Controllable Synthesis of SAPO-5 Molecular Sieves and Exploration of the Crystallization Process †

doi:10.7503/cjcu20200022

Abstract

Abstract:

SAPO-5 molecular sieves were synthesized in non-acetic acid systems through rotating and static crystallization routes, respectively. The effects of rotation speed, crystallization time and water-silicon ratio of the gel system on the crystallization process of SAPO-5 samples were explored. The crystallization process of SAPO-5 samples under static and rotating hydrothermal conditions were studied by XRD and SEM. The results show that SAPO-5 samples obtained under the static hydrothermal conditions for 6 h is spherical and hexagonal columnar aggregated crystals. While the SAPO-5 samples obtained at 20 r/min for 2 or 6 h are dispersed concave columnar crystals(about 6—8 μm in diameter) and uniformly dispersed spherical crystals(16 μm in diameter), respectively. And SAPO-5 samples obtained at 60 r/min by extending the crystallization time to 3 h is hexagonal columnar crystal(about 5—8 μm in diameter). Also, hexagonal columnar SAPO-5 samples can be obtained by crystallizing at a rotation speed of 100 and 140 r/min for only 1 h. In addition, this work by adjusting the water-silicon ratio, the optimal water-silicon ratio was determined to be 70(the crystal phase is pure and the molecular sieve has the best dispersion from the morphology). In summary, compared to static crystallization, rotational crystallization not only improves the dispersion of the crystal from the morphology, but also improves the crystallization efficiency of SAPO-5 samples through shortening the crystallization time and reducing the crystallization speed. At the same time, SAPO-5 samples was synthesized in a non-acetic acid system with a smaller water-silicon molar ratio(70) and a lower amount of template agent, which provided a simpler and economical method for the synthesis of SAPO-5 molecular sieve.

Key words: SAPO-5 molecular sieves, Rotation hydrothermal crystallization, Controllable synthesis, Crystallization process

CLC Number:

O611

TrendMD:

HE Zhechao, XIA Kun, WANG Jing, ZHOU Dan, LU Xinhuan, XIA Qinghua. Controllable Synthesis of SAPO-5 Molecular Sieves and Exploration of the Crystallization Process ^†[J]. Chem. J. Chinese Universities, 2020, 41(6): 1224.

Figures/Tables 8

References 27

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Sample	Rotating rate/ (r·min^-1)	Heating time at 180 ℃/h	Relative crystallinity(%)	Sample	Rotating rate/ (r·min^-1)	Heating time at 180 ℃/h	Relative crystallinity(%)
S-2	0	2	—	R-3-60	60	3	89.2
S-3	0	3	60.2	R-3-60-cal	60	3	85.3
S-3-cal	0	3	54.6	R-0.5-100	100	0.5	—
S-6	0	6	68.0	R-1-100	100	1	60.2
R-1-20	20	1	—	R-2-100	100	2	68.1
R-2-20	20	2	75.6	R-3-100	100	3	85.6
R-3-20	20	3	100.0	R-0.5-140	140	0.5	—
R-3-20-cal	20	3	97.2	R-1-140	140	1	53.9
R-1-60	60	1	—	R-2-140	140	2	75.6
R-2-60	60	2	61.2	R-3-140	140	3	94.7

Sample	Rotating rate/ (r·min^-1)	Heating time at 180 ℃/h	Relative crystallinity(%)	Sample	Rotating rate/ (r·min^-1)	Heating time at 180 ℃/h	Relative crystallinity(%)
S-2	0	2	—	R-3-60	60	3	89.2
S-3	0	3	60.2	R-3-60-cal	60	3	85.3
S-3-cal	0	3	54.6	R-0.5-100	100	0.5	—
S-6	0	6	68.0	R-1-100	100	1	60.2
R-1-20	20	1	—	R-2-100	100	2	68.1
R-2-20	20	2	75.6	R-3-100	100	3	85.6
R-3-20	20	3	100.0	R-0.5-140	140	0.5	—
R-3-20-cal	20	3	97.2	R-1-140	140	1	53.9
R-1-60	60	1	—	R-2-140	140	2	75.6
R-2-60	60	2	61.2	R-3-140	140	3	94.7