Template-based approach in the preparation of nanoporous silicas and titania-silicas
Mesoporous silicas and titania-silicas were synthesized with use as a template quaternary ammonium salts and their hydroxides. Fumed silica, tetraethyl orthosilicate and titanium(IV) tetraisopropoxide were applied as presursors. Syntheses were carried out in presence HCl and NH4OH. Mesoporous titani...
Gespeichert in:
| Datum: | 2001 |
|---|---|
| Hauptverfasser: | , , , , |
| Format: | Artikel |
| Sprache: | Englisch |
| Veröffentlicht: |
Chuiko Institute of Surface Chemistry National Academy of Sciences of Ukraine
2001
|
| Online Zugang: | https://surfacezbir.com.ua/index.php/surface/article/view/48 |
| Tags: |
Tag hinzufügen
Keine Tags, Fügen Sie den ersten Tag hinzu!
|
| Назва журналу: | Surface |
| Завантажити файл: | |
Institution
Surface| _version_ | 1869291129379225600 |
|---|---|
| author | Tertykh, V. A. Yanishpolskii, V. V. Pavlenko, A. N. Leboda, R. Skubiszewska-Zieba, J. |
| author_facet | Tertykh, V. A. Yanishpolskii, V. V. Pavlenko, A. N. Leboda, R. Skubiszewska-Zieba, J. |
| author_institution_txt_mv | [
{
"author": "V. A. Tertykh",
"institution": "Інститут хімії поверхні НАН України"
},
{
"author": "V. V. Yanishpolskii",
"institution": "Інститут хімії поверхні НАН України"
},
{
"author": "A. N. Pavlenko",
"institution": "Інститут хімії поверхні НАН України"
},
{
"author": "R. Leboda",
"institution": "Maria Curie-Sklodowska University"
},
{
"author": "J. Skubiszewska-Zieba",
"institution": "Maria Curie-Sklodowska University"
}
] |
| author_sort | Tertykh, V. A. |
| baseUrl_str | |
| collection | OJS |
| datestamp_date | 2018-11-27T09:42:39Z |
| description | Mesoporous silicas and titania-silicas were synthesized with use as a template quaternary ammonium salts and their hydroxides. Fumed silica, tetraethyl orthosilicate and titanium(IV) tetraisopropoxide were applied as presursors. Syntheses were carried out in presence HCl and NH4OH. Mesoporous titania-silicas with TiO2 contents from 1 up to 70 mol. % were prepared. Obtained samples have been characterized by the powder X-ray diffraction data and nitrogen adsorption at 77 K. Specific surface area, total pore volume, pore volume and area distribution were determined from nitrogen adsorption isotherm for synthesized titania-silicas. It was demonstrated that the ordered structures of MCM-41 type and bimodal porous materials with maximum pore diameter of 3 and 30 nm may be prepared depending of a synthesis conditions and a precursor nature. |
| first_indexed | 2025-09-24T17:44:38Z |
| format | Article |
| fulltext |
1 ,
: TЕMPLATЕ.BASЕD APPROAсII IN TIlЕ PRЕPARATION
oF NANoPoRoUs sILIсAs AND TITANIA.SILICAS
v.A. Tertykhl, v-.V. yanishpotskiir, A.N. pavlenkor,
R. Lеboda 2, and J. Skubiszewska.Zieba2
IInstitute of Suфсе Сhemistrу, Nаtionаl Асаdеmу of Scieпces,
,!368'0
Kуу|64, Gеn' Nаumov str' 17, UKRАINE; е.mаil.: tе}tуnh@public.uа.net,Fасultу of Chеmistry, Mаriа Сurie-Sklodowslrл (Jniуersilу, 20lЬ1 Гiьiti, iol,ц-io
Мesoporous siliсas and tiиnia-siliсas wеrе synthesized with usе as a tеmplatе
cгnary ammonium salts aпd thеir hydroxidеs. Fumed siliсa, tetraethyl orthosiliсate andtrnium(IV) tetraisopro-p-o-хide wеre appliеd as prеsursors. Synthеsеs wеre са:тied out in
FGsеnсе HCl and Nн4oI{. Мesoporous tiиnia-siliсas wlth тioz сontents from 1 up tо 70
*Нт.l'ЗT*-
o.lы]:o samples !9v3 b^een сharaсtеrized by the powder. x-ray
ff:''* 1* Pd
nitrogеn adsorption at77 K. Speсifiс surfaсe areц total poгe volume,'lЕЕ volume and arеa distribution wеre detеrminеd from nitrogen adsorption isotherm foi
AЬtraсt
resizеd titаnia-siliсas. It was demonstratеd that thе ordйс struсЬs of MCМ-41
and bimоdal pororrs materials with maximum porе diametеr of 3 and 30 nm rnay be
;rвpаred dеpеnding ofa synthesis сonditions and a prеоuгsor natЦre.
