阅读说明：本技术 一种乙醇为溶剂制备金属负载型介孔催化剂的方法 (Method for preparing metal-loaded mesoporous catalyst by using ethanol as solvent ) 是由 李湘萍 陈冠益 张建光 刘彬 于 2018-06-10 设计创作，主要内容包括：一种乙醇为溶剂制备金属负载型介孔催化剂的方法,从制备过程控制出发,通过研究金属物种与介孔无机材料表面的相互作用,选择合适的溶剂溶解金属物种,获得具有高金属物种分散度的金属负载型催化剂；这对提高金属负载型催化剂的催化性能及金属负载型催化剂的广泛应用具有重要意义；该发明中催化剂浸渍所用的溶剂为乙醇,对环境无污染,成本低,可应用于工业催化剂的生产过程。且金属负载型介孔催化剂的制备过程简单,可操作型强。(a method for preparing metal supported mesoporous catalyst with ethanol as solvent, from the control of preparation process, by studying the interaction between metal species and the surface of mesoporous inorganic material, selecting proper solvent to dissolve metal species, obtaining metal supported catalyst with high metal species dispersion degree; the method has important significance for improving the catalytic performance of the metal-loaded catalyst and the wide application of the metal-loaded catalyst; the solvent used for catalyst impregnation in the invention is ethanol, which has no pollution to the environment and low cost and can be applied to the production process of industrial catalysts. And the preparation process of the metal-loaded mesoporous catalyst is simple and the operability is strong.)

1. A method for preparing a metal-loaded mesoporous catalyst by using ethanol as a solvent is characterized by comprising the following steps: the specific experimental steps are as follows:

Firstly, weighing 3 g of mesoporous inorganic material and placing the mesoporous inorganic material into a round bottom crucible;

Secondly, putting a certain amount of nickel nitrate hexahydrate into a glass beaker with the capacity of 25 mL, then moving absolute ethyl alcohol with the volume equivalent to the pore volume of the mesoporous inorganic material into the glass beaker by using a liquid-moving gun, stirring the absolute ethyl alcohol by using a glass rod until the nickel nitrate is completely dissolved, and then sealing the opening of the beaker by using a sealing film to prevent the ethyl alcohol from volatilizing;

Thirdly, slowly and uniformly dripping the nickel nitrate-ethanol solution obtained in the second step into the mesoporous inorganic material in the first step by using a 5 mL disposable pipette, and stirring the mixture by using a glass rod until the mixture presents uniform color after dripping; then, taking a sealing film to seal the round-bottom crucible, standing at room temperature for 12 hours, putting the round-bottom crucible into an 80 ℃ oven, drying for 12 hours, grinding the obtained sample, and uniformly putting the sample into a square crucible;

Fourthly, placing the square crucible in a muffle furnace, heating the square crucible to 550 ℃ from room temperature at a heating rate of 10 ℃/min in an air atmosphere, and roasting the square crucible for 2 hours at the temperature; cooling to room temperature to obtain the metallic nickel-based supported mesoporous catalyst.

2. The method for preparing the metal-supported mesoporous catalyst by using ethanol as a solvent according to claim 1, wherein the method comprises the following steps: the mesoporous inorganic material comprises Al-SBA-15 and Al-MCM-41 with the Si/Al molar ratio ranging from 10 to 360; the adding amount of the nickel nitrate can be adjusted according to the specific gravity of Ni species in the catalyst, and the specific gravity range of the Ni species in the catalyst is limited to 8-30%.

Technical Field

The invention relates to the field of preparation of metal-supported catalysts, in particular to a method for preparing a metal-supported mesoporous catalyst by taking ethanol as a solvent, wherein the ethanol is used for regulating and controlling the dispersion degree of metal species in the catalyst.

background

The metal supported catalyst has wide application in the field of catalysis, and particularly, the non-noble metal supported molecular sieve catalyst is more and more emphasized due to higher economy, stability and uniform pore structure. The distribution of metal species on the surface of the support directly affects the catalytic performance of the catalyst. When the metal-loaded catalyst is applied to catalytic reaction, the carrier has very important influence on the catalytic performance of the catalyst, such as influence on product distribution, yield, carbon deposition behavior of the catalyst and the like. Therefore, how to effectively regulate and control the dispersion degree of the metal species on the surface of the carrier becomes a hot point of research.

