CN108579782A - A kind of visible light-responded composite material and its preparation and application - Google Patents
A kind of visible light-responded composite material and its preparation and application Download PDFInfo
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- CN108579782A CN108579782A CN201810236256.0A CN201810236256A CN108579782A CN 108579782 A CN108579782 A CN 108579782A CN 201810236256 A CN201810236256 A CN 201810236256A CN 108579782 A CN108579782 A CN 108579782A
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- 239000002131 composite material Substances 0.000 title claims abstract description 47
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 29
- 239000004202 carbamide Substances 0.000 claims abstract description 29
- 239000000843 powder Substances 0.000 claims abstract description 29
- 241000219138 Luffa Species 0.000 claims abstract description 19
- 235000003956 Luffa Nutrition 0.000 claims abstract description 19
- 238000001035 drying Methods 0.000 claims abstract description 15
- 238000000034 method Methods 0.000 claims abstract description 14
- 238000001354 calcination Methods 0.000 claims abstract description 13
- 230000015556 catabolic process Effects 0.000 claims abstract description 11
- 238000006731 degradation reaction Methods 0.000 claims abstract description 11
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229920000049 Carbon (fiber) Polymers 0.000 claims abstract description 10
- 239000004917 carbon fiber Substances 0.000 claims abstract description 10
- 239000000835 fiber Substances 0.000 claims abstract description 10
- 244000280244 Luffa acutangula Species 0.000 claims abstract description 5
- 235000009814 Luffa aegyptiaca Nutrition 0.000 claims abstract description 5
- 230000003197 catalytic effect Effects 0.000 claims abstract description 5
- 239000005416 organic matter Substances 0.000 claims abstract description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 22
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 19
- 239000000243 solution Substances 0.000 claims description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 16
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 13
- 239000007864 aqueous solution Substances 0.000 claims description 13
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 11
- 229910052757 nitrogen Inorganic materials 0.000 claims description 11
- 238000010438 heat treatment Methods 0.000 claims description 9
- 239000011259 mixed solution Substances 0.000 claims description 8
- 235000011121 sodium hydroxide Nutrition 0.000 claims description 8
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims description 7
- 239000008367 deionised water Substances 0.000 claims description 7
- 229910021641 deionized water Inorganic materials 0.000 claims description 7
- 239000005011 phenolic resin Substances 0.000 claims description 7
- 229920001568 phenolic resin Polymers 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 6
- 238000010792 warming Methods 0.000 claims description 6
- 238000001994 activation Methods 0.000 claims description 5
- 239000012153 distilled water Substances 0.000 claims description 5
- 229910002804 graphite Inorganic materials 0.000 claims description 5
- 239000010439 graphite Substances 0.000 claims description 5
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 claims description 5
- 230000008569 process Effects 0.000 claims description 4
- 239000007787 solid Substances 0.000 claims description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 3
- 238000004821 distillation Methods 0.000 claims description 3
- 239000007789 gas Substances 0.000 claims description 3
- 238000003837 high-temperature calcination Methods 0.000 claims description 3
- 239000001257 hydrogen Substances 0.000 claims description 3
- 229910052739 hydrogen Inorganic materials 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 3
- 238000000643 oven drying Methods 0.000 claims description 3
- 238000003763 carbonization Methods 0.000 claims description 2
- 230000003647 oxidation Effects 0.000 claims description 2
- 238000007254 oxidation reaction Methods 0.000 claims description 2
- 239000002253 acid Substances 0.000 claims 1
- 238000002386 leaching Methods 0.000 claims 1
- 150000003839 salts Chemical class 0.000 claims 1
- KKCBUQHMOMHUOY-UHFFFAOYSA-N sodium oxide Chemical compound [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 claims 1
- 229910001948 sodium oxide Inorganic materials 0.000 claims 1
- 239000003054 catalyst Substances 0.000 abstract description 10
- 230000000694 effects Effects 0.000 abstract description 7
- 239000000047 product Substances 0.000 abstract description 7
- 239000000376 reactant Substances 0.000 abstract description 4
- 239000012043 crude product Substances 0.000 abstract description 3
- 238000001179 sorption measurement Methods 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 229910052751 metal Inorganic materials 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- 239000000758 substrate Substances 0.000 abstract description 2
- 231100000614 poison Toxicity 0.000 abstract 1
- 230000007096 poisonous effect Effects 0.000 abstract 1
- 238000002203 pretreatment Methods 0.000 abstract 1
- 235000019441 ethanol Nutrition 0.000 description 6
