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I/ Gii thiu v Zeolite
Theo ting Hy Lp Zeo: si, Lithot: , v vy zeolite cngha l si.
Zeolite bt u c pht hin t nm 1756 bi Cronsted. Bronstedt l mt nh khong hc ngi Thy in pht
hin ra mt loi khong mi vi tn gi Zeolite. ng pht
hin ra Zeolite nh hi nc thot ra khi nung khong ny. Nm 1944, Barrer v Ibbitson ch ra hiu ng ry phn
t cho php tch cc n v iso-parafin. Nm 1956, cc Zeolite u tin c tng hp.
Hin nay c khong hn 15000 cng trnh cng b v10.000 pht minh sng kin tng hp zeolite.Nh vy zeolite c tm quan trng ln lao trong khoa hc vk thut.
1/ Ngun gc- nh ngha:
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Zeolite qua knh hin vi in t-trong t nhin
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Phn loi
Theokch thcmao qun
Theo
thnh phnha hc
2/ Phn loi
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mao qunrng
7 8 A0
mao qun trungbnh
5 6,9 A0
mao qun hp
< 5 A0
S nguyn t O trong1 ca s
ng knhmao qun ( A0 )
Loi zeolite
8 ( mao qun hp ) 4,3 A , Erionit
10 ( mao qun trungbnh ) 6,3 ZSM-5, Ferrierit
12 ( mao qun rng ) 8,0 X, Y, Mordenit
Phn loi da theo kch thcmao qun
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Phn loi theo thnh phn hahcTheo quy tc Loweinstein xc nh rng :
2 nguyn t Al khng th tn ti ln cn nhau, ngha l cu trc zeolite khng th tn ticc lin kt Al-O-Al m ch c cc lin kt Si-O-Al hay Si-O-Si
Ni cch khc ch tn ti loi t l Si/Al 1
TPHH
Zeolite ngho Si giu AlH zeolite
anuminophotphat
Zeolite c hm lngtrung bnh
Zeolite giu Si
Zeolite giu Si tch Al
Ry phn t zeolite
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Phn loi theo thnh phn hahc
Zeolite ngho Si giu Al
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Zeolite c hm lng Si trung bnh
Phn loi theo thnh phn hahc
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Zeolite giu Si & ry phn tzeolite
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Zeolite giu Si
Ry phn t zeolite
Phn loi theo thnh phn hahc
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Zeolite giu Si tch nhm
Bng cc phng php sau tng hp , ngi ta c th bini thnh phn ha hc ca zeolite. Mt s phn ng ha hcc th tch Al khi mng li tinh th v thay vo l Si
hoc nguyn t ha tr III hoc IV khc. Phng php ny cgi l phng php loi nhm tc l dsalumination.
Thng thng ngi ta dng zeolite X hoc Y c t l Si/Al =1,2 2,5 , sau khi loi nhm th thu c zeolite giu Si c tl Si/Al 9. vi phng php ny nu zeolite thu c c t lSi/Al > 9 th s ph v mng li tinh th ca zeolite.
Phn loi theo thnh phn hahc
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H zeolite aluminophotphat( AlPO )
Gn y c mt h cht rn mi c cu trc tinh th tng t zeolit gi lAluminophotphat (AlPO) c pht minh bi cc nh nghin cu ca Linhip Carbide trn c s cc nguyn t l Al v P.
Vt liu ny khng c cu to t cc t din SiO4 v AlO4- m c cu tot cc t din AlO4- v PO4+ theo t l 1:1 nn trung ha v in tch.
V cu trc trong h ny c loi AlPO-5 c cu trc hnh hc tng t hFaujazit v loi AlPO-11 c cu trc hnh hc tng t zeolit ZSM-5.
Cc c trng c bn ca cc AlPO l u c t l Al/P = 1, khng c mt cacacbon b tr, khng c kh nng trao i cation v v vy khng c tnh xctc.
Phn loi theo thnh phn hahc
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Cc bin tng ca AlPO l SAPO v MeAPO.
SAPO: khi a vo AlPO mt lng nh Si thay th P th vt liu thu
c gi l SAPO vi khung in tch m v do c kh nng trao ication.
