CN109092282A - A kind of hierarchical structure biomass carbon fiber/TiO2Photocatalytic degradation ammonia nitrogen material and preparation method thereof - Google Patents
A kind of hierarchical structure biomass carbon fiber/TiO2Photocatalytic degradation ammonia nitrogen material and preparation method thereof Download PDFInfo
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- CN109092282A CN109092282A CN201810935151.4A CN201810935151A CN109092282A CN 109092282 A CN109092282 A CN 109092282A CN 201810935151 A CN201810935151 A CN 201810935151A CN 109092282 A CN109092282 A CN 109092282A
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- 239000002028 Biomass Substances 0.000 title claims abstract description 122
- 239000004917 carbon fiber Substances 0.000 title claims abstract description 76
- 229920000049 Carbon (fiber) Polymers 0.000 title claims abstract description 74
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims abstract description 73
- XKMRRTOUMJRJIA-UHFFFAOYSA-N ammonia nh3 Chemical compound N.N XKMRRTOUMJRJIA-UHFFFAOYSA-N 0.000 title claims abstract description 61
- 239000000463 material Substances 0.000 title claims abstract description 42
- 238000002360 preparation method Methods 0.000 title claims abstract description 29
- 230000015556 catabolic process Effects 0.000 title description 4
- 238000006731 degradation reaction Methods 0.000 title description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 68
- 238000013033 photocatalytic degradation reaction Methods 0.000 claims abstract description 33
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 27
- 239000002994 raw material Substances 0.000 claims abstract description 14
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000006243 chemical reaction Methods 0.000 claims abstract description 13
- 229920002678 cellulose Polymers 0.000 claims abstract description 8
- 239000001913 cellulose Substances 0.000 claims abstract description 8
- 239000002070 nanowire Substances 0.000 claims abstract description 8
- 239000003054 catalyst Substances 0.000 claims abstract description 4
- 238000011065 in-situ storage Methods 0.000 claims abstract description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 140
- 239000000243 solution Substances 0.000 claims description 81
- 235000019441 ethanol Nutrition 0.000 claims description 70
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 52
- 238000003756 stirring Methods 0.000 claims description 48
- 229910052757 nitrogen Inorganic materials 0.000 claims description 28
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 25
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 24
- 238000001035 drying Methods 0.000 claims description 24
- 239000000725 suspension Substances 0.000 claims description 24
- 239000000835 fiber Substances 0.000 claims description 23
- 229960000583 acetic acid Drugs 0.000 claims description 20
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 17
- 239000010936 titanium Substances 0.000 claims description 17
- 229910052719 titanium Inorganic materials 0.000 claims description 17
- 239000003795 chemical substances by application Substances 0.000 claims description 15
- 238000005253 cladding Methods 0.000 claims description 13
- 239000007788 liquid Substances 0.000 claims description 12
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 11
- 239000000908 ammonium hydroxide Substances 0.000 claims description 11
- 238000001816 cooling Methods 0.000 claims description 11
- 239000008367 deionised water Substances 0.000 claims description 11
- 229910021641 deionized water Inorganic materials 0.000 claims description 11
- 238000010438 heat treatment Methods 0.000 claims description 11
- 239000011259 mixed solution Substances 0.000 claims description 11
- 238000001507 sample dispersion Methods 0.000 claims description 11
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 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 8
- 239000012362 glacial acetic acid Substances 0.000 claims description 8
- 244000025254 Cannabis sativa Species 0.000 claims description 6
- 235000012766 Cannabis sativa ssp. sativa var. sativa Nutrition 0.000 claims description 6
- 235000012765 Cannabis sativa ssp. sativa var. spontanea Nutrition 0.000 claims description 6
- KWYHDKDOAIKMQN-UHFFFAOYSA-N N,N,N',N'-tetramethylethylenediamine Chemical compound CN(C)CCN(C)C KWYHDKDOAIKMQN-UHFFFAOYSA-N 0.000 claims description 6
- 235000009120 camo Nutrition 0.000 claims description 6
- 235000005607 chanvre indien Nutrition 0.000 claims description 6
- 239000011487 hemp Substances 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 6
- VXUYXOFXAQZZMF-UHFFFAOYSA-N titanium(IV) isopropoxide Chemical compound CC(C)O[Ti](OC(C)C)(OC(C)C)OC(C)C VXUYXOFXAQZZMF-UHFFFAOYSA-N 0.000 claims description 6
- 240000008564 Boehmeria nivea Species 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
- 229920000742 Cotton Polymers 0.000 claims description 4
- 229920002153 Hydroxypropyl cellulose Polymers 0.000 claims description 4
- 239000002270 dispersing agent Substances 0.000 claims description 4
- 239000001863 hydroxypropyl cellulose Substances 0.000 claims description 4
- 235000010977 hydroxypropyl cellulose Nutrition 0.000 claims description 4
- 238000001354 calcination Methods 0.000 claims description 3
- 239000002699 waste material Substances 0.000 claims description 3
- 241000196324 Embryophyta Species 0.000 claims description 2
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 2
- 239000001866 hydroxypropyl methyl cellulose Substances 0.000 claims description 2
- 229920003088 hydroxypropyl methyl cellulose Polymers 0.000 claims description 2
- 235000010979 hydroxypropyl methyl cellulose Nutrition 0.000 claims description 2
- UFVKGYZPFZQRLF-UHFFFAOYSA-N hydroxypropyl methyl cellulose Chemical compound OC1C(O)C(OC)OC(CO)C1OC1C(O)C(O)C(OC2C(C(O)C(OC3C(C(O)C(O)C(CO)O3)O)C(CO)O2)O)C(CO)O1 UFVKGYZPFZQRLF-UHFFFAOYSA-N 0.000 claims description 2
- 241000219146 Gossypium Species 0.000 claims 1
- 238000002474 experimental method Methods 0.000 abstract description 13
