CN104109345A - Preparation method of modified nano-composite structure silicon dioxide toughened epoxy resin - Google Patents
Preparation method of modified nano-composite structure silicon dioxide toughened epoxy resin Download PDFInfo
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- CN104109345A CN104109345A CN201310134750.3A CN201310134750A CN104109345A CN 104109345 A CN104109345 A CN 104109345A CN 201310134750 A CN201310134750 A CN 201310134750A CN 104109345 A CN104109345 A CN 104109345A
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Abstract
The invention discloses a preparation method of modified nano-composite structure silicon dioxide toughened epoxy resin and belongs to the technical field of modification of an epoxy resin material. The material employs epoxy resin as a base material and is prepared by adding modified nano-composite structure silicon dioxide, as a toughening agent and a curing agent, and other additives. The modified nano-composite structure silicon dioxide is a novel nano-metered organic/inorganic composite toughening agent which is prepared by preparing nano-composite structure silicon dioxide and carrying out a graft modification process to the nano-composite structure silicon dioxide with a dendritic polymer, wherein the dendritic polymer accounts for 10%-30% of the toughening agent and the modified nano-composite structure silicon dioxide toughening agent accounts for 0.05-0.5% by weight of the resin. By means of the toughened epoxy resin material in the invention, various mechanical properties of a conventional epoxy resin material are greatly increased. Tensile yield strength, bending strength and notch impact strength and the like are all increased by 3-10 times. In addition, the toughened epoxy resin is low in raw material cost, is little in a usage amount of the toughening agent, is suitable for industrial production and has a wide market prospect.
Description
Technical field
The invention belongs to epoxide resin material modification technology field.Be specifically related to the preparation method by the epoxy resin toughened material of modified Nano composite structure silicon-dioxide, wherein toughner is the compound toughner of a kind of novel nano organic-inorganic.
Technical background
Epoxy resin has good physics, chemical property, it has excellent bonding strength to the surface of metal and non-metallic material, dielectric properties are good, set shrinking percentage is little, product size good stability, and hardness is high, snappiness is better, to alkali and most of solvent-stable, thereby be widely used in national defence, each department of national economy, pour into a mould, the purposes such as dipping, lamination material, caking agent, coating.Along with the raising of people to the requirement of epoxide resin material character.Add various auxiliary agents in order to improve the various mechanical properties of epoxide resin material.Wherein improving toughness reinforcing performance is the emphasis of research.
Main rubber elastomer, rigid particles, thermoplastic resin, liquid crystalline polymers and the core one shell structure polymkeric substance of adopting carries out toughness reinforcing to epoxy resin at present.
1. rubber elastomer is toughness reinforcing: as far back as the sixties in 20th century, with carboxyl end of the liquid acrylonitrile-butadiene rubber (CTBN), epoxy resin has been carried out to study on the modification, obtained good effect.Its toughening mechanism mainly contains partial cut surrender, the epoxy matrix Hole that comes off caused of rubber grain inner cavity or particle or the plasticity volumetric expansion in hole, and crackle is 3 kinds of the bridgings at rubber grain place etc.At present mainly there is active end group fluid rubber for epoxy resin toughened elastomerics, as carboxy terminated polybutadiene (CTPB), nbr carboxyl terminal (CTBN), hydroxy-terminated polybutadienes (HTPB), hydroxy'terminated butadiene nitrile rubber (HTBN); Silicone elastomer; Urethane etc.Be a feasible modification approach although active end group fluid rubber is epoxy resin toughened, price comparison costliness is mainly applied at present in war industry, in also not mass-producing use of civil area.HTBN fluid rubber price is relatively cheap, and good with epoxy resin compatibility, toughening effect and CTBN are suitable, by further improvement performance, is expected to play a significant role in epoxy resin modification.Also have in addition silicone elastomer toughness reinforcing, polyurethane toughened etc.
