CN109331805A - A kind of preparation method of carbon fiber loaded nano titanium dioxide photocatalysis composite material - Google Patents
A kind of preparation method of carbon fiber loaded nano titanium dioxide photocatalysis composite material Download PDFInfo
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- CN109331805A CN109331805A CN201811361011.7A CN201811361011A CN109331805A CN 109331805 A CN109331805 A CN 109331805A CN 201811361011 A CN201811361011 A CN 201811361011A CN 109331805 A CN109331805 A CN 109331805A
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- titanium dioxide
- carbon fiber
- coupling agent
- composite material
- containing vinyl
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- 229920000049 Carbon (fiber) Polymers 0.000 title claims abstract description 59
- 239000004917 carbon fiber Substances 0.000 title claims abstract description 59
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 title claims abstract description 49
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims abstract description 47
- 239000002131 composite material Substances 0.000 title claims abstract description 24
- 230000001699 photocatalysis Effects 0.000 title claims abstract description 24
- 238000007146 photocatalysis Methods 0.000 title claims abstract description 21
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 229920002554 vinyl polymer Polymers 0.000 claims abstract description 35
- -1 vinyl silicane Chemical compound 0.000 claims abstract description 34
- 239000007822 coupling agent Substances 0.000 claims abstract description 30
- 238000006243 chemical reaction Methods 0.000 claims abstract description 19
- 238000000034 method Methods 0.000 claims abstract description 18
- 230000008569 process Effects 0.000 claims abstract description 13
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims abstract description 12
- 230000003647 oxidation Effects 0.000 claims abstract description 12
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 12
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims abstract description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 41
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 30
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 30
- 235000019441 ethanol Nutrition 0.000 claims description 21
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 19
- 239000011259 mixed solution Substances 0.000 claims description 19
- 239000003921 oil Substances 0.000 claims description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- 239000000047 product Substances 0.000 claims description 14
- 239000000243 solution Substances 0.000 claims description 14
- 239000008367 deionised water Substances 0.000 claims description 13
- 229910021641 deionized water Inorganic materials 0.000 claims description 13
- 238000002525 ultrasonication Methods 0.000 claims description 13
- LCGLNKUTAGEVQW-UHFFFAOYSA-N Dimethyl ether Chemical compound COC LCGLNKUTAGEVQW-UHFFFAOYSA-N 0.000 claims description 6
- 244000028419 Styrax benzoin Species 0.000 claims description 6
- 235000000126 Styrax benzoin Nutrition 0.000 claims description 6
- ISAOCJYIOMOJEB-UHFFFAOYSA-N benzoin Chemical compound C=1C=CC=CC=1C(O)C(=O)C1=CC=CC=C1 ISAOCJYIOMOJEB-UHFFFAOYSA-N 0.000 claims description 6
- DURPTKYDGMDSBL-UHFFFAOYSA-N 1-butoxybutane Chemical compound CCCCOCCCC DURPTKYDGMDSBL-UHFFFAOYSA-N 0.000 claims description 3
- BWGNESOTFCXPMA-UHFFFAOYSA-N Dihydrogen disulfide Chemical compound SS BWGNESOTFCXPMA-UHFFFAOYSA-N 0.000 claims description 3
- 235000015511 Liquidambar orientalis Nutrition 0.000 claims description 3