- 239000002351 wastewater Substances 0.000 abstract description 12
- 238000007146 photocatalysis Methods 0.000 abstract description 7
- 239000002131 composite material Substances 0.000 abstract description 2
- 235000011054 acetic acid Nutrition 0.000 description 13
- -1 hydroxyl radical free radical Chemical class 0.000 description 11
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 11
- SUKJFIGYRHOWBL-UHFFFAOYSA-N sodium hypochlorite Chemical compound [Na+].Cl[O-] SUKJFIGYRHOWBL-UHFFFAOYSA-N 0.000 description 10
- 230000001699 photocatalysis Effects 0.000 description 4
- 229920003091 Methocel™ Polymers 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 230000006798 recombination Effects 0.000 description 3
- 238000005215 recombination Methods 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 150000001243 acetic acids Chemical class 0.000 description 2
- 238000011953 bioanalysis Methods 0.000 description 2
- 238000004061 bleaching Methods 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical class [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 235000019270 ammonium chloride Nutrition 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 238000012851 eutrophication Methods 0.000 description 1
- 235000010299 hexamethylene tetramine Nutrition 0.000 description 1
- VKYKSIONXSXAKP-UHFFFAOYSA-N hexamethylenetetramine Chemical compound C1N(C2)CN3CN1CN2C3 VKYKSIONXSXAKP-UHFFFAOYSA-N 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229960004011 methenamine Drugs 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 238000000053 physical method Methods 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000002798 spectrophotometry method Methods 0.000 description 1
- 230000000280 vitalizing effect Effects 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/18—Carbon
-
- B01J35/39—
-
- 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
- C02F1/32—Treatment of water, waste water, or sewage by irradiation with ultraviolet light
-
- 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
- C02F2101/10—Inorganic compounds
- C02F2101/16—Nitrogen compounds, e.g. ammonia
Abstract
The invention belongs to technical field of composite preparation, are related to photocatalytic degradation ammonia nitrogen material more particularly to a kind of hierarchical structure biomass carbon fiber/TiO2Photocatalytic degradation ammonia nitrogen material, by biomass carbon fiber and hierarchical structure TiO2Nano wire constitute, the biomass carbon fiber be using biomass as the extracted cellulose of raw material, charing after formed, diameter be 2~10 μm；The hierarchical structure TiO2Nano wire is as obtained by seed law hydro-thermal growth in situ, and nanowire diameter is 100~200nm, and length is 1~5 μm.The invention also discloses the preparation methods of the material, and are used as photochemical catalyst, remove ammonia nitrogen in water removal.Preparation process of the present invention is controllable and reaction condition is simple, by by the high-specific surface area and TiO of biomass carbon fiber2Photocatalysis performance combine, achieve the purpose that efficiently quickly removal ammonia nitrogen.Removal ammonia nitrogen waste water is simulated by experiment, the results showed that, removal rate is up to 97.3% under ultraviolet irradiation, provides reliable theoretical and actual support for practical application.
Description
Technical field
The invention belongs to technical field of composite preparation, are related to photocatalytic degradation ammonia nitrogen material, more particularly to a kind of point
Level structure biomass carbon fiber/TiO2Photocatalytic degradation ammonia nitrogen material and preparation method thereof, suitable for preparing photocatalysis water body
Degradation of ammonia nitrogen material.
Background technique
In recent years since fertilising is excessive, Pesticide use is unreasonable, so that a large amount of nitrogens input river, river, lake, lead to water
Worse and worse, especially water eutrophication increasingly takes place frequently environment, and Dissolved Oxygen in Water is caused to decline, water quality deterioration, thus broken
Bad water ecology balance.Ammonia nitrogen processing method is divided into physical method, bioanalysis and chemical method.It is raw at present for the ammonia nitrogen of low concentration
The processing of object method is relatively conventional；But under the conditions of high pollution ammonia nitrogen concentration, bioanalysis is to conditions such as weather, temperature, organic concentrations
It is more harsh, management investment and higher cost, it is therefore desirable to find efficient, quickly removal ammonia nitrogen method and material.
With the progress of science and technology, researcher's discovery is aobvious by the effect of photocatalytic degradation ammonia nitrogen using semiconductor material
It writes.So-called photocatalysis technology refers to the ultraviolet light vitalizing semiconductor using sunlight, forms it into electron-hole pair, to produce
Raw hydroxyl radical free radical, using the strong oxidizing property of hydroxyl radical free radical come degradation of ammonia nitrogen.Such as TiO2It is exactly a kind of more common half
Conductor material, but the electron-hole pair recombination rate of pure semiconductor material is higher, and adulterate it is nonmetallic can to avoid the disadvantage,
And band-gap energy can be reduced, photocatalysis efficiency is improved.
Summary of the invention
In view of the above-mentioned deficiencies in the prior art, the object of the present invention is to provide a kind of hierarchical structure biomass Carbon fibers
Dimension/TiO2Photocatalytic degradation ammonia nitrogen material and preparation method thereof.Material preparation process is controllable and experiment condition is simple, by that will give birth to
The high-specific surface area and TiO of substance Carbon fibe2Photocatalysis performance combine, achieve the purpose that efficiently quickly removal ammonia nitrogen.
