CN109569733A - A kind of cotton fiber base carbon composite metal oxide/polypyrrole photochemical catalyst and preparation method - Google Patents
A kind of cotton fiber base carbon composite metal oxide/polypyrrole photochemical catalyst and preparation method Download PDFInfo
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- CN109569733A CN109569733A CN201811454336.XA CN201811454336A CN109569733A CN 109569733 A CN109569733 A CN 109569733A CN 201811454336 A CN201811454336 A CN 201811454336A CN 109569733 A CN109569733 A CN 109569733A
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- Prior art keywords
- polypyrrole
- cotton fiber
- fiber base
- base carbon
- carbon composite
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- 229920000742 Cotton Polymers 0.000 title claims abstract description 68
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 59
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 54
- 229920000128 polypyrrole Polymers 0.000 title claims abstract description 44
- 229910044991 metal oxide Inorganic materials 0.000 title claims abstract description 34
- 150000004706 metal oxides Chemical class 0.000 title claims abstract description 34
- 239000002131 composite material Substances 0.000 title claims abstract description 32
- 239000003054 catalyst Substances 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 239000000243 solution Substances 0.000 claims abstract description 43
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims abstract description 28
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 26
- 229910052751 metal Inorganic materials 0.000 claims abstract description 25
- 239000002184 metal Substances 0.000 claims abstract description 25
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims abstract description 24
- 150000003839 salts Chemical class 0.000 claims abstract description 23
- 239000005457 ice water Substances 0.000 claims abstract description 18
- 238000011068 loading method Methods 0.000 claims abstract description 13
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000000203 mixture Substances 0.000 claims abstract description 12
- 150000001875 compounds Chemical class 0.000 claims abstract description 11
- 239000005708 Sodium hypochlorite Substances 0.000 claims abstract description 10
- 229910052746 lanthanum Inorganic materials 0.000 claims abstract description 10
- SUKJFIGYRHOWBL-UHFFFAOYSA-N sodium hypochlorite Chemical compound [Na+].Cl[O-] SUKJFIGYRHOWBL-UHFFFAOYSA-N 0.000 claims abstract description 10
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000001354 calcination Methods 0.000 claims abstract description 8
- 238000006303 photolysis reaction Methods 0.000 claims abstract description 6
- 229910017052 cobalt Inorganic materials 0.000 claims abstract description 5
- 239000010941 cobalt Substances 0.000 claims abstract description 5
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229910052742 iron Inorganic materials 0.000 claims abstract description 5
- 239000012984 antibiotic solution Substances 0.000 claims abstract description 4
- 229910052761 rare earth metal Inorganic materials 0.000 claims abstract description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 46
- 239000000835 fiber Substances 0.000 claims description 26
- 229910021529 ammonia Inorganic materials 0.000 claims description 23
- 238000001035 drying Methods 0.000 claims description 16
- 238000003756 stirring Methods 0.000 claims description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 206010013786 Dry skin Diseases 0.000 claims description 10
- 150000003233 pyrroles Chemical class 0.000 claims description 10
- 239000002994 raw material Substances 0.000 claims description 9
- NYNKCGWJPNZJMI-UHFFFAOYSA-N Clebopride malate Chemical compound [O-]C(=O)C(O)CC(O)=O.COC1=CC(N)=C(Cl)C=C1C(=O)NC1CC[NH+](CC=2C=CC=CC=2)CC1 NYNKCGWJPNZJMI-UHFFFAOYSA-N 0.000 claims description 8
- 239000007788 liquid Substances 0.000 claims description 8
- 239000007864 aqueous solution Substances 0.000 claims description 7
- YASYEJJMZJALEJ-UHFFFAOYSA-N Citric acid monohydrate Chemical compound O.OC(=O)CC(O)(C(O)=O)CC(O)=O YASYEJJMZJALEJ-UHFFFAOYSA-N 0.000 claims description 6
- 229960002303 citric acid monohydrate Drugs 0.000 claims description 6
- 239000012153 distilled water Substances 0.000 claims description 6
- 239000004744 fabric Substances 0.000 claims description 6
- 239000011259 mixed solution Substances 0.000 claims description 6
- 238000007146 photocatalysis Methods 0.000 claims description 6
- 230000001699 photocatalysis Effects 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- 239000000126 substance Substances 0.000 claims description 5
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 claims description 3
- 239000000356 contaminant Substances 0.000 claims description 3
- 229910052748 manganese Inorganic materials 0.000 claims description 3
