High-temperature hydrothermal synthesis method of phosphorus Al-Si SAPO-34

A SAPO-34, high-temperature hydrothermal technology, applied in the direction of molecular sieve and alkali exchange phosphate, molecular sieve characteristic silicoaluminophosphate, etc., can solve the problems of reduced catalytic effect, large particle size, etc., and achieve effective control of crystal grains and crystallization The effect of shortening the time and making the crystal grains smaller

Inactive Publication Date: 2009-09-16
SHANGHAI SECOND POLYTECHNIC UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In the catalytic reaction, the particle size of SAPO-34 is too large, which will greatly reduce the catalytic effect

Method used

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  • High-temperature hydrothermal synthesis method of phosphorus Al-Si SAPO-34
  • High-temperature hydrothermal synthesis method of phosphorus Al-Si SAPO-34

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] 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 255°C for 12 hours. After suction filtration, drying, and calcination at 600°C for 24 hours in an air atmosphere in a muffle furnace, the SAPO-34 material can be obtained. The grain size of SAPO-34 is 1-2 microns, and the product yield is 95%.

Embodiment 2

[0022] Al(OH) in molar ratio 3 : 0.3H 3 PO 4 : 0.1 SiO 2 :0.5R:10H 2 O mix aluminum isopropoxide, phosphoric acid, methyl orthosilicate and 2:1 diethylamine and triethylamine raw materials. Mix and stir evenly, seal and heat in an oven at 300°C for 5 hours. After suction filtration, drying, and calcination at 900°C for 12 hours in an air atmosphere in a muffle furnace, the SAPO-34 material can be obtained. The obtained SAPO-34 grain size is 0.5-1.5 microns, and the product yield is 99%.

Embodiment 3

[0024] 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 4:1 diethylamine and tetraethylammonium hydroxide raw materials. After sealing, heat in an oven at 350°C for 0.2 hours. After suction filtration, drying, and calcination at 400°C for 12 hours in an oxygen atmosphere in a muffle furnace, the SAPO-34 material can be obtained. The product yield was 99%. The XRD and SEM of the obtained SAPO-34 are attached figure 1 and figure 2 shown. from figure 1 It can be seen that the obtained crystals are the pure phase of SAPO-34 without any miscellaneous crystals. from figure 2 It can be seen that the obtained crystals have a size of 2-3 microns and are tetragonal block crystals, which is a typical crystal morphology of SAPO-34.

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Abstract

The invention relates to a high-temperature hydrothermal synthesis method of phosphorus Al-Si SAPO-34, the structural formula of which can be expressed by aR (SixAly Pz) O2, wherein x, y and z are respectively the mole fractions of Si, Al and P, and the template agent R is a nitrogen-containing organic compound of diethylamine and triethylamine or taking the diethylamine and the triethylamine as main material; the synthesis process is as follows: according to the molar volume of a molecular sieve: 0-500H2O, the template agent, silicon source, aluminum source, phosphorus source and water are respectively weighed and taken out; the materials are mixed and fully stirred so as to prepare gel; the gel is crystallized at the temperature of 250-350 DEG C for 0.1 to 12 hours; the gel is filtered after being crystallized completely, and then washed by water and dried while the drying can be implemented at the temperature of 25-120 DEG C. The method of the invention has short crystallization time, high product yield, small synthesis grain, and is simple and suitable for large-scale production and application.

Description

technical field [0001] The invention relates to an aluminum-phosphorus-silicon SAPO-34 and a synthesis method thereof, in particular to a rapid and efficient synthesis method of the aluminum-phosphorus-silicon SAPO-34 at a temperature higher than conventional hydrothermal crystallization. Background technique [0002] Synthetic phosphosilicate aluminum SAPO-34 molecular sieve is a molecular sieve composed of phosphorus, silicon, aluminum and oxygen with a chabazite-like structure. SAPO-34 molecular sieve has an elliptical cage structure composed of 8-membered ring openings and moderate acidity, and has attracted attention for its excellent catalytic performance in methanol-to-olefins (MTO) technology. [0003] European patent EP0103117 discloses a hydrothermal synthesis method commonly used for SAPO-34 molecular sieves. One of its technical characteristics is that tetraethylammonium hydroxide, isopropylamine or tetraethylammonium hydroxide and di-n-propylamine are used in th...

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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