2. Rigid Particles Toughened: in epoxy resin-base, add after rigid particles, during due to rigid particles generation plastic deformation, can effectively suppress the expansion of matrix resin crackle, and absorption portion energy, thereby play toughening effect.Research finds it is no matter the fracture toughness property (K or G) that talcum powder that intensity is lower or the higher silicon dioxide granule of intensity can improve epoxy resin significantly.The two toughening mechanism is similar, all turns to master with matrix yielding distortion and hole.In addition, aluminum oxide, nano titanium oxide also has good toughness reinforcing performance.
3. Toughened With High Performance Thermoplastics: tend to make modulus and the decline of cured article with Toughened Epoxy Resin by Elastomer, and not obvious to highly cross-linked system toughening effect.Since the eighties in 20th century, become a new focus with High performance plastic resin is epoxy resin toughened.Thermoplastic resin has the features such as the high and good heat resistance of good toughness, modulus, joins in epoxy resin-base, can not only improve the toughness of epoxy resin, and not affect modulus and the thermotolerance of curable epoxide thing.At present mainly contain polyethersulfone (PES), polysulfones (PSF), polyetherimide (PEI), polyimide (PI), polycarbonate (PC), polyphenylene oxide (PPO), polyether-ether-ketone etc. for epoxy resin toughened thermoplastic resin.
4. liquid crystalline polymers is toughness reinforcing: since the nineties in 20th century, and the epoxy resin toughened extensive concern that causes of liquid crystalline polymers (LCP).TLCP (TLCP) has the feature of high strength, high-modulus, and it can form filamentary structure while being subject to shear action during the course, produces height self-strengthening.Therefore, can improve greatly toughness, modulus and the thermotolerance of epoxy resin with a small amount of high-performance TLCP modified epoxy.The major cause that toughness improves is in macromolecular chain, to contain the mesomorphic unit of a large amount of rigidity; The liquid crystalline polymers of flexible spacer section, in improving epoxy matrix ductility, is dispersed in the form of particle or fento the energy-to-break that improves material in epoxy matrix again.
5. nuclear-structure polymer shell is toughness reinforcing: nucleusYishellcopolymer is a kind of polymer composite particle with unique texture, and the letex polymerization of general employing substep makes.Its core is rubber, gives goods tensile property, and shell is the plastics that have compared with high glass transition temperature, and major function is that particulate is isolated mutually.Promote the interaction between dispersion and increase and the matrix resin in matrix.Studied with core-shell structure particle PBA/PS, PBA/PMMA and the PBA/P (MMA-AA) of different shells epoxy resin toughenedly, toughening effect is better; P (MMAAA) shell that contains active group one COOH, can with epoxy group(ing) generation chemical reaction, therefore shearing resistance and stripping strength are all very high.
If obtain high epoxy resin toughened of good toughness, rigidity, it is very necessary adopting composite toughing agent or toughness reinforcing enhancing Composite technology.The present invention adopts modified Nano composite structure silicon-dioxide as toughner, and this is the compound toughner of a kind of organic-inorganic, and its advantage is that consumption is few, the various mechanical property excellences of gained epoxide resin material.
Summary of the invention
The object of this invention is to provide a kind of toughness reinforcing epoxide resin material of nanometer of mechanical property excellence.In the case of using the toughner of seldom measuring, can reach good toughening effect.With low cost, technique is simple, is applicable to suitability for industrialized production.
The present invention can be achieved through the following technical solutions: a kind of by epoxy resin toughened material of modified Nano composite structure silicon-dioxide and preparation method thereof, it is characterized in that: it comprises following raw material, epoxy resin, modified Nano composite structure silicon-dioxide toughner, auxiliary agent and solidifying agent.By modified Nano composite structure silicon-dioxide toughner, auxiliary agent and epoxy resin are blended in stirring at room temperature 1-3 hour, after fully mixing, add solidifying agent to stir 5-10 minute, and then vacuumize degassing bubble, pours into mould and be cured.Obtain a kind of by the epoxy resin toughened material of modified Nano composite structure silicon-dioxide.
The preparation method of wherein said modified Nano composite structure silicon-dioxide toughner is as follows: first prepare metal-doped nano composite structure silicon-dioxide, then carry out grafting with dendritic macromole and obtain new modified nano composite structure silicon-dioxide toughner.
