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Method for preparing H-SSZ-13 molecular sieve

A molecular sieve and template technology, which is applied in the field of preparation of H-SSZ-13 molecular sieve, can solve the problem of no substantial progress in the cost of the template, and achieve the effects of shortening the crystallization time, improving the utilization rate, and reducing the use of

Active Publication Date: 2018-05-22
SHANDONG QILU HUAXIN HIGH TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

These disclosed technologies have no substantial progress in reducing the cost of templates, and the obtained SSZ-13 molecular sieves also need to be ammonium exchanged

Method used

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  • Method for preparing H-SSZ-13 molecular sieve
  • Method for preparing H-SSZ-13 molecular sieve

Examples

Experimental program
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Effect test

Embodiment 1

[0031] The preparation method of H-SSZ-13 molecular sieve of the present invention is characterized in that comprising the following steps:

[0032] Add silica sol, N,N,N-trimethyladamantyl ammonium hydroxide and pseudo-boehmite into deionized water in sequence. The proportion of each component is SiO 2 :Al 2 o 3 :R:H 2 O=1:0.2:0.15:15. After mixing and stirring evenly, transfer to the reactor, and crystallize at 100° C. for 12 hours to obtain the directing agent slurry (G-1).

[0033] Add ethanol, triethylamine, N,N,N-trimethyladamantyl ammonium hydroxide, silica sol, and pseudoboehmite in sequence in deionized water, and stir well to form a uniform gel. The molar ratio of each component substance in the gel is SiO 2 :Al 2 o 3 :R:R1:C:H 2 O=1:0.02:0.03:1.5:0.05:14. A 4% directing agent solution (G-1) on a dry basis of the slurry was then added. After fully mixed, put it into the reaction kettle, and crystallize at 160°C for 72 hours. After the crystallization, the ...

Embodiment 2

[0035] The preparation method of H-SSZ-13 molecular sieve of the present invention is characterized in that comprising the following steps:

[0036] Add silica gel, N,N,N-trimethyladamantyl ammonium hydroxide, and pseudo-boehmite to deionized water in sequence. The proportion of each component is SiO 2 :Al 2 o 3 :R:H 2 O=1:0.25:0.18:16. After mixing and stirring evenly, it was transferred to a reaction kettle, and crystallized at 110° C. for 12 hours to obtain a directing agent slurry (G-2).

[0037] Add acetamide, diethylamine, N,N,N-trimethyladamantyl ammonium hydroxide, silica gel, and pseudoboehmite in sequence in deionized water, and stir well to form a uniform gel. The molar ratio of each component substance in the gel is SiO 2 :Al 2 o 3 :R:R1:C:H 2 O=1:0.0333:0.04:1.4:0.04:14. A 6% directing agent solution (G-2) on a dry basis of the slurry was then added. Put it into the reaction kettle after mixing well, and crystallize at 170°C for 60 hours. After the crys...

Embodiment 3

[0039] The preparation method of H-SSZ-13 molecular sieve of the present invention is characterized in that comprising the following steps:

[0040]Add silica sol, N,N,N-trimethyladamantyl ammonium hydroxide, and aluminum sulfate to deionized water in sequence. The proportion of each component is SiO 2 :Al 2 o 3 :R:H 2 O=1:0.2:0.14:16. After mixing and stirring evenly, transfer to the reaction kettle, and crystallize at 100° C. for 12 hours to obtain the directing agent slurry (G-3).

[0041] Add ethylene glycol, triethylamine, N,N,N-trimethyladamantyl ammonium hydroxide, silica sol, and aluminum sulfate in deionized water in sequence, and stir well to form a uniform gel. The molar ratio of each component substance in the gel is SiO 2 :Al 2 o 3 :R:R1:C:H 2 O=1:0.05:0.04:1.8:0.06:14. An 8% directing agent solution (G-3) on a dry basis of the slurry was then added. Put it into the reaction kettle after mixing well, and crystallize at 160°C for 60 hours. After the crys...

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Abstract

The invention relates to a method for preparing an H-SSZ-13 molecular sieve and belongs to the field of hydrogen molecular sieve catalyzed synthesis. The method comprises the following steps: a) uniformly stirring and mixing a silicon source, an aluminum source, a template agent and water; b) uniformly mixing the silicon source, the aluminum source, the template agent, a cosolvent and water to form initial gel, adding a guiding agent solution, and crystallizing after being uniformly stirred; and c) separating, washing, drying and calcining the product after crystallization completion, therebyobtaining the H-SSZ-13 molecular sieve. According to the method disclosed by the invention, due to use of the guiding agent solution and the aided template agent, the effects of reducing usage of an expensive template agent and shortening the crystallization time are achieved, so that the production cost is greatly reduced.

Description

technical field [0001] The invention relates to a preparation method of H-SSZ-13 molecular sieve, which belongs to the field of catalytic synthesis of hydrogen molecular sieves. Background technique [0002] Mobile source denitrification technology is currently a hot topic in research, especially the current increasing number of motor vehicles, resulting in more NO X emission. Ammonia selective catalytic reduction technology (NH 3 -SCR) is currently the most widely used NO in the world X Removal technology, the principle is based on NH 3 As a reducing agent, the NO X revert to harmless N 2 And emissions. The key to SCR technology is to develop an efficient and stable catalyst system to adapt to the special environment used by motor vehicles. [0003] SSZ-13 molecular sieve is a molecular sieve with a CHA topology structure, and its pore size is only 0.38nm, which belongs to small-pore molecular sieves. Cu-based SSZ-13 molecular sieve catalyst for NH 3 -During the SC...

Claims

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Application Information

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IPC IPC(8): C01B39/48B01J29/70C07C1/20C07C11/02B01D53/02B01D53/94B01D53/56
CPCB01D53/02B01D53/9418B01J29/70C01B39/48C01P2002/72C01P2004/03C07C1/20C07C11/02Y02A50/20Y02T10/12
Inventor 王龙周泳冰明曰信刘环昌陈文勇彭立
Owner SHANDONG QILU HUAXIN HIGH TECH
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