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 3
- 239000004870 Styrax Substances 0.000 claims description 3
- 235000008411 Sumatra benzointree Nutrition 0.000 claims description 3
- 229960002130 benzoin Drugs 0.000 claims description 3
- RWCCWEUUXYIKHB-UHFFFAOYSA-N benzophenone Chemical compound C=1C=CC=CC=1C(=O)C1=CC=CC=C1 RWCCWEUUXYIKHB-UHFFFAOYSA-N 0.000 claims description 3
- 239000012965 benzophenone Substances 0.000 claims description 3
- HRKQOINLCJTGBK-UHFFFAOYSA-N dihydroxidosulfur Chemical compound OSO HRKQOINLCJTGBK-UHFFFAOYSA-N 0.000 claims description 3
- 235000019382 gum benzoic Nutrition 0.000 claims description 3
- OFBQJSOFQDEBGM-UHFFFAOYSA-N n-pentane Natural products CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 claims description 3
- 229910000077 silane Inorganic materials 0.000 claims description 3
- 229960002317 succinimide Drugs 0.000 claims description 3
- AGUIILSGLFUTKG-UHFFFAOYSA-N CC(C)O.CC(C)O.CC(C)O.C=C[SiH3] Chemical compound CC(C)O.CC(C)O.CC(C)O.C=C[SiH3] AGUIILSGLFUTKG-UHFFFAOYSA-N 0.000 claims description 2
- 150000001335 aliphatic alkanes Chemical class 0.000 claims description 2
- NKSJNEHGWDZZQF-UHFFFAOYSA-N ethenyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)C=C NKSJNEHGWDZZQF-UHFFFAOYSA-N 0.000 claims description 2
- MBGQQKKTDDNCSG-UHFFFAOYSA-N ethenyl-diethoxy-methylsilane Chemical compound CCO[Si](C)(C=C)OCC MBGQQKKTDDNCSG-UHFFFAOYSA-N 0.000 claims description 2
- UKRDPEFKFJNXQM-UHFFFAOYSA-N vinylsilane Chemical class [SiH3]C=C UKRDPEFKFJNXQM-UHFFFAOYSA-N 0.000 claims 2
- XDLMVUHYZWKMMD-UHFFFAOYSA-N 3-trimethoxysilylpropyl 2-methylprop-2-enoate Chemical compound CO[Si](OC)(OC)CCCOC(=O)C(C)=C XDLMVUHYZWKMMD-UHFFFAOYSA-N 0.000 claims 1
- UXMQORVHJMUQFD-UHFFFAOYSA-N Heptanophenone Chemical compound CCCCCCC(=O)C1=CC=CC=C1 UXMQORVHJMUQFD-UHFFFAOYSA-N 0.000 claims 1
- 239000007795 chemical reaction product Substances 0.000 claims 1
- 239000003795 chemical substances by application Substances 0.000 claims 1
- 238000002242 deionisation method Methods 0.000 claims 1
- ZJLMKPKYJBQJNH-UHFFFAOYSA-N propane-1,3-dithiol Chemical compound SCCCS ZJLMKPKYJBQJNH-UHFFFAOYSA-N 0.000 claims 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims 1
- 230000004048 modification Effects 0.000 abstract description 6
- 238000012986 modification Methods 0.000 abstract description 6
- 230000003197 catalytic effect Effects 0.000 abstract description 5
- 239000006227 byproduct Substances 0.000 abstract description 4
- 230000035484 reaction time Effects 0.000 abstract description 4
- 239000004408 titanium dioxide Substances 0.000 description 9
- 239000000463 material Substances 0.000 description 8
- 241000209094 Oryza Species 0.000 description 5
- 235000007164 Oryza sativa Nutrition 0.000 description 5
- 235000009566 rice Nutrition 0.000 description 5
- 230000008859 change Effects 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000001179 sorption measurement Methods 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- CWAFVXWRGIEBPL-UHFFFAOYSA-N ethoxysilane Chemical compound CCO[SiH3] CWAFVXWRGIEBPL-UHFFFAOYSA-N 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000002957 persistent organic pollutant Substances 0.000 description 2
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- 230000002195 synergetic effect Effects 0.000 description 2
- 229910052719 titanium Inorganic materials 0.000 description 2
- 239000010936 titanium Substances 0.000 description 2
