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Application of nano-titania in water treatment
Dr. Radwa A. Elsalamony
Egyptian Petroleum Research Institute
EPRI
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Titanium dioxide, TiO2
Dr. Radwa A. Elsalamony EPRI1
Titanium dioxide, also known as titanium(I! oxideor titania,is the naturally occurrin oxide o! titanium, chemical !ormulaTiO2."hen used as a #iment, it is called titanium white, Pigment
"hite # (P"#!, or $I %%&'.
$enerally it is sourced !rom Ilmenite ore, Titanium dioxide occursin nature as well%known minerals rutile, anatase and &rookite.
It has a wide rane o! a##lications, !rom paint)sunscreen tofood coloring. Photocatalyst, Electronic data storagemedium, It can &e em#loyed !or solar energy con*ersion+ased on dye#olymer.'ynthetic sinle crystals and (lms o! TiO2are used as a
semiconductor)
and also in dielectric mirrors due to the hihre!racti)e index o! TiO2*2.+2.-.
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Photocatalyt
ic acti*ity ofTi,
Dr. Radwa A. Elsalamony EPRI
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Dr. Radwa A. Elsalamony EPRI/
Photocatalysisre!ers to the acceleration o! the rateo! chemical reactions *oxidation0reduction &rouht a&out &y the
acti)ation o! a catalyst, usually a semiconductor oxide, &yultra)iolet (! or *isi+le radiation.istory dates &acks to 1-2, when /u0ishima and 1ondadisco)ered that water can &e s#lit, i.e., simultaneously oxidi2edto oxygen and reduced to hydrogen, when a &ias #otential isa##lied to an 3illuminated4 TiO2 sinle crystal electrode. Thisremarka&le disco)ery marked the onset o! #hoto induced redoxreactions on semiconductor sur!aces. It was soon reali5ed thatsuch redox #rocesses could &e utili5ed !or en*ironmentalcleanup applications, when /ran3 and 4ard) in '%%,
showed the #hotocatalytic oxidation o! $56and 7,-8 usindi6erent semiconductor materials like Ti,) 9n,) $d7) /e,8and ",8.
Thus, a &rilliant start in Ti, #hotocatalysis was !ollowed &y
some nota&le de)elo#ments includin, metal ion doped Ti,*1--7, super-hydrophilic Ti,:lms *1--, anion doped
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Dr. Radwa A. Elsalamony EPRI7
;echanism of
Photocatalysis
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Dr. Radwa A. Elsalamony EPRI+
Ti, < hv = h+< e-
The #hoto%induced hole can oxidi5e a donor molecule(D!adsor&ed on the TiO2 sur!ace.
D < h+ = > DA-The stron oxidation #ower o! the holeena&les aone%electron oxidation ste# with water to #roduce ahydroxyl radical *:O.
1, < h
+
= >,1 < 1
,
-!. The
superoxide ion is a highly reactive particle, able tooxidize organic materials.
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Super-hydrophilicity
Dr. Radwa A. Elsalamony EPRI9
The su#erhydro#hilic e6ect is also caused to the#roduction o! holes&ecause the electrons tend toreduce the Ti*I;%cations to Ti*III%ions
e- < Ti
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"hy 5ano-si2ed Ti,@@
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The two most im#ortant #ro#erties o! a nano material, whichmakes it su#erior to other microsco#ic or macrosco#ic #articles!or a##lications in catalysis, are*i the high surface to *olume ratio, and*ii the uantum con:nement at the nano scale.The frst property results in catalysts with high sur!ace area andhih #orosity, which ensures enhanced reaction rates due to thehih le)el o! interaction o! the reactants with the acti)e sites.
The second #ro#erty o)erns the trans#ort o! electrons andholes !rom the &ulk to the sur!ace o! the material,whose lenthscale is also o! the order o! a !ew nanometers *called as electron=ohr radius.