.lrtroduсtion
Rеmarkable aсhiеvеmеnt of the lаst dеcade in the fiеld of synthesis of orderrd
ъоstruсtural matеrials is pгepаration of a new сlass МCМ-41 periodiс silicatеs,
&шinosiliсatеs [l.2] and non.siliсa pеriodiс mesostructurеd matеrials t3] with nore
tЁameter from 15 up to 100 A and high spесifiс surfaсe area (morе than tо.orj 1nъ ;'h
tс use of surfaоtants as suprаInolесular tеmplates. Suсh matеrials are used as Jutяy.t
Cшriегs due to thеir unique geomеtriсal struсture, high thеrmal stability and adsorptivф
[tЬ5]. Considеrablе rrсent attention has bееn foсusеd on synthеsis of MCМ.4l materiats
mtаinеd in their strшсture the ions of hansition metals, in partiсular tiиnium [5-11], foт
ре'paratiоn of matеrials with high сatalytiс aсtivity and whiсh are stablе at hеaйg й ;
mditions оf hydrоthermal treatment [51. so in thе work [5], hydrothermal stabiliiy up to
ш0 oC and stability in acid mеdium фH=2) was distingui.ii.с гo. obиined тi-мbй-+r
шяteгials in сontradistinсtion to zeolites whiсh aте muсh less stable in the same сonditions.
hсlusion of tiиnium into the skеlеton of mesoporous siliсa matriсеs permits one to creatе
сw matегials йth porе diamеtеr in thе range 15.100 A, high spесifiс surfaсe area аnd
пith сatalytiс aсtivity in oxidation rеaсtions of largе organiс moleсulеs, for whiсh
dsorption spaсe of known pеrspeсtive Ti.сonиining сatalysts of a ТS.1, ТS.2 and Тi-p
t1pеs is inaссеssiЬle [6]. The works [7,8] dealing with synthesis of Ti-МCМ*41 and Ti.
HМS must bе pointed out in this dirесtion. It has been shown, in partiсular, that Ti-МCМ.
|l matеrials, alongside йth Ts-l and Ti.tIMS, arе rffective сatalysts foг hydroxylation
rcaсtion of bеnzenе to phenol' The сaиlytiс aсtivity of Ti-HМS and Ti.МCМ.41 in thе
rcaсtion of 2,6-di-tеrt-buф phenol oxidation wаs also dеmonstratе d t7J, Titanium
сonиining siliсatеs drmonstatе also photoсatalytiс aсtivity [ 1 l. 1 3]
59
Тhе aim of this woгk is to оontinuе systеmatiс rеsеarсh in thе fiеld of synthesis and
сharaсtеrization of nanoporous purе silicas and titania-siliсas braring vаrious amоunts of
titanium.
Ехpеrimеntal
For prеpаration of mesoporous siliсa аrrd titania.siliсas tеtraеthyl orthosiliсatе
(TЕos) and дerosil 300 was usеd as a siliсa sourсe and titаnium(IV) tеtraisopropoхide
was сhosen as a titаnium sorrrсe' Quatеmary ammonium salts
oсtadeсyltrimеtфlammonium chloridе (oDTМAсl, сl8сl) and
hеxadесyltrimеthylammonium bromidе (HDTMABr, C16Br) and tеtramеthylammonium
bromidе. (TМAв;, ClBr) was applied as tеmplate' These salts чrеre transformed intо
hydroxyl form with an use of thе ion-ехоhangе сolumn filled by thе AB.17-8 anionitе in
hydroxyl form.. .Sуnthеsis
of mеSoporous silicаs frоm fumеd sl/iсс. Fumеd siliсa (aеrosil) was
suspеndrd in water or in aquеous solution of quaternаry amine hydroxidе at intensivе
stirring" Rеsulting siliоa сonсentration was about 30 wt %. Siliса/aminе ratios arе
indiсatеd in thе Тablе 1. obtained suspensions allow to stand for 24.28 hrs аt гoom
tеmperaturr, thеn wеre driеd up at 150oC and сalсinated at 540 oC for 6 h on air.
Sупthеsis of MСM-41 purе siliса paJ, weighеd portion of t}rе surfaсtant (8.3 g
сTМAB;) wаs dissolvеd in 42 ml of сonсentratеd ammonia solution and intегmixed to
homogеnеous milk.white miхture' After addition af 9,67 ml ТЕoS thе miхtuте obtаinеd
was st.iкed up to gеl.likе produсt formation. Thе samplеs prepаrеd wеrе dгiеd up at air and
сalсinatеd at 540 oс for 6 h on air.
