CN109277097A - A kind of TiO2/ cotton based carbon fiber photochemical catalyst and preparation method thereof - Google Patents
A kind of TiO2/ cotton based carbon fiber photochemical catalyst and preparation method thereof Download PDFInfo
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- CN109277097A CN109277097A CN201811439422.3A CN201811439422A CN109277097A CN 109277097 A CN109277097 A CN 109277097A CN 201811439422 A CN201811439422 A CN 201811439422A CN 109277097 A CN109277097 A CN 109277097A
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- carbon fiber
- based carbon
- tio
- cotton
- photochemical catalyst
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- 229920000742 Cotton Polymers 0.000 title claims abstract description 73
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 60
- 239000004917 carbon fiber Substances 0.000 title claims abstract description 57
- 229920000049 Carbon (fiber) Polymers 0.000 title claims abstract description 56
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims abstract description 56
- 239000003054 catalyst Substances 0.000 title claims abstract description 39
- 238000002360 preparation method Methods 0.000 title claims abstract description 28
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 claims abstract description 19
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000012299 nitrogen atmosphere Substances 0.000 claims abstract description 8
- 238000003756 stirring Methods 0.000 claims abstract description 5
- 238000005352 clarification Methods 0.000 claims abstract description 4
- 238000010438 heat treatment Methods 0.000 claims abstract description 4
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 28
- 238000003763 carbonization Methods 0.000 claims description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 7
- 229910052799 carbon Inorganic materials 0.000 abstract description 4
- 239000002994 raw material Substances 0.000 abstract description 2
- 239000010936 titanium Substances 0.000 abstract description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 abstract 1
- 239000012876 carrier material Substances 0.000 abstract 1
- 229910052719 titanium Inorganic materials 0.000 abstract 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 22
- 239000000047 product Substances 0.000 description 13
- 238000005255 carburizing Methods 0.000 description 9
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 6
- 239000003610 charcoal Substances 0.000 description 6
- 239000004408 titanium dioxide Substances 0.000 description 6
- 239000000463 material Substances 0.000 description 5
- 238000002474 experimental method Methods 0.000 description 4
- 239000000835 fiber Substances 0.000 description 4
- 238000009533 lab test Methods 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 3
- 229910052681 coesite Inorganic materials 0.000 description 3
- 229910052906 cristobalite Inorganic materials 0.000 description 3
- 229910021389 graphene Inorganic materials 0.000 description 3
- 230000007062 hydrolysis Effects 0.000 description 3
- 238000006460 hydrolysis reaction Methods 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 230000001699 photocatalysis Effects 0.000 description 3
- 238000007146 photocatalysis Methods 0.000 description 3
- 239000000377 silicon dioxide Substances 0.000 description 3
- 229910052682 stishovite Inorganic materials 0.000 description 3
- 229910052905 tridymite Inorganic materials 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 241000241602 Gossypianthus Species 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000000413 hydrolysate Substances 0.000 description 1
- 230000002779 inactivation Effects 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- STZCRXQWRGQSJD-GEEYTBSJSA-M methyl orange Chemical compound [Na+].C1=CC(N(C)C)=CC=C1\N=N\C1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-GEEYTBSJSA-M 0.000 description 1
- 229940012189 methyl orange Drugs 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000009466 transformation Effects 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
-
- B01J35/39—
-
- B01J35/58—
Abstract
The present invention relates to a kind of TiO2The preparation method of/cotton based carbon fiber photochemical catalyst obtains cotton based carbon fiber including the cotton cleaned is carbonized 2h in a nitrogen atmosphere；Later in HCl solution, butyl titanate is added in stirring, is transferred in water heating kettle after solution clarification, the cotton based carbon fiber of above-mentioned preparation, hydro-thermal reaction 12h is added；Obtained product is filtered, is washed with water, dries in an oven, finally roast 4h in a nitrogen atmosphere, obtain TiO2/ cotton based carbon fiber photochemical catalyst.For the fibrous carbon that above-mentioned preparation method obtains after being carbonized using cotton fiber as carrier, butyl titanate is nano-TiO2Predecessor, by hydro-thermal reaction by nano-TiO2Supported titanium can be obtained in carrier surface in uniform load2/ cotton based carbon fiber photochemical catalyst；The TiO2/ cotton based carbon fiber photochemical catalyst uses cotton based carbon fiber for carrier, and raw material is easy to get, low in cost, and can effectively prevent nano-TiO2Reunion.
Description
Technical field
The present invention relates to loaded photocatalyst technical fields, and in particular to a kind of TiO2The based carbon fiber photocatalysis of/cotton
Agent and preparation method thereof.
