CN107252696A - A kind of preparation method of sisal hemp carbon fiber photochemical catalyst - Google Patents
A kind of preparation method of sisal hemp carbon fiber photochemical catalyst Download PDFInfo
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- CN107252696A CN107252696A CN201710626824.3A CN201710626824A CN107252696A CN 107252696 A CN107252696 A CN 107252696A CN 201710626824 A CN201710626824 A CN 201710626824A CN 107252696 A CN107252696 A CN 107252696A
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- carbon fiber
- sisal hemp
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- solution
- molybdenum disulfide
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- 244000198134 Agave sisalana Species 0.000 title claims abstract description 91
- 235000011624 Agave sisalana Nutrition 0.000 title claims abstract description 79
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims abstract description 76
- 229920000049 Carbon (fiber) Polymers 0.000 title claims abstract description 75
- 239000004917 carbon fiber Substances 0.000 title claims abstract description 75
- 238000002360 preparation method Methods 0.000 title claims abstract description 36
- 239000003054 catalyst Substances 0.000 title claims abstract description 27
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 claims abstract description 57
- 229910052982 molybdenum disulfide Inorganic materials 0.000 claims abstract description 57
- 239000002096 quantum dot Substances 0.000 claims abstract description 40
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 35
- 238000001354 calcination Methods 0.000 claims abstract description 15
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 14
- 239000000243 solution Substances 0.000 claims description 49
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 41
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 39
- 229910001868 water Inorganic materials 0.000 claims description 22
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 21
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 20
- 239000008367 deionised water Substances 0.000 claims description 20
- 229910021641 deionized water Inorganic materials 0.000 claims description 18
- 239000000835 fiber Substances 0.000 claims description 16
- 239000007864 aqueous solution Substances 0.000 claims description 15
- 229960000583 acetic acid Drugs 0.000 claims description 10
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 claims description 10
- 238000001914 filtration Methods 0.000 claims description 10
- 239000007787 solid Substances 0.000 claims description 10
- 239000012362 glacial acetic acid Substances 0.000 claims description 9
- 238000010792 warming Methods 0.000 claims description 9
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 8
- 229910019964 (NH4)2MoS4 Inorganic materials 0.000 claims description 7
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 7
- 239000000706 filtrate Substances 0.000 claims description 7
- VWDWKYIASSYTQR-YTBWXGASSA-N sodium;dioxido(oxo)azanium Chemical compound [Na+].[O-][15N+]([O-])=O VWDWKYIASSYTQR-YTBWXGASSA-N 0.000 claims description 7
- 230000015572 biosynthetic process Effects 0.000 claims description 5
- 238000006243 chemical reaction Methods 0.000 claims description 5
- 239000003638 chemical reducing agent Substances 0.000 claims description 5
- 239000011365 complex material Substances 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- 238000001704 evaporation Methods 0.000 claims description 5
- 230000008020 evaporation Effects 0.000 claims description 5
- 239000011261 inert gas Substances 0.000 claims description 5
- 239000012982 microporous membrane Substances 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 5
- 230000035484 reaction time Effects 0.000 claims description 5
- 239000002904 solvent Substances 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 239000000725 suspension Substances 0.000 claims description 5
- 239000000047 product Substances 0.000 claims description 3
- 238000000502 dialysis Methods 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 14
- 229910052799 carbon Inorganic materials 0.000 abstract description 9
- 150000001875 compounds Chemical class 0.000 abstract description 8
- 238000000034 method Methods 0.000 abstract description 8
- 239000000463 material Substances 0.000 abstract description 6
- 239000008187 granular material Substances 0.000 abstract description 5
- 239000003575 carbonaceous material Substances 0.000 abstract description 4
- 238000006555 catalytic reaction Methods 0.000 abstract description 4
- 230000000694 effects Effects 0.000 abstract description 4
- 230000003287 optical effect Effects 0.000 abstract description 3
- 238000004065 wastewater treatment Methods 0.000 abstract description 3
- 230000008569 process Effects 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract 1
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical class [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 abstract 1
- 238000001179 sorption measurement Methods 0.000 abstract 1
- 230000015556 catabolic process Effects 0.000 description 6