Sуnthеsis of titаniа.siliса in prеsеncе of HСl. Меsoporous titаnosiliсas with molar
ratios Ti/(Ti + Si) еqual 1, 15,30,50, and 70oАwerc synthesized using thе tесhniquе
desсribеd in thе work [7]' Тhе nесеssary Ti(ЁoCзF{z)4 amount was added by small
pоrtions at stirring to TЕoS solution in miхturе of еthanоl and isopropаnol. Weighеd
portion of oDTМACl was dissolved at intеnsivе stirring in watег with addition of small
amount of сonсеntratеd HCl. obtainеd homogenеous milk.whitе suspеnsion was addеd to
initial miхturе at intensive stirring and hеating up to 60 oC for the gel prrparation (for l.5
h). Тhe gel was subjесted to aging foт 18 h on air. Samples wеrе driеd up at l20 oC for 3 h,
and thеn wеre calсinated at 540 oC fоr 6 h on air.
Sуnthesis of titаniа.siliса in presence of NHaОH' 0.124 ml (0.00043 mol) TiPoT
was addеd by small portions dt stirring to 9,52 ml (0.0426 mol) TЕos
(Til(Ti+Si)х10й1%). ConЬеntratеd ammonia solution (a2 ml) was addеd at stirring to the
*"igьeс portiоn of the srгfaсtant 8.3 g CTMAвr (0.0228) mol. obtainеd milk-white
mixturе was drawn togethеr йth an initial solution and was stirred up to gel.likе produсt
formation (5 hrs). Solid prоduсts wеrr сalсinatеd at 540 oC fоr 6 h on air. Samplеs йth thе
titanium contents l5, 30, и' 50Yo were preparеd in a similar mannеr.
Charaсtеrization of the synthesizеd samples was performеd by thе powdеr Х-гay
diffraсtion (xRD) data (automatеd diffraсtomеtеr DRON-3M, CuК{l radiation) and
nitrogеn adsorption isothеrm measurеments at 77 K on ASAP-2000 Мiсromeritiсs
еquifmrnt. Averagе porе diarnеter was estimatеd by Gurviоh method (d=4VlS)' The
ф"iл. sшfaсе *"u, Ъgg,, was dеtеrminrd from the linеaт part of thr BЕT equation (at
o,,, = 0.05-0.з5). Poгe volume distribution was сalсulatеd from desorption branсh of an
i'oЬ"* of nitтogеn adsoгption using thе Barrett-Joyner.Halеnda (BIII) formula [16'17].
Cоmparativе с-рlots [16,18,l9] wеre сonstгuсted using stаndard nitrogеn adsorption daи
for siliсa ofJaтoniес at al. [20].
lсrotв en.
Т}rc з
Ёя:пrщ11 i6
Ciri( тЪцs
lсr rmpoп
\rзаgс hr
.lrФal.'l d
E} l. с'соr
t-pac
s
S i
rct6
I
16.
I 6
I t
.t\
А
-{'
т
т
т
тl
п
п
п
п
тт
тт
тE
гЕ
! t
r t
r t
I t
l6ь
l 6
t 6
t6
г@d я]
саr}
Ргас
lA r
фс t*
цс und
b cэdд
$rcс
ltЬв rс
dlL prв
b:rtт rn
тЬ )!
в 'Cr
G r r в .
60
v
d
3
е
I
в
l.
L
and disсussion
Thс sourсеs of siliоa aеrosil аnd tеtraеthyl orthosiliсatr praсtiсally dо not соntain of
ions and sodium. All sрthesеs werе сanied оut also in absenсе of inorgаniс
Thus, obtainеd siliсas and titania-siliсas do not сontain ехtrarrrous impurity, that is
impоrtant for thrir usе in сatalysis. Bсsidеs usr of TЕoS allows onе to avoid a
hydrotermal trеatnеnt arrd tо сarry out of synthesis at room temperatuте. Somс
сhаraсtеristiсs of thе prеparеd samples arе submittеd in thе Тable 1.
l. Geomеtriсal сhaгaсtеristiсs of mеsoporous siliсas anf titаrria.siliсas.
