Nano-polycrystalline SAPO molecular sieve with high specific surface area, and preparation method and application thereof

A high specific surface area, SAPO-34 technology, applied in molecular sieve catalysts, molecular sieves and alkali-exchanged phosphates, molecular sieve characteristic silicoaluminophosphates, etc., can solve the problems of adverse effects on catalytic properties, long diffusion paths, and deterioration of dynamic adsorption properties

Inactive Publication Date: 2015-07-08
SHANGHAI FUYU NEW MATERIAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Since the openings of the molecular sieves with two structures of CHA and RHO are 0.38 and 0.36 nanometers respectively, and the reactant raw materials methanol, gaseous small molecules CO2, N2, CH The dynamic diameters of 4 are 0.390, 0.330, 0.364 and 0.380 nanometers, and the methanol molecule is very close to the pore size of the molecular sieve, and the diffusion path in the molecular sieve single crystal is longer, which obviously has an adverse effect on its catalytic properties
The adsorbent made of SAPO molecular sieve with large single crystal grain size can be used in pressure swing adsorption (PSA) CO2, N2, CH4, the dynamic adsorption properties will also deteriorate due to the same reason

Method used

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  • Nano-polycrystalline SAPO molecular sieve with high specific surface area, and preparation method and application thereof

Examples

Experimental program
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Effect test

preparation example Construction

[0028] Dry glue preparation

[0029] The raw material is hard kaolin from Mengxi Coal Measures in Inner Mongolia, with a fineness of 1250 mesh. Its chemical composition: SiO 2 : 46.5%, Al 2 o 3 : 38.3%, Fe 2 o 3 : 0.65%; SAR=2.09. The kaolin is heated to 550-600° C., kept for 4-6 hours, its crystal structure is destroyed to become amorphous metakaolin, and cooled to room temperature for use. Dilute phosphoric acid with a concentration of 85% in water, and aluminum hydroxide (Al 2 o 3 65%) powder is added slowly and vigorously stirred evenly, and then mixed with an appropriate amount of metakaolin in vigorously stirred to form a silica-aluminum-oxygen-phosphorus gel. The gel was heated at 90°C for 24 hours to form a dry gel. Grind it to dry rubber powder below 10 microns for use. Usually the molar composition of dry glue is SiO 2 :Al 2 o 3 :P 2 o 5 =0.6:1.0:1.0.

[0030] Examples of dry glue gas-solid phase crystallization reaction are listed in Table 1.

Embodiment 5

[0031] Embodiment 5, with the SAPO molecular sieve of embodiment 1,2,3,4 synthesis and reference sample commercially available SAPO-34 molecular sieve, at 550 0 C Roast for 4 hours, remove the organic matter and moisture in the molecular sieve channels and cool to room temperature, then put it into a BET adsorption instrument, under vacuum conditions at 350 0 C degassed for 5 hours, cooled to liquid nitrogen temperature (77K) to measure its nitrogen adsorption-desorption curve, see Figure 7 ~ Figure 10 . The calculated BET specific surface area, micropore surface area, external surface area, mesopore volume and micropore volume data are listed in Table 2. The data show that the BET surface area and mesopore volume of SAPO-34, SAPO-RHO and their eutectic molecular sieves synthesized by the present invention are significantly higher than that of the control sample. The adsorption-desorption isotherm shapes of the SAPO molecular sieves synthesized in Examples 1, 3, and the ref...

Embodiment 6

[0032] Example 6, the SAPO molecular sieves synthesized in Examples 1, 2, 3, and 4 and the commercially available SAPO-34 molecular sieve CO 2 , N 2 , CH 4 the equilibrium adsorption capacity. The adsorption temperature is 273K and the pressure is 100 Kpa. The pretreatment of the sample before the adsorption test was the same as in Example 5. CO 2 , N 2 , CH 4 Equilibrium adsorption capacity data, and the calculated CO 2 / N 2 , CO 2 / CH 4 The ratios (apparent adsorption selectivities) are listed in Table 2, respectively. Data show that the synthetic SAPO-34 of the present invention, SAPO-RHO and the eutectic molecular sieve CO of both 2 / CH 4 and CO 2 / N 2 The adsorption capacity ratio was significantly better than that of the control sample.

[0033] Catalyst preparation

[0034] The SAPO molecular sieve synthesized in Examples 1, 2, 3, 4 and the commercially available SAPO-34 molecular sieve of the reference sample are mixed with kaolin, aluminum sol and p...

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Abstract

The invention belongs to the technical field of zeolite molecular sieve materials, and concretely relates to a nano-polycrystalline SAPO molecular sieve with a high specific surface area, and a preparation method and an application thereof. The nano-polycrystalline SAPO molecular sieve with a high specific surface area is a CHA structure type or RHO structure type or CHA structure and RHO structure eutectic silicoaluminophosphate (SAPO) molecular sieve, is synthesized through a gas and solid phase crystal transformation reaction of a amorphous silica alumina phosphorus oxide dry glue in steam of a water and diethylamine mixed template, and is especially suitable for catalyzing adsorbing separation of micro-molecular gases from low carbon olefins prepared from methanol.

Description

technical field [0001] The invention belongs to the technical field of zeolite molecular sieve materials, and in particular relates to a silicon oxide aluminum oxygen phosphorus oxide (SAPO) molecular sieve and its preparation method and application. Background technique [0002] It is well known that SAPO-type silica aluminum oxygen phosphorus oxygen molecular sieve is a non-metallic oxide crystal composed of silicon oxygen tetrahedron, aluminum oxygen tetrahedron and phosphorus oxygen tetrahedron shared oxygen atom vertices, its skeleton structure contains regular and orderly arrangement, molecules The size of the channel or cage (pore diameter 0.33-1.5nm). It has the functions of shape-selective catalysis and molecular sieving, and is widely used in the fields of coal chemical industry, petrochemical industry and fine chemical industry. [0003] The silicoaluminophosphate molecular sieve SAPO-34 is the isomorph of the natural mineral zeolite Chabasite (Kalite). The struc...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/54C01B37/08B01J29/85B01J20/18C07C11/04C07C11/06C07C1/24
CPCY02P20/52
Inventor 龙英才林德昌魏小波陈伟
Owner SHANGHAI FUYU NEW MATERIAL TECH
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