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Sapo-34 molecular sieve having both micropores and mesopores and synthesis methods thereof

a technology of molecular sieve and micropore, which is applied in the direction of physical/chemical process catalysts, hydrocarbon oil treatment products, silicon compounds, etc., to achieve the effects of reducing or eliminating the influence of diffusion mass transfer, prolonging catalyst life, and reducing secondary reaction occurren

Inactive Publication Date: 2010-08-05
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Benefits of technology

[0005]An object of the present invention is to provide a SAPO-34 molecular sieve having both micropores and mesopores and the synthesis method thereof. By using the molecular sieve as a catalyst for MTO reaction, the limitation on diffusion mass transfer can be reduced or eliminated, the occurrence of secondary reaction can be decreased, and therefore the catalyst life can be prolonged, as well as the selectivity for ethylene and propylene can be increased.
[0024]By using the SAPO-34 molecular sieve having both micropores and mesopores synthesized in the present invention as the catalyst for MTO reaction, due to the presence of a hierachical structure, the influence on diffusion mass transfer can be reduced or eliminated, the occurrence of secondary reaction can be decreased, and therefore the catalyst life can be prolonged, as well as the selectivity for ethylene and propylene can be increased, greatly.

Problems solved by technology

Up till now, all the reported mesopore-micropore composite molecular sieves are of the molecular sieve system consisted of silicon and aluminum, however, as to the molecular sieve system consisted of silicon, phosphorus and aluminum, there are no opened literature reports because the synthesis system is relatively complex.

Method used

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  • Sapo-34 molecular sieve having both micropores and mesopores and synthesis methods thereof
  • Sapo-34 molecular sieve having both micropores and mesopores and synthesis methods thereof
  • Sapo-34 molecular sieve having both micropores and mesopores and synthesis methods thereof

Examples

Experimental program
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Effect test

example 1

[0043]Gauged raw materials were mixed in a certain sequence in an initial gel molar proportion of 3.0 TEA:0.4 SiO2:P2O5:Al2O3:50 H2O:1.0 T (T=n-propylamine), and all the raw materials used were TEA (analytical pure), silica sol (SiO2 content is 30 wt %), pseudobochmite (Al2O3 content is 70 wt %) and phosphoric acid (H3PO4 content is 85 wt %). A gel was formed by sufficient stirring, loaded into a stainless steel autoclave lined with polytetrafluoroethylene inside, sealed and heated to 200° C., and under autogenous pressure, a thermostatic crystallization was performed for 12 h. Then a solid product was separated by centrifugation, washed to be neutral with deionized water and dried in air at 120° C., and thus a SAPO-34 molecular sieve was obtained. After calcined the as-synthesized sample at 600° C. for 4 h to remove the template agent, a SAPO-34 molecular sieve having micropores and mesopores was obtained (the number was MSP34-1). The XRD pattern of the as-synthesized sample was sh...

example 2

[0045]The sample with a number of MSP34-1 obtained in example 1 and the sample with a number of SP34 obtained in comparative example 1 were subjected to a nitrogen physical adsorption characterization to measure the specific surface areas and the pore structures of the molecular sieves. The nitrogen adsorption isotherms and the mesopore distributions were shown in FIG. 3 and the specific surface areas and the pore volumes were shown in Table 1. The results indicated that SP34 sample had no mesopore structure and the specific surface area and pore volume thereof were all produced from the contribution of the micropore parts. MSP34-1 sample had a mesopore distribution with a mesopore pore diameter of 2.3 nm and a mesopore volume of 0.07 cm3 / g.

example 3

[0046]Gauged raw materials were mixed in a certain sequence in an initial gel molar proportion of 3.0 TEA:0.4 SiO2:P2O5:Al2O3:50 H2O:0.3 T (T=aqueous ammonia), and all the raw materials used were TEA (analytical pure), silica sol (SiO2 content is 30 wt %), pseudobochmite (Al2O3 content is 70 wt %) and phosphoric acid (H3PO4 content is 85 wt %). A gel was formed by sufficient stirring, loaded into a stainless steel autoclave lined with polytetrafluoroethylene inside, sealed and heated to 200° C., and under autogenous pressure, a thermostatic crystallization was performed for 12 h. Then a solid product was separated by centrifugation, washed to be neutral with deionized water and dried in air at 120° C., and thus a SAPO-34 molecular sieve was obtained. After calcined the sample at 600° C. for 4 h to remove the template agent, a SAPO-34 molecular sieve having micropores and mesopores was obtained (the number was MSP34-2). The XRD pattern of the as-synthesized sample was shown in FIG. 1...

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Abstract

The present invention relates to a SAPO-34 molecular sieve having both micropores and mesopores and synthesis method thereof. The mesopore diameter in the molecular sieve is in a range of 2-10 nm and the mesopore volume thereof is 0.03-0.3 cm3 / g. Triethylamine is used as a template agent and the pore size modifiers are added to the synthesis gel at the same time in the synthesis process, thereby the prepared molecular sieve crystals have mesopore distribution besides micropores. The SAPO-34 molecular sieve synthesized in the present invention can be used as catalysts for conversion of oxygen-containing compounds to lower olefins.

Description

FIELD OF THE INVENTION[0001]The present invention relates to a SAPO-34 molecular sieve having both micropores and mesopores, and the mesopore diameter of the molecular sieve is in a range of 2-10 nm and the pore volume thereof is 0.03-0.3 cm3 / g, as well as the synthesis method of the molecular sieve. The molecular sieve prepared by this method is used for the catalysis of the conversion reaction of oxygen-containing compounds to lower olefins.BACKGROUND[0002]The micropore-mesopore composite molecular sieves having double grade pores of micropores and mesopores have incorporated the pore advantage of mesopore materials with the strong acidic property and the high hydrothermal stability of micropore molecular sieves and made both of the materials complementary and cooperative. Furthermore, the pore diameter and acidic property are both adjustable, that is, a composite material with different pore allocations and acidic property distributions can be prepared by performing an optimized ...

Claims

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Application Information

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Patent Type & Authority Applications(United States)
IPC IPC(8): C01B39/04C01B39/54
CPCB01J29/85B01J35/1061B01J37/0018C01B37/08C10G2400/20C07C1/20C10G3/49C07C11/02Y02P30/20C01B39/04C01B39/10C01B39/54B01J35/647B01J29/041B01J35/60B01J35/69B01J35/643
Inventor XU, LEITIAN, PENGLIU, ZHONGMINYANG, LIXINMENG, SHUANGHEHE, CHANGQINGYUAN, CUIYUQI, YUE
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI