect, and can produce collaborative or add powerful effect.Functional composite material refers to the matrix material providing other physicalies except mechanical property.As: conduction, superconduction, partly lead, magnetic, piezoelectricity, damping, suction ripple, wave transparent, friction, shielding, fire-retardant, solar heat protection, sound absorption, heat insulation etc. highlight a certain function.Be referred to as functional composite material.Functional composite material is primarily of functive and reinforcement and matrix composition.Functive can be made up of one or more functional materialss.The matrix material of pluralistic function body can have several functions.Meanwhile, also likely new function is produced due to complex effect.Multifunctional composite is the developing direction of functional composite material.
Solid material commercially available at present adopts macromolecular material PVA and PVP to be sizing mostly, and the low and performance of tool solid glue stick of its production cost (cementability, moisture retention, embossability, is coated with the good market competitiveness.But these solid glue sticks or ubiquity perishable, thermo-labile, smear poor, the inflammable functional defect of poor performance, moisture retention.
Summary of the invention
The object of this invention is to provide a kind of novel flame-retardant composite solid material, it has excellent adhesiveproperties, particularly excellent fireproof performance.
To achieve the above object of the invention, the technical solution used in the present invention is: a kind of novel flame-retardant composite solid material, makes by after organic-inorganic composite body mold pressing, described organic-inorganic composite body is 100 by mass ratio: (7 ~ 12): (15 ~ 18): (18 ~ 22): (26 ~ 35): (18 ~ 20): (15 ~ 18): (6 ~ 10): (10 ~ 12): the polydimethylsiloxane of (0.5 ~ 0.8), thiocyanogen-1-(2-aminophenyl) ethyl ketone, 2-acrylamide-2-methylpro panesulfonic acid, cyanate ester resin prepolymer, epoxy prepolymer, silicon sol, trimethylsiloxysilicates, 1, 3, 5-three-glycidyl-S-triazinetrione, Succinic anhydried, zinc nitrate hexahydrate is that raw material obtains,
The molecular weight of described polydimethylsiloxane is 3000 ~ 5000;
Described cyanate ester resin prepolymer molecular weight is 2800 ~ 3600;
Described epoxy prepolymer molecular weight is 6800 ~ 8500.
In the present invention, cyanate ester resin is bisphenol A cyanate ester resin, bonding, reactive good; Epoxy resin is four-functional group epoxy resin, such as AG-80 or JD-919, and thermotolerance is better, reactive strong, good stability.
In the present invention, the solid content of silicon sol is 25 ~ 30%; The particle diameter of silicon-dioxide is 100 ~ 230 nanometers; The particle diameter of zinc nitrate hexahydrate is 200 ~ 330 nanometers.Silicon sol is not only beneficial to the dispersion of system, increases the normal temperature cementability of adhesive joint between solid material, works in coordination with zinc nitrate hexahydrate, heat can also be absorbed when burning produces high temperature, prevent adhesive failure, increase the reactivity of each organic constituent of system simultaneously, improve the over-all properties of adhesive joint between solid material.
Preferably, described organic-inorganic composite body is 100 by mass ratio: (9 ~ 10): 17: (20 ~ 21): (29 ~ 32): (18 ~ 20): (17 ~ 18): (7 ~ 8): (10 ~ 12): the polydimethylsiloxane of (0.5 ~ 0.6), thiocyanogen-1-(2-aminophenyl) ethyl ketone, 2-acrylamide-2-methylpro panesulfonic acid, cyanate ester resin prepolymer, epoxy prepolymer, silicon sol, trimethylsiloxysilicates, 1, 3, 5-three-glycidyl-S-triazinetrione, Succinic anhydried, zinc nitrate hexahydrate is that raw material obtains.
In the present invention, organic object is the primary bond composition of adhesive joint between solid material, is also the key ingredient of system heat-proof combustion-resistant simultaneously; The molecular weight of polydimethylsiloxane is 3000 ~ 5000, cyanate ester resin prepolymer molecular weight is 2800 ~ 3600, epoxy prepolymer molecular weight is 6800 ~ 8500, the bonding force that molecular weight shows for adhesive joint between solid material has material impact, in particular concerns cementability in the combustion environment after the solidification of adhesive joint between solid material; Molecular weight too low then filmogen rate of drying is comparatively slow, and high resin system consistency is not good.Organic-compound system of the present invention not only has the function of effectively solidification at normal temperatures, and can not melt during high temperature and cause adhesive failure, and the adhesives particularly after solidification can not be subject to thermal failure in the combustion environment, has good flame retardant effect.