- 239000011572 manganese Substances 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 2
- 239000007787 solid Substances 0.000 claims description 2
- 150000003751 zinc Chemical class 0.000 claims description 2
- 239000003795 chemical substances by application Substances 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 5
- 238000001027 hydrothermal synthesis Methods 0.000 abstract description 3
- 239000011701 zinc Substances 0.000 abstract description 3
- 229920000049 Carbon (fiber) Polymers 0.000 abstract description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 abstract description 2
- 239000004917 carbon fiber Substances 0.000 abstract description 2
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 abstract description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 abstract description 2
- 239000007800 oxidant agent Substances 0.000 abstract description 2
- 230000001590 oxidative effect Effects 0.000 abstract description 2
- 229910052725 zinc Inorganic materials 0.000 abstract description 2
- FDDDEECHVMSUSB-UHFFFAOYSA-N sulfanilamide Chemical compound NC1=CC=C(S(N)(=O)=O)C=C1 FDDDEECHVMSUSB-UHFFFAOYSA-N 0.000 description 10
- 229940124530 sulfonamide Drugs 0.000 description 10
- VAZSKTXWXKYQJF-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)OOS([O-])=O VAZSKTXWXKYQJF-UHFFFAOYSA-N 0.000 description 8
- FYDKNKUEBJQCCN-UHFFFAOYSA-N lanthanum(3+);trinitrate Chemical compound [La+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O FYDKNKUEBJQCCN-UHFFFAOYSA-N 0.000 description 8
- 239000000499 gel Substances 0.000 description 7
- MYSWGUAQZAJSOK-UHFFFAOYSA-N ciprofloxacin Chemical compound C12=CC(N3CCNCC3)=C(F)C=C2C(=O)C(C(=O)O)=CN1C1CC1 MYSWGUAQZAJSOK-UHFFFAOYSA-N 0.000 description 6
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 5
- 239000000908 ammonium hydroxide Substances 0.000 description 5
- 230000015556 catabolic process Effects 0.000 description 5
- 238000006731 degradation reaction Methods 0.000 description 5
- 230000015572 biosynthetic process Effects 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 4
- 238000003760 magnetic stirring Methods 0.000 description 4
- 239000002699 waste material Substances 0.000 description 4
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical compound [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 description 4
- 238000002835 absorbance Methods 0.000 description 3
- 229960003405 ciprofloxacin Drugs 0.000 description 3
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 3
- 238000006555 catalytic reaction Methods 0.000 description 2
- 229920002678 cellulose Polymers 0.000 description 2
- 239000001913 cellulose Substances 0.000 description 2
- GVPFVAHMJGGAJG-UHFFFAOYSA-L cobalt dichloride Chemical compound [Cl-].[Cl-].[Co+2] GVPFVAHMJGGAJG-UHFFFAOYSA-L 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 239000008236 heating water Substances 0.000 description 2
- 239000010903 husk Substances 0.000 description 2
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 description 2
- 229940099596 manganese sulfate Drugs 0.000 description 2
- 239000011702 manganese sulphate Substances 0.000 description 2
- 235000007079 manganese sulphate Nutrition 0.000 description 2
- SQQMAOCOWKFBNP-UHFFFAOYSA-L manganese(II) sulfate Chemical compound [Mn+2].[O-]S([O-])(=O)=O SQQMAOCOWKFBNP-UHFFFAOYSA-L 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000005070 sampling Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 235000013162 Cocos nucifera Nutrition 0.000 description 1
- 244000060011 Cocos nucifera Species 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000003115 biocidal effect Effects 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 239000002322 conducting polymer Substances 0.000 description 1
- 229920001940 conductive polymer Polymers 0.000 description 1
- GUJOJGAPFQRJSV-UHFFFAOYSA-N dialuminum;dioxosilane;oxygen(2-);hydrate Chemical compound O.[O-2].[O-2].[O-2].[Al+3].[Al+3].O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O GUJOJGAPFQRJSV-UHFFFAOYSA-N 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- MVFCKEFYUDZOCX-UHFFFAOYSA-N iron(2+);dinitrate Chemical compound [Fe+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MVFCKEFYUDZOCX-UHFFFAOYSA-N 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 229910052901 montmorillonite Inorganic materials 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 229920005615 natural polymer Polymers 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 238000000870 ultraviolet spectroscopy Methods 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
- B01J31/28—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24 of the platinum group metals, iron group metals or copper
-
- 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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/002—Mixed oxides other than spinels, e.g. perovskite
-
