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Synthesis method of SSZ-13 molecular sieve

A synthesis method and molecular sieve technology, applied in the direction of separation methods, molecular sieve catalysts, including molecular sieve catalysts, etc., can solve problems such as poor catalytic activity, particle agglomeration, poor dispersion, etc., to reduce tail gas treatment costs, increase yield, The effect of good economic benefits

Inactive Publication Date: 2019-03-29
SHANDONG SINOCERA FUNCTIONAL MATERIAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] However, according to the above method, non-skeletal aluminum is prone to appear during preparation, and the particles are prone to agglomeration, poor dispersion, and poor catalytic activity.

Method used

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  • Synthesis method of SSZ-13 molecular sieve
  • Synthesis method of SSZ-13 molecular sieve
  • Synthesis method of SSZ-13 molecular sieve

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0058] The present embodiment provides a kind of synthetic method of SSZ-13 molecular sieve, comprises the following steps:

[0059] 1) Pretreatment of seed crystals: pretreat SSZ-13 molecular sieve seeds, specifically: take the finished SSZ-13 molecular sieve seeds, make slurry according to the material-to-water ratio of 1:3, and pass through the mechanical Pulverize and ultrasonically disperse to obtain seed crystals with a particle size of D50=0.236;

[0060] 2) Silicon source pretreatment: the solid silicon source is turned into a powder that can pass through 300 mesh or have a bulk density less than or equal to 0.30 g / ml after passing through the gas powder;

[0061] 3) Add 414 grams of 9.5 mol / L ammonia solution to 2 L of aluminum chloride solution with a concentration of 0.26 mol / L, add pure water to dilute to 3 L, and press filter to obtain a primary precursor of aluminum hydroxide; body, add pure water to make a slurry and dilute to 3L, press filter to obtain the sec...

Embodiment 2

[0068] The present embodiment provides a kind of synthetic method of SSZ-13 molecular sieve, comprises the following steps:

[0069] 1) seed crystal pretreatment: with embodiment 1;

[0070] 2) silicon source pretreatment: with embodiment 1;

[0071] 3) Add 765 grams of 9.5 mol / L ammonia solution to 2 L of aluminum chloride solution with a concentration of 0.48 mol / L, add pure water to dilute to 3 L, and press filter to obtain a primary precursor of aluminum hydroxide; body, add pure water to make a slurry and dilute to 3L, press filter to obtain the secondary precursor of aluminum hydroxide, and obtain the tertiary precursor in the same way.

[0072] 4) Add the aluminum hydroxide precursor to 3L of pure water for beating, perform ultrasonic dispersion treatment, control the ultrasonic frequency to 30KHz, and ultrasonic for 12 minutes; add 134 grams of amantadine hydrochloride as a template agent, and continue ultrasonic for 10 minutes; obtain Contains aluminum hydroxide col...

Embodiment 3

[0078] The present embodiment provides a kind of synthetic method of SSZ-13 molecular sieve, comprises the following steps:

[0079] 1) seed crystal pretreatment: with embodiment 1;

[0080] 2) silicon source pretreatment: with embodiment 1;

[0081] 3) Add 1275 grams of 9.5 mol / L ammonia solution in 2 L of aluminum chloride solution with a concentration of 0.80 mol / L, add pure water to dilute to 3.5 L, and press filter to obtain a primary precursor of aluminum hydroxide; For the precursor, add pure water to beat and dilute to 3.5L, press filter to obtain the secondary precursor of aluminum hydroxide, and similarly prepare the tertiary precursor.

[0082] 4) Add the aluminum hydroxide precursor to 3L of pure water for beating, perform ultrasonic dispersion treatment, control the ultrasonic frequency to 20KHz, and ultrasonic for 20 minutes; add 89 grams of amantadine hydrochloride as a template, and continue ultrasonic for 10 minutes; obtain Contains aluminum hydroxide colloi...

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Abstract

The invention relates to a synthesis method of a SSZ-13 molecular sieve. The synthesis method includes: 1) adding an inorganic alkali solution to an aluminum source solution to prepare an Al(OH)3 precipitate, and press-filtering and washing the Al(OH)3 precipitate to prepare an Al(OH)3 precursor; 2) adding the Al(OH)3 precursor into pure water to make slurry, ultrasonically dispersing the slurry,adding a template agent, amantadine hydrochloride, and continuously performing ultrasonic dispersion to form an Al(OH)3 colloid, concentration being 0.1-0.7 mol / L; 3) under intensive stirring, addingan inorganic alkali solution, a template agent N,N,N-trimethyl-1-adamantyl amine hydroxide, a SSZ-13 molecular sieve seed crystal, and a silicon source, performing intensive stirring to uniform mixing, thereby preparing sol, solid content being 20-40%; 4) crystallizing the sol at 150-200 DEG C for 20-60 h; 5) washing, drying and roasting the product. The synthesis method achieves controllability on particle size and appearance of the SSZ-13 molecular sieve.

Description

technical field [0001] The invention relates to the field of molecular sieve synthesis, in particular to a method for synthesizing SSZ-13 molecular sieves. Background technique [0002] SSZ-13 molecular sieve is a molecular sieve with a CHA topology. On October 1, 1985, US Patent No. 4544538 disclosed the synthesis method of molecular sieve SSZ-13 for the first time. In N,N,N-trimethyl-1-adamantane SSZ-13 molecular sieves can be synthesized under the condition of ammonium hydroxide (TMAA+) organic cation as structure directing agent. However, due to the high cost of the product, the application of SSZ-13 in production is limited. Afterwards, how to reduce the cost has been done a lot of exploration in the replacement of templates. For example, in 2013, BASF patent CN 107673366 A used at least two mixed templates. In 2014, the catalyst patent CN105645426 A used N,N,N- Trimethyl-1.3.5.7-tetraazatricyclo﹝3.3.1.1﹞decane-2-ammonium hydroxide was used as a templating agent. [...

Claims

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Application Information

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IPC IPC(8): C01B39/04B01J29/70B01J29/76C07C1/20C07C11/02B01D53/86B01D53/56
CPCB01D53/8628C01B39/04C07C1/20B01J29/70B01J29/76C01P2004/62C01P2004/03C07C2529/70C07C2529/76C07C11/02
Inventor 宋锡滨董成利焦英训潘光军艾辽东
Owner SHANDONG SINOCERA FUNCTIONAL MATERIAL CO LTD
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