CN105642364B - A kind of composite photo-catalyst and its preparation method and application - Google Patents
A kind of composite photo-catalyst and its preparation method and application Download PDFInfo
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- CN105642364B CN105642364B CN201610043759.7A CN201610043759A CN105642364B CN 105642364 B CN105642364 B CN 105642364B CN 201610043759 A CN201610043759 A CN 201610043759A CN 105642364 B CN105642364 B CN 105642364B
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- 239000002131 composite material Substances 0.000 title claims abstract description 29
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title abstract description 8
- 238000005311 autocorrelation function Methods 0.000 claims abstract description 47
- 238000006243 chemical reaction Methods 0.000 claims abstract description 36
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 21
- 239000003054 catalyst Substances 0.000 claims abstract description 13
- 235000003301 Ceiba pentandra Nutrition 0.000 claims abstract description 9
- 244000146553 Ceiba pentandra Species 0.000 claims abstract description 9
- 238000000034 method Methods 0.000 claims abstract description 7
- 229910052961 molybdenite Inorganic materials 0.000 claims description 27
- 229910052982 molybdenum disulfide Inorganic materials 0.000 claims description 27
- 239000000243 solution Substances 0.000 claims description 27
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical group S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 claims description 20
- 238000001035 drying Methods 0.000 claims description 17
- 238000002791 soaking Methods 0.000 claims description 13
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- 230000015556 catabolic process Effects 0.000 claims description 10
- 238000006731 degradation reaction Methods 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 10
- 239000006228 supernatant Substances 0.000 claims description 10
- 238000001354 calcination Methods 0.000 claims description 8
- 230000003197 catalytic effect Effects 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- DDFHBQSCUXNBSA-UHFFFAOYSA-N 5-(5-carboxythiophen-2-yl)thiophene-2-carboxylic acid Chemical compound S1C(C(=O)O)=CC=C1C1=CC=C(C(O)=O)S1 DDFHBQSCUXNBSA-UHFFFAOYSA-N 0.000 claims description 5
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 5
- 239000004202 carbamide Substances 0.000 claims description 5
- 150000001868 cobalt Chemical class 0.000 claims description 5
- 239000012153 distilled water Substances 0.000 claims description 5
- 239000000835 fiber Substances 0.000 claims description 5
- 239000011259 mixed solution Substances 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- 235000015393 sodium molybdate Nutrition 0.000 claims description 5
- 239000002351 wastewater Substances 0.000 claims description 5
- 239000000975 dye Substances 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 2
- 238000004090 dissolution Methods 0.000 claims description 2
- 238000001802 infusion Methods 0.000 claims description 2
- 229910052710 silicon Inorganic materials 0.000 claims description 2
- 239000010703 silicon Substances 0.000 claims description 2
- 238000006555 catalytic reaction Methods 0.000 abstract description 3
- 239000010865 sewage Substances 0.000 abstract description 2
- 229910002515 CoAl Inorganic materials 0.000 abstract 1
- 239000003245 coal Substances 0.000 abstract 1
- 239000000463 material Substances 0.000 abstract 1
- IQFVPQOLBLOTPF-HKXUKFGYSA-L congo red Chemical compound [Na+].[Na+].C1=CC=CC2=C(N)C(/N=N/C3=CC=C(C=C3)C3=CC=C(C=C3)/N=N/C3=C(C4=CC=CC=C4C(=C3)S([O-])(=O)=O)N)=CC(S([O-])(=O)=O)=C21 IQFVPQOLBLOTPF-HKXUKFGYSA-L 0.000 description 12
- 230000001699 photocatalysis Effects 0.000 description 6
- 238000007146 photocatalysis Methods 0.000 description 5
- 238000010521 absorption reaction Methods 0.000 description 4
- 159000000013 aluminium salts Chemical class 0.000 description 3
- 229910000329 aluminium sulfate Inorganic materials 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- 239000011592 zinc chloride Substances 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 229920000742 Cotton Polymers 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 238000005215 recombination Methods 0.000 description 2
- 230000006798 recombination Effects 0.000 description 2
- 238000002336 sorption--desorption measurement Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 description 2
- 239000002023 wood Substances 0.000 description 2
- 238000002835 absorbance Methods 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000013066 combination product Substances 0.000 description 1
- 229940127555 combination product Drugs 0.000 description 1
- 239000002552 dosage form Substances 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000000724 energy-dispersive X-ray spectrum Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- -1 hydroxide class Compound Chemical class 0.000 description 1
- 150000004679 hydroxides Chemical class 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000010025 steaming Methods 0.000 description 1
