Summary: The article is used contain Rn amino silicon alkyl coupling agent to accept rice 2 oxidation silicon undertakes the surface is decorated, next again with the methylic acrylic acid that contains carboxyl group armour ester copolymer reacts, get polymer wraps Fu 2 oxidation silicon is small pull child. Use FTIR and pull diameter to distributing appearance is small to this pull child have appraisal and observation, confirm polymer combines packet of Fu to be in through chemical bond surface of 2 oxidation silicon. Research contains this small pull child the mechanical function of epoxy resin condensate. When corpuscular adds a quantity to be 2wt% , hardness of day of its tensile strength, impact strength got rising certainly, have the more apparent effect that add pliable but strong. The methodological bag Fu that 1 foreword combines organic material through chemical bond is in accept rice surface of 2 oxidation silicon, all sorts of attainable having the functional sex of stable condition is atomic child, the method of this kind of chemical bond is different from the method of the physisorption such as use surface activator, obtains functional sex small particle its organic bag cladding and 2 oxidation silicon won't be broken away from commonly, suffer the effect of treatment and use condition not easily. Small particle of sex of this kind of function, especially of accept rice class, wide applied perspective is had in composite material domain. Compound technology can get use accept rice all sorts of high-powered composite material, use all sorts of direct modified that exceed subtle particle to use high polymer data to business especially, can avoid a large number of trival handiwork to work, it is to win low case one of important methods of high-powered composite material. Consequently, nearly 10 come for years, business of ／ of functional sex small particle already made one of popular research tasks with high polymer composite material. Epoxy resin is one kind is had be able to bear or endure chemistry is caustic strong, felt function is integrated and tall, mechanical the material of high polymer of hot solid sex with superior sex. But, epoxy resin also has be able to bear or endure wet sex reachs ageing resistance difference, brittleness to wait for defect greatly. To improve epoxy resin integral performance, in recent years a few investigator use all sorts of accept rice small particle and compound technology to undertake modified to epoxy resin, in order to obtain high-powered composite material. The article synthesized the methylic acrylic acid that contains shuttle radical first latex of armour ester copolymer, use this copolymer latex and classics next amino kind of silicon alkyl coupling agent is treated reaction of 2 oxidation silicon, the methodological bag Fu that makes polymer passes chemical bond is in accept rice gas phase surface of 2 oxidation silicon, the become apparent that realized 2 oxidation silicon learns to decorate, obtained dispersive sex to exceed subtle particle goodly. Undertake small particle and this epoxy resin be mixinged in all again, got containing exceeding condensate of fine corpuscular epoxy resin, discussed its mechanical function. Laboratory of 2.1 main raw material uses 2 experiments part main raw material is methylic acrylic acid (MAA, limited company of chemical industry of Tianjin Bo Di) ; Methylic acrylic acid armour vinegar (MMA, factory of chemical reagents of Fu Chen of city of overhead keep under control) ; α- sulphur acerbity natrium - amber acid - double (2- second base) ester of different Xin Chun (EC8600, report of Japanese brilliance of the rising sun changes a company limited) ; XCT-30 scanty to hydrate divides powder (modified gets together latex of silicon oxygen alkyl, limited company of technology of Wuhan forerunner chemistry) ; Ammoniac propyl 3 second oxygen base silicon alkyl (DB-550, limited company of new material of chemical industry of Ying Chengde nation) ; Accept rice gas phase 2 oxidation silicon (A-200, inc. of Shenyang chemical industry) ; Epoxy resin L235 (company of Hexion Specialty Chemicals) ; Solidify agent H239 (company of Hexion Specialcy Chemicals) . 2.2 methylic acrylic acid - methylic acrylic acid the synthesis of latex of armour ester copolymer [- Page-] consults the method of a record and narrate, dispersive agent joins scanty to hydrate of the EC-8600 of 36.5g water, will certain amount and XCT-30 of agitate child, thermometer and the 250 Min that condensation is in charge of in 3 flask, room temperature agitate 20 minutes, add methylic acrylic acid of 4.3g methylic acrylic acid and 20g next armour ester, when 60 ℃ beforehand emulsification 0.5 H, will measured potassium sulfate to dissolve certainly next in water, cent second in joining flask, undertake emulsification reacts, after be being added, continue to react below 75 ℃ again 3h. After refrigeration reachs room temperature after, get content is the methylic acrylic acid of 36.33% originallying - methylic acrylic acid armour ester (MAA-MMA copolymer) latex. The surface of 2 oxidation silicon decorates gas phase of 2.3 accept rice in reactor of 5OOmL stainless steel, add coupling agent of 2g silicon alkyl first DB-550 and go after agitate of ionic water 200mL is dispersive, gas phase of rice of rejoin 20g accept 2 oxidation silicon, o.5h of room temperature agitate, stop reaction, smoke filter, get the surface contains material of amino oar of 2 oxidation silicon. 