In the present invention, 2-acrylamide-2-methylpro panesulfonic acid, trimethylsiloxysilicates, 1,3,5-three-glycidyl-S-triazinetrione are reactive good organism, these organism make each component stable dispersion by space stability ultimate load effect, reach good com-patibilising effect; In the reaction process preparing adhesives, each component can be connected, form good toughness, have the solid phase prod of certain cross-linking density.
In the present invention, by cyanate resin alicyclic monomer in 105 DEG C of reactions 10 ~ 15 minutes, obtain cyanate ester resin prepolymer; By epoxy monomer in 160 DEG C of reactions 35 ~ 40 minutes, obtain epoxy prepolymer.
Inserted by organic-inorganic composite body in mould, mold pressing (pressure is 0.2 ~ 0.3MPa), namely obtains flame retarding solid adhesives; Preferably, molding temperature is 50 DEG C.
Because technique scheme is used, the present invention compared with prior art has following advantages:
1. the organic-inorganic composite body that the present invention utilizes forms rationally, between each component, consistency is good, prepare novel flame-retardant composite solid material thus, there is good mechanical property, adhesiveproperties, resistance toheat, there is excellent flame retardant properties especially, meet the development and application of novel flame-retardant composite solid material.
2. novel flame-retardant composite solid material disclosed by the invention can form finer and close protective layer when being heated and burn, reach excellent hot oxygen shielding effect, thus give thermotolerance and the flame retardant resistance of adhesive joint between solid material excellence, mechanical property, adhesiveproperties are good simultaneously; Overcome a difficult problem for bonding decline that prior art filler fire retardant brings and the mechanical properties decrease that reactive flame retardant brings, heat-resisting decline.
3. disclosed by the inventionly prepare in novel flame-retardant composite solid material raw material, raw material is simple and easy to get, without the need to the complex reaction of prior art, the novel flame-retardant composite solid material of preparation has excellent adhesiveproperties, the solidification of normal temperature lower part organism fully, solidification effect is good, by such as cyanate, the heat resistive compounds segments such as epoxy resin tangle, be wrapped in polymer segment, when being heated, silicon sol and the slow dehydration of zinc nitrate hexahydrate, catalyzing organic (cyanate, epoxy resin) react further, form stable structure, thus further increase the flame retardant resistance of system, ensure high temperature bonding stability simultaneously, achieve beyond thought effect.
Embodiment
Below in conjunction with embodiment, the invention will be further described:
Embodiment one
By bisphenol A cyanate ester resin monomer in 105 DEG C of reactions 10 minutes, obtain cyanate ester resin prepolymer (molecular weight is 2800 ~ 3200); By epoxy resin AG-80 monomer in 160 DEG C of reactions 35 minutes, obtain epoxy prepolymer (molecular weight is 6800 ~ 7500); By 19g silicon sol, (solid content is 28%; The particle diameter of silicon-dioxide is 100 ~ 160 nanometers), 17g trimethylsiloxysilicates, 7g1,3,5-three-glycidyl-S-triazinetrione mixes 2 hours, obtains mixture; Successively by 9g thiocyanogen-1-(2-aminophenyl) ethyl ketone, 17g2-acrylamide-2-methylpro panesulfonic acid add in mixture, and stir 1.1 hours, then add 10g Succinic anhydried, 0.5g zinc nitrate hexahydrate, stir 2 hours in 50 DEG C; Finally add 100g polydimethylsiloxane (molecular weight 3000 ~ 4000), 20g cyanate ester resin prepolymer, 30g epoxy prepolymer, stir 1.5 hours in 80 DEG C, obtain organic-inorganic composite body; Insert in mould by organic-inorganic composite body again, (molding pressure is 0.2MPa in mold pressing; Molding temperature is 50 DEG C), namely obtain solid composite bonding material.
