高纯纳米氧化镁制备工艺研究

①胡章文1,饶丹丹1,杨保俊2,单承湘2,陶庭先1(1.,241000;2.,230009)　:MgCl26H2O,,,。,25min,3h,:35℃,(NH3H2O∶MgCL26H2O)2.2∶1,Mg2+1.3mol/L,2mL,700℃。,99%。X,,、,35nm,。,,。:;;;:TQ123.4:A:0253-6099(2006)05-0068-04PreparationParametersofHigh-purityNanometerMagnesiumOxideHUZhang-wen1,RAODan-dan1,YANGBao-jun2,SHANCheng-xiang2,TAOTing-xian1(1.DepartmentofBiochemicalEngineering,AnhuiUniversityofTechnologyandScience,Wuhu241000,Anhui,China;2.SchoolofChemicalEngineering,HefeiUniversityofTechnology,Hefei230009,Anhui,China)Abstract:UsingMgCl26H2Oasprecursor,PVAasthedispersantandNH3H2Oasprecipitatingagent,amagnesi-umoxideofhighpurityandnanometercanbeprepared.Theresultsofsinglefactorandorthogonalexperimentsindicatethattheoptimumtechnologicalconditionsareasfollows:reactiontimeof25mins,calcinationstimeof3h,reactiontemperatureof35℃,ammonia/magnesiumproportionof2.2∶1(mole),concentrationofMg2+of1.3mol/L,disper-santof2mL,calcinationstemperatureof700℃.Themorphologyofthepowderswascharacterizedbytransmissionelec-tronmicroscopy(TEM)andX-raydiffraction(XRD).Theresultsindicatethatmagnesiumhydroxideparticlesarewelldispersedwithanarrowsizedistributionandanaveragesizeisof35nm,anditmeetsthedemandforhigh-puritynano-metermagnesiumoxide.Thesimpleprocessintroducedcanbringsteadyproductqualityandcanbeeasilyindustrial-ized.Keywords:highpuritymagnesiumoxide;nanometer;preparationprocess;ammoniawaterprecipitating　　,,、、、、[1～3]。,、、、,、、、、、、、、[4～6]。,[7～9],。、、、、;,,[10～11]。,98%,,1,1/10,。、,、。,96%,。,,[12～13]。MgCl26H2O,①:2006-03-24:(20471002);(2006KJ034A):(1969-),,,,,。265200610矿　冶　工　程MININGANDMETALLURGICALENGINEERINGVo.l26№5October2006,,,。,,,。1　1.1　1)。MgCl26H2O,,;NH3H2O,,;(PVA),,。2)。SX2-8-10,;LXJ-Ⅱ,;FC104,;GZX-400-BS-Ⅱ,。1.2　,,,,。NH3H2O、NaOH、(NH4)2CO3、Na2CO3。NH3H2O,MgCl2,。:MgCl2+2NH3H2OMg(OH)2+2NH4ClMg(OH)2MgO+H2O,。1.3　MgCl2100mL,,PVA。,MgCl2100mL,25min。,,120℃2h。,3h,。1.4　1。1　1.5　MgOCa、Fe、Al、Cl、Si、SO42-、GB9004-88。1.6　D/max-γBX-ray(Cu,λ0.1540nm,40kV,100mA,4Deg/min,2θ=10°～70°)。H-600、。2　2.1　2.1.1　反应温度的影响　Mg2+1mol/L、(NH3H2O:MgCl26H2O)2.4∶1、5mL、25min、800℃、3h,2。2　2,,;45℃,;,。,;,NH3H2O,。,,。2.1.2　Mg2+摩尔浓度的影响　2.4∶1、5mL、25min、45℃、800℃、3h,Mg2+3。3　695:,,Mg2+1.2mol/L,,,Mg2+。,;,。2.1.3　原料摩尔比(NH3H2O∶MgCl26H2O)的影响　Mg2+1.0mol/L,5mL,25min,800℃,3h,4。4　,,。,,。2.1.4　分散剂用量的影响　Mg2+1.0mol/L、2.4∶1、25min、800℃、3h,5。5　5,,4mL,。、。2.1.5　煅烧温度的影响　Mg2+1mol/L、2.4∶1、5mL、25min、45℃,3h,6。6　6,,。,,Mg(OH)2,,,MgO。2.2　,,MgO,MgO、、、、5,L16(45)。1,2。,。2R,RA=1.15,RB=0.89,Mg2+RC=1.00,RD=0.84,RE=0.96,:A、Mg2+C、E、B、D。A2B1C3D1E3。,99%,A2B1C3D1E3。35℃,2.2∶1,Mg2+1.3mol/L,2mL,700℃。1　(A)/℃(B)Mg2+(C)/(molL-1)PVA(D)/mL(E)/℃1302.2:11.026002352.4:11.236503402.7:11.347004453.0:11.5580070　　　262　ABCDEMgO/%11111199.0821222296.4231333398.2641444497.4652123498.7062214398.2172341299.4582432196.9693134296.44103243196.07113312495.80123421397.60134142399.70144231496.27154324197.48164413296.86K1391.22392.92388.95392.4387.59K2392.32386.97389.2389.88387.97K3388.91386.56393.03388.89393.77K4388.31386.88392.68389.57388.23k198.7898.7598.3499.1598.07k299.2198.0398.6598.4598.34k398.15.97.8698.9698.3199.03k498.0698.1297.9698.5898.54R1.150.891.000.840.96A2B1C3D1E32.3　2.3.1　XRD表征　7XRD,,,。7　XRD2.3.2　TEM表征　8(12)。8,、,15nm。8　TEM3　　　MgCl26H2O,,,。,25min,3h,:35℃,2.2∶1,Mg2+1.3mol/L,2mL,700℃。,99%,。XRD,。TEM,、,15nm。,,,。:[1]　.[M].:,2004.[2]　MishakowIV,BediloAF,RichardsRM,etal.NanocrystallineMgOasadehydrohalogenationcatalyst[J].JCatal,2002,206:40-48[3]　,,,.[J].,2004,19(4):18-21.[4]　,.[J].,2001(12):696-698.[5]　　,,,.[J].,2004,37(3):73-77.[6]　,,　,.MgO[J].,2001,17(3):361-365.[7]　　.[J].,1999,30(2):193-194.[8]　,.CaCO3[J].,2003,44(5):243-245.[9]　,,　.[J].,2002,33(5):521-523.[10]　.[J].,2005,34(3):12-13.[11]　,.[J].,2001,30(6):16-18.[12]　　,,,.[J].,2002,20(3):152-154.[13]　,,,.[J].,2001,30(1):20-22.715: