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Synthetic method of phosphoric acid silicon-aluminium molecular sieve

A technology of silicoaluminophosphate and synthesis method, applied in the direction of molecular sieve characteristic silicoaluminophosphate, molecular sieve and alkali-exchanged phosphate, etc., can solve the problems of expensive raw materials, high synthesis cost, and the addition amount cannot be less than a specific value, etc. The cost is low, the method is simple, and the effect of saving chemical raw materials

Inactive Publication Date: 2014-09-24
北京禾木科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Raw materials are expensive, and the amount added cannot be less than a specific value, and the synthesis cost is high

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] A method for silicoaluminophosphate (SAPO-34) molecular sieve, comprising the following steps:

[0014] The fly ash (its SiO 2 The content is 61.7%, and its Al 2 o 3 The content is 16.5%, the loss on ignition is 1.2%), after drying at 105°C for 2h, mix it with KF, the mixing mass ratio is fly ash:KF=10:1, and roast in a muffle furnace at 700°C for 3h. The activated fly ash, pseudo-boehmite, phosphoric acid, morpholine and water are sequentially mixed to form a working solution. Its molar composition is SiO 2 :Al 2 o 3 :P 2 o 5 :H 2 0: template agent=1.0:1.0:0.5:100:2.5, adjust pH=8.5. After stirring for 30 minutes, pour it into the reaction kettle, gradually raise the temperature to 230°C, and keep it for 15 hours. The slurry after the crystallization reaction was filtered to separate the solid product, washed, and dried at 105° C. for 6 hours to obtain the SAPO-34 molecular sieve product.

Embodiment 2

[0016] A method for silicoaluminophosphate (SAPO-18) molecular sieve, comprising the following steps:

[0017] With reference to the steps of Example 1, fly ash is activated. The activated fly ash, tetraethyl orthosilicate, phosphoric acid, N,N-diisopropylethylamine and water are mixed in turn to form a working solution. Its molar composition is SiO 2 :Al 2 o 3 :P 2 o 5 :H 2 0: Templating agent=1.5:2.5:2.2:125:4.0, adjust PH=8.5. After stirring for 30 minutes, pour it into the reactor, first keep it at 30°C for 24h, then gradually raise the temperature to 180°C, and keep it for 40h. The slurry after the crystallization reaction was filtered to separate the solid product, washed, and dried at 105°C for 6 hours to obtain the SAPO-18 molecular sieve product.

Embodiment 3

[0019] A method for silicoaluminophosphate (SAPO-5) molecular sieve, comprising the following steps:

[0020] The fly ash (its SiO 2 The content is 33.9%, and its Al 2 o 3 The content is 36.4%, the loss on ignition is 23.5%), after drying at 105°C for 2h, mix it with KF, the mixing mass ratio is fly ash:KF=10:1, and roast in a muffle furnace at 900°C for 1h. The activated fly ash, aluminum isopropoxide, phosphorous acid, triethylamine and water are mixed successively to form a working solution. Its molar composition is SiO 2 :Al 2 o 3 :P 2 o 5 :H 2 0: Templating agent=1.0:1.0:1.5:100:2.0, adjust PH=6.0. After stirring for 30 minutes, pour it into the reaction kettle, gradually raise the temperature to 180°C, and keep it for 72 hours. The slurry after the crystallization reaction was filtered to separate the solid product, washed, and dried at 105° C. for 6 hours to obtain the SAPO-5 molecular sieve product.

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PUM

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Abstract

The invention discloses a synthesis method of silicoaluminophosphate molecular sieve, which comprises: mixing fly ash and KF for roasting, the mixing mass ratio is fly ash:KF=10:1, the activation roasting temperature is 700-900°C, The roasting time is 1-3h; the activated fly ash is mixed with auxiliary silicon source or auxiliary aluminum source, phosphorus source, templating agent and water to make a slurry, and the molar ratio of the slurry is SiO2:Al2O3:P2O5:H20: Templating agent=(0.5-1.5):(1.0-4.0):(0.5-10):(30-125):(1.5-20), pH=6.0-8.5, after stirring for 30 minutes to mix evenly, pour into the closed synthetic Keep in the reactor at 180-230°C for 15-72h; or first keep at 30-60°C for 10-24h, then raise the temperature to 180-230°C and keep for 10-40h; filter the slurry after the crystallization reaction to separate the solid product , washed, and dried at 105°C for 6 hours to obtain a silicoaluminophosphate molecular sieve. The method of the invention is simple and low in cost, and can realize emission reduction.

Description

technical field [0001] The invention belongs to the technical field of chemical industry, and in particular relates to a method for synthesizing silicoaluminophosphate molecular sieves. Background technique [0002] In 1984, United Carbide Corporation (UCC) in AlPO 4 Si elements were introduced into the series of molecular sieves, and silicoaluminophosphate molecular sieves (SAPO-n) were developed. This kind of microporous catalyst has suitable proton acidity, large specific surface area, good adsorption performance and hydrothermal stability, etc., and has been widely used in petrochemical and petroleum processing, especially in the isopropane of normal alkanes. It has high catalytic activity and selectivity in many reactions such as structuralization, dehydrocyclization of paraffins and methanol conversion. The methods for preparing SAPO molecular sieves include hydrothermal synthesis, gas phase crystallization, liquid phase crystallization, microwave hydrothermal method...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B37/08C01B39/54
Inventor 刘飞曹建新李婷林倩许芳王晓丹
Owner 北京禾木科技有限公司
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