- 238000006731 degradation reaction Methods 0.000 description 6
- 238000002604 ultrasonography Methods 0.000 description 5
- 230000003197 catalytic effect Effects 0.000 description 4
- 239000003610 charcoal Substances 0.000 description 4
- 230000001699 photocatalysis Effects 0.000 description 4
- 238000007146 photocatalysis Methods 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 3
- 229910052802 copper Inorganic materials 0.000 description 3
- 239000010949 copper Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 229910052709 silver Inorganic materials 0.000 description 3
- 239000004332 silver Substances 0.000 description 3
- 235000017166 Bambusa arundinacea Nutrition 0.000 description 2
- 235000017491 Bambusa tulda Nutrition 0.000 description 2
- 239000002028 Biomass Substances 0.000 description 2
- 244000060011 Cocos nucifera Species 0.000 description 2
- 235000013162 Cocos nucifera Nutrition 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- 244000082204 Phyllostachys viridis Species 0.000 description 2
- 235000015334 Phyllostachys viridis Nutrition 0.000 description 2
- 239000011425 bamboo Substances 0.000 description 2
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 239000003344 environmental pollutant Substances 0.000 description 2
- 125000004185 ester group Chemical group 0.000 description 2
- 125000000524 functional group Chemical group 0.000 description 2
- 229910021389 graphene Inorganic materials 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 239000002957 persistent organic pollutant Substances 0.000 description 2
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 2
- 231100000719 pollutant Toxicity 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 238000000197 pyrolysis Methods 0.000 description 2
- 239000010865 sewage Substances 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- LLYXJBROWQDVMI-UHFFFAOYSA-N 2-chloro-4-nitrotoluene Chemical compound CC1=CC=C([N+]([O-])=O)C=C1Cl LLYXJBROWQDVMI-UHFFFAOYSA-N 0.000 description 1
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- 241000790917 Dioxys <bee> Species 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 238000005411 Van der Waals force Methods 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-O ammonium group Chemical group [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000012620 biological material Substances 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 230000001186 cumulative effect Effects 0.000 description 1
- 238000005202 decontamination Methods 0.000 description 1
- 230000003588 decontaminative effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 239000003651 drinking water Substances 0.000 description 1
- 235000020188 drinking water Nutrition 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 239000010903 husk Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 238000003780 insertion Methods 0.000 description 1
- 230000037431 insertion Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 229910052961 molybdenite Inorganic materials 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 239000002135 nanosheet Substances 0.000 description 1
- 239000001814 pectin Substances 0.000 description 1
- 235000010987 pectin Nutrition 0.000 description 1
- 229920001277 pectin Polymers 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000027756 respiratory electron transport chain Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 238000003911 water pollution 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
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/04—Sulfides
- B01J27/047—Sulfides with chromium, molybdenum, tungsten or polonium
- B01J27/051—Molybdenum
- B01J27/0515—Molybdenum with iron group metals or platinum group metals
-
- 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
-
- 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
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Catalysts (AREA)
Abstract
The present invention relates to wastewater treatment catalysis material field, disclose a kind of preparation method of sisal hemp carbon fiber photochemical catalyst, it is the porous carbon fiber with very strong adsorption effect first by sisal hemp calcining, titanium dioxide nano granule and molybdenum disulfide quantum dot are loaded on porous carbon by sol-gal process, the porous carbon materials of tri compound are obtained.Photochemical catalyst not only reduces the energy gap of titanium dioxide, enhances the transfer efficiency of electronics, improves the visible light-responded scope of catalyst, and modified titanium dioxide optical catalyst has response to wavelength >=460nm visible ray；The present invention makes full use of natural sisal hemp, realizes the efficient utilization of resource, meets the Ecological Concept of green.The preparation method technique of chemically modified sisal hemp carbon fiber photochemical catalyst is simple, cost is low, it is adaptable to industrialized production.
Description
Technical field
The present invention relates to wastewater treatment catalysis material field, more particularly to a kind of preparation side of sisal hemp carbon fiber photochemical catalyst
Method.