MeAPO: nu a cc nguyn t khc nh Co, Mn, Fe, V, Ga... voSAPO th nhn c h ry phn t mi, k hiu l MeAPO, km theo
l s thay i tnh cht axit - baz, oxy ha kh ca vt liu. V cutrc hnh hc cc vt liu Co-APO, Mn-APO, V-APO c cu trc tngt AlPO5, AlPO11, AlPO17, AlPO31.
H zeolite aluminophotphat( AlPO )
Phn loi theo thnh phn hahc
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3. Cc loi Cu trc
Zeolita. Cu trc Zeolite tng qutb. Cu trc Zeolit A, X, Yc. Cu trc ZSM5d. Cu trc USY
Ngoi ra cn c zeolite aluminophotphat cu tot cc t din AlO4- v PO4+ nh AlPO-5
(ging Zeolite X,Y) ALPO-11(ging ZSM5).
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a. Cu trc Zeolite tngqut:Cng thc chung:
Me2/n.Al2O3.xSiO2.yH2O Me: kim loi kim hay kim th
n:ho tr ca kim loi
3. Cc loi Cu trc
Zeolit
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Cu trc s cp
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1.Tm: Al hay Si2.nh: O
3. Cc loi Cu trcZeolit
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Cc t din trn lin kt vi nhau quanguyn t oxy thnh Cu trc th cp
a. Cu trc Zeolite tngqut:
3. Cc loi Cu trcZeolit
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b. Cu trc Zeolit A, X,Y
Cu trc th cp: hnh bt din ctgm :
8 mt lc 6mt vung 24 nh(Si v Al) 36 cnh (v tr ca O)
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Cu trc Zeolit A(LTA)
Cc soalit ghp ni
vi nhau ti cc mt4cnh thng qua trunggian lng tr to thnhZeolite A
b. Cu trc Zeolit A, X,Y
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Cu trc Zeolit A (LTA)b. Cu trc Zeolit A, X,Y
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LTA
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LTA
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Cu trc Zeolit X,Y
Sodalit ghp vi nhau ti ccmt 6cnh thnh Zeolite X,Y
kch thc l Zeolite A< X,Y
T l Si/Al ca Zeolit X
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Cu trc Zeolite Xb. Cu trc Zeolit A, X,Y
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FAU
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Zeolite siu bn
USYXc tc mi yu cutch bt Al ra khi mngZeolite, gim hm lng
Na trong Zeolite tngkh nng to olefin.Zeolite siu bn
(UltraStable Y : USY). bn cao hn nhiu
so vi Zeolite Y truynthng.
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c. Cu trc USY
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Cu trc th cp:12 t din SiO4/2 vAlO4/2 ghp vi nhaunh hnh bn to
d. Cu trc ZSM-5
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Cc chuilin ktthnh lp
d. Cu trc ZSM-5
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d. Cu trc ZSM-5
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S phn b cc tm acid l mt yu t nh hngc bn n hot tnh v tnh chn lc ca Zeolite.
V d : Mt Zeolite c UCS thp t tm acid trn1 . Cc tm acid t, li cch xa nhau nn trnhc phn ng Chuyn hydro, do lm tng chs Octane ca xng cng nh tng hiu sut thusn phm C3 vcc sn phm nh hn.(S tng
ch s Octane ny l do nng cao ca Olefintrong xng).Zeolite USY c UCS thp c hot tnh km hn loi
REY truyn thng. Tuy nhin, Zeolitec UCS thpc kh nng gi c hot tnh di iu kin
hot ng khc nghit ca qu trnh, do cnc gi l UltraStable YZeolite mi sn xut c UCS kh cao trong
khong 24.5 n 24.75 A. Mi trng nhit vthy nhit trong thit b ti sinh rt cc nhmalumina (AlO2) lm gim UCS.
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ZSM-5 l mt loiZeolite c cu trc xpkhc vi Y-Zeolite. Kch
thc l rng ca ZSM-5 nh hn so vi Y-Zeolite (5.1-5.6 so vi8-9).