Embodiment two
By bisphenol A cyanate ester resin monomer in 105 DEG C of reactions 15 minutes, obtain cyanate ester resin prepolymer (molecular weight is 3000 ~ 3600); By epoxy resin AG-80 monomer in 160 DEG C of reactions 40 minutes, obtain epoxy prepolymer (molecular weight is 7800 ~ 8500); By 20g silicon sol, (solid content is 30%; The particle diameter of silicon-dioxide is 150 ~ 230 nanometers), 17g trimethylsiloxysilicates, 8g1,3,5-three-glycidyl-S-triazinetrione mixes 3 hours, obtains mixture; Successively by 9g thiocyanogen-1-(2-aminophenyl) ethyl ketone, 17g2-acrylamide-2-methylpro panesulfonic acid add in mixture, and stir 1.5 hours, then add 11g Succinic anhydried, 0.5g zinc nitrate hexahydrate, stir 3 hours in 50 DEG C; Finally add 100g polydimethylsiloxane (molecular weight 3000 ~ 4000), 21g cyanate ester resin prepolymer, 32g epoxy prepolymer, stir 2 hours in 80 DEG C, obtain organic-inorganic composite body; Insert in mould by organic-inorganic composite body again, (molding pressure is 0.2MPa in mold pressing; Molding temperature is 50 DEG C), namely obtain solid composite bonding material.
Embodiment three
By bisphenol A cyanate ester resin monomer in 105 DEG C of reactions 15 minutes, obtain cyanate ester resin prepolymer (molecular weight is 3000 ~ 3600); By epoxy resin JD-919 monomer in 160 DEG C of reactions 40 minutes, obtain epoxy prepolymer (molecular weight is 7300 ~ 8200); 20g silicon sol, 15g trimethylsiloxysilicates, 6g1,3,5-three-glycidyl-S-triazinetrione are mixed 2.5 hours, obtains mixture; Successively by 7g thiocyanogen-1-(2-aminophenyl) ethyl ketone, 18g2-acrylamide-2-methylpro panesulfonic acid add in mixture, and stir 2 hours, then add 10g Succinic anhydried, 0.8g zinc nitrate hexahydrate, stir 2 hours in 60 DEG C; Finally add 100g polydimethylsiloxane (molecular weight 3000 ~ 4000), 22g cyanate ester resin prepolymer, 35g epoxy prepolymer, stir 2 hours in 90 DEG C, obtain organic-inorganic composite body; Insert in mould by organic-inorganic composite body again, (molding pressure is 0.3MPa in mold pressing; Molding temperature is 50 DEG C), namely obtain solid composite bonding material.
Embodiment four
By bisphenol A cyanate ester resin monomer in 105 DEG C of reactions 12 minutes, obtain cyanate ester resin prepolymer (molecular weight is 2900 ~ 3300); By epoxy resin JD-919 monomer in 160 DEG C of reactions 38 minutes, obtain epoxy prepolymer (molecular weight is 7000 ~ 8000); 18g silicon sol, 18g trimethylsiloxysilicates, 10g1,3,5-three-glycidyl-S-triazinetrione are mixed 3 hours, obtains mixture; Successively by 11g thiocyanogen-1-(2-aminophenyl) ethyl ketone, 15g2-acrylamide-2-methylpro panesulfonic acid add in mixture, and stir 1 hour, then add 12g Succinic anhydried, 0.5g zinc nitrate hexahydrate, stir 2 hours in 60 DEG C; Finally add 100g polydimethylsiloxane (molecular weight 3500 ~ 4800), 18g cyanate ester resin prepolymer, 33g epoxy prepolymer, stir 1.5 hours in 90 DEG C, obtain organic-inorganic composite body; Insert in mould by organic-inorganic composite body again, (molding pressure is 0.3MPa in mold pressing; Molding temperature is 50 DEG C), namely obtain solid composite bonding material.