Background technology
Water pollution is always that people pay close attention to most environmental problems, and the kind and discharge capacity of waste water print in cumulative year after year
Contaminate waste water one of major polluting sources as water system environment.There are various carbon materials to be synthesized at present to prepare and applied to light
Catalytic field, includes mesoporous carbon, graphene, CNT etc..But in view of the large-scale application of photochemical catalyst, with renewable
Biomass be raw material prepare high performance catalysis material, can not only realize the high value added utilization of biomass, and
Effectively reduce the cost of photochemical catalyst.Sisal hemp carbon fiber is product of the sisal fiber after high temperature pyrolysis.
Conductor photocatalysis degradation technique is the environment that a kind of most possible utilization nature sunshine realizes cleaning decontamination
Friendly technology, oneself is as the more method of wastewater treatment of people's concern at present.Two in numerous photocatalysis semi-conducting materials
Titania photocatalyst has the advantages that cheap, pollution-free, anti-light corrosion is described as environment-friendly pollution processing material, its ring
Protect and the application prospect of energy-conservation is widely paid close attention to.Although numerous organic pollutions can be by under the irradiation of ultraviolet light conditions
TiO2Effectively it is degraded to CO2And H2O, but its utilization ratio is very low under the irradiation of visible ray, and ultraviolet light in sunshine
Only 3% or so, it have impact on TiO2Photocatalytic degradation effect.
Molybdenum disulfide is a kind of typical transition metal two-dimensional layer sulfide, and the molybdenum disulfide of individual layer is by S-Mo-S atoms
Layer is covalently constituted, and is combined between layers by weaker Van der Waals force.With the graphite with two-dimensional layered structure
Alkene is different, and molybdenum disulfide has regulatable bandgap structure.When block molybdenum disulfide is changed into molybdenum disulfide nano sheet layer, two
The energy gap of molybdenum sulfide increases with the reduction of its number of plies.Compared to the graphene of zero band gap, individual layer molybdenum disulfide is shown
More excellent physicochemical characteristics, has very in fields such as optics, lithium ion battery, photoelectrocatalysis, ultracapacitors
High application prospect, has attracted the extensive concern of researcher.At present, on molybdenum disulfide report more rest on nanometer sheet
Layer scope, for MoS2The report of quantum dot is relatively fewer.
The content of the invention
In order to solve the above-mentioned technical problem, the invention provides a kind of preparation method of sisal hemp carbon fiber photochemical catalyst.This
Invention preparation method is the metal-doped porous charcoal such as silver, copper first by sisal fiber calcining, by sol-gal process by dioxy
Change titanium nanoparticle and molybdenum disulfide quantum dot is loaded on porous carbon, obtain the porous carbon materials of tri compound.Such modification
The photoresponse scope of titanium dioxide is substantially increased, and serves the purpose of degradation of organic substances pollutant.
The present invention concrete technical scheme be：A kind of preparation method of sisal hemp carbon fiber photochemical catalyst, comprises the following steps：
Step 1：The preparation of sisal hemp carbon fiber：Sisal fiber is soaked with the NaOH aqueous solution, then rinsed with water to neutrality, then is used
Ammonium dibasic phosphate aqueous solution impregnates, and pulls out, dries；Dried sisal fiber will be pre-processed and be put into calcining in Muffle furnace, cooling
Porous sisal hemp carbon fiber is obtained afterwards.
Step 2：Sisal hemp carbon fiber in step 1 is placed on (NH4)2S2O8Ultrasonic in solution, filtering is clear with deionized water
95-105g/L NaOH solution 4-6min is immersed in after washing, the unreacted (NH in surface is washed with deionized water4)2S2O8。
Step 3：The preparation of molybdenum disulfide quantum dot：By (NH4)2MoS4It is dissolved in water, ultrasonic 10-20min, adds
N2H4As reducing agent, mixture is transferred in ptfe autoclave and carries out hydro-thermal reaction, reaction is cooled to room after terminating
Temperature, using 0.22um filtering with microporous membrane, obtained filtrate is dialysed in water, last evaporation solvent, is obtained after drying
Solid extremely molybdenum disulfide quantum dot.
