Synthesis method of nano sapo-34 molecular sieve, sapo-34 molecular sieve catalyst and application thereof

A technology of SAPO-34 and molecular sieve, which is applied in the field of molecular sieves, can solve the problems of limiting molecular mass transfer process, large particle size of molecular sieves, unfavorable MTO catalytic reaction results, etc., and achieves the effects of increased selectivity, prolonged catalyst life, and excellent catalytic performance

Active Publication Date: 2019-12-27
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In addition, the particle size of SAPO-34 molecular sieve guided by triethylamine is relatively large (3-5 μm), which will limit the molecular mass transfer process in the MTO reaction.
These are not conducive to obtaining excellent MTO catalytic reaction results

Method used

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  • Synthesis method of nano sapo-34 molecular sieve, sapo-34 molecular sieve catalyst and application thereof
  • Synthesis method of nano sapo-34 molecular sieve, sapo-34 molecular sieve catalyst and application thereof
  • Synthesis method of nano sapo-34 molecular sieve, sapo-34 molecular sieve catalyst and application thereof

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Experimental program
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preparation example Construction

[0036] In the present invention, preferably, the synthetic method of described nanometer SAPO-34 molecular sieve comprises following synthetic steps:

[0037] a) After dissolving functionalized organosilane in water, sequentially add aluminum source, phosphorus source, organic amine and additional silicon source (ie organic silicon source or inorganic silicon source) to obtain a mixture with the following molar ratio (wherein The addition amount of functionalized organosilane and the additional silicon source is SiO 2 In terms of moles, the amount of phosphorus source added is P 2 o 5 In terms of moles, the amount of aluminum source added is Al 2 o 3 in moles):

[0038] SiO 2 :P 2 o 5 :Al 2 o 3 : Organic amine: H 2 O=0.2~1.2: 0.5~1.5: 0.6~1.4: 1.5~5.5: 50~200;

[0039]b) crystallize the mixture obtained in step a) at 150-220° C. for 0.4-10 days;

[0040] c) After the crystallization of the step b) is completed, the solid product is separated, washed and dried to ob...

Embodiment 1

[0063] The molar proportions of each raw material, crystallization conditions and elemental composition of the samples are shown in Table 1. The specific batching process is as follows:

[0064] 9.28g PiSi-3 and 71.40g deionized water were mixed and stirred for 1 hour, and 135.64g pseudoboehmite (Al 2 o 3 Mass percentage composition 72.5%), 34.58g phosphoric acid (H 3 PO 4 85% by mass), 20.24g of triethylamine and 8.33g of tetraethyl orthosilicate, and then stirred and aged for 24 hours, and then the gel mixture was transferred to a stainless steel reactor. The molar ratio of each component in the synthesis system is 0.8SiO 2 : 1.5P 2 o 5 : 0.8Al 2 o 3 :2TEA:80H 2 O, the molar ratio of PiSi-3 to ethyl orthosilicate is 1:1.

[0065] After putting the reaction kettle into the oven, the temperature was programmed to rise to 200°C, and the static crystallization was carried out for 48 hours. After the reaction, the solid product was centrifuged, washed repeatedly with d...

Embodiment 2～12

[0079] The specific batching ratio and crystallization conditions are shown in Table 1, and the specific batching process is the same as in Example 1.

[0080] Carry out XRD analysis to embodiment 2~12 gained sample, data result is close to table 2, namely peak position and shape are identical, according to the variation of synthetic conditions, the relative peak intensity of peak fluctuates in ± 10% scope, shows that synthetic product has SAPO Features of -34 structures.

[0081] XRF elemental composition analysis was performed on the samples obtained in Examples 2-12, and the results are shown in Table 1.

[0082] Adopt scanning electron microscope to analyze the morphology of embodiment 2~12 gained sample, gained electron micrograph is all with figure 1 resemblance.

[0083] Table 1: Molecular sieve synthesis ingredients, crystallization conditions and elemental composition

[0084]

[0085] Table 2: XRD results of the samples obtained in Example 1

[0086]

[0087]...

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Abstract

The application relates to a method for synthesizing nanometer SAPO-34 molecular sieves, SAPO-34 molecular sieve catalysts and applications thereof. Synthesis by adding microporous templates and having formula I (wherein R 1 ~R 3 , x, y and n are as defined herein) the functionalized organosilane templating agent of the structure shown in, synthesized nanometer SAPO-34 molecular sieve. The nano SAPO-34 molecular sieve is calcined to obtain a SAPO-34 molecular sieve catalyst, which can be used in the reaction of producing low-carbon olefins from oxygen-containing compounds. The nano SAPO-34 molecular sieve obtained by the method of the present invention has a pure CHA crystal phase, and the SAPO-34 molecular sieve catalyst obtained by the method of the present invention shows excellent catalytic performance in the MTO reaction, the catalyst life is significantly prolonged, low carbon Olefin selectivity is improved.

Description

technical field [0001] The invention relates to the field of molecular sieves, in particular to a synthesis method of SAPO-34 molecular sieves, a SAPO-34 molecular sieve catalyst and applications thereof. Background technique [0002] The framework structure of silicoaluminophosphate molecular sieve (SAPO-n) is various, and its three-dimensional framework structure is composed of PO 2 + , AlO 2 - and SiO 2 tetrahedron composition. The Si atom isomorphically replaces part of the P atoms in the neutral aluminum phosphate skeleton structure or simultaneously replaces the P and Al atoms, so that the skeleton generates a net negative charge, causing proton acidity, thereby endowing the SAPO molecular sieve with acid catalytic properties. [0003] Among them, the SAPO-34 molecular sieve with CHA topology has been successfully applied in the MTO commercialization process due to its excellent catalytic performance in the methanol-to-olefins (MTO) reaction. However, the intrins...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/54C01B37/08B82Y30/00B01J29/85C07C1/20C07C11/04C07C11/06
CPCB01J29/85B01J35/1023B01J35/1038B82Y30/00C01B37/08C01B39/54C01P2002/72C01P2004/03C01P2004/32C01P2004/61C01P2006/12C01P2006/14C07C1/20C07C11/04C07C11/06Y02P20/52Y02P30/20Y02P30/40
Inventor 吴鹏飞杨淼田鹏刘中民王林英刘琳
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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