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Preparation method of graphene/TiO2 fiber

A graphene and fiber technology, applied in the field of graphene/TiO2 fiber composite material preparation, can solve the problems of large forbidden band width and carrier recombination probability, reduced contact area, catalyst loss, etc., and achieve excellent photocatalytic performance , reduce churn, the effect of simple process

Inactive Publication Date: 2013-05-22
SHANDONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] TiO 2 It is a relatively effective and commonly used photocatalyst, but it has the following disadvantages: poor adsorption to organic molecules, high band gap and high recombination probability of carriers, which severely limit the photocatalytic reaction.
[0003] However, graphene / TiO 2 Powder, when applied, forms a particle suspension system with liquid. It is very difficult to separate and recover the fine powder in the later stage of the reaction, and the loss of catalyst is serious, which limits its practical application.
At the same time, the surface area and volume ratio of the catalyst are greatly reduced, which seriously affects its catalytic activity.
And graphene on TiO 2 The surface attachment of nanotubes greatly reduces the contact area between the two, and the photooxidative performance is low, which is not suitable for photocatalytic reactions.
Graphene / TiO 2 Fiber is exactly a kind of graphene and TiO suitable for this demand 2 Combined application forms have not yet been reported

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] (1) Add 0.15g of graphene to 26.2mL of tetrahydrofuran, ultrasonically disperse for 30min, then add 1.11mL of ethyl acetoacetate as a chelating agent, measure 19.8mL of tetrabutyl titanate, and shake well to mix. in N 2 Heating to 82° C. under atmosphere for 1 h to obtain liquid A. Add 200.6 mL of tetrahydrofuran into the dropping funnel, then add 1.57 mL of deionized water, and shake well to prepare liquid B. After liquid A is cooled, under the action of magnetic stirring, liquid B is added dropwise into liquid A for reaction to obtain liquid C.

[0016] (2) Prepare spinning solution. N 2 In the atmosphere, liquid C was heated to reflux at 70° C. for 1 h to obtain a slurry-like solution. Transfer liquid C to a rotary evaporator, adjust the temperature of the water bath to 44°C, and concentrate the solution by evaporating the solvent to make the viscosity reach 5 Pa·s, and a transparent, uniform, and stable spinning solution can be obtained.

[0017] (3) spinning. ...

Embodiment 2

[0020] As described in Example 1, the difference is that the viscosity of the spinning solution in step (2) reaches 75 Pa·s, and the spinning method in step (3) is changed to dry spinning. Move the spinning solution into the liquid material tank in the dry spinning device, vacuum defoam for 15 minutes, and apply a pressure of 2.0 MPa to the spinning solution under the condition of a temperature of 25°C and a relative humidity of 40%, so that it can be removed from a hole diameter of 0.15 mm niobium-tantalum alloy spinning plate is sprayed out, drawn and collected by drum, and after the same temperature program, the final tensile strength is 90MPa ~ 1.0GPa, the diameter is 9μm ~ 20μm, and the BET specific surface area is 100m 2 / g~200m 2 / g, pore diameter 5nm~10nm, grain size 10nm~30nm, TiO 2 Graphene / TiO with anatase crystal phase 2 continuous fiber.

Embodiment 3

[0022] As described in Example 2, the difference is that the graphene in step (1) is changed to 0.20 g, and the heating program of 25°C to 450°C in step (4) is changed as follows: 25°C to 95°C heating rate 100 °C / h, 42min, and keep warm at 95°C for 24h; 350°C-450°C heating rate 300°C / h, 10min, and keep warm at 450°C for 1h; Natural cooling, tensile strength 90MPa ~ 1.0GPa, diameter 9μm ~ 20μm, continuous length of monofilament 5cm ~ 50cm, BET specific surface area 350m 2 / g, pore diameter 5nm~10nm, grain size 10nm~30nm, of which TiO 2 Graphene / TiO with anatase crystal phase 2 Porous continuous fibers.

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Abstract

The invention provides a preparation method of a graphene / TiO2 fiber composite material. The method comprises the following steps: ultrasonically dispersing different amounts of graphene into tetrahydrofuran; mxing with ethyl acetoacetate used a chelating agent and tetrabutyl titanate used as a titanium source to form a homogeneous graphene dispersion solution; magnetically stirring the dispersion solution and adding a proper amount of tetrahydrofuran and a small amount of deionized water and reacting; carrying out heating reflux to form a spinning solution; injecting the spinning solution into a spin throwing machine to carry out a spin throwing treatment so as to obtain a precursor fiber; placing the precursor fiber in a procedure heating furnace to carry out a procedure heating treatment at the temperature of 25 to 450 DEG C in a N2 atmosphere; naturally cooling naturally to obtain the graphene / TiO2 fiber. The graphene / TiO2 fiber has excellent photocatalytic performance and is suitable for the treatment of drinking water and the later-period deep treatment of sewage.

Description

1. Technical field [0001] The invention belongs to the field of functional fiber materials, in particular to a graphene / TiO that can be used as a photocatalyst 2 Process for the preparation of fiber composites. 2. Technical background [0002] TiO 2 It is a relatively effective and commonly used photocatalyst, but it has the following disadvantages: poor adsorption to organic molecules, high band gap and recombination probability of carriers, which severely limit the photocatalytic reaction. Graphene is a very good semiconductor thin film material. Its superior electron capture and transport capabilities, good photoelectric conversion performance, large specific surface area and strong adsorption affinity for organic molecules can well overcome TiO 2 lack of. The existing doping method is mainly TiO 2 Simple mix with graphene, mostly TiO 2 Powder with Graphene or TiO 2 Mixture of nanotubes and graphene. [0003] However, graphene / TiO 2 The powder forms a particle sus...

Claims

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Application Information

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IPC IPC(8): B01J21/18B01J35/06
Inventor 包南张清哲张成禄吴国林何随关瑾
Owner SHANDONG UNIV
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