Step 4：Sisal hemp carbon fiber and molybdenum disulfide quantum dot is scattered in deionized water, and ultrasonic 25-35min is obtained
The suspension of sisal hemp carbon fiber/molybdenum disulfide.
Step 5：The preparation of ternary complex material：First ethanol is mixed with butyl titanate, 10-20min is stirred, is formed
Solution A；Sisal hemp carbon fiber/molybdenum disulfide quantum dot solution is mixed with glacial acetic acid again, the solution B of formation；Under stirring,
20-30 by volume:Solution B is slowly dropped in solution A by 25-35, is then placed in 60-80 DEG C of water-bath and is persistently stirred 50-
70min, is made taupe gel, obtained gel is put into after being dried in 60-80 DEG C of baking oven, is heated to 125-135 DEG C and holds
Continuous 10-15min, obtains beige solid；Ground, obtain sisal hemp carbon fiber/titanium dioxide/molybdenum disulfide nano and be combined
Thing.
Preparation method of the present invention is the metal-doped porous charcoals such as silver, copper first by sisal fiber calcining, solidifying by colloidal sol
Glue method loads to titanium dioxide nano granule and molybdenum disulfide quantum dot on porous carbon, obtains the porous carbon materials of tri compound.
Molybdenum disulfide quantum dot is introduced so that TiO2Organic contamination that can effectively in catalytic degradation sewage in visible-range
Thing.And sisal hemp carbon fiber can be very good improve material electrical conductivity and its chemical property, become good electronics by
Body, compensate for the electron-hole pair of titanium dioxide easily compound defect to a certain extent.Such modification substantially increases two
The photoresponse scope of titanium oxide, and serve the purpose of degradation of organic substances pollutant.
Preferably, in step 1, the mass concentration of the NaOH aqueous solution is 5wt%, soak time 20-28 hours, phosphoric acid hydrogen
The mass concentration of two aqueous ammoniums is 5%, and dip time is 20-28 hours.
Be using NaOH aqueous solution soakings in order to remove the pectin on surface, the purpose of ammonium dibasic phosphate aqueous solution dipping be for
The hole count of increase carbon fiber.
Preferably, in step 1, calcining as step calcination：200-300 DEG C is first warming up to, 25-35min is kept, then heat up
To 800-900 DEG C, 2-3h is kept, speed is 5-6 DEG C/min, leads to inert gas.
The purpose of step calcination is to obtain higher porosity.The porous of sisal hemp carbon fiber provide not only bigger ratio
Surface area, it is effective to improve dirt even more in order to which the insertion of titanium dioxide nano granule and molybdenum disulfide quantum dot provides space
Water treatment capacity.
Preferably, in step 2, (NH4)2S2O8The concentration of solution is 100-200g/L, and ultrasonic time is 1-2h.
(NH with oxidation is immersed in by the porous carbon fiber formed after sisal hemp is calcined4)2S2O8Enter in solution
Row is ultrasonically treated, can cause porous carbon surface is oxidized to produce hydroxyl, ester group and carboxyl, and these reactive functional groups are deposited
To the bonded most important of next step and titanium dioxide nano granule.The presence of chemical bond improves electron transfer rate, effectively
The separative efficiency of electron-hole pair must be improved.
Preferably, in step 3, hydrothermal temperature is 150-200 DEG C, and the reaction time is 6-9h；Filtrate dialysis time
For 3-5 days.
For molybdenum disulfide quantum dot is compared with curing molybdenum sheet, molybdenum disulfide quantum dot not only has bigger specific surface area,
Significant edge effect, while having the unique optical property of quantum dot, makes it more with potential applications in field of the present invention.
Preferably, in step 3, (NH4)2MoS4Mass ratio with water is 1:95-105.
Preferably, in step 4, sisal hemp carbon fiber, molybdenum disulfide quantum dot, the mass ratio of deionized water are 1:0.5:
（20-40）.
Preferably, in step 5, the volume ratio of ethanol and butyl titanate is 10 in solution A:1；Sisal hemp carbon in solution B
The volume ratio of fiber/molybdenum disulfide quantum dot solution and glacial acetic acid mixed liquor is 10:1.
