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273河北工业科技Vol.27,No.320105HebeiJournalofIndustrialScienceandTechnologyMay2010:10081534(2010)03018504,,,,(青岛科技大学化工学院,山东青岛266042):在一定的温度和压力条件下,采用单质硅溶解法,用正交试验法研究了反应温度反应压力反应时间氢氧化钠及硅粉用量等对硅溶胶收率及粒径的影响实验结果表明,硅溶胶制备实验的最佳工艺条件如下:压力为0.5MPa,在200mL去离子水中加入15g硅粉和0.4g氢氧化钠,并控温度为160反应9h,在此条件下制得的硅溶胶平均粒径为174.4nm,收率为80.15%平行实验结果表明,该最佳工艺条件具有良好的重现性:压力;单质硅;硅溶胶;正交试验:TQ330:AStudyonpreparationoflargeparticalsizesilicasolbymodifiedsilicadissolutionmethodZHANGYuanjing,LIZhenqiu,LIJinghua,HUANGCaixia,YUGuang(DepartmentofChemistryEngineering,QingdaoUniversityofScienceandTechnology,QingdaoShandong266042,China)Abstract:Thesilicasolwassynthesizedundertheconditionofcertaintemperatureandpressure,withsilicaasreactionsandsodiumhydroxideascatalyst.Thefactorsthataffectsilicasol,suchasthereactiontemperatureandpressure,reactiontime,amountofcatalystandsilicon,werestudiedbyorthogonalexperimentinthispaper.Theresultsshowthattheoptimumconditionsareasfollows:siliconpowder15g,sodiumhydroxide0.4gin200mLdeionizedwater.Thereactionwascarriedoutfor9hat160,0.5MPa.Theparallelexperimentresultsshowthattheseoptimumconditionscouldbereplayed.Keywords:pressure;silicon;silicasol;orthogonalexperiment:20091216;:20100310::(1983),,,,(silicasol),,,,[12],,[3],,[4],:100~130nm[5];100nm[6],,,,,,11.11.1.1,99%,200,1410,2335,2.33,;,;,,;,99.99%,AS40,40%,17nm1.1.2GSHA1,;NDJ55,;,pHS3C,;,;JEM1200EX,1.21.2.1,,,,,,,,,,:Si+4H2O=H4SiO4+2H2,H4SiO4=H2SiO3+H2O,H2SiO3+2NaOH=Na2SiO3+2H2O,,,,,,,,,,,,,;,,1.2.2,0,2,4,6,8MPa(80),80,100,120,150,180,ZetapH1.2.3,,L16(45),(A)(B)(C)(D)(E)5,4,1表1因子水平表Tab.1Factorsandlevels(A)/(B)/MPa(C)/h(D)/g(E)/g11200.57100.221401.08150.331601.59200.441802.010250.522.12.1.1,80,200mL,10g,0.3g,8h,21(1d,)表2反应压力对硅溶胶制备的影响Tab.2Influenceofpressureonsilicasolpreparation/MPa/nm/(MPa!s)/%pH076.43.0401.48.22120.02.9421.17.5484.02.9711.57.86111.03.4451.68.08112.03.2271.68.0图1不同压力下所得硅溶胶的粒径分布Fig.1Sizedistributionofthesilicasolondiffenentpressureconditions21,,,2MPa,,18627,(1),,,2MPa2.1.2,200mL,10g,0.3g,8h,32表3反应温度对硅溶胶制备的影响Tab.3Influenceoftemperatureonsilicasolpreparation//nm/(MPa!s)/%pH80120.02.9421.17.510068.63.0641.58.012088.13.0733.58.3150176.73.2575.78.0180115.93.1133.37.532,,,图2反应温度150硅溶胶粒径分布图Fig.2Sizedistributionofthesilicasolat150,,;,150,,,176.7nm:150,2MPa,,2.24表4正交试验结果Tab.4ResultsoftheorthogonaltestABCDE/%/nm11111175.0111.9221222277.0102.0031333373.0114.1241444474.4100.8852123486.0120.0062214376.0117.0072341275.0113.4482432183.3148.0093134289.6129.17103243169.5130.11113312482.7135.00123421386.0118.01134142378.0174.70144231473.0115.86154324182.0100.69164413280.096.00K174.85082.15078.42577.25077.450K280.07573.87582.75080.25080.400K381.95078.17579.72577.12578.250K478.25080.92574.22580.50079.025R7.1008.2758.5253.3752.950CBADEk1107.230133.947114.980114.808122.680k2124.610116.243110.175139.925110.153k3128.072115.813126.787115.058130.957k4121.813115.722129.782111.935117.935R∀20.84218.22519.60727.99020.804DAECB18732.32.3.1,120~180,,,,,,1602.3.20.5~2MPa,,,,,0.5MPa2.3.3,,,,,9h2.3.4,10~25g,,15g2.3.5,,;,,,,,,0.4g,,0.4g,CBADE;,DAECB,,,,52DAECBC2B1A3D4E2;D2A3E3C4B1D2A3E3C3B12.43,175.2nm,80.15%,Zeta-58.7~-47.2V,pH8.54~9.34,,AS40(40%,17nm),3,17.24nm,150,,图3AS40粒径分布图Fig.3SizedistributionofAS40,,4图4AS40及平行实验自制硅溶胶TEM图Fig.4TEMofAs40andtheparalleltestsofsilicasol(203)188274,:a2d2ydt2+a1dydt+a0y=b0x;H(S)=1(S0)2+20S+1;H(j)=11-(0)2+20j,2PVDF,,10-5~109Hz,,,PVDF,,,PVDF,1500Hz51):0~70MPa;2):39pC/Pa;3):10136,PVDF,,,,:[1],,.[J].,1992(8):1822.[2],,.PVDF[J].,2004(4):688692.(188)31)2):160,0.5MPa,9h,15g,0.4g175.2nm,80.15%,3):[1],.[J].,2005(6):2733.[2].[J].(),2002,23(4):1920.[3],,.[J].,2007(2):811.[4],,,.[J].,2003(5):512514.[5],,,.[P].:1594080A,20050316.[6],,,.[J].,2005(8):925929.[7],,,.[J].,2010,27(1):912.[8],.LICVD[J].,2004,25(3):1115.(195):[1],,.[J].,2004,21(3):3741.[2],.[J].,2006,23(4):125129.[3].[M].:,2001.[4].[J].,1992,2(1):1220.[5].[J].,1991,8(4):379388.[6],.[J].,2000(6):5964.2033PVDF