用湿法磷酸制纯磷酸一铵

323四川大学学报(工程科学版)Vol.32No.320005JOURNALOFSICHUANUNIVERSITY(ENGINEERINGSCIENCEEDITION)May2000:1009-3087(2000)03-0077-04王国平1,黄隐华2,钟本和1,张允湘1(1.,610065;2.,611930):;,,:;;;:TQ442.9:AManufactureofPureMonoammoniumPhosphatefromWet-processPhosphoricAcidWANGGuo-ping1,HUANGYin-hua2,ZHONGBen-he1,ZHANGYun-xiang1(1.Dept.ofChem.Eng.,SichuanUniv.,Chengdu610065,China;2.Chengduteacherscollege,pengzhousichuan611930,China)Abstract:Inthispaper,atwo-stepmethodforpurifyingnon-concentratedwe-tprocessphosphoricacidwasdeveloped.Firstlyaproperquantityofsodiumsulfateandphosphaterockwereaddedforpartiallyde-flourinatingandde-sulfatingtheacid,secondlythepre-purifiedacidwasneutralizedwithammoniaforfurtherremovalofflourineandentirelypre-cipitatingthemetalionsintheacid.Whenthefinelypurifiedammoniumphosphatesolutionwasconcentratedtoaproperfinaldensityandthencooled,crystallized,thesolidproductcouldmeetthegradedesired.Thephosphate-containedresidueinthepurifyingprocessmaybefedbacktotheproductionofammoniumphosphatefertilizer.Keywords:ammoniumphosphate;thepurificationofwe-tprocessphosphoricacid;de-flourination;de-sulfation,,,:,,,,,,:1999-07-06:(1973-),,.:.,!∀#∃%&∋[1,2],pH!∀#[3]!∀#[4]CaO-P2O5-NH3-H2O,,,11.11%~3%F-,SiF2-6,:SiF2-6+4OH-+(n-2)H2OSiO2.nH2O+6F-,SiF2-6Na2SiF6,,2%~4%SO2-4,,,SO2-4,,pH,(Fe,Al)(NH4)2Mg(HPO4)2F3(Fe,Al)NH4(HPO4)21/2H2OCaHPO4MgHPO43H2O,CaF2,1.2(100),1,2;(NH328%)1Tab.1AnalysisofJinhephosphaterockP2O5CaOFAl2O3Fe2O3MgO/%29.4041.072.823.293.051.832Tab.2AnalysisofJinhephosphoricacidP2O5CaOFSO3Al2O3Fe2O3MgO/%20.280.101.743.870.920.422.121.3SO3,,CaO=CaO(mol)CaO(mol)Na2SO4=Na2SO4(mol)Na2SO4(mol)=-+100%=SO3-SO3SO3+Na2SO4SO3100%,,:40~60;1.0~1.4;0.45~0.7015400g,5min,30min,10min10cm0.06MPa,,,P2O5CaOSO31.4pHCaOP2O5CaO;,1mL50mL,pHpH,pH,30min,pH550,P2O5CaOSO3,,P2O5,:P2O5=P2O5P2O5+P2O5100%1.51000mL,,,16,,P2O5NSO3F,[5]22.1153478()323Tab.3Experimentalresultsofpre-purificationofphosphoricacid/%/%37.653.248.146.456.350.04Tab.4Optimumconditionsforpre-purificationofphosphoricacid/CaONa2SO440.00.551.303,50%:Na2SiF6,Al3+:Al3++SiF2-6+2H2O=AlF2-6+SiO2+4H+,AlF2-6,,,,,CaO2.22.2.1磷酸氨化终点pH的影响1:pH=3.8~5.3,99%,P2O570%,,pH3,CaF2,[Ca2+][F-]2=410-11Ca2+,P2O5,,P2O51P2O5pH(CaO=0.55)Fig.1Deflourinationandphosphaterecoveryratiovs.finalpHofthesolution2:pH,pH,pH,CaOpH,pH2()CaOpH(CaO=0.55)Fig.2RateofFiltration(drymaterial)andconcentra-tionofCaOinsolutionvs.finalpHofsolution(stoichiometricratioofCaO=0.55)2.2.2CaO计量比的影响3:99%,;P2O5,,3P2O53P2O5CaO(pH=5)Fig.3Deflourinationandphosphaterecoveryratiovs.stoichiometricratioofCaO4CaO[2]1~1.5,,CaF2,F-2.2.3氨化速率的影响,,,5,,793,4()CaOCaO(pH=5)Fig.4RateofFiltration(drymateral)andconcentrationofCaOinsolutionvs.stoichiometricratioofCaO(pH=5)5Tab.5Effectsofammoniatingrateonfilterability/min0.25101520()/(kgm-2h-1)14.6143.4265.8354.1440.52.3,6:1.26g/cm3P2O5NNH4H2PO4,,,P2O545.2%,,,P2O540%,SO38%((NH4)2SO4),9%(CaHPO4),CaSO4CaHPO4,Ca2+SO2-4,CaHPO4CaSO4,;SO2-4(NH4)2SO4,,31):50%,6Tab.6Analysisofammoniumphosphateproductobtainedbyconcentratingpurifiedliquortodifferentfinaldensity/(gcm-3)/%NP2O5N/P2O5SO3FP2O5/%P2O5/%11.25711.961.140.1940.330.006045.245.221.30011.961.060.1950.390.0080.1319.164.331.38010.946.740.2335.200.0161.5523.487.749.4739.730.2388.330.0759.0612.3100.0-1.3811.656.180.2061.920.0100.5387.687.6-11.253.770.2082.990.0211.95100.0100.02),pH=599%,()400Kg/(m2h),P2O570%,,3)1.38g/cm3,,P2O587%;1.30g/cm3,,P2O564%,:[1]!∀#∃%&∋(),!∀#∃%&,!∀#∃%&∋∋,!∀#∀!∀#∃%&∋&())#∗+,,−∃∋∀&−.#∗∗/01#∃%#∀∃#!!∀#∃%!&∋())([J].!∀#∃%&#∋,1995,68(3):366~371.[2]!∀#∃%&∋(),M!∀#!∃%&.!∀#∃%#&∋()∗!∀#∀∃%∃%∀&&∋(∃%∋!∀)∗∗)∀∋∀(+)∃,[J].!∀#∃%,1990,63(3):644~648.[3]!∀#∃%,!∀#∃%,!∀#∃%&∋()∀∗!∃+%!)∀+!∀#∃%O-P2O5-NH3-H2O45,60,75,90[J].!∀#∃%&∋(,1972,17(3):829~832.[4]!∀#∃∃,!∀#∃%&∋(.!∀#∃#%&&∋&()∗!!∀#∃%&∀∋!()∃∗∗∋∗∃(∃+∀,[J].!,1981,(8):470~2.[5][M].:,1991.()80()32