- 238000010521 absorption reaction Methods 0.000 description 3
- 230000004913 activation Effects 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 231100000252 nontoxic Toxicity 0.000 description 3
- 230000003000 nontoxic effect Effects 0.000 description 3
- 230000004044 response Effects 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- 238000001228 spectrum Methods 0.000 description 3
- 230000008901 benefit Effects 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- 238000002336 sorption--desorption measurement Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000011001 backwashing Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 150000008282 halocarbons Chemical class 0.000 description 1
- 150000002391 heterocyclic compounds Chemical class 0.000 description 1
- 231100000171 higher toxicity Toxicity 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 230000010355 oscillation Effects 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 150000002989 phenols Chemical class 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 238000001782 photodegradation Methods 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- 239000003403 water pollutant Substances 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
- B01J27/24—Nitrogen compounds
-
- 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
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0259—Compounds of N, P, As, Sb, Bi
-
- 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
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
-
- B01J35/39—
-
- 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
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
Abstract
The invention discloses a kind of visible light-responded composite materials and its preparation and application.It mainly includes the following steps that：To loofah fiber carry out pre-treatment, after be fired into luffa based active carbon fiber (L ACF)；Crude product is made in the L ACF that calcining is attached with urea；Drying and processing is rinsed, g C are obtained3N4/ L ACF composite materials.Two kinds of raw material in this method are cheap and easy to get, compared to catalyst of the tradition containing metallic element, this product is environment-protecting and non-poisonous, and manufacture craft is simple, as L ACF large specific surface areas of substrate, mesh structural porous in composite material, there is excellent adsorption and enrichment performance to reactant, significantly increases reactant and catalyst g C in this way3N4Contact probability, have the effect of good catalytic degradation organic matter in visible-range, while solving the problems, such as that conventional powder shape catalyst is difficult to recycle, great practical value.
Description
Technical field
The invention belongs to technical field of composite materials, and in particular to a kind of visible light-responded composite material and its prepare and
Using.
Background technology
In recent years, industrialized rapid development brings great convenience to social progress and people’s lives, but with
And come environmental problem it is also very prominent, especially water pollution problems is quite severe, contained by the waste water generated in industrial production
There is the substances such as some phenolic compounds, heterocyclic compound and halogenated hydrocarbons higher toxicity, current processing method mainly to have object
Reason absorption or biological treatment etc., but all more or less presence such as inefficiency, process is cumbersome, generates secondary pollution problems.
Therefore Photocatalitic Technique of Semiconductor comes into being, and semiconductor light-catalyst directly utilizes solar energy, by macromolecular organic pollution
It directly degrades, has many advantages, such as efficient, low energy consumption, nontoxic.
Since TiO2It is used for being made photodegradation aquatic products hydrogen after hydrogen battery, TiO for the first time by Fujishima et al.2As semiconductor
Photochemical catalyst obtains the concern and research of a large number of researchers, TiO2With stability height, good in optical property, nontoxic and energy
Low advantage being consumed, but due to its greater band gap, it is seen that optical Response is low, thus it is relatively low for solar energy utilization ratio, therefore study
Developing, there is efficient visible light-responded catalyst to seem particularly urgent.
In recent years, graphite phase carbon nitride (g-C3N4) because it is with preferable chemical stability, thermal stability and visible light sound
Ying Xing, therefore the concern of Many researchers is obtained, but due to its powdered form, when being scattered in photocatalyst in liquid,
It is easy to happen aggregation, and powdered form recycling is more difficult, these significantly limit g-C3N4Popularization and application.
Therefore, how by g-C3N4Powder is effectively loaded, and so that it is kept higher catalytic activity and is easily recycled, is
One good problem to study.
Invention content
Present invention aims at provide a kind of composite material of load graphite phase carbon nitride so that the composite material has can
It is light-exposed response degradation water pollutant effect and be easily recycled.
