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Method for synthesizing SAPO-35 molecular sieve by using bi-template

A technology of SAPO-35 and molecular sieve, which is applied in the direction of molecular sieve and alkali exchange phosphate, molecular sieve characteristic silicoaluminophosphate, etc., can solve the problems of long crystallization time, achieve high thermal stability, hydrothermal stability, and high specific surface area Effect

Active Publication Date: 2009-04-29
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method can only be used in higher template dosage, longer crystallization time, and only SiO in the reaction mixture 2 / Al 2 o 3 = 0.1 ~ 1.0 (molar ratio) to obtain pure SAPO-35 molecular sieve

Method used

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  • Method for synthesizing SAPO-35 molecular sieve by using bi-template
  • Method for synthesizing SAPO-35 molecular sieve by using bi-template
  • Method for synthesizing SAPO-35 molecular sieve by using bi-template

Examples

Experimental program
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Effect test

Embodiment 1

[0033] 22.1g phosphoric acid (containing H 3 PO 4 85w%, industrial product) and 77.8g deionized water are added in the gel forming kettle and mixed and stirred evenly under the condition of 60 ℃, after stirring for 10 minutes, 14.6g of hydrated aluminum oxide (containing Al 2 o 3 70w%), continue to stir for no less than 1 hour, then add 7.2g silica sol (containing SiO 2 25w%) and stirred for 0.5 hour, and then the mixture of (8.4g hexamethyleneimine+2.1g cyclohexylamine) was added into the above-mentioned gelling kettle and mixed evenly to prepare a reaction mixture. The above-mentioned part of the mixed material was transferred into a stainless steel crystallization kettle and sealed, and rotated and dynamically crystallized at 200° C. under 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 product A1. The X-ray powder diffraction measurement results of A1 are consistent wit...

Embodiment 2

[0047] In Example 1, change 7.2g silica sol to 14.4g silica sol, change 77.8g deionized water to 72.3g deionized water, then change (8.4g hexamethyleneimine+2.1g cyclohexylamine) to (10.5g hexamethyleneimine + 4.5g cyclohexylamine), the gelation temperature is 55°C, and 1.4g SAPO-35 molecular sieve is added as a seed crystal, the rest of the components and synthesis conditions remain unchanged, and the product is analyzed by XRD It is SAPO-35 molecular sieve. The specific surface area of ​​the molecular sieve after calcination to remove the template agent is 493m 2 / g, the pore volume is 0.25ml / g.

Embodiment 3

[0049] In Example 1, change 7.2g silica sol to 24g silica sol, change 77.8g deionized water to 65.1g deionized water, then change (8.4g hexamethyleneimine+2.1g cyclohexylamine) to (10.5g hexamethyleneimine + 4.5g cyclohexylamine), the gelation temperature is 65°C, and 1.52g SAPO-35 molecular sieve is added as a seed crystal, the remaining components and synthesis conditions remain unchanged, and the product is analyzed by XRD as SAPO-35 molecular sieve. The specific surface area of ​​the molecular sieve after calcination to remove the template agent is 490m 2 / g, the pore volume is 0.25ml / g.

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Abstract

The invention discloses a method for synthesizing an SAPO-35 molecular sieve by a two-mode agent, which is characterized in that the method comprises the steps of mixing aluminum source, phosphorus source, silicon source and an organic template to glue at the temperature of room temperature to 100 DEG C and preparing into the reaction mixture with the molar ratio components of a1R1+a2R2: Al2O3: bP2O5: cSiO2: dH2O, wherein R1 and R2 are the organic templates, the value of a1 is 0.5-1.8, the value of a2 is 0.1-1.0, the value of b is 0.5-1.5, the value of c is 0.05-2.5, and the value of d is 10-150; the reaction mixture undergoes hydrothermal crystallization for 0.5-500 hours at the temperature of 150-250 DEG C and the crystallization product is recovered. The R1 is hexamethylene imine, and the R2 is any of cyclohexane, piperidine, tropine, diethylamine and triethylamine. The method provided by the invention can synthesize the high-crystallinity SAPO-35 molecular sieve in a relatively wide silica content range. The SAPO-35 molecular sieve synthesized by the method of the invention is applicable to the hydrocarbon conversion technology. Applied to the olefin preparation reaction by methanol dehydration, the molecular sieve has very low alkane selectivity and high product yield of ethylene and propylene.

Description

technical field [0001] The invention relates to a method for synthesizing molecular sieves, more specifically, a method for synthesizing SAPO-35 molecular sieves with double templates. Background technique [0002] Aluminum phosphate molecular sieve is a new generation of molecular sieve (US 4310440) invented by UCC in the early 1980s after aluminum silicate molecular sieve. Alternately connected, because 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] When silicon is introduced into the framework of aluminum phosphate molec...

Claims

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Application Information

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Patent Type & Authority Applications(China)
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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