Verified by C-n. Wu, by I. Dwyer, and by J. Zhao

Type Material Na₄₀[Al₄₀Si₁₅₂O₃₈₄]. (15-Crown-5)₈ (H₂O)₆₀

Method T. Chatelain, J. Patarin, M. Soulard, J.-L Guth, P. Schulz [1]

Batch Composition 2.1 Na₂O :10 SiO₂ : Al₂O₃ : 0.5(15-crown-5) : 100 H₂O

distilled water
crown ether (Aldrich 15-crown-5, 98%)
sodium hydroxide (Fluka, 98%)
sodium aluminate (Carlo Erba, 56% Al₂O₃, 37% Na₂O)
silica sol (Ceca, 40% SiO₂)

Batch Preparation^b (for 15 g product)^c

(1) [17.75 g water + 2.25 g crown ether], dissolve under continuous stirring
(2) [(1 + 1.65 g sodium hydroxide], dissolve under continuous stirring
(3) [(2) + 3.64 g sodium aluminate], dissolve under continuous stirring
(4) [(3) 30.00 g silica sol] stir with a magnetic bar at approximately 200 rpm Continue stirring for 24 hours at room temperature.^d Gel pH = 13.5-14

Vessel: Teflon-lined stainless steel autoclave (150 mL)
Temperature: 110¡C
Time: 8 days
Agitation: none
Final pH = approximately 12.5

(1) Filter and wash with distilled water until pH of the filtrate is close to 6
(2) Dry at 60-70¡C overnight
(3) Yield: 99% based on alumina (as-synthesized product containing the organic template and some water)^e

[1] T. Chatelain, J. Patarin, M. Soulard, J.-L Guth, P. Schulz, Zeolites 15 (1995) 90
[2] D. Anglerot, F. Fitoussi, P. Schulz, T. Chatelain, F. Dougnier, J. Patarin, J.-L Guth, in Synthesis of Porous Materials, Zeolites, Clays and Nanostructures, M. L Occelli, H. Kessler (eds.), Marcel Dekker, New York, 1996, p. 325

a. EMC-1 = Elf Mulhouse Chemistry number one.

b. The starting mixture is prepared in a polypropylene bottle.

c. This synthesis has been successfully carried out at the kilogram scale [2].

d. The mixture is aged in a closed polypropylene bottle.

e. Calcination at 450¡C in air removes the template.