CN109847734A - A kind of preparation method of carbon fiber loaded titania nanotube composite material - Google Patents
A kind of preparation method of carbon fiber loaded titania nanotube composite material Download PDFInfo
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- CN109847734A CN109847734A CN201811453441.1A CN201811453441A CN109847734A CN 109847734 A CN109847734 A CN 109847734A CN 201811453441 A CN201811453441 A CN 201811453441A CN 109847734 A CN109847734 A CN 109847734A
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Abstract
The present invention relates to technical field of composite materials, more particularly to a kind of preparation method of carbon fiber loaded titania nanotube composite material, the method includes the following steps: the method includes the following steps: S1, carbon fiber being placed in solution of tetrabutyl titanate, dipping, it is dry, calcining, obtains carbon fiber/titanium dioxide seed layer；S2, carbon fiber/titanium dioxide seed layer, solution of tetrabutyl titanate, hydrogen chloride solution, acetone soln being mixed, heating, isothermal reaction is washed, and it is dry, obtain carbon fiber/titanium dioxide nano thread；S3, carbon fiber/titanium dioxide nano thread is mixed with sodium hydroxide solution, is heated up, insulation reaction immerses in hydrogen chloride solution, and washing to neutrality is dry, and calcining obtains carbon fiber loaded titania nanotube composite material.The invention also discloses the applications of the composite material.The present invention can be improved the photocatalytic degradation effect of carbon fiber loaded titania nanotube composite material.
Description
Technical field
The present invention relates to technical field of composite materials, and in particular to a kind of carbon fiber loaded titania nanotube composite wood
The preparation method of material.
Background technique
Photochemical catalyst of the titanium dioxide as most application potential has high-specific surface area, high catalytic activity, nontoxic and honest and clean
The advantages that valence, titanium dioxide optical catalyst obtain significant ground effect in terms of degrading waste water.However, practical application shows powdery two
Titania photocatalyst in wastewater treatment process there are easy to reunite, difficult separation and recycling the problems such as, thus to a certain extent
Constrain the industrialized development of titanium dioxide optical catalyst.
The main preparation method of nano-titanium dioxide includes anodizing, hydro-thermal method and template etc., usual nanometer two
Carrying method of the titanium oxide on carrier is by anodizing or template.Anodizing is usually in specific electricity
It solves in matter environment, in the method that metallic titanium surface prepares nano-titanium dioxide, this method has harsh requirement to carrier.Using
For template when preparing nano-titanium dioxide on carrier, the size and shape of nano-titanium dioxide are by template pattern and microstructure
Influence, and preparation process is relative complex, it is more difficult to realize and prepare nano-titanium dioxide in carrier surface.
Summary of the invention
Technical problems based on background technology, it is multiple that the invention proposes a kind of carbon fiber loaded titania nanotubes
The preparation method of condensation material compensates for the non-uniform defect of carbon fiber loaded titania nanotube in the prior art.
A kind of preparation method of carbon fiber loaded titania nanotube composite material proposed by the present invention, the method packet
Include following step:
S1, carbon fiber is placed in solution of tetrabutyl titanate, is impregnated, dry, it is brilliant to obtain carbon fiber/titanium dioxide for calcining
Kind layer；
S2, carbon fiber/titanium dioxide seed layer, solution of tetrabutyl titanate, hydrogen chloride solution, acetone soln are mixed, is risen
Temperature, isothermal reaction are washed, dry, obtain carbon fiber/titanium dioxide nano thread；
S3, carbon fiber/titanium dioxide nano thread is mixed with sodium hydroxide solution, is heated up, insulation reaction immerses hydrogen chloride
In solution, washing to neutrality is dry, and calcining obtains carbon fiber loaded titania nanotube composite material.
Preferably, it in S1, impregnates for ultrasonic immersing 0.5-1.5h.
Preferably, in S1, drying temperature is 70-90 DEG C, drying time 1.5-2.5h.
Preferably, in S1, calcining carries out in the atmosphere of inert gas, and calcination temperature is 400-500 DEG C, and calcination time is
0.5-1.5h。
Preferably, in S2, the reaction temperature of isothermal reaction is 160-200 DEG C, reaction time 0.5-2h.