si Aсrosil
l Aеrosil
AеrosiI
l TЕos
|6a TЕos
16 TEOS
l8 TЕos
l8 ТЕos
l8 TЕos
8 TЕos
8 ТЕos
l6b ТЕos
16 TЕos
16 TЕos
t6 TEOS
TМA-o}I
сl6-CIн
Cl6-Br
C16-Bг
Cl6-Br
сl8сl
с l8Cl
с l8с l
с l8с l
с l8C l
Cl6-8r
Cl6-Br
Cl6-8г
C16-Br
. н2o
0.20 Hzo
0.10 Hzo
0.53 NI{4oн
o,27 нсl
0'27 }Iсl
0.2,| I{сl
0'27 нсl
0'27 tlсl
0.27 нсl
a.27 нсl
0.53 NI{4OI{
0.5з NI{4oн
0.53 NTI4Oн
0.5з NtI{oII
Sioz Tio2 Tеmplatе
preсrrгsor сontent
s,
moL'Уo
Tеmplatе Меdia
/oхide
molar
тatio
вЕT Toиl Poгс
surfaсе pore diamеtеr,
arеa' volumr, A'
iц сm3/g
25з I.32 208
206 1.08 2r0
4|6 |.42 |з6
|29| l.з0 40
1284 0.89 28
987 o'79 з2
924 0.47 20
805 0.45 22'702 0.52 30
529 0.59 46
35з 0.45 5l
900 0.98 4з
618 1.04 67
459 0.94 82
з40 0.48 57
0
0
0
0
I
l 5
I
l 5
30
50
70
I
l 5
30
50
Fшtеd siliсa is oftеn appliеd for prepаration of aеrosilogеl, suitablе foг usе as a сaгriеr
сatalysts inсluding enzymrs. As it is visiblе from Fig.l aerosilogеl has no
Praсtiсally all its spесifiс srrrfaсе сonsists from a suгfaоe of mсsopore urall йth
200A аnd abovе. At rеalizatiоn of sщthеsеs at prеsеnсе of tymеttlylammonium
the total speсifiс surfaсe arеa f$dесгеased and pore diamеtеr сalculatеd by Gurviсh
was unсhanged. Howevеr, as shown in Fig 2 the sample has miсroporоsity. It is
to ехplain this faсt by aсtion teframethylammonium ions as a tеmplate. Usе mоrе
tспrplate с16oн rrsults to bimodal mсsoporous samplе (Fig. 3). As shown in Fig.3,
2 thеrе aге two maxima on aсurvr of pоre disfribution at 30 and 300A аnd praсtiсally
howеver in ХRD pattегn of this samplе doеs not find out prеsеnсе of thс ordrrеd
шс' Thе ХRD diffraсtоgram for МCМ-4l samplе is slrown in Fig.4 аnd lattiсе
is rеprеsеntеd in Тable 2. This samplе eйibitеd ХRD pattеm with diftaсtion
whiсh аrе сharaсteristiс of wеll.ordеrеd hеxagonal struоhше (4 reflесtions). Fig. 5
il of thе pores whiсh diameter are eguаl to those сalсulatеd by Gurviоh mеtltod (136 А),
;юrе diametеr 30 A in this sample сorrеsponds to pore diamеtеr of materials МсМ-41
6 l
dеmonstrates irdsorption isotherm шrd porе distribution whiсh is typical for hiфquality
matedals of МCМ-41 typе.
t000
800
600
G
t-Ф
o
a)()
тi
o
ll
oo
tlб
o
Е
эo
400
200
0
0.5 r.o 1.5 2.0 2'3
Standard Adвorption сl.
Fig. l. Comparativе сo.plot for aеrosilogel (Sample Si.in Tablеl)
Fis. 2. Comparativе щ-plot for arrosilogll- гrеpаrеd in the prеsоnсe of TМAOH
(Sarrple siсl i,I ;;i;ri.i*;isс
.;fЁ,-ъ*.;=50 m2lg, d--l6 A,
V'i=0.02mУg
o 600
o
tt
(t
ч 40(т'Фд
oв'
Е 2o .
o
Еэ
o
1.0 1.5 2-O
ш
lqю
800
600
140
120
< 100
вq 8 oЕ
з 6 0gt
< 4 0
20
0
o.7
0.6
0.5
в
0.o Ё
o.
'з
0.2 <
0.12сю
0 10 1ф 1oo0
Pore dlemetвr (Aagstrom) t0.5
RЕlative preзз uгo, P/P0
'f .0 .t.5 2.0 2.5 3.0
Standard Adsorptlon с.
F.ig.3. Nifrogеn isotherm at -l96oC (/), porе volume and porе surfaсe arеa
distributions (2) and сomp#ativе щ-plot (3) for bimodal mesoporous siliсa
(Samplе siсl6 in Tablel).
63
Tablо 2. Х-тay diftaоtion datдof МCM-4l
d;;;Ы;. сеll pшrrrеtеr, a=453 A
bkl
ffiы Catсulatеd
i.valuеs, d-valuеs,
Angstrom Angstrom
ffi
iio 22.66 22.СI
ioo |9.Ф 19.63
11o 14E5 14'84
4 O
2 o(dcgrcв)
Fie. 4. Х.ray diffiaсtion Pattеrns.oflvICM4l t1рe silica
. .'. --
Gйlе MCМ-41 in Tablеl).
