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A kind of molecular sieve sapo‑34 with low silicon content and preparation method thereof

A SAPO-34, silicon content technology, applied in the direction of molecular sieve and alkali exchange phosphate, molecular sieve characteristic silicoaluminophosphate, etc., can solve the problems of difficult to obtain pure phase SAPO-34 molecular sieve, unfavorable scale-up production, etc., to achieve the reduction of impurities, Inexpensive, high catalytic performance effect

Inactive Publication Date: 2017-08-29
天津神能科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The problem to be solved by the present invention is that when the existing silicoaluminophosphate molecular sieve SAPO-34 is synthesized, impurities are likely to be produced after the feed ratio of the silicon source in the raw material is reduced, and it is difficult to obtain a pure phase SAPO-34 molecular sieve, which is not conducive to industrial scale-up production

Method used

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  • A kind of molecular sieve sapo‑34 with low silicon content and preparation method thereof
  • A kind of molecular sieve sapo‑34 with low silicon content and preparation method thereof

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Embodiment 1

[0026] A preparation method of molecular sieve SAPO-34 with low silicon content comprises the following steps:

[0027] (1) Gelling: Dissolve 264g of phosphorous acid in 500ml of water, add 200ml of phosphoric acid dropwise while stirring, mix this mixed acid solution with 16.9ml of silica sol, and then mix it with a solution of 212.3g of pseudo-boehmite and 500ml of water And stir quickly, add 202.4g triethylamine while stirring, stir for 1 hour, then add 500ml water, mix well to obtain synthetic colloid, gel forming temperature is 25°C.

[0028] (2) Hydrothermal crystallization: The synthetic colloid obtained in step (1) was ultrasonicated at 20 kHz for 1 hour, then transferred into a stainless steel reactor, and hydrothermally crystallized at 190° C. and autogenous pressure for 30 hours.

[0029] (3) Post-treatment: the product after hydrothermal crystallization in step (2) was collected, washed, and dried at 60° C. to obtain the silicoaluminophosphate molecular sieve SAPO-...

Embodiment 2

[0033] A preparation method of molecular sieve SAPO-34 with low silicon content comprises the following steps:

[0034] (1) Gel formation: Dissolve 82 g of phosphorous acid in 500 ml of water, and add 133.3 ml of phosphoric acid dropwise during stirring to obtain a mixed acid solution. Mix the mixed solution of 4g of white carbon black and 100ml of water with the mixed acid solution to obtain the mixture A. Mix 200g of pseudo-boehmite powder with 200ml of water to obtain mixture B. Then, add mixture A to mixture B and stir rapidly. After 40 minutes, add 202.4 g of triethylamine and 500 ml of water while stirring, and stir for 1 hour to obtain a synthetic colloid. The gel forming temperature is 30°C.

[0035] (2) Hydrothermal crystallization: The synthetic colloid obtained in step (1) was ultrasonicated at 30 kHz for 2 hours, then moved into a stainless steel reactor, and hydrothermally crystallized at 192° C. and autogenous pressure for 24 hours.

[0036] (3) Post-treatment:...

Embodiment 3

[0038] A preparation method of molecular sieve SAPO-34 with low silicon content comprises the following steps:

[0039] (1) Gelling: dissolve 61.5g of phosphorous acid in 600ml of water, then add 150ml of phosphoric acid dropwise, add this mixed acid aqueous solution to 364.3g of aluminum isopropoxide solid powder and stir rapidly for 120min, while stirring, add 303.6g of triethylamine , add 1000ml of water, and finally add 4.7g of white carbon black, stir until uniform, then continue to stir for 2h, and obtain a synthetic colloid at 35°C.

[0040](2) Hydrothermal crystallization: The synthetic colloid obtained in step (1) was ultrasonicated at 25 kHz for 3 hours, then moved into a stainless steel reactor, and hydrothermally crystallized at 196° C. and autogenous pressure for 36 hours.

[0041] (3) Post-treatment: the hydrothermal crystallized product in step (2) was collected, washed, and dried at 75° C. to obtain the silicoaluminophosphate molecular sieve SAPO-34.

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Abstract

The invention provides a molecular sieve SAPO-34 with a low content of silicon and a preparation method of the molecular sieve and belongs to the technical field of synthesis and preparation of molecular sieves. The preparation method of the molecular sieve comprises the following steps: gelling, carrying out hydrothermal crystallization and carrying out post-treatment, wherein the raw materials comprise SiO2, Al2O3, P, R and H2O in a mole ratio of (0.01-0.15) to (0.3-1.5) to 3 to (0.5-8.0) to (30-150); a phosphorus source is a mixture of phosphorous acid and phosphoric acid; the mole ratio of H2PO4 to H3PO3 is 0.5-9; an organic amine template agent is triethylamine. The preparation method of the molecular sieve SAPO-34 with the low content of silicon is simple in step and convenient to operate; products with few impurities can be prepared at a low silicon charging ratio; the preparation method of the molecular sieve SAPO-34 with the low content of silicon is suitable for industrial expanded production.

Description

technical field [0001] The invention relates to the technical field of synthesis and preparation of molecular sieves, in particular to a molecular sieve SAPO-34 with low silicon content and a preparation method thereof. Background technique [0002] The skeleton of silicoaluminophosphate molecular sieve SAPO-34 is composed of Si, P, Al, O elements, which belongs to the chabazite structure, and the International Zeolite Society named it CHA. A cage-shaped channel system with an eight-membered ring opening has a free diameter of 0.43 nm, belongs to a trigonal crystal system, and has a unit cell size of a=b=1.37nm and c=1.48nm. Due to the existence of Si-O-Al links in the framework structure of SAPO-34, the molecular sieve is acidic. They have high thermal stability and hydrothermal stability, and have adsorption stability and skeleton stability under the conditions of high temperature and the presence of a large amount of water vapor. It is precisely because of its unique sm...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/54C01B37/08
CPCC01B37/08C01B39/54C01P2002/72C01P2004/02
Inventor 王震宇王宝义贾志远
Owner 天津神能科技有限公司