Technical solution:
A kind of hierarchical structure biomass carbon fiber/TiO2Photocatalytic degradation ammonia nitrogen material, by biomass carbon fiber and hierarchical structure
TiO2Nano wire constitute, the biomass carbon fiber be using biomass as the extracted cellulose of raw material, charing after formed, diameter
It is 2~10 μm；The hierarchical structure TiO2Nano wire is the nanowire diameter 100 as obtained by seed law hydro-thermal growth in situ
~200nm, length are 1~5 μm.
The invention discloses above-mentioned hierarchical structure biomass carbon fiber/TiO2The preparation side of photocatalytic degradation ammonia nitrogen material
Method includes the following steps:
A) it after shredding biomass material, is added based on 40~60g biomass raw material by every 100mL aqueous slkali, is added to quality
Score is 80 DEG C of 4 h of stirring in the aqueous slkali of 3~9wt%, takes out and is washed with deionized to neutrality, drying；Preparation 2~
The NaClO of 8wt%2PH value is simultaneously adjusted to 4 with acetic acid by solution, by the drying sample dispersion in NaClO270 DEG C of stirrings in solution
5 h are bleached, and are then cleaned with deionized water and ethyl alcohol to neutrality, and biomass fiber is obtained after 70 DEG C of baking 12h；
B) biomass fiber is placed in tube furnace, rises to 400~600 DEG C with the heating rate of 5~10 DEG C/min, protected in nitrogen
Shield, which is descended, calcines 2~4 h, preferably 500 DEG C calcining 3h, obtains biomass carbon fiber after natural cooling；
C) mixed solution A for preparing second alcohol and water in proportion, be added in every 100mL solution A 0.1~0.3g biomass carbon fiber and
0.2~0.4g dispersing agent, stirring 30min obtains unit for uniform suspension B after ultrasonic 30min；
D) solution C is obtained after being mixed evenly according to every 2mL titanium source with 20mL ethanol solution, will using the low liquid funnel of constant pressure
Solution C instills in suspension B, and keeping drop speed is 1 drop/sec, stirs 10~15h, takes out samples with water and ethyl alcohol cleans 3 times,
10h is dried under the conditions of 80 DEG C and obtains titanium cladding biomass carbon fiber, wherein the ethyl alcohol of the ethanol solution and the volume ratio of water are
10:1；The volume ratio that solution C instills suspension B is 22mL:100mL；
E) titanium cladding biomass carbon fiber and guiding agent is added in every 60mL glacial acetic acid, and wherein guiding agent and sample quality ratio are 1g:5
~10g adjusts solution ph 9~11 using ammonium hydroxide, is transferred in reaction kettle after stirring 30min, 120~160 DEG C of hydro-thermal reactions 20
~30h is cleaned three times after taking-up with water and ethyl alcohol, 80~100 DEG C of drying 10h.
In the more excellent disclosed example of the present invention, biomass described in step a) is plant biomass, especially waste and old biomass, such as cotton
Any one of flower, hemp or ramie etc..
In the more excellent disclosed example of the present invention, aqueous slkali described in step a) is potassium hydroxide or sodium hydroxide, preferably hydroxide
Sodium.
In the more excellent disclosed example of the present invention, ratio described in step c) is that the volume ratio of second alcohol and water is 90~110:1, preferably
100:1；The dispersing agent is hydroxypropyl cellulose or hydroxypropyl methyl cellulose, preferably hydroxypropyl cellulose.
In the more excellent disclosed example of the present invention, titanium source described in step d) is isopropyl titanate or butyl titanate, preferably four fourth of metatitanic acid
Ester.
In the more excellent disclosed example of the present invention, guiding agent described in step e) is N, N, N, N '-tetramethylethylenediamine, urea, six
Any one of methenamine, preferably N, N, N, N '-tetramethylethylenediamine.
The invention also discloses by the hierarchical structure biomass carbon fiber/TiO2Photocatalytic degradation ammonia nitrogen material is answered
With, be used as photochemical catalyst, go water removal in ammonia nitrogen.
Simulated experiment removes nitrogen-containing wastewater
(1) it is soluble in water through 100 DEG C of dried excellent pure grade ammonium chlorides to weigh 0.3819g, moves into 1000mL volumetric flask, dilution
To graticule, this solution concentration is 100mg/L ammonia nitrogen；
(2) 100mL ammonia nitrogen solution is taken, 25mg hierarchical structure biomass carbon fiber/TiO is weighed2Photochemical catalyst is dispersed in ammonia
In nitrogen solution, photocatalytic degradation, illumination 10h are simulated using the ultraviolet lamp that power is 25W；
(3) using ammonia nitrogen solution concentration after spectrophotometry measurement photocatalytic degradation, ammonia nitrogen removal frank is calculated.
Beneficial effect
The invention discloses a kind of hierarchical structure biomass carbon fiber/TiO2Photocatalytic degradation ammonia nitrogen material and preparation method thereof.
Material preparation process is controllable and reaction condition is simple, by by the high-specific surface area and TiO of biomass carbon fiber2Photocatalytic
It can combine, achieve the purpose that efficiently quickly removal ammonia nitrogen.Removal ammonia nitrogen waste water is simulated by experiment, the results showed that, ultraviolet
Removal rate is up to 97.3% under the irradiation of line, provides reliable theoretical and actual support for practical application.