2.4 polymer wrap Fu 2 oxidation silicon (small particle) synthesis consults the method of a record and narrate, take methylic acrylic acid - methylic acrylic acid 26.5 ML of latex of armour ester copolymer (solid content 4.5g) with in join stainless steel container, sufficient agitate mixes. The face that adds afore-mentioned getting next contains material of amino oar of 2 oxidation silicon, after mixture agitate 1h, cease. Through taking filter eliminate water, generate contain amino carboxylic acid the intermediate child of saline radical. Intermediate child leaves vacuum in 130 ℃ after dry 8h, get polymer to wrap Fu 2 oxidation silicon (small particle) . The small particle that the 2.5 preparation that contain condensate of corpuscular epoxy resin will measure certainly joins the agitate in solidify agent H-239 after dispersive 20min, again as sufficient as epoxy resin agitate mixes 20min. Colophony mixture is after in metallic mould pouring, solidify. Solidify condition is ℃ of 4h/80 of ＋ of 6h/ room temperature. 2.6 tests analysis consults the method of a record and narrate, UV-160 of ferry of island of Japan of use spectrophotometer 〔 ) analytic corpuscular scanty to hydrate is spent, pour 1g sample and 100ml water into 200ml flask to shake adequately, agitate 5min, after quiet place Lmin, from flask bottom draw-out a few liquids are stand-by. Use UV-160 to undertake to taking out a liquid in 550nm place transmitance checks next, the transmitance of will pure water is surely 100, measure so that take out the scanty to hydrate of sample of the cipher out after liquid transmitance and pure water are compared to spend. Use NICOLET60-SXB infra-red spectrometer checks, use sample of preparation of KBr sheeting law, undertake FT-IR spectrum is analysed. In alcohol - water mixes solution (50/50 bulk is compared) in join a few particle child after mixing adequately equably, use LA-500 (Horiba, ja-pan) bead diameter distributings determine diameter of bead of appearance analysis corpuscular reachs his to distributing. Consult respectively GB/T2570-1995 and GB/T 2571-1995 standard, use RGT-30 electron is all-purpose material experiment machine (Er of Shenzhen luck case limited company) reach XJJ-50 to pound experiment machine (machine of Cheng Deshi check is finite liability company) all sorts of mechanical performance that check epoxy resin condensate. [- Page-] consults GB3854-83 standard, use cling to family name sclerometer (institute of metric science of the city that do not have stannum) determine the hardness of epoxy resin condensate. 3 results and discuss 3.1 corpuscular hydrophoby can scanty to hydrate spends a test to make clear, MAA-MMA copolymer wraps Fu 2 oxidation silicon (small particle) have exceedingly good hydrophoby can, its are scanty to hydrate is spent be as high as 93 ％ . The FT-IR spectrum scheme that 3.2 FT-IR spectrum analyses 3.2.1 MAA-MMA copolymer shows 3502cm-1 place 1 times to be - the adjustable vibration of OH absorbs a peak, 2997cm-1 place absorbs a peak for C-H adjustable vibration, 1731 Cm-1 place bolts for ester adjustable vibration recruits medium carboxyl group peak, 1450cm-1 place is - of CH2- be out of shape vibration absorbs a peak, 1200cm-1 place absorbs a peak for the adjustable vibration of C-C. The adjustable vibration of C ＝ C absorbs a peak to be 1650cm-1, in the graph this peak disappears basically, explain the Shuang Jian in armour ester has passed methylic acrylic acid and methylic acrylic acid freedom radical reaction is complete. [- the figure of infra-red and spectral contrast of 2 oxidation silicon shows from beginning to end of Fu of Page-] 3.2.2 polymer bag 2 times (A) in the dissymmetry that 1109cm-1 place bolts for Si-O-Si is adjustable and oscillatory absorb a peak, 805cm-1 is in the symmetrical and adjustable vibration that bolts for Si-O-Si to absorb a peak, 472cm-1 is in what bolt for Si-O-Si to curve vibration to absorb a peak. 3448cm-1 place is - the adjustable vibration of OH absorbs a peak. (The feature that place of the 1109cm-1 in B) is 2 oxidation silicon is adjustable and oscillatory absorb a peak, 805cm-1 is out of shape with what 472cm-1 is 2 oxidation silicon vibration absorbs a peak. 1560cm-1 office appears - the feature of NH absorbs a peak, 1640cm-1 is in occurrence acyl the feature of amine radical absorbs a peak, show face of 2 oxidation silicon - NH2 already was mixed in MAA-MMA copolymer - COOH produced reaction. Additionally 1731cm-1 is in in