Preparation method of sapo-34/sapo-5 composite molecular sieve

A technology of SAPO-34 and SAPO-5, which is applied in the field of molecular sieve synthesis, can solve the problems of poor product repeatability and complicated steps, and achieve the effect of long butene selectivity, strong repeatability and good repeatability

Active Publication Date: 2020-06-05
XIAN ORIGIN CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the preparation of composite molecular sieves has poor reproducibility due to the use of more types of raw materials, more complex steps, and finer control requirements for conditions. Said to be a severe technical challenge

Method used

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  • Preparation method of sapo-34/sapo-5 composite molecular sieve
  • Preparation method of sapo-34/sapo-5 composite molecular sieve
  • Preparation method of sapo-34/sapo-5 composite molecular sieve

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Embodiment 1

[0026] The preparation method of the present embodiment SAPO-34 / SAPO-5 composite silicoaluminophosphate molecular sieve comprises the following steps:

[0027] Step 1, 0.12mol phosphoric acid (in P 2 o 5 In terms of), 0.12mol silica sol (as SiO 2 After mixing with 1mol deionized water evenly, add slowly while stirring (adding in 30 times, adding in 80 minutes) 0.11mol pseudo-boehmite (in the form of Al 2 o 3 After stirring for 30 minutes, 0.36 mol of triethylamine was added, and the first gel mixture was obtained after stirring evenly. Then, the first gel mixture was placed in a crystallization kettle, and the temperature was kept at 200° C. for 22 hours for the second gel mixture. A hydrothermal crystallization treatment, cooling to obtain the first crystallization liquid after crystallization;

[0028] Step 2. Slowly add (add in 30 times, finish adding in 60 minutes) 0.014mol pseudo-boehmite (with Al 2 o 3 meter), continue to stir for 30min and then add 0.013mol phosph...

Embodiment 2

[0032] The preparation method of the present embodiment SAPO-34 / SAPO-5 composite silicoaluminophosphate molecular sieve comprises the following steps:

[0033] Step 1, 0.18mol phosphoric acid (in P 2 o 5 In terms of), 0.17mol ethyl orthosilicate (as SiO 2 After mixing evenly with 1mol deionized water, add slowly while stirring (adding in 25 times, adding in 80min) 0.15mol pseudo-boehmite (in the form of Al 2 o 3 After stirring for 30 minutes, 0.30 mol of morpholine was added, and the first gel mixture was obtained after stirring evenly. Then, the first gel mixture was placed in a crystallization kettle, and the temperature was kept at 220° C. for 18 hours to carry out the first gel mixture. Hydrothermal crystallization treatment, cooling to obtain the first crystallization liquid after crystallization;

[0034] Step 2. Slowly add (add in 25 times, finish adding in 60 minutes) 0.01mol pseudo-boehmite (with Al 2 o 3 meter), continue to stir for 30min and then add 0.01mol p...

Embodiment 3

[0037] The preparation method of the present embodiment SAPO-34 / SAPO-5 composite silicoaluminophosphate molecular sieve comprises the following steps:

[0038] Step 1, 0.15mol phosphoric acid (in P 2 o 5 In terms of), 0.14mol silica sol (as SiO 2 After mixing evenly with 1mol deionized water, add slowly while stirring (adding in 35 times, adding in 80 minutes) 0.13mol pseudo-boehmite (in the form of Al 2 o 3 After stirring for 30 minutes, 0.24 mol of triethylamine was added, and the first gel mixture was obtained after stirring evenly. Then, the first gel mixture was placed in a crystallization kettle, and the temperature was kept at 180° C. for 24 hours to carry out the second gel mixture. A hydrothermal crystallization treatment, cooling to obtain the first crystallization liquid after crystallization;

[0039] Step 2. Slowly add (add in 35 times, finish adding in 60 minutes) 0.012mol pseudo-boehmite (with Al 2 o 3 meter), continue to stir for 30min and then add 0.012m...

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Abstract

The invention provides a preparation method of an SAPO-34 / SAPO-5 composite molecular sieve. The preparation method comprises the following steps: 1, mixing a first phosphorus source, a first silicon source and deionized water uniformly, adding a first aluminum source, adding a first template agent, and performing first hydrothermal crystallization treatment after uniform stirring to obtain a firstcrystallization / crystallized solution; 2, adding a second aluminum source to the first crystallization solution, then adding a second phosphorus source and a second template agent, performing secondhydrothermal crystallization treatment after uniform stirring, and performing filtering to obtain a filter cake; 3, washing, drying and roasting the filter cake sequentially, and naturally cooling aproduct to obtain the SAPO-34 / SAPO-5 molecular sieve. The composite silicoaluminophosphate molecular sieve prepared with the method has pore channel characteristics of SAPO-34 and SAPO-5, and pore channels and acid site distribution of the composite molecular sieve can be adjusted by adjusting preparation conditions.

Description

technical field [0001] The invention belongs to the technical field of molecular sieve synthesis, and in particular relates to a preparation method of a SAPO-34 / SAPO-5 composite molecular sieve. Background technique [0002] United Carbide Corporation (UCC) invented the silicoaluminophosphate molecular sieve (SAPO molecular sieve) with a pore size of about 0.4nm in 1984. SAPO molecular sieves have AlO linked by oxygen atoms 4 , SiO 4 and PO 4 Tetrahedral network, the pores in the crystal are due to Si 4+ replace P 5+ or Al 3+ The acidity produced or replaced by metals makes the molecular sieve play an important role in the catalysis of methanol to light olefins (MTO). Silicoaluminophosphate molecular sieve is another kind of molecular sieve catalytic material besides silica-alumina molecular sieve, which has been widely used in petrochemical and petroleum processing. SAPO-34 and SAPO-5 are two representative molecular sieves among silicoaluminophosphate molecular siev...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B37/08C01B39/54
Inventor 曾清湖高亚娜宋庆锋潘喜强张勇王瑞李玉洁吴西宁
Owner XIAN ORIGIN CHEM TECH
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