Preparation method of silicon aluminum phosphate molecular sieve of multilevel porous structure, prepared molecular sieve and application of molecular sieve

A silicoaluminophosphate, pore structure technology, applied in molecular sieve and alkali-exchanged phosphate, molecular sieve catalyst, chemical instruments and methods, etc., can solve the problems of high cost, cumbersome operation process, etc. The effect of good catalytic performance

Inactive Publication Date: 2018-07-10
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The technical problem to be solved by the present invention is the cumbersome operation process and high cost problems existing in the synthesis of mesoporous templates in the prior art, and a new method for preparing a multi-stage pore structure silicoaluminophosphate molecular sieve is provided

Method used

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  • Preparation method of silicon aluminum phosphate molecular sieve of multilevel porous structure, prepared molecular sieve and application of molecular sieve
  • Preparation method of silicon aluminum phosphate molecular sieve of multilevel porous structure, prepared molecular sieve and application of molecular sieve
  • Preparation method of silicon aluminum phosphate molecular sieve of multilevel porous structure, prepared molecular sieve and application of molecular sieve

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] To prepare SAPO-34 molecular sieve with hierarchical pore structure, the raw material is taken from the conventional SAPO-34 molecular sieve A prepared according to [Comparative Example 1], which only contains micropores.

[0037] Weigh 30g of molecular sieve A and place it in 0.05M citric acid solution, wherein the amount of citric acid solution is 0.9L, stir at 75°C for 3 hours, filter, wash, dry and roast to obtain product B.

[0038] The XRD spectrum of B is as figure 1 shown, from figure 1 It can be seen that the synthesized molecular sieve has the characteristic diffraction peaks of SAPO-34 molecular sieve, indicating that the synthesized product is pure SAPO-34 molecular sieve with a relative crystallinity of 95%.

[0039] The SEM photograph of B is as image 3 As shown, obvious pore structure appeared on the surface of molecular sieve.

[0040] The micropore diameter of B is distributed in 0.3-0.5nm, the mesopore diameter is distributed in 5-18nm, and the mac...

Embodiment 2

[0043] Same as [Example 1], except that the raw material used is the conventional SAPO-34 molecular sieve A roasted product prepared according to the method of [Comparative Example 1], which only contains micropores. The final obtained SAPO-34 molecular sieve with hierarchical pore structure is denoted as C.

[0044] The XRD spectrum of C is as figure 1 shown, from figure 1 It can be seen that the synthesized molecular sieve has the characteristic diffraction peaks of SAPO-34 molecular sieve, indicating that the synthesized product is pure SAPO-34 molecular sieve with a relative crystallinity of 92%.

[0045] SEM photographs of C with image 3 similar.

[0046] C The micropore diameter is distributed in 0.3-0.5nm, the mesopore diameter is distributed in 8-28nm, and the macropore diameter is distributed in 50-250nm; the pore volume contributed by the micropore is 0.21cm 3 / g, the pore volume contributed by mesopores is 0.25cm 3 / g, the pore volume contributed by macropores...

Embodiment 3

[0049] Same as [Example 1], except that the concentration of citric acid is 0.1M, the consumption of citric acid is 0.6L, the reaction temperature is 65°C, and the reaction time is 6 hours, and the obtained product is marked as D.

[0050] The XRD spectrum of D is as figure 1 shown, from figure 1 It can be seen that the synthesized molecular sieve has the characteristic diffraction peaks of SAPO-34 molecular sieve, indicating that the synthesized product is pure SAPO-34 molecular sieve with a relative crystallinity of 89%.

[0051] The SEM photograph of D with image 3 similar.

[0052] D The micropore diameter is distributed in 0.3-0.5nm, the mesopore diameter is distributed in 5-30nm, and the macropore diameter is distributed in 50-250nm; the pore volume contributed by the micropore is 0.20cm 3 / g, the pore volume contributed by mesopores is 0.25cm 3 / g, the pore volume contributed by macropores is 0.19cm 3 / g.

[0053] According to the SEM photographs and the pore vol...

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Abstract

The invention relates to a preparation method of a silicon aluminum phosphate molecular sieve of a multilevel porous structure, the prepared molecular sieve and application of the molecular sieve. Thepreparation method and the prepared molecular sieve are mainly used for solving the problems that the operation process is complicated and the cost is high since mesoporous template agents are adopted for synthesis in the prior art. The method includes the step of adopting the silicon aluminum phosphate molecular sieve of the porous structure for being in contact with a solution containing a modifier, wherein at least one of ammonium hydroxide, oxalic acid, acetic acid, ethanedioic acid, citric acid, sodium carbonate, sodium acetate trihydrate, sodium acetate, sodium hypochlorite, tetraethylammonium hydroxide, tetrapropylammonium hydroxide and tetrabutyl ammonium hydroxide is adopted as the modifier. By means of the technical scheme, the problems above are well solved, and the preparationmethod can be applied to industrial production of silicon aluminum phosphate molecular sieves of multilevel porous structures.

Description

technical field [0001] The invention relates to a preparation method of a silicon-aluminophosphate molecular sieve with a hierarchical pore structure, the prepared molecular sieve and its application. Background technique [0002] In 1984, United Carbide Corporation (UCC) invented a silicoaluminophosphate molecular sieve (SAPO molecular sieve) with a pore size of about 0.4nm. SAPO molecular sieve is made of AlO 4 , SiO 4 and PO 4 The crystal network structure composed of tetrahedrons, the pores in the crystal are due to Si 4+ replace P 5+ or Al 3+ The acidity produced or replaced by metals to produce acidity. Among SAPO series molecular sieves, SAPO-34 molecular sieve is widely used in modern petroleum processing industry because of its good thermal and hydrothermal stability, moderate acidity, high specific surface area and highly ordered micropore channels. middle. The most striking thing is that the molecular sieve is used in the reaction of methanol to olefins (M...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/54B01J29/85
CPCB01J29/85C01B39/54C01P2002/72C01P2004/03C01P2006/14C01P2006/16C01P2006/17
Inventor 丁佳佳刘红星陆贤张玉贤钱坤
Owner CHINA PETROLEUM & CHEM CORP
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