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Method for preparing hierarchical pore SAPO-20 molecular sieve from illite

A SAPO-20, illite technology, applied in molecular sieve and alkali-exchanged phosphate, molecular sieve characteristic silicoaluminophosphate and other directions, can solve the problem that the research of hierarchical porous SAPO-20 molecular sieve has not yet been reported, and achieves the goal of reducing synthesis cost. Effect

Pending Publication Date: 2021-04-30
XIAN UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In summary, zeolite molecular sieves can be successfully synthesized using illite as raw material, but the research on the synthesis of hierarchically porous SAPO-20 molecular sieves using illite as raw material has not been reported yet.

Method used

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  • Method for preparing hierarchical pore SAPO-20 molecular sieve from illite
  • Method for preparing hierarchical pore SAPO-20 molecular sieve from illite
  • Method for preparing hierarchical pore SAPO-20 molecular sieve from illite

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Embodiment 1

[0042] The illite that present embodiment provides prepares the method for hierarchical porous SAPO-20 molecular sieve comprising:

[0043] 1) Calcining and activating illite minerals and sodium carbonate powder, cooling and grinding to obtain activated illite;

[0044] The activation process is that the mass ratio of illite minerals to sodium carbonate is 1:0.6, the calcination temperature is 600°C, the calcination time is 90min, and the particle size of illite raw ore is 100 mesh. Grinding after cooling to obtain activated illite;

[0045] 2) Mix activated illite and 2mol / L hydrochloric acid at a mass volume ratio of 1:13.5mL, stir in a water bath at 80°C for 4 hours, centrifuge, wash, and dry to obtain activated illite silica slag with a purity ≥ 65%;

[0046] 3) Activated illite silica slag, aluminum source, phosphorus source, water, microporous template agent and mesoporous template agent are made into slurry, and the pH value is maintained at 9; the molar ratio of each ...

Embodiment 2

[0052] The method that utilizes illite to prepare microporous SAPO-20 molecular sieve that the present embodiment provides comprises:

[0053] 1) Calcining and activating illite minerals and sodium carbonate powder, cooling and grinding to obtain activated illite;

[0054] The activation process is that the mass ratio of illite minerals to sodium carbonate is 1:0.8, the calcination temperature is 900°C, the calcination time is 60min, and the particle size of illite raw ore is 200 mesh. Grinding after cooling to obtain activated illite;

[0055] 2) Mix activated illite and 2mol / L hydrochloric acid at a mass volume ratio of 1:13.5mL, stir in a water bath at 95°C for 3 hours, centrifuge, wash, and dry to obtain activated illite silica slag with a purity ≥ 65%;

[0056] 3) The activated illite silicon slag is made into slurry with aluminum source, phosphorus source, water, microporous template agent and mesoporous template agent, and the pH value is maintained at 6; the molar rat...

Embodiment 3

[0062] The method that utilizes illite to prepare microporous SAPO-20 molecular sieve that the present embodiment provides comprises:

[0063] 1) Calcining and activating illite minerals and sodium carbonate powder, cooling and grinding to obtain activated illite;

[0064] The activation process is that the mass ratio of illite minerals to sodium carbonate is 1:1.2, the calcination temperature is 700°C, the calcination time is 90min, and the particle size of illite raw ore is 300 mesh. Grinding after cooling to obtain activated illite;

[0065] 2) Mix activated illite and 2mol / L hydrochloric acid at a mass volume ratio of 1:13.5mL, stir in a water bath at 85°C for 3.5h, centrifuge, wash and dry to obtain activated illite silica slag with a purity ≥ 65%;

[0066] 3) Activated illite silicon slag, aluminum source, phosphorus source, water, microporous template and mesoporous template are made into slurry, and the pH value is kept at 7; the molar ratio of each substance in the s...

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Abstract

The invention belongs to the technical field of chemical material synthesis, and relates to a method for preparing a hierarchical pore SAPO-20 molecular sieve from illite. The method comprises the following steps: 1) calcining illite minerals and sodium carbonate to obtain activated illite; 2) mixing the activated illite with hydrochloric acid according to a mass-volume ratio of 1g to 13.5 mL, and stirring, centrifuging, washing and drying the mixture to obtain activated illite silicon slag; 3) mixing deionized water, a phosphorus source, an aluminum source, a microporous template agent, a mesoporous template agent, the acid-washed activated illite silicon slag and ethanol to obtain reactant gel, and crystallizing, centrifuging, washing, drying and calcining the reactant gel to obtain molecular sieve raw powder; and 4) calcining the molecular sieve raw powder in flowing air, and cooling the powder to obtain the hierarchical pore SAPO-20 molecular sieve. The hierarchical pore SAPO-20 molecular sieve is synthesized by taking the natural illite mineral as the raw material, so that the raw material source of the hierarchical pore SAPO-20 molecular sieve is broadened; the method has the advantages of short production process and low energy consumption, and the synthesis cost is greatly reduced.

Description

technical field [0001] The invention belongs to the technical field of porous material synthesis, and relates to a method for preparing multi-level porous SAPO-20 molecular sieves with illite as the main silicon source. Background technique [0002] SAPO-20 molecular sieve is composed of six rings, has a SOD structure, belongs to the cubic crystal system, and its space group is Im 3 m, the pore size is 0.3nm, and the pore volume is 0.40cm 3 / g, therefore, the hierarchical porous SAPO-20 molecular sieve is expected to be widely used in the fields of organic catalysis, hydrogen storage and gas separation, etc., and has broad development and application prospects. [0003] At present, the synthesis of SAPO-20 molecular sieve is mainly based on SiO 2 Powder, tetraethyl silicate, silica sol, etc. are used as silicon sources, aluminum isopropoxide, pseudoboehmite, etc. Synthesized by traditional hydrothermal synthesis method or liquid phase crystallization method. [0004] Syn...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/54C01B37/08
CPCC01B39/54C01B37/08C01P2002/72C01P2004/03
Inventor 陈治平王苗苗张旭辉芦静韦晓艺周文武李建伟汪广恒
Owner XIAN UNIV OF SCI & TECH
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