CN110124649A - A kind of preparation method of the carbon material supported photocatalyst composite material of porous graphiteization - Google Patents
A kind of preparation method of the carbon material supported photocatalyst composite material of porous graphiteization Download PDFInfo
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- CN110124649A CN110124649A CN201910404748.0A CN201910404748A CN110124649A CN 110124649 A CN110124649 A CN 110124649A CN 201910404748 A CN201910404748 A CN 201910404748A CN 110124649 A CN110124649 A CN 110124649A
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- photocatalyst
- timber
- composite material
- preparation
- porous carbon
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- 239000011941 photocatalyst Substances 0.000 title claims abstract description 59
- 239000002131 composite material Substances 0.000 title claims abstract description 16
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 239000003575 carbonaceous material Substances 0.000 title description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 31
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 25
- 239000002023 wood Substances 0.000 claims abstract description 14
- 238000001035 drying Methods 0.000 claims abstract description 6
- 238000002604 ultrasonography Methods 0.000 claims abstract description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 4
- 239000011121 hardwood Substances 0.000 claims description 2
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- 238000001914 filtration Methods 0.000 claims 1
- 239000007788 liquid Substances 0.000 claims 1
- 230000003197 catalytic effect Effects 0.000 abstract description 3
- 238000004375 physisorption Methods 0.000 abstract description 3
- 238000000280 densification Methods 0.000 abstract 1
- 238000000034 method Methods 0.000 description 8
- 239000000463 material Substances 0.000 description 7
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 6
- 239000003054 catalyst Substances 0.000 description 4
- 238000011049 filling Methods 0.000 description 4
- 229910002804 graphite Inorganic materials 0.000 description 4
- 239000010439 graphite Substances 0.000 description 4
- 238000005087 graphitization Methods 0.000 description 4
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 238000000137 annealing Methods 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 201000010099 disease Diseases 0.000 description 2
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000002708 enhancing effect Effects 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- -1 formaldehyde, benzene class Chemical class 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000007654 immersion Methods 0.000 description 2
- 239000012299 nitrogen atmosphere Substances 0.000 description 2
- 238000007146 photocatalysis Methods 0.000 description 2
- 230000001699 photocatalysis Effects 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- PMZURENOXWZQFD-UHFFFAOYSA-L sodium sulphate Substances [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 240000005020 Acaciella glauca Species 0.000 description 1
- 235000017166 Bambusa arundinacea Nutrition 0.000 description 1
- 235000017491 Bambusa tulda Nutrition 0.000 description 1
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- 244000082204 Phyllostachys viridis Species 0.000 description 1
- 235000015334 Phyllostachys viridis Nutrition 0.000 description 1
- 229910021607 Silver chloride Inorganic materials 0.000 description 1
- 240000007313 Tilia cordata Species 0.000 description 1
- 240000007591 Tilia tomentosa Species 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000011425 bamboo Substances 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003610 charcoal Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000005367 electrostatic precipitation Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000003837 high-temperature calcination Methods 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- VUZPPFZMUPKLLV-UHFFFAOYSA-N methane;hydrate Chemical compound C.O VUZPPFZMUPKLLV-UHFFFAOYSA-N 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 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
- 238000011056 performance test Methods 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 235000003499 redwood Nutrition 0.000 description 1
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052938 sodium sulfate Inorganic materials 0.000 description 1
- 230000001954 sterilising effect Effects 0.000 description 1
- 238000000967 suction filtration Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000004506 ultrasonic cleaning Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 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
-
- B01J35/33—
-
- B01J35/39—
-
- B01J35/60—
-
- B01J35/61—
Abstract
The invention discloses a kind of preparation methods of porous carbon load photocatalyst composite material, include the following steps: S1: wood is cut along the direction of timber conduit, and cut lengths are 1 ~ 5mm, dry after ultrasound；S2: 8 ~ 10 h are calcined at being 800 ~ 1200 DEG C in temperature by the timber after drying；S3: calcined timber is ultrasonic, the timber after photocatalyst solution to be poured into ultrasound, dry, 1.5 ~ 2.5 h that anneal at 350 ~ 400 DEG C load photocatalyst composite material to get to porous carbon.Graphited timber and photocatalyst can be carried out good combination, be greatly improved the application range of photocatalyst, enhance the catalytic activity of photocatalyst by the present invention by simply handling.While the hole configurations of graphited timber densification provides condition for the attachment of photocatalyst, also there is physisorption, extend the application range of photocatalyst.
