Nhm 5

1. Trn M Anh 61100145

2. ng Th Hng 61101032
3. L Thin Thy Nh 61102455
4. Nguyn c Minh Trang 61103728
5. L Trn Phng Uyn 61104155
1
Tm hiu v pha tnh Silica
gel v Alumina trong sc k
hp ph
10/28/2014
Ni dung
1. Silica gel
Nguyn tc, phng php iu ch
Cu trc
Phng php xc nh cu trc ca cht
iu kin s dng
V d ng dng thc t
2. Alumina
3. So snh gia Silica gel v Alumina
2 10/28/2014
3 10/28/2014
Silica gel
Cng thc phn t: SiO
2
.nH
2
O

Silica gel pha thun
4 10/28/2014
Phng php iu ch
Silica gel pha thun c ch ha
Thay nhm -OH thnh cc nhm chc phenyl, cyano,
amino, diol,
ci thin tnh phn cc ca pha thun, tnh bn vi
cc loi dung mi
5 10/28/2014
Phng php iu ch
Silica phenyl Silica diol
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Phng php iu ch
10/28/2014 7
Phng php iu ch
8 10/28/2014
Phng php iu ch
Silica gel pha o
9 10/28/2014
Cu trc
Gm 3 nhm chc:
Silanol t do
Silanol kt hp
Siloxane
Tm hot tnh: Si-OH

Hydrogen bonds
Siloxane
Isolated
hydroxyl
groups
10 10/28/2014
Cu trc
Khi b mt silica hp ph nc
Hot tnh tm hp ph gim
iu chnh hot tnh bng cch iu chnh
lng nc

10/28/2014 11
12 10/28/2014
Cu trc
Silica gel pha o

Xc nh din tch b mt v phn b l xp: BET
(thng s dng hp ph kh Nit 77K)
Phng trnh BET:


S
BET
= X
m
.A
m
.N.10
-18
(m
2
/g)
X
a
= hp ph ca Nit (moles/gam cht hp ph)
X
m
= hp ph n lp ca Nit (moles/gam cht hp
ph)
C l hng s, N l hng s Avogadro
A
m
khi lng phn t Nit
13 10/28/2014
Phng php xc nh cu trc
( )
0
0
1 1
a m m
p p C
.
X p p X C X C p

= +

Xc nh s nhm silanol Si-OH: Ph IR

14 10/28/2014
Phng php xc nh cu trc
Peak (cm
-1
) Band assignment
3700-3550 OH stretch silanol groups
3400-3500
OH stretch hydrogen boded silanol
groups
4540
Combination band OH stretching
and bending silanol groups
5265
Combination band OH stretching
and bending water molecules
6800-7300
Overtones of OH stretch silanol
groups and hydrogen bonded
silanol groups
o cn hng ngoi Table 1. Mid-IR and NIR Band assignments
for water adsorbed silicagel samples.
15 10/28/2014
Phng php xc nh cu trc
Xc nh s nhm silanol Si-OH: phng php
Deuterium exchange (DE)
Xc nh nng ca nhm hydroxyl trn b mt
Da trn s trao i gia D
2
O vi nhm -OH trn
b mt silica gel
Da vo nng [H]/[D] xc nh c s
nhm OH
16 10/28/2014
Phng php xc nh cu trc
Xc nh kch thc ht v kch thc l xp ca silica
gel: phng php knh hin vi in t qut (SEM)
17 10/28/2014
Phng php xc nh cu trc
18 10/28/2014
Phng php xc nh cu trc
Kh nng hp ph nc ca Silicagel

