沉淀法制备白炭黑绿色新工艺

,,,(武汉工程大学化工与制药学院,绿色化工过程省部共建教育部重点实验室,湖北武汉430074):,,,,,,82,40%,15min,NaP910,,1.28%,,:;;;GreenProcessofWhiteCarbonBlackPreparationbyPrecipitationMethodXIONGXiang-zu,XUBiao,HULi-feng,DUWen(KeyLaboratoryforGreenChemicalProcessofMinistryofEducation,SchoolofChemicalEngineering&Pharmacy,WuhanInstituteofTechnology,HubeiWuhan430074,China)Abstract:Whitecarbonblacksaltwaspreparedbythemethodofprecipitationwithphosphoricacidandsodiumsilicateasrawmaterials,onthepremiseofnoaffectiontothequalityofwhitecarbonblackandsodiumphosphate,thetechnologiesofproductionofwhitecarbonandsodiumphosphatewerecombinedorganically.Itwouldsolvetheproblemsofthesaleofby-products,andtheoriginalcomprehensivetechnicalandeconomicindexesofsodiumsaltwouldbeeffectivelyimproved.SomeimportantfactorswhichaffectedthecontentofremnantphosphorinproductssuchasthemassratioofNatoP,thewaterconten,tthereactiontemperature,andthereactiontimewerestudied,respectively.TheresultsshowedthattheremnantPinthefinalproductswashedbySulfuricacidcannotbedetected,andthepercentageofremnantPinintermediateproductswas1.28%,whenthereactiontemperaturewas82,thepercentageofwatercontentwas40%,thereactiontimewas15min,andthemassratioofNatoPwas910.Keywords:phosphoricacid;whitecarbonblack;phosphate;sodiumsalt:(1951-),,:(1987-),,E-mai:[e-mail],,,[1-2],,,,,,,,,,,SiO2nH2O,[3],,,,,,11.185%();M=3.4234.64%;GB/T625-2007();HHS-4S;HN101-0;1.2,:Na2OSiO2+H3PO4!SiO2nH2O+NaH2PO4,NaH2PO4,,SiO2nH2O,,,,,732011391,,,[4-5],:NaP,1.3(1):3.42,34.64%100g;85%60%40%20%,40%60%80%;68~82;11H2SO4(2):1NaP0.9~1.1,,10~20min,pH=4.2~4.8,(0.9~1.1),(3):2,,70~100pH6.5~7.0,,,(4):310mL11H2SO4,pH7.0,,,,,SiO2∀∀∀(5):3,11Fig.1Processflowchart1.4,,,11Table1NormaldesignforexperimentalfactorsNaP(A)/%(B)T/(C)t/min(D)11140681020.9160751531.1180822022.1[6-7],,L9(34),4,22Table2ExperimentalresultsNaP/%T/t/min/%114068102.620.017420.96068152.160.014531.18068202.400.015840.98075102.640.175051.14075151.900.0126616075205.100.012471.16082102.960.0193818082150.600.003990.94082200.600.0042233Table3AnalysisofexperimentalresultsNaP(A)/%(B)T/(C)t/min(D)/%K18.325.127.188.22K25.4010.229.644.66K37.265.644.168.10K42.771.712.392.74K51.803.413.211.55K62.421.881.392.702.925.105.483.56CBDAC3B1D2A22.22Fig.2RelationbetweenNaPofrawmaterialsandremnantPcontentinwhitecarbonblack7420113912,,SiO2H2SO4,NaP3Fig.3RelationbetweenwatercontentinphosphoricacidandremnantPcontentinwhitecarbonblack3,,,60%4Fig.4RelationbetweenreactiontemperatureandremnantPcontentinwhitecarbonblack4,,,,,,SiO2nH2O,,,,[8-9],SiO2nH2O,78~825Fig.5RelationbetweenreactiontimeandremnantPcontentinwhitecarbonblack5,15min,3,:C3B1D2A2,82,40%,15min,NaP0.9,,,1.28%,,3,,,,,,,,,[1]WUYuan().SubmergedCirculativeImpingingStreamReactorChemistry[J].onInternet,2002,4(9):049044pe.[2]WANGZhonggen().ManufactureofWhiteBlack[J].InorganicSaltIndustry(),1994(3):22.[3],.[J].,2008,40(1):8-10.[4],,,.[J].,1999,22(1):17-18.[5],.#∃[J].,2003,54(10):1381-1386.[6],,,.[J].,2008,40(11):37-39.[7],.[J].,2006,25(1):100-104.[8],.[J].,1997(7):348-351.[9],,,.[J].,2003,17(11):56-59.752011391