$
E
ri
йo
toш
A
E
os"
&
!, coo
I eoo
o
.. тoo
E
o 6 0 0
a
Ь э o o
o
! roo
! зooЕ
2 zo<
o
) r o t
o .o 0 ' 5
s t r n d l r d A d t o r p t l o n с .
Fis. 5. Niшogеn isothеrm at -l96oC (l), .pore
volume аnd por€ surfaсе
disшibшioпs d;d i.йin" *.piot (3) for МсМ41 prrre siliсa.
t10
900
800
7о0
600
500
400
з00
200
ioo
0
tt
Е
ta
Еo
Ё
J
o
Еб
в
€ o
o
Е
ш
0.6 0.8
Rg|etlv € proвзurэ,P|Po
o.2 0.4
900 1
l
8(ю ]
7 Ф '
G00
500
400
300
200
tФ
0
' ] o r . ь 2 . 0
64
ш
O
o
t'
I
t s
€ Б
a
t
E
6
OW
50о
400
300
200
100
0
t 7oo
Ч о00
Е 5o0
i F- a00
€ 6 з o o
3 zoo
! roo
эo, | 2 з
stаndard Adзorptlon сr.
1 2 з
standard Adsorption с.
n,,6. Comparative сu-plot fоr mesoporous titania-siliсa prеpаrеd in HCl media (1)
(BЕT surfaсе arca1.284 m./g, S3*1=l4 m./g, Samplе TilSiCl6a) and in
NIl4oH mеdia (2), (BЕТ surfaсr area 900 m./g, 3"*1=21| m.lg, Samplе
тi ls ic l6b).
a
c
i
€
a
aсэ
c
з 0
Tablе 3. Х-ray diffraction data оf titania.
siliсa withl5% Ti.
Hеxagonal unit сеll paramеtеt, a=50,3 A
2 0
1 0
hkr Ехpеri.
mental
d-valuеs,
Ansstrorт
Calсu-
latrd
d.valuсs,
A noсff^fr
100 46.59
l l 0 25.46 25.17
240 2t.92 2l -802 3 1
2 @ ( d e g r e в s )
J|1 . X-raу diffraсtion pattеrns of tiиnia-siliсa with |5% Ti
(SamplеTil5C16 in Tablеl) prеparеd in NHloH mеdia.
From Fig. 6, сurvе l is visiblс that titania-siliсa obtainеd in HCl media has not
-3nifiсаrrt еxtemal surfaое in сontrast of thе samplе prepared in N}I+OH mеdia (Fig. 6,
Crc 2). At synthesis titаnia-siliсa by.tесhniquе usеd for synthesis of purе MCМ-4l siliсa
Ьrgonal struсture is kept up to 15 % of thе сontеnts of tiиnium (Fig.7 and Tablе 3).
DiffIaсtoglаms of the obtainеd titanium-сontaining matеrials prеparеd in HCl arе
q1lsсntеd on Fig. 8. It is nесеssary to notе that thouф samplеs of titania.siliсas rесеivеd bу
f iп нсl mеdia havе a еxtrеmеly high spесifiс surfaсе arеa and uniform poте distгibution
tу arе not well ordеred.
65
Е
AYa
t 6 с
!
h1
а
c
ii
Is
5
2 e . D э 3 r э з l
Fic.8.,Ёray фqry-*T#Ё;!*ЕъТЁi;:s
йttr vшious titаrrium сontents (in шol Уo)
prepared intlсl
0.1
0.08
d d 0.06
Еf,:.il
0
,ю 80 t2o .160 2fll
dд
0.15
.; S o'r
Е l '
Е Е o.os
0.15
с' < 0.l
э о
Е B o'os
0
'Еl
Ф so 12o 160 200
d,A А"
o 40 Ф t2o t60 дl0
d ,A
o12
0.1
.i < 0.08
з Е 0.06
= g o.o1- - o.o2
0
Tig. ?. r.9:.".:lу: uif.lЁI38''iJu1iГ#Г}.
lжl,ii''ifr ъTJ#Ы' ;;;й;" . с t всt ь
нсl.04080ТTТ
d ' A
5 0 t
J O $
t l t
6 *
t t
Е
Е
66
Цs
Vr
iп
Availabilф of small.angle pеak on ХRD pattсгn of thе mеsoporous siliса" сontaining
l mol. % of titanium, tеstifirs about ехistеnсе in this samplе of ordеrеd struсfule, but nо
stгuсtural information сan bе ехtraсtеd from this diffraсtograms [21]. Pеaks at 20 в 25o is
сharaсtеristiс of anatаsе struсturе tеndеd to inсrеasе with inсrеasе in mеtal сontents in
titаnium-сontaining siliсas.
