A kind of so42-/tio2-c nanotube, preparation method and application thereof

A nanotube, tio2-c technology, applied in the field of nanotubes, can solve the problems of sulfate radical loss, activity attenuation, etc., and achieve the effects of not easy coking, active and simple and feasible preparation method.

Active Publication Date: 2019-06-25
SINOPEC YANGZI PETROCHEM +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, an unavoidable problem in the application of this type of catalyst is that the loss of sulfate radicals leads to the attenuation of activity. How to maintain the activity of this type of catalyst is an important issue for scientists.

Method used

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  • A kind of so42-/tio2-c nanotube, preparation method and application thereof
  • A kind of so42-/tio2-c nanotube, preparation method and application thereof
  • A kind of so42-/tio2-c nanotube, preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] TiO 2 Add 100 parts of powder to 500 parts of NaOH aqueous solution with a mass fraction of 10%, hydrothermally react at 120°C for 24 hours to obtain a hydrothermal product, filter and wash the product after hydrothermal reaction, and dry at 60°C for 5 hours to obtain a solid containing titanic acid . Take 100 parts of dried solids and mix them with 60 parts of glucose aqueous solution, stir, dry at 40°C, and dry under N 2 Calcined at 400°C in a mixed atmosphere with n-propanol to obtain TiO 2 -C nanotubes. will be on TiO 2 - 10 parts of C nanotubes are dispersed in 0.5 parts of 35% sulfuric acid aqueous solution, stirred, dried at 50°C, and roasted at 400°C to obtain SO 4 2- / TiO 2 -C nanotube A, measured in which TiO 2 The mass percentage is 95%, the carbon mass percentage is 3.9%, the sulfate radical mass percentage is 1.1%, and the carbon 98% is covered in TiO 2 The inner surface of the nanotube has an average diameter of 9.5nm.

Embodiment 2

[0036] TiO 2 Add 100 parts of powder to 400 parts of KOH aqueous solution with a mass fraction of 20%, hydrothermally react at 130°C for 48 hours to obtain a hydrothermal product, filter and wash the product after hydrothermal reaction, and dry at 70°C for 5 hours to obtain a solid containing titanic acid . Take 100 parts of dried solid and 80 parts of water-methanol solution of phenolic resin, mix, stir, dry at 50°C, and dry in N 2 Calcined at 420°C in a mixed atmosphere with n-butanol to obtain TiO 2 -C nanotubes. will be on TiO 2 - Disperse 10 parts of C nanotubes in 1 part of 35% sulfuric acid aqueous solution, stir, dry at 50°C, and roast at 450°C to obtain SO 4 2- / TiO 2 -C nanotube B, measured in which TiO 2 The mass percentage is 93%, the carbon mass percentage is 5.8%, the sulfate radical mass percentage is 1.2%, and the carbon 97.5% is covered in TiO 2 The inner surface of the nanotube has an average diameter of 9.0nm.

Embodiment 3

[0038] TiO 2 Add 100 parts of powder to 400 parts of KOH aqueous solution with a mass fraction of 20%, hydrothermally react at 100°C for 48 hours to obtain a hydrothermal product, filter and wash the product after hydrothermal reaction, and dry at 65°C for 5 hours to obtain a solid containing titanic acid . Take 100 parts of the dried solid and mix 90 parts of furfural in n-butanol solution, stir, dry at 50°C, and dry under N 2 Calcined at 380°C in a mixed atmosphere with isobutanol to obtain TiO 2 -C nanotubes. will be on TiO 2 - Disperse 10 parts of C nanotubes in 1 part of 50% sulfuric acid aqueous solution, stir, dry at 60°C, and roast at 500°C to obtain SO 4 2- / TiO 2 -C nanotube C, measured in which TiO 2 The mass percentage is 90%, the carbon mass percentage is 8.1%, the sulfate radical mass percentage is 1.9%, and the carbon 96.5% is covered in TiO 2 The inner surface of the nanotube has an average diameter of 6.3nm.

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Abstract

The invention relates to a SO42- / TiO2-C nanotube, and a preparation method and application thereof, belonging to the field of nanotubes. The SO42- / TiO2-C nanotube comprises TiO2 with the percentage mass content of 85 to 98%, carbon with the percentage mass content of 1 to 12%, and sulfate radical with the percentage mass content of 0.5 to 5.5%, wherein 93% to 98% of carbon in percentages by mass is covered on the inner surface of a TiO2 nanotube. The preparation method comprises the following steps: weighing TiO2 powder, then adding an alkali liquid with a concentration of 5% to 40%, and carrying out a hydrothermal reaction at 100 to 180 DEG C for 12 to 48 hours so as to obtain a hydrothermal product; carrying out filtering and washing, and carrying out drying at 40 to 85 DEG C so as to obtain a solid containing titanic acid; then carrying out contacting with an organic polymer so as to obtain a contact product; subjecting the contact product to calcination under inert gas entrained with organic alcohol so as to obtain a TiO2-C composite nanotube; and carrying out contacting with a sulfuric acid aqueous solution, carrying out drying, and carrying out calcination under inert gas so as to obtain a SO42- / TiO2-C nanotube catalyst. The catalyst is applied in reactions of esterification, hydrolysis and dehydration, and has good activity and long service life. The nanotube catalyst comprises mesoporous channels, and facilitates to diffusion of reactants and products; and the surface of the catalyst is not easy to coke.

Description

technical field [0001] The invention relates to a nanotube, in particular to a SO 4 2- / TiO 2 -C nanotubes and their preparation methods and applications. Background technique [0002] Since the discovery of carbon nanotubes by Japanese scientist Lijima in the 1990s, TiO as a semiconductor material 2 Nanotubes have attracted extensive attention from academia and industry due to their surface electron-rich structure. The focus of attention is mainly on the improvement of the preparation process and the surface functionalization to endow them with catalytic, adsorption and photoelectric properties (D.V.Bavykin, J.M. Friedrich, F.C.Walsh, Protonated Titanates and TiO 2 Nanostructured Materials: Synthesis, Properties, and Applications, 2006 Advanced Materials, Vol. 18, 2006, pp. 2807-2824). TiO 2 The preparation process of nanotubes mainly includes anodic oxidation electrochemical method, template method and hydrothermal synthesis under alkaline conditions. Among them, t...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J27/053C07C67/08C07C69/68C07C27/02C07C59/08C07C31/08C07C57/065C07C51/377
Inventor 刘经伟方晓江陈韶辉杨爱武李泽壮王英武刘丽娟
Owner SINOPEC YANGZI PETROCHEM
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