The invention has the characteristics that
(1) using waste and old biomass as the presoma of biomass carbon fiber, have it is low in cost, stable, without secondary pollution with
And the features such as environmentally protective；
(2) hierarchical structure biomass carbon fiber/TiO2Photocatalytic degradation ammonia nitrogen material is by by the Gao Bibiao of biomass carbon fiber
Area and TiO2Photocatalysis performance combines, and achievees the effect that efficiently quickly removal ammonia nitrogen；
(3) simple TiO2Catalytic effect is unsatisfactory due to electron-hole pair recombination rate is high, can by adulterating with non-metal carbon
Electron-hole pair recombination rate and band-gap energy are reduced, photocatalysis efficiency is improved.
Detailed description of the invention
Fig. 1 is hierarchical structure biomass carbon fiber/TiO prepared by embodiment 52Photocatalytic degradation ammonia nitrogen material
SEM。
Specific embodiment
The following describes the present invention in detail with reference to examples, so that those skilled in the art more fully understand this hair
It is bright, but the invention is not limited to following embodiments.
Embodiment 1
Hierarchical structure biomass carbon fiber/TiO2The preparation method of photocatalytic degradation ammonia nitrogen material, includes the following steps:
A) it after shredding old and useless cotton, is added based on 40g biomass raw material by 100mL aqueous slkali, being added to mass fraction is
In the sodium hydroxide solution of 3wt%, under 80 DEG C of environment, after stirring 4 h, takes out and be washed with deionized to neutrality, drying.
Prepare the NaClO of 2wt%2Solution and pH value is adjusted to 4 with acetic acid, by above-mentioned drying sample dispersion in NaClO2It is carried out in solution
Bleaching stirs 5 h, is then cleaned with deionized water and ethyl alcohol to neutrality, dried in 70 DEG C of baking oven in the environment of 70 DEG C
Biomass fiber is obtained after 12h.
B) biomass fiber is placed in tube furnace, rises to 400 DEG C with the heating rate of 5 DEG C/min, under nitrogen protection
2 h are calcined, obtain biomass carbon fiber after natural cooling.
C) ethyl alcohol by volume: water=90:1 ratio prepares mixed solution A, takes 0.1g biomass carbon fiber and 0.2g hydroxyl
Propyl methocel is dissolved in 100mL solution A, and 30min is stirred after ultrasonic 30min and obtains unit for uniform suspension B.
D) 2mL isopropyl titanate and 20mL ethyl alcohol (volume ratio ethyl alcohol: water=10:1) is taken to mix, stirring 10min obtains solution C,
Solution C is instilled in suspension B using constant pressure low liquid funnel, and keeping speed is 1 drop/sec, then stirs 10h, takes out sample
It is cleaned 3 times with water and ethyl alcohol, 10h is dried under the conditions of 80 DEG C and obtains titanium cladding biomass carbon fiber.
E) it based on by guiding agent and sample quality ratio for 1:5, takes 1g sample and 0.2g urea to be placed in 60mL glacial acetic acid, utilizes
Ammonium hydroxide adjusts pH value of solution=9, is transferred in reaction kettle after stirring 30min, hydro-thermal 20h under the conditions of 120 DEG C, uses water after taking out sample
After ethyl alcohol cleaning three times, 10h is dried under the conditions of 80 DEG C.
Nitrogen-containing wastewater, ammonia nitrogen removal frank 79.1% are removed by simulated experiment.
Embodiment 2
Hierarchical structure biomass carbon fiber/TiO2The preparation method of photocatalytic degradation ammonia nitrogen material, includes the following steps:
A) it after shredding old and useless cotton, is added based on 50g biomass raw material by 100mL aqueous slkali, being added to mass fraction is
In the sodium hydroxide solution of 9wt%, under 80 DEG C of environment, after stirring 4 h, takes out and be washed with deionized to neutrality, drying.
Prepare the NaClO of 5wt%2Solution and pH value is adjusted to 4 with acetic acid, by above-mentioned drying sample dispersion in NaClO2It is carried out in solution
Bleaching stirs 5 h, is then cleaned with deionized water and ethyl alcohol to neutrality, dried in 70 DEG C of baking oven in the environment of 70 DEG C
Biomass fiber is obtained after 12h.
B) biomass fiber is placed in tube furnace, rises to 500 DEG C with the heating rate of 8 DEG C/min, under nitrogen protection
3 h are calcined, obtain biomass carbon fiber after natural cooling.
C) ethyl alcohol by volume: water=100:1 ratio prepares mixed solution A, takes 0.2g biomass carbon fiber and 0.2g hydroxyl
Propyl methocel is dissolved in 100mL solution A, and 30min is stirred after ultrasonic 30min and obtains unit for uniform suspension B.
D) 2mL isopropyl titanate and 20mL ethyl alcohol (volume ratio ethyl alcohol: water=10:1) is taken to mix, stirring 10min obtains solution C,
Solution C is instilled in suspension B using constant pressure low liquid funnel, and keeping speed is 1 drop/sec, then stirs 12h, takes out sample
It is cleaned 3 times with water and ethyl alcohol, 10h is dried under the conditions of 80 DEG C and obtains titanium cladding biomass carbon fiber.
E) based on by guiding agent and sample quality ratio for 1:8,1.6g sample and 0.2g N, N, N, N '-tetramethylethylenediamine are taken
It is placed in 60mL glacial acetic acid, adjusts pH value of solution=10 using ammonium hydroxide, be transferred in reaction kettle after stirring 30min, under the conditions of 140 DEG C
Hydro-thermal 26h, take out sample after cleaned three times with water and ethyl alcohol after, dry 10h under the conditions of 90 DEG C.