>oreo)er, !or #hoto%a##lications, the catalyst should a+sor+)and not +loc3 or scatter, incident radiation, and generatecharge carriers &y &and a# excitation.This is #ossi&le only with nano%si5ed semiconductor materials
with suita&le &and a# enery. There!ore, owin to the enhancedmolecular trans#ort #ro#erties at the sur!ace, it is e)ident that
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Dr. Radwa A. Elsalamony EPRI-
?ano%TiO2#hotocatalysts ha)e &een synthesi5ed indi6erent shapesand morphologies)which include,nanoparticles,. nanorods, nanotubes, nanopillars andnanowire arrays, nanobowls, nanowhiskers, aerogels,nanosheets, opal and inversed opals
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Dr. Radwa A. Elsalamony EPRI18
'ynthesis o!
TiO2
$as
#hase
'olution
#hase
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7olutionphase
sol method(non-
hydrolytic
sol-gel!
sol-gelmethod
7ol*o-thermal
synthesis
Precipitation method
1ydrothermal synthesis
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7olutionphase
$om+ustionsynthesis
Electrochemical
synthesis
7ono-chemicalsynthesis
;icrowa*esynthesis
methodologies
;icelle andin*ersemicellemethod
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$hemical*apor
deposition ($D!
Physical
*apordepositio
n
7praypyrolysisdepositio
n
Basphase
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Dr. Radwa A. Elsalamony EPRI19
The fnal properties o! the TiO2 nano#articles like
the #hase com#osition *anatase C rutile, particlesi2e) porosity) surface area) +and gap andsurface hydroxyl content can &e tailored &y)aryin the reaction conditions like@the precursor compound (TiCl4, titanium(!"isopropoxide, etc.",hydrolyzing agent (in the case o# sol$gel synthesis",#uel (in the case o# solution combustion synthesis",molar composition o# the reactants,
reaction temperature,reaction time (ageing time",calcination temperatureandpresence o# gas atmosphere (air, %r, &'
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Preparation ofTi,
Precipitation;ethod
Eect ofprecursor
Eect ofcalcinations
temperature)
Degradationof 4lac3-+ dye
4y gamma rayirradiation
Eect ofpreparation
method)Degradation
of
p-nitrophenol
Preparation ofRuFTi,
Eect ofmetal loading)
Degradationof -
chlorophenol
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Photo%catalytic A##aratus
Dr. Radwa A. Elsalamony EPRI%
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Preparation of Ti, +y
Precipitation ;ethod
Dr. Radwa A. Elsalamony EPRI1
Titanium tetrachloride *TiBl7, 1+C was used as a #recursor!or #re#arin nanosi5ed TiO2 #owder &y #reci#itation method
usin ammonia solution as #reci#itatin aent and ethanolas dis#ersin aent.
G ml Ti$l? was dissol)ed in H ml distilled water in an ice%water &ath. The titanium solution was then slowly mixed with 8Hml distilled water and Hml ethanol under )iorous stirrin,
then ammonia solution was added dro#wise until p1 '. Durinthe ammonic addition, an intensi)e #reci#itation occurred.
A!ter the sol)ent was e)a#orated at &H$ for 27h, the#reci#itates were dried at 8HH$ !or 2h to remo)e ?7Bl, then
calcinedin an air stream !or 7h.
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Preparation of Ti, +y
J7ol-gelK ;ethod
Dr. Radwa A. Elsalamony EPRI2
A second method !or TiO2 nano#articles#re#aration sol%el method3. Ti*O7 sol was
#re#ared &y mixin Gml titaniumtetraisopropoxide *Ti*OB*B/27, --.+C, Aldrichwith GH ml isopropanol*Adwic, A.R. under )iorousstirrin.
The mixture was then allowed to undero #artial
hydrolysis at room tem#erature &y dro#%wiseaddition o! Gml isopropanol and ml 1$l *# /%7with constant stirrin.
Ti*O7 el was dried at 188 oB o)erniht then
calcined in an air stream !or 7h each.
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T l d l i f
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7ampl
es
Phase ratio
a
$rystal si2e a
(nm! 7peci:c
surface
area+
(mFg!
PoreRadiu
s
D* (r!c
*nm
Totalpore
olumec
(ccFg!
A R 4 DA DR D4
A GHH18
88 8
2.
+% % 9-.+ 7.1 8.21
A #HH 'G G H#.
