Contributed by Avelino Corma

Verified by J. Weitkamp and by N. Kumar

Type Material Na_0.08[Al₄Si₆₈O₁₄₄] : (C₆H₁₂NH)₁₀.₈ [1]^a

Method A. Corma, C. Corell, J. Pérez-Pariente [1]

Batch Composition 2.7 Na₂O : Al₂O₃ : 30 SiO₂ : 1347 H₂O : 15 HMI ^b (HMI = hexamethyleneimine)

Source Materials

deionized water
sodium alummate (Carlo Erba, 56% Al₂O₃, 37% Na₂O)
sodium hydroxide (98% NaOH)
hexamethyleneimine C₆H₁₂NH (Aldrich, 99% HMi)
silica (Degussa, Aerosil 200, or Cab-O-Sil M5)

Batch Preparation (for 12.8 g dry product)^c

(1) [124.20 g water + 0.92 g sodium aluminate + 0.60 g sodium hydroxide], stir until dissolved ^d
(2) [(1) + 7.61 g hexamethyleneimine], mix thoroughly^e
(3) [(2) + 9.23 g silica], mix thoroughly^f

Crystallization

Vessel: PTFE-lined stainless steel autoclaves
Time: 7 days
Temperature: 150¡C
Agitation: 60 rpm

Product Recovery

(1) Dilute the reaction mixture with distilled water
(2) Filter and wash with distilled water
(3) Dry at 100¡C overnight
(4) Yield; 99% based on alumina

Product Characterization

XRD: MCM-22 [2]; competing phases: FER (when crystallized under static conditions), ZSM-5 (when gel SiO₂/A1₂O₃> 100), ZSM-12 (when gel SiO₂/Al₂O₃> 200)
Elemental Analysis: 0.02 Na₂O : Al₂O₃ : 34 SiO₂
Crystal Size and Habit: small thin platelets occasionally forming spherical aggregates of 6-8 um ^g
Click here to view XRD pattern

References

[1] A. Corma, C. Corell, J. Pérez-Pariente, Zeolites 15 (1995) 2
[2] M. K. Rubin, P. Chu, US Patent 4 954 325 (1990)

Notes

a. Missing cations assumed to be protonated HMI.

b. H₂O includes water from sodium aluminate and added water.

c. Use polypropylene vessel and vigorous stirring for 30 minutes.

d. Clear solution

e. Slightly yellow clear solution

f. White and fluid gel

g. Toluene sorptive capacity at 0.1 KPa, 42⁰C : 10.07 mmol/g. The sample was heated in oxygen flow (30 cm³/min^-1) up to 500⁰C and outgassed overnight at 500⁰C in a vacuum better than 1 mPa.