A kind of silver titanium dioxide-metal organic framework structure composite material and its preparation method and application

A metal-organic framework, titanium dioxide technology, applied in chemical instruments and methods, organic compound/hydride/coordination complex catalysts, nitrogen preparation, etc., can solve the problems of low efficiency and low nitrogen selectivity

Inactive Publication Date: 2019-08-23
NORTHEAST NORMAL UNIVERSITY
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, its efficiency in catalytic reduction of nitrate is low, and its nitrogen selectivity is not high, and further improvement is needed
Existing Ag / TiO 2 Binary photocatalyst, which is used for the degradation of nitrate, realizes the high-efficiency reduction of nitrate, but there is still room for further improvement in the reduction rate of nitrate and nitrogen selectivity
(Zhang F, Jin R, Chen J, et al. High photocatalytic activity and selectivity for nitrogen in nitratereduction onAg / TiO 2 ,catalyst with fine silver clusters[J].Journal ofCatalysis,2005,232(2):424-431.) Metal-organic frameworks (MOFs) have the advantages of large specific surface area, regular pore structure, and strong modification. The field of homogeneous catalytic reactions has received extensive attention, but the use of MOFs to prepare silver titania-metal organic framework composites and its application in the photocatalytic reduction of nitrate to nitrogen has not been reported yet.

Method used

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  • A kind of silver titanium dioxide-metal organic framework structure composite material and its preparation method and application
  • A kind of silver titanium dioxide-metal organic framework structure composite material and its preparation method and application
  • A kind of silver titanium dioxide-metal organic framework structure composite material and its preparation method and application

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preparation example Construction

[0026] The present invention also provides a preparation method of silver titanium dioxide-metal organic framework structure composite material, comprising:

[0027] Step 1: Mix and stir tetraisobutyl titanate, AgMIL-101(Cr), and silver nitrate in an alcohol solvent to obtain a mixed solution;

[0028] Step 2: Put the mixed solution obtained in Step 1 into the reaction kettle, -1 The rate is raised from room temperature to 130-150°C, and kept for 8-12h to obtain a mixture;

[0029] Step 3: Centrifuge, wash and dry the mixture obtained in Step 2 to obtain a silver titanium dioxide-metal organic framework composite material.

[0030] According to the present invention, add tetraisobutyl titanate and AgMIL-101 (Cr) into the alcohol solvent and stir, add silver denitrate and ionized water, stir at a low speed until the solution becomes gelatinous, and obtain a mixed solution; the raw materials are added The sequence is preferably: first add alcohol solvent, then add tetraisobuty...

Embodiment 1

[0042] Add 0.5mL of tetraisobutyl titanate to 25mL of isopropanol, and start stirring at a stirring rate of 150 rpm. During stirring, first add 0.27g of AgMIL-101 (Cr), then add 0.086g, 0.172 g, 0.43g of silver nitrate, and finally add 0.6mL of deionized water, and continue to stir for 4-8h until the mixed solution is called a green gel. Afterwards, the mixture was transferred into a polytetrafluoroethylene-lined reactor and placed in a temperature-programmed oven at 2 °C min -1 The temperature was raised from room temperature to 130°C and kept for 12h, the cooled mixture was taken out, the powder was collected by centrifugation, the obtained powder was washed twice with deionized water, and dried at 80°C for 12h to obtain the silver content of the total catalyst. 1%, 2%, 5% silver titanium dioxide-metal organic framework composites by mass.

[0043] The 5wt%Ag / TiO that embodiment 1 obtains 2 / AgMIL-101 (Cr) surface physical and chemical properties are: average pore diameter...

Embodiment 2

[0045] Add 1 mL of tetraisobutyl titanate to 25 mL of isopropanol, start stirring at a stirring rate of 150 rpm, add 0.54 g of AgMIL-101 (Cr) first, and then add 0.43 g of silver nitrate , and finally add 1mL of deionized water, and continue to stir for 4-8h until the mixed solution is called a green gel. Afterwards, the mixture was transferred into a polytetrafluoroethylene-lined reactor, placed in a temperature-programmed oven, and heated at 2 °C min -1 The temperature was raised from room temperature to 140°C and kept for 10h, the cooled mixture was taken out, the powder was collected by centrifugation, the obtained powder was washed twice with deionized water, and dried at 80°C for 12h to obtain silver titanium dioxide-metal organic framework Structural composites.

[0046] The Ag / TiO that embodiment 2 obtains 2 / AgMIL-101 (Cr) surface physical and chemical properties are: average pore diameter: 3.67nm; BET specific surface area: 346.54m 2 g -1 ;Total pore volume: 0.31...

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Abstract

The invention provides a silver titanium dioxide-metal organic frame structure composite material as well as a preparation method and application thereof and belongs to the field of composite materials. The chemical formula of the composite material is: Ag / TiO2 / AgMIL-101 (Cr). The invention further provides a preparation method of the silver titanium dioxide-metal organic frame structure composite material. The preparation method comprises the following steps: firstly, mixing and stirring titanium tetraisobutanolate, AgMIL-101(Cr) and silver nitrate in an alcohol solvent so as to obtain a mixed solution; putting the mixed solution into a reaction kettle, heating to 130-150 DEG C from the room temperature at a speed of 2 DEG C / minute, and keeping the temperature for 8-12 hours so as to obtain a mixture; finally centrifuging the mixture, washing, and drying, thereby obtaining the silver titanium dioxide-metal organic frame structure composite material. The invention further provides application of the silver titanium dioxide-metal organic frame structure composite material as a photocatalyst which is capable of reducing nitrate into nitrogen in an efficient and high selectivity manner.

Description

technical field [0001] The invention belongs to the field of composite materials, and in particular relates to a silver titanium dioxide-metal organic frame structure composite material and a preparation method and application thereof. Background technique [0002] With the development and utilization of resources, groundwater nitrate pollution is becoming more and more serious. The traditional nitrate treatment technology cannot meet the current needs, and there is an urgent need for a treatment technology for efficient conversion of nitrate and high nitrogen selectivity. The photocatalytic technology using solar energy is expected to provide a sustainable solution for the treatment of nitrate pollution in groundwater. [0003] The core of photocatalytic treatment of nitrate in water is to develop a photocatalyst with high degradation efficiency and high nitrogen selectivity. Titanium dioxide has attracted the attention of scientific and technological workers from all ove...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/38C01B21/02
CPCC01B21/02B01J31/38B01J35/61B01J35/39
Inventor 杨霞马国强王昭华耿直李相辰李朝阳齐新
Owner NORTHEAST NORMAL UNIVERSITY
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