Thm vo , s spxp l rng ca ZSM-5khc so vi Y-zeolite.
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4. Tnh cht b mt caZeolit
4 Tnh cht b mt ca
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a. Tnh trao i ion
S oxy ha ca Si:+4, Al:+3
Tm Si trung ha in
Tm Al t ch in m trung ha bi 1iondng( ion kim hoc kim th) trao i ion
4. Tnh cht b mt caZeolit
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a. Tnh trao i ion
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Khng lm thay i cu trctinh th
v tr khc nhau, tc traoi khc nhauov tr m(b mt) : d dngo v tr kn (soalit, lng tr):
kh khn
a. Tnh trao i ion
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tng trao i ion:o x l vi dd cha ion trao i nhiu ln
o Gia cc ln phi sy kh v x lnhit(nung 5000C)o Phn b ng u cation cc v tr khc
nhau
o 1phn cation di chuyn t v tr kn mo d trao i
a. Tnh trao i ion
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Trao i ion hnh thnh tm axit
Qu trnh hnh thnh tm axit:
4. Tnh cht b mt caZeolitb. S hnh thnh cc tm axit
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T0C
TmLewis
Cli k t dit M t t t t l
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Khi tin hnh x l nhit khong nhit 400 500oC th xut hin cc tmaxt Lewis theo s sau:
Cc ion nhNa+,Mg2+ hay proton s trung ho in
tch ny v hnhthnh tm axitBronsted
4 T h h b
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o Cc Tm axit to nn hot tnh xc tc
o T l Si/Al tng s tm axit gim, bn tm axit tng
o v tr khc nhau linh ng cacc proton khc nhau axit khngng u.
4. Tnh cht b mt caZeolitb. S hnh thnh cc tm axit
4 Tnh cht b mt ca
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4. Tnh cht b mt caZeolitc. Tnh chn lc hnh hc
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4 d Z lit
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Trong ha phn tLm cht xc tc
Cc qu trnh tch
Lm cht trao i ion
4. ng dng ca Zeolit
4 d Z lit
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Tch C2H2 ra khi butadien,khng kh lng
Tch NO ra khi kh v cht lng
Lm kh cc cht lng v hi
Tch hi du khi kh nn
Tch CO khi He v H2
ng dng chocc qu trnh
tch
4. ng dng ca Zeolit
4 d Z lit
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Dng
AgA
lm
chth
mu
tron
gchn
khn
g
Lmctp
hntch
trongsck
khhpph
Phntch
m
Haphntch
4. ng dng ca Zeolit
4 d Z lit
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o i ion
Nhng cation kim loi c th b tch rakhi nc thi : Cu2+ , NH+4, Pb2+ ,Zn2+ , Hg2+ , Cr3+ , Fe3+ , Cd2+ ,
Ca2+ , Al3+ , Cs2+ , Sr2+ .
c trao i vi Ag to thnh
NaAAg, gii quyt 1 lng nhnc ngt khi gp nn bin
4. ng dng ca Zeolit
4 d Z lit
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Lm cht xc
tc
Lm cht xctc cho phnng ng phnha C5, C6
nhm nng caoch s octan
Lm cht xctc cho qutrnhCracking,ehydro,ehydrat( USY dngtrong FCC )Fe-ZSM-5 :
xc tc chohn n
Dng lm chtmang cho cc
loi xc tckhc.
4. ng dng ca Zeolit
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Gas separation membrane using zeolite
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Zeolite Gas-Pump With No MovingParts, But With A High Rate Of Gas
Flow
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Dr Peter Maier-Laxhuber & Zeolite Cooler
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Dr. Peter Maier-Laxhuber, et al.
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Zeolite Heat
Pump withIntegrated Ice-Storage
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Oil Purification
Zeolite StationMCU-4,3
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II/ T NG HP ZEOLITE
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II/ T NG HP ZEOLITE
Zeolite l cc aluminosilicat ngm nc,c hnh thnh di cc iu kin thunhitNgha l mt h lng, cha cc thnhphn ho hc thch hp c kt tinh
di tc dng ca nhit.
