CAN

CAN

Cancrinite

Si(50), Al(50)

Contributed by J.-Ch. Buhl

Verified by C. Williams and by M. Bottale

Type Material Na₈[AlSiO₄]₆CO₃. 4H₂O

Method J.-Ch. Buhl [1]

Batch Composition 93 Na₂O : Al₂O₃: 2 SiO₂: 10 NaHCO₃: 1386 H₂O^a

Source Materials

distilled water
sodium hydroxide (Merck pellets, analytical grade)
kaolin (Fluka)
sodium bicarbonate (Merck, analytical grade, NaHCO₃)

Batch Preparation (for 0.6 g product)

(1) [45 mL water + 14.4 g sodium hydroxide], stir until dissolved
(2) [(1) + 0.5 g kaolin + 1.7 g sodium bicarbonate], mix until uniform slurry

Crystallization

Vessel: Teflon-lined steel autoclave
Temperature: 200¡C
Time: 48 hours
Agitation: none

Product Recovery

(1) Cool to ambient temperature. Filter
(2) Wash free of NaOH residuals (approximately 150 mL water)
(3) Dry at 80¡C
(4) Yield: close to 100%

Product Characterization

XRD: CAN; small amounts of a disordered phase between CAN and SOD and amorphous material could be detected in the polycrystalline sample [1,2]
Elemental Analysis: Na₈[AlSiO₄]₆CO₃. 4H₂O^bCrystal Size and Habit: small elongated needles
Click here to view XRD pattern

References

[1] J.-Ch. Buhl, Thermochiniica Acta 178 (1991) 19
[2] G. Hermeler, J.-Ch. Buhl, W. Hoffmann, Catalysis Today 8 (1991) 415
[3] C. Liu, S. Li, K. Tu, R Xu, J. Chem. Soc., Chem. Commun. (1993) 1645

Notes

a. CAN-formation in the water-free system is reported using butane-1,3-diol. [3]

b. Analysis of the guest anions according to the combination of simultaneous thermal analysis (TG, DTG, DTA), IR-spectroscopy and MAS NMR (¹³C).

c. Single crystals can be prepared from a gel consisting of [50 mg kaolin (heated at 1400¡C for two hours) + 168 mg NaHCO₃+ 320 mg NaOH + 1 mL distilled water] treated at 500¡C for 48 hours in a silver-lined steel autoclave.