In order to achieve the above objectives, as follows using technical solution：
A kind of visible light-responded composite material, by graphite phase carbon nitride powder (g-C3N4) it is carried on luffa activated carbon
It is prepared on fiber.
The preparation method of above-mentioned visible light-responded composite material, includes the following steps：
1) loofah fiber is placed in sodium hydrate aqueous solution and impregnates 20-24h, cleaned to neutrality, set with deionized water
It is dried in baking oven；It is subsequently placed in phenolic resin aqueous solution and impregnates 20-24h, taking-up naturally dry, which is placed in baking oven, toasts
1-2h；
2) continue to be placed in high temperature tubular resistor furnace pre-oxidized, be carbonized, activation process, be passed through nitrogen therebetween and protect
Gas；
3) continue to impregnate 2h with hydrochloric acid solution, be cleaned to neutrality with deionized water, it is fine that drying obtains luffa matrix activated carbon
It ties up (L-ACF)；
4) luffa based active carbon fiber is cut into small pieces, immerses in urea supersaturated solution, is carried out at the same time supersound process,
After be put into baking oven and dry；
5) the luffa based active carbon fiber that surface is attached with to urea is put into crucible, and is wrapped up with urea powder, is added
Lid forms semiclosed shape, is put into Muffle furnace and carries out high-temperature calcination, after calcining, cooled to room temperature；
6) it is rinsed with distilled water and alcohol mixed solution, to remove the loose g-C in surface3N4Powder is then put
Enter in baking oven and dries to get g-C3N4/ L-ACF composite materials.
By said program, in step 1, the concentration of the sodium hydrate aqueous solution is 2wt%；Baking in the baking oven twice
Roasting temperature is 105 DEG C；The solid content of the phenolic resin aqueous solution is 36wt%.
By said program, in step 2, pre-oxidation, carbonization, activation heating procedure be：It is warming up to from room temperature through 22min
200 DEG C, keep temperature 120min；750 DEG C are warming up to by 70min, keeps temperature 70min；Stop heating, it is naturally cold
But；Nitrogen starts to be passed through after keeping 120min at 200 DEG C, until stopping being passed through nitrogen when naturally cooling to 200 DEG C.
By said program, in step 3, the concentration of the hydrochloric acid solution is 1mol/L, and the drying temperature is 60 DEG C.
By said program, in step 4, described to immerse the time being ultrasonically treated in urea supersaturated solution be 20min,
Ultrasonic power is 100w；The temperature of baking oven drying is 60 DEG C.
By said program, in step 5, the package mode is the urea powder that crucible bottom first spreads one layer of about 2-3cm thickness
End, after be put into surface and be attached with the L-ACF of urea, then cover the urea powder of 4-5cm thickness, finally cover crucible cover；Muffle furnace
Calcination temperature be 550 DEG C, calcination time 3h, heating rate be 2 DEG C/min.
By said program, in step 6, the volume ratio of the ethyl alcohol and distillation water mixed solution is 1：1；Drying temperature is 60
℃。
Application of the above-mentioned visible light-responded composite material in catalytic degradation organic matter field.
The luffa based active carbon fiber (L-ACF) that the present invention has been fired by the method for high temperature cabonization, it is rear using use
The method of ultrasonic immersing, urea is attached on L-ACF, the L-ACF of urea is attached with by calcining, successfully by g-C3N4Powder
It is carried on L-ACF so that g-C obtained3N4/ L-ACF composite materials have visible light-responded effect, and are shone in visible light
Lower removable organic pollutants are penetrated, while solving the problems, such as that powder catalyst recycling is difficult.
Beneficial effects of the present invention：
Method of the present invention by calcining urea on luffa based active carbon fiber, is prepared for g-C3N4/ L-ACF is compound
Material.Two kinds of raw material in this method are cheap and easy to get, and compared to catalyst of the tradition containing metallic element, this product is environmental protection
Non-toxic material, and manufacture craft is simple, as the luffa based active carbon fiber large specific surface area of substrate, netted in composite material
It is porous, there is excellent adsorption and enrichment performance to reactant, significantly increases reactant and catalyst g-C3N4Contact it is several
Rate has the effect of good catalytic degradation organic matter in visible-range, while it is difficult to solve conventional powder shape catalyst
The problem of to recycle, great practical value.