1. Nguyn tc chung
Ph h hi l
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Phn ng thu nhit lg?
Co nhieu nh ngha va nhan nh khac nhau : Morey & Niggli (1913) ,
Rabenau (1985) , Lobachev (1973) , Yoshimura(1994)
Phan ng thuy nhiet la bat c phan ng d the vi s co matcua dung moi (nc hoac khong phai la nc) dien ra tai nhiet oln hn nhiet o phong va ap suat ln hn 1 atm trong 1 thiet b kn.
V phan ng dien ra can s co mat cua pha long nhng nhiet ocan at ti lai qua cao khien cho pha long khong ton tai c nenphai dung en ap suat cao e at en nhiet o cho phan ng xay
ra ma van am bao con moi trng cho cac tac chat
Qua trnh thuy nhiet c tien hanh trong cac thiet b chu ap suatcao va nhiet o cao goi la autoclave
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ieu kien tonghp Zeolite
Nguyn liu u: hot tnh cao
pH mi trng: kh kimNhit : thpp sut: thc hin p sut hi bo ha ca ncMc qu bo ha ca dung dch kt tinh phi
ph hp khng qu ln cng khng qu b.
1. Nguyn tc chung
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Qu trnh to gel
Qu trnh lm mui
Qu trnh kt tinh
Qu trnh lc ra
Qu trnh kt tinh Zeolite gm cc giai on:
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Qu trnh to gel: quan trng nhto Ch xy ra trong dung dch, mi trng kim mnho Ch to thnh trong khong gii hn t l Si/Al thch hpo Hnh thnh lin kt Si-O-Al trong khung gel do tng tc ca dd silicat v
aluminate phn ng a trng ngng:
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Qu trnh lm mui: cn thit cho tomm tinh th
o Mm tinh th bt u hnh thnh trong phalng ca gel hoc ti b mt phn cch pha (gel-dd)
o Khi cu trc tinh th c to t cc t din[SiO4] v [AlO4]
Pha rn v nh hnh Pha lng
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Pha rn v nh hnh Pha lng
Gel aluminosilicate ban u
Pha rnv nh hnh
Kt tinh gel Pha lng
Hnh thnhmm tinh th
Kt t li thnhtinh th zeolite
un nng
t0C ha tan lm nng tng phn na t
T xc tc lm tng tc ha tan pha rn v nh hnh
SN PHM KT TINH
QU TRNH KT TINH ZEOLITE
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Qu trnh lc ra:o Loi lng kim cha trong cc xoang
tinh th. Cng sch kim, cht lngZeolite cng cao
oThc t, pH nc ra cn khong 8-9 lt yu cu.
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Trong cc yu t nh hng qu trnh kt tinh, bncht v tnh cht zeolite, thnh phn gel ban u l quan
trng nht.
Cc yu t
nhhngn qutrnh tng
hpZeolite
Na2SiO3 NaOH Al(OH)3
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Na2SiO3 NaOH Al(OH)3
NaAlO2
H2O
H2O
To gel
Lm mui
Kt tinh
Lc
H2O thi
H2O m
Sn phm
S QUY TRNH TNG HP ZEOLITE
2.Tng hp Zeolite t hp cht v ckh t
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Nguyn liu
Cc Zeolite t nhin c tinh ch, loi b tp cht.
Cc ngun nguyn liu t nhin: kaolin, t st c bin tnh bng ha cht
Thnh phn gel:
SiO2/Al2O3 = 1,3- 2,2Na2O/SiO2 = 1,7- 2,8
[Na2O] =0.33- 0.92 mol/l
a. Phng php tng hp
zeolite A
g p pkhng c cu trc
a Phng php tng hp
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Phng php 1:To gel aluminosilicat t thy tinh lng hay tinh th natri silicattrn vi natri aluminat bng cch khuy trn nhit phng( thng l 3 gi)
Kt tinh hn hp trn iu kin bnh thng (theo nh s kt tinh nu phn trc).Phng php 2:
To gel ban u bng cch rt dung dch natri silicat vo natrialuminat trong kim nhit kt tinh v khuy u.
