Synthesis method of low-silicon nano SAPO-34 molecular sieve

A technology of SAPO-34, synthesis method, applied in the field of molecular sieve, can solve the problem of high crystallization temperature

Active Publication Date: 2013-06-05
SHANGHAI LVQIANG NEW MATERIALS CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This patent shortens the crystallization time, but the crystallization temperature is higher

Method used

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  • Synthesis method of low-silicon nano SAPO-34 molecular sieve
  • Synthesis method of low-silicon nano SAPO-34 molecular sieve
  • Synthesis method of low-silicon nano SAPO-34 molecular sieve

Examples

Experimental program
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Effect test

Embodiment 1

[0037] Silica sol, pseudo-boehmite, tetraethylammonium hydroxide, and deionized water are n (Al 2 o 3 ): n(P 2 o 5 ):n(SiO 2 ):n(TEAOH):n(H 2 (0)=1:2:0.4:3.5:140 mixed, stirred at 30°C for 2h, and then slowly added phosphoric acid solution dropwise. After continuing to stir for 2 hours, the obtained solution was put into a stainless steel autoclave lined with polytetrafluoroethylene, and then crystallized in a conventional reactor at 130°C for 3 hours to obtain primary crystals containing aging liquid, which were poured into primary crystals Add a certain volume of distilled water (the ratio of the volume of the aging solution is 1:2) and stir evenly, place it in an autoclave, crystallize in a microwave reactor at 160°C for 80min, wash, dry at 120°C, and dry at 550°C Calcination to obtain SAPO-34 molecular sieve (sample number S-1). Its XRD pattern is shown in figure 1 , SEM photo see figure 2 , It can be seen from the photo that the obtained SAPO-34 molecular sieve i...

Embodiment 2

[0041]Silica sol, pseudo-boehmite, tetraethylammonium hydroxide, and deionized water are n (Al 2 o 3 ): n(P 2 o 5 ):n(SiO 2 ):n(TEAOH):n(H 2 (0)=1:2:0.4:3.5:140 mixed, stirred at 30°C for 2h, and then slowly added phosphoric acid solution dropwise. After continuing to stir for 2 hours, the obtained solution was put into a stainless steel autoclave lined with polytetrafluoroethylene, and then crystallized in a conventional reactor at 130°C for 3 hours to obtain primary crystals containing aging liquid, which were poured into primary crystals Add a certain amount of sodium lauryl sulfate solution S (S: Al 2 o 3 =0.01:1) and stirred evenly, placed in an autoclave, crystallized in a microwave reactor at 160°C for 80min, washed, dried at 120°C, and calcined at 550°C to obtain SAPO-34 molecular sieve (sample number S- 3). Its XRD pattern is shown in figure 1 , SEM photo see image 3 , It can be seen from the photo that the obtained SAPO-34 molecular sieve is in the form of...

Embodiment 3

[0043] Silica sol, pseudo-boehmite, tetraethylammonium hydroxide, and deionized water are n (Al 2 o 3 ): n(P 2 o 5 ):n(SiO 2 ):n(TEAOH):n(H 2 (0)=1:2:0.4:3.5:140 mixed, stirred at 30°C for 2h, and then slowly added phosphoric acid solution dropwise. After continuing to stir for 2 hours, the obtained solution was put into a stainless steel autoclave lined with polytetrafluoroethylene, and then crystallized in a conventional reactor at 130°C for 3 hours to obtain primary crystals containing aging liquid, which were poured into primary crystals Add a certain amount of sodium lauryl sulfate solution S (S: Al 2 o 3 = 1:1) and stirred evenly, placed in an autoclave, crystallized in a microwave reactor at 160°C for 80min, washed, dried at 120°C, and calcined at 550°C to obtain SAPO-34 molecular sieve (sample number S- 4). Its XRD pattern is shown in figure 1 , confirmed to be SAPO-34 molecular sieve and flake shape, about 50×300nm.

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Abstract

The invention relates to a synthesis method of a low-silicon nano SAPO-34 molecular sieve, which comprises the following steps: sequentially mixing a silicon source, an aluminum source, a template agent R, deionized water and a phosphorus source to obtain a gel mixture; placing the gel mixture in a stainless steel high-pressure reaction kettle of which the liner is made of polytetrafluoroethylene, sealing, putting into a drying oven, and performing primary traditional hydrothermal crystallization; adding a dispersant agent S into the primary traditional hydrothermal crystallization solution, stirring for 0.5-4 hours, transferring into the reaction kettle of which the liner is made of polytetrafluoroethylene, sealing, putting into a microwave reactor, and performing secondary microwave hydrothermal crystallization; and washing, drying, and roasting to obtain the nano SAPO-34 molecular sieve. Compared with the prior art, the invention greatly lowers the crystallization temperature and shortens the time of the whole synthesis process. The nano molecular sieve can be widely used for conversion, separation and absorption of hydrocarbons, and especially has the advantages of high conversion rate, high low-carbon alkene selectivity, low carbon deposition rate, long reaction life and the like in the process of preparing alkene from methanol.

Description

technical field [0001] The invention belongs to the technical field of molecular sieves, and in particular relates to a preparation method of low-silicon nanometer SAPO-34 molecular sieves. Background technique [0002] In 1984, United Carbide Corporation (UCC) developed a series of silicoaluminophosphate molecular sieves (SAPO-n, n represents the structural model). One of the most eye-catching is SAPO-34 molecular sieve. The MTO catalytic performance of this molecular sieve is excellent, the conversion rate of methanol is 100% or nearly 100%, the selectivity of ethylene and propylene is about 60%, and there is almost no C 5 + products of the above. In particular, the catalyst with SAPO-34 as the active component developed by UOP has a significantly better ethylene selectivity than ZSM-5, making a breakthrough in the MTO process. [0003] The SAPO-34 molecular sieve synthesized by the traditional hydrothermal method is prone to carbon deposition, which leads to a short o...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/54B82Y30/00
Inventor 胡杰徐华胜王鹏飞
Owner SHANGHAI LVQIANG NEW MATERIALS CO LTD
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