Description
Technical field
The invention belongs to photocatalysis fields, and in particular to a kind of carbon material supported photocatalyst composite material of porous graphiteization
Preparation method.
Background technique
With society, the continuous development of science and technology, the change of leap is brought to people's lives quality, can not ignore simultaneously
, every environmental problem also threatens people's health therewith.Wherein indoor environmental pollution has seriously perplexed the day of people
Often life.Show that the number of indoor environmental pollution is died of up to 2,800,000 in the whole world every year according to WTO relevant information, so, it is indoor dirty
The solution of the problem of dye is anxious to new breakthrough.It is reported that having about 68 % human body diseases there are 300 multiple pollutants in room air
Disease is related with indoor pollution.Wherein formaldehyde, benzene class TVOC are most representative.
The most common administering method of indoor pollution has at present: 1. physisorphtions.2. ozone purification method.3. electrostatic precipitation
Method.4. the negative oxygen ion method of purification.5. sterilizing and purifying method.6. photocatalyst light degradation method.
Photocatalyst is a kind of using Nano titanium dioxide as the total of the photosemiconductor material with photo-catalysis function of representative
Title is current most clean surrounding purifying material most safe in the world and currently the only other than natural light, does not need volume
The outer consumption energy can persistently remove a kind of material of formaldehyde and purifying air.Photocatalyst generates tool under the irradiation of light in air
There is the free group of Strong oxdiative-reproducibility, to decompose the organic compound in air, is broken down into harmless carbon dioxide
And water, to achieve the purpose that purify air.
Summary of the invention
The purpose of the present invention is photocatalyst is poured into active carbon inside and surface, by annealing so that both materials are tighter
Close combination can be applied to environmentally friendly furniture, strainer, filter core etc..
The purpose of the present invention is achieved by the following technical programs:
The present invention provides a kind of preparation methods of porous carbon load photocatalyst composite material, include the following steps:
S1: wood is cut along the direction of timber conduit, and cut lengths are 1 ~ 5 mm, is dried after ultrasound；
S2: 8 ~ 10 h are calcined at being 800 ~ 1200 DEG C in temperature by the timber after drying；
S3: calcined timber is ultrasonic, the timber after photocatalyst solution to be poured into ultrasound, it is dry, it is moved back at 350 ~ 400 DEG C
1.5 ~ 2.5 h of fire load photocatalyst composite material to get to porous carbon.
Preferably, the type of wood is hardwood in step S1.Such as linden, redwood, bamboo etc..
Preferably, it is calcined under nitrogen atmosphere in S2, air-flow is 180 ~ 200 sccm within most junior three hour, most
Seven hours are 40 ~ 60 sccm afterwards；Heating rate is 10 ~ 50 DEG C/min.
Preferably, photocatalyst is injected in timber using suction filtration in step S3.
Preferably, the mass concentration of photocatalyst is 0.1%-0.5% in photocatalyst solution.
Inventors have found that the harder timber of material density is cut according to perpendicular to section, protected down by nitrogen atmosphere
Timber can be graphitized by high-temperature process, and the conduit of timber forms natural hole, and gauffer provides for the load of photocatalyst
Condition, increases the specific surface area of photocatalyst, and conductivity will greatly improve, so that it is in addition to conventional carbon
It is also conductive other than absorption property, in conjunction with photocatalyst material, be theoretically greatly improved the application range of photocatalyst with
And the catalytic activity of enhancing photocatalyst.While its fine and close hole configurations provides condition for the attachment of photocatalyst, also have
Physisorption extends the application range of photocatalyst.
Compared with prior art, the present invention has following technical effect that
Graphited timber and photocatalyst can be carried out good combination, are greatly improved by the present invention by simply handling
The application range of photocatalyst and the catalytic activity for enhancing photocatalyst.Its fine and close hole configurations provides for the attachment of photocatalyst
While condition, also there is physisorption, extend the application range of photocatalyst.
Detailed description of the invention
Fig. 1 is preparation flow figure of the invention；
(a) is the wood chip before graphitization in Fig. 2, is (b) wood chip after graphitization；
(a) is SEM figure in carbon plate section after filling photocatalyst in Fig. 3, (b) is schemed to fill partial enlargement SEM after photocatalyst, is (c) filling light
Carbon plate faces SEM figure after catalyst.