- 229910052717 sulfur Inorganic materials 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
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- 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
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/26—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24
- B01J31/34—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24 of chromium, molybdenum or tungsten
-
- 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
- B01J35/50—Catalysts, in general, characterised by their form or physical properties characterised by their shape or configuration
- B01J35/58—Fabrics or filaments
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- 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
- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
- B01J35/61—Surface area
- B01J35/613—10-100 m2/g
-
- 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
- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
- B01J35/63—Pore volume
- B01J35/633—Pore volume less than 0.5 ml/g
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- 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
- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
- B01J35/64—Pore diameter
- B01J35/643—Pore diameter less than 2 nm
-
- 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
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/30—Nature of the water, waste water, sewage or sludge to be treated from the textile industry
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W10/00—Technologies for wastewater treatment
- Y02W10/30—Wastewater or sewage treatment systems using renewable energies
- Y02W10/37—Wastewater or sewage treatment systems using renewable energies using solar energy
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- Life Sciences & Earth Sciences (AREA)
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- Water Supply & Treatment (AREA)
- Catalysts (AREA)
Abstract
The invention discloses a kind of composite photo-catalyst and its preparation method and application, belongs to catalysis material technical field.The present invention is prepared for NACF by biological template of kapok（ACFs）, MoS is grown using hydro-thermal method simultaneously on ACFs2With CoAl LDH, MoS is finally given2/ CoAl-LDH/ACFs composite photo-catalysts.The present invention is easy to operate, technique is simple, and reaction condition is gentle, and the catalyst appearance structure of acquisition is novel special, the organic pollution in its sewage that can efficiently be degraded under simulated solar light irradiation.
Description
Technical field
The present invention relates to the catalyst in terms of a kind of sewage disposal, and in particular to it is a kind of prepared using kapok as template it is porous
MoS2/ CoAl-LDH/ACFs composite photo-catalysts and its preparation method and application.
Background technology
The species of Pollutants in Wastewater has a lot, and wherein organic pollution accounts for major part, is one mostly in waste water from dyestuff
A little molecular structures hardly possiblies are decomposed, the organic matter that chemical property is sufficiently stable, therefore application photocatalytic oxidation degradation Organic Pollution is
As one of important method, and photocatalysis technology non-secondary pollution.
MoS2Energy gap is narrower, about 1.97eV, under visible light illumination, has excellent photocatalysis performance.However,
MoS2Although photochemical catalyst response optical wavelength can extend to visible-range, because its photo-generate electron-hole recombination rate is fast, inhales
Attached poor performance make it that its visible light catalytic performance is not especially high.The present invention is by ACF and MoS2Compound, ACF can be used as electronics
Grabber, so as to reduce photo-generate electron-hole recombination rate, to improve its photocatalysis efficiency.Layered double hydroxide class
Compound（Layered double hydroxides, LDHs）, due to its special layer structure, surface positively charged, interlayer can be cloudy
Ion, which swaps etc., assigns its wide application, such as absorption, photocatalysis, medical science field.By LDHs and MoS2, ACF it is multiple
Close, not only the absorption property of combination product improves, and the efficiency of photocatalytic degradation dirt Organic substance in water is also greatly improved.
The content of the invention
It is an object of the invention to provide a kind of composite photo-catalyst and its preparation method and application.
The present invention is achieved through the following technical solutions：
A kind of composite photo-catalyst, it is characterised in that the catalyst is MoS2/ CoAl-LDH/ACFs composite photo-catalysts.
Described composite photo-catalyst, it is characterised in that it is made of the MoS using kapok as biological template2And CoAl-
LDH is grown on ACFs fibers, micropore and mesoporous graded porous structure be present simultaneously on every fiber.