- 239000006087 Silane Coupling Agent Substances 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- ZNAAXKXXDQLJIX-UHFFFAOYSA-N bis(2-cyclohexyl-3-hydroxyphenyl)methanone Chemical compound C1CCCCC1C=1C(O)=CC=CC=1C(=O)C1=CC=CC(O)=C1C1CCCCC1 ZNAAXKXXDQLJIX-UHFFFAOYSA-N 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- ARYZCSRUUPFYMY-UHFFFAOYSA-N methoxysilane Chemical compound CO[SiH3] ARYZCSRUUPFYMY-UHFFFAOYSA-N 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/18—Carbon
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Catalysts (AREA)
- Chemical Or Physical Treatment Of Fibers (AREA)
Abstract
The present invention provides a kind of preparation methods of carbon fiber loaded nano titanium dioxide photocatalysis composite material, and its step are as follows: (1) being surface-treated using hydrogen peroxide to carbon fiber, obtain oxidation processes carbon fiber；(2) it reacts to obtain modifying carbon fibers containing vinyl silicane coupling agent with containing vinyl silicane coupling agent by oxidation processes carbon fiber；(3) it reacts to obtain containing vinyl silicane coupling agent modification nano-titanium dioxide with containing vinyl silicane coupling agent by nano-titanium dioxide；(4) vinyl silicane coupling agent modifying carbon fibers will be contained, containing vinyl silicane coupling agent modification nano-titanium dioxide and dimercaptan mixing, using the reaction between ultraviolet light-initiated sulfydryl and vinyl, carbon fiber loaded nano titanium dioxide photocatalysis composite material is finally obtained.Reaction time of the invention is shorter, yield is high, by-product is few and harmless, and obtained optic catalytic composite material photocatalytic activity is high.
Description
Technical field
The present invention relates to catalysis material technical fields, and in particular to a kind of carbon fiber loaded nano titanium dioxide photocatalysis
The preparation method of composite material.
Background technique
Since 21 century, China promotes industrialized paces to accelerate, and consequent is that more and more resources, environment are asked
Topic needs to handle.Nano-titanium dioxide is a kind of catalysis material of function admirable, and has high activity, low cost, environment
The advantages such as close friend, oneself is through being widely used in administering various environmental pollutions.But there are volatile for powdered nano-titanium dioxide
It lives, be easily aggregated and be difficult to the problems such as separating and recovering, this is the weight for limiting nano-titanium dioxide large-scale application in reality production
Want one of reason.The important channel for solving the problems, such as this is supported on nano-titanium dioxide on suitable carrier, common at present
Carrier include carbon fiber, carbon nanotube and active carbon etc..Carbon fiber not only has biggish compared with other carriers
Specific surface area, and have very strong response to visible light, substantially increase the photocatalytic activity and stabilization of nano-titanium dioxide
Property, it is the ideal carrier of load nano-titanium dioxide.Therefore, nano-titanium dioxide loads to light obtained on carbon fiber and urges
Change composite material to have a wide range of applications in environmental pollution, life production field.
Summary of the invention
Problem to be solved by this invention is: providing a kind of carbon fiber loaded nano titanium dioxide photocatalysis composite material
Preparation method, reaction time is shorter, yield is high, by-product is few and harmless, and obtained optic catalytic composite material photocatalysis is living
Property it is high.