Background technique
As the problem of environmental pollutions such as atmosphere pollution, water environment pollution are increasingly serious, conductor photocatalysis material due to
The great potential of Environment control etc. causes the concern of researcher.In common semiconductor material, titanium dioxide
(TiO2) because its have many advantages, such as it is cheap, stablize, have excellent performance, nontoxic goed deep into and widely study.Nano-TiO2Powder
Although catalytic activity with higher, there is the disadvantages of easy aggregation, easy in inactivation, more difficult recycling, limit its use.And it is right
TiO2It carries out supported being the effective way for solving the problems, such as this.Current various materials are all used as nano-TiO2Load
Body, including mesoporous SiO2, graphene etc., TiO2There is better photocatalysis performance with the composite material that these carriers are formed.So
And mesoporous SiO2, the materials such as graphene prepare it is cumbersome, it is expensive.Therefore, it needs to design a kind of new technical solution, with comprehensive
It closes and solves problems of the prior art.
Summary of the invention
The object of the present invention is to provide a kind of TiO2/ cotton based carbon fiber photochemical catalyst, the fibre after being carbonized with cotton fiber
Dimension shape charcoal is carrier, can effectively prevent nano-TiO2Reunion, preparation method is easy, can effectively solve existing mesoporous SiO2、
Preparation process cumbersome problem when the materials such as graphene are as carrier.
In order to solve the above technical problems, the invention adopts the following technical scheme:
TiO of the present invention2The preparation method of/cotton based carbon fiber photochemical catalyst the following steps are included:
S1. by clean cotton 300~800 DEG C of carbonization 2h in a nitrogen atmosphere, cotton based carbon fiber is obtained；
S2. in HCl solution, butyl titanate is added in stirring, is transferred in water heating kettle after solution clarification, step is added
(1) the cotton based carbon fiber prepared in, hydro-thermal reaction 12h；
S3. the product of step S2 is filtered, is washed with water, dries in an oven, finally roast 4h in a nitrogen atmosphere, obtains
To TiO2/ cotton based carbon fiber photochemical catalyst.
Wherein the concentration of HCl solution is 2~6mol/L in step S2；And butyl titanate, cotton based carbon fiber and HCl solution
Mass ratio be 1.05~8.4:1:250.
The temperature of above-mentioned hydro-thermal reaction is 150~180 DEG C；Maturing temperature is 450 DEG C.
The TiO prepared using the above method2/ cotton based carbon fiber photochemical catalyst, the fibre obtained after being carbonized with cotton fiber
Dimension shape charcoal is carrier, and butyl titanate is nano-TiO2Predecessor, by hydro-thermal reaction by nano-TiO2Uniform load is in carrier table
Face obtains supported titanium2/ cotton based carbon fiber photochemical catalyst.
The TiO that above-mentioned technical proposal provides2/ cotton based carbon fiber photochemical catalyst and preparation method thereof, with prior art phase
Than, there are following the utility model has the advantages that
(1) for carrier, raw material is easy to get the cotton based carbon fiber for using cotton fiber nitrogen to be carbonized, low in cost, comes
Source is abundant；
(2) nano-TiO2Load capacity on cotton based carbon fiber surface can pass through butyl titanate in reaction system and cotton
The mass ratio of base carbon fibre, which facilitates, to be regulated and controled；
(3) with unsupported nano-TiO2It compares, nano-TiO can be effectively prevent2Reunion, and its catalyst is using
After can by filtering be recycled, recycle it is convenient and simple.
Detailed description of the invention
Fig. 1 a is the scanning electron microscope (SEM) photograph of cotton based carbon fiber prepared by the embodiment of the present invention 1；
Fig. 1 b and Fig. 1 c are TiO prepared by the embodiment of the present invention 12/ cotton based carbon fiber photochemical catalyst is in different times magnifications
Scanning electron microscope (SEM) photograph under several；
Fig. 2 is that the embodiment of the present invention 1 prepares TiO2/ cotton based carbon fiber photochemical catalyst and commercially available P25 nano-TiO2In phase
With the degradation curve of photo-catalytic degradation of methyl-orange under experiment condition；
Fig. 3 is TiO of the present invention2The preparation method flow chart of/cotton based carbon fiber photochemical catalyst.
Specific embodiment
In order to which objects and advantages of the present invention are more clearly understood, the present invention is carried out specifically with reference to embodiments
It is bright.It should be appreciated that following text is only used to describe one or more of specific embodiments of the invention, not to the present invention
The protection scope specifically requested carries out considered critical.
Embodiment 1
(1) by clean cotton in tube furnace 500 DEG C of carbonization 2h under nitrogen atmosphere, obtain cotton based carbon fiber；
(2) in the HCl solution of 50mL 2mol/L, it is quickly added with stirring 0.84g butyl titanate, after solution clarification
It is transferred in water heating kettle, adds 0.20g cotton based carbon fiber, 150 DEG C of hydro-thermal reaction 12h；
(3) product is filtered, is washed with water, dried in an oven, finally 450 DEG C of roastings under nitrogen atmosphere in tube furnace
4h obtains TiO2/ cotton based carbon fiber photochemical catalyst.
