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Method for preparing SAPO (Silico-Aluminophosphate) molecular sieve material with multi-level-hole structure

A molecular sieve and multi-stage pore technology, applied in the direction of molecular sieve and alkali exchange phosphate, molecular sieve characteristic silicoaluminophosphate, etc., can solve the problem that it is difficult to obtain the SAPO molecular sieve overall material with a multi-stage pore structure, and achieve easy control and preparation process simple effect

Inactive Publication Date: 2011-10-19
CHINA PETROLEUM & CHEM CORP +1
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The technical problem to be solved by the present invention is that it is difficult to obtain a SAPO molecular sieve monolithic material with a multi-level pore structure in the existing preparation methods, and a new preparation method for a SAPO molecular sieve monolithic material containing mesopores or macropores is provided

Method used

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  • Method for preparing SAPO (Silico-Aluminophosphate) molecular sieve material with multi-level-hole structure
  • Method for preparing SAPO (Silico-Aluminophosphate) molecular sieve material with multi-level-hole structure
  • Method for preparing SAPO (Silico-Aluminophosphate) molecular sieve material with multi-level-hole structure

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Embodiment 1

[0023] 6.63 grams of aluminum chloride hexahydrate, 0.82 grams of methyl orthosilicate, 1.5 grams of polyethylene glycol (molecular weight 10,000, referred to as PEG) and 3.36 grams of dipotassium hydrogen phosphate were added to the mixed solution of 4.35 grams of ethanol and 15.99 grams of water, Stir to dissolve at room temperature, add 5.00 g of propylene oxide (PO) to the mixed solution, and stir evenly. Pour the mixture into a mold to seal it, and place it in an oven at 60°C for 24 hours of aging. After taking it out, it was demoulded, dried at 60°C, and finally calcined at 550°C for 8 hours to obtain a silicon phosphorus aluminum oxide monolithic material. The obtained amorphous silicon phosphorus aluminum oxide monolith was immersed in the tetraethylammonium hydroxide solution for 24 hours, dried at room temperature for 24 hours, then placed on the upper part of the gas phase reactor, and water was added to the bottom of the reactor. Crystallization at 200°C for 3 day...

Embodiment 2

[0025] 6.63 grams of aluminum chloride hexahydrate, 0.82 grams of methyl orthosilicate, 1.5 grams of polyethylene glycol (molecular weight 10,000, referred to as PEG), and 7.83 grams of disodium hydrogen phosphate were added to a mixed solution of 4.35 grams of ethanol and 15.99 grams of water, Stir to dissolve at room temperature, then adjust the pH value to 8 with alkali, add 5.00 g of propylene oxide (PO) to the mixed solution, and stir evenly. Pour the mixture into a mold to seal it, and place it in an oven at 60°C for 24 hours of aging. After taking it out, it was demoulded, dried at 60°C, and finally calcined at 550°C for 8 hours to obtain a silicon phosphorus aluminum oxide monolithic material. Place the obtained amorphous silicon phosphorus aluminum oxide monolith in the upper part of the gas phase reactor, add tetraethylammonium hydroxide solution at the bottom of the reactor, and crystallize at 200°C for 3 days; after the reaction, the reactor is cooled in a natural ...

Embodiment 3

[0027] 6.63 grams of aluminum chloride hexahydrate, 0.82 grams of methyl orthosilicate, 1.5 grams of polyethylene glycol (molecular weight 10,000, referred to as PEG), and 5.83 grams of dipotassium hydrogen phosphate were added to a mixed solution of 4.35 grams of ethanol and 15.99 grams of water, Stir to dissolve at room temperature, then adjust the pH value to 8 with alkali, add 5.00 g of propylene oxide (PO) to the mixed solution, and stir for 1 minute. Pour the mixture into a mold to seal it, and place it in an oven at 60°C for 24 hours of aging. After taking it out, it was demoulded, dried at 60°C, and finally calcined at 550°C for 8 hours to obtain a silicon phosphorus aluminum oxide monolithic material. The obtained amorphous silicon phosphorus aluminum oxide monolith was immersed in the tetraethylammonium hydroxide solution for 24 hours, dried at room temperature for 24 hours, then placed on the upper part of the gas phase reactor, and water was added to the bottom of ...

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Abstract

The invention relates to a method for preparing SAPO (SIlico-Aluminophosphate) molecular sieve material with a multi-level-hole structure, mainly solving the problem that the whole SAPO molecular sieve material with the multi-level-hole structure is difficult to obtain in the prior art. The method adopts the following technical scheme for better solving the problem: adopting and hydrolyzing a mixture of phase-separation inducer R1, a gel accelerator R2, an organic solvent R3, water, a phosphorus source, a silicon source and an aluminum source to obtain a precursor I of silicon-phosphorus-aluminum oxide material; carrying out gel aging on the precursor I, thus obtaining a precursor II of the silicon-phosphorus-aluminum oxide material; drying and roasting the precursor II of the silicon-phosphorus-aluminum oxide material, thus obtaining silicon-phosphorus-aluminum oxide material III with a double-continuous-large-hole structure; dipping the silicon-phosphorus-aluminum oxide material III into solution containing a template agent, drying the silicon-phosphorus-aluminum oxide material III, then arranging the silicon-phosphorus-aluminum oxide material III at the upper part of a reaction kettle, adding organic amine solution at the bottom of the reaction kettle, and then crystallizing; and after the crystallization, washing, drying and roasting a sample, thus obtaining the whole SAPO molecular sieve material with the multi-level-hole structure. The method can be used for industrial production of the molecular sieve with multi-level-hole structure.

Description

technical field [0001] The invention relates to a preparation method of a SAPO molecular sieve integral material with a hierarchical pore structure. Background technique [0002] Due to its suitable distribution of acid centers and special pore structure, SAPO molecular sieves are widely used in cracking, alkylation, isomerization, polymerization, reforming, hydrogenation, dehydrogenation, hydration and other hydrocarbon reactions. In the reaction, especially in the reaction of catalyzing methanol to olefins, it shows excellent catalytic performance, but the application of SAPO molecular sieve is restricted due to the problems of pore structure, morphology and preparation method. The first is the pore structure, because the traditional SAPO molecular sieve only has a microporous structure, which greatly limits the mass transfer and diffusion of macromolecules such as heavy oil components in the catalyst, thereby inhibiting the reactivity, selectivity and life of the catalyst...

Claims

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Application Information

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IPC IPC(8): C01B39/54C01B37/08
Inventor 杨贺勤谢在库刘志成高焕新
Owner CHINA PETROLEUM & CHEM CORP
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