Method for synthesizing SAPO-5 with diethylamine as a template and recovering template

A SAPO-5, recovery method technology, applied in molecular sieve and alkali-exchanged phosphate, molecular sieve characteristic silicoaluminophosphate and other directions, can solve the problems of unrecoverable template agent, low product yield, long crystallization time, etc. The effect of short chemical reaction time, high product yield and low cost

Inactive Publication Date: 2008-11-12
SHANGHAI SECOND POLYTECHNIC UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The object of the present invention is to provide a kind of method simple, lower cost SAPO-5 material and preparation method thereof, overcome the shortcoming of long crystallization time in the prior art, product yield is low, template agent can't be recycled, expand SAPO-5 5 Preparation temperature range

Method used

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  • Method for synthesizing SAPO-5 with diethylamine as a template and recovering template
  • Method for synthesizing SAPO-5 with diethylamine as a template and recovering template

Examples

Experimental program
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Effect test

Embodiment 1

[0018] Al(OH) in molar ratio 3 : 2H 3 PO 4 : 1SiO 2 :2R:500H 2 O mixed pseudo-boehmite, phosphoric acid, white carbon black and diethylamine raw materials. Mix and stir evenly, seal and heat in an oven at 345°C for 0.2 hours. Suction filtration, drying, and calcination at 600°C for 24 hours in an air atmosphere in a muffle furnace to obtain the SAPO-5 material. The grain size of SAPO-5 is 4-10 microns, and the product yield is 99%. After diethylamine was recovered at 250°C, infrared experiments showed that the diethylamine template was almost contained in the pores of SAPO-5.

Embodiment 2

[0020] Al(OH) in molar ratio 3 : 0.5H 3 PO 4 : 0.1SiO2 2 :0.5R:10H 2 O mix aluminum isopropoxide, phosphoric acid, ethyl orthosilicate and 8:1 diethylamine and triethylamine raw materials. Mix and stir evenly, seal and heat in an oven at 165°C for 48 hours. After suction filtration, drying, and calcination at 900°C for 12 hours in an air atmosphere in a muffle furnace, the SAPO-5 material can be obtained. The obtained SAPO-5 grain size is 0.5-5 microns, and the product yield is 65%. After recovering part of diethylamine at 250°C, infrared experiments showed that the pores of SAPO-5 still contained a very small amount of template agent.

Embodiment 3

[0022] Al(OH) in molar ratio 3 : 1H 3 PO 4 : 0.5SiO2 2 :1R:100H 2 O Mix aluminum isopropoxide, phosphoric acid, silica sol, and a 16:1 ratio of diethylamine to tetraethylammonium hydroxide starting material. After sealing, heat in an oven at 300° C. for 2 hours. After suction filtration, drying, and calcination at 400°C for 12 hours in an oxygen atmosphere in a muffle furnace, the SAPO-5 material can be obtained. The grain size of SAPO-5 is 1-3 microns, and the product yield is 98%. The XRD and SEM of the obtained SAPO-5 are attached figure 1 and figure 2 shown. After recovering part of diethylamine at 250°C, infrared experiments showed that the pores of SAPO-5 still contained a very small amount of template agent.

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Abstract

The invention provides a method for synthesizing SAPO-5 by using diethylamine as template and recovering the template of the SAPO-5. The structural formula of the SAPO-5 is represented by aR x (SixAlyPz)O2, wherein, the x, y and z are a molar fraction of Si, a molar fraction of Al and a molar fraction of P respectively, and meet a relation of x+y+z =1; the R is the template; and the a is the mole number of the template, and a is between 0.5 and 2.5. The invention is characterized in that: the template adopts the diethylamine or mixture of nitrogenous organic substances mainly containing the diethylamine ; and the method comprises the following steps of: weighing the template, a silicon source, an aluminium source, a phosphorus source and water according to the mole amount of H2O on a molecular sieve with meshes between 0 and 500; preparing gel through sufficiently mixing and stirring the materials; crystallizing the gel at a temperature of between 160 and 350 DEG C with a reaction time not shorter than 0.1 hour; filtering, washing and drying after complete crystallization, and performing drying under a temperature of between 25 and 120 DEG C; heating up the gel to a temperature not higher than 250 DEG C after molecular sieve synthesis, and condensing and volatilizing diethylamine template which can be reused. The method has the advantages of simple preparation method, low cost and high product yield.

Description

technical field [0001] The present invention relates to a novel environment-friendly synthesis method of SAPO-5 molecular sieve, specifically providing a method for synthesizing phosphorus-aluminosilicate SAPO-5 molecular sieve with diethylamine as the main template agent at relatively high temperature and its template agent recovery method . Background technique [0002] Phosphosilicate aluminum SAPO-5 molecular sieve is composed of phosphorus, silicon, aluminum and oxygen. SAPO-5 molecular sieves have 12-membered ring straight channels, moderate acidity and high thermal stability, and are valued for their unique properties in catalysis, adsorption and assembly. [0003] The synthesis of SAPO-5 molecular sieve requires the use of organic templates, including triethylamine, tripropylamine, isotripropylamine, etc. The molecular size of these templates has a good match with the SAPO-5 pore size of 0.73nm, so it is beneficial to the synthesis of SAPO-5 as a template. But at ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/54C01B37/08
Inventor 王利军
Owner SHANGHAI SECOND POLYTECHNIC UNIVERSITY
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