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Method for synthesizing SAPO-35 molecular sieve

A technique for the synthesis of SAPO-35, which is applied in the direction of molecular sieves, alkali-exchanged phosphates, molecular sieve characteristic silicoaluminophosphates, etc., to achieve the effects of high product yield, high specific surface area, good thermal stability and hydrothermal stability

Active Publication Date: 2009-04-01
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This method uses hexamethyleneimine (HMI) and hexamethylenediamine (HDA) as dual templates, but only gives SiO 2 / Al 2 o 3 Example of synthesizing SAPO-35 molecular sieve when =0.3

Method used

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  • Method for synthesizing SAPO-35 molecular sieve
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  • Method for synthesizing SAPO-35 molecular sieve

Examples

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Embodiment 1

[0027] This example illustrates the synthesis method of the SAPO-35 molecular sieve provided by the present invention.

[0028] 155g phosphoric acid (containing H 3 PO 4 85w%, industrial product) and 619.9g of deionized water are added to the gelling kettle placed in a water bath of 60°C and mixed and stirred evenly. After stirring for 10 minutes, 102g of hydrated aluminum oxide (containing Al 2 o 3 70w%), continue stirring for no less than 1 hour, then add 33.6g silica sol (containing SiO 2 25w%) and stirred for 0.5 hour, then added 105.2g of hexamethyleneimine (chemically pure) into the above-mentioned gelling kettle and mixed evenly to prepare a reaction mixture. Part of the above-mentioned mixed material was transferred into a stainless steel crystallization kettle and sealed, and stirred and crystallized at 200° C. and autogenous pressure for 24 hours. The crystallized product is then filtered, washed, and dried at 100-110°C to obtain the molecular sieve raw powder pr...

Embodiment 2

[0034] This example illustrates the synthesis method of the SAPO-35 molecular sieve provided by the present invention.

[0035] In Example 1, 33.6g of silica sol was changed into 50.5g of silica sol, 619.9g of deionized water was changed into 607.8g of deionized water, and gel was mixed in a gelling kettle placed in a water bath at 70°C. The separation and synthesis conditions were unchanged, and the molecular sieve raw powder product A2 was obtained, and the XRD analysis results of A2 were consistent with the data in Table 1, indicating that it was a SAPO-35 molecular sieve. The X-ray powder diffraction measurement result of the molecular sieve after roasting removes template agent accords with the data in table 2, and the element chemical composition of this molecular sieve is Al 2 o 3 :P 2 o 5 :SiO2 2 =1:0.77:0.31, the specific surface area after calcining to remove the template is 493m 2 / g, the pore volume is 0.254ml / g.

Embodiment 3

[0039] This example illustrates the synthesis method of the SAPO-35 molecular sieve provided by the present invention.

[0040] Change 33.6g of silica sol in Example 1 to 134.6g of silica sol, 619.9g of deionized water to 544.2g of deionized water, the gelling temperature is 50°C, and the remaining components and synthesis conditions remain unchanged to obtain the molecular sieve raw powder The XRD analysis results of sample A3 and A3 are consistent with the data in Table 1, indicating that it is SAPO-35 molecular sieve. The X-ray powder diffraction measurement results of the molecular sieve after the template agent was removed by calcination accord with the data in Table 2. The elemental chemical composition of the molecular sieve is Al 2 o 3 :P 2 o 5 :SiO2 2 =1:0.79:0.75, the specific surface area after calcining to remove the template is 491m 2 / g, the pore volume is 0.31ml / g.

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Abstract

The invention provides a method for synthesizing a SAPO-35 molecular sieve, comprising the steps as follows: aluminium source, silicon source, phosphor source and organic template agent are mixed as glue so as to prepare reaction mixture with the mol composition of aR:Al2O3:bP2O5:cSiO2:dh2O under the temperature of 35-100 DEG C; the mixture is hydro-thermally crystallized for 0.5-500 hours under the temperature of 150-210 DEG C and the self-pressure; the SAPO-35 molecular sieve is gained by recovering crystallized product; wherein, the organic template agent is hexamethylene imine; wherein, a is 0.5-1.8; b is 0.5-1.5, c is 0.05-2.5 and d is 10-150; the method can synthesize the SAPO-35 molecular sieve with high crystallinity under wide silicon content range; the structure of the SAPO-35 molecular sieve synthesized by the method is basically unchanged before and after the release agent is baked and deprived under high temperature and the SAPO-35 molecular sieve has high specific surface area. The molecular sieve has extremely low alkane selection when being applied to the olefin preparation reaction from dehydration of carbinol; furthermore, the outcome yield of ethane and propylene is high.

Description

technical field [0001] The invention relates to a method for synthesizing SAPO-35 molecular sieves, more specifically, a method for synthesizing SAPO-35 molecular sieves using hexamethyleneimine as a template. Background technique [0002] Aluminum phosphate molecular sieve is a new generation of molecular sieve (US4310440) invented by UCC Company in the United States in the early 1980s after aluminum silicate molecular sieve. Since the molecular sieve framework is electrically neutral, it has no cation exchange performance and catalytic reaction performance. Aluminum phosphate molecular sieves are a series of molecular sieves with unique XRD characteristic spectra and data. Among them, there are molecular sieves with the same crystal structure as the existing aluminum silicate molecular sieves, and there are also new structures that are not found in the existing aluminum silicate molecular sieves. of molecular sieves. [0003] Introducing silicon into the framework of alu...

Claims

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Application Information

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IPC IPC(8): C01B39/54C01B37/08
Inventor 张凤美匡晓辉李黎声舒兴田王卫东秦凤明
Owner CHINA PETROLEUM & CHEM CORP
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