阅读说明：本技术 一种快速制备介孔二氧化硅球的方法及介孔二氧化硅球 (Method for rapidly preparing mesoporous silica spheres and mesoporous silica spheres ) 是由 朱坤磊 刘西成 景志红 于 2019-07-11 设计创作，主要内容包括：本发明公开一种快速制备介孔二氧化硅球的方法,包括如下步骤：1)将0.2-2.0g表面活性剂加至100mL溶剂中,溶解；2)加入0.5-5.0mL浓氨水、0.5-5.0mL硅盐及50mL蒸馏水,搅拌均匀后得到反应液；3)将反应液移至200mL反应釜中,在100-220摄氏度下溶剂热反应0.5-8小时；4)反应结束后,将釜自然冷却至室温,通过离心将所得产物分离,并用乙醇洗涤,得沉淀,自然烘干；5)之后将沉淀转移至马弗炉中,在空气中高温锻烧,即得介孔SiO<Sub>2</Sub>球。还公开了介孔二氧化硅球直径大小为0.5-4.0μm,比表面积为50-500m<Sup>2</Sup>g<Sup>-1</Sup>,孔径大小为2-25nm。(The invention discloses a method for rapidly preparing mesoporous silica spheres, which comprises the following steps: 1) adding 0.2-2.0g of surfactant into 100mL of solvent for dissolving; 2) adding 0.5-5.0mL of concentrated ammonia water, 0.5-5.0mL of silicate and 50mL of distilled water, and uniformly stirring to obtain a reaction solution; 3) transferring the reaction liquid to a 200mL reaction kettle, and carrying out solvothermal reaction for 0.5-8 hours at the temperature of 100-220 ℃; 4) after the reaction is finished, naturally cooling the kettle to room temperature, separating the obtained product through centrifugation, washing the product with ethanol to obtain a precipitate, and naturally drying the precipitate; 5) then transferring the precipitate into a muffle furnace, and calcining at high temperature in the air to obtain the mesoporous SiO 2 A ball. Also discloses mesoporous silica spheres with the diameter of 0.5-4.0 mu m and the specific surface area of 50-500m 2 g ‑1 The pore size is 2-25 nm.)

1. A method for rapidly preparing mesoporous silica spheres is characterized by comprising the following steps:

1) adding 0.2-2.0g of surfactant into 100mL of solvent for dissolving;

2) adding 0.5-5.0mL of concentrated ammonia water, 0.5-5.0mL of silicate and 50mL of distilled water, and uniformly stirring to obtain a reaction solution;

3) transferring the reaction liquid to a 200mL reaction kettle, and carrying out solvothermal reaction for 0.5-8 hours at the temperature of 100-220 ℃;

4) after the reaction is finished, naturally cooling the kettle to room temperature, separating the obtained product through centrifugation, washing the product with ethanol to obtain a precipitate, and naturally drying the precipitate;

5) then transferring the precipitate into a muffle furnace, and calcining at high temperature in the air to obtain the mesoporous SiO₂A ball.

2. The method for rapidly preparing mesoporous silica spheres according to claim 1, wherein the surfactant in the step 1) is preferably any one of dodecylamine, tetradecylamine, hexadecylamine or octadecylamine.

3. The method for rapidly preparing mesoporous silica spheres as claimed in claim 1, wherein the solvent in step 1) is preferably one or more of methanol, ethanol, isopropanol, n-propanol and n-butanol.

4. The method for rapidly preparing mesoporous silica spheres as claimed in claim 1, wherein the silicon salt in step 2) is preferably any one of ethyl orthosilicate, ethyl orthosilicate isopropyl ester or ethyl orthosilicate butyl ester.

5. The method for rapidly preparing mesoporous silica spheres according to any one of claims 1 to 4, wherein the mesoporous silica spheres have a diameter of 0.5 to 4.0 μm and a specific surface area of 50 to 500m²g^-1The pore size is 2-25 nm.

Technical Field

The invention relates to the technical field of preparation in the field of inorganic functional materials, in particular to a method for quickly preparing mesoporous silicon dioxide.

Background

MCM-41 mesoporous molecular sieve was first prepared since 1992 [1]. The mesoporous material can be applied to various fields such as energy storage and conversion, catalysis, biomedicine, sensors and the like [2-5 ]]And attract the attention of people. However, in the previous reports, the preparation of mesoporous materials takes a long time, such as 12 hours of stirring and 8 hours of reaction [6 ]]Standing for 24 hours and hydrothermal reaction for 4 hoursTime [7 ]]Standing for 20 hours and aging for 40 hours [8 ]]And stirred for 24 hours and sonicated for 4 hours [9]. This will greatly reduce the preparation efficiency of the mesoporous material and increase the production time cost. The invention adopts a one-step hydrothermal method to rapidly prepare mesoporous SiO₂The reaction time required by the mesoporous spheres is only 2 hours, and the method is simple, quick and effective and is hopefully amplified to large-scale production.

