Crystallized mesoporous zinc silicate/silicon oxide composite powder and preparation method thereof

Abstract

The invention discloses crystallized mesoporous zinc silicate / silicon oxide composite powder and a preparation method thereof. The composite powder is of a two-dimensional hexagonal mesoporous structure and the mesoporous wall is composed of crystalline zinc silicate and amorphous silicon oxide. The preparation method comprises the following steps of firstly preparing mesoporous silicon oxide and dissolving the inorganic salt of zinc in ethanol to prepare a zinc salt solution; adding the mesoporous silicon oxide in the zinc salt solution according to compositions of the prepared powder, wherein the molar ratio of the mesoporous silicon oxide to the zinc salt is 2-25; uniformly dispersing the mesoporous silicon oxide into the zinc salt solution through fully stirring; and in the meantime, continuing stirring at room temperature, volatilizing the ethanol to obtain powder and obtaining the crystallized mesoporous zinc silicate / silicon oxide composite powder via vacuum drying and calcination. The preparation method is simple and convenient in operation; and the prepared mesoporous zinc silicate / silicon oxide composite powder is high in order degree, large in pore size and specific surface area, high in crystallinity and good in stability.

Description

technical field

[0001] The invention relates to inorganic nanometer materials, in particular to a crystallized zinc silicate / silicon oxide composite powder with ordered mesoporous structure and a preparation method thereof. Background technique

[0002] Mesoporous materials are a new type of self-assembled materials and belong to the new frontier of nanomaterials research. Mesoporous materials have excellent properties such as highly ordered pore structure, uniform pore size distribution, high specific surface area and porosity, and adjustable pore types. This provides favorable conditions for the adsorption, mass transfer, transport and reaction of substances, and has potential application prospects in many fields such as energy and environment, biotechnology, adsorption separation, catalysis, sensors, light, and electromagnetism, and is subject to the research of inorganic materials. extensive attention of the audience.

[0003] At present, the research focus of mesoporo...

Examples

Embodiment 1

[0020] Preparation of Mesoporous Silica

[0021] Prepare a mixed solution consisting of 15mL deionized water and 60mL 2mol / L hydrochloric acid, add 2g of triblock copolymer P123 to the above mixed solution, and fully stir at 37°C for 4 hours until P123 is completely dissolved. Then 4.25 g of tetraethyl orthosilicate was added to the above solution, and after stirring at 37° C. for 24 hours, the reactant was transferred to a reaction kettle with a volume of 100 mL, and hydrothermally treated at 100° C. for 24 hours. After filtering, washing with deionized water for 4 times, and drying at room temperature, a white powder was obtained. The powder was calcined at 550° C. for 6 hours with a heating rate of 1° C. / min to obtain a mesoporous silicon oxide powder.

[0022] Weigh 0.189g of zinc nitrate hexahydrate in a 25mL beaker, then add 4mL of ethanol, fully stir and dissolve to obtain zinc nitrate ethanol solution. Add 1 g of the prepared mesoporous silica powder into the zinc ni...

Embodiment 2

[0024] The preparation of mesoporous silica is the same as in Example 1.

[0025] Weigh 0.833g of zinc nitrate hexahydrate in a 25mL beaker, then add 6mL of ethanol, fully stir and dissolve to obtain zinc nitrate ethanol solution. Add 1 g of the prepared mesoporous silica powder into the zinc nitrate solution under stirring, stir and volatilize the ethanol solvent at room temperature to obtain a white powder, then dry the powder in vacuum at 50°C for 8 hours, and then calcinate at 800°C for 4 hour, the heating rate is 1° C. / min, and the crystallized mesoporous zinc silicate / silicon oxide composite powder is obtained, and the molar ratio of silicon oxide to zinc silicate in the powder is 11. figure 2 It is the wide-angle X-ray diffraction pattern of the prepared crystalline mesoporous zinc silicate / silicon oxide composite powder.

Embodiment 3

[0027] The preparation of mesoporous silica is the same as in Example 1.