Basеd on adsorption rеsеarсh it rvas shorпn that valuеs of speсifiс srrrfaсe атea in thе
titаrrium.сontaining siliсas, dеtеrmined by BЕТ method, dесrеasе with thе inстеаsе of
tiиnium сontrnts both in aсid and basе сonditions (Tablel)'
For samplе obtainеd in HCl mеdia with Cl8сl template thе pore diameters, сalсulatеd
by Glrrviсh mеthod, arе inсreased from 20 up to 51 A at slightly varying total porе volumе
(0.45.0.60 с-3/g;. As thе tiиnium сontrnt in the samples is inсгеasеd, the йapе of thе
пitrogеn adsorрtion isothеrms is сhangеd from I up to IV typе with oссuпrnсr of hystеrеsis
loops сharaсtrristiс of mеsoporous struсturеs and оlosе undеr form to Hl фpе [16]. .Thе
сцryеs of porе volumе distributions on pore diametеr for thе synt}'еsizеd titanium-сontaining
mсsoporоus matегials arс suЬmittеd on Fig. 9. At low titаnium сontents in samplеs (dоvrn to
30 mol' %) the ruшrow volumе pоrе distribution on porr diamеtеr is obsеrved.
Conеlusion
Thе obtainеd expеrimеntal data tеstify an oppor|unф of tеmplatс sytrthesis оf
Einoрorous siliсa and titаnia-siliсas with high titanium сontеnts and advanсed spесifiс surfaсе
зеаs. Мorе ordеred struоturеs of purе siliсa and titаnia siliсa MCМ-4l typе is possiblе to
FrParr inNЦoH mеdia.
Aсknorмlеdgement
The rrsеarсh dеsсribed in this publiсation was suppoгted in part by NATO grant
No.ЕST.CLG.976890 and by Forrndation of Fundamental Rеseаrсh of thе Мinisф for
Еduсation and Sсiеnое ofUkrainе
Rеferеnсes
t. B€сk J.s., vаrtuli J.C., Roth V/.J., Leonowiсz М.Е., Kresgе C.Т., Sсhmitt K.D.,
Chц C.T-W., olson D.H., Sheppard Е.W., МсСullen S'B., Higgins J.B., аnd Sоhlеnkеr J.L.
A nеw family of mеsoporous molесular siеvеs prеparеd with liquid сrystal templatеs // J.
Am. Chem. Soс. . 1992. . v.114. - P.l0834.l0843.
2. Сiеsla U. аrrd Sсhtith F. ordеred mesoporous matеrials /l Мiсroporous and Меsoporous
Мatеr.- 1999'- У.2'I.. P.13 l.l49.
3. Sayari A. and Liu P. Non.siliсa pеriodiс mesostrцcturеd materials: recеnt progrеss//
Мiсroporous Мatеr. - 1997. -У.|2,.p.|49-|77,
l. Coгma A. From miсroporous to mesoporous mlесular siеvе materials and thеir use in
саиlysis// Chem. Rеv. - l997. -v.97. -P.2373-247з'
t. Chеn L'Y., Jaeniсkе S., and сhuah G.K. Thermal and hydrothermal sиbility of framеwork.
substitutеd МсМ-4l mеsoporous mateia|sllМiсroporous Мatеr. - |997'-у.|2. - P'з2з-
330.
Zhao Х.S., ф,(ax) Lu G.Q., and Millar G.J. Advanсеs in mesopoгous molесular siеve
мсМ.4l // Ind. Еng. Chеm. Rеs. . l996' - v.35. .P.2075-2090,
Тanеv P.T., Chibwе М., and Pinnavaia Т.J. Тitалium-сontaining mеsopororrs moleсulаr
siеves for сatalfiiс оxidation of aromatiс сompounds// Naturс. - |994. -v.з68. -P'з2|-32з'
6',7
8. Zhang W.. .w*g .J.i Tanеv P.T', T1 ̂ '.'Ж:1Ь}l;iif*;,Bi:r]ДТжs. :"iffi:
"
;;; iransition.mеtal substitutеd hеxagonы :
v. в.. p.этs.T
т*.u-i T. Synthesis of titanium-соntaining МсМ-41// Мiсroporous
9. KoYano K.A. шto l,
й;;--1997..v.l0.