[1]C.T.Kresge,M.E.Leonowicz,W.J.Roth,J.C.Vartuli and J.S.Beck,Nature,1992,359:710-712.

[2]W.Li,J.Liu and D.Zhao,Nature Reviews Materials,2016,1:16023.

[3]J.Liang,Z.Liang,R.Zou and Y.Zhao,Advanced Materials,2017,29:1701139.

[4]J.Wang,Q.Ma,Y.Wang,Z.Li,Z.Li and Q.Yuan,Chemical Society Reviews,2018,47:8766-8803.

[5]W.Luo,T.Zhao,Y.Li,J.Wei,P.Xu,X.Li,Y.Wang,W.Zhang,A.A.Elzatahry,A.Alghamdi,Y.Deng,L.Wang,W.Jiang,Y.Liu,B.Kong and D.Zhao,Journal of theAmerican Chemical Society,2016,138:12586-12595.

[6]X.Wang,Y.Zhang,W.Luo,A.A.Elzatahry,X.Cheng,A.Alghamdi,A.M.Abdullah,Y.Deng and D.Zhao,Chemistry of Materials,2016,28:2356-2362.

[7]H.Zhang and S.Liu,Materials Letters,2018,221:119-122.

[8]M.Jahandar Lashaki and A.Sayari,Chemical Engineering Journal,2018,334:1260-1269.

[9]S.-D.Jiang,G.Tang,Z.Bai and Y.Pan,Materials Letters,2019,247:139-142.

Disclosure of Invention

The invention aims to overcome the defects of the prior art and provide a method for quickly preparing mesoporous SiO₂A method for preparing the mesoporous silica spheres and mesoporous silica spheres.

The invention is realized by the following technical scheme: a method for rapidly preparing mesoporous silica spheres comprises the following steps:

1) adding 0.2-2.0g of surfactant into 100mL of solvent for dissolving;

2) adding 0.5-5.0mL of concentrated ammonia water, 0.5-5.0mL of silicate and 50mL of distilled water, and uniformly stirring to obtain a reaction solution;

3) transferring the reaction liquid to a 200mL reaction kettle, and carrying out solvothermal reaction for 0.5-8 hours at the temperature of 100-220 ℃;

4) after the reaction is finished, naturally cooling the kettle to room temperature, separating the obtained product through centrifugation, washing the product with ethanol to obtain a precipitate, and naturally drying the precipitate;

5) then transferring the precipitate into a muffle furnace, and calcining at high temperature in the air to obtain the mesoporous SiO₂A ball.

Preferably, the surfactant in step 1) is any one of dodecylamine, tetradecylamine, hexadecylamine and octadecylamine.

Preferably, the solvent in the step 1) is one or a mixture of methanol, ethanol, isopropanol, n-propanol or n-butanol.

Preferably, the silicon salt in step 2) is any one of ethyl orthosilicate, ethyl orthosilicate isopropyl ester or ethyl orthosilicate butyl ester.

The second technical scheme of the invention is to adopt the method to rapidly prepare the mesoporous silica spheres, the diameter of the mesoporous silica spheres is 0.5-4.0 mu m, and the specific surface area is 50-500m²g^-1The pore size is 2-25 nm.

Advantageous effects

The invention has the beneficial effect that the mesoporous SiO is rapidly prepared by the one-step solvothermal method₂Balls, not only SiO prepared₂The ball has uniform size, large specific surface and rich pore diameter, and more importantly, the preparation time is greatly shortened.

Drawings

FIG. 1 shows mesoporous SiO₂Scanning electron microscope pictures of the ball.

FIG. 2 shows mesoporous SiO₂Transmission electron microscopy of the ball.

FIG. 3 is a diagram of mesoporous SiO₂X-ray diffraction pattern of spheres: (a) wide angle, (b) small angle.

FIG. 4 shows mesoporous SiO₂Ball characteristic curve: (a) a nitrogen adsorption and desorption curve and (b) a pore size distribution curve.

(example 4)

Detailed Description

The invention is further described below with reference to the following figures and specific examples. It is to be understood that the embodiments discussed herein are for illustrative purposes only and that modifications or changes in light thereof will be suggested to persons skilled in the art and are to be included within the purview of the appended claims.