SSZ -13 molecular sieve preparing method

A molecular sieve and crystal growth technology, applied in the field of molecular sieves, can solve the problems of uneven particle size, affecting the catalytic performance of molecular sieves, poor crystal form of SSZ-13 molecular sieves, etc., to simplify the production process, avoid the ammonium exchange process, and facilitate industrial operation Effect

Inactive Publication Date: 2017-01-11
SHANDONG QILU HUAXIN HIGH TECH
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Problems solved by technology

[0003] At present, the main method to reduce the synthesis cost of SSZ-13 molecular sieve is to reduce the use of N,N,N-trimethyladamantyl ammonium hydroxide. The common method is to find a suitable template to replace SDA, such as organic template tetraethyl Ammonium h

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  • SSZ -13 molecular sieve preparing method
  • SSZ -13 molecular sieve preparing method
  • SSZ -13 molecular sieve preparing method

Examples

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Example Embodiment

[0032] A preparation method of SSZ-13 molecular sieve, comprising the following steps:

[0033] ①Mix the N,N,N-trimethyladamantane ammonium hydroxide and the crystal growth agent uniformly, add them into the autoclave, then add silicon source, aluminum source and water in sequence, and stir to obtain the initial gel; N,N,N-trimethyladamantane ammonium hydroxide in the initial gel: crystal growth agent: SiO 2 : Al 2 O 3 :H 2 The molar ratio of O is 0.06-0.25:0.00085-0.025:1:0.017-0.063:20-40; the crystal growth agent is piperazine;

[0034] 2. Crystallize the initial gel obtained in step 1 at 155-175° C. for 17-72 hours to obtain a crystallized product;

[0035] 3. centrifugation of the crystallization product obtained in step 2. to obtain filter cake and filtrate, the obtained filter cake is washed with deionized water to pH 7 to 8, and then dried at 100 to 120 ° C for 10 to 13 hours to obtain SSZ- 13 molecular sieves.

[0036] Preferably, the silicon source is silica so...

Example Embodiment

[0048] Example 1

[0049] ①Mix 31.3kg of N,N,N-trimethyladamantane ammonium hydroxide (SDA 25wt%) and 0.01kg of crystal growth agent anhydrous piperazine (100wt%), add them into the autoclave, and then add them in sequence 13.3kg aluminum sulfate solution (Al 2 O 3 7.16wt%), 35.6kg silica sol (SiO 2 25wt%) and 71.1kg of water, and the initial gel was obtained after stirring; ② the initial gel obtained in step ① was crystallized at 155 ° C for 72 hours to obtain a crystallized product;

[0050] 3. centrifuge the crystallization product obtained in step 2. to obtain a filter cake and a filtrate, wash the obtained filter cake with deionized water to pH 7, and then dry at 100 ° C for 13 hours to obtain SSZ-13 molecular sieves, wherein the sodium content with Na 2 0%, the numerical range is 0.01%, the obtained SSZ-13 molecular sieve is pure phase SSZ-13 molecular sieve by X-ray diffraction (XRD) test, and the X-ray diffraction pattern of the sample is attached figure 1 The sca...

Example Embodiment

[0051] Example 2

[0052] ①Mix 12.1kg of N,N,N-trimethyladamantane ammonium hydroxide (SDA 25wt%) and 0.03kg of crystal growth agent anhydrous piperazine (100wt%), add them into the autoclave, and then add them to it in turn 0.56kg pseudo-boehmite (Al 2 O 3 66.1wt%), 19.2kg ethyl orthosilicate (SiO 2 25wt%) and 120.2kg of water, the initial gel was obtained after stirring;

[0053] ② Crystallize the initial gel obtained in step ① at 175°C for 17 hours to obtain a crystallized product;

[0054] 3. centrifuge the crystallization product obtained in step 2. to obtain filter cake and filtrate, wash the obtained filter cake with deionized water to pH to 8, and then dry at 130 ° C for 10 hours to obtain SSZ-13 molecular sieve, wherein the sodium content with Na 2 0%, the numerical range is 0.02%, the obtained SSZ-13 molecular sieve is pure phase SSZ-13 molecular sieve by X-ray diffraction (XRD) test, and the X-ray diffraction pattern of the sample is attached figure 2 The sca...

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Abstract

The invention discloses a SSZ -13 molecular sieve preparing method comprising the steps of (1) evenly mixing and putting N,N,N- trimethyl adamantane ammonium hydroxide and crystal growth agent into high-pressure reaction kettle, then adding silicon source, aluminium source and water successively into it and obtaining initial gel after mixing; (2) crystallizing the initial gel obtained in step (1) under 155-175oC for 17-72 hours and obtaining crystallized product; (3) centrifugalizing the crystallized product obtained in step (2) to obtain filter cake and filtrate, washing the obtained filter cake by deionized water to pH 7-8, then drying it for 10-13 hours under 100-120oC to obtain the SSZ -13 molecular sieve; the SSZ -13 molecular sieve preparing method in the invention may realize the free modulation for partical size of SSZ -13 molecular sieve from 0. 3-17Mum through adding crystal growth agent; the addition of crystal growth agent in the invention makes more even dispersion of molecular sieve crystal.

Description

technical field [0001] The invention relates to the technical field of molecular sieves, in particular to a preparation method of SSZ-13 molecular sieves. Background technique [0002] SSZ-13 molecular sieve has an ellipsoidal cage with an eight-membered ring structure and a three-dimensional intersecting channel structure, and its specific surface area can reach up to 700m 2 / g, because of its exchangeable cations and surface proton acid centers, it is often used as an adsorbent or catalyst, but the template commonly used in the synthesis of SSZ-13 molecular sieves is N,N,N-trimethyladamantane hydrogen Ammonium oxide SDA is expensive, which seriously restricts its industrialization process. The synthesis cost of SSZ-13 molecular sieve is the main factor restricting the industrial production of SSZ-13 molecular sieve. For molecular sieves, particle size is a very important quality index. Usually, small particle size molecular sieves have relatively high reactivity due to th...

Claims

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Application Information

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IPC IPC(8): C01B39/04
CPCC01B39/04C01P2002/72C01P2004/03C01P2004/61C01P2004/62
Inventor 梁光华陈文勇明曰信彭立周泳冰
Owner SHANDONG QILU HUAXIN HIGH TECH
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