- 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
-
- 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
- B01J31/32—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24 of manganese, technetium or rhenium
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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
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/34—Organic compounds containing oxygen
-
- 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
- C02F2101/36—Organic compounds containing halogen
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- 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
- C02F2101/38—Organic compounds containing nitrogen
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- 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
- C02F2101/40—Organic compounds containing sulfur
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
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Abstract
The invention discloses a kind of cotton fiber base carbon composite metal oxide/polypyrrole photochemical catalyst and preparation methods, the pretreatment including discarding cotton fiber, the process of the calcining of supported mixed metal salt and compound polypyrrole.Discarded flocking first use the solution of sodium hypochlorite and sodium hydroxide pre-process, then use hydro-thermal method loading metal-salt, metal salt include rare-earth elements of lanthanum respectively with iron, cobalt, manganese, zinc mixture.Cotton fiber after loading metal-salt is calcined to obtain metal salt carbon fiber, then using ammonium persulfate as the compound polypyrrole of oxidant under the conditions of ice-water bath.Obtained cotton fiber base carbon composite metal oxide/polypyrrole photochemical catalyst has good photodissociation ability to antibiotic solution.
Description
Technical field
The present invention relates to environmental catalysis and technical field of nano material, more particularly to a kind of cotton fiber base carbon composite metal
Oxide/polypyrrole photochemical catalyst and preparation method.
Background technique
Active carbon is a kind of porous carbon material with highly developed pore structure and very big specific surface area.The overwhelming majority contains
Carbonizable substance can prepare active carbon, currently, the Jian of low cost, the activated carbon raw material that source is wide, performance is high is sent out gradually by people
Concern.It is the research day that raw material prepares active carbon with agriculture waste material such as corncob, palm shell, rice husk, Zhu Lian, coconut husk etc.
Become extensive.The main component of cotton fabric is cellulose, and content of cellulose accounts for about 90%-94%, is the highest natural polymer of phosphorus content
Sub- compound, discarded cotton fabric is less as the report of activated carbon raw material.
Electric polypyrrole (ppy) is the intrinsically conducting polymer containing long-range conjugated structure, and conducting carriers are main
For polaron and bipolaron.With good electrochemistry and chemistry redox stability.Research shows that ppy and montmorillonite,
Its electric conductivity can be significantly improved after carbon nanotube is compound.But polypyrrole is used for the photocatalytic degradation of environmental contaminants simultaneously
It is rare.
Summary of the invention
The present invention provides a kind of cotton fiber base carbon composite metal oxide/polypyrrole photochemical catalyst and preparation method, including
The process of the pretreatment of discarded cotton fiber, the calcining of supported mixed metal salt and compound polypyrrole.Discarded flocking first uses sodium hypochlorite
Pre-processed with the solution of sodium hydroxide, then use hydro-thermal method loading metal-salt, metal salt include rare-earth elements of lanthanum respectively with iron,
Cobalt, manganese, zinc mixture.Cotton fiber after loading metal-salt is calcined to obtain metal salt carbon fiber, then under the conditions of ice-water bath with
Ammonium persulfate is the compound polypyrrole of oxidant.Obtained cotton fiber base carbon composite metal oxide/polypyrrole photochemical catalyst confrontation
Raw element solution has good photodissociation ability.
A kind of cotton fiber base carbon composite metal oxide/polypyrrole photochemical catalyst of the invention and preparation method technical solution
For a kind of cotton fiber base carbon composite metal oxide/polypyrrole photochemical catalyst is born using the fiber carrier of discarded cotton fiber preparation
After carrying metal salt, compound polypyrrole obtains cotton fiber base carbon composite metal oxide/polypyrrole photochemical catalyst, and cotton fiber base carbon is multiple
Closing metal oxide/polypyrrole photochemical catalyst has good photodissociation ability to antibiotic solution.
