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Synthesis method of Cu-SSZ-13 molecular sieve

A technology of cu-ssz-13, synthesis method, applied in the direction of crystalline aluminosilicate zeolite, bulk chemical production, combustion engine, etc., can solve the problems of reduced activity, reduced specific surface area and pore volume of Cu-SSZ-13, etc.

Active Publication Date: 2021-05-18
CHINA CHEM TECH RES INST +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Li et al. (Chem. Eng. J., 2013, 225, 323-330) found that hydrothermal treatment significantly reduced the specific surface area and pore volume of Cu-SSZ-13, causing isolated Cu 2+ Migrate to the outside of the molecular sieve to form aggregated CuO particles, making the NH 3 -Reduced SCR activity

Method used

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

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] 1) Using sodium metaaluminate, silica sol, NaOH, N,N,N-trimethyl-1-adamantyl ammonium hydroxide as raw materials, synthesize molecular sieves according to the following molar ratio of raw materials:

[0031] h 2 O:OH - :Al 2 o 3 : SiO 2 :R=60:0.4:0.0667:1:0.2;

[0032] 2) Dissolve 0.07g of sodium metaaluminate and 0.02g of sodium hydroxide in 5.29g of deionized water, and add 1.10g of N,N,N-trimethyl-1-adamantyl with a mass fraction of 25% after completely dissolving Aqueous solution of ammonium hydroxide, after stirring and dissolving, slowly add 1.30g of SiO2 dropwise under rapid stirring conditions 2 Silica sol with a mass fraction of 30%. Afterwards 0.87 g of CuO loading at 2%, SiO 2 / Al 2 o 3 =15 commercial Cu-SSZ-13 molecular sieves (commercial Cu-SSZ-13 molecular sieves were purchased from China Catalyst Co., Ltd., product number SSZ-13; SiO in commercial Cu-SSZ-13 2 / Synthesis of SiO in Gels 2 =2), and stir well.

[0033] 3) The obtained mixture was...

Embodiment 2

[0038] 1) Aluminum isopropoxide, precipitated SiO 2 , NaOH, and choline chloride are raw materials, and molecular sieves are synthesized according to the following molar ratio of raw materials:

[0039] h 2 O:OH - :Al 2 o 3 : SiO 2 :R=80:0.4:0.0333:1:0.2;

[0040] 2) Dissolve 2.28g of aluminum isopropoxide and 2.67g of sodium hydroxide in 235.50g of deionized water, add 6.58g of choline chloride aqueous solution with a mass fraction of 70% after dissolving completely, and add 10.00g of precipitated SiO after dissolving 2 and 48.94g CuO loading at 5%, SiO 2 / Al 2 o 3 =30 commercial Cu-SSZ-13 molecular sieve (wherein, the SiO in the commercial Cu-SSZ-13 raw material 2 / Precipitated SiO 2 SiO in 2 =4), and stir well.

[0041] 3) The obtained mixture was transferred to a stainless steel autoclave lined with polytetrafluoroethylene, and crystallized at 170° C. for 48 h.

[0042] 4) After the crystallization is stopped, the temperature is lowered to below 60°C, the pro...

Embodiment 3

[0044] 1) Using aluminum isopropoxide, precipitated white carbon black, NaOH, and choline chloride as raw materials, synthesize a molecular sieve catalyst according to the following molar ratio of raw materials:

[0045] h 2 O:OH - :Al 2 o 3 : SiO 2 :R=100:0.5:0.02:1:0.2;

[0046] 2) Dissolve 1.37g of aluminum isopropoxide and 3.33g of sodium hydroxide in 294.89g of deionized water, add 6.58g of choline chloride aqueous solution with a mass fraction of 70% after dissolving completely, and then add 10.00g of precipitated white carbon black and 59.13 g CuO loading at 5%, SiO 2 / Al 2 o 3 =80 commercial Cu-SSZ-13 molecular sieve (wherein, the SiO in the commercial Cu-SSZ-13 raw material 2 / precipitated SiO 2 SiO in 2 =5), and stir evenly.

[0047] 3) The obtained mixture was transferred to a stainless steel autoclave lined with polytetrafluoroethylene, and crystallized at 170° C. for 48 h.

[0048] 4) After the crystallization is stopped, the temperature is lowered to ...

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Abstract

The invention provides a synthesis method of a Cu-SSZ-13 (at) SSZ-13 molecular sieve. The synthesis method is characterized by comprising the following steps: 1) preparing Cu-SSZ-13 (at) SSZ-13 synthetic gel from a shell layer consisting of an SSZ-13 molecular sieve; (2) a core layer is composed of Cu-SSZ-13, the Cu-SSZ-13 serving as a core layer material is added into a high-pressure kettle to be evenly mixed with the synthetic gel, stirring is conducted, the temperature is increased to 120-200 DEG C, and crystallization is conducted for 0.1-100 h; and 3) stopping crystallization, cooling to below 60 DEG C, filtering, washing, drying a solid sample, and roasting to obtain the Cu-SSZ-13 (at) SSZ-13 molecular sieve. According to the method disclosed by the invention, the Cu-SSZ-13 (at) SSZ-13 structure is constructed, so that the interior of the molecular sieve is rich in Cu, the surface of the molecular sieve is less / free of Cu, the generation of CuO particles is reduced in the use process, the proportion of NH3 oxidation reaction is reduced, and the catalytic performance of the catalyst in a high-temperature region is further improved.

Description

technical field [0001] The disclosure relates to the field of chemical production technology, in particular to a synthesis method of Cu-SSZ-13 molecular sieve. Background technique [0002] SSZ-13 is a molecular sieve with CHA topology, which is composed of AlO 4 and SiO 4 The tetrahedra are connected end to end by oxygen atoms, and are arranged in an orderly manner into an ellipsoidal cage (0.73 nm×1.2 nm) with an eight-membered ring structure and a three-dimensional intersecting channel structure with a channel size of 0.38 nm × 0.38 nm. Among them, the Cu-SSZ-13 catalyst with Cu ion exchange is the main means of reducing nitrogen oxides (NOx) in diesel engine exhaust - ammonia selective catalytic reduction (NH 3 -SCR) technology shows a wide activity temperature window and excellent N 2 Selectivity has shown great promise in commercial applications. With the continuous upgrading of the aftertreatment system of diesel engines, especially after the diesel particulate fi...

Claims

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Application Information

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IPC IPC(8): C01B39/06C01B39/04
CPCC01B39/06C01B39/04C01P2002/72C01P2006/12C01P2004/82Y02T10/12
Inventor 刘中清王倩赵峰邓兆敬
Owner CHINA CHEM TECH RES INST