Embodiment five
By bisphenol A cyanate ester resin monomer in 105 DEG C of reactions 15 minutes, obtain cyanate ester resin prepolymer (molecular weight is 3000 ~ 3600); By epoxy resin JD-919 monomer in 160 DEG C of reactions 40 minutes, obtain epoxy prepolymer (molecular weight is 7300 ~ 8200); 20g silicon sol, 18g trimethylsiloxysilicates, 8g1,3,5-three-glycidyl-S-triazinetrione are mixed 3 hours, obtains mixture; Successively by 9g thiocyanogen-1-(2-aminophenyl) ethyl ketone, 17g2-acrylamide-2-methylpro panesulfonic acid add in mixture, and stir 2 hours, then add 120g Succinic anhydried, 0.6g zinc nitrate hexahydrate, stir 2 hours in 60 DEG C; Finally add 100g polydimethylsiloxane (molecular weight 4000 ~ 5000), 20g cyanate ester resin prepolymer, 30g epoxy prepolymer, stir 1.8 hours in 90 DEG C, obtain organic-inorganic composite body; Insert in mould by organic-inorganic composite body again, (molding pressure is 0.3MPa in mold pressing; Molding temperature is 50 DEG C), namely obtain solid composite bonding material.
Comparative example one
By bisphenol A cyanate ester resin monomer in 105 DEG C of reactions 30 minutes, obtain cyanate ester resin prepolymer (molecular weight is 6000 ~ 7600); By epoxy resin JD-919 monomer in 160 DEG C of reactions 55 minutes, obtain epoxy prepolymer (molecular weight is 10300 ~ 11200); 20g silicon sol, 18g trimethylsiloxysilicates, 8g1,3,5-three-glycidyl-S-triazinetrione are mixed 3 hours, obtains mixture; Successively by 9g thiocyanogen-1-(2-aminophenyl) ethyl ketone, 17g2-acrylamide-2-methylpro panesulfonic acid add in mixture, and stir 2 hours, then add 120g Succinic anhydried, 0.6g zinc nitrate hexahydrate, stir 2 hours in 60 DEG C; Finally add 100g polydimethylsiloxane (molecular weight 12000 ~ 15000), 20g cyanate ester resin prepolymer, 30g epoxy prepolymer, stir 1.8 hours in 90 DEG C, obtain organic-inorganic composite body; Insert in mould by organic-inorganic composite body again, (molding pressure is 0.3MPa in mold pressing; Molding temperature is 50 DEG C), namely obtain solid composite bonding material.
Comparative example two
By bisphenol A cyanate ester resin monomer in 105 DEG C of reactions 15 minutes, obtain cyanate ester resin prepolymer (molecular weight is 3000 ~ 3600); By epoxy resin JD-919 monomer in 160 DEG C of reactions 40 minutes, obtain epoxy prepolymer (molecular weight is 7300 ~ 8200); By 18g trimethylsiloxysilicates, 8g1,3,5-three-glycidyl-S-triazinetrione mixes 3 hours, obtains mixture; 17g2-acrylamide-2-methylpro panesulfonic acid is added in mixture, stirs 2 hours, then add 120g Succinic anhydried, stir 2 hours in 60 DEG C; Finally add 100g polydimethylsiloxane (molecular weight 4000 ~ 5000), 20g cyanate ester resin prepolymer, 30g epoxy prepolymer, stir 1.8 hours in 90 DEG C, obtain organic-inorganic composite body; Insert in mould by organic-inorganic composite body again, (molding pressure is 0.3MPa in mold pressing; Molding temperature is 50 DEG C), namely obtain solid composite bonding material.
Performance test
Utilize dimension card thermal distortion instrument test heat-drawn wire (CTE/ DEG C); Electronic universal tester is utilized to test flexural strength (Rt/MPa); Liquid crystal type balance weight impact testing machine is utilized to test shock strength (α/KJ/m
2); Oxygen index tester is utilized to measure oxygen index; Adopt dynamic mechanical test instrument test storage modulus (E/MPa(35 DEG C)); Utilize 3M 600 adhesive tape, drawing coating test sticking power; In 150 heating 2 minutes, test sticking power R; Hot weightless instrument is utilized to test temperature of initial decomposition (T
0/ DEG C).
The performance test results of above-mentioned composite solid adhesives is in table 1.
