Efficient Synthesis of Highly Uniform AlPO4-11 Microcrystalline and Study on the Crystallization Process†

doi:10.7503/cjcu20180103

Abstract

Abstract:

AlPO₄-11 microcrystalline molecular sieve was synthesized rapidly and efficiently in the rotation hydrothermal crystallization mode. In the static hydrothermal crystallization mode, the pure phase of the AlPO₄-11 molecular sieve cannot be obtained, and the crystal size is large, which consists of 50—70 μm rod crystals and 5—10 μm spherical crystals. Compared with the static hydrothermal crystallization mode, the rotation hydrothermal crystallization mode(rotational speed: 100 r/min) can greatly shorten the crystallization time of AlPO₄-11 molecular sieve(the shortest crystallization time is 40 min) and significantly reduce the grain size with the crystal being 1 μm×0.5 μm microcrystalline. The crystallization process of AlPO₄-11 was studied by means of powder XRD, scanning electron microscope(SEM), confocal microscopy Raman spectroscopy and Fourier transform infrared(FTIR) spectroscopy.

Key words: Zeolite, Hydrothermal synthesis, Rotation crystallization, AlPO₄-11, Raman spectroscopy

CLC Number:

O611.4

TrendMD:

XIA Kun, ZHOU Dan, YANG Yun, YANG Shuijin, XIA Qinghua. Efficient Synthesis of Highly Uniform AlPO₄-11 Microcrystalline and Study on the Crystallization Process^†[J]. Chem. J. Chinese Universities, 2018, 39(8): 1624.

Figures/Tables 8

Fig.1 XRD patterns of AlPO4-11 samples prepared under static conditions and simulated XRD pattern of AlPO4-11

Fig.2 XRD patterns of AlPO4-11 samples prepared under rotation conditions at different rotating rates and simulated XRD pattern of AlPO4-11Rotating rate/(r·min-1): (A) 20; (B) 60; (C) 100; (D) 140.

Table 1 Relative crystallinity of AlPO4-11 samples prepared under rotation and static conditions

Sample	Rotating rate/ (r·min^-1)	Heating time at 200 ℃/min	Relative crystallinity(%)	Sample	Rotating rate/ (r·min^-1)	Heating time at 200 ℃/min	Relative crystallinity(%)
S-20	0	20	—	R-60-60	60	60	93.6
S-30	0	30	44.3	R-120-60	60	120	95.3
S-60	0	60	64.3	R-10-100	100	10	—
S-120	0	120	83.2	R-20-100	100	20	44.9
S-180	0	180	90.0	R-30-100	100	30	89.4
R-10-20	20	10	—	R-40-100	100	40	94.1
R-20-20	20	20	14.8	R-60-100	100	60	100
R-30-20	20	30	45.4	R-120-100	100	120	100
R-40-20	20	40	67.9	R-10-140	140	10	—
R-60-20	20	60	79.5	R-20-140	140	20	25.9
R-120-20	20	120	92.8	R-30-140	140	30	68.9
R-10-60	60	10	—	R-40-140	140	40	85.1
R-20-60	60	20	18.8	R-60-140	140	60	94.5
R-30-60	60	30	56.5	R-120-140	140	120	96.2
R-40-60	60	40	82.3

Fig.3 Relative crystallinity of AlPO4-11 samples prepared under rotation and static conditions against heating time at 200 ℃a. Static; b. 20 r/min; c. 60 r/min; d. 100 r/min; e. 140 r/min.

Fig.4 SEM images of AlPO4-11 samples prepared under static conditions with different magnification(A1)—(A3) S-60; (B1)—(B3) S-120; (C1)—(C3) S-1440.

Fig.5 SEM images of AlPO4-11 samples prepared under rotating conditions at different rotating rate with different magnification(A1), (A2) R-60-20; (B1), (B2) R-60-60; (C1), (C2) R-60-100; (D1), (D2) R-60-140.

Fig.6 IR spectra of AlPO4-11 samples prepared at 100 r/min with different heating time at 200 ℃

Fig.7 Raman spectra of AlPO4-11 samples prepared at 100 r/min with different heating time at 200 ℃

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Efficient Synthesis of Highly Uniform AlPO₄-11 Microcrystalline and Study on the Crystallization Process^†

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