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A kind of synthesis method of mesoporous silicon oxide solid acid catalyst with high doping amount and high acidity site

A technology of solid acid catalyst and mesoporous silica, which is applied in the direction of physical/chemical process catalyst, molecular sieve catalyst, chemical instrument and method, etc., can solve the problem of low doping amount, achieve simple treatment process, low cost, and improve catalytic performance. performance effect

Active Publication Date: 2021-05-07
BAOJI UNIV OF ARTS & SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] Common methods for doping transition metal (M) into the framework structure of mesoporous silica include one-step synthesis method "J. Colloid Interface Sci. , 26(4), 618-623; Chinese Journal of Environmental Engineering, 2014, 8(4), 1454-1460" and the post-processing method "Talanta 148(2016) 22-28", etc., but for positive divalent transition metal elements such as Zn , Ni, Mn, Cu, Co and other elements, the general problem of the above methods is that the doping amount in the mesoporous silica framework is low, less than 5%, especially the doping of Zn and Ni in the framework has not yet According to reports, it is mainly the loading of ZnO and NiO in mesoporous channels
[0004] By searching the existing technologies at home and abroad, no one has proposed to use acetate to promote the doping amount of transition metal elements in the mesoporous silica framework, and to prepare a solid acid catalyst with highly dispersed transition metal elements

Method used

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  • A kind of synthesis method of mesoporous silicon oxide solid acid catalyst with high doping amount and high acidity site
  • A kind of synthesis method of mesoporous silicon oxide solid acid catalyst with high doping amount and high acidity site
  • A kind of synthesis method of mesoporous silicon oxide solid acid catalyst with high doping amount and high acidity site

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] Example 1 Preparation of copper-doped mesoporous silica molecular sieve material:

[0045] Take 0.25g of SBA-15, MCM-41, FDU-5, KIT-6, HMS and MSU, respectively, and disperse them in 25ml of ethanol solution, add 0.28g of copper acetate and stir for 25min; In a stainless steel reaction kettle lined with tetrafluoroethylene, place the reaction kettle in a preheated 80°C electric blast drying oven to react for 14 hours, then take out the reaction kettle to cool naturally, and the product is suction filtered, washed, and dried at 60°C After 12 hours, the obtained powder sample was placed in a muffle furnace to raise the temperature to 550° C. at a heating rate of 2° C. / min, and then calcined for 5 hours to obtain a dark green doped mesoporous silica molecular sieve.

[0046] The composition, mesoporous structure, and microscopic shape of the prepared copper-doped SBA-15 mesoporous molecular sieve materials are analyzed by means of XRD, SEM, TEM, EDS, ICP-OES, solid ultravi...

Embodiment 2

[0060] Example 2 Zinc-doped mesoporous silica molecular sieve material preparation:

[0061] Take 0.25g of SBA-15, MCM-41, FDU-5, KIT-6, HMS and MSU, respectively, and disperse them in 21ml of ethanol solution, add 0.26g of zinc acetate and stir for 27min; In a stainless steel reaction kettle lined with tetrafluoroethylene, place the reaction kettle in a preheated 70°C electric blast drying oven to react for 16 hours, then take out the reaction kettle and let it cool naturally. The product is suction filtered, washed, and dried at 80°C After 8 hours, the obtained powder sample was placed in a muffle furnace to raise the temperature to 500° C. at a heating rate of 1° C. / min, and then calcined for 6 hours to obtain a white doped mesoporous silica molecular sieve.

[0062] The products were analyzed and characterized by XRD, SEM, TEM, ICP-OES, solid ultraviolet, physical adsorption and chemical adsorption, indicating that the zinc-doped mesoporous silica molecular sieve material ...

Embodiment 3

[0064] Example 3: Preparation of nickel-doped mesoporous silica molecular sieve material:

[0065] Take 0.25g of SBA-15, MCM-41, FDU-5, KIT-6, HMS and MSU, respectively, and disperse them in 25ml of ethanol solution, add 0.3g of nickel acetate and stir for 30min; In a stainless steel reaction kettle lined with tetrafluoroethylene, place the reaction kettle in a preheated 80°C electric blast drying oven to react for 15 hours, then take out the reaction kettle and let it cool naturally. The product is suction filtered, washed, and dried at 70°C After 10 hours, the obtained powder sample was placed in a muffle furnace to raise the temperature to 480° C. at a heating rate of 1° C. / min, and then calcined for 6 hours to obtain a doped mesoporous silica molecular sieve.

[0066] The above products were characterized by XRD, SEM, TEM, ICP-OES, solid ultraviolet, physical adsorption and chemical adsorption analysis, which showed that the cobalt-doped mesoporous silica molecular sieve m...

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Abstract

The invention discloses a method for synthesizing a solid acid catalyst of mesoporous silicon oxide with high doping amount and high acidity. The method comprises the following steps: (1) dispersing mesoporous silicon oxide in ethanol, and then adding a divalent transition metal Substances of ions and acetate groups; (2) react the reaction system obtained in step 1 at 70-80°C for 14-16h under sealed conditions, and naturally cool to room temperature after the reaction, and the product is suction filtered, washed, and dried to obtain a powder Substance; (3) Calcining the powdery substance obtained in step 2 after heating up to obtain a doped mesoporous silica molecular sieve. Through the selection of raw materials, the control of reaction solvent, reaction environment and parameters, the method of the present invention realizes the uniform doping of divalent transition metal elements in the skeleton structure of mesoporous silica molecular sieves, and at the same time avoids the formation of metal oxides, and the whole reaction The treatment process is simple, controllable, low in cost, green and free of pollutants, and can be produced on a large scale.

Description

technical field [0001] The invention belongs to the technical field of preparation of inorganic non-metallic materials, and in particular relates to a synthesis method of a mesoporous silicon oxide solid acid catalyst with high doping amount and high acidity. Background technique [0002] Due to its controllable pore structure and high specific surface area, mesoporous silica materials are widely used in related fields such as catalysis, drug loading, adsorption separation, sensor and nanomaterial preparation. However, untreated mesoporous silica lacks chemical activity, and its application in the chemical industry is very limited. One of the common methods for activating mesoporous silica is to introduce other elements (doping) into its silicon-oxygen framework, such as Various transition metal elements such as aluminum and iron make it have ion exchange ability, acid center generation and various catalytic activities. Transition metal elements are catalyst active componen...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J29/04C02F1/72C02F101/30
CPCB01J29/041B01J29/044B01J29/045C02F1/722C02F1/725C02F2101/308C02F2305/02
Inventor 罗小林苗康康裴霏冯国栋潘哲郭家乐王伟
Owner BAOJI UNIV OF ARTS & SCI