Preferably, in step 5, the drop rate of solution B is 1-1.5mL/ seconds.
It is compared with the prior art, the beneficial effects of the invention are as follows：
1st, sisal hemp carbon fiber is product of the sisal fiber after high temperature pyrolysis.In sisal hemp carbon fiber containing potassium, silicon, calcium, magnesium, copper,
The abundant element such as silver, can be very good to improve light-catalysed effect.Sisal hemp Carbon fibe after overactivation, its specific surface area
Up to 1200m2/ more than g, is far longer than the activated carbon of general coconut husk, bamboo charcoal and other conventional matrix, thus with excellent
Absorption and catalytic performance, to a variety of harmful dyestuffs, heavy metal ion and germ in water quality have absorption, degradation.Therefore sword
Numb carbon plays the role of positive to photocatalysis in itself.The abundant pore structure of the invention for utilizing it to produce after firing and energy are effective
Electronics is transmitted, sisal hemp carbon fiber is used for photochemical catalyst.Sisal hemp carbon fiber makees photochemical catalyst, can not only reclaim biological material
Utilize, due to its considerable absorption property and electronic transmission performance, moreover it is possible to efficient degradable organic pollutant.
2nd, (the NH with oxidation is immersed in by the porous carbon formed after sisal fiber is calcined4)2S2O8In solution
Progress is ultrasonically treated, can cause porous carbon surface is oxidized to produce hydroxyl, ester group and carboxyl, these reactive functional groups
In the presence of to the bonded most important of next step and titanium dioxide nano granule.
3rd, the present invention introduces the molybdenum disulfide quantum dot with bigger serface, can cause compound rear TiO2Visible
Organic pollution that can effectively in catalytic degradation sewage in optical range.
4th, the characteristics of present invention is maximum is that the sisal hemp carbon fiber catalysis material for designing and preparing has photo and thermal stability
Good, specific surface area is big, visible ray is wide using wavelength（Wavelength >=460nm）, while having very high visible light photocatalysis active
The advantages of, can as photocatalytic degradation organic pollutant catalyst.
Embodiment
With reference to embodiment, the invention will be further described.
Embodiment 1
A kind of preparation method of sisal hemp carbon fiber photochemical catalyst, comprises the following steps：
Step 1：The preparation of sisal hemp carbon fiber：Sisal fiber is soaked 20 hours with the 5wt% NaOH aqueous solution, then rushed with water
Neutrality is washed till, then is impregnated 20 hours with 5wt% ammonium dibasic phosphate aqueous solution, pulls out, dry；Dried sisal hemp will be pre-processed
Fiber is put into step calcination in Muffle furnace：First it is warming up to 200 DEG C, keeps 35min, then be warming up to 800 DEG C, keeps 3h, speed is 5
DEG C/min, lead to inert gas.Porous sisal hemp carbon fiber is obtained after calcining cooling.
Step 2：Sisal hemp carbon fiber in step 1 is placed on the (NH that concentration is 100g/L4)2S2O8Ultrasound 2h in solution,
Filtering, is immersed in 95g/L NaOH solution 6min, surface is washed with deionized water unreacted after being cleaned with deionized water
(NH4)2S2O8。
Step 3：The preparation of molybdenum disulfide quantum dot：In mass ratio 1:95 by (NH4)2MoS4It is dissolved in water, ultrasound
20min, adds N2H4As reducing agent, mixture is transferred in ptfe autoclave and carries out hydro-thermal reaction, hydro-thermal reaction
Temperature is 150 DEG C, and the reaction time is 9h；Reaction is cooled to room temperature after terminating, and using 0.22um filtering with microporous membrane, will obtain
Filtrate dialysed in water 3 days, last evaporation solvent, the solid extremely molybdenum disulfide quantum dot that obtains after drying.
