Features of crystallization of aluminophosphate gels with different di-n-propilamine/Al2O3 ratio into micro-mesoporous molecular sieve AlPO4-11

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Abstract

Crystallization of aluminophosphate gels prepared using aluminum isopropoxide with di-n-propylamine/Al2O3 ratios of 1.0, 1.4, and 1.8 is studied. Changing the template/Al2O3 ratio in the reaction gels is shown to make various intermediate phases form during crystallization into the AlPO4-11 molecular sieve. A method to control its secondary porous structure based on adjusting the template/Al2O3 ratio in the reaction gels is proposed.

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About the authors

M. R. Agliullin

Institute of Petrochemistry and Catalysis, Ufa Federal Research Centre, Russian Academy of Sciences

Email: kuvatova2010@mail.ru
Russian Federation, Ufa, 450075

V. Y. Guskov

Ufa University of Science and Technology

Email: kuvatova2010@mail.ru
Russian Federation, Ufa, 450076

R. Z. Kuvatova

Institute of Petrochemistry and Catalysis, Ufa Federal Research Centre, Russian Academy of Sciences

Author for correspondence.
Email: kuvatova2010@mail.ru
Russian Federation, Ufa, 450075

V. V. Lazarev

Ufa University of Science and Technology

Email: kuvatova2010@mail.ru
Russian Federation, Ufa, 450076

B. I. Kutepov

Institute of Petrochemistry and Catalysis, Ufa Federal Research Centre, Russian Academy of Sciences

Email: kuvatova2010@mail.ru
Russian Federation, Ufa, 450075

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Supplementary files

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2. Fig. 1. X-ray diffraction patterns of reactive aluminophosphate gels, intermediate phases, and molecular sieves prepared at different DPA/Al2O3 ratios: a – Gel-IPA-1.0 sample, b – Gel-IPA-1.4, c – Gel-IPA-1.8, d – AlPO4-IF-1.0, d – AlPO4-IF-1.4, e – AlPO4-IF-1.8, g – AlPO4-11–1.0, h – AlPO4-11–1.4, i – AlPO4-11–1.8.

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3. Fig. 2. 27Al (a) and 31P (b) NMR spectra of aluminophosphate gels prepared at different DPA/Al2O3 ratios.

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4. Fig. 3. 27Al (a) and 31P (b) NMR spectra of intermediate phases formed 2 hours after the start of crystallization.

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5. Fig. 4. Raman spectra of intermediate phases formed 2 hours after the start of crystallization: a – sample IF-IPA-1.0; b – sample IF-IPA-1.4; c – sample IF-IPA-1.8.

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6. Fig. 5. Transmission electron microscopy images of intermediate phases formed 2 hours after the start of crystallization: a – sample IF-IPA-1.0; b – sample IF-IPA-1.4; c – sample IF-IPA-1.8.

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7. Fig. 6. Kinetics of crystallization of reaction gels into aluminophosphate sieves AlPO4-11.

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8. Fig. 7. SEM images of aluminophosphate molecular sieves: a – AlPO4-11-1.0 sample; b – AlPO4-11-1.4 sample; c – AlPO4-11-1.8 sample.

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9. Fig. 8. Nitrogen adsorption-desorption isotherms and pore size distribution of aluminophosphate molecular sieves synthesized from gels with different DPA/Al2O3 ratios: a – AlPO4-11-1.0 sample; b – AlPO4-11-1.4; c – AlPO4-11-1.8.

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10. Fig. 9. Kinetics of n-octane and isooctane adsorption on aluminophosphate molecular sieves: a – n-octane adsorption; b – isooctane adsorption.

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11. Fig. 10. Crystallization scheme of aluminophosphate molecular sieve AlPO4-11 from gels with different DPA/Al2O3 ratios.

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