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Preparation method of solid acid catalyst for oxidative coupling of methane to ethylene

A technology of solid acid catalyst and oxidative coupling, which is applied in the direction of carbon compound catalyst, metal/metal oxide/metal hydroxide catalyst, physical/chemical process catalyst, etc., and can solve the problem of low methane conversion rate, existence safety, and yield Low-level problems, to achieve the effect of good catalytic performance, enhanced activity, and simple preparation method

Active Publication Date: 2019-02-01
LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

CN1389293A discloses a kind of SiO 2 as a carrier, loaded with Mn 2 o 3 、Na 2 WO 4 and SnO 2 The multi-component catalyst, under pressure (0.6 MPa), can obtain higher methane conversion and C 2 Selectivity, but the reaction process needs to be pressurized, and there are potential safety hazards
CN1696084A discloses a kind of active component is Ag, and carrier is SiO 2 、Al 2 o 3 , SBA-15 and other catalysts, although methane oxidative coupling reaction can be carried out at lower temperature, but its C 2 low yield
CN 102471181 A discloses a Ba-modified MgO catalyst for the selective oxidation of methane to ethylene, which can carry out methane oxidative coupling reaction at a lower temperature, but the conversion rate of methane is relatively low

Method used

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  • Preparation method of solid acid catalyst for oxidative coupling of methane to ethylene
  • Preparation method of solid acid catalyst for oxidative coupling of methane to ethylene
  • Preparation method of solid acid catalyst for oxidative coupling of methane to ethylene

Examples

Experimental program
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Effect test

Embodiment 1

[0024] Example 1 A method for preparing a solid acid catalyst for oxidative coupling of methane to ethylene, comprising the following steps:

[0025] (1) Add 2 g of anatase TiO 2 Fully ground to 6000~7000 mesh, added to 0.112 g / 5 mL ammonium metatungstate solution, ultrasonically impregnated for 20 minutes under the condition of ultrasonic frequency of 45KHz and temperature of 20°C, and then stirred and evaporated to dryness in 80°C water bath to obtain Tungsten-titanium solid acid precursor; the tungsten-titanium solid acid precursor is heated to 800°C at a heating rate of 4°C / min in a muffle furnace, roasted for 3 hours, and then ground into powder to obtain WO 3 5 wt% solid acid WO 3 / TiO 2 carrier.

[0026] (2) Add 0.138 g LiNO to 10 mL ionized water in sequence 3 , 0.358 g Mn(NO 3 ) 2 (50%), and make it dissolve completely, then add 1.448 g solid acid WO 3 / TiO 2 The carrier is impregnated by an excessive impregnation method to obtain an impregnation;

[0027] (3...

Embodiment 2

[0031] Example 2 A method for preparing a solid acid catalyst for oxidative coupling of methane to ethylene, comprising the following steps:

[0032] (1) Add 2 g of anatase TiO 2 After being fully ground to 6000~7000 mesh, it was added to 0.185 g / 5 mL ammonium metatungstate solution, ultrasonically impregnated for 20 minutes under the conditions of ultrasonic frequency of 200KHz and temperature of 60°C, and then stirred and evaporated to dryness in a water bath of 80°C to obtain Tungsten-titanium solid acid precursor; the tungsten-titanium solid acid precursor is heated to 800°C at a heating rate of 4°C / min in a muffle furnace, roasted for 3 hours, and then ground into powder to obtain WO 3 8 wt% solid acid WO 3 / TiO 2 carrier.

[0033] (2) Add 0.138 g LiNO to 10 mL ionized water in sequence 3 , 0.358 g Mn(NO 3 ) 2 (50%), and make it dissolve completely, then add 1.493 g solid acid WO 3 / TiO 2 The carrier is impregnated by an excessive impregnation method to obtain an ...

Embodiment 3

[0038] Example 3 A method for preparing a solid acid catalyst for oxidative coupling of methane to ethylene, comprising the following steps:

[0039] (1) Add 2 g of anatase TiO 2 Fully ground to 6000~7000 mesh, added to 0.112 g / 5 mL ammonium metatungstate solution, ultrasonically impregnated for 20 minutes under the condition of ultrasonic frequency of 45KHz and temperature of 20°C, and then stirred and evaporated to dryness in 80°C water bath to obtain Tungsten-titanium solid acid precursor; the tungsten-titanium solid acid precursor is heated to 800°C at a heating rate of 4°C / min in a muffle furnace, roasted for 2 hours, and then ground into powder to obtain WO 3 5 wt% solid acid WO 3 / TiO 2 carrier.

[0040] (2) Add 0.138 g LiNO to 10 mL ionized water in sequence 3 , 0.358 g Mn(NO 3 ) 2 (50%), and make it dissolve completely, then add 1.448 g solid acid WO 3 / TiO 2 The carrier is impregnated by an excessive impregnation method to obtain an impregnation;

[0041] (3...

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Abstract

The invention relates to a preparation method of a solid acid catalyst for oxidative coupling of methane to ethylene. The method comprises the steps of: (1) fully grinding TiO2 to 6000-7000 meshes, then adding the ground TiO2 into a tungsten salt solution, conducting ultrasonic impregnation, stirring and evaporation to dryness in water bath to obtain a tungsten-titanium solid acid precursor; roasting and grinding the tungsten-titanium solid acid precursor into powder, thus obtaining a WO3 / TiO2 carrier with a WO3 content of 5wt%-15wt%; (2) adding LiNO3 and Mn(NO3)2 into ionized water in order for complete dissolution, and then impregnating the solid acid WO3 / TiO2 carrier by excessive impregnation process to obtain an impregnated substance; and (3) subjecting the impregnated substance to stirring and evaporation to dryness in water bath, performing grinding into powder, and then conducting roasting to obtain the solid acid catalyst. The preparation method provided by the invention has the characteristics of simplicity, mild preparation conditions and few industrial three wastes, and the obtained catalyst has the advantages of good performance, long service life and the like.

Description

technical field [0001] The invention relates to the technical field of chemical catalysts, in particular to a preparation method of a solid acid catalyst for oxidative coupling of methane to ethylene. Background technique [0002] The oxidative coupling of methane to low-carbon olefins is an important development direction for the comprehensive utilization of natural gas to replace the petroleum cracking route. Its industrialization can realize the direct synthesis of ethylene from natural gas, and will provide a new source of ethylene raw materials when oil resources are in short supply in the future. It has a major strategy Significance and great industrial application value. There are a lot of documents and patents related to the catalyst system in this field, but as far as the catalyst system in this field is concerned, the methane oxidative coupling catalyst has C 2 The low yield of hydrocarbons and the high temperature required for the reaction make the industrializat...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/34C07C2/84C07C11/04
CPCB01J23/002B01J23/34C07C2/84C07C2523/34C07C11/04Y02P20/52
Inventor 丑凌军程飞杨建宋焕玲赵军赵华华闫亮牛建中张兵
Owner LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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