-Р.259-21|' юrous molесulаr.sievе
, o. ojil". Yo: : .l* .з "*-*жiTi,
J :'lЁ."в;lЖ::' Ьъ'fi Ы -i .ill в-ztвz,
МCМ-4l: syntIrеsrs 1flЦ-vuвсv*..;^.: D т wоns J.. and Pinnavata l.J. rvlc-ьUPvrt.'.',.ii***;чlч:^#$"ъ1"Т'н#"'*i'ж1з.д:,ffi;**'yiJry.:Щ*
titanosiliсше mo]^е.с.$ar ']:T:'*Т"H:-1#;;;i,oiЪrpьy*iсal propеrtiеs andсatаlytiс
*;T*:}Т*j:'lJ frfiЁ'!I.i"rii:#^ff;:Тй . v r r в" - i,g t вц.g ll t,
12. Мatthеws t,.к. ani;;Ъ. ть" i*gn9,"йЪi'i*iu into:nоdifiеd siliоatеs fof solаr
photodеgrad*"' }ln"Ё"*,p""йl l: sТiЁ"ii"i""* and Tесhnology. . 1997.. V.8. -
P,619.62з.
13. Stonо V.F. Jr' and Davis R.J. Sщthеsis, оhаraсtеrizatio1r, and Dhotoсatalytiс aсtivity of
titаnia and niobia i,",Ьpo,oo, molrсular;;;Jiъh;*. Мatеr. ] tqgв. . v.10. . P'l468.
1,414.
14.AnpoM' ,Yamash i taH. , IkеuсK. , .Fu j i iY . ,ZhangS.G, , , . Iф inash iY . ,PаrkD.R. '
Suzukiv., кoy#l;,,й.i;,;,*r т
"iЬ*Ь.JйiJ.rеduсtion of Coz with l{zo on
тiMсM.41 ш,o.ii-йсм.48 mеsoporо.j..,,""ii," i"ыysts// Cata'ysis Today . 1998. .
i.цi-p.зzl-ззэ. R. A 28.yеar-old synthesis of miоеllе-tеmplated
'' ;j,ffffiI;,iffi','il",h"Hi''''ii.''.".ъй : v, iы. - P.2li3-286. t..
16. Grеgg S.J. antl ii,щ к.s.w. дс,o,p,ion],s,*i""" д'""Ыо Pйsity, London: Aсademiс
Pтеss, t982'
17.BarrеttЕ.P.,JoщеrL.J.,аndHalеndaP.P.Thеdеtеrminationofporеvolumеandaтеa
distributions *',"."-,"J*,Ь.j..^l.^ё;;;й""s
from nitrogen isothеrms// J. Am.
Ёi;;. .;". . l95i. - v.73. - P. 3]'1'389. Mesopoте sizе. and surfaсе
1 8. Fenеlonou v.B,,,io;.йko" J N : Td
Dеrеvyankin A.Yu.
arеaсalсulati"";i;;;;й9".ly.'::9d;;;^й"'йсм-4.l,FsМ.16,еtс.)usinglow-
anglе ХRD *u""i."*iiЫ iata ||Мi;,.;;;;.*а М",opo,ous Мatеr. - |999. - v.28. -
P- 51.,72'
19. Sсhulz-Еkloff G.. kft"YЧ.j:, зnd Zukal A. Controlling of morphology and
оharaсtетizatio., Ъi po," struсtче oi. o,а.,"a mеsoporous
..iii"*ll
Мiоtoporous arrd
,.$ffijJff*'fl: .Jч,,]::i#,i,.J.'. o*u*o t,,oo*"o adsorг]i91 daи foт
сharaсtеrizat,""Тr?*",orou; gi'сii,ril*Ь'i'. i!3я. ..v..rs.
. P.5410.5413.
21. Sсhaсht ,"' ,J"ЁJй;*1-*"*.il?"J"rьc }:,uy.ry;;*-
and TЕМ images of
МсМ-41 // Мicroporоus and м..opo,*, й;й. - iqяв' -у.22,-P,485-493.