The present invention in order to solve the above problem provided by technical solution are as follows: a kind of carbon fiber loaded nano-titanium dioxide light is urged
Change the preparation method of composite material, it is characterised in that: the described method comprises the following steps:
Step 1: 5g carbon fiber is immersed in the hydrogen peroxide that 100~200mL mass percent solubility is 30%, at room temperature
It ultrasonication 30~60 minutes, is then reacted 1~3 hour under the conditions of 60~90 DEG C of oil baths, product is spent after reaction
Ionized water cleans 5 times, is placed in 110 DEG C of vacuum ovens dry 24 hours to get oxidation processes carbon fiber is arrived；
Step 2: 5g oxidation processes carbon fiber is added to the ethyl alcohol and contain vinyl that 100~200mL volume ratio is 97:3
In silane coupling agent mixed solution, solution ph is adjusted to 4~6 with acetic acid, at room temperature ultrasonication 30~60 minutes, so
It is reacted 4~8 hours under the conditions of 60~90 DEG C of oil baths afterwards, product ethyl alcohol and deionized water mixed solution are clear after reaction
It washes 5 times, is placed in drying 24 hours in 100 DEG C of vacuum ovens, modifying carbon fibers containing vinyl silicane coupling agent can be obtained；
Step 3: 1g nano-titanium dioxide is distributed to the ethyl alcohol and silicon containing vinyl that the volume ratio of 30~50mL is 97:3
In alkane coupling agent mixed solution, solution ph is adjusted to 4~6 with acetic acid, at room temperature ultrasonication 30~60 minutes, then
It is reacted 4~6 hours under the conditions of 60~80 DEG C of oil baths, product ethyl alcohol and deionized water mixed solution clean 5 after reaction
It is secondary, it is then 24 hours dry in 120 DEG C of vacuum ovens, it can be obtained and modify nano-silica containing vinyl silicane coupling agent
Change titanium；
Step 4: 2g modifying carbon fibers containing vinyl silicane coupling agent, 0.5g modification containing vinyl silicane coupling agent are received
The dimercaptan of rice titanium dioxide and 0.1~1g are dispersed in the dimethylformamide of 80~150mL, at room temperature
Ultrasonication 30~60 minutes, the photoinitiator of 0.01~0.1g is then added, uses wavelength for the ultraviolet lighting of 365nm
It penetrates 10~30 minutes, filters after completion of the reaction, and cleaned 4 times with dimethylformamide, it is dry in 110 DEG C of vacuum ovens
48 hours, carbon fiber loaded nano titanium dioxide photocatalysis composite material can be obtained.
Preferably, the vinyl silicane coupling agent that contains in the step 2 is vinyltrimethoxysilane, vinyl three
Ethoxysilane, methyl vinyl diethoxysilane, vinyl silane triisopropoxide, methacryloxypropyl three
Any one in methoxy silane or methacryloxypropyl.
Preferably, the dimercaptan of the step 4 is Isosorbide-5-Nitrae-succinimide mercaptans, 1,6- ethanthiol, 1,3- the third two sulphur
Alcohol or 1, any one in 5- pentane disulfide thioalcohol.
Preferably, the photoinitiator in the step 4 is benzophenone, styrax n-butyl ether, benzoin dimethylether or 1-
Any one in hydroxycyclohexyl phenyl ketone.
Compared with prior art, the invention has the advantages that the present invention is negative in carbon fiber surface using the method for click chemistry
Nano-titanium dioxide is carried, reaction time is shorter, yield is high, by-product is few and harmless, obtained optic catalytic composite material light
Catalytic activity is high.Using carbon fiber loaded nano-titanium dioxide, can effective degradable organic pollutant, it is easy to solve carbonaceous class material
The problems such as reaching adsorption saturation and the recycling of powdered titanium dioxide, while can increase the specific surface area of material, enhance electronics circle
Face effect increases stability of material；It is weak and in the solution to solve nano-titanium dioxide selection adsorption capacity by the present invention simultaneously
Nano-titanium dioxide is loaded the stability that nano-titanium dioxide can be improved on carbon fiber by the problems such as easy secondary agglomeration；In addition,
Carbon fiber and nano-titanium dioxide have good synergistic effect, can effectively improve the efficiency of photochemical catalyst, while expanding nanometer
Application of the titanium dioxide in photocatalysis field.
Specific embodiment
Below by by embodiment come the embodiment that the present invention will be described in detail, whereby to the present invention how application technology hand
Section solves technical problem and reaches the realization process of technical effect to fully understand and implement.
Embodiment 1:
This example demonstrates that a kind of system of carbon fiber loaded nano titanium dioxide photocatalysis composite material provided by the invention
Preparation Method.
