SUPPORTING INFORMATION

Rapid Room Temperature Synthesis of Tin-based Mesoporous Solids: Influence of the Particle Size on the

Production of Ethyl LactateNicolas Godard, Xavier Collard, Alvise Vivian, Lucia Anna Bivona, Luca

Fusaro, Sonia Fiorilli, Carmela Aprile*

Contents:

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1. Mean particle size as function of synthesis time for mp materials. S1

2. TEM, XRD, N2 ads/des and 29Si NMR of material mp_5min. S2

3. TEM, XRD, N2 ads/des and 29Si NMR of material mp_30min. S3

4. TEM images of mp materials (A to E). S4

5. TEM, XRD, N2 ads/des and 29Si NMR of material mp-A. S5

6. TEM, XRD, N2 ads/des and 29Si NMR of material mp-E. S6

7. Table: Textural properties of the synthetized mp and Sn-mp materials. S7

8. XRD patterns of the synthetized Sn-mp materials (F to J). S8

9. Isotherm nitrogen adsorption/desorption and pore size distribution (PSD) of material G. S9

10. Isotherm nitrogen adsorption/desorption and pore size distribution (PSD) of material H. S10

11. Isotherm nitrogen adsorption/desorption and pore size distribution (PSD) of material I. S11

12. Solid state 29Si MAS NMR spectra of the materials F and J. S12

13. TEM, XRD, N2 ads/des and 29Si NMR of Sn-mp-J-5min. S13

14. Energy dispersive X-ray spectroscopy mapping S14

15. FTIR spectra relative to the adsorption of NH3 on materials Sn-mp-G, Sn-mp-H and Sn-mp-I S15

16. 1H NMR of ethyl lactate in CDCl3. S16

17. 13C NMR of ethyl lactate in CDCl3. S17

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S1. Mean particle size as function of synthesis time for mp materials. Average estimated over 100 TEM measurements.

S2.TEM micrograph (a), small angle XRD pattern (b), nitrogen adsorption-desorption (c) and 29Si MAS NMR recorded in the solid state (d) of mp material synthetized in 5 min.

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S3. TEM micrograph (a), small angle XRD pattern (b), nitrogen adsorption-desorption (c) and 29Si MAS NMR recorded in the solid state (d) of mp material synthetized in 30 min.

S4. TEM images of mp materials (A to E). mp materials synthetized with different ammonia concentrations (A: 0.05 M, B: 0.11 M, C: 0.16 M, D: 0.21 M, E: 0.26 M). The scale is identical for all micrographs.

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S5. TEM image (a), small angle XRD pattern (b), nitrogen adsorption-desorption (c) and solid state 29Si MAS NMR (d) of the mp-A.

S6. TEM image (a), small angle XRD pattern (b), nitrogen adsorption-desorption (c) and solid state 29Si MAS NMR (d) of the material mp-E.

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S7. Table resuming the textural properties of the synthetized mp and Sn-mp materials.

Sample [NH4OH] (mol L-1)

MPS (nm)

BET SSA(m2 g-1)

BJH average pore size

(nm)

Tot. Pore volume (cm3 g-1)a

Inter-reticular distance (nm)

Si/Sn (exp)b

B 0.11 53 1099 2.1 1.57 3.9 -C 0.16 67 1087 2.1 1.31 3.8 -D 0.21 85 1089 2.0 1.04 3.7 -G 0.11 113 1007 2.4 0.98 4.0 47H 0.16 139 1054 2.2 0.84 3.9 43I 0.21 175 1031 2.1 0.75 3.8 41

a : Total pore volume at relative pressure 0.9 p/p0. b : Si/Sn calculated from EDX analysis. The values are averages of multiple EDX analyses on various parts of the samples.

2 4 6 8 10

Inte

nsity

(a.u

.)

2 (degrees)

J

I

H

G

F

S8: XRD patterns of the synthetized Sn-mp materials (F to J).

S9: Isotherm nitrogen adsorption/desorption and pore size distribution of material G.

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S10: Isotherm nitrogen adsorption/desorption and pore size distribution of material H.

S11: Isotherm nitrogen adsorption/desorption and pore size distribution of material I.

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S12: Solid state 29Si MAS NMR spectra of the material F (right) and J (left).

S13. TEM image (a), small angle XRD pattern (b), nitrogen adsorption-desorption (c) and solid state 29Si MAS NMR (d) of the material Sn-mp-J-5min.

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a)

b)

S14: Energy dispersive X-ray spectroscopy mapping of material Sn-mp-F (a) and Sn-mp-J (b).

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S15: FTIR spectra relative to the adsorption of NH3 on materials Sn-mp-G (a), Sn-mp-H (b) and Sn-mp-I (c) outgassed at 400 °C. Curves 1 and 2 were obtained under 5 and 1 mbar NH3 equilibrium pressures and curve 3 corresponds to prolonged outgassing at room temperature after NH 3 dosages. The spectra show a break in the 2500-1950 cm–1 range

S16: 1H NMR of ethyl lactate in CDCl3.

S17: 13C NMR of ethyl lactate in CDCl3.

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