Cotton fiber base carbon composite metal oxide/polypyrrole photochemical catalyst preparation method, comprising the following steps:
(1) preparation of fiber carrier: after the washing solution that fibrous raw material sodium hypochlorite and sodium hydroxide form is impregnated 2-3h
Mixture boiled in 70-80 DEG C 30-40 minutes, washed after removing surface and oil contaminant and foul with clear water, 50-60 DEG C of low temperature dries
To fiber carrier；
(2) cotton fiber base carbon original position loading metal-salt oxide: fiber carrier is immersed in metal salts object solution and is stirred
After 3-4h, 1-12h is reacted at 180-200 DEG C, takes out filtration washing, 50-60 DEG C of constant temperature drying, 350-650 DEG C of calcining 0.5-
Cotton fiber base carbon original position loading metal-salt oxide is obtained after 1h；
(3) ammonia cotton fiber base carbon composite metal oxide/polypyrrole: is added in cotton fiber base carbon original position loading metal-salt oxide
In aqueous solution, ice-water bath stirring a period of time after pyrroles is added, ammonium persulfate ammonia spirit is added, ice-water bath stirs for 24 hours；It will produce
Object is cleaned with distilled water, and cotton fiber base carbon composite metal oxide/polypyrrole of black is obtained after 60 DEG C of dryings.
In step (1), the fibrous raw material is to be crushed using discarded fabric and obtained the clast of similar cotton-wool.
In step (1), the solid-to-liquid ratio of cotton clast and washing solution is 10g/L-20g/L, washs sodium hypochlorite in solution
Concentration is 2%-5% (v/v), and the concentration of sodium hydroxide is 2%-3% (M/M).
In step (2), the metal salts object solution is the metal salt and another metal using rare-earth elements of lanthanum
The liquid-solid ratio of the mixture solution of salt, fiber carrier and metal salts object solution is 10-20g/L.
In step (2), citric acid monohydrate is added simultaneously in metal salts object solution, and the amount of substance is lanthanum salt and another
Then the sum of the amount of metal salt substance is added ammonia spirit and adjusts pH value；Another metal salt is iron, cobalt, manganese or zinc salt.
In step (3), the ammonia spirit concentration is 0.1mol/L, and adjusting pH range is 0.789-7.613.
In step (3), the concentration after pyrroles's addition ammonia spirit is 0.06-0.07 (V/V), ammonium persulfate ammonia spirit
Concentration is 133-152g/L.
In step (3), cotton fiber base carbon original position loading metal-salt oxide and ammonia spirit, pyrroles and ammonium persulfate ammonium hydroxide
The solid-to-liquid ratio of the mixed solution of solution composition is 5-20g/L.
The evaluation method of photocatalysis performance:
Entire light-catalyzed reaction carries out in photo catalysis reactor, using mercury lamp as light source, respectively by the antibiotic of 50mL 10mg/L
It is added in photocatalysis test tube, 0.01g cotton fiber base carbon composite metal oxide/polypyrrole photochemical catalyst is added, preceding 30min is dark
Under the conditions of adsorbed, then open carry out photocatalytic degradation.It is surveyed every sampling in 5 minutes using ultraviolet-uisible spectrophotometer
Measure absorbance.Record concentration changes with time relationship.
The invention has the benefit that using discarded fabric be carrier as the fibrous template of metal oxide, it is at low cost, just
Method is simple；Hydro-thermal method can oxidize metal object uniform " growth " on cotton fiber surface；The compound gold of cotton fiber base carbon of the invention
Belonging to oxide/polypyrrole photochemical catalyst has good photodissociation ability to antibiotic solution.
Fig. 1 is the compound lanthanum ferroelectric metal oxide of cotton fiber base carbon of the present invention/polypyrrole photochemical catalyst (LaFe/ppy-CC)
SEM picture, it is seen then that the surface LaFeCC is covered with polypyrrole spheric granules.Fig. 2 show cotton fiber base carbon composite metal oxygen of the present invention
Compound/polypyrrole photochemical catalyst (LaFe/ppy-CC, LaCo/ppy-CC, LaMn/ppy-CC and LaZn/ppy-CC) is to sulfanilamide (SN)
Light degradation curve, it is seen then that four kinds of composite photo-catalysts can good light degradation sulfanilamide (SN) solution, the photodissociation of LaZn/ppy-CC
Ability is slightly below other three kinds.
