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Metal supported MCM-22 molecular sieve hollow sphere bifunctional catalyst preparation method and application thereof

A bifunctional catalyst and molecular sieve technology, which is applied in molecular sieve catalysts, catalyst activation/preparation, physical/chemical process catalysts, etc., can solve the problems of short catalytic life and catalyst deactivation, and achieve low cost, simplified operation steps, and operational processes simple and easy effects

Active Publication Date: 2010-01-06
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the oxygen-free aromatization of methane still faces the most serious problem, that is, due to the low conversion rate of methane, the reaction needs to be carried out at high temperature, and the severe carbon deposition leads to the rapid deactivation of the catalyst. Catalytic life is short, mostly no more than 20 hours

Method used

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  • Metal supported MCM-22 molecular sieve hollow sphere bifunctional catalyst preparation method and application thereof
  • Metal supported MCM-22 molecular sieve hollow sphere bifunctional catalyst preparation method and application thereof
  • Metal supported MCM-22 molecular sieve hollow sphere bifunctional catalyst preparation method and application thereof

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Experimental program
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Effect test

Embodiment 1

[0025] Preparation of hollow spheres of MCM-22 molecular sieve with hierarchical pore structure: 0.94g NaOH, 1.6gNaAlO 2 Soluble in 170g H 2 Mix well in O to form solution A, then weigh 10.7g hexamethyleneimine and add solution A, stir to form solution B, then add 12g carbon black spherical particle template to solution B, stir vigorously until uniform, and finally in 1 Add 31.6g of silica sol within 1 hour and keep stirring vigorously overnight to obtain the molar ratio of the synthetic liquid system: SiO 2 : Al 2 o 3 :Na 2 O:R:H 2O=1:0.03:0.1:2:50, then transfer the obtained mixture to a stainless steel reaction kettle with a polytetrafluoroethylene liner and rotate it at 150°C for 7 days, and the product is cooled and washed to obtain a completely crystallized product . After drying, heat up to 550°C in a muffle furnace at a rate of 0.5°C / min and bake for 8 hours to remove the carbon black spherical template and organic template to obtain MCM-22 zeolite molecular siev...

Embodiment 2

[0027] Preparation of Mo / HMCM-22 hollow sphere catalyst with hierarchical pore structure: Na-type MCM-22 molecular sieve hollow spheres were exchanged 3 times with 1M ammonium nitrate solution at 80-100°C, washed 3 times with water, and then heated in air at 550°C Calcined in atmosphere for 6 hours to obtain HMCM-22 for future use. Weigh 3 grams of HMCM-22, place it in 30 ml of 0.011 g / ml ammonium molybdate solution, stir and impregnate overnight. Dry at 100°C for 6 hours, and then bake at 500°C in an air atmosphere for 6 hours to obtain the product Mo / HMCM-22 hollow sphere catalyst, which is crushed to 40 mesh for use.

Embodiment 3

[0029] Reaction evaluation of Mo / HMCM-22 hollow sphere catalyst: Methane anaerobic aromatization reaction is carried out on a continuous flow fixed bed, the reactor is a quartz reaction tube with an inner diameter of 8 mm, the catalyst is loaded with 0.5 grams each time, and the reaction pressure is one Atmospheric pressure, the reaction temperature is 700°C, and the methane feed space velocity is 1500ml / g·h. The catalyst was pretreated with He gas at 700 °C for 30 minutes and then switched to feed gas (composition of 10% N 2 , 90% CH 4 ) for catalytic reaction, using N 2 Calculation of carbon balance results including carbon deposition for internal standards. The reaction methane conversion rate and the yield of aromatics are listed in Figure 4 , Figure 5 , the result proves that the hollow sphere catalyst prepared by the present invention has higher activity relative to conventional catalysts, and is very superior in anti-coking ability, thus has very long catalyst lif...

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Abstract

The invention relates to a metal supported MCM-22 molecular sieve hollow sphere bifunctional catalyst preparation method and an application thereof, belonging to the molecular sieve catalysis technology. The method is characterized in that carbon black sphere particles are used as template, molecular sieve hollow spheres with multi-stage pore path structure is prepared by rotation hydrothermal crystallization and by using metal active components the prepared molecular sieve hollow spheres are loaded and modified. The prepared Mo / HMCM-22 molecular sieve hollow sphere bifunctional catalyst can be used in methane non-oxidative aromatization reaction system. The effect and the benefit of the invention is that the preparation method of the molecular sieve hollow spheres has simple operation and low cost, and the prepared hollow sphere catalyst has excellent catalytic performance in the methane non-oxidative aromatization reaction, high methane conversion rate and aromatics yield and very long catalyst life.

Description

technical field [0001] The invention belongs to the technical field of molecular sieve catalysis, and relates to a preparation method of a molecular sieve catalyst with a novel hollow structure and a multi-level pore structure, and specifically relates to the one-step synthesis of a zeolite molecular sieve hollow sphere catalyst with a multi-level pore structure by using carbon black ball particles as a template And apply it to the technical field of producing aromatics by methane oxygen-free dehydrogenation aromatization. Background technique [0002] As a kind of aluminosilicate material, molecular sieve is often used as catalyst or catalyst carrier due to its stable solid acidity, large specific surface area, and regular and uniform pore structure. MCM-22 molecular sieve is a molecular sieve with MWW structure, which was first synthesized by Mobil Corporation (USP4,954,325). Since then, reports on the application of MCM-22 molecular sieve at home and abroad have been incr...

Claims

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Application Information

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IPC IPC(8): B01J29/78B01J37/08B01J37/02B01J35/08C07C2/58
Inventor 王金渠杨建华初乃波鲁金明张艳殷德宏
Owner DALIAN UNIV OF TECH
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