Description of the drawings
Fig. 1：The g-C of embodiment 13N4/ L-ACF composite products figure and SEM scanning electron microscope (SEM) photographs；
Fig. 2：The g-C of embodiment 13N4/ L-ACF composite materials, g-C3N4The UV-Vis collection of illustrative plates of powder；
Fig. 3：The g-C of embodiment 13N4The N of/L-ACF composite materials2Adsorption/desorption figure and composite material graph of pore diameter distribution；
Fig. 4：The g-C of embodiment 13N4/ L-ACF composite materials, g-C3N4The XRD spectrum of powder, L-ACF；
Fig. 5：The g-C of embodiment 13N4/ L-ACF composite materials and L-ACF degrade under visible light RhB degradation time and
The relational graph of residual concentration；
Fig. 6：The g-C of embodiment 13N4/ L-ACF composite materials use 5 degradation rate figures to RhB under visible light.
Specific implementation mode
Following embodiment further illustrates technical scheme of the present invention, but not as limiting the scope of the invention.
The present invention is by graphite phase carbon nitride powder (g-C3N4) be carried in luffa activated carbon fibre visible light is prepared
The composite material of response, detailed process are as follows：
Loofah fiber is placed in sodium hydrate aqueous solution after immersion 20-24h by step 1), NaOH solution is discarded, to go
Ionized water is cleaned to neutrality, after be put into baking oven and dry；Luffa after drying is placed in phenolic resin aqueous solution and impregnates 20-
For 24 hours, taking-up naturally dry, which is placed in baking oven, toasts 1-2h；The mass concentration of the sodium hydrate aqueous solution is 2%, twice institute
It is 105 DEG C to state the baking temperature in baking oven, and the solid content of the phenolic resin aqueous solution is 36% or so.
The luffa dried in step 1 is placed in high temperature tubular resistor furnace by step 2) to be pre-oxidized, is carbonized, at activation
Reason, and be passed through nitrogen and make protection gas；The heating procedure that the high temperature tubular resistor furnace is pre-oxidized, is carbonized, activated is：From 20
DEG C 200 DEG C are warming up to through 22min, keep temperature 120min, 750 DEG C are warming up to by 70min, keep temperature 70min, after
Terminating heating program makes its natural cooling；Since the nitrogen that is passed through be passed through keeping after 200 DEG C of 120min, until nature
Stop being passed through nitrogen when being cooled to 200 DEG C, the flow for being passed through nitrogen is 60-80ml/min.
Step 3) by products therefrom taking-up in step 2 with hydrochloric acid solution carry out impregnate 2h processing, after cleaned with deionized water
It to neutrality, is then dried for standby, products therefrom is luffa based active carbon fiber (L-ACF)；The concentration of the hydrochloric acid solution
It is 1mol/L, the drying temperature is 60 DEG C.
L-ACF is cut into about 3 × 3cm fritters by step 4), is immersed in urea supersaturated solution, be put into ultrasonator into
Row is ultrasonically treated, after be put into baking oven and dry；It is described to immerse time for being ultrasonically treated in urea supersaturated solution and be
20min, ultrasonic power 100w, the temperature of the baking oven drying is 60 DEG C.
The L-ACF that the surface dried in step 4 is attached with urea by step 5) is put into crucible, and is wrapped up with urea powder
End, capping form semiclosed shape, are put into Muffle furnace and carry out high-temperature calcination, after calcining, cooled to room temperature is to get g-
C3N4/ L-ACF composite material crude products；The package mode is the urea powder that crucible bottom first spreads one layer of about 2-3cm thickness,
It is put into surface afterwards and is attached with the L-ACF of urea, then covers the urea powder of 4-5cm thickness, finally covers crucible cover；The Muffle furnace
Calcination temperature be 550 DEG C, calcination time 3h, heating rate be 2 DEG C/min.
Surface in step 5 is attached with g-C by step 6)3N4L-ACF take out, carried out with distilled water and alcohol mixed solution
It rinses, to remove the loose g-C in surface3N4Powder then puts it into baking oven and dries to get g-C3N4/ L-ACF composite woods
Material；The volume ratio of the ethyl alcohol and distillation water mixed solution is 1：1, the backwashing manner is repeatedly to rinse comprehensively, until L-
The surfaces ACF are without g-C3N4Until shed powder；The drying temperature is 60 DEG C.