Detailed description of the invention:
Fig. 1 show the SEM picture of the compound lanthanum ferroelectric metal oxide/polypyrrole photochemical catalyst of cotton fiber base carbon；
Fig. 2 show cotton fiber base carbon composite metal oxide/polypyrrole photochemical catalyst to the light degradation curve of sulfanilamide (SN)；
Fig. 3 show cotton fiber base carbon composite metal oxide/polypyrrole photochemical catalyst to the light degradation curve of Ciprofloxacin.
Specific embodiment:
For a better understanding of the present invention, below with specific example come the technical solution that the present invention will be described in detail, but it is of the invention
It is not limited thereto.
Embodiment 1
By 2g fibrous raw material (fibrous raw material is to be crushed using discarded fabric and obtained the clast of similar cotton-wool) concentration point
Not Wei 2% sodium hypochlorite and 2% sodium hydroxide mixed aqueous solution 100mL after 80 DEG C of heating water baths handle 0.5h, clear water drift
It washes, fiber carrier is made in 50 DEG C of low temperature dryings for 24 hours.
Lanthanum nitrate and iron nitrate solution is respectively configured, makes the molar ratio 1:1 of lanthanum element and ferro element, two kinds of solution are mixed
It closes, takes the mixed solution of 50ml lanthanum nitrate and ferric nitrate, the citric acid monohydrate that 2mmol/L is added is placed on magnetic stirring apparatus
Stirring, it is 3.0 that ammonium hydroxide, which is added dropwise, and adjusts the pH value of mixed liquor, prepares brown yellow gel.0.8g fiber carrier is taken to be added above-mentioned
3-4h, 180-200 DEG C of reaction 6h are stirred in gel.Then it after by fiber carrier as 60 degree of low temperature dryings in drying box, will dry
Dry fiber carrier is placed in Muffle furnace, and 350 DEG C of calcining 30min obtain LaFeCC (LaFe cotton carbon).
It takes 1g LaFeCC to be added in 30mL 0.1mol/L ammonia spirit, continuously adds 1.5mL pyrroles, stirred in ice-water bath
Mix 30min.It weighs 4.564g ammonium persulfate and is added to formation APS solution in the ammonia spirit of 30mL0.01mol/L, APS is molten
Liquid stirs 30min in ice-water bath.Then APS solution is added in above-mentioned solution, ice-water bath stirs for 24 hours.Product is steamed
Distilled water is cleaned, and is put into baking oven and is dried to obtain LaFe/ppy-CC (LaFe/ppy cotton carbon) for 60 DEG C.
Embodiment 2
It with concentration is respectively 2% sodium hypochlorite and 2% sodium hydroxide mixed aqueous solution 100mL in 80 DEG C by 2g waste cotton clast
After heating water bath handles 0.5h, fiber carrier is made in clear water rinsing, 50 DEG C of low temperature dryings for 24 hours.
Lanthanum nitrate and cobalt chloride solution is respectively configured, makes the molar ratio 1:1 of lanthanum element and cobalt element, two kinds of solution are mixed
It closes, takes 50ml lanthanum nitrate and cobalt chloride mixed solution, the citric acid monohydrate that 2mmol/L is added, which is placed on magnetic stirring apparatus, to be stirred
It mixes, it is 3.0 that ammonium hydroxide, which is added dropwise, and adjusts the pH value of mixed liquor, prepares brownish black gel.0.8g fiber carrier is taken to be added above-mentioned solidifying
3-4h, 180-200 DEG C of reaction 6h are stirred in glue.Then it after by fiber carrier as 60 degree of low temperature dryings in drying box, will dry
Fiber carrier be placed in Muffle furnace, 350 DEG C of calcining 30min obtain LaCoCC (LaCo cotton carbon).
It takes 1g LaCoCC to be added in 30mL 0.1mol/L ammonia spirit, continuously adds 1.5mL pyrroles, stirred in ice-water bath
Mix 30min.It weighs 4.564g ammonium persulfate and is added to formation APS solution in the ammonia spirit of 30mL 0.01mol/L, APS is molten
Liquid stirs 30min in ice-water bath.Then APS solution is added in above-mentioned solution, ice-water bath stirs for 24 hours.Product is steamed
Distilled water is cleaned, and is put into baking oven and is dried to obtain LaCo/ppy-CC (LaCo/ppy cotton carbon) for 60 DEG C
Embodiment 3
The sodium hypochlorite and sodium hydroxide mixed aqueous solution 100mL for being respectively 2% with concentration for 2g waste cotton clast are in 80oC water-bath
After heating 0.5h, fiber carrier is made in clear water rinsing, 50 DEG C of low temperature dryings for 24 hours.
