Preparation method of Ce modified Cu-Fe-SSZ-13 molecular sieve

A cu-fe-ce-ssz-13, molecular sieve technology, applied in separation methods, molecular sieve catalysts, chemical instruments and methods, etc., can solve the problems of unsatisfactory hydrothermal stability, complex preparation process and high cost, and achieve The effect of improving the damage degree of the skeleton, simple preparation process and low cost

Active Publication Date: 2021-05-28
SHANDONG SINOCERA FUNCTIONAL MATERIAL CO LTD
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  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although Fe / Cu-SSZ-13 molecular sieves have improved low-temperature and high-temperature performance compared to Cu-SSZ-13, their hydrothermal stability after aging of low-silicon-aluminum ratio molecular sieves is still not ideal
[0004] Chinese patent document CN110180583A (application number: 201910573377.9) discloses a copper-containing iron-cerium-based molecular sieve material and its preparation method and catalyst; the method uses Fe2+ as the active center, but the present invention uses Fe3+ as the active center. In addition, the preparation process of this method is complicated, the cost is high, and it is difficult to implement in industry. The present invention adopts a one-step method to synthesize Cu -Fe-Ce-SSZ-13 molecular sieve, avoiding the use of expensive templating agents, has greatly improved in terms of cost and industrial ease of implementation

Method used

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  • Preparation method of Ce modified Cu-Fe-SSZ-13 molecular sieve

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] A kind of preparation method of Cu-Fe-Ce-SSZ-13 molecular sieve D0, comprises the steps:

[0038] (1) 2.7g CuSO 4 ·5H 2 Dissolve O in 15mL deionized water, stir well, add 14.88g tetraethylenepentamine (TEPA) dropwise, and continue stirring for 1 hour; then add 0.6g Ce(NO) 3 ·6H 2O and 4.8gFe(NO) 3 A solution fully dissolved in 33.78g of water, and then 10.4g of NaOH was added thereto to prepare A solution.

[0039] (2) Add 5.6gNaAlO to the A liquid prepared in step (1) 2 (41.0% Al by mass fraction 2 o 3 ), after stirring for 1 hour, add 60.0g silica sol (31.5% SiO by mass fraction 2 ), and then stirred for 2-3 hours, then put it into a polytetrafluoroethylene-lined steel reactor, aged for 12 hours, and subjected the obtained sol-gel precursor to a homogeneous hydrothermal reaction at 160°C for 72 hours, and crystallized After completion, centrifuge, wash with water to pH = 7, dry, and then calcined at 550° C. for 8 hours to obtain a Cu-Fe-Ce-SSZ-13 molecular sie...

Embodiment 2

[0047] A preparation method of Cu-Fe-Ce-SSZ-13 molecular sieve D1, comprising the steps of:

[0048] (3) 3.9g CuSO 4 ·5H 2 Dissolve O in 15ml deionized water, stir well, add 14.88g tetraethylenepentamine (TEPA) dropwise, continue stirring for 1 hour, then add 1.0g Ce(NO) 3 ·6H 2 O and 3.6gFe(NO) 3 Mix well and add 10.4g of NaOH to prepare liquid A.

[0049] (4) Add 5.6gNaAlO to the A liquid prepared in step (1) 2 (41.0% Al by mass fraction 2 o 3 ), after stirring for 1 hour, add 60.0g silica sol (31.5% SiO by mass fraction 2 ), and then stirred for 2-3 hours, then put it into a polytetrafluoroethylene-lined steel reactor, aged for 12 hours, and subjected the obtained sol-gel precursor to a homogeneous hydrothermal reaction at 160°C for 72 hours, and crystallized After completion, centrifuge, wash with water to pH = 7, dry, and then calcined at 550° C. for 8 hours to obtain a Cu-Fe-Ce-SSZ-13 molecular sieve catalyst.

[0050] The contents of Cu, Fe and Ce in the molecu...

Embodiment 3

[0052] A preparation method of Cu-Fe-Ce-SSZ-13 molecular sieve D2, comprising the steps of:

[0053] (1) 6.3g CuSO 4 ·5H 2 O was dissolved in 50ml of deionized water, stirred evenly, added dropwise 36.7g of tetraethylenepentamine (TEPA), continued to stir for 1 hour, and then added 1.5g of Ce(NO) 3 ·6H 2 O and 9.0gFe(NO) 3 A solution fully dissolved in 178.53g of water, and then 25.38g of NaOH was added thereto to obtain liquid A.

[0054] (2) Add 51.9g aluminum sulfate octadecahydrate in the A liquid that step (1) makes, add 60g solid silica gel (in terms of mass fraction 98%SiO2) after stirring for 1 hour 2 ), and then stirred for 2-3 hours, then put it into a polytetrafluoroethylene-lined steel reactor, aged for 12 hours, and subjected the obtained sol-gel precursor to a homogeneous hydrothermal reaction at 160°C for 96 hours, and crystallized After completion, centrifuge, wash with water to pH = 7, dry, and then calcined at 550° C. for 8 hours to obtain a Cu-Fe-Ce-SSZ...

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Abstract

The invention relates to a preparation method of a Ce-modified Cu-Fe-SSZ-13 molecular sieve. The method particularly comprises: slowly dropwise adding tetraethylenepentamine into a copper sulfate solution under intense stirring, sequentially adding cerous nitrate and ferric nitrate after the reaction is finished, fully and uniformly mixing, and adding sodium hydroxide to prepare a solution A; and adding sodium metaaluminate or aluminum sulfate octadecahydrate into the solution A, stirring for 1-2 hours, then adding silica sol, continuously stirring for 2-3 hours, then putting into a steel reaction kettle with a polytetrafluoroethylene lining, aging for 12-14 hours, carrying out homogeneous hydrothermal reaction on the obtained sol-gel precursor at 120-180 DEG C for 72-96 hours, after crystallization is finished, carrying out solid-liquid separation, washing the solid with water until the pH is neutral, drying, and calcining the solid at the temperature of between 500 and 550 DEG C for 4 to 8 hours to obtain the Cu-Fe-Ce-SSZ-13 molecular sieve.

Description

technical field [0001] The invention relates to a preparation method of an SSZ-13 molecular sieve catalyst, in particular to a preparation method of a Ce-modified Cu-Fe-SSZ-13 molecular sieve, which belongs to the field of industrial catalysis. Background technique [0002] Nitrogen oxides (NOx) from vehicle exhaust and industrial combustion of fossil fuels are harmful to ecosystems and humans. use NH 3 Selective catalytic reduction (SCR) as a reductant is an effective method for the removal of NO from the exhaust of diesel vehicles or coal-fired power plants. X Technology. V 2 o 5 -WO 3 / TiO 2 SCR-based catalysts have been commercially used in stationary source denitration processes since the 1970s, but vanadium-based catalysts have some unavoidable problems, such as narrow operating temperature range and toxicity of vanadium species. Therefore, it is crucial to develop vanadium-free SCR catalysts for NOx removal. with V 2 o 5 -WO 3 / TiO 2 Compared with other co...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J29/76B01J35/10B01D53/56B01D53/94
CPCB01J29/76B01J35/1023B01D53/9418
Inventor 宋锡滨邢晶张军亮鞠云忠
Owner SHANDONG SINOCERA FUNCTIONAL MATERIAL CO LTD
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