Wherein said metal-doped nano composite structure silicon-dioxide preparation method as follows: by triblock copolymer, ethanol and mixed in hydrochloric acid, add organic granular, adds aluminum contained compound, then add tetraethoxy.Certain temperature stirring reaction 20 hours, then crystallization after 3 days at a certain temperature, suction filtration, washing, dries, and roasting at a certain temperature 5 hours, obtains nano composite structure silicon-dioxide.
Wherein said dendritic macromole is polyamide-amide (PAMAM), and that the present invention uses is the 5th generation molecule G5.0PAMAM, the 7th generation molecule G7.0PAMAM, one or more mixing in the tenth generation molecule G10.0PAMAM.Nano composite structure silicon-dioxide and dendritic macromole are joined in organic solvent, at 80 degree heated and stirred 8 hours, suction filtration, dry, obtain modified Nano composite structure silicon-dioxide toughner.
Nano composite structure silicon-dioxide has good dispersing property than single structure silicon-dioxide, solve the shortcoming that single structure silicon-dioxide is easily reunited, and in the time carrying out grafting with dendritic macromole, there is a more binding site, more various bonding mode, dendritic macromole combines with the inorganic nano combined structural silica dioxide of rigidity, in epoxide resin material, disperse to form island structure, thereby make the modified Nano composite structure silicon-dioxide toughner in the present invention there is excellent toughness reinforcing performance.
The present invention compared with prior art, there is following apparent outstanding feature and remarkable advantage: what the present invention adopted is the compound toughening technology of novel organic-inorganic, than single toughening technology, epoxide resin material mechanical property improves significantly, and the addition of toughner still less.Be conducive to add other auxiliary agents in order to improve other performances of epoxide resin material.And technique is relatively simple, with low cost, be applicable to suitability for industrialized production, there are wide market outlook.
Embodiment:
Embodiment 1,
Step 1: 40 grams of polyether glycols (P123) are dissolved in 600 milliliters of ethanol and 10 milliliters of 0.5M hydrochloric acid solns, add 3 grams of polystyrene spheres, add 5 grams of aluminum isopropylates, then add 67 grams of tetraethoxys.Under 60 degree, stir 20 hours, then in 100 degree crystallization after 3 days, suction filtration, washing, dries, and under 600 degree, roasting 5 hours, obtains nano composite structure silicon-dioxide.Nano composite structure silicon-dioxide toughner and dendritic macromole polyamide-amine (G5.0PAMAM) are added in acetonitrile, stir 8 hours at 80 DEG C, suction filtration, dries, and obtains modified Nano composite structure silicon-dioxide toughner.
Step 2: epoxy resin toughened material preparation, it is 600 parts according to weight part note epoxy resin, 2 parts of the modified Nano composite structure silicon-dioxide toughner of being prepared by step 1,30 parts of stirring at room temperature 1-3 hour of auxiliary agent mix, after fully mixing, add solidifying agent to stir 5-10 minute, then vacuumize degassing bubble, pours into mould and is cured.Obtain a kind of by the epoxy resin toughened material of modified Nano composite structure silicon-dioxide.
Embodiment 2,
40 grams of polyether glycols (P123) are dissolved in 600 milliliters of ethanol and 10 milliliters of 0.5M hydrochloric acid solns, add 3 grams, piemarker bar core, add 67 grams of tetraethoxys.Under 30 degree, stir 20 hours, then in 100 degree crystallization after 3 days, suction filtration, washing, dries, and under 550 degree, roasting 5 hours, obtains nano composite structure silicon-dioxide.Nano composite structure silicon-dioxide toughner and dendritic macromole polyamide-amine (G5.0PAMAM) are added in acetonitrile, stir 8 hours at 80 DEG C, suction filtration, dries, and obtains modified Nano composite structure silicon-dioxide toughner.
Step 2: epoxy resin toughened material preparation, it is 600 parts according to weight part note epoxy resin, 2 parts of the modified Nano composite structure silicon-dioxide toughner of being prepared by step 1,30 parts of stirring at room temperature 1-3 hour of auxiliary agent mix, after fully mixing, add solidifying agent to stir 5-10 minute, then vacuumize degassing bubble, pours into mould and is cured.Obtain a kind of by the epoxy resin toughened material of modified Nano composite structure silicon-dioxide.