occurrence copolymer ester radical is luscious round - the adjustable vibration of COOL- absorbs a peak, demonstrative MAA-MMA copolymer wraps Fu to be in through chemical bond surface of 2 oxidation silicon. Diameter of 3.3 atomic seed and its structure analysis [- because Page-] is atomic child can better be in dispersedly alcohol - the mixture solution of water (50/50 bulk is compared) in. Determine through reaching what its distributing to corpuscular bead diameter knowable, although accept rice gas phase was used in corpuscular synthesis 2 oxidation silicon, but of the oneself in because 2 oxidation silicon is in accept rice gas phase,reacting reunite, can produce the particle of micron class only, its bead diameter distributings inside the limits in 1~10μm, and the bead diameter of MAA-MMA copolymer latex basically distributings inside the limits in 0.1~5μm. The influence watch that 3.4.1 solidify temperature learns function to condensate force shows the mechanical function of condensate of 3.4 epoxy resin 1 times to be opposite for solidify temperature condensate of blank epoxy resin (did not add particle child) the influence of mechanical function. By the watch 1 knowable, when solidify time is same, epoxy resin condensate gets when solidify temperature is 80 ℃ after, its each mechanical function temperature of the solidify after excel is 40 ℃ , consequently, when preparation contains condensate of corpuscular epoxy resin, choose 6h/ room temperature + the solidify condition of 4h/80 ℃ . The effect that 3.4.2 different small particle add a quantity to learn function to condensate force [- Page-] graph shows the effect that adds the tensile strength that measures pair of epoxy resin condensate and impact strength for corpuscular 3 times. By the graph 3 can see, after small particle is joined, after increasing first, the tensile strength of material and impact strength are reduced, when percentage of small particle quality is 2 ％ , both achieves great value to be 73.19MPa and 30.49kJ/m2 respectively, the impact strength of the tensile strength of the 66.25MPa that compares condensate of blank epoxy resin and 19.39kJ/m2 rises respectively 10.5% with 57.3 ％ . Because hydrophoby polymer is right,the surface of 2 oxidation silicon wraps Fu, improved its the dispersive sex in epoxy resin, and small particle itself has very tall tigidity and dispersive sex, can evener ground distributings in epoxy resin high polymer in the space of catenary. So, the tensile strength impact strength of solidify system all follows small particle dosage increase to increase first, when exceeding 2wt% , reduce again. The mechanical function when small particle content exceeds 2wt% reduces a phenomenon likelihood and exceed subtle particle to be concerned in the dispersive condition in epoxy resin condensate, conjectural likelihood is corpuscular is formed to reunite inside condensate the phenomenon produces hole, make particle dispersive in colophony thereby inhomogenous, bring about mechanical function to drop. The 3.5 hardness figures that contain condensate of corpuscular epoxy resin are shown 4 times be is atomic child add those who measure pair of epoxy resin condensate cling to the influence of family name hardness. By the graph 4 can see, when adding small particle, of condensate cling to family name hardness is 11.8, add a quantity to increase ceaselessly as corpuscular, of solidify body other people cling to family name hardness (fight deformation ability) appear increase a current, when adding a quantity to achieve 4wt% , hardness is achieved 24.2, be when be not being added 2 times much. Of epoxy resin condensate cling to family name hardness as small particle a few accretion increase and the tigidity of oneself of corpuscular of phenomenal specification hydrophoby that extent changes greatly has apparent effect to raising the hardness of matrix colophony whole. [- Page-] 4 conclusion (1) contains reaction of amino 2 oxidation silicon with the surface through using the MAA-MMA copolymerization that contains shuttle radical to get together, can get tall scanty to hydrate is spent (93 ％ ) polymer wraps Fu 2 oxidation silicon (small particle) , its bead diameter distributings inside the limits in 1~μm; (2) polymer wraps Fu 2 oxidation silicon (small particle) the tensile strength that minim adds pair of epoxy resin condensate and impact strength have very big effect, when small particle adds a quantity to be 2wt% in condensate, tensile strength and impact strength have a high cost (73.19 MPa and 30.49kJ/m2) , rose respectively than blank sample respectively 10.5% with 57.3% ; (3) polymer wraps Fu 2 oxidation silicon (small particle) minim joins what can raise epoxy resin condensate substantially cling to family name hardness. When adding a quantity to be 4wt% , hardness is achieved 24.2, the hardness that compares blank sample raised nearly 2 times.
Polymer wraps Fu 2 oxidation silicon and epoxy resin are compound the research of content
