Amphiphilic Lindqvist-type polyacid TiO2 composite nanofiber as well as preparation method and application thereof

A composite nanofiber and nanofiber technology, applied in chemical instruments and methods, refining with oxygen-containing compounds, organic compound/hydride/coordination complex catalyst, etc., can solve problems such as weak repeatability and multi-acid agglomeration

Active Publication Date: 2018-12-07
NORTHEAST NORMAL UNIVERSITY
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The purpose of the present invention is to solve the problem of weak reproducibility of multi-acid as a homogeneous catalyst, and a large amount of agglomeration of multi-acid caused by loaded titanium dioxide nanomate

Method used

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  • Amphiphilic Lindqvist-type polyacid TiO2 composite nanofiber as well as preparation method and application thereof
  • Amphiphilic Lindqvist-type polyacid TiO2 composite nanofiber as well as preparation method and application thereof
  • Amphiphilic Lindqvist-type polyacid TiO2 composite nanofiber as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Embodiment 1 (C 15 h 34 N) 2 (Mo 6 o 19 ) / TiO 2 Preparation of composite nanofibers

[0037] 1. (C 15 h 34 N) 2 (Mo 6 o 19 )Synthesis:

[0038] 2.50 g Na 2 MoO 6 2H 2 O (10.3 mmol) dissolved in 10~20 mL water, with 6mol L -1 HCl solution (2.5~3.0mL) was acidified, stirred vigorously for 1~5 min, added 2 mL of aqueous solution containing 1.16g (3.75 mmol) dodecyltrimethylammonium bromide, and heated the mixed solution to 75~80 °C, Heating for 40~50min, filtering the resulting precipitate and washing with ether 2~3 times, drying for 8~12h, to obtain (C 15 h 34 N) 2 (Mo 6 o 19 );

[0039] 2. TiO2 2 Synthesis of Nanofibers:

[0040] Using butyl titanate as a titanium source, it was completely dissolved in a mixed solvent formed by N,N-dimethylformamide, glacial acetic acid and acetylacetone, and then polyvinylpyrrolidone with a molecular weight of 1,300,000 was added as a template agent, using Electrospinning technology to get TiO 2 Nanofibers;

[0...

Embodiment 2

[0045] Example 2 Extraction Catalytic Oxidative Desulfurization Experiment of Simulated Oil Containing Dibenzothiophene

[0046] Completely dissolve 0.10g of biphenyl and 0.21g of dibenzothiophene in 100mL of n-octane to obtain 100mL of simulated oil containing 500ppm of dibenzothiophene; first, add 5 mL of simulated oil sample into a 25mL round bottom flask , keep the temperature in a water bath at 40-80 ℃ for 15 min; then, add 10.21-30.63 μL H 2 o 2 , 0.005-0.02g (C 15 h 34 N) 2 (Mo 6 o 19 ) / TiO 2 Composite nanofibers and 1 mL of ionic liquid [Bmim]PF 6 , magnetically stirred for 10-90min, and the upper oil sample was taken out every 10min for gas chromatography analysis, the results showed that: adding 11μL of H 2 o 2 , 0.01g at 60°C (C 15 h 34 N) 2 (Mo 6 o 19 ) / TiO 2 100% desulfurization efficiency can be achieved within 40 minutes, see the experimental results Figure 4 shown; after the reaction, the upper layer of simulated oil was dumped as much as possi...

Embodiment 3

[0047] Embodiment 3 (C 15 h 34 N) 2 (Mo 6 o 19 ) / TiO 2 Preparation of composite nanofibers

[0048] 1. (C 19 h 42 N) 2 (Mo 6 o 19 )Synthesis:

[0049] 2.50 g Na 2 MoO 6 2H 2 Dissolve O (10.3 mmol) in 10-20 mL of water, acidify with 2.5-3.0 mL of HCl solution, stir vigorously for 1-5 min, add 2 mL of cetyltrimethylammonium bromide containing 1.37 g (3.75 mmol) The aqueous solution, the mixed solution was heated to 75 ~ 80 ℃, heated for 40 ~ 50min, the resulting precipitate was filtered and washed with ether 2 ~ 3 times, dried for 8 ~ 12h, that is (C 19 h 42 N) 2 (Mo 6 o 19 );

[0050] 2. TiO2 2 Synthesis of Nanofibers:

[0051] Using butyl titanate as a titanium source, it was completely dissolved in a mixed solvent formed by N,N-dimethylformamide, glacial acetic acid and acetylacetone, and then polyvinylpyrrolidone with a molecular weight of 1,300,000 was added as a template agent, using Electrospinning technology to get TiO 2 Nanofibers;

[0052] 3. (C...

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Abstract

The invention discloses an amphiphilic Lindqvist-type polyacid TiO2 composite nanofiber. A preparation method of the nanofiber comprises the following steps: (1) under magnetic stirring, adding a cetyltrimethylammonium bromide water solution into a Na2MoO6.2H2O water solution acidized by hydrochloric acid, heating, filtering, washing with water and diethyl ether, and drying; (2) dissolving butyl titanate and polyvinylpyrrolidone into a mixed solvent of N,N-dimethylformamide, glacial acetic acid and diacetone, and preparing a TiO2 nanofiber by virtue of an electrostatic spinning method; and (3)dispersing the TiO2 nanofiber into ethanol, and stirring, so as to obtain a solution A, dissolving surfactant-packaged Lindqvist-type polyacid into ethanol, stirring to obtain a solution B, slowly dropwise adding the solution B into the solution A, stirring, washing with water and ethanol, and carrying out vacuum drying, so as to obtain the composite nanofiber. The preparation method is simple; the agglomeration problem of polyacid is effectively solved; the composite nanofiber is easy to separate and recycle; and an extraction catalytic oxidation desulfurization system is formed by hydrogenperoxide and ionic liquid [Bmim]PF6, so that the utilization rate of hydrogen peroxide is increased, the desulfurization efficiency is high, and the reusability is good.

Description

technical field [0001] The invention belongs to the technical field of preparation of functional nanomaterials and catalytic desulfurization, and in particular relates to an amphiphilic Lindqvist type polyacid TiO 2 Composite nanofibers and methods for their preparation and applications. Background technique [0002] The massive release of sulfide not only causes environmental problems such as acid rain, but also has adverse effects on human health and ecological balance. Therefore, ultra-deep desulfurization has become an urgent need. As a traditional desulfurization process, hydrodesulfurization is widely used in petroleum refining industry. Chinese patent CN 1488715A adopts hydrodesulfurization and dearomatization method to realize deep desulfurization of diesel oil. However, the harsh operating conditions and low removal efficiency of aromatic ring sulfides are the disadvantages of this system. Therefore, various non-hydrogenation desulfurization methods have been cont...

Claims

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Application Information

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IPC IPC(8): B01J31/38C10G27/12
CPCB01J31/38C10G27/12
Inventor 张宏付佳伟郭宇马雯雯
Owner NORTHEAST NORMAL UNIVERSITY
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