68
эo f
ьЕ
Ltt
b
-q
-
D
|
| id | oai:ojs.pkp.sfu.ca:article-48 |
| institution | Surface |
| keywords_txt_mv | keywords |
| language | English |
| last_indexed | 2025-09-24T17:44:38Z |
| publishDate | 2001 |
| publisher | Chuiko Institute of Surface Chemistry National Academy of Sciences of Ukraine |
| record_format | ojs |
| resource_txt_mv | surfacezbircomua/bc/97ec1fd6eed787abaf01f04df343d3bc.pdf |
| spelling | oai:ojs.pkp.sfu.ca:article-482018-11-27T09:42:39Z Template-based approach in the preparation of nanoporous silicas and titania-silicas Template-based approach in the preparation of nanoporous silicas and titania-silicas Template-based approach in the preparation of nanoporous silicas and titania-silicas Tertykh, V. A. Yanishpolskii, V. V. Pavlenko, A. N. Leboda, R. Skubiszewska-Zieba, J. Mesoporous silicas and titania-silicas were synthesized with use as a template quaternary ammonium salts and their hydroxides. Fumed silica, tetraethyl orthosilicate and titanium(IV) tetraisopropoxide were applied as presursors. Syntheses were carried out in presence HCl and NH4OH. Mesoporous titania-silicas with TiO2 contents from 1 up to 70 mol. % were prepared. Obtained samples have been characterized by the powder X-ray diffraction data and nitrogen adsorption at 77 K. Specific surface area, total pore volume, pore volume and area distribution were determined from nitrogen adsorption isotherm for synthesized titania-silicas. It was demonstrated that the ordered structures of MCM-41 type and bimodal porous materials with maximum pore diameter of 3 and 30 nm may be prepared depending of a synthesis conditions and a precursor nature. Mesoporous silicas and titania-silicas were synthesized with use as a template quaternary ammonium salts and their hydroxides. Fumed silica, tetraethyl orthosilicate and titanium(IV) tetraisopropoxide were applied as presursors. Syntheses were carried out in presence HCl and NH4OH. Mesoporous titania-silicas with TiO2 contents from 1 up to 70 mol. % were prepared. Obtained samples have been characterized by the powder X-ray diffraction data and nitrogen adsorption at 77 K. Specific surface area, total pore volume, pore volume and area distribution were determined from nitrogen adsorption isotherm for synthesized titania-silicas. It was demonstrated that the ordered structures of MCM-41 type and bimodal porous materials with maximum pore diameter of 3 and 30 nm may be prepared depending of a synthesis conditions and a precursor nature. Mesoporous silicas and titania-silicas were synthesized with use as a template quaternary ammonium salts and their hydroxides. Fumed silica, tetraethyl orthosilicate and titanium(IV) tetraisopropoxide were applied as presursors. Syntheses were carried out in presence HCl and NH4OH. Mesoporous titania-silicas with TiO2 contents from 1 up to 70 mol. % were prepared. Obtained samples have been characterized by the powder X-ray diffraction data and nitrogen adsorption at 77 K. Specific surface area, total pore volume, pore volume and area distribution were determined from nitrogen adsorption isotherm for synthesized titania-silicas. It was demonstrated that the ordered structures of MCM-41 type and bimodal porous materials with maximum pore diameter of 3 and 30 nm may be prepared depending of a synthesis conditions and a precursor nature. Chuiko Institute of Surface Chemistry National Academy of Sciences of Ukraine 2001-06-10 Article Article application/pdf https://surfacezbir.com.ua/index.php/surface/article/view/48 Surface; No. 4-6 (2001): Chemistry, Physics and Technology of Surface; 59-68 Поверхность; № 4-6 (2001): Химия, физика и технология поверхности; 59-68 Поверхня; № 4-6 (2001): Хімія, фізика та технологія поверхні; 59-68 3154-8091 3154-8083 en https://surfacezbir.com.ua/index.php/surface/article/view/48/47 Авторське право (c) 2001 V.A. Tertykh, V.V. Yanishpolskii, AN. Pavlenko, R. Leboda, and J. Skubiszewska-Zieba |
| spellingShingle | Tertykh, V. A. Yanishpolskii, V. V. Pavlenko, A. N. Leboda, R. Skubiszewska-Zieba, J. Template-based approach in the preparation of nanoporous silicas and titania-silicas |
| title | Template-based approach in the preparation of nanoporous silicas and titania-silicas |
| title_alt | Template-based approach in the preparation of nanoporous silicas and titania-silicas Template-based approach in the preparation of nanoporous silicas and titania-silicas |
| title_full | Template-based approach in the preparation of nanoporous silicas and titania-silicas |
| title_fullStr | Template-based approach in the preparation of nanoporous silicas and titania-silicas |
| title_full_unstemmed | Template-based approach in the preparation of nanoporous silicas and titania-silicas |
| title_short | Template-based approach in the preparation of nanoporous silicas and titania-silicas |
| title_sort | template-based approach in the preparation of nanoporous silicas and titania-silicas |
| url | https://surfacezbir.com.ua/index.php/surface/article/view/48 |
| work_keys_str_mv | AT tertykhva templatebasedapproachinthepreparationofnanoporoussilicasandtitaniasilicas AT yanishpolskiivv templatebasedapproachinthepreparationofnanoporoussilicasandtitaniasilicas AT pavlenkoan templatebasedapproachinthepreparationofnanoporoussilicasandtitaniasilicas AT lebodar templatebasedapproachinthepreparationofnanoporoussilicasandtitaniasilicas AT skubiszewskaziebaj templatebasedapproachinthepreparationofnanoporoussilicasandtitaniasilicas |