Step 4：Sisal hemp carbon fiber and molybdenum disulfide quantum dot is scattered in deionized water, and ultrasonic 25min obtains sisal hemp
The suspension of carbon fiber/molybdenum disulfide.Wherein, sisal hemp carbon fiber, molybdenum disulfide quantum dot, the mass ratio of deionized water are 1:
0.5:20。
Step 5：The preparation of ternary complex material：First ethanol is mixed with butyl titanate（Ethanol and butyl titanate
Volume ratio be 10:1）, 10min is stirred, solution A is formed；Again by sisal hemp carbon fiber/molybdenum disulfide quantum dot solution and glacial acetic acid
Mixing（The volume ratio of sisal hemp carbon fiber/molybdenum disulfide quantum dot solution and glacial acetic acid mixed liquor is 10:1）, the solution B of formation；
Under stirring, by volume 20:25 are added drop-wise to solution B in solution A by the drop rate of 1mL/ seconds, are then placed in 60 DEG C
70min is persistently stirred in water-bath, taupe gel is made, obtained gel is put into after being dried in 60 DEG C of baking ovens, is heated to
125 DEG C continue 15min, obtain beige solid；Ground, obtain sisal hemp carbon fiber/titanium dioxide/molybdenum disulfide nano multiple
Compound.
Embodiment 2
A kind of preparation method of sisal hemp carbon fiber photochemical catalyst, comprises the following steps：
Step 1：The preparation of sisal hemp carbon fiber：Sisal fiber is soaked 24 hours with the 5wt% NaOH aqueous solution, then rushed with water
Neutrality is washed till, then is impregnated 24 hours with 5wt% ammonium dibasic phosphate aqueous solution, pulls out, dry；Dried sisal hemp will be pre-processed
Fiber is put into step calcination in Muffle furnace：250 DEG C are first warming up to, 30min is kept, then be warming up to 850 DEG C, holding 2.5h, speed
For 5.5 DEG C/min, lead to inert gas.Porous sisal hemp carbon fiber is obtained after calcining cooling.
Step 2：Sisal hemp carbon fiber in step 1 is placed on the (NH that concentration is 150g/L4)2S2O8It is ultrasonic in solution
1.5h, filtering, is immersed in 100g/L NaOH solution 5min, surface unreacted is washed with deionized water after being cleaned with deionized water
(NH4)2S2O8。
Step 3：The preparation of molybdenum disulfide quantum dot：In mass ratio 1:100 by (NH4)2MoS4It is dissolved in water, ultrasound
15min, adds N2H4As reducing agent, mixture is transferred in ptfe autoclave and carries out hydro-thermal reaction, hydro-thermal reaction
Temperature is 180 DEG C, and the reaction time is 8h；Reaction is cooled to room temperature after terminating, and using 0.22um filtering with microporous membrane, will obtain
Filtrate dialysed in water 4 days, last evaporation solvent, the solid extremely molybdenum disulfide quantum dot that obtains after drying.
Step 4：Sisal hemp carbon fiber and molybdenum disulfide quantum dot is scattered in deionized water, and ultrasonic 30min obtains sisal hemp
The suspension of carbon fiber/molybdenum disulfide.Wherein, sisal hemp carbon fiber, molybdenum disulfide quantum dot, the mass ratio of deionized water are 1:
0.5:30。
Step 5：The preparation of ternary complex material：First ethanol is mixed with butyl titanate（Ethanol and butyl titanate
Volume ratio be 10:1）, 15min is stirred, solution A is formed；Again by sisal hemp carbon fiber/molybdenum disulfide quantum dot solution and glacial acetic acid
Mixing（The volume ratio of sisal hemp carbon fiber/molybdenum disulfide quantum dot solution and glacial acetic acid mixed liquor is 10:1）, the solution B of formation；
Under stirring, by volume 25:30 are added drop-wise to solution B in solution A by the drop rate of 1.5mL/ seconds, are then placed in 70
60min is persistently stirred in DEG C water-bath, taupe gel is made, obtained gel is put into after being dried in 70 DEG C of baking ovens, reheated
Continue 12min to 130 DEG C, obtain beige solid；Ground, obtain sisal hemp carbon fiber/titanium dioxide/molybdenum disulfide nano
Compound.