Preferably, in S2, drying temperature is 70-90 DEG C, drying time 1.5-2.5h.
Preferably, in S2, solution of tetrabutyl titanate, hydrogen chloride solution, acetone soln volume ratio be 1-3:9-11:9-
11。
Preferably, in S3, the time immersed in hydrogen chloride solution is 22-26h.
Preferably, in S3, the reaction temperature of insulation reaction is 160-200 DEG C, reaction time 8-24h.
Preferably, in S3, drying temperature is 70-90 DEG C, drying time 1.5-2.5h.
Preferably, in S3, calcination temperature is 450-550 DEG C, calcination time 0.5-1.5h.
The present invention also provides a kind of applications of carbon fiber loaded titania nanotube composite material, by the carbon fiber
It ties up carried titanium dioxide nanometer tube composite materials and is applied to wastewater treatment.
The invention has the benefit that the present invention is using flexible non-metallic carbon fiber as carrier, using hydro-thermal method in carbon fiber
Dimension table face load nano-titanium dioxide, and alkali process is carried out to carbon fiber obtained in it/titanium dioxide nano thread, it can make to receive
Rice titanium dioxide is evenly distributed in carbon fiber surface, and then the light for improving carbon fiber loaded titania nanotube composite material is urged
Change degradation effect, and then overcome composite material in wastewater treatment process there are easy to reunite, difficult separation and recycling the problems such as, improve
Treatment effect of the composite material for waste water.
Detailed description of the invention
Fig. 1 is that carbon fiber/titanium dioxide seed layer, carbon fiber/titanium dioxide nano thread, carbon fiber that the present invention obtains are negative
The scanning electron microscope diagram of carrying of titanium dioxide nanometer tube composite materials.
Fig. 2 is the transmission electron microscope picture for the carbon fiber loaded titania nanotube composite material that the present invention obtains.
Fig. 3 is the energy spectrum diagram for the carbon fiber loaded titania nanotube composite material that the present invention obtains.
Fig. 4 is the X-ray diffractogram for the carbon fiber loaded titania nanotube composite material that the present invention obtains.
Fig. 5 is the photocatalytic degradation analysis chart for the carbon fiber loaded titania nanotube composite material that the present invention obtains.
Specific embodiment
In the following, technical solution of the present invention is described in detail by specific embodiment.
Embodiment 1
A kind of preparation method of carbon fiber loaded titania nanotube composite material, the method includes the following steps:
S1, the 0.1mol/L solution of tetrabutyl titanate of clean carbon fiber and 200ml is placed in 500ml beaker, is impregnated,
It is placed in a vacuum drying oven drying, is placed in high temperature process furnances and calcines, obtains carbon fiber/titanium dioxide seed layer (CFs/TiO2-
SL), scanning electron microscope diagram is referring to Fig. 1；
S2, by carbon fiber/titanium dioxide seed layer, solution of tetrabutyl titanate, the hydrogen chloride solution of 37wt%, acetone soln
It is placed in ptfe autoclave, heats up, isothermal reaction washs through dehydrated alcohol and deionized water, is placed in vacuum oven
Middle drying obtains carbon fiber/titanium dioxide nano thread (CFs/TiO2- NWs), scanning electron microscope diagram is referring to Fig. 1；
S3, the polytetrafluoro that the 10mol/L sodium hydroxide solution of carbon fiber/titanium dioxide nano thread and 18ml is placed in 25ml
In ethylene reaction kettle, heating, insulation reaction is immersed in the 1wt% hydrogen chloride solution of 100mL, is washed with deionized to neutrality,
It is placed in a vacuum drying oven drying, is placed in high temperature process furnances and calcines, obtains carbon fiber loaded titania nanotube composite wood
Expect (CFs/TiO2- NTs), referring to Fig.1, referring to fig. 2, energy spectrum diagram is referring to Fig. 3, X for transmission electron microscope picture for scanning electron microscope diagram
X ray diffration pattern x is referring to fig. 4；
Wherein, it in S1, impregnates for ultrasonic immersing 1h；
In S1, drying temperature is 80 DEG C, drying time 2h；
In S1, calcining carries out in the atmosphere of inert gas, and calcination temperature is 450 DEG C, calcination time 1h；
In S2, the reaction temperature of isothermal reaction is 180 DEG C, reaction time 1h；
In S2, drying temperature is 80 DEG C, drying time 2h；
In S2, solution of tetrabutyl titanate, hydrogen chloride solution, acetone soln volume ratio be 2:10:10；
In S3, the time immersed in hydrogen chloride solution is for 24 hours；
In S3, the reaction temperature of insulation reaction is 180 DEG C, reaction time 16h；
In S3, drying temperature is 80 DEG C, drying time 2h；
In S3, calcination temperature is 500 DEG C, calcination time 1h.