Step 1: 5g carbon fiber is immersed in the hydrogen peroxide that 100mL mass percent solubility is 30%, ultrasonic wave at room temperature
Processing 30 minutes, then reacts 3 hours under the conditions of 60 DEG C of oil baths, product is cleaned 5 times with deionized water after reaction, is set
24 hours are dried in 110 DEG C of vacuum ovens to get oxidation processes carbon fiber is arrived；
Step 2: 5g oxidation processes carbon fiber is added to the ethyl alcohol and vinyl trimethoxy that 100mL volume ratio is 97:3
In base silane mixed solution, solution ph is adjusted to 6 with acetic acid, at room temperature ultrasonication 30 minutes, then in 60 DEG C of oil baths
Under the conditions of react 8 hours, product ethyl alcohol and deionized water mixed solution clean 5 times after reaction, are placed in 100 DEG C of vacuum
It is 24 hours dry in drying box, modifying carbon fibers containing vinyl silicane coupling agent can be obtained；
Step 3: the ethyl alcohol and vinyl trimethoxy that are 97:3 by the volume ratio that 1g nano-titanium dioxide is distributed to 30mL
In silane mixture solution, solution ph is adjusted to 6 with acetic acid, at room temperature ultrasonication 30 minutes, then in 60 DEG C of oil bath items
It is reacted under part 6 hours, product ethyl alcohol and deionized water mixed solution clean 5 times after reaction, then in 120 DEG C of vacuum
It is 24 hours dry in drying box, it can be obtained and modify nano-titanium dioxide containing vinyl silicane coupling agent；
Step 4: 2g modifying carbon fibers containing vinyl silicane coupling agent, 0.5g modification containing vinyl silicane coupling agent are received
Isosorbide-5-Nitrae-succinimide mercaptans of rice titanium dioxide and 0.1g are dispersed in the dimethylformamide of 80mL, at room temperature at ultrasonic wave
Then the benzophenone of 0.01g is added in reason 30 minutes, use wavelength for ultraviolet light 30 minutes of 365nm, end of reaction
After filter, and cleaned 4 times with dimethylformamide, it is 48 hours dry in 110 DEG C of vacuum ovens, carbon fiber can be obtained
Load nano-titanium dioxide photocatalysis composite material.
Embodiment 2:
This example demonstrates that a kind of system of carbon fiber loaded nano titanium dioxide photocatalysis composite material provided by the invention
Preparation Method.
Step 1: 5g carbon fiber is immersed in the hydrogen peroxide that 150mL mass percent solubility is 30%, ultrasonic wave at room temperature
Processing 45 minutes, then reacts 2 hours under the conditions of 80 DEG C of oil baths, product is cleaned 5 times with deionized water after reaction, is set
24 hours are dried in 110 DEG C of vacuum ovens to get oxidation processes carbon fiber is arrived；
Step 2: 5g oxidation processes carbon fiber is added to the ethyl alcohol and methacryloxypropyl that 150mL volume ratio is 97:3
In base propyl trimethoxy silicane mixed solution, solution ph is adjusted to 5 with acetic acid, at room temperature ultrasonication 45 minutes, so
It is reacted 6 hours under the conditions of 80 DEG C of oil baths afterwards, product ethyl alcohol and deionized water mixed solution clean 5 times after reaction, set
It is 24 hours dry in 100 DEG C of vacuum ovens, modifying carbon fibers containing vinyl silicane coupling agent can be obtained；
Step 3: the ethyl alcohol and methacryloxy that are 97:3 by the volume ratio that 1g nano-titanium dioxide is distributed to 40mL
In propyl trimethoxy silicane mixed solution, solution ph is adjusted to 5 with acetic acid, at room temperature ultrasonication 45 minutes, then
React 5 hours under the conditions of 70 DEG C of oil baths, product ethyl alcohol and deionized water mixed solution clean 5 times after reaction, then
It is 24 hours dry in 120 DEG C of vacuum ovens, it can be obtained and modify nano-titanium dioxide containing vinyl silicane coupling agent；
Step 4: 2g modifying carbon fibers containing vinyl silicane coupling agent, 0.5g modification containing vinyl silicane coupling agent are received
1, the 6- ethanthiol of rice titanium dioxide and 0.8g are dispersed in the dimethylformamide of 100mL, at room temperature at ultrasonic wave
Then reason 45 minutes is added the styrax n-butyl ether of 0.08g, uses wavelength for ultraviolet light 20 minutes of 365nm, react
After filter, and cleaned 4 times with dimethylformamide, it is 48 hours dry in 110 DEG C of vacuum ovens, carbon can be obtained
Fiber-loaded nano titanium dioxide photocatalysis composite material.
