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Fast synthetic method for phosphorus-silicon-aluminum molecular sieve

A technology of SAPO-34 and synthesis method, applied in the field of molecular sieves, can solve the problems of long crystallization time, large energy consumption, and use of template agents, etc., and achieve the effect of improving selectivity

Active Publication Date: 2008-02-13
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, in these patents, more templates are used and the crystallization time is longer, and the energy consumption is larger

Method used

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  • Fast synthetic method for phosphorus-silicon-aluminum molecular sieve
  • Fast synthetic method for phosphorus-silicon-aluminum molecular sieve
  • Fast synthetic method for phosphorus-silicon-aluminum molecular sieve

Examples

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preparation example Construction

[0034] A kind of rapid synthesis method of phosphorus silicon aluminum SAPO-34 molecular sieve of the present invention, concrete steps are:

[0035] a) template agent, phosphorus source, aluminum source, silicon source and water are formulated into the initial gel mixture of SAPO-34 molecular sieve in proportion;

[0036] b) adding a metered organic amine accelerator to the initial gel mixture obtained in step a), and stirring to obtain a uniform initial gel mixture;

[0037] c) Put the homogeneous initial gel mixture obtained in step b) into a polytetrafluoroethylene-lined stainless steel synthesis kettle, seal it, and perform aging at room temperature to 180°C for 1 to 12 hours.

[0038] d) Further heat the aging mixture obtained in step c) to the crystallization temperature in a closed manner, and carry out constant temperature crystallization under autogenous pressure. The crystallization temperature is 180-250° C., and the crystallization time is 0.5-12 hours, preferably...

Embodiment 1

[0043] Embodiment 1 (SAPO-34 molecular sieve synthesis)

[0044] In the initial gel ratio 3.0TEA:0.6SiO 2 :P 2 o 5 : Al 2 o 3 :50H 2 O (TEA is a triethylamine template agent) Mix the measured raw materials in a certain order, stir well to form a gel, age at 80°C for 5 hours, then put it into a stainless steel autoclave lined with polytetrafluoroethylene, and heat it in a closed To 200°C, under autogenous pressure, constant temperature crystallization for 5 hours. The solid product was separated by centrifugation, washed with deionized water until neutral, and dried in air at 120°C. The XRD analysis is shown in Table 1. The synthesized product is the original powder of SAPO-34 molecular sieve.

[0045] Table 1 Example 1 synthetic sample X-ray diffraction analysis result

[0046] 2θ

[0047] 20.52

Embodiment 2

[0048] Embodiment 2 (SAPO-34 molecular sieve synthesis)

[0049] At the initial gel ratio 2.5TEA:0.6SiO 2 :P 2 o 5 : Al 2 o 3 :50H 2 O: 0.1CTAB (TEA is a triethylamine template, CTAB is hexadecyltrimethylammonium bromide) Mix the measured raw materials in a certain order, fully stir to form a gel, age at 100°C for 8 hours, and then Put it into a stainless steel autoclave lined with polytetrafluoroethylene, seal it and heat it to 180°C, and crystallize at constant temperature for 2 hours under autogenous pressure. The solid product was separated by centrifugation, washed with deionized water until neutral, and dried in air at 120°C. The XRD analysis is shown in Table 2. The synthesized product is the original powder of SAPO-34 molecular sieve.

[0050] Table 2 Example 2 synthetic sample X-ray diffraction analysis results

[0051] 2θ

[0052] 12.76

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Abstract

Provided is a method for rapidly synthesizing a silicoaluminophosphate SAPO-34 molecular sieve, wherein triethylamine and / or diethylamine are / is used as templating agents, an organic amine accelerator is added to the initial gel for synthesis at the same time, and the gel mixture is optionally subjected to aging treatment. The method could give SAPO-34 molecular sieves with high crystallization degree in a relative short crystallization period. The SAPO-34 molecular sieve catalysts synthesized by the method can be used in the MTO or DTO reaction, the selectivity of C2~C3 olefins in the product could be up to about 90%.

Description

technical field [0001] The invention discloses a rapid synthesis method of phosphorus-silicate-aluminum SAPO-34 molecular sieve, relates to the technical field of molecular sieves, and can synthesize SAPO-34 molecular sieve with high crystallinity within a relatively short crystallization time. Background technique [0002] Phosphosilicate SAPO-34 molecular sieve is a molecular sieve with chabazite-like structure composed of phosphorus, silicon, aluminum and oxygen. Its structural unit consists of PO 2 + , SiO 2 and AlO 2 - Tetrahedral structure, anhydrous chemical composition can be expressed as: mM (Si x ·Al y ·P z )O 2 , in the above formula, M is the template agent present in the micropores of the molecular sieve crystal, m is the mole number of M, and x, y, z are the mole fractions of Si, Al, and P respectively, and satisfy x+y+z=1. European patent EP0103117 discloses a hydrothermal synthesis method of SAPO-34 molecular sieve, which uses tetraethylammonium hydr...

Claims

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Application Information

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IPC IPC(8): C01B39/54C01B37/08B01J29/85C07C1/20
CPCC01B39/54C07C2529/85C07C1/20C01B37/08C10G2400/20B01J29/85C10G3/49Y02P20/52Y02P30/20Y02P30/40C07C11/02
Inventor 刘中民许磊田鹏杨越杨立新何长青吕志辉孟霜鹤王公慰孙新德杨虹熠王贤高袁翠峪李铭芝魏迎旭齐越朱书魁张今令陆晓王华谢鹏李冰
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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