compared with microporous catalyst, the existence of mesopores in the catalyst is beneficial to overcoming diffusion limitation of reactants and intermediates so that the reactants and the intermediates are easy to adsorb and activate on metal active sites, thereby improving the catalytic activity. The mesoporous molecular sieve can accommodate reactants with large molecular size, and is an ideal catalyst carrier. The metal-loaded catalyst taking the mesoporous inorganic material as the carrier shows higher catalytic activity in the hydrodeoxygenation reaction of the bio-based phenolic compound. The impregnation method is to put the carrier into the liquid or gas containing active substance to make it adsorbed on the surface of the carrier gradually, and then to dry, roast and activate to obtain the needed catalyst.

however, in the existing method for preparing the supported mesoporous catalyst by the impregnation method, the metal species to be supported is mainly dissolved by using water as a solvent, and then the supported mesoporous catalyst is prepared and obtained by the impregnation method. In the process, the introduction of water can cause the change of the pore structure of the mesoporous inorganic material, thereby influencing the interaction between the metal species and the carrier and finally influencing the reaction result. How to find a suitable solvent to improve the dispersion degree of the metal species on the carrier and maintain the structure of the mesoporous inorganic material unchanged is a difficult problem to be solved urgently.

Disclosure of Invention

Aiming at the problems in the prior art, the invention provides a method for preparing a metal-loaded mesoporous catalyst by taking ethanol as a solvent, which is characterized in that from the control of a preparation process, a proper solvent is selected to dissolve metal species by researching the interaction between Ni species and the surface of a mesoporous molecular sieve, so that the metal-loaded catalyst with high metal species dispersion degree is obtained; the method has important significance for improving the catalytic performance of the metal-loaded catalyst and the wide application of the metal-loaded catalyst.

a method for preparing a metal-loaded mesoporous catalyst by using ethanol as a solvent comprises the following specific experimental steps:

Firstly, weighing 3 g of mesoporous inorganic material and placing the mesoporous inorganic material into a round bottom crucible;

and secondly, putting a certain amount of nickel nitrate hexahydrate into a glass beaker with the capacity of 25 mL, then transferring absolute ethyl alcohol with the volume equivalent to the pore volume of the mesoporous inorganic material into the glass beaker by using a liquid transfer gun, stirring the absolute ethyl alcohol by using a glass rod until the nickel nitrate is completely dissolved, and then sealing the opening of the beaker by using a sealing film to prevent the ethyl alcohol from volatilizing.

And thirdly, slowly and uniformly dripping the nickel nitrate-ethanol solution obtained in the second step into the mesoporous inorganic material in the first step by using a 5 mL disposable pipette, and stirring the mixture by using a glass rod until the mixture shows a uniform color after the dripping is finished. And then, taking a sealing film to seal the round-bottom crucible, standing at room temperature for 12 hours, then putting the round-bottom crucible into an oven with the temperature of 80 ℃, and drying for 12 hours. The obtained sample was ground and uniformly placed in a square crucible.

Fourthly, placing the square crucible in a muffle furnace, heating the square crucible to 550 ℃ from room temperature at a heating rate of 10 ℃/min in an air atmosphere, and roasting the square crucible for 2 hours at the temperature; cooling to room temperature to obtain the needed metal nickel-based supported mesoporous catalyst.

The mesoporous inorganic material comprises Al-SBA-15 and Al-MCM-41 with Si/Al ratio ranging from 10 to 360; the adding amount of the metal nickel nitrate can be adjusted according to the specific gravity of Ni species in the catalyst, and the specific gravity range of the Ni species in the catalyst is limited to 8-30%.

The solvent used for catalyst impregnation in the invention is ethanol, which has no pollution to the environment and low cost and can be applied to the production process of industrial catalysts. And the preparation process of the metal-loaded mesoporous catalyst is simple and the operability is strong. Compared with the traditional metal loaded mesoporous material catalyst, the method greatly improves the dispersion degree of metal species on the mesoporous material, and has important significance for improving the catalytic performance of the metal loaded catalyst and the wide application of the metal loaded catalyst.

Detailed Description

the present invention will be described in further detail with reference to specific examples.