Nitrogen-containing wastewater, ammonia nitrogen removal frank 83.6% are removed by simulated experiment.
Embodiment 3
Hierarchical structure biomass carbon fiber/TiO2The preparation method of photocatalytic degradation ammonia nitrogen material, includes the following steps:
A) it after shredding hemp, is added based on 60g biomass raw material by 100mL aqueous slkali, being added to mass fraction is 5wt%'s
In sodium hydroxide solution, under 80 DEG C of environment, after stirring 4 h, takes out and be washed with deionized to neutrality, drying.It prepares
The NaClO of 8wt%2Solution and pH value is adjusted to 4 with acetic acid, by above-mentioned drying sample dispersion in NaClO2It is floated in solution
It is white, in the environment of 70 DEG C, 5 h are stirred, is then cleaned with deionized water and ethyl alcohol to neutrality, is dried in 70 DEG C of baking oven
Biomass fiber is obtained after 12h.
B) biomass fiber is placed in tube furnace, rises to 600 DEG C with the heating rate of 10 DEG C/min, under nitrogen protection
4 h are calcined, obtain biomass carbon fiber after natural cooling.
C) ethyl alcohol by volume: water=110:1 ratio prepares mixed solution A, takes 0.3g biomass carbon fiber and 0.3g hydroxyl
Propyl methocel is dissolved in 100mL solution A, and 30min is stirred after ultrasonic 30min and obtains unit for uniform suspension B.
D) 2mL isopropyl titanate and 20mL ethyl alcohol (volume ratio ethyl alcohol: water=10:1) is taken to mix, stirring 10min obtains solution C,
Solution C is instilled in suspension B using constant pressure low liquid funnel, and keeping speed is 1 drop/sec, then stirs 13h, takes out sample
It is cleaned 3 times with water and ethyl alcohol, 10h is dried under the conditions of 80 DEG C and obtains titanium cladding biomass carbon fiber.
E) based on by guiding agent and sample quality ratio for 1:10,2.0g sample and 0.2g hexa is taken to be placed in 60mL
In glacial acetic acids, pH value of solution=11 are adjusted using ammonium hydroxide, are transferred in reaction kettle after stirring 30min, hydro-thermal 30h under the conditions of 160 DEG C,
After being cleaned three times after taking-up sample with water and ethyl alcohol, 10h is dried under the conditions of 100 DEG C.
Nitrogen-containing wastewater, ammonia nitrogen removal frank 86.9% are removed by simulated experiment.
Embodiment 4
Hierarchical structure biomass carbon fiber/TiO2The preparation method of photocatalytic degradation ammonia nitrogen material, includes the following steps:
A) it after shredding hemp, is added based on 40g biomass raw material by 100mL aqueous slkali, being added to mass fraction is 7wt%'s
In sodium hydroxide solution, under 80 DEG C of environment, after stirring 4 h, takes out and be washed with deionized to neutrality, drying.It prepares
The NaClO of 2wt%2Solution and pH value is adjusted to 4 with acetic acid, by above-mentioned drying sample dispersion in NaClO2It is floated in solution
It is white, in the environment of 70 DEG C, 5 h are stirred, is then cleaned with deionized water and ethyl alcohol to neutrality, is dried in 70 DEG C of baking oven
Biomass fiber is obtained after 12h.
B) biomass fiber is placed in tube furnace, rises to 400 DEG C with the heating rate of 5 DEG C/min, under nitrogen protection
2 h are calcined, obtain biomass carbon fiber after natural cooling.
C) ethyl alcohol by volume: water=90:1 ratio prepares mixed solution A, takes 0.1g biomass carbon fiber and 0.4g hydroxyl
Hydroxypropyl methyl fiber is dissolved in 100mL solution A, and 30min is stirred after ultrasonic 30min and obtains unit for uniform suspension B.
D) 2mL isopropyl titanate and 20mL ethyl alcohol (volume ratio ethyl alcohol: water=10:1) is taken to mix, stirring 10min obtains solution C,
Solution C is instilled in suspension B using constant pressure low liquid funnel, and keeping speed is 1 drop/sec, then stirs 15h, takes out sample
It is cleaned 3 times with water and ethyl alcohol, 10h is dried under the conditions of 80 DEG C and obtains titanium cladding biomass carbon fiber.
E) based on by guiding agent and sample quality ratio for 1:5,1.0g sample and 0.2g urea is taken to be placed in 60mL glacial acetic acid,
PH value of solution=9 are adjusted using ammonium hydroxide, are transferred in reaction kettle after stirring 30min, hydro-thermal 20h under the conditions of 120 DEG C, after taking out sample
After being cleaned three times with water and ethyl alcohol, 10h is dried under the conditions of 80 DEG C.
Nitrogen-containing wastewater, ammonia nitrogen removal frank 91.5% are removed by simulated experiment.
Embodiment 5
Hierarchical structure biomass carbon fiber/TiO2The preparation method of photocatalytic degradation ammonia nitrogen material, includes the following steps:
A) it after shredding hemp, is added based on 50g biomass raw material by 100mL aqueous slkali, being added to mass fraction is 6wt%'s
In sodium hydroxide solution, under 80 DEG C of environment, after stirring 4 h, takes out and be washed with deionized to neutrality, drying.It prepares
The NaClO of 5wt%2Solution and pH value is adjusted to 4 with acetic acid, by above-mentioned drying sample dispersion in NaClO2It is floated in solution
It is white, in the environment of 70 DEG C, 5 h are stirred, is then cleaned with deionized water and ethyl alcohol to neutrality, is dried in 70 DEG C of baking oven
Biomass fiber is obtained after 12h.