The TiO obtained according to above-mentioned steps2TiO in/cotton based carbon fiber photochemical catalyst2Content is 46.6%.
Embodiment 2
4 groups of parallel laboratory tests are designed, investigate butyl titanate additional amount to TiO2TiO in/cotton based carbon fiber photochemical catalyst2Contain
The influence of amount, butyl titanate additional amount are respectively 0.21g, 0.42g, 0.84g and 1.68g, remaining step and experiment condition and reality
It is identical to apply example 1.
TiO in photochemical catalyst made from the different butyl titanate additional amounts of table 12The content table of comparisons
Seen from table 1, TiO2TiO in/cotton based carbon fiber photochemical catalyst2Content can pass through metatitanic acid fourth in reaction system
The additional amount of ester facilitates control, with the increase of butyl titanate additional amount, TiO in photochemical catalyst2Content is gradually increased.For table
The sample that in 1 prepared by group number 1 and 2, butyl titanate additional amount is less, and the surface of cotton base charcoal is not used effectively, cotton base charcoal
There are many surfaces not by TiO2Particle covering；For sample prepared by group number 4 in table 1, since butyl titanate additional amount is excessive, produce
Raw TiO2It has been more than the load limit of cotton base charcoal, many of product is scattered in except cotton carbon fiber and is not supported TiO2
Particle；The preparation condition of group number 3 is best, and cotton base carbon surface is almost by TiO2It is covered, while not also being supported
The TiO being scattered2Particle.
Embodiment 3
4 groups of parallel laboratory tests are designed, investigate the carburizing temperature of cotton to TiO2The preparation of/cotton based carbon fiber photochemical catalyst and production
TiO in object2The influence of content, the carburizing temperature of cotton are respectively 200 DEG C, 300 DEG C, 500 DEG C and 800 DEG C, remaining step and reality
It is same as Example 1 to test condition.
The different cotton carburizing temperatures of table 2 are to TiO2TiO in the preparation of/cotton based carbon fiber photochemical catalyst and product2Content influences
The table of comparisons
As can be seen from Table 2, cotton carburizing temperature is for TiO2TiO in the preparation of/cotton based carbon fiber photochemical catalyst and product2Contain
Measurer has a major impact.For group number 1, since carburizing temperature is lower, carbonized product organic matter is higher, after hydro-thermal reaction,
Obtained product is in grey black pulpous state, shows that the Carbon fibe obtained under low carburizing temperature is destroyed under hydrothermal conditions；Carbonization
When temperature is higher than 300 DEG C (group number 2,3 and 4), obtained cotton based carbon fiber is stable under hydrothermal conditions；Carburizing temperature is for cotton
Flower based carbon fiber is to TiO2Load have a major impact, as can be seen from Table 2, carburizing temperature is higher, the TiO of load2It is fewer.This be by
Higher in carburizing temperature, carbon fiber surface polar group tails off, and is unfavorable for TiO2Load on its surface.
Embodiment 4
4 groups of parallel laboratory tests are designed, investigate concentration of hydrochloric acid to TiO2In the preparation of/cotton based carbon fiber photochemical catalyst and product
TiO2The influence of content, concentration of hydrochloric acid are respectively 1.0mol/L, 2.0mol/L, 4.0mol/L and 6.0mol/L, remaining step and
Experiment condition is same as Example 1.
The different concentration of hydrochloric acid of table 3 are to TiO2TiO in the preparation of/cotton based carbon fiber photochemical catalyst and product2Content influences control
Table
Seen from table 3, in reaction system concentration of hydrochloric acid for TiO2In the preparation of/cotton based carbon fiber photochemical catalyst and product
TiO2Content has great influence.For group number 1, since concentration of hydrochloric acid is lower, when butyl titanate is added, butyl titanate hydrolysis
Generate many white precipitates, it is difficult to dissolve；When improving concentration of hydrochloric acid (group number 2,3 and 4), after butyl titanate is added, under stirring
To clear solution；Concentration of hydrochloric acid is for cotton based carbon fiber to TiO2Load have a major impact, seen from table 3, hydrochloric acid is dense
Spend higher, the TiO of load2It is fewer.This is because concentration of hydrochloric acid is higher, butyl titanate hydrolysis is slower, thus anti-in same hydrolysis
The TiO generated between seasonable2It is fewer.
Embodiment 5
3 groups of parallel laboratory tests are designed, investigate hydrothermal temperature to TiO2The preparation of/cotton based carbon fiber photochemical catalyst and product
Middle TiO2The influence of content, hydrothermal temperature are respectively 130 DEG C, 150 DEG C and 180 DEG C, remaining step and experiment condition and embodiment 1
It is identical.