Tinh th Zeolite thu c trng hp ny c kch thc lnhn cch tng hp theo phng php 1.
a. Phng php tng hpzeolite A
a. Phng php tng hp
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Na2SiO3
NaOHNaAlO2
t0 kt tinh
khuy u
To gel
Phng php 2:
a2SiO3 NaOH Al(OH)3
NaAlO2
H2O
To gel
t0 phng
Phng php 1:
a. Phng php tng hpzeolite A
a Phng php tng hp
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Cc yu t nh hng
Nhit : tng hp p sut thng th khong nhit dao ng khrng.
p sut: thng tng hp p sut kh quyn.
Thi gian kt tinh: t 8-12h trong u kin khuy lin tc nhit ~90oC.Nu nhit tng th thi gian kt tinh sn phm gim i.
Hm lng kim: nng qu cao th thi gian kt tinh di, nhngnng thp th kh kt tinh c gel aluminosilicat.
Hm lng nc: nh hng n qu trnh to gel ban u, hm lngnc cng cao th trng kt tinh ca NaA cng rng
a. Phng php tng hpzeolite A
a. Phng php tng hp
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a. Phng php tng hpzeolite A
b Phng php tng hp zeolite
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Zeolit X: SiO2/Al2O3 =2-3 ; Zeolit Y: SiO2/Al2O3= 4
Nguyn liu: natri silicat, natri aluminat, NaOH v cc
cht khc.Thnh phn gel tng hp Zeolite NaX: SiO2/Al2O3 = 2,2-3.2 Na2O/SiO2 = 1.0-2.3 H2O/Na2O =25-65Thnh phn gel tng hp Zeolite Y: SiO2/Al2O3 = 8 Na2O/SiO2 = 0.4 H2O/Na2O =10
b. Phng php tng hp zeoliteX,Y
NaAlO2 Kt tinhDd c khuytrn kt t
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TB phn ng
TB kt tinh
Lc khung bn
Ra
Nghin
To vin
Sy
Sng quay
L nung
zeolite
Na2O.nH2O
Loi kim d
m 35%
120-150oC
Loi bi
Dng tinh th
30-40 ph m 35%
Zeolite A: 80-90oC trong 6
Zeolite X: 95-100oC trong12hZeolite Y: 990C trong10h. pH 10,5
Tch dd thu kt tahydro Aluminosilicat
trn, kt tthnh ta gel xpAluminosilicat
575-6500C624h
Tng hpzeolite loiX,Y
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c. Phng php tng hp
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vCc phng php iu ch zeolite Y c t
s Si/Al caoTng hp zeolite Y c t s Si/Al ~2.5, sau tng t s Si/Al bng
phng php sau:
X l nhit v nhit hi nc
X l ha hcKt hp x l thy nhit v x l ha hc
Tng hp trc tip: Phng php ny kh thc hin, hn na tnghp zeolite Y c Si/Al cao hn 33.5 l khng th thc hin c quy m cng nghip
g p p g pUSY
vCc phng php iu ch zeolite Y c t sSi/Al cao
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X l ha hc: tch Al t zeolite thng thng km theocc phn ng gia zeolite vi cc tc nhn ha hc. C2 trng hp :
Trng hp c th Si vo mng:
Tch nhm vi (NH4)2SiF6
Tch nhm bng SiCl4Trng hp khng th Si vo mng:
Bng tc nhn selat
Bng cc halogen bay hi Bng flourin
Si/Al cao
vCc phng php iu ch zeolite Y c t s
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X l nhit v nhit hi nc :
Nung zeolite Y trao i vi NH4+ trong mitrng hi nc nhit cao
Trong qu trnh tch nhm c th lm ph v mtphn cu trc ca tinh th zeolite to ra mt s
dng oxyt nhm ,oxyt silic ,aluminosilicate v nhhnh
Kt hp x l nhit v x l ha hcPhng php ny nhm chuyn zeolite Y dng
amoni (NH4+-Y) thnh dng siu bn bng x lnhit,tip n x l Al bng phng php ngoimng.