B) biomass fiber is placed in tube furnace, rises to 500 DEG C with the heating rate of 8 DEG C/min, under nitrogen protection
3 h are calcined, obtain biomass carbon fiber after natural cooling.
C) ethyl alcohol by volume: water=100:1 ratio prepares mixed solution A, takes 0.2g biomass carbon fiber and 0.3g hydroxyl
Propyl cellulose is dissolved in 100mL solution A, and 30min is stirred after ultrasonic 30min and obtains unit for uniform suspension B.
D) 2mL butyl titanate and 20mL ethyl alcohol (volume ratio ethyl alcohol: water=10:1) is taken to mix, stirring 10min obtains solution
C is instilled solution C in suspension B using the low liquid funnel of constant pressure, and keeping speed is 1 drop/sec, then stirs 12h, takes out sample
Product water and ethyl alcohol clean 3 times, and 10h is dried under the conditions of 80 DEG C and obtains titanium cladding biomass carbon fiber.
E) based on by guiding agent and sample quality ratio for 1:8,1.6g sample and 0.2g N, N, N, N '-tetramethylethylenediamine are taken
It is placed in 60mL glacial acetic acid, adjusts pH value of solution=10 using ammonium hydroxide, be transferred in reaction kettle after stirring 30min, under the conditions of 140 DEG C
Hydro-thermal 26h, take out sample after cleaned three times with water and ethyl alcohol after, dry 10h under the conditions of 90 DEG C.
Nitrogen-containing wastewater, ammonia nitrogen removal frank 97.3% are removed by simulated experiment.
Embodiment 6
Hierarchical structure biomass carbon fiber/TiO2The preparation method of photocatalytic degradation ammonia nitrogen material, includes the following steps:
A) it after shredding hemp, is added based on 60g biomass raw material by 100mL aqueous slkali, being added to mass fraction is 3wt%'s
In potassium hydroxide solution, under 80 DEG C of environment, after stirring 4 h, takes out and be washed with deionized to neutrality, drying.It prepares
The NaClO of 8wt%2Solution and pH value is adjusted to 4 with acetic acid, by above-mentioned drying sample dispersion in NaClO2It is floated in solution
It is white, in the environment of 70 DEG C, 5 h are stirred, is then cleaned with deionized water and ethyl alcohol to neutrality, is dried in 70 DEG C of baking oven
Biomass fiber is obtained after 12h.
B) biomass fiber is placed in tube furnace, rises to 600 DEG C with the heating rate of 10 DEG C/min, under nitrogen protection
4 h are calcined, obtain biomass carbon fiber after natural cooling.
C) ethyl alcohol by volume: water=110:1 ratio prepares mixed solution A, takes 0.3g biomass carbon fiber and 0.2g hydroxyl
Propyl cellulose is dissolved in 100mL solution A, and 30min is stirred after ultrasonic 30min and obtains unit for uniform suspension B.
D) 2mL butyl titanate and 20mL ethyl alcohol (volume ratio ethyl alcohol: water=10:1) is taken to mix, stirring 10min obtains solution
C is instilled solution C in suspension B using the low liquid funnel of constant pressure, and keeping speed is 1 drop/sec, then stirs 10h, takes out sample
Product water and ethyl alcohol clean 3 times, and 10h is dried under the conditions of 80 DEG C and obtains titanium cladding biomass carbon fiber.
E) based on by guiding agent and sample quality ratio for 1:10,2.0g sample and 0.2g hexa is taken to be placed in 60mL
In glacial acetic acids, pH value of solution=11 are adjusted using ammonium hydroxide, are transferred in reaction kettle after stirring 30min, hydro-thermal 30h under the conditions of 160 DEG C,
After being cleaned three times after taking-up sample with water and ethyl alcohol, 10h is dried under the conditions of 100 DEG C.
Nitrogen-containing wastewater, ammonia nitrogen removal frank 90.4% are removed by simulated experiment.
Embodiment 7
Hierarchical structure biomass carbon fiber/TiO2The preparation method of photocatalytic degradation ammonia nitrogen material, includes the following steps:
A) it after shredding ramie, is added based on 60g biomass raw material by 100mL aqueous slkali, being added to mass fraction is 6wt%'s
In potassium hydroxide solution, under 80 DEG C of environment, after stirring 4 h, takes out and be washed with deionized to neutrality, drying.It prepares
The NaClO of 2wt%2Solution and pH value is adjusted to 4 with acetic acid, by above-mentioned drying sample dispersion in NaClO2It is floated in solution
It is white, in the environment of 70 DEG C, 5 h are stirred, is then cleaned with deionized water and ethyl alcohol to neutrality, is dried in 70 DEG C of baking oven
Biomass fiber is obtained after 12h.
B) biomass fiber is placed in tube furnace, rises to 400 DEG C with the heating rate of 5 DEG C/min, under nitrogen protection
2 h are calcined, obtain biomass carbon fiber after natural cooling.
C) ethyl alcohol by volume: water=90:1 ratio prepares mixed solution A, takes 0.1g biomass carbon fiber and 0.4g hydroxyl
Propyl cellulose is dissolved in 100mL solution A, and 30min is stirred after ultrasonic 30min and obtains unit for uniform suspension B.
