Low-silicon composite molecular sieve, and synthetic method and application thereof

A technology of composite molecular sieve and synthesis method, which is applied in the field of low-silicon composite molecular sieve and its synthesis, can solve the problems of increased synthesis cost, single pore size of porous material, complex synthesis process, etc., to reduce the cost of waste liquid treatment and improve the utilization rate of silicon , The effect of simple synthesis process

Active Publication Date: 2015-02-04
天津众智科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] Patent CN102372290A discloses a synthesis method of SAPO-5 and SAPO-34 symbiotic molecular sieves, which solves the problem of single pore size and low activity of porous materials in technical synthesis, but the preparation of SiO in the gel mixture 2 :Al 2 o 3 =(0.1-2.0):1.0, the Si content in the prepared product is higher
[0004] Patent CN102336413A discloses a method for synthesizing low-silicon pure-phase SAPO-34 molecular sieves, using a two-step method, first preparing high-silicon SAPO-34 initial gel, crystallizing at a suitable temperature for a certain period of time, and then adding aluminum phosphate and organic amines The formed gel continues to crystallize, and the synthesis process is more complicated
[0005] Patent CN103011195A discloses a method for preparing hydrogen-type SAPO-5 and SAPO-34 symbiotic hierarchical porous molecular sieves in one step, which uses an organosilicon surfactant while using tetraethylammonium hydroxide as a template agent, and the template agent contains The higher the proportion, the higher the synthesis cost

Method used

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  • Low-silicon composite molecular sieve, and synthetic method and application thereof
  • Low-silicon composite molecular sieve, and synthetic method and application thereof
  • Low-silicon composite molecular sieve, and synthetic method and application thereof

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Experimental program
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Effect test

Embodiment 1

[0026] Gel preparation: first mix 252.5 grams of 35wt% tetraethylammonium hydroxide aqueous solution with 314.9 grams of distilled water, 15 ° C water bath, stirring speed 200 rpm, then slowly add 221.4 grams of 85wt% phosphoric acid and stir evenly, then slowly add 9.0 grams of 40wt% silica sol, continue to stir evenly; then slowly add 141.3 grams of pseudoboehmite, increase the stirring speed to 1200 rpm and stir for 5 hours, so that the solution becomes a uniform gel;

[0027] Crystallization: transfer the homogeneous gel to a hydrothermal reaction kettle, raise the temperature to the crystallization temperature of 160°C at a heating rate of 5°C / hour, the crystallization time is 96h, and the stirring speed is 150 rpm, after the crystallization is complete , cooled rapidly with cold water, and finally the reacted mixture was separated by suction filtration, washed with distilled water until pH = 7, and then dried at 100°C to obtain the molecular sieve powder;

[0028] Activa...

Embodiment 2

[0031] Gel preparation: first mix 420.9 grams of 35wt% tetraethylammonium hydroxide aqueous solution with 296.5 grams of distilled water, put in a water bath at 20°C, and stir at a speed of 250 rpm, then slowly add 230.6 grams of 85wt% phosphoric acid and stir evenly, then slowly add 15.0 grams of 40wt% silica sol, continue to stir evenly; then slowly add 149.6 grams of pseudoboehmite, increase the stirring speed to 1000 rpm and stir for 2 hours, so that the solution becomes a uniform gel;

[0032]Crystallization: transfer the homogeneous gel to a hydrothermal reaction kettle, heat up to a crystallization temperature of 168°C at a heating rate of 10°C / hour, the crystallization time is 72h, and the stirring speed is 200 rpm. After the crystallization is complete , cooled rapidly with cold water, and finally the reacted mixture was separated by suction filtration, washed with distilled water until pH = 7.5, and then dried at 110°C to obtain the molecular sieve powder;

[0033] A...

Embodiment 3

[0036] Gel preparation: first mix 315.6 grams of 25wt% tetraethylammonium hydroxide aqueous solution with 268.6 grams of distilled water in a 30°C water bath with a stirring speed of 300 rpm, then slowly add 276.7 grams of 80wt% phosphoric acid and stir evenly, then slowly add 12.0 grams of 30wt% silica sol, continue to stir evenly; then slowly add 149.6 grams of pseudo-boehmite, increase the stirring speed to 800 rpm and stir for 4 hours, so that the solution becomes a uniform gel;

[0037] Crystallization: transfer the homogeneous gel to a hydrothermal reaction kettle, heat up to a crystallization temperature of 170°C at a heating rate of 15°C / hour, crystallization time is 48h, stirring speed is 250 rpm, after crystallization is complete , cooled rapidly with cold water, and finally the reacted mixture was separated by suction filtration, washed with distilled water until pH = 7, and then dried at 120°C to obtain the molecular sieve powder;

[0038] Activation: Raise the mol...

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Abstract

A low-silicon composite molecular sieve comprises, by mass, 2-25% of an SAPO-5 molecular sieve and 75-98% of an SAPO-34 molecular sieve, and a molar ratio of SiO2 / Al2O3 is 0.07-0.15. The low-silicon composite molecular sieve has the advantages of low silicon, low cost, simple synthesis technology, high average diolefin selectivity in a methanol-to-olefin reaction, and long life.

Description

technical field [0001] The invention belongs to a molecular sieve and its preparation method, in particular to a low-silicon composite molecular sieve, its synthesis method and its application. Background technique [0002] The methanol-to-olefins (MTO) process is a new process for preparing low-carbon olefins such as ethylene and propylene from coal or natural gas through methanol. In U.S. Patent No. 4,440,871, U.S. Carbide Corporation (UCC) developed a new series of silicoaluminophosphate molecular sieves (SAPO-n). Among them, SAPO-34 molecular sieve is made of SiO 2 , AlO 2 - 、PO 2 + Three kinds of tetrahedrons are connected with each other and have a chabazite-like (CHA) structure. It is an ellipsoidal cage composed of eight-membered rings and a three-dimensional pore structure. The diameter of the window is 0.38 nanometers, and the spatial symmetry group is R3m. SAPO-34 is currently recognized as the best molecular sieve for MTO reaction. The study found that the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B37/08C01B39/54B01J29/80C07C11/04C07C11/06C07C1/20
CPCY02P20/52Y02P30/20Y02P30/40
Inventor 常云峰丁月
Owner 天津众智科技有限公司
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