The performance of table 1 composite solid material
| CTE | Oxygen index | α | Rt | Sticking power | Sticking power R | E | T 0 | |
| Embodiment one | 189 | 28.4 | 3.9457 | 65 | >5B | 5B | 880 | 387 |
| Embodiment two | 180 | 28.1 | 3.9397 | 65 | >5B | 5B | 870 | 369 |
| Embodiment three | 186 | 29.6 | 3.6221 | 64 | >5B | 5B | 860 | 375 |
| Embodiment four | 191 | 29.5 | 3.7845 | 66 | >5B | 5B | 865 | 381 |
| Embodiment five | 190 | 29.7 | 3.8841 | 65 | >5B | 5B | 859 | 379 |
| Comparative example one | 120 | 24.3 | 2.1456 | 41 | 4B | - | 721 | 257 |
| Comparative example two | 118 | 24.1 | 2.1324 | 35 | 4B | - | 701 | 231 |
The above results shows novel flame-retardant composite solid material of the present invention composition rationally, and each component Harmony is good, system excellent combination property; Composite solid adhesives entirety of the present invention is not brominated, iodine, fluorine and chlorine, meets EN61249-2-21(fluorine, chlorine, bromine, iodine≤900ppm or mg/kg, chlorine+bromine≤1500 ppm or mg/kg) Halogen-free requirement that specifies of standard; There is good oxidation-resistance, resistance toheat, there is excellent mechanical property, flame retardant properties especially, meet the development and application of composite solid adhesives.
Claims (8)
1. a novel flame-retardant composite solid material, is characterized in that: be made up of organic-inorganic composite body mold pressing, described organic-inorganic composite body is 100 by mass ratio: (7 ~ 12): (15 ~ 18): (18 ~ 22): (26 ~ 35): (18 ~ 20): (15 ~ 18): (6 ~ 10): (10 ~ 12): the polydimethylsiloxane of (0.5 ~ 0.8), thiocyanogen-1-(2-aminophenyl) ethyl ketone, 2-acrylamide-2-methylpro panesulfonic acid, cyanate ester resin prepolymer, epoxy prepolymer, silicon sol, trimethylsiloxysilicates, 1, 3, 5-three-glycidyl-S-triazinetrione, Succinic anhydried, zinc nitrate hexahydrate is that raw material obtains,
The molecular weight of described polydimethylsiloxane is 3000 ~ 5000;
Described cyanate ester resin prepolymer molecular weight is 2800 ~ 3600;
Described epoxy prepolymer molecular weight is 6800 ~ 8500.
2. novel flame-retardant composite solid material according to claim 1, is characterized in that: described cyanate ester resin is bisphenol A cyanate ester resin; Epoxy resin is four-functional group epoxy resin.
3. novel flame-retardant composite solid material according to claim 1, is characterized in that: described molding pressure is 0.2 ~ 0.3MPa; Molding temperature is 50 DEG C.
4. novel flame-retardant composite solid material according to claim 1, is characterized in that: the solid content of described silicon sol is 25 ~ 30%; The particle diameter of silicon-dioxide is 100 ~ 230 nanometers.
5. novel flame-retardant composite solid material according to claim 1, it is characterized in that: described organic-inorganic composite body is 100 by mass ratio: (9 ~ 10): 17: (20 ~ 21): (29 ~ 32): (18 ~ 20): (17 ~ 18): (7 ~ 8): (10 ~ 12): the polydimethylsiloxane of (0.5 ~ 0.6), thiocyanogen-1-(2-aminophenyl) ethyl ketone, 2-acrylamide-2-methylpro panesulfonic acid, cyanate ester resin prepolymer, epoxy prepolymer, silicon sol, trimethylsiloxysilicates, 1, 3, 5-three-glycidyl-S-triazinetrione, Succinic anhydried, zinc nitrate hexahydrate is that raw material obtains.
6. novel flame-retardant composite solid material according to claim 1, is characterized in that: described cyanate ester resin prepolymer is obtained in 105 DEG C of reactions by cyanate resin alicyclic monomer for 10 ~ 15 minutes.
7. novel flame-retardant composite solid material according to claim 1, is characterized in that: described epoxy prepolymer is obtained in 160 DEG C of reactions by epoxy monomer for 35 ~ 40 minutes.
8. novel flame-retardant composite solid material according to claim 1, is characterized in that: the particle diameter of described zinc nitrate hexahydrate is 200 ~ 330 nanometers.
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Cited By (1)
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| CN108093614A (en) * | 2017-12-13 | 2018-05-29 | 江西伟普科技有限公司 | A kind of preparation method that there is sound insulation to inhale ripple heat-insulating environment-protection type composite material |
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Application publication date: 20150909 |