D) 2mL butyl titanate and 20mL ethyl alcohol (volume ratio ethyl alcohol: water=10:1) is taken to mix, stirring 10min obtains solution
C is instilled solution C in suspension B using the low liquid funnel of constant pressure, and keeping speed is 1 drop/sec, then stirs 13h, takes out sample
Product water and ethyl alcohol clean 3 times, and 10h is dried under the conditions of 80 DEG C and obtains titanium cladding biomass carbon fiber.
E) based on by guiding agent and sample quality ratio for 1:5,1.0g sample and 0.2g urea is taken to be placed in 60mL glacial acetic acid,
PH value of solution=9 are adjusted using ammonium hydroxide, are transferred in reaction kettle after stirring 30min, hydro-thermal 20h under the conditions of 120 DEG C, after taking out sample
After being cleaned three times with water and ethyl alcohol, 10h is dried under the conditions of 80 DEG C.
Nitrogen-containing wastewater, ammonia nitrogen removal frank 86.1% are removed by simulated experiment.
Embodiment 8
Hierarchical structure biomass carbon fiber/TiO2The preparation method of photocatalytic degradation ammonia nitrogen material, includes the following steps:
A) it after shredding ramie, is added based on 50g biomass raw material by 100mL aqueous slkali, being added to mass fraction is 7wt%'s
In potassium hydroxide solution, under 80 DEG C of environment, after stirring 4 h, takes out and be washed with deionized to neutrality, drying.It prepares
The NaClO of 5wt%2Solution and pH value is adjusted to 4 with acetic acid, by above-mentioned drying sample dispersion in NaClO2It is floated in solution
It is white, in the environment of 70 DEG C, 5 h are stirred, is then cleaned with deionized water and ethyl alcohol to neutrality, is dried in 70 DEG C of baking oven
Biomass fiber is obtained after 12h.
B) biomass fiber is placed in tube furnace, rises to 500 DEG C with the heating rate of 8 DEG C/min, under nitrogen protection
3 h are calcined, obtain biomass carbon fiber after natural cooling.
C) ethyl alcohol by volume: water=100:1 ratio prepares mixed solution A, takes 0.2g biomass carbon fiber and 0.4g hydroxyl
Propyl cellulose is dissolved in 100mL solution A, and 30min is stirred after ultrasonic 30min and obtains unit for uniform suspension B.
D) 2mL butyl titanate and 20mL ethyl alcohol (volume ratio ethyl alcohol: water=10:1) is taken to mix, stirring 10min obtains solution
C is instilled solution C in suspension B using the low liquid funnel of constant pressure, and keeping speed is 1 drop/sec, then stirs 14h, takes out sample
Product water and ethyl alcohol clean 3 times, and 10h is dried under the conditions of 80 DEG C and obtains titanium cladding biomass carbon fiber.
E) based on by guiding agent and sample quality ratio for 1:8,1.6g sample and 0.2g hexa is taken to be placed in 60mL ice
In acetic acid, pH value of solution=10 are adjusted using ammonium hydroxide, are transferred in reaction kettle after stirring 30min, hydro-thermal 26h under the conditions of 140 DEG C takes
After being cleaned three times after sample with water and ethyl alcohol out, 10h is dried under the conditions of 90 DEG C.
Nitrogen-containing wastewater, ammonia nitrogen removal frank 82.6% are removed by simulated experiment.
Embodiment 9
Hierarchical structure biomass carbon fiber/TiO2The preparation method of photocatalytic degradation ammonia nitrogen material, includes the following steps:
A) it after shredding ramie, is added based on 40g biomass raw material by 100mL aqueous slkali, being added to mass fraction is 9wt%'s
In potassium hydroxide solution, under 80 DEG C of environment, after stirring 4 h, takes out and be washed with deionized to neutrality, drying.It prepares
The NaClO of 8wt%2Solution and pH value is adjusted to 4 with acetic acid, by above-mentioned drying sample dispersion in NaClO2It is floated in solution
It is white, in the environment of 70 DEG C, 5 h are stirred, is then cleaned with deionized water and ethyl alcohol to neutrality, is dried in 70 DEG C of baking oven
Biomass fiber is obtained after 12h.
B) biomass fiber is placed in tube furnace, rises to 600 DEG C with the heating rate of 10 DEG C/min, under nitrogen protection
4 h are calcined, obtain biomass carbon fiber after natural cooling.
C) ethyl alcohol by volume: water=110:1 ratio prepares mixed solution A, takes 0.3g biomass carbon fiber and 0.2g hydroxyl
Propyl cellulose is dissolved in 100mL solution A, and 30min is stirred after ultrasonic 30min and obtains unit for uniform suspension B.
D) 2mL butyl titanate and 20mL ethyl alcohol (volume ratio ethyl alcohol: water=10:1) is taken to mix, stirring 10min obtains solution
C is instilled solution C in suspension B using the low liquid funnel of constant pressure, and keeping speed is 1 drop/sec, then stirs 15h, takes out sample
Product water and ethyl alcohol clean 3 times, and 10h is dried under the conditions of 80 DEG C and obtains titanium cladding biomass carbon fiber.
E) based on by guiding agent and sample quality ratio for 1:10,2.0 g samples and 0.2g N, N, N, N are taken '-tetramethyl second two
Amine is placed in 60mL glacial acetic acid, is adjusted pH value of solution=11 using ammonium hydroxide, is transferred in reaction kettle after stirring 30min, in 160 DEG C of conditions
Lower hydro-thermal 30h, take out sample after cleaned three times with water and ethyl alcohol after, dry 10h under the conditions of 100 DEG C.