A kind of preparation method of composite photo-catalyst, it is characterised in that it is prepared by following methods：
（1）Configure the ZnCl that 75 ~ 85 mL concentration are 95 mg/L2Solution, while 15mg neopelexes are added,
2g kapoks are put into the solution after time of infusion, take out drying；
（2）Take step（1）In obtained kapok, it is then heated to 900 DEG C of progress in the environment of logical nitrogen
Calcining, is then cooled to 300 DEG C, finally naturally cools to room temperature, wash, dry to obtain ACFs；
（3）By 20mg steps（2）The ACFs of middle gained and 0.242 g sodium molybdates, 0.38g thiocarbamide mixed dissolutions are in 55 ~ 65
In mL distilled water, stir；
（4）By step（3）The middle reaction solution configured is transferred in hydrothermal reaction kettle liner, is fitted into hydrothermal reaction kettle anti-
Should, reaction is cooled to room temperature after terminating, and supernatant is removed, and filters, washs, drying and obtain MoS2/ACFs；
（5）Take 200mg steps（4）Described in MoS2/ ACFs is placed in 55 ~ 65 mL cobalt salts, silicon source, urea and ammonium fluoride
It is according to mol ratio（2~3）:1:25:（8~9）In the mixed solution of composition, stir to obtain mixed reaction solution；
（6）By step（5）Gained mixed reaction solution is transferred in hydrothermal reaction kettle liner, is fitted into hydrothermal reaction kettle and is reacted,
Reaction is cooled to room temperature after terminating, and supernatant is removed, filters, wash, drying to MoS2/CoAl-LDH/ACFs。
The step（1）Dip time is 2h, and drying temperature is 80 DEG C.
The step（2）Rate of heat addition during middle calcining is 5 DEG C/min, calcination time 1h.
The step（4）Middle reaction temperature is 210 DEG C, soaking time 24h.
The step（6）Middle reaction temperature is 100 DEG C, soaking time 10-24h.
Above-mentioned composite photo-catalyst can be used for catalytic degradation processing waste water from dyestuff.The photochemical catalyst is right in 120 min
Congo red degradation rate reaches more than 78%, shows that the composite photo-catalyst has efficient catalytic effect to congo red.
The beneficial effects of the invention are as follows：The present invention prepares MoS by biological template of kapok2/ CoAl-LDH/ACFs complex lights
Catalyst, required raw material are easy to get, and cost is cheap, preparation technology is simple, easy to operate, efficiency high, the composite photocatalyst dosage form of acquisition
Looks structure is special, has micropore and mesoporous graded porous structure.Due to the MoS of preparation2/ CoAl-LDH/ACFs complex lights are urged
Agent has special graded porous structure, therefore has excellent absorption property.The composite photo-catalyst is in radiation of visible light
Under there is preferable degradation efficiency to organic pollution, more than 78% is reached to Congo red degradation rate in 120 min.
Brief description of the drawings
Fig. 1 is the made photochemical catalysts of embodiment 1-3 in the present invention under visible light to Congo red degraded figure.
Fig. 2 is the XRD curves of 3 made photochemical catalyst of embodiment in the present invention；
Fig. 3 is the SEM figures and EDS spectrograms of 3 made photochemical catalyst of embodiment in the present invention；In figure, (a) is that embodiment 3 is made
The MoS obtained2The SEM figures of/CoAl-LDHs/ACFs composite photo-catalysts, (b), (c) are（a）In corresponding to 1,2 point EDS spectrum
Figure.
Fig. 4 is the N of 3 made photochemical catalyst of embodiment in the present invention2Adsorption/desorption curve and respective aperture distribution curve.
Embodiment
With reference to specific embodiment, the present invention is described further.
