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Preparation method and application of SSZ-13 molecular sieve catalyst

A molecular sieve and catalyst technology, which is applied in the field of molecular sieve preparation and environmental catalysts, can solve the problems of poor molecular sieve quality, high raw material cost, long working hours, etc., and achieve the effect of wide active window, excellent performance and high quality

Pending Publication Date: 2022-04-29
VALIANT CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Aiming at the deficiencies in the prior art, the present invention provides a method for preparing a high-quality copper-based SSZ-13 molecular sieve catalyst using cheap aluminum-rich A-type molecular sieves, which overcomes the high cost of raw materials, long working hours and low quality of molecular sieves in the current preparation process. poor disadvantage

Method used

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  • Preparation method and application of SSZ-13 molecular sieve catalyst
  • Preparation method and application of SSZ-13 molecular sieve catalyst
  • Preparation method and application of SSZ-13 molecular sieve catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] (1) Synthesis of N,N-dimethyl-hydroxyethyl-cyclohexyl-ammonium bromide

[0041] First add 10g N,N-dimethylcyclohexylamine, 30g toluene, add 10.5g bromoethanol dropwise under stirring condition, after dropwise addition, stir and react for 2-3 days, add deionized water after reaction, separate organic phase, water The phase is an aqueous solution of N,N-dimethyl-hydroxyethyl-cyclohexyl-ammonium bromide.

[0042] (2) Synthesis of SSZ-13 molecular sieve

[0043] First add 23.2g of deionized water, 11.4g of N,N-dimethyl-hydroxyethyl-cyclohexyl-ammonium bromide aqueous solution, and slowly add 18.4g of silica sol and 23.0g of water glass into the kettle while stirring, Then add 4.1g NaA molecular sieve and 0.025g SSZ-13 molecular sieve raw powder into the system as seed crystals, stir evenly to obtain the initial gel; transfer the gel to a stainless steel reaction kettle, and crystallize at 165°C for 18 hours; , after cooling, suction filtration, washing with deionized wate...

Embodiment 2

[0048] (1) Treatment of type A molecular sieve

[0049] Add 12g of ammonium sulfate to a small beaker, add 88g of water, fully dissolve, add 5g of NaA molecular sieve, exchange ammonium at 80°C for 1h, filter, rinse with deionized water, and dry at 120°C to obtain NH 4 A molecular sieve.

[0050] (2) Synthesis of SSZ-13 molecular sieve

[0051] First add 7.5g deionized water, 21.0g N,N,N-trimethyl-benzyl-ammonium hydroxide aqueous solution, slowly add 10.1g silica sol, 39.8g water glass in the tank under stirring, then add Add 1.5g NH to the system 4 A molecular sieve and 0.003g SSZ-13 molecular sieve finished product were used as seed crystals, stirred evenly to obtain an initial gel; the gel was transferred to a stainless steel reaction kettle, and crystallized at 135°C for 24 hours; Washing with ionized water and drying at 120°C for 4 hours to obtain the raw powder of SSZ-13 molecular sieve; then exchanged with ammonium and roasted at 550°C for 5 hours to obtain the fini...

Embodiment 3

[0056] (1) Synthesis of SSZ-13 molecular sieve

[0057] First add 1.7g of deionized water, 20.4g of N,N,N-triethyl-cyclohexyl ammonium bromide aqueous solution, slowly add 17.8g of silica sol, 38.6g of water glass into the tank under stirring, and then add to the system Add 1.5g NaA molecular sieve and 0.025g SSZ-13 molecular sieve finished product as crystal seeds, stir evenly to obtain the initial gel; transfer the gel to a stainless steel reaction kettle, and crystallize at 165°C for 24h; after crystallization, cool, Suction filtration, washing with deionized water, and drying at 120°C for 4 hours to obtain the raw powder of SSZ-13 molecular sieve; then exchanged with ammonium, and roasted at 530°C for 5 hours to obtain the finished product of SSZ-13 molecular sieve.

[0058] (2) Preparation of copper-based SSZ-13 molecular sieve catalyst

[0059] Consistent with part (2) of Example 1.

[0060] The silicon-aluminum ratio of the molecular sieve prepared in Example 3 is 38....

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Abstract

The invention relates to an SSZ-13 molecular sieve catalyst preparation method, which comprises: adding water and a template agent [R1R2R3N-R4] < + > Q <->, adding an alkali source and a silicon source, stirring until the system is uniform, adding an A molecular sieve as an aluminum source, adding a seed crystal, stirring at a high speed until the system is uniform so as to obtain an initial gel, carrying out a crystallization reaction to obtain a crystallization slurry, and drying the crystallization slurry so as to obtain the SSZ-13 molecular sieve catalyst. Cooling, filtering, washing with deionized water, drying to obtain an SSZ-13 molecular crystallization product, removing sodium ions, and removing the template agent to obtain an SSZ-13 molecular sieve; and carrying out ion exchange loading on the SSZ-13 molecular sieve finished product and a copper salt, filtering, washing with deionized water, drying to obtain a copper-based SSZ-13 molecular sieve, and carrying out crushing, roasting activation, tabletting and crushing to obtain the copper-based SSZ-13 molecular sieve catalyst. The method has the advantages of short crystallization time, low raw material cost, high molecular sieve quality, and high ammonia selective catalytic reduction activity.

Description

technical field [0001] The present invention relates to a kind of method for preparing SSZ-13 molecular sieve catalyst by the method of crystallization and its preparation in NO x The application in selective catalytic reduction reaction belongs to the technical field of molecular sieve preparation and environmental protection catalyst. Background technique [0002] The "National Six A" standard will be implemented from July 1, 2020, and the "National Six B" will be fully implemented from July 1, 2023. Compared with the "National V" standard, the emission limit of nitrogen oxides has been increased 77%, while diesel engine exhaust NO X It is mainly through SCR reduction treatment, which puts higher requirements on SCR catalysts, especially in the direction of cold start, that is, puts forward higher requirements on the low-temperature activity of catalysts. [0003] SSZ-13 molecular sieve is a kind of AlO 4 and SiO 4 Tetrahedrons are connected end to end by oxygen atoms,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J29/72B01J37/30B01D53/94B01D53/56C01B39/04
CPCB01J29/723B01J37/30B01D53/9413C01B39/04B01J2229/186B01D2251/2062C01P2002/72
Inventor 王继华魏玉林陈士辉李玉赵春利张一鸣牛盼盼
Owner VALIANT CO LTD