CN108993506A - A kind of preparation method of Fe2O3 doping titanium dioxide-carbon fibre composite - Google Patents
A kind of preparation method of Fe2O3 doping titanium dioxide-carbon fibre composite Download PDFInfo
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- CN108993506A CN108993506A CN201810910915.4A CN201810910915A CN108993506A CN 108993506 A CN108993506 A CN 108993506A CN 201810910915 A CN201810910915 A CN 201810910915A CN 108993506 A CN108993506 A CN 108993506A
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- Prior art keywords
- titanium dioxide
- fibre composite
- carbon fibre
- fe2o3 doping
- doping titanium
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- 239000002131 composite material Substances 0.000 title claims abstract description 32
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 title claims abstract description 29
- GCNLQHANGFOQKY-UHFFFAOYSA-N [C+4].[O-2].[O-2].[Ti+4] Chemical compound [C+4].[O-2].[O-2].[Ti+4] GCNLQHANGFOQKY-UHFFFAOYSA-N 0.000 title claims abstract description 26
- 239000000835 fiber Substances 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 229920000049 Carbon (fiber) Polymers 0.000 claims abstract description 20
- 239000004917 carbon fiber Substances 0.000 claims abstract description 20
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 17
- 238000013019 agitation Methods 0.000 claims abstract description 14
- 239000007788 liquid Substances 0.000 claims abstract description 12
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 claims abstract description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229960000935 dehydrated alcohol Drugs 0.000 claims abstract description 10
- 239000012298 atmosphere Substances 0.000 claims abstract description 7
- 238000001816 cooling Methods 0.000 claims abstract description 7
- 239000008367 deionised water Substances 0.000 claims abstract description 7
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 7
- MVFCKEFYUDZOCX-UHFFFAOYSA-N iron(2+);dinitrate Chemical compound [Fe+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MVFCKEFYUDZOCX-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000003756 stirring Methods 0.000 claims abstract description 7
- 239000002253 acid Substances 0.000 claims description 15
- 238000000034 method Methods 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 7
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 6
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 6
- 238000005516 engineering process Methods 0.000 claims description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 3
- 239000012300 argon atmosphere Substances 0.000 claims description 3
- 239000000428 dust Substances 0.000 claims description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 abstract description 23
- 239000004408 titanium dioxide Substances 0.000 abstract description 10
- 230000003197 catalytic effect Effects 0.000 abstract description 6
- 230000001699 photocatalysis Effects 0.000 abstract description 6
- 230000015556 catabolic process Effects 0.000 abstract description 5
- 238000006731 degradation reaction Methods 0.000 abstract description 5
- 239000005416 organic matter Substances 0.000 abstract description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 14
- 239000000463 material Substances 0.000 description 7
- 229910052742 iron Inorganic materials 0.000 description 5
- 238000007146 photocatalysis Methods 0.000 description 4
- 150000001298 alcohols Chemical class 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 2
- 229960005191 ferric oxide Drugs 0.000 description 2
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 2
- 235000013980 iron oxide Nutrition 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000002121 nanofiber Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- ZWYDDDAMNQQZHD-UHFFFAOYSA-L titanium(ii) chloride Chemical compound [Cl-].[Cl-].[Ti+2] ZWYDDDAMNQQZHD-UHFFFAOYSA-L 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 239000002351 wastewater Substances 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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/74—Iron group metals
- B01J23/745—Iron
-
- 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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/002—Mixed oxides other than spinels, e.g. perovskite
-
- B01J35/39—
-
- B01J35/399—
-
- B01J35/58—
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
Abstract
The invention discloses a kind of preparation methods of Fe2O3 doping titanium dioxide-carbon fibre composite, it include: in the presence of (1) is sour, butyl titanate is dissolved in dehydrated alcohol, 10~15min of magnetic agitation, a certain amount of iron nitrate solution is added, 30~45min of stirring is continued, deionized water is added, 1~2h of magnetic agitation, obtains mixed liquor A under 50~60 DEG C of water bath conditions;(2) a certain amount of carbon fiber is added in the mixed liquor A in step (1), 2~4h of ultrasonic disperse obtains mixed liquid B, wherein 10~100g carbon fiber is added in every 1 liter of mixed liquor A;(3) under inert atmosphere conditions by the mixed liquid B in step (2), cooling in 400~600 DEG C of 1~3h of roasting temperature, grinding obtains Fe2O3 doping titanium dioxide-carbon fibre composite.In composite material of the invention, Fe2O3 doping titanium dioxide can be evenly dispersed in carbon fiber, therefore under visible light conditions, the organic matter which can well in catalytic degradation water body, photocatalytic activity it is reproducible.