Embodiment 3
A kind of preparation method of sisal hemp carbon fiber photochemical catalyst, comprises the following steps：
Step 1：The preparation of sisal hemp carbon fiber：Sisal fiber is soaked 28 hours with the 5wt% NaOH aqueous solution, then rushed with water
Neutrality is washed till, then is impregnated 28 hours with 5wt% ammonium dibasic phosphate aqueous solution, pulls out, dry；Dried sisal hemp will be pre-processed
Fiber is put into step calcination in Muffle furnace：First it is warming up to 300 DEG C, keeps 25min, then be warming up to 900 DEG C, keeps 2h, speed is 6
DEG C/min, lead to inert gas.Porous sisal hemp carbon fiber is obtained after calcining cooling.
Step 2：Sisal hemp carbon fiber in step 1 is placed on the (NH that concentration is 200g/L4)2S2O8Ultrasound 1h in solution,
Filtering, is immersed in 105g/L NaOH solution 4min, surface is washed with deionized water unreacted after being cleaned with deionized water
(NH4)2S2O8。
Step 3：The preparation of molybdenum disulfide quantum dot：In mass ratio 1:105 by (NH4)2MoS4It is dissolved in water, ultrasound
10min, adds N2H4As reducing agent, mixture is transferred in ptfe autoclave and carries out hydro-thermal reaction, hydro-thermal reaction
Temperature is 200 DEG C, and the reaction time is 6h；Reaction is cooled to room temperature after terminating, and using 0.22um filtering with microporous membrane, will obtain
Filtrate dialysed in water 5 days, last evaporation solvent, the solid extremely molybdenum disulfide quantum dot that obtains after drying.
Step 4：Sisal hemp carbon fiber and molybdenum disulfide quantum dot is scattered in deionized water, and ultrasonic 35min obtains sisal hemp
The suspension of carbon fiber/molybdenum disulfide.Wherein, sisal hemp carbon fiber, molybdenum disulfide quantum dot, the mass ratio of deionized water are 1:
0.5:40。
Step 5：The preparation of ternary complex material：First ethanol is mixed with butyl titanate（Ethanol and butyl titanate
Volume ratio be 10:1）, 20min is stirred, solution A is formed；Again by sisal hemp carbon fiber/molybdenum disulfide quantum dot solution and glacial acetic acid
Mixing（The volume ratio of sisal hemp carbon fiber/molybdenum disulfide quantum dot solution and glacial acetic acid mixed liquor is 10:1）, the solution B of formation；
Under stirring, by volume 30:35 are added drop-wise to solution B in solution A by the drop rate of 1.5mL/ seconds, are then placed in 80
50min is persistently stirred in DEG C water-bath, taupe gel is made, obtained gel is put into after being dried in 80 DEG C of baking ovens, reheated
Continue 10min to 135 DEG C, obtain beige solid；Ground, obtain sisal hemp carbon fiber/titanium dioxide/molybdenum disulfide nano
Compound.
Sisal hemp carbon fiber produced by the present invention, its specific surface area is up to 1200m2/ more than g, and common normal drinking water
The specific surface area of the cocoanut active charcoal of processing is 1000-1100m2/g；Bamboo charcoal specific surface area is in 150-700m2Between/g.Thus
Understand its performance more preferably, be more suitable for being used as the carrier of titanium dioxide and molybdenum disulfide.
Raw materials used in the present invention, equipment, is the conventional raw material, equipment of this area unless otherwise noted；In the present invention
Method therefor, is the conventional method of this area unless otherwise noted.
It is described above, only it is presently preferred embodiments of the present invention, not the present invention is imposed any restrictions, it is every according to the present invention
Any simple modification, change and equivalent transformation that technical spirit is made to above example, still fall within the technology of the present invention side
The protection domain of case.