The different hydrothermal temperatures of table 4 are to TiO2TiO in the preparation of/cotton based carbon fiber photochemical catalyst and product2Content influences
The table of comparisons
By table 4 as it can be seen that hydrothermal temperature is for TiO2TiO in the preparation of/cotton based carbon fiber photochemical catalyst and product2Contain
Measurer has a major impact.For group number 1, since hydrothermal temperature is lower, hydro-thermal reaction is slow, so that being supported on cotton base charcoal
TiO on fiber2It is less；For group number 3, since hydro-thermal reaction is excessively high, hydro-thermal reaction is fast, a large amount of hydrolysate liquid phase at
Core, and the TiO being supported on cotton based carbon fiber2It is less.Therefore, 150 DEG C of hydrothermal temperature is best.
Above in conjunction with embodiment, the embodiments of the present invention are described in detail, but the present invention is not limited to above-mentioned realities
Mode is applied, for those skilled in the art, in knowing the present invention after contents, is not departing from this hair
Under the premise of bright principle, several same transformation and substitution can also be made to it, these convert and substitute on an equal basis and also should be regarded as belonging to
In protection scope of the present invention.
Claims (6)
1. a kind of TiO2The preparation method of/cotton based carbon fiber photochemical catalyst, it is characterised in that the following steps are included:
S1. by clean cotton 300~800 DEG C of carbonization 2h in a nitrogen atmosphere, cotton based carbon fiber is obtained；
S2. in HCl solution, butyl titanate is added in stirring, is transferred in water heating kettle, is added in step (1) after solution clarification
The cotton based carbon fiber of preparation, hydro-thermal reaction 12h；
S3. the product of step S2 is filtered, is washed with water, dries in an oven, finally roast 4h in a nitrogen atmosphere, obtains
TiO2/ cotton based carbon fiber photochemical catalyst.
2. TiO according to claim 12The preparation method of/cotton based carbon fiber photochemical catalyst, it is characterised in that: step S2
The concentration of middle HCl solution is 2~6mol/L.
3. TiO according to claim 1 or 22The preparation method of/cotton based carbon fiber photochemical catalyst, it is characterised in that: step
The mass ratio of butyl titanate, cotton based carbon fiber and HCl solution is 1.05~8.4:1:250 in rapid S2.
4. TiO according to claim 12The preparation method of/cotton based carbon fiber photochemical catalyst, it is characterised in that: the water
The temperature of thermal response is 150~180 DEG C.
5. TiO according to claim 12The preparation method of/cotton based carbon fiber photochemical catalyst, it is characterised in that: the roasting
Burning temperature is 450 DEG C.
6. a kind of TiO2/ cotton based carbon fiber photochemical catalyst, it is characterised in that: be by of any of claims 1-5
TiO2The preparation method of/cotton based carbon fiber photochemical catalyst is made.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201811439422.3A CN109277097A (en) | 2018-11-29 | 2018-11-29 | A kind of TiO2/ cotton based carbon fiber photochemical catalyst and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811439422.3A CN109277097A (en) | 2018-11-29 | 2018-11-29 | A kind of TiO2/ cotton based carbon fiber photochemical catalyst and preparation method thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110180520A (en) * | 2019-05-08 | 2019-08-30 | 陕西科技大学 | A kind of recyclable mesoporous carbon@TiO2/ carbon fiber catalysis material and preparation method thereof |
| CN110732338A (en) * | 2019-10-25 | 2020-01-31 | 湖北工业大学 | Carbon nanowire/g-C3N4Composite visible light catalyst and preparation method thereof |
| CN113716605A (en) * | 2021-09-22 | 2021-11-30 | 重庆文理学院 | Wavy black TiO2Preparation method of micron tube |
-
2018
- 2018-11-29 CN CN201811439422.3A patent/CN109277097A/en active Pending
Non-Patent Citations (1)
| Title |
|---|
| 和娇娇等: ""天然炭纤维负载二氧化钛颗粒的制备与光催化活性"", 《硅酸盐通报》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110180520A (en) * | 2019-05-08 | 2019-08-30 | 陕西科技大学 | A kind of recyclable mesoporous carbon@TiO2/ carbon fiber catalysis material and preparation method thereof |
| CN110732338A (en) * | 2019-10-25 | 2020-01-31 | 湖北工业大学 | Carbon nanowire/g-C3N4Composite visible light catalyst and preparation method thereof |
| CN110732338B (en) * | 2019-10-25 | 2022-08-09 | 湖北工业大学 | Carbon nanowire/g-C 3 N 4 Composite visible light catalyst and preparation method thereof |
| CN113716605A (en) * | 2021-09-22 | 2021-11-30 | 重庆文理学院 | Wavy black TiO2Preparation method of micron tube |
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Application publication date: 20190129 |