Synthesis of STW-zeotype Germanosilicate via Steam-assisted Crystallization†

doi:10.7503/cjcu20180859

Abstract

Abstract:

STW-zeotype germanosilicate was synthesized via the steam-assisted conversion(SAC) approach with N,N'-diethylethylenediamine(DEEDA) as an organic template. The effect of additional water on the resultant materials was systematically investigated by powder X-ray diffraction(XRD), scanning electron microscopy(SEM), energy dispersive spectrometer(EDS) and thermogravimetric(TG) analyses. In comparison with the conventional hydrothermal synthesis, the SAC method needs significantly less organic templates, through which the synthesized germanosilicate exhibits a high crystallinity and much more Si element content, as well as the high structural stability. The framework of STW-zeotype germanosilicate prepared by the SAC method remains stable even after undergoing a high temperature calcination(600 ℃).

Key words: Germanosilicate, Steam-assisted crystallization, STW zeolite, Thermal stability

CLC Number:

O611.4

TrendMD:

FANG Xijie,LIU Ruiyun,LIN Sen,SHI Lei,WANG Runwei,LI Yi,LI Junying. Synthesis of STW-zeotype Germanosilicate via Steam-assisted Crystallization^†[J]. Chem. J. Chinese Universities, 2019, 40(5): 867.

Figures/Tables 6

Fig.1 Powder X-ray diffraction patterns of GeSi-STW-SAC(a), Ge Si-STW-HT(b), and simulated XRD pattern of GeSi-STW(c)

Fig.2 SEM images of GeSi-STW-SAC(A—C) and GeSi-STW-HT(D)

Fig.3 TG analysis of GeSi-STW-SAC(a) and GeSi-STW-HT(b)

Table 1 Effect of H2O/GeO2 molar ratio on the final products synthesized following the steaming assisted conversion approach

Sample	n(H₂O)/n(GeO₂)	Product
S1	0—11.6	Amorphous
S2	11.6—20.9	GeO₂
S3	20.9—26.7	STW
S4	26.7—29.0	GeO₂+STW
S5	29.0—34.8	GeO₂+STW+MFI
S6	> 34.8	MFI

Fig.4 Powder X-ray diffraction patterns of materials prepared by SAC method undergoing drying treatment time Time/d: a. 0; b. 1; c. 2; d. 3. The drying treatment temperature is 70 ℃.

Fig.5 Powder X-ray diffraction patterns of GeSi-STW-SAC calcined in air at various temperatures Temperature/℃: a—j. 25, 50, 100, 200, 300, 400, 500, 600, 700, 800.

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