A kind of low silicon sapo-34 molecular sieve and its preparation method and application

A molecular sieve, silica sol technology, applied in the direction of molecular sieve and alkali exchange phosphate, molecular sieve catalyst, molecular sieve characteristic silicoaluminophosphate, etc., can solve the problem of pure phase SAPO-34 molecular sieve difficult to directly synthesize and so on, achieve the inhibition of heterocrystalline Generation, usage reduction, grain size reduction effect

Active Publication Date: 2021-02-12
CHIA TAI ENERGY MATERIALS DALIAN
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The technical problem to be solved by the present invention is to overcome the defects of the prior art, provide a low-silicon SAPO-34 molecular sieve and its preparation method and application, and solve the problem that the pure-phase SAPO-34 molecular sieve with a low silicon-aluminum ratio is difficult to synthesize by a direct method

Method used

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  • A kind of low silicon sapo-34 molecular sieve and its preparation method and application
  • A kind of low silicon sapo-34 molecular sieve and its preparation method and application
  • A kind of low silicon sapo-34 molecular sieve and its preparation method and application

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Effect test

Embodiment 1

[0024] Disperse 25g of pseudo-boehmite, 1.7g of ethyl silicate and SAPO-34 seed crystals into an appropriate amount of water, add 16g of triethylamine, 16g of diisopropylamine and 7g of tetraethylammonium hydroxide mixed template and stir for 10min to Disperse evenly, slowly add 40g of phosphorus source to the above mixture, after the reaction is sufficient, add 1.8g of silica sol to form a uniform gel, and transfer it to a stainless steel reactor, aging at room temperature for 1 hour, and raising the temperature at a rate of 1°C / min to Crystallize at 170°C for 12 hours, then heat up to 200°C for 10 hours in 90 minutes. After the crystallization, the mixture was cooled to room temperature, and the crystallized product was separated and washed repeatedly with deionized water until the filter cake was neutral. The molecular sieve crystallized product was dried in an oven at 110°C for 8 hours to obtain the original powder of SAPO-34 molecular sieve, which was calcined at 300°C fo...

Embodiment 2

[0030] Disperse 25g of pseudo-boehmite, 3.4g of ethyl silicate and SAPO-34 seed crystals into an appropriate amount of water, add 16g of triethylamine, 16g of diisopropylamine and 7g of tetraethylammonium hydroxide mixed template and stir for 10min to Disperse evenly, slowly add 40g of phosphorus source to the above mixture, after the reaction is sufficient, add 3.6g of silica sol to form a uniform gel, and transfer it to a stainless steel reactor, aging at room temperature for 1 hour, and raising the temperature at a rate of 0.5°C / min to Crystallize at 170°C for 10 hours, then heat up to 200°C for 8 hours in 90 minutes. After the crystallization, the mixture was cooled to room temperature, and the crystallized product was separated and washed repeatedly with deionized water until the filter cake was neutral. The molecular sieve crystallized product was dried in an oven at 110°C for 8 hours to obtain the original powder of SAPO-34 molecular sieve, which was calcined at 300°C f...

Embodiment 3

[0032] Disperse 25g of pseudo-boehmite, 4.4g of ethyl silicate and SAPO-34 seed crystals into an appropriate amount of water, add 32g of triethylamine and 7g of tetraethylammonium hydroxide mixed template agent and stir for 10min until the dispersion is uniform. Slowly add 40g of phosphorus source to the mixture. After the reaction is sufficient, add 3.6g of silica sol to form a uniform gel, and transfer it to a stainless steel reaction kettle, aging at room temperature for 2 hours, and crystallize at 170°C at a heating rate of 0.3°C / min. After 90 minutes, the temperature was raised to 200°C for 12 hours of crystallization. After the crystallization, the mixture was cooled to room temperature, and the crystallized product was separated and washed repeatedly with deionized water until the filter cake was neutral. The molecular sieve crystallized product was dried in an oven at 110°C for 8 hours to obtain the original powder of SAPO-34 molecular sieve, which was calcined at 300°...

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Abstract

The invention relates to a preparation method of a low-silicon SAPO‑34 molecular sieve, belonging to the technical field of synthesis and preparation of molecular sieves. By adding different proportions of silica sol and ethyl silicate step by step to control the interaction between the silicon source, the phosphorus source, the aluminum source and the template agent, and adopting a slow temperature rise method, the equilibrium between the solid phase and the liquid phase of the gel is achieved, so that the synthesized The molecular sieve has a relatively uniform acidity and particle size distribution. By adding SAPO-34 seeds to reduce the grain size, inhibit the formation of miscellaneous crystals, improve the selectivity of low-carbon olefins and prolong the catalyst life, and by reducing the proportion of water, Control the basicity of the synthesis system and reduce the amount of template used to realize the low-template synthesis of ultra-low silicon-aluminum ratio and small-grained SAPO-34 molecular sieve. The synthetic SAPO-34 molecular sieve of the present invention can be used for the reaction of methanol or dimethyl ether to produce low-carbon olefins, and C in its product 2 ~C 3 Olefin selectivity can reach 80%~86%.

Description

technical field [0001] The invention relates to a low-silicon SAPO-34 molecular sieve and its preparation method and application, which is a catalyst for the reaction of preparing olefins from methanol or dimethyl ether, and belongs to the technical field of molecular sieve preparation and application. Background technique [0002] SAPO-34 is an eight-membered ring small-pore silicon-aluminum-phosphorus molecular sieve with a chabazite (CHA) structure. It was first synthesized by Union Carbide in 1984. Its skeleton structure is composed of SiO 2 , AlO 2 - 、PO 2 + Three tetrahedral units are connected to each other. SAPO-34 has a three-dimensional pore structure with a pore diameter of about 0.38nm. Smaller gases such as ethylene, propylene, and butene can selectively pass through the pores of SAPO-34. SAPO-34 molecular sieve has moderate acidity, rich pore structure and good hydrothermal stability and thermal stability, which make it exhibit excellent catalytic performa...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B37/08C01B39/54B01J29/85B01J37/08C07C1/20C07C11/04C07C11/06
CPCB01J29/85B01J37/0018C01B37/08C01B39/54C01P2004/38C07C1/20C07C11/04C07C11/06Y02P20/52Y02P30/20Y02P30/40
Inventor 王闯王凤周君梦刘禹徐双
Owner CHIA TAI ENERGY MATERIALS DALIAN
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