Embodiment 3:
This example demonstrates that a kind of system of carbon fiber loaded nano titanium dioxide photocatalysis composite material provided by the invention
Preparation Method.
Step 1: 5g carbon fiber is immersed in the hydrogen peroxide that 200mL mass percent solubility is 30%, ultrasonic wave at room temperature
Processing 60 minutes, then reacts 1 hour under the conditions of 90 DEG C of oil baths, product is cleaned 5 times with deionized water after reaction, is set
24 hours are dried in 110 DEG C of vacuum ovens to get oxidation processes carbon fiber is arrived；
Step 2: 5g oxidation processes carbon fiber is added to the ethyl alcohol and methyl ethylene two that 200mL volume ratio is 97:3
In Ethoxysilane mixed solution, solution ph is adjusted to 4 with acetic acid, at room temperature ultrasonication 60 minutes, then at 90 DEG C
It is reacted 4 hours under the conditions of oil bath, product ethyl alcohol and deionized water mixed solution clean 5 times after reaction, are placed in 100 DEG C
It is 24 hours dry in vacuum oven, modifying carbon fibers containing vinyl silicane coupling agent can be obtained；
Step 3: the ethyl alcohol and methyl ethylene diethyl that are 97:3 by the volume ratio that 1g nano-titanium dioxide is distributed to 50mL
In oxysilane mixed solution, solution ph is adjusted to 4 with acetic acid, at room temperature ultrasonication 60 minutes, then in 80 DEG C of oil
It is reacted 4 hours under the conditions of bath, product ethyl alcohol and deionized water mixed solution clean 5 times after reaction, then at 120 DEG C
It is 24 hours dry in vacuum oven, it can be obtained and modify nano-titanium dioxide containing vinyl silicane coupling agent；
Step 4: 2g modifying carbon fibers containing vinyl silicane coupling agent, 0.5g modification containing vinyl silicane coupling agent are received
1, the 5- pentane disulfide thioalcohol of rice titanium dioxide and 1g are dispersed in the dimethylformamide of 150mL, at room temperature ultrasonication
60 minutes, the benzoin dimethylether of 0.1g is then added, uses wavelength for ultraviolet light 10 minutes of 365nm, end of reaction
After filter, and cleaned 4 times with dimethylformamide, it is 48 hours dry in 110 DEG C of vacuum ovens, carbon fiber can be obtained
Load nano-titanium dioxide photocatalysis composite material.
The beneficial effects of the present invention are: the present invention loads nanometer titanium dioxide in carbon fiber surface using the method for click chemistry
Titanium, reaction time is shorter, yield is high, by-product is few and harmless, and obtained optic catalytic composite material photocatalytic activity is high.
Using carbon fiber loaded nano-titanium dioxide, can effective degradable organic pollutant, solve carbonaceous class material and easily reach adsorption saturation
And powdered titanium dioxide recycling the problems such as, while can increase the specific surface area of material, enhance electronic interface effect, increase
Stability of material；The present invention solves that nano-titanium dioxide selection adsorption capacity is weak and easy secondary agglomeration in the solution simultaneously
The problems such as, nano-titanium dioxide is loaded to the stability that nano-titanium dioxide can be improved on carbon fiber；In addition, carbon fiber and receiving
Rice titanium dioxide has good synergistic effect, can effectively improve the efficiency of photochemical catalyst, while expanding nano-titanium dioxide and existing
The application of photocatalysis field.