Description
Technical field
The present invention relates to field of material technology, more particularly to a kind of Fe2O3 doping titanium dioxide-carbon fibre composite
Preparation method.
Background technique
Titanium dioxide is generally considered important photochemical catalyst because of the advantages that its is nontoxic, chemical stability is good, cheap.It will
Titanium dioxide is made into nanoparticle or nanofiber form, can effectively improve the specific surface area of titanic oxide material, enhances it
Catalytic efficiency.And it is composite modified to nano-titanium dioxide progress, titanium dioxide forbidden bandwidth on the one hand can be reduced, spectrum is improved
On the other hand utilization rate can promote electron-hole pair to separate, improve optically catalytic TiO 2 performance.
Iron and its compound have visible light photocatalysis performance, while the compound of most of iron can express at room temperature
It is preferable magnetic, it can easily realize the recycling and reusing of material.Nano-level iron or to its it is composite modified after, specific surface area and
Contact area greatly increases, so that such material has more superior photocatalysis performance.
Iron and titanium dioxide are compound, can improve the visible light photocatalysis performance and chemical property of titanium dioxide, shadow
Ring the crystal transition of titanium dioxide.But the composite material of granular iron and titanium dioxide is because of small, easy to reunite, the difficult recycling of its partial size
The disadvantages of, greatly limit the application field of such material.Therefore, by iron and titanium dichloride load on high specific surface carrier
Research just become increasingly important.But the catalytic degradation performance of iron in the prior art and composite titania material
It is ideal not enough.
For this reason, it is necessary in view of the above-mentioned problems, propose a kind of preparation side of Fe2O3 doping titanium dioxide-carbon fibre composite
Method is able to solve problems of the prior art.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation method of Fe2O3 doping titanium dioxide-carbon fibre composite, with gram
Take deficiency in the prior art.
To achieve the above object, the invention provides the following technical scheme:
A kind of preparation method of Fe2O3 doping titanium dioxide-carbon fibre composite, comprising:
(1) in the presence of acid, butyl titanate is dissolved in dehydrated alcohol, 10~15min of magnetic agitation, is added certain
The iron nitrate solution of amount, continues 30~45min of stirring, and deionized water is added, under 50~60 DEG C of water bath conditions magnetic agitation 1~
2h obtains mixed liquor A;
(2) a certain amount of carbon fiber is added in the mixed liquor A in step (1), 2~4h of ultrasonic disperse obtains mixed liquor
B, wherein 10~100g carbon fiber is added in every 1 liter of mixed liquor A;
(3) under inert atmosphere conditions by the mixed liquid B in step (2), in 400~600 DEG C of 1~3h of roasting temperature,
Cooling, grinding obtains Fe2O3 doping titanium dioxide-carbon fibre composite.
Preferably, in step (1), the acid is selected from one of dilute hydrochloric acid, dilute sulfuric acid, dust technology, and the acid is to adjust
Saving pH value is 2~7.
Preferably, in step (1), the acid is 6 to adjust pH value.
Preferably, in step (1), the ratio between volume of the butyl titanate and the dehydrated alcohol is 1~10:50.
Preferably, the ratio between volume of the butyl titanate and the dehydrated alcohol is 3:50.
Preferably, in step (2), 50g carbon fiber is added in every 1 liter of mixed liquor A.
Preferably, in step (3), the inert atmosphere is nitrogen atmosphere or argon atmosphere.
Preferably, in step (3), the heating rate of roasting process is 2~10 DEG C/min.