Embodiment 1
（1）Configure 75 mL 95 mg/L ZnCl2Solution, while 15 mg neopelexes are added, by 2 g wood
Cotton is put into the solution impregnated for 2 h times after, take out after 80 DEG C of drying, then 900 DEG C of calcinings under logical nitrogen by it, forge
Heating rate is 5 DEG C/min during burning, and soaking time is 1 h, is then cooled to 300 DEG C, finally naturally cools to room temperature,
Obtain ACFs；
（2）Take 20 mg steps（1）Described in ACFs mix with 0.242 g sodium molybdates, 0.38 g thiocarbamides and be dissolved in 60 mL
In distilled water, stir, the reaction solution configured is transferred in 100 mL hydrothermal reaction kettle liners, load hydrothermal reaction kettle
Middle reaction, reaction temperature are 210 DEG C, and soaking time is 24 h, and reaction is cooled to room temperature after terminating, and supernatant is removed, mistake
Filter, washing, drying obtain MoS2/ACFs；
（3）Take 200 mg steps（2）Described in MoS2/ ACFs is placed in 60 mL cobalt salts, aluminium salt, urea and ammonium fluoride and rubbed
You are than being 2:1:25:In 9 mixed solution, stir, the reaction solution configured is transferred to 100 mL hydrothermal reaction kettles
In liner, it is fitted into hydrothermal reaction kettle and reacts, reaction temperature is 100 DEG C, and soaking time is 10 h, and reaction is cooled to after terminating
Room temperature, supernatant is removed, filter, wash, drying and obtain MoS2/CoAl-LDH/ACFs。
Embodiment 2
（1）Configure 85mL 95mg/L ZnCl2Solution, while 15mg neopelexes are added, 2g kapoks are put
Enter after impregnating the 2h times in the solution, take out after 80 DEG C of drying, then calcine it for 900 DEG C under logical nitrogen, calcination process
Middle heating rate is 5 DEG C/min, soaking time 1h, is then cooled to 300 DEG C, finally naturally cools to room temperature, obtain ACF；
（2）Take 20 mg steps（1）Described in ACF mixed with 0.242 g sodium molybdates, 0.38 g thiocarbamides be dissolved in 60 mL steaming
In distilled water, stir, the reaction solution configured is transferred in 100 mL hydrothermal reaction kettle liners, is fitted into hydrothermal reaction kettle
Reaction, reaction temperature are 210 DEG C, and soaking time is 24 h, and reaction is cooled to room temperature after terminating, and supernatant is removed, filtering,
Washing, drying obtain MoS2/ACFs；
（3）Take 200 mg steps（2）Described in MoS2/ ACFs is placed in 60 mL cobalt salts, aluminium salt, urea and ammonium fluoride and rubbed
You are than being 3:1:25:In 8 mixed solution, stir, the reaction solution configured is transferred to 100 mL hydrothermal reaction kettles
In liner, it is fitted into hydrothermal reaction kettle and reacts, reaction temperature is 100 DEG C, and soaking time is 15 h, and reaction is cooled to after terminating
Room temperature, supernatant is removed, filter, wash, drying and obtain MoS2/CoAl-LDH/ACFs。
Embodiment 3
（1）Configure 80 mL 95 mg/L ZnCl2Solution, while 15 mg neopelexes are added, by 2 g wood
Cotton is put into the solution impregnated for 2 h times after, take out after 80 DEG C of drying, then 900 DEG C of calcinings under logical nitrogen by it, forge
Heating rate is 5 DEG C/min during burning, and soaking time is 1 h, is then cooled to 300 DEG C, finally naturally cools to room temperature,
Obtain ACFs；
（2）Take 20 mg steps（1）Described in ACFs mix with 0.242 g sodium molybdates, 0.38 g thiocarbamides and be dissolved in 60 mL
In distilled water, stir, the reaction solution configured is transferred in 100 mL hydrothermal reaction kettle liners, load hydrothermal reaction kettle
Middle reaction, reaction temperature are 210 DEG C, and soaking time is 24 h, and reaction is cooled to room temperature after terminating, and supernatant is removed, mistake
Filter, washing, drying obtain MoS2/ACFs；