Embodiment 1
Step 1：Loofah fiber is placed in the NaOH aqueous solutions that mass concentration is 2% after impregnating for 24 hours, it is molten to discard NaOH
Liquid is cleaned with deionized water to neutrality, after be put into baking oven in 105 DEG C drying；Luffa after drying, which is placed in solid content, is
It is impregnated in 36% phenolic resin aqueous solution for 24 hours, takes out naturally dry and be placed in baking oven, 1.5h is toasted in 105 DEG C；
Step 2：The luffa dried in step 1 is placed in high temperature tubular resistor furnace and pre-oxidized, be carbonized, at activation
Reason, the heating procedure of resistance furnace are：200 DEG C are warming up to from 20 DEG C through 22min, temperature 120min is kept, heats up by 70min
To 750 DEG C, keep temperature 70min, after terminate heat program make its natural cooling；Lead to since keeping after 200 DEG C of 120min
Inbound traffics are the nitrogen of 70ml/min, until stopping being passed through when naturally cooling to 200 DEG C；
Step 3：Products therefrom in step 2 is taken out and is carried out impregnating 2h processing with the hydrochloric acid solution of a concentration of 1mol/L, after
It is cleaned to neutrality with deionized water, is subsequently placed in baking oven and is dried for standby at 60 DEG C, products therefrom is luffa matrix activated carbon
Fiber (L-ACF)；
Step 4：L-ACF is cut into about 4 × 4cm fritters, is immersed in the urea supersaturated solution of 100ml, is put into ultrasound and shakes
Swing the oscillation of power 20min with 100w in device, after be put at 60 DEG C of baking oven and dry；
Step 5：The urea powder of 2cm thickness, the surface that will be dried in step 4 are laid in crucible bottom big 330ml in advance
The L-ACF for being attached with urea is put into wherein, then is laid with the urea powder of one layer of 4cm thickness on surface, and rear capping forms semiclosed shape,
It is put into Muffle furnace and rises to 550 DEG C with the heating rate of 2 DEG C/min, keep temperature 3h, after calcining, naturally cool to room
Temperature is attached with g-C to get surface3N4L-ACF g-C3N4/ L-ACF composite material crude products；
Step 6：Surface in step 5 is attached with g-C3N4L-ACF take out, with distilled water and ethyl alcohol volume ratio for 1：1
Mixed solution repeatedly rinse comprehensively, until surface is without g-C3N4Until shed powder, then put it into baking oven in 60 DEG C
Lower drying is to get g-C3N4/ L-ACF composite materials.
With 1 gained g-C of embodiment3N4/ L-ACF composite materials, g-C3N4Powder, L-ACF are characterized as follows：
As shown in Figure 1, being observed under scanning electron microscope, it is seen that g-C3N4It is successfully wrapped on the single fiber of L-ACF, and
And the fiber surface under high power under visible package is rich in porous.
As shown in Fig. 2, by g-C3N4Its UV-Vis absorption curves have no large change after being carried on L-ACF, visible
Still there is preferable assimilation effect in light region.
Table 1
As shown in table 1, g-C3N4After being carried on L-ACF, g-C3N4The specific surface area of/L-ACF composite materials on
It rises, is conducive to it to pollutant fast enriching, is finally reached the purpose of efficient degradation.
As shown in figure 3, being g-C3N4/ L-ACF composite materials, g-C3N4The N of powder2The hole of adsorption/desorption figure and composite material
Diameter distribution map, as seen from the figure, composite material is mainly based on mesoporous.
As shown in figure 4, g-C3N4/ L-ACF composite materials, g-C3N4Powder, L-ACF three XRD spectrum show, g-
C3N4There is g-C simultaneously in the XRD spectrum of/L-ACF composite materials3N4The characteristic absorption peak of powder and L-ACF, shows g-C3N4
Powder is successfully wrapped on L-ACF.