Lanthanum nitrate and manganese sulfate solution is respectively configured, makes the molar ratio 1:1 of lanthanum element and manganese element, two kinds of solution are mixed
It closes, takes the mixed solution of 50ml lanthanum nitrate and manganese sulfate, the citric acid monohydrate that 2mmol/L is added is placed on magnetic stirring apparatus
Stirring, it is 3.0 that ammonium hydroxide, which is added dropwise, and adjusts the pH value of mixed liquor, prepares brown-green gel.0.8g fiber carrier is taken to be added above-mentioned
3-4h, 180-200 DEG C of reaction 6h are stirred in gel.Then it after by fiber carrier as 60 degree of low temperature dryings in drying box, will dry
Dry fiber carrier is placed in Muffle furnace, and 350 DEG C of calcining 30min obtain LaMnCC (LaMn cotton carbon).
It takes 1g LaMnCC to be added in 30mL 0.1mol/L ammonia spirit, continuously adds 1.5mL pyrroles, stirred in ice-water bath
Mix 30min.It weighs 4.564g ammonium persulfate and is added to formation APS solution in the ammonia spirit of 30mL0.01mol/L, APS is molten
Liquid stirs 30min in ice-water bath.Then APS solution is added in above-mentioned solution, ice-water bath stirs for 24 hours.Product is steamed
Distilled water is cleaned, and is put into baking oven and is dried to obtain LaMn/ppy-CC (LaMn/ppy cotton carbon) for 60 DEG C
Embodiment 4
The sodium hypochlorite and sodium hydroxide mixed aqueous solution 100mL for being respectively 2% with concentration for 2g waste cotton clast are in 80oC water-bath
After heating 0.5h, fiber carrier is made in clear water rinsing, 50 DEG C of low temperature dryings for 24 hours.
Lanthanum nitrate and zinc nitrate solution is respectively configured, makes the molar ratio 1:1 of lanthanum element and Zn-ef ficiency, two kinds of solution are mixed
Close, take 50ml lanthanum nitrate and zinc nitrate mixed solution, the citric acid monohydrate that 2mmol/L is added is placed on magnetic stirring apparatus
Upper stirring, it is 3.0 that ammonium hydroxide, which is added dropwise, and adjusts the pH value of mixed liquor, prepares white gels.0.8g fiber carrier is taken to be added above-mentioned
Gel stirs 3-4h, 180-200 DEG C of reaction 6h.Then it after by fiber carrier as 60 degree of low temperature dryings in drying box, will dry
Fiber carrier be placed in Muffle furnace, 350 DEG C of calcining 30min obtain LaZnCC (LaZn cotton carbon).
It takes 1g LaZnCC to be added in 30mL 0.1mol/L ammonia spirit, continuously adds 1.5mL pyrroles, stirred in ice-water bath
Mix 30min.It weighs 4.564g ammonium persulfate and is added to formation APS solution in the ammonia spirit of 30mL0.01mol/L, APS is molten
Liquid stirs 30min in ice-water bath.Then APS solution is added in above-mentioned solution, ice-water bath stirs for 24 hours.Product is steamed
Distilled water is cleaned, and is put into baking oven and is dried to obtain LaZn/ppy-CC (LaZn/ppy cotton carbon) for 60 DEG C.
Product (abbreviation La-Fe, La-Co, La-Mn and La-Zn) prepared by embodiment 1-4 carries out photocatalysis performance
Evaluation, specific experiment are as follows:
The sulfanilamide (SN) of 50mL 10mg/L, Ciprofloxacin are added in photocatalysis test tube respectively, are separately added into 0.01g LaFe/ppy-
CC, LaCo/ppy-CC, LaMn/ppy-CC and LaZn/ppy-CC sample are adsorbed under preceding 30min dark condition, are then beaten
Open the light source progress photocatalytic degradation.Measurement of ultraviolet-visible spectrophotometer absorbance is utilized every sampling in 5 minutes.Record absorbance
Change with time relationship, respectively as shown in Fig. 2 Fig. 3.As it can be seen that various cotton fiber base carbon composite metal oxide/polypyrrole light
Catalyst has faster degradation rate to sulfanilamide (SN) and Ciprofloxacin.
