Synthesis of Aluminophosphate Molecular Sieves by Ball Milling and Recrystallization†

doi:10.7503/cjcu20180114

Abstract

Abstract:

A rapid synthetic strategy through ball milling and recrystallization was successfully developed. Aluminophosphate molecular sieve with AWO topology was prepared by the precursor of two-dimensional(2D) layered aluminophosphate AlPO-IM. Simultaneously, metal-containing aluminophosphate molecular sieves with LAU topology were synthesized by introducing the metal heteroatoms in the ball-milling process. The phase transformation mechanism was comprehensively analyzed by Raman spectroscopy and CShM calculation. The results show that metal heteroatoms have an inorganic structure-directing effect in the synthesis of LAU molecular sieves. The ball milling-recrystallization method not only greatly shortens the crystallization time, but also converts the 2D layered aluminophosphates into a 3D molecular sieve under solvent-free conditions. Compared with the traditional hydrothermal/solvothermal synthesis, the ball milling-recrystallization method has the characteristics of high efficiency and energy saving, which expands the synthetic route of aluminophosphate molecular sieves.

Key words: Ball milling, Aluminophosphate, Structural transformation, Green synthesis

CLC Number:

O611

TrendMD:

WANG Shuang,YU Yue,BAI Pu,LIU Jiancong,LI Lin,SONG Xiaowei. Synthesis of Aluminophosphate Molecular Sieves by Ball Milling and Recrystallization^†[J]. Chem. J. Chinese Universities, 2018, 39(9): 1859.

Figures/Tables 8

Fig.1 XRD patterns(A) and SEM image(B) of AlPO-CJ73a, XRD patterns of AlPO-IM before and after the mechanochemical treatment(C) and XRD patterns of AlPO-CJ73a after different reaction time(D)

Fig.2 XRD patterns of MgAPO-CJ73b and ZnAPO-CJ73c(A) and SEM images of MgAPO-CJ73b(B) and ZnAPO-CJ73c(C)

Fig.3 FTIR spectra of MgAPO-CJ73b(a), ZnAPO-CJ73c(b) and APlO-IM before(c) and after(d) mechanochemical treatment

Table 1 Elemental analysis of the MAPO-CJ73(M=Mg, Zn)

Sample	Content, w(%)
Sample	Al	M	P	C	N	H
MgAPO-CJ73b	12.0	3.16	17.8	8.15	6.72	1.24
ZnAPO-CJ73c	10.5	11.2	16.9	7.29	5.76	0.98

Fig.4 XRD patterns of the products under different mass ratios of the ball-milling samples to water(A) and under different reaction time(B)

Fig.5 SEM images of AlPO-IM before(A) and after(B) the mechanochemical treatment, XRD patterns of AlPO-IM before and after the mechanochemical treatment(C) and the products under different ball-milling time(D)

Fig.6 Scheme of structural transformation between AlPO-IM, AlPO-21 and MAPO-LAU

Fig.7 Raman spectra of AlPO-CJ73a(A) and MgAPO-CJ73b(B) with different crystallization time

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