Embodiment 2
A kind of preparation method of carbon fiber loaded titania nanotube composite material, the method includes the following steps:
S1, the 0.1mol/L solution of tetrabutyl titanate of clean carbon fiber and 200ml is placed in 500ml beaker, is impregnated,
It is placed in a vacuum drying oven drying, is placed in high temperature process furnances and calcines, obtains carbon fiber/titanium dioxide seed layer；
S2, by carbon fiber/titanium dioxide seed layer, solution of tetrabutyl titanate, the hydrogen chloride solution of 37wt%, acetone soln
It is placed in ptfe autoclave, heats up, isothermal reaction washs through dehydrated alcohol and deionized water, is placed in vacuum oven
Middle drying obtains carbon fiber/titanium dioxide nano thread；
S3, the polytetrafluoro that the 10mol/L sodium hydroxide solution of carbon fiber/titanium dioxide nano thread and 18ml is placed in 25ml
In ethylene reaction kettle, heating, insulation reaction is immersed in the 1wt% hydrogen chloride solution of 100mL, is washed with deionized to neutrality,
It is placed in a vacuum drying oven drying, is placed in high temperature process furnances and calcines, obtains carbon fiber loaded titania nanotube composite wood
Material；
Wherein, it in S1, impregnates for ultrasonic immersing 0.5h；
In S1, drying temperature is 90 DEG C, drying time 1.5h；
In S1, calcining carries out in the atmosphere of inert gas, and calcination temperature is 500 DEG C, calcination time 0.5h；
In S2, the reaction temperature of isothermal reaction is 200 DEG C, reaction time 0.5h；
In S2, drying temperature is 90 DEG C, drying time 1.5h；
In S2, solution of tetrabutyl titanate, hydrogen chloride solution, acetone soln volume ratio be 3:9:11；
In S3, the time immersed in hydrogen chloride solution is 22h；
In S3, the reaction temperature of insulation reaction is 200 DEG C, reaction time 8h；
In S3, drying temperature is 90 DEG C, drying time 1.5h；
In S3, calcination temperature is 550 DEG C, calcination time 0.5h.
Embodiment 3
A kind of preparation method of carbon fiber loaded titania nanotube composite material, the method includes the following steps:
S1, the 0.1mol/L solution of tetrabutyl titanate of clean carbon fiber and 200ml is placed in 500ml beaker, is impregnated,
It is placed in a vacuum drying oven drying, is placed in high temperature process furnances and calcines, obtains carbon fiber/titanium dioxide seed layer；
S2, by carbon fiber/titanium dioxide seed layer, solution of tetrabutyl titanate, the hydrogen chloride solution of 37wt%, acetone soln
It is placed in ptfe autoclave, heats up, isothermal reaction washs through dehydrated alcohol and deionized water, is placed in vacuum oven
Middle drying obtains carbon fiber/titanium dioxide nano thread；
S3, the polytetrafluoro that the 10mol/L sodium hydroxide solution of carbon fiber/titanium dioxide nano thread and 18ml is placed in 25ml
In ethylene reaction kettle, heating, insulation reaction is immersed in the 1wt% hydrogen chloride solution of 100mL, is washed with deionized to neutrality,
It is placed in a vacuum drying oven drying, is placed in high temperature process furnances and calcines, obtains carbon fiber loaded titania nanotube composite wood
Material；
Wherein, it in S1, impregnates for ultrasonic immersing 1.5h；
In S1, drying temperature is 70 DEG C, drying time 2.5h；
In S1, calcining carries out in the atmosphere of inert gas, and calcination temperature is 400 DEG C, calcination time 1.5h；
In S2, the reaction temperature of isothermal reaction is 160 DEG C, reaction time 2h；
In S2, drying temperature is 70 DEG C, drying time 2.5h；
In S2, solution of tetrabutyl titanate, hydrogen chloride solution, acetone soln volume ratio be 1:11:9；
In S3, the time immersed in hydrogen chloride solution is 26h；
In S3, the reaction temperature of insulation reaction is 160 DEG C, and the reaction time is for 24 hours；
In S3, drying temperature is 70 DEG C, drying time 2.5h；
In S3, calcination temperature is 450 DEG C, calcination time 1.5h.