Claims (9)
1. a kind of preparation method of sisal hemp carbon fiber photochemical catalyst, it is characterised in that comprise the following steps：
Step 1：The preparation of sisal hemp carbon fiber：Sisal fiber is soaked with the NaOH aqueous solution, then rinsed with water to neutrality, then is used
Ammonium dibasic phosphate aqueous solution impregnates, and pulls out, dries；Dried sisal fiber will be pre-processed and be put into calcining in Muffle furnace, cooling
Porous sisal hemp carbon fiber is obtained afterwards；
Step 2：Sisal hemp carbon fiber in step 1 is placed on (NH4)2S2O8Ultrasonic in solution, filtering is soaked after being cleaned with deionized water
The NaOH solution 4-6min in 95-105g/L is steeped, the unreacted (NH in surface is washed with deionized water4)2S2O8；
Step 3：The preparation of molybdenum disulfide quantum dot：By (NH4)2MoS4It is dissolved in water, ultrasonic 10-20min, adds N2H4Make
For reducing agent, mixture is transferred in ptfe autoclave and carries out hydro-thermal reaction, reaction is cooled to room temperature after terminating, and adopts
With 0.22um filtering with microporous membrane, obtained filtrate is dialysed in water, last evaporation solvent, the solid pole obtained after drying
For molybdenum disulfide quantum dot；
Step 4：Sisal hemp carbon fiber and molybdenum disulfide quantum dot is scattered in deionized water, and ultrasonic 25-35min obtains sisal hemp
The suspension of carbon fiber/molybdenum disulfide；
Step 5：The preparation of ternary complex material：First ethanol is mixed with butyl titanate, 10-20min is stirred, solution is formed
A；Sisal hemp carbon fiber/molybdenum disulfide quantum dot solution is mixed with glacial acetic acid again, the solution B of formation；Under stirring, by body
Product compares 20-30:Solution B is slowly dropped in solution A by 25-35, is then placed in 60-80 DEG C of water-bath and is persistently stirred 50-
70min, is made taupe gel, obtained gel is put into after being dried in 60-80 DEG C of baking oven, is heated to 125-135 DEG C and holds
Continuous 10-15min, obtains beige solid；Ground, obtain sisal hemp carbon fiber/titanium dioxide/molybdenum disulfide nano and be combined
Thing.
2. a kind of preparation method of sisal hemp carbon fiber photochemical catalyst as claimed in claim 1, it is characterised in that in step 1,
The mass concentration of the NaOH aqueous solution is 5wt%, and soak time 20-28 hour, the mass concentration of ammonium dibasic phosphate aqueous solution is 5%,
Dip time is 20-28 hours.
3. a kind of preparation method of sisal hemp carbon fiber photochemical catalyst as claimed in claim 1, it is characterised in that in step 1, forge
Burn for step calcination：First it is warming up to 200-300 DEG C, keeps 25-35min, then be warming up to 800-900 DEG C, keeps 2-3h, speed is
5-6 DEG C/min, lead to inert gas.
4. a kind of preparation method of sisal hemp carbon fiber photochemical catalyst as claimed in claim 1, it is characterised in that in step 2,
(NH4)2S2O8The concentration of solution is 100-200g/L, and ultrasonic time is 1-2h.
5. a kind of preparation method of sisal hemp carbon fiber photochemical catalyst as claimed in claim 1, it is characterised in that in step 3, water
Thermal response temperature is 150-200 DEG C, and the reaction time is 6-9h；Filtrate dialysis time is 3-5 days.
6. a kind of preparation method of sisal hemp carbon fiber photochemical catalyst as described in claim 1 or 5, it is characterised in that step 3
In, (NH4)2MoS4Mass ratio with water is 1:95-105.
7. a kind of preparation method of sisal hemp carbon fiber photochemical catalyst as claimed in claim 1, it is characterised in that in step 4, sword
Numb carbon fiber, molybdenum disulfide quantum dot, the mass ratio of deionized water are 1:0.5:（20-40）.
8. a kind of preparation method of sisal hemp carbon fiber photochemical catalyst as claimed in claim 1, it is characterised in that molten in step 5
The volume ratio of ethanol and butyl titanate is 10 in liquid A:1；Sisal hemp carbon fiber/molybdenum disulfide quantum dot solution and ice in solution B
The volume ratio of acetic acid mixed liquor is 10:1.
9. a kind of preparation method of sisal hemp carbon fiber photochemical catalyst as described in claim 1 or 8, it is characterised in that step 5
In, the drop rate of solution B is 1-1.5mL/ seconds.
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