（3）Take 200 mg steps（2）Described in MoS2/ ACFs is placed in 60 mL cobalt salts, aluminium salt, urea and ammonium fluoride and rubbed
You are than being 2:1:25:In 8 mixed solution, stir, the reaction solution configured is transferred in 100 mL hydrothermal reaction kettles
In lining, it is fitted into hydrothermal reaction kettle and reacts, reaction temperature is 100 DEG C, and soaking time is 24 h, and reaction is cooled to room after terminating
Temperature, supernatant is removed, filter, wash, drying and obtain MoS2/CoAl-LDH/ACFs。
Test case
The present invention have studied the MoS prepared by embodiment 1-32/ CoAl-LDH/ACFs composite photo-catalysts are under visible light
Catalytic effect.Dirty organic pollutants are simulated with Congo red solution, its method is：0.1 g embodiments 1-3 is taken to prepare respectively
MoS2/ CoAl-LDH/ACFs composite photo-catalysts are put into the mg/L of 80 mL 200 Congo red solution, first in dark ring
30 min are placed under border, to adsorption equilibrium.After the completion of absorption, light-catalyzed reaction, photocatalysis are carried out under the irradiation of 500 W xenon lamps
Cheng Zhong, the Congo red solution of 4 mL is taken out as sample every 10 min, 5 min are centrifuged under 4000 r/min, with light splitting
Photometer tests the absorbance of Congo red solution under different catalysis times and is converted into concentration, to characterize degradation effect, specific knot
Fruit sees Fig. 1.Fig. 1 is degradation rate and the relation curve of time when photocatalytic degradation is Congo red under simulated solar light irradiation.By scheming
1 is visible, and three samples are to Congo red degradation rate more than 70%, and the photochemical catalyst wherein prepared by embodiment 3 is in 120 min
It is interior that more than 78% is reached to Congo red degradation rate, show that the photochemical catalyst has efficient catalytic effect to congo red, can use
In the efficient process of waste water from dyestuff.
The present invention is investigated the MoS prepared by embodiment 32The XRD of/CoAl-LDH/ACFs composite photo-catalyst samples
Spectrogram, as shown in Figure 2.Sample is by MoS it can be seen from Fig. 2 XRD spectra2, CoAl-LDH and amorphous activated carbon composition.
MoS2Sharp peak is respectively provided with CoAl-LDH, illustrates well-crystallized.The sample prepared by embodiment 3 is also have detected simultaneously
SEM schemes and EDS spectrograms, as shown in Figure 3.In Fig. 3（a）It is MoS2The SEM figures of/CoAl-LDH/ACFs composite photo-catalysts, by scheming
In it can be seen that ACFs fibers be in hollow tubulose, diameter is about 20 μm, has the MoS of sheet in its superficial growth2And CoAl-
LDH, CoAl-LDH size are about 1.5-2 μm；（b）It is（a）In 1 point of EDS spectrograms, as can be seen from Figure containing Co, Al, C,
O elements, with reference to XRD spectrum above, it can be seen that CoAl-LDH has been grown on ACF；（c）It is（a）In 2 points of EDS spectrograms,
As can be seen from Figure containing elements such as Mo, S, with reference to XRD spectra above, it is known that MoS2Grow on ACFs.
The present invention also have detected the N of the sample prepared by embodiment 32Adsorption/desorption curve and respective aperture distribution curve,
As shown in Figure 4.In Fig. 4（a）It can be seen that low-pressure end is inclined to X-axis, and V-type etc. is belonged to by obvious hysteresis loop at mesohigh end
Warm line, show to exist in sample a number of mesoporous；In Fig. 4（b）It can be seen that containing substantial amounts of mesoporous, and have a small amount of micro-
Hole, illustrate to be successfully prepared the MoS containing micropore Yu mesoporous graded porous structure2/ CoAl-LDH/ACFs composite photocatalysts
Agent.The sample specific surface area is 34.04 m2/ g, total pore volume are 0.2 cm3/ g, average pore size are 1.04 nm.