Compared with the prior art, the advantages of the present invention are as follows: in composite material of the invention, Fe2O3 doping titanium dioxide can
It is evenly dispersed in carbon fiber, therefore under visible light conditions, which can be well in catalytic degradation water body
Organic matter, photocatalytic activity it is reproducible.
Specific embodiment
The present invention is described further by the following example: according to following embodiments, the present invention may be better understood.
However, as it will be easily appreciated by one skilled in the art that specific material ratio, process conditions and its result described in embodiment are only used
In illustrating the present invention, without the present invention described in detail in claims should will not be limited.
The present invention discloses a kind of preparation method of Fe2O3 doping titanium dioxide-carbon fibre composite, comprising:
(1) in the presence of acid, butyl titanate is dissolved in dehydrated alcohol, 10~15min of magnetic agitation, is added certain
The iron nitrate solution of amount, continues 30~45min of stirring, and deionized water is added, under 50~60 DEG C of water bath conditions magnetic agitation 1~
2h obtains mixed liquor A;
(2) a certain amount of carbon fiber is added in the mixed liquor A in step (1), 2~4h of ultrasonic disperse obtains mixed liquor
B, wherein 10~100g carbon fiber is added in every 1 liter of mixed liquor A;
(3) under inert atmosphere conditions by the mixed liquid B in step (2), in 400~600 DEG C of 1~3h of roasting temperature,
Cooling, grinding obtains Fe2O3 doping titanium dioxide-carbon fibre composite.
Wherein, in step (1), the acid is selected from one of dilute hydrochloric acid, dilute sulfuric acid, dust technology, and the acid is to adjust
PH value is 2~7, it is preferred that the acid is 6 to adjust pH value;The volume of the butyl titanate and the dehydrated alcohol it
Than for 1~10:50, it is preferred that the ratio between volume of the butyl titanate and the dehydrated alcohol is 3:50.
Wherein, in step (2), 50g carbon fiber is added in every 1 liter of mixed liquor A.
Wherein, in step (3), the inert atmosphere is nitrogen atmosphere or argon atmosphere;The heating rate of roasting process is 2
~10 DEG C/min, it is preferred that the heating rate of roasting process is 5 DEG C/min.
It is following that Fe2O3 doping titanium dioxide-carbon fibre composite preparation in the present invention is illustrated with specifically embodiment
Method.
Embodiment 1
(1) in the presence of acid, 1 volume butyl titanate is dissolved in 50 volume dehydrated alcohols, the pH value for controlling solution is
2, magnetic agitation 10min add a certain amount of iron nitrate solution, continue to stir 30min, deionized water are added, in 50 DEG C of water
Magnetic agitation 1h under the conditions of bath, obtains mixed liquor A;
(2) a certain amount of carbon fiber being added in the mixed liquor A in step (1), ultrasonic disperse 2h obtains mixed liquid B,
In, 10g carbon fiber is added in every 1 liter of mixed liquor A;
(3) by the mixed liquid B in step (2) under the conditions of nitrogen atmosphere, with the heating rate of 2 DEG C/min, in 400 DEG C of temperature
Degree is lower to roast 1h, and cooling, grinding obtains Fe2O3 doping titanium dioxide-carbon fibre composite.
Embodiment 2
(1) in the presence of acid, 3 volume butyl titanates are dissolved in 50 volume dehydrated alcohols, the pH value for controlling solution is
6, magnetic agitation 12min add a certain amount of iron nitrate solution, continue to stir 38min, deionized water are added, in 55 DEG C of water
Magnetic agitation 1.5h under the conditions of bath, obtains mixed liquor A;
(2) a certain amount of carbon fiber being added in the mixed liquor A in step (1), ultrasonic disperse 3h obtains mixed liquid B,
In, 50g carbon fiber is added in every 1 liter of mixed liquor A;
(3) by the mixed liquid B in step (2) under the conditions of nitrogen atmosphere, with the heating rate of 5 DEG C/min, in 500 DEG C of temperature
Degree is lower to roast 2h, and cooling, grinding obtains Fe2O3 doping titanium dioxide-carbon fibre composite.
