Synthesis of Zeolite Form Lake Sludgeusing Microwave HeatingWenjing Wang1, Chris Salim2, Winarto Kurniawan1 and Hirofumi Hinode11Tokyo Institute of Technology, Department of International Development Engineering2Surya University, Department of Environmental Engineering7th AUN/SEED-Net Regional Conference on Chemical Engineering

The Kasumigaura Lake is located in the extent from Southeast Ibaraki to Northeast Chiba.*/16

Back ground*/16

Sludge from Kasumigaura lake (Si,Al,O,C etc.)Mineralizer: NaOH

Table the chemical component of lake sludge from KasumigauraMaterial*/16

ElementOSiAlFeCHFSClNOthersContent[wt%]32.625.711.48.133.011.300.780.480.310.2916

Definition : porous crystalline aluminosilicate Components : silica and alumina

(Crystal structure)

Characteristicscatalytic activity, adsorption ability, ion exchange ability etc. xM2OyAl2O3zSiO2nH2O(structural formula)Introduction - Zeolite*/16

Research objectives Synthesis of zeolite from lake sludge using hydrothermal reaction in alkali solutionInvestigation of microwave irradiation effects on synthesis of zeolites

Investigation of the effect of ultrasonic mixing*/16

Methodology - Synthesis procedure of zeolite

zeolite product drying of sludge (105) (from kasumigaura)crushing and sieving (

ExperimentalTreatment with alkali solution(1,2,3M NaOH)Crushing and sieving (

10m

10m

10m

Q : Quartz - SiO2P : Na-P1(Na6Al6Si10O3212H2O)(24h, Si/Al=1.9, 120, 2M NaOH) Results Effect of L / S ratio*/16

The influence of heating methodConventional heating method : mixing time 24h, heating time 24h Microwave heating method : mixing time 24h, heating time 6h Synthesis condition : Si/AL = 1.9, CNaOH = 2M, heating temperature = 120Q : Quartz SiO2 P1: Zeolite P1(Na) Na6Al6Si10O32!12H2O U : Unnamed zeolite Na6[AlSiO4]6!4H2O A : Analcime-C Na(Si2Al)O6!H2O*/16

Na-P1GismondineGIS */16

Analcime-Cstructure

8-ring in respect channel*/16

The influence of ultrasonic mixingMixing time : 3h Microwave heating time = 3h , NaOH = 2MSynthesis condition : Si/AL = 1.9, heating temperature = 120Q : Quartz SiO2U : Unnamed zeolite Na6[AlSiO4]6!4H2OP1: Zeolite P1(Na) Na6Al6Si10O32!12H2O*/16

The influence of ultrasonic mixingMicrowave heating method : mixing time 24h, heating time 6hUltrasonic assisted microwave heating method : mixing time 3h, heating time 6hSynthesis condition : Si/AL = 1.9, CNaOH = 2M, heating temperature = 120Q : Quartz SiO2 P1: Zeolite P1(Na) Na6Al6Si10O32!12H2OU : Unnamed zeolite Na6[AlSiO4]6!4H2O A : Analcime-C Na(Si2Al)O6!H2OU*/16

ConclusionZeolites are synthesized successfully from lake sludge by using microwave heating method.Microwave heating requires shorter synthesis time. Output control is easy and fast. (10min is needed to ramp to target temperature while 20min for drying oven. Cooling down is done automatically after heating )In order to improve the synthesis of zeolites, the advantages of using ultrasonic mixing is studied. The XRD result shows that ultrasonic mixing is more effective than stirrer mixing. Mixing time is shortened from 24h to 3h.By calculating the energy 0.57kWh is needed for US mixing while magnetic mixing is 1.9kWh for 4 samples. Ultrasonic mixing required lesser energy.*/16