19 10/28/2014
Phng php xc nh cu trc
10/28/2014 20
iu kin s dng
SILICA GEL PHA THUN SILICA GEL PHA O
Cn hot ha trc khi s dng
Khng sy qu lu trnh lm mt
nhm silanol bt hot
Ty cht cn phn tch m hot
ha silicagel khc nhau
Khng cn hot ha trc khi s
dng
Th t ra gii cc cht: nhm
COOH alcol/phenol amin
ether/aldehyde cetone hp
cht halogen alkan
Kch thc cc l l 40, 60 v 100
, trong Si-60 dng nhiu nht
- Khi lng ring xp t 0,4-0,6
g/cm
3
, nhiu nht l 2,2 g/cm
3

i vi sc k ch ha s dng
trong PTN: thng dng loi c
kch thc 15-25 m, 25-40 m
hay 40-63 m
Silica gel c gn mt chui carbon
di thng l 18C (C-18) hay 8C
(C-8): SiOSini Carbon
10/28/2014 21
SILICA GEL PHA THUN SILICA GEL PHA O
Tu theo vic chn dung mi
dng tch cc hp cht base
(alkaloid) hay hp cht a du.
Phn tch cc cht c phn
cc gn vi n.
Silica gel l s la chn tt nht
lm pha tnh khi phn tch cc
cht c khi lng phn t nh (<
2000 Da)
Dung dch thn nc c th i qua
H thit lp cn bng nhanh
chng

Kh nng tch ca silica gel tt
hn khi tm n bng dung dch
AgNO
3
10-12%, dung dch acid
boric, ammoniac, dung dch m
phosphate
Tch tt i vi cc cht phn cc
iu kin s dng
V d
10/28/2014 22
V d
10/28/2014 23
V d
10/28/2014 24
10/28/2014 25
Alumina
Cng thc phn t: Al
2
O
3
10/28/2014 26
Phng php iu ch
Mui Al thy gii to kt ta keo trng Al(OH)
3

nhit phn to alumina Al
2
O
3
Al(NO
3
)
3
+ 3NH
3
+ 3H
2
O Al(OH)
3
+ 3NH
4
NO
3


Al(OH)
3
Al
2
O
3
+ H
2
O
C th iu chnh pH ca dung dch phn ng
sn xut ra ht alumina vi b mt c tnh acid, tnh
kim, hay trung tnh.


10/28/2014 27
Phng php iu ch
28 10/28/2014
Cu trc
Ty thuc vo s phn hy nhit ca aluminium
hydroxides v oxyhydroxides nhiu trng thi tinh th
khc nhau: o, _, q, o, k, u, ,
29 10/28/2014
Cu trc
Cu trc ca -Al
2
O
3
Tm hot tnh: Al
3+
, O
2-
Hot tnh gim khi Al
2
O
3
ht m
30 10/28/2014
Cu trc
Al
3+
: acid Lewis, in tch dng
hp ph cc cht giu electron
(nh aren hay alcen)
Bng: Nng lng ta ra ca Al khi hp
ph CO
Al
III
Al
IVb
Al
IVa

AE
ads
-74 -46 -34
O
2-
: base Lewis hp ph cc cht cho proton
Kh nng hp ph ca cc tm O: O
2b
> O
2a
> O
3b
> O
3a
(PDOS technical analysis)
Xc nh s nhm -OH xung quanh nguyn t Al:
Ph IR

31 10/28/2014
Phng php xc nh cu trc
Xc nh kch thc tinh th: phng php knh hin
vi in t qut (SEM)
32 10/28/2014
Phng php xc nh cu trc
10/28/2014 33
Phng php xc nh cu trc
10/28/2014 34
Tm ra hnh th mng c s v cc v tr ca nguyn
t Al, O: phng php nhiu x tia X XRD
Phng php xc nh cu trc
35 10/28/2014
iu kin s dng
Mun hot ha alumina sy loi b lng nc hp ph i.

Alumina c nhiu c ht, ht cng b kh nng hp ph cng cao.

Trong sc k, c 3 dng alumina: trung tnh, acid, base.

xp ca alumina khong 0,9 g/cm
3
n 4,0 g/cm
3
.
36 10/28/2014
iu kin s dng
Alumina phn tch tt cc cht phn cc yu n trung bnh,
thng dng phn tch cc hp cht thm (c i lc mnh vi
OH phenol) v cc HC ng phn ca n.