Embodiment 3,
40 grams of polyether glycols (F127) are dissolved in 600 milliliters of ethanol and 10 milliliters of 0.5M hydrochloric acid solns, add 3 grams, stem or leaf of cattail bar core, add 5 grams, Tai-Ace S 150, then add 67 grams of tetraethoxys.Under 40 degree, stir 20 hours, then in 150 degree crystallization after 3 days, suction filtration, washing, dries, and under 550 degree, roasting 5 hours, obtains nano composite structure silicon-dioxide.Nano composite structure silicon-dioxide toughner and dendritic macromole polyamide-amine (G7.0PAMAM) are added in dimethylbenzene and tetrahydrofuran (THF) mixed solvent, stir 8 hours at 80 DEG C, suction filtration, dries, and obtains modified Nano composite structure silicon-dioxide toughner.
Step 2: epoxy resin toughened material preparation, it is 600 parts according to weight part note epoxy resin, 2 parts of the modified Nano composite structure silicon-dioxide toughner of being prepared by step 1,30 parts of stirring at room temperature 1-3 hour of auxiliary agent mix, after fully mixing, add solidifying agent to stir 5-10 minute, then vacuumize degassing bubble, pours into mould and is cured.Obtain a kind of by the epoxy resin toughened material of modified Nano composite structure silicon-dioxide.
Embodiment 4,
40 grams of polyether glycols (P123) are dissolved in 600 milliliters of ethanol and 10 milliliters of 0.5M hydrochloric acid solns, add 3 grams of carbon dusts (1000 order), add 5 grams of aluminum isopropylates, then add 67 grams of tetraethoxys.Under 50 degree, stir 20 hours, then in 120 degree crystallization after 3 days, suction filtration, washing, dries, and under 500 degree, roasting 5 hours, obtains nano composite structure silicon-dioxide.Nano composite structure silicon-dioxide toughner and dendritic macromole polyamide-amine (G10.0PAMAM) are added in dimethylbenzene and acetonitrile mixed solvent, stir 8 hours at 80 DEG C, suction filtration, dries, and obtains modified Nano composite structure silicon-dioxide toughner.
Step 2: epoxy resin toughened material preparation, it is 600 parts according to weight part note epoxy resin, 2 parts of the modified Nano composite structure silicon-dioxide toughner of being prepared by step 1,30 parts of stirring at room temperature 1-3 hour of auxiliary agent mix, after fully mixing, add solidifying agent to stir 5-10 minute, then vacuumize degassing bubble, pours into mould and is cured.Obtain a kind of by the epoxy resin toughened material of modified Nano composite structure silicon-dioxide.
Table one
| Performance | Unit | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 |
| Tensile strength | Mpa | 71.2 | 65.3 | 78.1 | 68.1 |
| Elongation at break | ％ | 21.5 | 18.5 | 20.2 | 19.8 |
| Shock strength | J/m | 1513.2 | 1305.3 | 1278.6 | 1428.6 |
Claims (9)
1. modified Nano composite structure silicon-dioxide is epoxy resin toughened, it is characterized in that: it comprises following raw material, epoxy resin, modified Nano composite structure silicon-dioxide toughner, solidifying agent, auxiliary agent; By modified Nano composite structure silicon-dioxide toughner, auxiliary agent and epoxy resin are blended in stirring at room temperature 1～3 hour, after fully mixing, add solidifying agent to stir 5～10 minutes, then vacuumize degassing bubble, pour into mould and be cured, obtain by the epoxy resin toughened material of modified Nano composite structure silicon-dioxide.