Thank you for listening */16

X[mg/g]C[ppm]Langmuir adsorption isotherm of the Cu2+ ion Si/Al=1.5, 90, L/S=5ml/g, 2M NaOHNaP1Si/Al=1.5, 150, L/S=5ml/g, 2M NaOHAnalcime-CSi/Al=2.5, 120, L/S=5ml/g, 2M NaOHNaP1, Species-PResults Adsorption of Cu2+ ion (30, 24 h)

X[mg/g]C[ppm]Langmuir adsorption isotherm of the Pb2+ ion Si/Al=1.5, 90, L/S=5ml/g, 2M NaOHNaP1Si/Al=1.5, 150, L/S=5ml/g, 2M NaOHAnalcime-CSi/Al=2.5, 120, L/S=5ml/g, 2M NaOHNaP1, Species-PResults Adsorption of Pb2+ ion (30, 24 h)

X[mg/g]C[ppm]Langmuir adsorption isotherm of the Cd2+ ion Si/Al=1.5, 90, L/S=5ml/g, 2M NaOHNaP1Si/Al=1.5, 150, L/S=5ml/g, 2M NaOHAnalcime-CSi/Al=2.5, 120, L/S=5ml/g, 2M NaOHNaP1, Species-PResults Adsorption of Cd2+ ion (30, 24 h)

Results Heavy metal adsorption(Xm : calculated by Langmuir adsorption isotherm equation)

Major phaseSynthesis conditionCEC (meq/100g)Xm(mg/g) for Cu2+Xm(mg/g) for Pb2+Xm(mg/g) for Cd2+NaP1, Species-PSi/Al=2.5, 120, L/S=5ml/g, 2M NaOH36253.155.340.9NaP1Si/Al=1.5, 90, L/S=5ml/g, 2M NaOH31331.741.135.2Analcime-CSi/Al=1.5, 150, L/S=5ml/g, 2M NaOH15819.637.324.0

Conclusions From lake sludge, several types of zeolites were successfully synthesized by hydrothermal reaction in alkali solution.

Zeolite Na-P1 and Zeolite Species-P that were formed at Si/Al ratio of 2.5 and reaction temperature of 120 showed the highest value of CEC (362meq/100g).

The L/S ratio showed no effect on the type of zeolite formed.

The zeolite product showed adsorption ability for Cu2+ (Xm=53.1mg/g), Pb2+ (Xm=55.3mg/g) and Cd2+ (Xm=40.9mg/g). These values were higher than those reported on previous study. (Activated carbon Xm(Pb2+)=35.7mg/g and artificial zeolite Xm(Cd2+)=38.55mg/g).

The artificial zeolite applied in various fields such as agriculture, fisheries, stockbreeding, civil engineering,architecture and environment improvement.

The example of utilizing the ability of cation exchange Soil improvement, water purification, water processing / sewage treatment

The example of utilizing the ability of adsorption Deodorization, moisture absorption, humidity regulation; the adsorption of the poisonous gas; waste oil processing; adsorption separation; the adsorption decomposition of the dioxin

The mechanism of microwave heatingMicrowave heating belongs to dielectric heating an internal heating method.The object to be heated is the heating element during heating. When it is put in the electric field of the microwave, molecules (permanent dipole) are subject to the radio forces. Molecules in electrical neutral state are displaced and polarized, they will vibrate violently according to the frequency of microwave. (In the case of 2450MHz, 2.45 billion times/sec.)ElectronicPolarizationOrientationpolarizationIonicpolarizationInterfacepolarizationDielectric polarization types by microwave heatingReference : Microwave Engineering homepage http://www.microwave.ne.jp/06/001.html

The mechanism of ultrasonicUltrasonic belongs to longitudinal wave that is transmitted through a medium.When sound source vibrates, the medium (water) around it is pushed or pulled resulting in periodical density change.The reduced pressure cause bubbles which didnt dissolve in water completely.Cavitation occurs when bubbles burst and water molecules accelerated by ultrasonic are considered to result in a good mix of the sludge - NaOH mixture in a shorter time.

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