Claims (9)
1. a kind of cotton fiber base carbon composite metal oxide/polypyrrole photochemical catalyst, which is characterized in that using discarded cotton fiber system
After standby fiber carrier loading metal-salt, compound polypyrrole obtains cotton fiber base carbon composite metal oxide/polypyrrole photocatalysis
Agent, cotton fiber base carbon composite metal oxide/polypyrrole photochemical catalyst have good photodissociation ability to antibiotic solution.
2. the preparation method of cotton fiber base carbon composite metal oxide/polypyrrole photochemical catalyst as described in claim 1, special
Sign is, comprising the following steps:
(1) preparation of fiber carrier: after the washing solution that fibrous raw material sodium hypochlorite and sodium hydroxide form is impregnated 2-3h
Mixture boiled in 70-80 DEG C 30-40 minutes, washed after removing surface and oil contaminant and foul with clear water, 50-60 DEG C of low temperature dries
To fiber carrier；
(2) cotton fiber base carbon original position loading metal-salt oxide: fiber carrier is immersed in metal salts object solution and is stirred
After 3-4h, 1-12h is reacted at 180-200 DEG C, takes out filtration washing, 50-60 DEG C of constant temperature drying, 350-650 DEG C of calcining 0.5-
Cotton fiber base carbon original position loading metal-salt oxide is obtained after 1h；
(3) ammonia cotton fiber base carbon composite metal oxide/polypyrrole: is added in cotton fiber base carbon original position loading metal-salt oxide
In aqueous solution, ice-water bath stirring a period of time after pyrroles is added, ammonium persulfate ammonia spirit is added, ice-water bath stirs for 24 hours；It will produce
Object is cleaned with distilled water, and cotton fiber base carbon composite metal oxide/polypyrrole of black is obtained after 60 DEG C of dryings.
3. the preparation method of cotton fiber base carbon composite metal oxide/polypyrrole photochemical catalyst according to claim 2,
It is characterized in that, in step (1), the fibrous raw material is to be crushed using discarded fabric and obtained the clast of similar cotton-wool.
4. the preparation method of cotton fiber base carbon composite metal oxide/polypyrrole photochemical catalyst according to claim 2,
It is characterized in that, in step (1), the solid-to-liquid ratio of cotton clast and washing solution is 10g/L-20g/L, washs sodium hypochlorite in solution
Concentration is 2%-5% (v/v), and the concentration of sodium hydroxide is 2%-3% (M/M).
5. the preparation method of cotton fiber base carbon composite metal oxide/polypyrrole photochemical catalyst according to claim 2,
It is characterized in that, in step (2), the metal salts object solution is the metal salt and another metal using rare-earth elements of lanthanum
The liquid-solid ratio of the mixture solution of salt, fiber carrier and metal salts object solution is 10-20g/L.
6. the preparation method of cotton fiber base carbon composite metal oxide/polypyrrole photochemical catalyst according to claim 2,
It is characterized in that, in step (2), is added citric acid monohydrate simultaneously in metal salts object solution, the amount of substance is lanthanum salt and another
Then the sum of the amount of one metal salt substance is added ammonia spirit and adjusts pH value；Another metal salt is iron, cobalt, manganese or zinc
Salt.
7. the preparation method of cotton fiber base carbon composite metal oxide/polypyrrole photochemical catalyst according to claim 6,
It is characterized in that, the ammonia spirit concentration is 0.1mol/L, and adjusting pH range is 0.789-7.613.
8. the preparation method of cotton fiber base carbon composite metal oxide/polypyrrole photochemical catalyst according to claim 2,
It is characterized in that, in step (3), the concentration after pyrroles's addition ammonia spirit is 0.06-0.07 (V/V), ammonium persulfate ammonia spirit
Concentration be 133-152g/L.
9. the preparation method of cotton fiber base carbon composite metal oxide/polypyrrole photochemical catalyst according to claim 2,
It is characterized in that, in step (3), cotton fiber base carbon original position loading metal-salt oxide and ammonia spirit, pyrroles and ammonium persulfate ammonia
The solid-to-liquid ratio of the mixed solution of aqueous solution composition is 5-20g/L.
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| CN113457647A (en) * | 2021-07-29 | 2021-10-01 | 东南大学 | Cobalt-modified carbon-based fiber membrane and preparation method thereof |
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