Mesoporous materials: Synthesis and characterization

Mesoporous materials: Synthesis
and characterization
Dr. Roberto Hanoi Labrador,
Project manager
Outline
• Nanoporous materials classification
• Mesoporous materials: Synthesis and
characterization
• Nanologica AB, company profile
Classification of Nanoporous Materials
Pore Size (Å)
Macroporous
600
500
100
Mesoporous
80
60
40
20
10
Microporous
5
Important parameters of Nanoporous Materials
Surface area> increases contact area between reactants and products,
Pore size> allows to exclude/include/separate/adsorb/absorb…
Composition and surface properties> mechanical, conductive, magnetic
hydrophobic-hydrophilic properties, create interactions…
Connectivity and pore structure> allows to fine tune
selectivity/diffusion…
1-D
2-D
3-D
MESOPOROUS
2nm<Pore size<50nm
MCM-41 in 1992
Surface area 400-1500m2/g
Novel drug vehicle systems
SYNTHESIS OF MESOPOROUS SILICA
Typical Sol-gel route
Template agents
Silica precursors
•Anionic surfactants
•Cationic surfactants
•Geminal surfactants
•Polymers
•Other molecules (FA)
•Tetramethyl ortosolicato (TMOS)
•Tetraethyl ortosilicato (TEOS)
•Sodium silicate
Surface Chemistry
Post-synthetic functionalisation
In situ functionalisation
EtO
EtO
Si
OEt
OEt
+
O
EtO
EtO
Si
R
O
EtO
O
R
Si
Si
O
Si O Si
(EtO)3SiPrNH2
O
Cl
Si O
(EtO)3SiPrSH
Si OH
Si OH
Si OH
(EtO)3SiPrCl
(EtO)3SiPrCN
Si O
OH
Si O
Si O Si
Si O
Surfactant template
SiO2
SH
O
R
R
Si O
Si O
O
O
O Si
O
R
R
Si O Si
Si
SiO2
R
Si O
O
O
Template removal by
solvent extraction
OH
Si
O
Silica wall
Siliceous surface
NH2
Si O Si
CN
Si O
(EtO)3SiPh
Si O
H+/H2O
Si O Si
Si O
EtOH
SiO2
R
R
R
EtOH
R
R
SiO2
SiO2
R
R
R
SiO2
OH
Si O Si
R
R
Si O
Si O
O
SYNTHESIS OF MESOPOROUS SILICA NFM-1*
Folic acid
as TA
Schematic representation of self-assembled hexagonal columnar phase
* Nanologica´s patent WO2009/101110A9
TUNNING THE NFM-1: Concentration of FA
Sample
d100
FA-x
(Å)
FA-1.02
FA-0.85
FA-0.68
FA-0.51
39.4
39.7
38.4
39.1
Surface
Area
(BET)
(m²/g)
563
721
847
851
Avrg. Pore
Size
(DFT)
(Å)
30.7
30.9
30.9
30.8
Pore Volume
(cm³/g)
0.39
0.45
0.45
0.45
TUNNING THE NFM-1: Concentration of TEOS
TUNNING THE NFM-1: Stirring speed
Sample
SR –
‘‘R’’
(rpm)
d100
BET
Surface
Area
Pore
Size
(DFT)
Pore
Volume
(m²/g)
(Å)
(cm³/g)
(Å)
R – 250
38.0
571
23
0.29
R – 500
39.7
583
23
0.29
R – 750
39.0
596
26
0.30
R – 1000
37.7
769
26
0.39
R – 1400
37.3
941
23
0.47
Physico-Chemical Characterization of Nanomaterials
*OECD Guidance Manual for the testing of manufactured nanomaterials. ENV/JM/MONO(2009)20/REV
Characterizing mesoporous silica: Surface area and porosity
Surface area: Brunauer-Emmett-Teller (BET)
Pore size and pore volume:
Barret-Joyner-Hallenda (BJH)
Characterizing mesoporous silica: Morphology
Scanning Electron Microscopy (SEM)
Different morphologies in NFM-1 (templated by FA): Spheres, roid type and spherical shell
Different morphologies for silica particles templated with different polimeric agents: P123 (b) and
F127(d)
Characterizing mesoporous silica: Particle size
Dynamic light scattering (DLS)
Particle size in disperssion
Transmission Electron Microscopy (TEM)
Particle size and information on pore structure
Characterizing mesoporous silica: Identifying the mesophase
Powder X-Ray Diffraxion Analysis (XRD)
Transmission Electron Microscopy (TEM)
Characterizing loaded/functionalized mesoporous silica: Loading %
Thermo Gravimetric Analysis (TGA) of a mesoporous silica loaded with Vitamin A (Retinol)
TGA
22
20
18
16
49%
12
NPF-Si/Retinol
10
8
6
51%
4
2
T(deg)
998
950
901
852
804
755
706
658
609
560
512
463
414
366
317
268
220
171
122
73.7
0
25
m(mg)
14
Making Space for Innovation
Interdisciplinary Solutions for
Loading and Release
www.nanologica.com
Nanologica AB
• Spin-off company founded in August 2004, emerging from
the Structural Chemistry Department at the University of
• Stockholm
Nanologica has the ability to create nanoporous
structures with novel properties and functions because
of their size, shape or composition
• Nanologica AB is producing cutting edge nanostructured
materials with properties tailored for specific applications
• The Business concept of Nanologica is to develop and sell
products based on our material innovation
Nanologica AB area of Applications
Diagnostics
Separation
Drug Delivery
Sensors
Water Purification
NANOPOROUS
MATERIALS
Insulators
Fuel Cells
Gas-Separation
Clean Tech
Catalysis
Innovative Oral Drug
Delivery Solutions
Stable and amorphous APIs inside
the pores of silica particles
In-vitro enhancement of solubility
Dissolution curves of free Atazanavir
(ATV) and three different porous silica
particles loaded with ATV in simulated
Intestine fluid* (SIF, pH 6.8)
* Nanologica´s patent WO2012/03507A1
Making Space for Innovation
Interdisciplinary Solutions for
Loading and Release
www.nanologica.com

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