Mesoporous materials: Synthesis Mesoporous materials: Synthesis and characterizationand characterization

Dr. Roberto Hanoi Labrador,

Project manager

• Nanoporous materials classification

• :Mesoporous materials Synthesis and characterization• Nanologica AB, company profile

Outline Outline

Pore Size (Å)

40

60

5

10

20

Mesoporousporous

Microporousporous

80

500

100

600Macroporousporous

Classification of Nanoporous MaterialsClassification of Nanoporous Materials

>Surface area increases contact area between reactants and products, increases contact area between reactants and products,

>Pore size / / / /allows to exclude include separate adsorb absorb/ / / /allows to exclude include separate adsorb absorb……

>Composition and surface properties mechanical, conductive, magnetic mechanical, conductive, magnetic hydrophobichydrophobic--hydrophilic properties, create interactionshydrophilic properties, create interactions……

1-D 2-D 3-D

>Connectivity and pore structure allows to fine tune allows to fine tune /selectivity diffusion/selectivity diffusion……

Important parameters of Nanoporous MaterialsImportant parameters of Nanoporous Materials

MESOPOROUS

2nm<Pore size<50nm Surface area 400-1500m2/g

MCM-41 in 1992 Novel drug vehicle systems

SYNTHESIS OF MESOPOROUS SILICA

Typical Sol-gel route

Template agents•Anionic surfactants•Cationic surfactants•Geminal surfactants•Polymers•Other molecules (FA)

Silica precursors•Tetramethyl ortosolicato (TMOS)•Tetraethyl ortosilicato (TEOS)•Sodium silicate

In situ functionalisation

Template removal bysolvent extraction

Post-synthetic functionalisation

SiOEt

OEtEtO

EtO RSiEtO

EtOEtO

OH

O

OSi

O

SiO

SiO

O

R

O

O

SiO

Si

O

OO

O

OH+

Si OH

Si OH

Si OH

Siliceous surface

(EtO)3SiPrCl

(EtO)3SiPh

(EtO)3SiPrSH

(EtO)3SiPrNH2

Si O

Si O

Si O

Si SH

Si O

Si O

Si O

Si NH2

Si O

Si O

Si O

Si Cl

Si O

Si O

Si O

Si

Si O

Si O

Si O

Si CN

(EtO)3SiPrCN

Si O

Si O

Si O

SiOH

O

H+/H2O

R R RR R

SiO2

SiO2

R R RR R

SiO2

SiO2

R R RR R

SiO2

SiO2EtOH

EtOH

Surfactant template

Silica wall

Surface ChemistrySurface Chemistry

SYNTHESIS OF MESOPOROUS SILICA NFM-1*

Folic acidas TA

Schematic representation of self-assembled hexagonal columnar phase

* Nanologica´s patent WO2009/101110A9

TUNNING THE NFM-1: Concentration of FA

Sample

FA-x

d100

(Å)

Surface Area(BET)(m²/g)

Avrg. Pore Size

(DFT)(Å)

Pore Volume

(cm³/g)

FA-1.02 39.4 563 30.7 0.39FA-0.85 39.7 721 30.9 0.45FA-0.68 38.4 847 30.9 0.45FA-0.51 39.1 851 30.8 0.45

TUNNING THE NFM-1: Concentration of TEOS

TUNNING THE NFM-1: Stirring speed

SampleSR –‘‘R’’

(rpm)

d100

(Å)

BET Surface

Area

(m²/g)

Pore Size

(DFT)

(Å)

Pore Volume

(cm³/g)

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

0

2

4

6

8

10

12

14

16

18

20

22

25

73.7

122

171

220

268

317

366

414

463

512

560

609

658

706

755

804

852

901

950

998

T(deg)

m(m

g)

NPF-Si/Retinol

49%

51%

Making Space for InnovationInterdisciplinary Solutions for

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• The Business concept of Nanologica is to develop and sell products based on our material innovation

• Nanologica AB is producing cutting edge nanostructured materials with properties tailored for specific applications

• 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 Nanologica AB

NANOPOROUSNANOPOROUSMATERIALSMATERIALS

Diagnostics

Drug Delivery

Water Purification

Insulators

Clean Tech

Catalysis

Gas-Separation

Separation

Sensors

Fuel Cells

Nanologica AB area of ApplicationsNanologica AB area of Applications

Innovative Oral DrugDelivery SolutionsStable and amorphous APIs inside the pores of silica particles

Dissolution curves of free Atazanavir (ATV) and three different porous silica particles loaded with ATV in simulated Intestine fluid* (SIF, pH 6.8)

In-vitro enhancement of solubility

* Nanologica´s patent WO2012/03507A1

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