(a) is the wood chip XRD spectrum after graphitization in Fig. 4, (b) loads photocatalyst XRD spectrum for porous carbon materials.
Fig. 5 is that the wood chip after pouring into photocatalyst is schemed with the wood chip photoresponse current vs for not filling photocatalyst.
Specific embodiment
To make the object, technical solutions and advantages of the present invention clearer, combined with specific embodiments below to of the invention
Technical solution is described in detail.Obviously, described embodiments are only a part of the embodiments of the present invention, rather than all
Embodiment.Based on the embodiments of the present invention, those of ordinary skill in the art are without making creative work
Obtained all other embodiment belongs to the range that the present invention is protected.
Except specified otherwise, equipment used in the present embodiment is routine experiment equipment, and reagent used is that analysis is pure
Reagent.
Embodiment 1
Linden wood is cut perpendicular to timber conduit, about 2 mm thickness of cut lengths is tentatively polished with coarse sandpaper
It is smooth, as half an hour ultrasonic in ultrasonic cleaning machine, drying.
Wood chip obtained in the previous step is subjected to calcining 10 in nitrogen environment as in high vacuum tube furnace with 1000 DEG C
It is 200 sccm in h, most junior three hour, last seven hours are 60 sccm.Heating rate is 20 DEG C/min.
By the carbon plate after charing obtained in the previous step, polished flat with fine sandpaper.It is cleaned by ultrasonic again 10 minutes.Then as
At the filter core of nutsch filter, by the P25 titania solution prepared (0.1 g/L 100mL) as being taken out in nutsch filter
Filter, obtains the carbon plate for pouring into photocatalyst.
The carbon plate obtained in the previous step for pouring into photocatalyst is placed in 60 DEG C of 2 h of drying of drying box, then is placed in vacuum tube furnace
In 400 DEG C of 2 h of annealing, activated carbon surface can be obtained and inner conduit loads the composite material of photocatalyst.
Fig. 3 show the carbon plate SEM figure after filling photocatalyst.Wherein (a) is sectional view, it can be seen that TiO2Successfully fill
Enter to wood chip catheter interior.Wood chip does not destroy the structure of itself after high-temperature calcination, makes its natural cavernous structure, is
The attachment of photocatalyst and absorption organic pollutant provide structure basis.(b) figure is partial cross section's enlarged drawing.(c) figure is charcoal
Piece/photocatalyst composite material front view, it can be seen that part TiO2It is attached to carbon plate conduit channel surfaces.
Performance test:
(1) pattern measures
The SEM figure provided by Fig. 3 for embodiment, sectional view, section partial enlarged view and front view, by means of the present invention
Photocatalyst can be poured into well to the inside and surface of graphitized stephanoporate material with carbon element.Realize answering for photocatalyst and porous carbon materials
It closes.
(2) structure determination
If Fig. 4 is the XRD x ray diffraction map that embodiment provides.As seen from the figure, in 2 θ=23 °, nearby there are two opposite for 2 θ=44 °
Weaker diffraction maximum, this respectively corresponds (002) and (100) crystal face of crystal structure of graphite, by graphited carbon plate
What diffraction maximum can determine whether the graphite crystallization to be formed is not very well, may there is segmental defect, so causing diffraction maximum very weak, fills light
The carbon plate figure of catalyst is in TiO2In the very strong situation of peak intensity, the peak of graphite is by TiO2Diffraction maximum cover, naked eyes almost
It can't see the presence of graphite peaks.
(3) light-catalyzed reaction measures
This test utilize electrochemical workstation three-electrode system, i.e. Pt be to electrode, Ag/AgCl is reference electrode, along with to
The three-electrode system for surveying electrode composition, the Na for being 1 mol/l with concentration2SO4Sodium sulphate be electrolyte, add 0.03 V bias.With
Sample in embodiment is used as working electrode, and light source is 200 W xenon lamps.The present embodiment is in order to compare, by the light of same concentrations
Carbon plate after graphitization is carried out immersion treatment by catalyst solution, as shown in figure 5, only pouring into the carbon plate (light in other words of photocatalyst
Catalyst imports internal) just generate stronger photoelectric current as electrode, illustrate cannot to make only by immersion photocatalyst performance compared with
Good effect.