Test example 1
Photocatalytic degradation analysis is carried out to the carbon fiber loaded titania nanotube composite material that embodiment 1-3 is obtained,
Successively it is denoted as CFs/TiO2-NTs-1、CFs/TiO2-NTs-2、CFs/TiO2- NTs-3 analyzes result referring to Fig. 5.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
Anyone skilled in the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention and its
Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.
Claims (10)
1. a kind of preparation method of carbon fiber loaded titania nanotube composite material, which is characterized in that the method includes
Following step:
S1, carbon fiber is placed in solution of tetrabutyl titanate, is impregnated, dry, calcining obtains carbon fiber/titanium dioxide seed layer；
S2, carbon fiber/titanium dioxide seed layer, solution of tetrabutyl titanate, hydrogen chloride solution, acetone soln are mixed, heating is permanent
Temperature reaction, is washed, dry, obtains carbon fiber/titanium dioxide nano thread；
S3, carbon fiber/titanium dioxide nano thread is mixed with sodium hydroxide solution, is heated up, insulation reaction immerses hydrogen chloride solution
In, washing to neutrality is dry, and calcining obtains carbon fiber loaded titania nanotube composite material.
2. the preparation method of carbon fiber loaded titania nanotube composite material according to claim 1, which is characterized in that
In S1, impregnate for ultrasonic immersing 0.5-1.5h；Preferably, in S1, drying temperature is 70-90 DEG C, drying time 1.5-2.5h.
3. the preparation method of carbon fiber loaded titania nanotube composite material according to claim 1 or claim 2, feature exist
In in S1, calcining carries out in the atmosphere of inert gas, and calcination temperature is 400-500 DEG C, calcination time 0.5-1.5h.
4. the preparation method of any one of -3 carbon fiber loaded titania nanotube composite materials according to claim 1,
It is characterized in that, in S2, the reaction temperature of isothermal reaction is 160-200 DEG C, reaction time 0.5-2h.
5. the preparation method of any one of -4 carbon fiber loaded titania nanotube composite materials according to claim 1,
It is characterized in that, in S2, drying temperature is 70-90 DEG C, drying time 1.5-2.5h.
6. the preparation method of any one of -5 carbon fiber loaded titania nanotube composite materials according to claim 1,
Be characterized in that, in S2, solution of tetrabutyl titanate, hydrogen chloride solution, acetone soln volume ratio be 1-3:9-11:9-11.
7. the preparation method of any one of -6 carbon fiber loaded titania nanotube composite materials according to claim 1,
It is characterized in that, in S3, the time immersed in hydrogen chloride solution is 22-26h；Preferably, in S3, the reaction temperature of insulation reaction is
160-200 DEG C, reaction time 8-24h.
8. the preparation method of any one of -7 carbon fiber loaded titania nanotube composite materials according to claim 1,
It is characterized in that, in S3, drying temperature is 70-90 DEG C, drying time 1.5-2.5h.
9. the preparation method of any one of -8 carbon fiber loaded titania nanotube composite materials according to claim 1,
It is characterized in that, in S3, calcination temperature is 450-550 DEG C, calcination time 0.5-1.5h.
10. a kind of application of any one of -9 carbon fiber loaded titania nanotube composite materials according to claim 1,
It is characterized in that, the carbon fiber loaded titania nanotube composite material is applied to wastewater treatment.
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