#
%.
8- G?.8 #.' H.8G
A %HH &8 % H 8%.&
?#.?
- ?#.# #.' H.'
4 GHH 97 1- 11.
1
/7.
/-. 91./ /.1 8.1/+
4 #HH +2 7 8
2+.
/2.
1 % 21. /.- 8.891
Textural and structural properties ofTi,samples
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Dr. Radwa A. Elsalamony EPRI22
The euent water o! many industries, such as textiles)leather) paper) printing) cosmetics, etc., containslare amount o! ha5ardous dyes.These com#ounds can cause chanes in +iologicalcycles, #articularly in the #hotosynthesis #rocess. Thesedyes can +loc3 +oth sunlight penetration andoxygen dissolution, which are essential !or aFuatic li!e.>oreo)er, some o! these com#ounds can &ecarcinogenic Presence o! color and color%causin
com#ounds has always &een undesira&le in water !or anyuse. Thus there is a considera&le need to treat thesecolored euents &e!ore discharin them to )arious water&odies.
1a2ardous
Eect ofDyes
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Dr. Radwa A. Elsalamony EPRI2
4lac3-+ Dye
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Ti*O7el was o&tained at room tem#erature &y the addition o!concentrated ammonia solution */+C ?/ dro#wise to a
)iorously stirred dilute solution o! TiBl7*Gluka 1+C until a # -
was attained. The ammonia solution was added dro#wise to#re)ent #article adhesion and sudden rain rowth o! #articles.
The white hydrous Ti *O7
solution was irradiated under a#H$o source (5$RRT! with 8H 3By and at a dose rate of8.8?%# 3ByFh. The reactant solution was stirred mildly whileirradiatin it, so as not to &ecome alomerated with each other.
The #articles were then washed riorously and re#eatedly with&idistilled water to remo)e any remainin im#urities. A!ter thesol)ent was e)a#orated at HH$ for ? h, the #reci#itateswere dried at 8HH$ for h to remo)e ?
7Bl, and then
calcined at +88HB !or 7 h to et titania TiO2.
Ti,Anatase nano-powder Prepared
+y a Bamma Ray Irradiation
Dr. Radwa A. Elsalamony EPRI2+
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Dr. Radwa A. Elsalamony EPRI29
Bu%do#ed TiO2 nano#articles containin 8.+wtC Bu *II iondo#ant were synthesi5ed )ia a co-preceptation.
=riey, # mL ethanol solution o! 8.+ > o! Bu*?O/.9
2O was
added dro#wise to Ti$l?solution under stirrerin. The # )alue
o! the reaction solution was adJusted to ca. ' +y ammonia.
Then the &lue and dense colloid was !ormed. The colloid wasstirred ently !or 8h, and then washed riorously and re#eatedlywith &idistilled water to remo)e any remainin im#urities.
A!ter the sol)ent was e)a#orated at HH$ for ? h, the#reci#itates were dried at 8HH$ !or 2 h to remo)e ?
7Bl, and
then calcined in an air stream o! 788HB !or 7 h.
reparation of $u-doped Ti,
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Dr. Radwa A. Elsalamony
EPRI2
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7amples
$rystal
si2e of
Ti,
)nm(
7peci:c
surface
area
)mFg(
Pore
Radius
D* (r!
(nm!
Total
pore
olum
e)ccFg(
Acidity
MmolFg
m
N-Ti, 22.35 127.1 1.27 0.334 6055
$uFN-Ti, 16.91 115.8 1.13 8./27 9//7
$u-Ti, 18.62 60.8 1.81 0.476 13343
Textural and structural propertiesof Ti, $atalysts
Dr. Radwa A. Elsalamony EPRI2-
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P-5itrophenol
Dr. Radwa A. Elsalamony EPRI/8
Phenolic com#ounds are amon the mostre!ractory #ollutants #resent in industrialwastewater.Their hih sta+ility and solu+ility in waterre#resent the main o&stacles to com#leteremo)al.Puri(cation o! wastewater contaminated withthese #ollutants is )ery diKcult since they
are resistant to con)entional treatmenttechniFues.