As shown in figure 5, reaction condition is, the g-C of about 4 × 4cm3N4The L-ACF of/L-ACF composite materials or 4 × 4cm,
It is added in the RhB solution of a concentration of mg/L of 200ml, the high-pressure sodium lamp of 500W is selected to make visible light source, it can be with from degradation curve
Find out, composite material and L-ACF have RhB certain adsorption effect, but load g-C3N4L-ACF afterwards can persistently to RhB into
Row degradation, it is seen that photocatalytic degradation effect is preferable.
As shown in fig. 6, g-C3N4/ L-ACF composite materials degrade to RhB using 5 times, take out use after use every time
Distilled water and alcohol mixed solution carry out cleaning down, then 60 DEG C of drying are for use, the results showed that, still using its degradation rate after 5 times
60% or more can be so maintained at, it is shown that its good recycle value.
Claims (9)
1. a kind of visible light-responded composite material, it is characterised in that by graphite phase carbon nitride powder load in luffa activated carbon
It is prepared on fiber.
2. the preparation method of visible light-responded composite material described in claim 1, it is characterised in that include the following steps：
1) loofah fiber is placed in sodium hydrate aqueous solution and impregnates 20-24h, cleaned to neutrality with deionized water, be placed in baking
It is dried in case；It is subsequently placed in phenolic resin aqueous solution and impregnates 20-24h, taking-up naturally dry, which is placed in baking oven, toasts 1-2h；
2) continue to be placed in high temperature tubular resistor furnace pre-oxidized, be carbonized, activation process, be passed through nitrogen therebetween and make protection gas；
3) continue to impregnate 2h with hydrochloric acid solution, be cleaned to neutrality with deionized water, drying obtains luffa based active carbon fiber L-
ACF；
4) luffa based active carbon fiber is cut into small pieces, immerse urea supersaturated solution in, be carried out at the same time supersound process, after put
Enter in baking oven and dries；
5) the luffa based active carbon fiber that surface is attached with to urea is put into crucible, and is wrapped up with urea powder, and shape is capped
At semiclosed shape, it is put into Muffle furnace and carries out high-temperature calcination, after calcining, cooled to room temperature；
6) it is rinsed with distilled water and alcohol mixed solution, to remove the loose g-C in surface3N4Powder then puts it into baking
Drying is to get g-C in case3N4/ L-ACF composite materials.
3. the preparation method of visible light-responded composite material as claimed in claim 2, it is characterised in that in step 1, the hydrogen
The concentration of aqueous solution of sodium oxide is 2wt%；The baking temperature in the baking oven is 105 DEG C twice；The phenolic resin is water-soluble
The solid content of liquid is 36wt%.
4. the preparation method of visible light-responded composite material as claimed in claim 2, it is characterised in that in step 2, pre-oxidation,
Carbonization, the heating procedure activated are：200 DEG C are warming up to from room temperature through 22min, keeps temperature 120min；It heats up by 70min
To 750 DEG C, temperature 70min is kept；Stop heating, natural cooling；Nitrogen starts to be passed through after keeping 120min at 200 DEG C, until
Stop being passed through nitrogen when naturally cooling to 200 DEG C.
5. the preparation method of visible light-responded composite material as claimed in claim 2, it is characterised in that in step 3, the salt
The concentration of acid solution is 1mol/L, and the drying temperature is 60 DEG C.
6. the preparation method of visible light-responded composite material as claimed in claim 2, it is characterised in that in step 4, the leaching
It is 20min, ultrasonic power 100w to enter the time being ultrasonically treated in urea supersaturated solution；The temperature of baking oven drying is 60
℃。
7. the preparation method of visible light-responded composite material as claimed in claim 2, it is characterised in that described in step 5
Package mode is that crucible bottom first spreads the urea powder of one layer of about 2-3cm thickness, after be put into the L-ACF that surface is attached with urea, then
The urea powder for covering 4-5cm thickness, finally covers crucible cover；The calcination temperature of Muffle furnace is 550 DEG C, calcination time 3h, is risen
Warm rate is 2 DEG C/min.
8. the preparation method of visible light-responded composite material as claimed in claim 2, it is characterised in that in step 6, the second
The volume ratio of alcohol and distillation water mixed solution is 1：1；Drying temperature is 60 DEG C.
9. application of the visible light-responded composite material in catalytic degradation organic matter field described in claim 1.
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