Cn dng tch: hydrocacbon, alkaloid, cht mu thc phm,
lipid, vitamin, carotene, acid amin.

tch tt hn ngi ta x l alumina vi cc dung dch acid
hoc base.
37 10/28/2014
iu kin s dng
Alumina kim:
Khi s dng vi dung mi hu c: hp thu cc cht
thm, hydrocarbon bt bo ha, carotenoid, steroid,
alcaloid v nhiu loi hp cht t nhin khc.

Khi s dng vi dung mi nc hoc dung dch alcol
nc: c tnh trao i cng r nt hn c th hp
thu cc hp cht nh: phm nhum c tnh kim, amino
acid c tnh kim, cation v c.

38 10/28/2014
iu kin s dng
Alumina trung tnh:
S dng ch yu vi cc dung mi hu c, thch hp
tch cc cht d b hng.

Alumina acid:
Dng tch cc hp cht c tnh acid hoc trung tnh
vi iu kin cc cht ny khng b hy hoi bi acid.
Trong mi trng nc hoc alcol, alumina acid c
dng nh cht trao i ion

10/28/2014 39
V d
S dng ct sc k cha alumina trong sc k
lng vi mu th plasma nhm xc nh
catecholamines.
10/28/2014 40
So snh Silica gel v Alumina
SILICA GEL ALUMINA
GING
NHAU
u s dng dng oxide.
Tm hp ph mnh, s dng nhiu trong sc k hp ph.
B mt c nhiu l xp nh, din tch b mt hp ph ln.
KHC
NHAU
c iu ch bng qu trnh ng t
hay ngng t t acid
Bn cht l nhit phn base khng tan
Tnh hot tnh: nhm silanol (Si-OH),
c tnh acid hp ph cc cht c
tnh base
Tm hot tnh: Al
3+
v O
2-

Al
3+
: acid lewis hp ph cc cht
giu electron
O
2-
: base lewis hp ph cc cht
cho proton
2 loi: Silica gel pha thun v o 3 loi: alumina trung tnh, acid, base
10/28/2014 41
KHC
NHAU
C th hot ha hoc khng trc khi
s dng (ty theo pha thun hay o)
Nhit hot ha loi nc: 120
150
o
C, trn 300
o
C lm gim hot tnh
Hot ha bng cch sy loi nc
Nhit hot ha loi nc t 400
450
o
C
Tng nhit gim hot tnh (do to
nhm siloxane)
Tng nhit tng hot tnh (trong
gii hn cho php)
xp t 0,4-0,6 g/cm
3
, nhiu nht l
2,2 g/cm
3

xp khong 0,9 g/cm
3
n khong
4,0 g/cm
3

C th lm vic trong mi trng
nhim nc
Ch cn mt lng nh nc cng
nh hng hot tnh ca Alumina
Kh nng hp ph mnh hn silica
gel nn c th gy cc phn ng ha
hc ph
So snh Silica gel v Alumina
10/28/2014 42
Ti liu tham kho
1. Horacio E.Bergnaand William O.Roberts, Colloidal Silica fundamentals
and applications , CRC Press Taylors and Francis Group, 2006.
2. S. Musi, N. Filipovi-Vincekoviand L. Sekovani, Precipitation of
amorphous SiO2particles and their properties, BrazillianJournal of
Chemical Engineering, Vol. 28, No. 01, pp. 89 94, 2011.
3. Takashi Shirai, Hideo Watanabe, Structural properties and surface
characteristics on Aluminmun Oxide powders, Nagoya Institute od
Technology, 2009.
4. J.B. Peri, A. L. Hensley, The structure of silica gel, Research and
Development Department.
5. Karen Davis, Material Review: Alumina (Al
2
O
3
), Belgium.
6. The World of Alumina (n.d.), Alumina, modern material with varied
applications. Retrieved on December 14, 2002.
7. Larry L. Hench, Stephen Wallace, Structural analysis of water adsorbed in
Silica gel, University of Florida, 1994.

10/28/2014 43
Cm n thy v cc bn
ch lng nghe
10/28/2014 44