Claims (7)
1. a kind of composite photo-catalyst, it is characterised in that the catalyst is MoS2/ CoAl-LDH/ACFs composite photo-catalysts；Institute
The composite photo-catalyst stated is prepared by following methods：
（1）Configure the ZnCl that 75 ~ 85 mL concentration are 95 mg/L2Solution, while 15mg neopelexes are added, by 2g
Kapok is put into the solution after time of infusion, takes out drying；
（2）Take step（1）In obtained kapok, it is then heated to 900 DEG C in the environment of logical nitrogen and forged
Burn, be then cooled to 300 DEG C, finally naturally cool to room temperature, wash, dry to obtain ACFs；
（3）By 20mg steps（2）The ACFs of middle gained and 0.242 g sodium molybdates, 0.38g thiocarbamides mixed dissolution steam in 55 ~ 65 mL
In distilled water, stir；
（4）By step（3）The middle reaction solution configured is transferred in hydrothermal reaction kettle liner, is fitted into hydrothermal reaction kettle and is reacted,
Reaction is cooled to room temperature after terminating, and supernatant is removed, and filters, washs, drying and obtain MoS2/ACFs；
（5）Take 200mg steps（4）Described in MoS2/ ACFs is placed in 55 ~ 65 mL cobalt salts, silicon source, urea and ammonium fluoride according to rubbing
You are at ratio（2~3）:1:25:（8~9）In the mixed solution of composition, stir to obtain mixed reaction solution；
（6）By step（5）Gained mixed reaction solution is transferred in hydrothermal reaction kettle liner, is fitted into hydrothermal reaction kettle and is reacted, reaction
Room temperature is cooled to after end, supernatant is removed, filters, wash, drying to MoS2/CoAl-LDH/ACFs。
2. composite photo-catalyst according to claim 1, it is characterised in that it be made of using kapok as biological template,
MoS2It is grown in CoAl-LDH on ACFs fibers, micropore and mesoporous graded porous structure is present simultaneously on every fiber.
3. composite photo-catalyst according to claim 1, it is characterised in that the step（1）Dip time is 2h, drying
Temperature is 80 DEG C.
4. composite photo-catalyst according to claim 1, it is characterised in that the step（2）Heating speed during middle calcining
Rate is 5 DEG C/min, calcination time 1h.
5. composite photo-catalyst according to claim 1, it is characterised in that the step（4）Middle reaction temperature is 210
DEG C, soaking time 24h.
6. composite photo-catalyst according to claim 1, it is characterised in that the step（6）Middle reaction temperature is 100
DEG C, soaking time 10-24h.
7. the application of the composite photo-catalyst described in a kind of claim 1 or 2, it is characterised in that available for catalytic degradation processing
Waste water from dyestuff.
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| CN106629983B (en) * | 2016-12-29 | 2019-06-25 | 苏州科技大学 | Application of the molybdenum sulfide composite reactive Carbon Materials near infrared light catalysis denitrogenation |
| CN107096525B (en) * | 2017-05-04 | 2019-08-27 | 济南大学 | A kind of composite photo-catalyst and its preparation method and application |
| CN108103766B (en) * | 2017-12-29 | 2021-07-30 | 澄江市力点科技有限公司 | Molybdenum disulfide composite fiber photocatalyst for sewage treatment and preparation method thereof |
| CN108246281B (en) * | 2018-01-04 | 2020-11-24 | 中国地质大学（北京） | Carbon fiber @ molybdenum dioxide nanoparticle core-shell composite structure and preparation method thereof |
| CN108435191B (en) * | 2018-04-26 | 2023-08-18 | 济南大学 | SnNb (tin-zinc-niobium) alloy 2 O 6 CoFe-LDH (CoFe-LDH) plate composite magnetic heterostructure catalyst and preparation method and application thereof |
| US11351532B2 (en) | 2018-07-30 | 2022-06-07 | Suzhou University of Science and Technology | Photocatalytic composite material and preparation method and application thereof |
| CN109433179A (en) * | 2018-11-29 | 2019-03-08 | 西安科技大学 | A kind of preparation method of petal shape hydrotalcite-active carbon composite photo-catalyst |
| CN109778225B (en) * | 2019-01-31 | 2021-08-17 | 上海应用技术大学 | N, S co-doped graphene/molybdenum selenide/CoFe-LDH aerogel and preparation thereof |
| CN112604707B (en) * | 2021-01-12 | 2022-08-09 | 天津理工大学 | Preparation method and application of CuO QDs/CoAl-LDHs composite material photocatalyst |
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