The #%nitro #henol which are used in )ariousindustries like textiles) pulp) paper) leather)wool) sil3 etc. ultimately enter into aFuaticsystem as euent and create )ariousen)ironmental #ro&lems.
The #%nitro #henols exert )arious &iochemicaland mor holo ical e6ects on lants and
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?-5P concentration *s. irradiation timeusing dierent photocatalysts under
irradiation
Dr. Radwa A. Elsalamony EPRI/1
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Dr. Radwa A. Elsalamony EPRI/2
The apparent :rst-order 3ineticsfor the photocatalysts
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Dr. Radwa A. Elsalamony EPRI2
Gor meso#orous TiO2materials, 8.# g of tetra&utyltitanate was dissol)ed in a&solute ethanol with aweiht ratio o! 10 under stirrin. The resultinsus#ension was stirred !or / h at room tem#erature,and then G ml of deioni2ed water was addeddro#wise.
The solution was stirred !or an additional 2 h,
!ollowed &y e)a#oration at 1+8 oB. The o&tained solid#roduct was exhausti)ely washed with deioni5edwater and ethanol, dried at 8 oB o)erniht, and thencalcined at +88 oB !or / h.
reparation of mesoporous Ti,
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Ru0TiO2 sam#les with Ru loadin ranin !rom 8.2 to8. C *w0w usin TiO2was #re#ared &y inci#ient wetim#renation method with an aFueous solution o!ruthenium trichloride trihydrate. An a##ro#riateamount o! the #recursor, so as to o&tain the desiredRu concentration in TiO2, was mixed with TiO2indistilled water.
The resultin slurry was su&Jected to continuous
stirrin at am&ient tem#erature, and su&seFuentlydried in an o)en at 118 oB !or 18 h. The solidresidue was then crushed and calcined in air !or + h.
reparation of RuFTi, samples
Dr. Radwa A. Elsalamony EPRI2-
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Textural and structuralproperties of Ti, and RuFTi,
samples
7amplesAnataseC
Rutile
$rystalsi2e 7peci:c
surfacearea
(cmFg!
PoreRadius D*
(r!(nm!
Total pore*olume(ccFg!DA DR
Ti, 8 @ /8 //.+ +8.9 2. 9.2 8.12/
H. RuF Ti, ## C 888.%
% &.G #.# H.G
H.? RuF Ti, G% C ?8 &.&GH.#
8.? %.' H.H%
H.# RuF Ti, 99 @ /7 1-.7 2/. 27. 9.9 8.12
H.& RuF Ti, 9/ @ / //.9 9.+ 22.- 9.1 8.8-7
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Dr. Radwa A. Elsalamony EPRI/7
-$lorophenolThey can &e !ound in round waters, waste waters
and e)en low #ollution le)els. They miht #roducedisareea&le taste and odor to drinkin water atconcentrations &elow 8.1 L %1 and ad)erse e6ectson the en)ironment.Bhloro#henols are thus !ound on &oth the .7.En*ironmental Protection Agency list and the
European community red list of priority.B#s are into the en)ironment as a result o! se)eralman%made acti)ities. =ecause o! their &roads#ectrum antimicro&ial #ro#erties, B#s has &eenused as preser*ati*e agents for wood) paints)*egeta+le :+ers and leather and asdisinfectants. In addition, they ha)e &een widelyem#loyed in many industrial #rocesses as synthesisintermediates or as raw materials in themanu!acturin o! her&icides, !unicides, #esticides,insecticides, #harmaceuticals, dyes, and in themanu!acture o! #a#er B#s may &e also eneratedas &y%#roducts durin waste incineration, the
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Dr. Radwa A. Elsalamony EPRI/1
Eect of Ru doping concentrations on the O$Pphotodegradation using irradiation
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Dr. Radwa A. Elsalamony EPRI/
/ormation of chloride ions during thephotodegradation of O$P using light
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/ormation of acetate ions during thephotodegradation of O$P using light
Dr. Radwa A. Elsalamony EPRI/-
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Dr. Radwa A.Elsalamony
EPRI
T1A5
7