Nitrogen-containing wastewater, ammonia nitrogen removal frank 77.8% are removed by simulated experiment.
The above description is only an embodiment of the present invention, is not intended to limit the scope of the invention, all to utilize this hair
Equivalent structure or equivalent flow shift made by bright specification is applied directly or indirectly in other relevant technical fields,
Similarly it is included within the scope of the present invention.
Claims (10)
1. a kind of hierarchical structure biomass carbon fiber/TiO2Photocatalytic degradation ammonia nitrogen material, by biomass carbon fiber and hierarchical structure
TiO2Nano wire is constituted, it is characterised in that: the biomass carbon fiber is using biomass as the extracted cellulose of raw material, charing
After formed, diameter be 2~10 μm；The hierarchical structure TiO2Nano wire is the nanometer as obtained by seed law hydro-thermal growth in situ
Linear diameter is 100~200nm, and length is 1~5 μm.
2. a kind of prepare hierarchical structure biomass carbon fiber/TiO as described in claim 12The side of photocatalytic degradation ammonia nitrogen material
Method, which comprises the steps of:
It after biomass material is shredded, is added based on 40~60g biomass raw material by every 100mL aqueous slkali, is added to quality point
Number is 80 DEG C of 4 h of stirring in the aqueous slkali of 3~9wt%, takes out and is washed with deionized to neutrality, drying；Prepare 2~8wt%
NaClO2PH value is simultaneously adjusted to 4 with acetic acid by solution, by the drying sample dispersion in NaClO270 DEG C of 5 h of stirring in solution
It is bleached, is then cleaned with deionized water and ethyl alcohol to neutrality, biomass fiber is obtained after 70 DEG C of baking 12h；
Biomass fiber is placed in tube furnace, 400~600 DEG C are risen to the heating rate of 5~10 DEG C/min, in nitrogen protection
2~4 h of lower calcining, after natural cooling biomass carbon fiber, preferably 500 DEG C calcining 3h；
The mixed solution A for preparing second alcohol and water in proportion, be added in every 100mL solution A 0.1~0.3g biomass carbon fiber and
0.2~0.4g dispersing agent, stirring 30min obtains unit for uniform suspension B after ultrasonic 30min；
Solution C is obtained after being mixed evenly according to every 2mL titanium source with 20mL ethanol solution, will be molten using the low liquid funnel of constant pressure
Liquid C is instilled in suspension B, and keeping drop speed is 1 drop/sec, stirs 10~15h, is taken out samples with water and ethyl alcohol and is cleaned 3 times, and 80
10h is dried under the conditions of DEG C obtains titanium cladding biomass carbon fiber, wherein the volume ratio of the ethyl alcohol of the ethanol solution and water is 10:
1；The volume ratio that solution C instills suspension B is 22mL:100mL；
Titanium cladding biomass carbon fiber and guiding agent is added in every 60mL glacial acetic acid, wherein guiding agent and sample quality ratio be 1g:5~
10g adjusts solution ph 9~11 using ammonium hydroxide, is transferred in reaction kettle after stirring 30min, and 120~160 DEG C of hydro-thermal reactions 20~
30h is cleaned three times after taking-up with water and ethyl alcohol, 80~100 DEG C of drying 10h.
3. hierarchical structure biomass carbon fiber/TiO according to claim 22The preparation method of photocatalytic degradation ammonia nitrogen material,
It is characterized by: biomass described in step a) is plant biomass.
4. hierarchical structure biomass carbon fiber/TiO according to claim 22The preparation method of photocatalytic degradation ammonia nitrogen material,
It is characterized by: biomass described in step a) is any one of waste and old biomass, such as cotton, hemp or ramie.
5. hierarchical structure biomass carbon fiber/TiO according to claim 22The preparation method of photocatalytic degradation ammonia nitrogen material,
It is characterized by: aqueous slkali described in step a) is potassium hydroxide or sodium hydroxide.
6. hierarchical structure biomass carbon fiber/TiO according to claim 22The preparation method of photocatalytic degradation ammonia nitrogen material,
It is characterized by: aqueous slkali described in step a) is sodium hydroxide.
7. hierarchical structure biomass carbon fiber/TiO according to claim 22The preparation method of photocatalytic degradation ammonia nitrogen material,
It is characterized by: the volume ratio that ratio described in step c) is second alcohol and water is 90~110:1, preferably 100:1；The dispersing agent
For hydroxypropyl cellulose or hydroxypropyl methyl cellulose, preferably hydroxypropyl cellulose.
8. hierarchical structure biomass carbon fiber/TiO according to claim 22The preparation method of photocatalytic degradation ammonia nitrogen material,
It is characterized by: titanium source described in step d) is isopropyl titanate or butyl titanate, preferably butyl titanate.
9. hierarchical structure biomass carbon fiber/TiO according to claim 22The preparation method of photocatalytic degradation ammonia nitrogen material,
It is characterized by: guiding agent described in step e) is N, N, N, N '-tetramethylethylenediamine, appointing in urea, hexa
One kind, preferably N, N, N, N '-tetramethylethylenediamine.
10. hierarchical structure biomass carbon fiber/TiO described in a kind of claim 12The application of photocatalytic degradation ammonia nitrogen material, it is special
Sign is: being used as photochemical catalyst, removes ammonia nitrogen in water removal.
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