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Composite nanofibers as well as preparation method and application thereof

A composite nanofiber, nanofiber technology, applied in chemical instruments and methods, refining with oxygenated compounds, organic compounds/hydrides/coordination complex catalysts, etc., can solve the problems of polyacid agglomeration, difficult separation and recovery, etc.

Active Publication Date: 2018-11-23
NORTHEAST NORMAL UNIVERSITY
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

[0005] The purpose of the present invention is to solve the problem that polyacid is difficult to separate and recycle as a homogeneous catalyst, and a large amount of agglomeration of polyacid is caused by loaded titanium dioxide nanomaterials, and to provide a composite nanofiber that realizes effective recycling and minimizes the sulfur content of fuel oil And its preparation method and application

Method used

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  • Composite nanofibers as well as preparation method and application thereof
  • Composite nanofibers as well as preparation method and application thereof
  • Composite nanofibers as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Example 1 (OTA) 10 [Co 4 (H 2 O) 2 (VW 9 o 34 ) 2 ] / TiO 2 Preparation of composite nanofibers

[0034] A (OTA) 10 [Co 4 (H 2 O) 2 (VW 9 o 34 ) 2 ] / TiO 2 Composite nanofiber synthesis steps are as follows:

[0035] (1) Na 10 [Co 4 (H 2 O) 2 (VW 9 o 34 ) 2 ] 35H 2 Synthesis of O:

[0036] 1.2g Co(NO 3 ) 2 ·6H 2 O and 6g Na 2 WO 4 2H 2 O was completely dissolved in 120mL 0.5M NaAC / HAC buffer solution (pH=4.8) under magnetic stirring, and then 0.27g NaVO 3 , the mixed solution was heated to 80°C and kept for 2h, and the hot filtered brown solid was vacuum-dried in a drying oven for 24h, and finally, Na 10 [Co 4 (H 2 O) 2 (VW 9 o 34 ) 2 ] 35H 2 O;

[0037] (2) TiO 2 Synthesis of Nanofibers:

[0038] 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 ...

Embodiment 21

[0043] Example 2 1 (OTA) 10 [Co 4 (H 2 O) 2 (VW 9 o 34 ) 2 ] / TiO 2 Preparation of composite nanofibers

[0044] A (OTA) 10 [Co 4 (H 2 O) 2 (VW 9 o 34 ) 2 ] / TiO 2 Composite nanofiber synthesis steps are as follows:

[0045] (1) Na 10 [Co 4 (H 2 O) 2 (VW 9 o 34 ) 2 ] 35H 2 Synthesis of O:

[0046] 1.2g Co(NO 3 ) 2 ·6H 2 O and 6g Na 2 WO 4 2H 2 O was completely dissolved in 120mL 0.5M NaAC / HAC buffer solution (pH=4.8) under magnetic stirring, and then 0.27g NaVO 3 , the mixed solution was heated to 75°C and kept for 2.5h, and the hot filtered brown solid was vacuum-dried in a drying oven for 30h, and finally, Na 10 [Co 4 (H 2 O) 2 (VW 9 o 34 ) 2 ] 35H 2 O;

[0047] (2) TiO 2 Synthesis of Nanofibers:

[0048] 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 ad...

Embodiment 3

[0053] Example 3 Extraction Catalytic Oxidative Desulfurization Experiment of Simulated Oil Containing Benzothiophene

[0054] Completely dissolve 0.10g of biphenyl and 0.21g of benzothiophene in 100mL of n-octane to obtain 100mL of simulated oil containing 500ppm benzothiophene; first, add 5mL of simulated oil to 25mL of Place the round bottom flask in a temperature-controlled water bath and activate it for 15 min; then, add 21 μL hydrogen peroxide, 1 mL ionic liquid [Bmim]PF to the above flask 6 and 0.01g of the composite nanofiber prepared in Example 1, magnetically stirred for 90min, and the upper oil sample was taken out every 10min for gas chromatography analysis. The results showed that adding 21 μL of H 2 0 2 , after 90 minutes of reaction, the catalytic efficiency of 0.01g of this catalyst at 50°C is 79%, see Figure 4 Shown; after the reaction finishes, the upper strata simulated oil product is dumped as much as possible, then with dichloromethane the residue in th...

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PUM

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Abstract

The invention discloses composite nanofibers, and the molecular formula of the composite nanofibers is (OTA)10[Co4(H2O)2(VW9O34)2] / TiO2. A preparation method of the composite nanofibers comprises thefollowing steps: (1) dissolving Co(NO3)2.6H2O and Na2WO4.2H2O in 0.5M NaAC / HAC buffer solution under the condition of magnetic stirring, then adding NaVO3, heating, carrying out hot filtration, and drying to obtain Na10[Co4(H2O)2(VW9O34)2].35H2O; (2) dissolving butyl titanate and polyvinylpyrrolidone in a mixed solvent of N, N-dimethylformamide, glacial acetic acid and acetylacetone, and using anelectrospinning method to obtain TiO2 nanofibers; (3) dispersing the TiO2 nanofibers in 30-50mL of ethanol, stirring, adding C18H37N(CH3)3.Cl, and continuously stirring to obtain a solution A; dissolving the Na10[Co4(H2O)2(VW9O34)2].35H2O in 20-40mL of water to obtain a solution B; slowly dropwise adding the solution B into the solution A, stirring for 20-30 hours, washing with water and ethanol,and drying under the vacuum condition to obtain the composite nanofibers. The composite nanofibers effectively solve the problem of polyacid agglomeration; the catalytic efficiency is not significantly reduced after 5 cycles of use; the composite nanofibers form an extraction catalytic oxidative desulfurization system together with hydrogen peroxide and ionic liquid [Bmim] PF6, thus showing higherdesulfurization efficiency and excellent reusability.

Description

technical field [0001] The invention belongs to the technical field of preparation of functional nanometer materials and catalytic desulfurization, and specifically relates to a composite nanofiber and its preparation method and application. Background technique [0002] A large number of sulfur compounds released by incomplete combustion of fuel oil seriously harm the ecological environment and human health, and it is an inevitable trend to reduce the sulfur content of fuel oil to the greatest extent. Due to the harsh operating conditions, high production costs and the disadvantages of difficult removal of heterocyclic sulfur-containing compounds, the application of hydrodesulfurization is limited. Therefore, various non-hydrogenation desulfurization processes are emerging, such as biological desulfurization, oxidative desulfurization and extraction catalytic oxidative desulfurization. Among them, a large number of studies have shown that extraction catalytic oxidation des...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/38B01J35/00B01J35/02B01J35/06C10G27/10
CPCC10G27/10B01J31/38C10G2300/202B01J35/40B01J35/58B01J35/39
Inventor 张宏付佳伟马雯雯
Owner NORTHEAST NORMAL UNIVERSITY
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