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 PDF

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Publication number
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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China
Prior art keywords
titanium dioxide
fibre composite
carbon fibre
fe2o3 doping
doping titanium
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CN201810910915.4A
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Chinese (zh)
Inventor
陆伟
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Zhangjiagang City Department Of Dingxin Mstar Technology Ltd
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Zhangjiagang City Department Of Dingxin Mstar Technology Ltd
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Priority to CN201810910915.4A priority Critical patent/CN108993506A/en
Publication of CN108993506A publication Critical patent/CN108993506A/en
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/70Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
    • B01J23/74Iron group metals
    • B01J23/745Iron
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/002Mixed oxides other than spinels, e.g. perovskite
    • B01J35/39
    • B01J35/399
    • B01J35/58
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/30Treatment of water, waste water, or sewage by irradiation
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/30Organic compounds
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2305/00Use of specific compounds during water treatment
    • C02F2305/10Photocatalysts

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

A kind of preparation method of Fe2O3 doping titanium dioxide-carbon fibre composite
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.
CN201810910915.4A 2018-08-10 2018-08-10 A kind of preparation method of Fe2O3 doping titanium dioxide-carbon fibre composite Withdrawn CN108993506A (en)

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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