[0028] Weigh 1.963g of zinc nitrate hexahydrate in a 25mL beaker, then add 8mL of ethanol, fully stir and dissolve to obtain zinc nitrate ethanol solution. Add 1 g of the prepared mesoporous silica powder into the zinc nitrate solution under stirring, stir and volatilize the ethanol solvent at room temperature to obtain a white powder, then dry the powder in vacuum at 50°C for 8 hours, and then calcinate at 800°C for 4 hour, the heating rate is 1° C. / min, and the crystallized mesoporous zinc silicate / silicon oxide composite powder is obtained, and the molar ratio of silicon oxide and zinc silicate in the powder is 4. image 3 It is a transmission electron micrograph of the prepared crystalline mesoporous zinc silicate / silicon oxide composite powder. Figure 4 Nitrogen adsorption and desorption spectra of the prepared crystalline mesoporous zinc silicate / silicon oxide composite powder.

technical field

[0001] The invention relates to inorganic nanometer materials, in particular to a crystallized zinc silicate / silicon oxide composite powder with ordered mesoporous structure and a preparation method thereof. Background technique

[0002] Mesoporous materials are a new type of self-assembled materials and belong to the new frontier of nanomaterials research. Mesoporous materials have excellent properties such as highly ordered pore structure, uniform pore size distribution, high specific surface area and porosity, and adjustable pore types. This provides favorable conditions for the adsorption, mass transfer, transport and reaction of substances, and has potential application prospects in many fields such as energy and environment, biotechnology, adsorption separation, catalysis, sensors, light, and electromagnetism, and is subject to the research of inorganic materials. extensive attention of the audience.

[0003] At present, the research focus of mesoporo...

Examples

Embodiment 1

[0020] Preparation of Mesoporous Silica

[0021] Prepare a mixed solution consisting of 15mL deionized water and 60mL 2mol / L hydrochloric acid, add 2g of triblock copolymer P123 to the above mixed solution, and fully stir at 37°C for 4 hours until P123 is completely dissolved. Then 4.25 g of tetraethyl orthosilicate was added to the above solution, and after stirring at 37° C. for 24 hours, the reactant was transferred to a reaction kettle with a volume of 100 mL, and hydrothermally treated at 100° C. for 24 hours. After filtering, washing with deionized water for 4 times, and drying at room temperature, a white powder was obtained. The powder was calcined at 550° C. for 6 hours with a heating rate of 1° C. / min to obtain a mesoporous silicon oxide powder.

[0022] Weigh 0.189g of zinc nitrate hexahydrate in a 25mL beaker, then add 4mL of ethanol, fully stir and dissolve to obtain zinc nitrate ethanol solution. Add 1 g of the prepared mesoporous silica powder into the zinc ni...

Embodiment 2

[0024] The preparation of mesoporous silica is the same as in Example 1.

[0025] Weigh 0.833g of zinc nitrate hexahydrate in a 25mL beaker, then add 6mL of ethanol, fully stir and dissolve to obtain zinc nitrate ethanol solution. Add 1 g of the prepared mesoporous silica powder into the zinc nitrate solution under stirring, stir and volatilize the ethanol solvent at room temperature to obtain a white powder, then dry the powder in vacuum at 50°C for 8 hours, and then calcinate at 800°C for 4 hour, the heating rate is 1° C. / min, and the crystallized mesoporous zinc silicate / silicon oxide composite powder is obtained, and the molar ratio of silicon oxide to zinc silicate in the powder is 11. figure 2 It is the wide-angle X-ray diffraction pattern of the prepared crystalline mesoporous zinc silicate / silicon oxide composite powder.

Embodiment 3

[0027] The preparation of mesoporous silica is the same as in Example 1.

[0028] Weigh 1.963g of zinc nitrate hexahydrate in a 25mL beaker, then add 8mL of ethanol, fully stir and dissolve to obtain zinc nitrate ethanol solution. Add 1 g of the prepared mesoporous silica powder into the zinc nitrate solution under stirring, stir and volatilize the ethanol solvent at room temperature to obtain a white powder, then dry the powder in vacuum at 50°C for 8 hours, and then calcinate at 800°C for 4 hour, the heating rate is 1° C. / min, and the crystallized mesoporous zinc silicate / silicon oxide composite powder is obtained, and the molar ratio of silicon oxide and zinc silicate in the powder is 4. image 3 It is a transmission electron micrograph of the prepared crystalline mesoporous zinc silicate / silicon oxide composite powder. Figure 4 Nitrogen adsorption and desorption spectra of the prepared crystalline mesoporous zinc silicate / silicon oxide composite powder.

Images