Only highly preferred embodiment of the present invention is described above, but is not to be construed as limiting the scope of the invention.This
Invention is not only limited to above embodiments, and specific structure is allowed to vary.All protection models in independent claims of the present invention
Interior made various change is enclosed to all fall in the scope of protection of the present invention.
Claims (4)
1. a kind of preparation method of carbon fiber loaded nano titanium dioxide photocatalysis composite material, it is characterised in that: the method
The following steps are included:
Step 1: 5g carbon fiber being immersed in the hydrogen peroxide that 100~200mL mass percent solubility is 30%, ultrasonic at room temperature
Wave is handled 30~60 minutes, then reacts 1~3 hour under the conditions of 60~90 DEG C of oil baths, after reaction product deionization
Water cleans 5 times, is placed in 110 DEG C of vacuum ovens dry 24 hours to get oxidation processes carbon fiber is arrived；
Step 2: 5g oxidation processes carbon fiber is added to the ethyl alcohol and contain vinyl silanes that 100~200mL volume ratio is 97:3
In coupling agent mixed solution, solution ph is adjusted to 4~6 with acetic acid, at room temperature ultrasonication 30~60 minutes, then 60
It is reacted 4~8 hours under the conditions of~90 DEG C of oil baths, product ethyl alcohol and deionized water mixed solution clean 5 times after reaction, set
It is 24 hours dry in 100 DEG C of vacuum ovens, modifying carbon fibers containing vinyl silicane coupling agent can be obtained；
Step 3: 1g nano-titanium dioxide is distributed to the volume ratio of 30~50mL for the ethyl alcohol of 97:3 and containing vinyl silanes idol
Join in agent mixed solution, adjust solution ph to 4~6 with acetic acid, at room temperature ultrasonication 30~60 minutes, then 60~
React 4~6 hours under the conditions of 80 DEG C of oil baths, product ethyl alcohol and deionized water mixed solution clean 5 times after reaction, then
It is 24 hours dry in 120 DEG C of vacuum ovens, it can be obtained and modify nano-titanium dioxide containing vinyl silicane coupling agent；
Step 4: 2g modifying carbon fibers containing vinyl silicane coupling agent, 0.5g are modified into nanometer two containing vinyl silicane coupling agent
The dimercaptan of titanium oxide and 0.1~1g are dispersed in the dimethylformamide of 80~150mL, at room temperature ultrasonic wave
Then processing 30~60 minutes is added the photoinitiator of 0.01~0.1g, uses wavelength for the ultraviolet light 10~30 of 365nm
Minute, it filters after completion of the reaction, and cleaned 4 times with dimethylformamide, it is 48 hours dry in 110 DEG C of vacuum ovens, i.e.,
Carbon fiber loaded nano titanium dioxide photocatalysis composite material can be obtained.
2. a kind of preparation method of carbon fiber loaded nano titanium dioxide photocatalysis composite material as described in claim 1,
Be characterized in that: in the step 2 is vinyltrimethoxysilane, vinyl triethoxyl containing vinyl silicane coupling agent
Silane, methyl vinyl diethoxysilane, vinyl silane triisopropoxide, methacryloxypropyl trimethoxy silicon
Any one in alkane or methacryloxypropyl.
3. a kind of preparation method of carbon fiber loaded nano titanium dioxide photocatalysis composite material as described in claim 1,
Be characterized in that: the dimercaptan of the step 4 be Isosorbide-5-Nitrae-succinimide mercaptans, 1,6- ethanthiol, 1,3- dimercaptopropane or 1,
Any one in 5- pentane disulfide thioalcohol.
4. a kind of preparation method of carbon fiber loaded nano titanium dioxide photocatalysis composite material as described in claim 1,
Be characterized in that: the photoinitiator in the step 4 is benzophenone, styrax n-butyl ether, benzoin dimethylether or 1- hydroxyl ring
Any one in hexyl phenyl ketone.
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