vCc phng php iu ch zeolite Y c t sSi/Al cao
c. Phng php tng hp
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Tng hp USY
o K thut truyn thng s dng nhit cao 1300oF n 1500oF(704oC n 816oC) dng hi nung zeolit HY
o Lc bng axit, trch li ho hc v thay th ho hc l tt c ccdng ca tch nhm, dng ph bin trong nhng nm gn y.
o u im chnh ca nhng qu trnh ny so vi tch nhm truyn
thng l vic loi b ca zeolit khng c nhm trong khung hay lht gi Al2O3trong lng cu trc zeolit.
g gUSY
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S kt tinh, trao i ion v bin tnh cu trc Zeolite Y(RE: cation ca nguyn t t him)
d Ph h h
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Qua trnh tao
el
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d. Phng php tng hpZSM-5
d Ph h t h
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d. Phng php tng hpZSM-5
d. Phng php tng hpZSM 5
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Template : cht to cu truc
nh hng n qu trnh gel ha v to nhntinh th : to ra nhng hnh thi nh trc cho
qu trnh to nhn v tinh th
Lm bn b khung nh cc tng tc lc ht H,tnh in
Tng kh nng tng hp c hm lng Si cao
ZSM-5
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TMA +tetramethylammonium cations
(TPA+ ) tetrapropylammonium saltsTEA Triethanolamine
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d. Phng php tng hpZSM 5
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SolSiO2
Al2O3+
DdNaOH
Template+
Mm
Gel
130 -220 oC
15- 75 gipH= 10-10,5
Lc,Ra
NaZSM-5
ZSM-5
2.Tng hp Zeolite t hp cht v c ccu trc
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Kaolin l mt khong sn phi kim c hnh thnh do qu trnhphong ha ca phenpat ch yu l octodaz v anbit. Qu trnhphong ha trn c gi l qu trnh kaolin ha.
Ngun kaolin Vit Nam d bo khong 15 triu tn, hmlng Al2O3 trong kaolin khong t 29% n 50%. Qungkaolin tp trung ch yu cc tnh nh Lo Cai, Yn Bi, Ph
Th, Qung Ninh, Tuyn Quang, Lm ng, ng Nai
Cng thc ha hc: Al2O3.2SiO2.2H2O Thnh phn l thuyt: Al2O3 39,48%
SiO2 46,6%
H2O 13,92%
T trng: 2,57 2,61 cng: 1 -2,5
CHUYN HA KAOLIN THNHZEOLITE
cu trc
Kaolin bt+NaHCO3
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Nghin
Lm mn
nh hnh
Lm kh
NungTch bi
Kt tinh dng quay
RaSy
Zeolite
30-40
m 33-34%
m 15-17%
6000C12-24h
95-1000C
pH~11,5
CHUYNHAKAOLINTHNHZEOLITE
CHUYN HA KAOLIN THNH
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CHUYN HA KAOLIN THNHZEOLITE
References
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References Properties, Preparation and Application of
Zeolites (Wolfgang Schmidt , Dr. rer. natMax-Planck-Institut fr Kohlenforschung)
http://www.grace.com/EngineeredMaterials/MaterialSciences/Zeolites/ZeoliteStructure.aspx
www.oilgasportalvn.com
Introduction to zeolite science and practice 3rd revisededition
Zeolitic Materials: Ion Exchange and Shape Selective-
Catalysis Angus P. Wilkinson-School of Chemistry andBiochemistry-Georgia Institute of Technology
Catalysist by Metal containing Zeolites( Martin Wallau andUlf Schuchardt- Campinas Brazil)
References
http://www.oilgasportalvn.com/http://www.oilgasportalvn.com/ -
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Gio trnh xc tc d th (H S Thong)
Nghin cu tng hp zeolite A,X v kho st kh nng s dng lm kh ru (Lun vn cao hc- GV Nguyn Th Thu Vn)
Atlas of Zeolite Framework types- Fifth revised edition- 2001
Gio trnh k thut xc tc- Thy Mai Hu Khim
ZSM-5 type zeolites:Synthesis and use in gasphase reactions with ammonia- F.J. van derGaag
References