2. modified Nano composite structure silicon-dioxide according to claim 1 is epoxy resin toughened, it is characterized in that: the preparation method of described modified Nano composite structure silicon-dioxide toughner, it is characterized in that: by triblock copolymer, ethanol and mixed in hydrochloric acid, add organic granular, add aluminum contained compound, then add tetraethoxy; Stirring reaction 20～30 hours under 30～60 degree, then under 100～150 degree, crystallization is after 2～3 days, and suction filtration, washs, and dries, and under 500～600 degree, roasting 5～6 hours, obtains nano composite structure silicon-dioxide; Then nano composite structure silicon-dioxide and dendritic macromole are joined in organic solvent, spend heated and stirred 6～8 hours 80～120, suction filtration, dries, and obtains modified Nano composite structure silicon-dioxide toughner.
3. according to claim 2, the preparation method of modified Nano composite structure silicon-dioxide toughner, it is characterized in that: described triblock copolymer is polyether glycol (P123), one or both mixing in polyether glycol (F127).
4. according to claim 2, the preparation method of modified Nano composite structure silicon-dioxide toughner, it is characterized in that: described organic granular is polystyrene sphere, carbon dust (1000 order), or natural phant particle is as piemarker bar core, one or more in stem or leaf of cattail bar core are mixed, 5%～20% (weight ratio) that add-on is triblock copolymer.
5. according to claim 2, the preparation method of modified Nano composite structure silicon-dioxide toughner, is characterized in that: described aluminum contained compound is sodium metaaluminate, aluminum isopropylate, one in Tai-Ace S 150,0%～20% (weight ratio) that add-on is tetraethoxy.
6. according to claim 2, the preparation method of modified Nano composite structure silicon-dioxide toughner, it is characterized in that: described dendritic macromole is polyamide-amide (PAMAM), that the present invention uses is the 5th generation molecule G5.0PAMAM, the 7th generation molecule G7.0PAMAM, one or more in the tenth generation molecule G10.0PAMAM are mixed, and add-on is silica weight 5～30%.
7. according to claim 2, the preparation method of modified Nano composite structure silicon-dioxide toughner, is characterized in that: described solvent is methyl alcohol, dimethylbenzene, tetrahydrofuran (THF), one or more mixing in acetonitrile.
8. modified Nano composite structure silicon-dioxide according to claim 1 is epoxy resin toughened, it is characterized in that: the add-on of described modified Nano composite structure silicon-dioxide toughner is weight epoxy 0.05～0.5%.
9. modified Nano composite structure silicon-dioxide according to claim 1 is epoxy resin toughened, it is characterized in that: described auxiliary agent is 3-r-chloropropyl trimethoxyl silane, 3-aminopropyl triethoxysilane, methacrylic acid, methylene-succinic acid, antioxidant 1010, carbon black, paraffin, stearic acid, oleic acid, several mixing in naphthenic oil, add-on is weight epoxy 1～5%.
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| CN106589314A (en) * | 2016-12-06 | 2017-04-26 | 大连理工大学 | Preparation method for composite resin system copolymerized by silicon dioxide and epoxy resin and compatible with liquid oxygen |
| CN106893442A (en) * | 2015-12-17 | 2017-06-27 | 中国科学院金属研究所 | A kind of transparent nano silicon-anti-corrosive paint of epoxy resin and preparation method |
| CN107189329A (en) * | 2017-06-26 | 2017-09-22 | 王蒙 | A kind of toughener |
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| CN106893442B (en) * | 2015-12-17 | 2019-08-16 | 中国科学院金属研究所 | A kind of transparent nano silica-anti-corrosive paint of epoxy resin and preparation method |
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| CN114656744A (en) * | 2022-05-20 | 2022-06-24 | 广东乔艺塑胶有限公司 | Low-odor PP/AS/POK ternary composite resin, cosmetic packaging material and preparation method thereof |
| CN114656744B (en) * | 2022-05-20 | 2022-07-29 | 广东乔艺塑胶有限公司 | Low-odor PP/AS/POK ternary composite resin, cosmetic packaging material and preparation method thereof |
| CN115044173A (en) * | 2022-07-11 | 2022-09-13 | 中山超分子新材料有限公司 | Corrosion-resistant high-elasticity composite fiber and preparation method thereof |
| CN116425496A (en) * | 2023-03-17 | 2023-07-14 | 泰山石膏（江阴）有限公司 | High-strength gypsum-based fiber board and preparation method thereof |
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