Claims (6)
1. a kind of preparation method of porous carbon load photocatalyst composite material, which comprises the steps of:
S1: wood is cut along the direction of timber conduit, and cut lengths are 1 ~ 5 mm, is dried after ultrasound；
S2: 8 ~ 10 h are calcined at being 800 ~ 1200 DEG C in temperature by the timber after drying；
S3: calcined timber is ultrasonic, the timber after photocatalyst solution to be poured into ultrasound, it is dry, it is moved back at 350 ~ 400 DEG C
1.5 ~ 2.5 h of fire load photocatalyst composite material to get to porous carbon.
2. the preparation method of porous carbon load photocatalyst composite material according to claim 1, which is characterized in that in step S1
The type of wood is hardwood.
3. the preparation method of porous carbon load photocatalyst composite material according to claim 1, which is characterized in that in nitrogen in S2
Atmosphere is calcined under enclosing, and air-flow is 180 ~ 200 sccm within most junior three hour, and last seven hours are 40 ~ 60 sccm；It rises
Warm speed is 10 ~ 50 DEG C/min.
4. the preparation method of porous carbon load photocatalyst composite material according to claim 1, which is characterized in that in step S3
Photocatalyst is injected in timber using filtering.
5. the preparation method of porous carbon load photocatalyst composite material according to claim 1, which is characterized in that photocatalyst is molten
The mass concentration of photocatalyst is 0.1%-0.5% in liquid.
6. it is a kind of according to claim 1 ~ 5 in the obtained porous carbon load photocatalyst composite material of any preparation method.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910404748.0A CN110124649A (en) | 2019-05-16 | 2019-05-16 | A kind of preparation method of the carbon material supported photocatalyst composite material of porous graphiteization |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910404748.0A CN110124649A (en) | 2019-05-16 | 2019-05-16 | A kind of preparation method of the carbon material supported photocatalyst composite material of porous graphiteization |
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| CN110124649A true CN110124649A (en) | 2019-08-16 |
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| CN201910404748.0A Withdrawn CN110124649A (en) | 2019-05-16 | 2019-05-16 | A kind of preparation method of the carbon material supported photocatalyst composite material of porous graphiteization |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2023107038A1 (en) * | 2021-12-07 | 2023-06-15 | T.C. Ankara Universitesi Rektorlugu | A method of producing support material for photocatalyst from waste masks |
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| CN1970141A (en) * | 2005-11-24 | 2007-05-30 | 严义清 | Nano photo-catalytic modified carbon adsorption-sterilization material and preparing process thereof |
| CN101780952A (en) * | 2010-03-26 | 2010-07-21 | 上海交通大学 | Method for preparing loading functional oxide porous carbon |
| KR20110082749A (en) * | 2010-01-12 | 2011-07-20 | 한밭대학교 산학협력단 | Active carbon and manufacturing method thereof, and filter with the same |
| CN103041796A (en) * | 2011-10-17 | 2013-04-17 | 中国石油化工股份有限公司 | TiO2 photocatalyst and preparation method thereof |
| CN109174141A (en) * | 2018-10-12 | 2019-01-11 | 宝鸡文理学院 | A kind of preparation method of composite Nano catalysis material |
| CN109225224A (en) * | 2018-10-24 | 2019-01-18 | 北方民族大学 | Wooden macroporous carbon catalysis electrode material and its preparation method and application |
-
2019
- 2019-05-16 CN CN201910404748.0A patent/CN110124649A/en not_active Withdrawn
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1970141A (en) * | 2005-11-24 | 2007-05-30 | 严义清 | Nano photo-catalytic modified carbon adsorption-sterilization material and preparing process thereof |
| KR20110082749A (en) * | 2010-01-12 | 2011-07-20 | 한밭대학교 산학협력단 | Active carbon and manufacturing method thereof, and filter with the same |
| CN101780952A (en) * | 2010-03-26 | 2010-07-21 | 上海交通大学 | Method for preparing loading functional oxide porous carbon |
| CN103041796A (en) * | 2011-10-17 | 2013-04-17 | 中国石油化工股份有限公司 | TiO2 photocatalyst and preparation method thereof |
| CN109174141A (en) * | 2018-10-12 | 2019-01-11 | 宝鸡文理学院 | A kind of preparation method of composite Nano catalysis material |
| CN109225224A (en) * | 2018-10-24 | 2019-01-18 | 北方民族大学 | Wooden macroporous carbon catalysis electrode material and its preparation method and application |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2023107038A1 (en) * | 2021-12-07 | 2023-06-15 | T.C. Ankara Universitesi Rektorlugu | A method of producing support material for photocatalyst from waste masks |
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