Embodiment 3
(1) in the presence of acid, 10 volume butyl titanates are dissolved in 50 volume dehydrated alcohols, the pH value for controlling solution is
7, magnetic agitation 15min add a certain amount of iron nitrate solution, continue to stir 45min, deionized water are added, in 60 DEG C of water
Magnetic agitation 2h under the conditions of bath, obtains mixed liquor A;
(2) a certain amount of carbon fiber being added in the mixed liquor A in step (1), ultrasonic disperse 4h obtains mixed liquid B,
In, 100g carbon fiber is added in every 1 liter of mixed liquor A;
(3) by the mixed liquid B in step (2) under the conditions of nitrogen atmosphere, with the heating rate of 10 DEG C/min, in 600 DEG C
1~3h of roasting temperature, cooling, grinding obtains Fe2O3 doping titanium dioxide-carbon fibre composite.
In Fe2O3 doping titanium dioxide-carbon fibre composite of the invention, Fe2O3 doping titanium dioxide can be uniformly dispersed
In the carbon fibers, therefore under visible light conditions, the organic matter which can well in catalytic degradation water body, light is urged
Change active reproducible.After radiation of visible light waste water 60min, the degradation rate of organic matter is up to 95.6%.Therefore, this hair
Fe2O3 doping titanium dioxide-carbon fibre composite in bright has broad application prospects in terms of photocatalysis.
Finally, it is to be noted that, the terms "include", "comprise" or its any other variant be intended to it is non-exclusive
Property include so that include a series of elements process, method, article or equipment not only include those elements, but also
Further include other elements that are not explicitly listed, or further include for this process, method, article or equipment it is intrinsic
Element.
Claims (8)
1. a kind of preparation method of Fe2O3 doping titanium dioxide-carbon fibre composite characterized by comprising
(1) in the presence of acid, butyl titanate is dissolved in dehydrated alcohol, 10~15min of magnetic agitation is added a certain amount of
Iron nitrate solution, continues 30~45min of stirring, is added deionized water, 1~2h of magnetic agitation under 50~60 DEG C of water bath conditions,
Obtain mixed liquor A;
(2) a certain amount of carbon fiber being added in the mixed liquor A in step (1), 2~4h of ultrasonic disperse obtains mixed liquid B,
In, 10~100g carbon fiber is added in every 1 liter of mixed liquor A;
It is (3) under inert atmosphere conditions by the mixed liquid B in step (2), cooling in 400~600 DEG C of 1~3h of roasting temperature,
Grinding, obtains Fe2O3 doping titanium dioxide-carbon fibre composite.
2. the preparation method of Fe2O3 doping titanium dioxide-carbon fibre composite according to claim 1, which is characterized in that
In step (1), the acid is selected from one of dilute hydrochloric acid, dilute sulfuric acid, dust technology, and the acid is 2~7 to adjust pH value.
3. the preparation method of Fe2O3 doping titanium dioxide-carbon fibre composite according to claim 2, which is characterized in that
In step (1), the acid is 6 to adjust pH value.
4. the preparation method of Fe2O3 doping titanium dioxide-carbon fibre composite according to claim 1, which is characterized in that
In step (1), the ratio between volume of the butyl titanate and the dehydrated alcohol is 1~10:50.
5. the preparation method of Fe2O3 doping titanium dioxide-carbon fibre composite according to claim 2, which is characterized in that
The ratio between volume of the butyl titanate and the dehydrated alcohol is 3:50.
6. the preparation method of Fe2O3 doping titanium dioxide-carbon fibre composite according to claim 1, which is characterized in that
In step (2), 50g carbon fiber is added in every 1 liter of mixed liquor A.
7. the preparation method of Fe2O3 doping titanium dioxide-carbon fibre composite according to claim 1, which is characterized in that
In step (3), the inert atmosphere is nitrogen atmosphere or argon atmosphere.
8. the preparation method of Fe2O3 doping titanium dioxide-carbon fibre composite according to claim 1, which is characterized in that
In step (3), the heating rate of roasting process is 2~10 DEG C/min.
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Cited By (1)
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CN114308136A (en) * | 2021-07-30 | 2022-04-12 | 台湾塑胶工业股份有限公司 | Carbon fiber composite material and method for producing same |
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Application publication date: 20181214 |