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N-doped TiO2-C material as well as preparation method and application thereof

A technology of nitrogen doping and tio2-c, which is applied in the preparation of amino compounds, chemical instruments and methods, and the preparation of organic compounds, etc., can solve the problems of harsh nitro reduction catalytic reaction conditions, low reserves of precious metal catalysts, and unfriendly environment , to achieve the effect of environmental friendliness, mild reaction conditions and simple steps

Active Publication Date: 2018-05-04
FUJIAN INST OF RES ON THE STRUCTURE OF MATTER CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of this application is to provide a nitrogen-doped TiO 2 -C material, which is used as a nitro reduction catalyst, can solve the disadvantages of harsh nitro reduction catalytic reaction conditions, unfriendly environment, low reserves and poor stability of precious metal catalysts in the prior art; the material can exist stably in water, It can efficiently catalyze the nitro reduction reaction under mild conditions (room temperature), so that the nitro reduction reaction can be carried out in a water-solvent system and under mild conditions. The catalyst has excellent cycle stability and is conducive to large-scale industrial production

Method used

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  • N-doped TiO2-C material as well as preparation method and application thereof
  • N-doped TiO2-C material as well as preparation method and application thereof
  • N-doped TiO2-C material as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0053] Example 1 Nitrogen-doped TiO 2 -C material sample preparation

[0054] Carbon Nitride C 3 N 4 Preparation of nanosheets:

[0055] Put 40 grams of urea in the crucible, start heating from room temperature, the heating rate is 10 ° C per minute, after rising to 500 ° C, keep warm for 2 hours under the air atmosphere, naturally cool down to room temperature, and obtain carbon nitride (C 3 N 4 )Nanosheets.

[0056] Nitrogen doped TiO 2 Preparation of -C material samples:

[0057] The C obtained in step (1) 3 N 4 Disperse in 100mL ethanol solution, add structure directing agent, and 0.45mL water, add titanium source under ice bath conditions, stir for a period of time under ice bath conditions, and then centrifugally dry to obtain TiO 2 -C 3 N 4 composite nanosheets.

[0058] (3) TiO obtained in step (2) 2 -C 3 N 4 After the composite nanosheets were calcined in a nitrogen atmosphere, the temperature was naturally lowered under the protection of nitrogen ...

Embodiment 2

[0062] Example 2 Sample 1 # ~Sample 6 # representation of

[0063] Sample 1 was analyzed by X-ray powder diffraction # ~Sample 6 # XRD characterization was carried out, and the results showed that sample 1 # ~Sample 6 # TiO in 2 Anatase crystal form and / or rutile crystal form, as sample 1 # It is a typical representative, and its XRD data are shown in Table 2:

[0064] Table 2

[0065] 2θ (°)

Relative peak intensity (%)

25.4

25.7

27.5

100

36.1

47.1

41.3

22.9

44.0

75.0

48.1

8.2

54.4

74.2

56.6

17.4

62.8

24.9

64.1

13.4

69.0

22.6

[0066] Sample 1 was examined by transmission electron microscopy # ~Sample 6 # was characterized to sample 1 # is a typical representative, and its transmission electron microscope pictures are as follows figure 1 As shown in (a), it can be seen from the figure that the obtained sample is a two-dimensional sheet structure with...

Embodiment 3

[0079] Example 3 Sample 1 # and sample D-2 # As a catalyst for the preparation of p-aminophenol from p-nitrophenol

[0080] First, dissolve 20mg of p-nitrophenol as a solid in 500mL of water, take 30mL of the above solution, and add sample 1 respectively # and sample D-2 # 10mg each as a catalyst, ultrasonically dispersed, then add 20mg sodium borohydride as a reducing agent, then the reaction system was stirred at room temperature, after 10 minutes of reaction, centrifuged to obtain the supernatant, which was the aqueous solution of p-aminophenol, and the bottom precipitate was the catalyst sample 1 # and sample D-2 # . Wash 3 times with deionized water and dry in an oven at 80°C before using again.

[0081] The reduction process of p-nitrophenol was tested by UV-Vis absorption spectrometer. Such as figure 2 shown in sample 1 # When used as a catalyst, the absorbance of p-nitrophenol decreased rapidly with time, while the concentration of p-aminophenol gradually inc...

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Abstract

The invention provides an N-doped TiO2-C material. Chemical composition of the material is (TiO2)xCyNz, wherein x represents the mass fraction of TiO2 per unit mass of the N-doped TiO2-C material, andx equals 0.10-0.80; y represents the mass fraction of C per unit mass of the N-doped TiO2-C material and y equals 0.08-0.35; z represents the mass fraction of N per unit mass of the N-doped TiO2-C material, and z equals 0.12-0.55. The material can exist stably in water and can efficiently catalyze the nitro reduction reaction under the mild condition (room temperature), so that the nitro reduction reaction can be performed in a system with water as a solvent under the mild condition, a catalyst has excellent cycling stability, and large-scale industrial production is facilitated.

Description

technical field [0001] The application relates to a nitrogen-doped TiO 2 The -C material, its preparation method and its application as a catalyst for nitro group reduction at room temperature belong to the field of nano catalytic materials. Background technique [0002] The hydrogenation reduction of nitro compounds is an important industrial reaction because the resulting amine compounds are important raw materials for many fine chemicals. Usually, the hydrogenation of nitro compounds requires the use of toxic reducing agents, organic solvents and harsh reaction conditions. Therefore, the catalytic nitro reduction process using water as a solvent has become an ideal technology to solve these disadvantages due to its green and non-polluting properties. However, it should be pointed out that currently the most researched system for catalytic hydrogenation of nitro compounds is mainly a homogeneous catalytic system based on ruthenium and rhodium. A significant disadvantage...

Claims

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Application Information

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IPC IPC(8): B01J27/24C07B43/04C07C209/36C07C211/51C07C211/47C07C213/02C07C215/76C07C217/84
CPCB01J27/24C07B43/04C07C209/36C07C213/02C07C211/51C07C211/47C07C215/76C07C217/84
Inventor 潘晓阳龙佩青易志国
Owner FUJIAN INST OF RES ON THE STRUCTURE OF MATTER CHINESE ACAD OF SCI
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