One-step method for synthesizing copper-containing CHA type molecular sieve with high hydro-thermal stability

A thermally stable, molecular sieve technology, applied in the direction of molecular sieve and alkali exchange phosphate, molecular sieve characteristic silicoaluminophosphate, etc., can solve the problems of low utilization rate of metal ions, decreased molecular sieve stability, long synthesis time, etc., and shorten the preparation time. effect of time, high crystallinity and specific surface area, simplified operation steps

Active Publication Date: 2014-05-28
WUXI WEIFU ENVIRONMENT PROTECTION CATALYST
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  • Abstract
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  • Claims
  • Application Information

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Problems solved by technology

[0004] The purpose of the present invention is to solve the problem of many exchange process steps, low utilization rate of metal ions, long synthesis time, many waste water and many problems due to the hydrolysis of the molecular sieve skeleton in the exchange process in the process of preparing copper-containing SAPO-34 molecular sieve by ion exchange method in the prior art. The disadvantages such as the serious decline in the stability

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  • One-step method for synthesizing copper-containing CHA type molecular sieve with high hydro-thermal stability
  • One-step method for synthesizing copper-containing CHA type molecular sieve with high hydro-thermal stability

Examples

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Embodiment 1

[0018] (1) First stir pseudo-boehmite fully in deionized water, then slowly add phosphoric acid to completely peptize pseudo-boehmite; after peptization is complete, add fumed silica and copper acetate and stir evenly, then add four Ethylammonium hydroxide and diethylenetriamine are stirred vigorously; the molar ratio P of each reaction raw material in the molecular sieve synthesis liquid 2 o 5 :Al 2 o 3 :SiO2 2 :T:L:CuO:H 2 O is 0.9:1.0:0.5:2.0:0.2:0.05:80, where T is tetraethylammonium hydroxide, L is diethylenetriamine, and after stirring for 4 hours, put it into tetrafluoroethylene or p-polystyrene In a lined stainless steel reactor; crystallize this reactor at 160°C for 5 days;

[0019] (2) After the crystallization is completed, the obtained product is suction-filtered, washed several times with deionized water until the washing liquid is neutral, and the obtained solid product is dried in an oven at 80°C for 6 hours; then the dried product is dried in a muffle furn...

Embodiment 2

[0025] (1) First, fully stir the pseudo-boehmite in deionized water, then slowly add phosphoric acid to completely peptize the pseudo-boehmite; after the peptization is complete, add fumed silica and copper acetate and stir evenly, then add three Ethylamine and diethylenetriamine are stirred vigorously; the molar ratio P of each reaction raw material in the molecular sieve synthesis liquid 2 o 5 :Al 2 o 3 :SiO2 2:T:L:CuO:H 2 O is 0.9:1.0:0.5:3.0:0.3:0.1:80, where T is triethylamine and L is diethylenetriamine; after stirring for 4 hours, put it into stainless steel lined with tetrafluoroethylene or p-polystyrene In the reactor; crystallize the reactor at 200°C for 3 days;

[0026] (2) After the crystallization is completed, the obtained product is centrifuged and washed several times until the washing liquid is neutral, and the obtained solid product is dried in an oven at 80°C for 6 hours; then the dried product is placed in a muffle furnace under an air atmosphere to T...

Embodiment 3

[0029] (1) First, fully stir the aluminum sol in deionized water, then slowly add phosphoric acid to dissolve the aluminum sol; after the dissolution is complete, add silica sol and copper chloride with a mass fraction of 40% and stir evenly, then add triethylamine and diethylenetriamine and vigorously stirred; the molar ratio P of each reaction raw material in the molecular sieve synthesis liquid 2 o 5 :Al 2 o 3 :SiO2 2 :T:L:CuO:H 2 O is 0.8:1.0:0.5:2.5:0.1:0.1:80, where T is triethylamine and L is diethylenetriamine; after stirring for 8 hours, put it into stainless steel lined with tetrafluoroethylene or p-polystyrene In the reactor; crystallize the reactor at 190°C for 5 days;

[0030] (2) After the crystallization is completed, the obtained product is filtered by plate and frame, and washed several times with deionized water until the washing liquid is neutral, and the obtained solid product is dried in an oven at 80°C for 6 hours; then the dried product is dried at ...

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Abstract

The invention relates to a one-step method for synthesizing a copper-containing CHA type molecular sieve with high hydro-thermal stability. The method comprises the steps of (1) firstly stirring an aluminium source in deionized water thoroughly, then slowly adding phosphoric acid to dissolve the aluminium source completely, adding a certain amount of a silicon source and a copper source, stirring uniformly, adding an organic amine template and a ligand reagent with vigorous stirring, stirring for 2-8 hours, adding an obtained solution into a stainless steel reaction kettle with a polytetrafluoroethylene or polyphenylene lining, crystallizing for 0.5-5 days at a temperature of 140-210 DEG C; and (2) washing the obtained product, drying for 3-8 hours at a temperature of 60-110 DEG C; and roasting a dried product for 2-8 hours at a temperature of 450-600 DEG C to obtain the copper-containing CHA type molecular sieve. The template used in the method is cheap and easily available. One-step synthesis of the copper-containing CHA type molecular sieve omits a plurality of copper-containing salt solution ion exchange and roasting processes, simplifies operation steps and saves energy. The prepared copper-containing CHA type molecular sieve has relatively high degree of crystallinity and specific surface area, and has good hydro-thermal stability.

Description

technical field [0001] The invention relates to a method for synthesizing high hydrothermal stability copper-containing CHA molecular sieves in one step, in particular to a method for directly synthesizing high hydrothermal stability copper-containing CHA molecular sieves in one step using a template agent-ligand reagent, belonging to Technical field of molecular sieve catalyst preparation. Background technique [0002] CHA-type (Chabazite) molecular sieves have good hydrothermal stability. Among them, silicon-aluminum-type SSZ-13 molecular sieves and silicon-aluminophosphate-type SAPO-34 molecular sieves have broad application prospects in the field of catalysis due to their suitable acidity and pore structure. In the selective catalytic reduction (NOx Selective Catalytic Reduction, NOx-SCR) reaction of motor vehicle exhaust nitrogen oxides, copper-containing Cu / SSZ-13 and Cu / SAPO-34 both exhibit excellent catalytic performance. At present, most of the introduction of copp...

Claims

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Application Information

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IPC IPC(8): C01B39/54C01B37/08
Inventor 金炜阳岳军王卫东赵德鹏陈同同盛丽萍肖蓉王均吴嘉昉贾莉伟王家明
Owner WUXI WEIFU ENVIRONMENT PROTECTION CATALYST
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