CN106630023A - Modified carbon fiber electrode with function of removing carbazole through electrocatalysis and preparation method thereof - Google Patents

Modified carbon fiber electrode with function of removing carbazole through electrocatalysis and preparation method thereof Download PDF

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CN106630023A
CN106630023A CN201611055946.3A CN201611055946A CN106630023A CN 106630023 A CN106630023 A CN 106630023A CN 201611055946 A CN201611055946 A CN 201611055946A CN 106630023 A CN106630023 A CN 106630023A
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不公告发明人
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Beijing Qingyuan Environmental Protection Technology Co Ltd
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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
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
    • C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
    • C02F1/46104—Devices therefor; Their operating or servicing
    • C02F1/46109—Electrodes
    • C02F1/46114—Electrodes in particulate form or with conductive and/or non conductive particles between them
    • 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
    • C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
    • C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
    • C02F1/467—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis by electrochemical disinfection; by electrooxydation or by electroreduction
    • C02F1/4672—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis by electrochemical disinfection; by electrooxydation or by electroreduction by electrooxydation
    • 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
    • C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
    • C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
    • C02F1/46104—Devices therefor; Their operating or servicing
    • C02F1/46109—Electrodes
    • C02F2001/46133—Electrodes characterised by the material
    • 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
    • C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
    • C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
    • C02F1/46104—Devices therefor; Their operating or servicing
    • C02F1/46109—Electrodes
    • C02F2001/46133—Electrodes characterised by the material
    • C02F2001/46138—Electrodes comprising a substrate and a coating
    • C02F2001/46142—Catalytic coating
    • 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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  • Chemical Kinetics & Catalysis (AREA)
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  • General Chemical & Material Sciences (AREA)
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  • Hydrology & Water Resources (AREA)
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  • Environmental & Geological Engineering (AREA)
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Abstract

The invention discloses a modified carbon fiber electrode with a function of removing carbazole through electrocatalysis and a preparation method thereof. Carbon fiber, trichloromethane and ethyl alcohol are prepared into a substance A; the substance A is prepared into a substance E through modifying a mixed solution prepared from silver nitrate, platinum nitrate, diethyl ether and Sb(NO3)3; the substance E is prepared into a substance H through modifying a mixed solution prepared from Pb(NO3)2, ethyl alcohol, AlCl3, PtCl4, CdCl2 and PdCl2; the substance H is prepared into a substance K through modifying a mixed solution prepared from lauryl sodium sulfate, n-hexane, n-butyl alcohol, ammonium metavanadate, sodium citrate, CdCl2 and PdCl2; the substance K is prepared into a substance through modifying a mixed solution prepared from polyvinyl alcohol and HAuCl4; the obtained substance is the modified carbon fiber electrode with a function of removing carbazole through electrocatalysis.

Description

The modified carbon fiber granule electrode and preparation method of carbazole function are removed with electro-catalysis
Technical field
The invention belongs to organic wastewater with difficult degradation thereby Electrocatalytic Oxidation processing technology field, more particularly to one kind are urged with electricity Change the modified carbon fiber granule electrode and preparation method for removing carbazole function.
Background technology
Electro-catalytic oxidation technology is a kind of very promising water technology for gradually growing up in recent years, mainly Oxidative degradation is carried out to the organic pollution in waste water by producing the active groups with strong oxidizing property such as hydroxyl radical free radical, can So that hardly degraded organic substance or bio-toxicity pollutant be converted into into biodegradable or innocuous substance, that improves waste water can be biochemical Property, so as to be beneficial to follow-up biological treatment.Therefore, electrocatalytic oxidation water technology is processing high concentration, bio-refractory work The features such as industry waste water aspect has non-secondary pollution, low cost, strong applicability, efficiency high.Electrode material is electrocatalytic oxidation skill The core component of art, its performance has decisive influence for the treatment effeciency and operating cost of electro-catalytic oxidation technology, because This electrocatalysis material for exploring and preparing good combination property is the research emphasis of current electro-catalytic oxidation technology.But traditional electrode The resistance of material is larger, conductance is low so that its in the treatment of waste water current efficiency is low, stability not enough, short life, electrode material Material is relatively costly, limits popularization and application of the electro-catalytic oxidation technology in water process and development, so new electrode materials Research also needs to further reinforcement with preparation.Also lack at present and there is efficient electric catalytic elimination function to carbazole specific pollutants Electrode material and preparation method.
The content of the invention
It is an object of the invention to provide a kind of modified carbon fiber granule electrode and system that carbazole function is removed with electro-catalysis Preparation Method, its preparation method is comprised the following steps that：
(1) 500mL beakers are put into after are washed with 1000mL deionized waters the 133g carbon fiber particles that particle diameter is 4～6mm In, 300mL molar concentrations are added for the hydrochloric acid solution of 0.1mol/L and soak 0.5h, liquid is removed after filtration and obtains substance A 01, Substance A 01 is added to into the AgNO that 250mL molar concentrations are 1.84mol/L3In solution, shake in the shaking table that temperature is 65 DEG C 15 minutes, it is cooled to after room temperature and is filtered to remove liquid and obtains substance A 02, the Jing 900mL mass percent concentrations of substance A 02 is 95% Ethanol washing after place 1.5h in 85 DEG C of drying box, be subsequently placed in Muffle furnace the roasting 1h under the conditions of 480 DEG C, obtain Substance A 1；
(2) it is in 1000mL conical flasks, in 1000r/ 8.99 grams of platinum nitrates and 800mL deionized waters to be added to into volume Stir 3 minutes under the conditions of min, add 15mL red fuming nitric acid (RFNA)s, 4 parts of equivalent is divided into after shaking up, obtain mixed liquor K1, mixed liquor K2, mix Close liquid K3, mixed liquor K4；
(3) by 627 milligrams of Sb (NO3)3With the AgNO that 30mL molar concentrations are 0.44mol/L3Solution is added to mixed liquor K1 In, stir 3 minutes under the conditions of 1000r/min, obtain mixed liquor L1；
(4) substance A 1 is added in mixed liquor L1, is shaken 15 minutes in the shaking table that temperature is 45 DEG C, be cooled to room temperature After be filtered to remove liquid and obtain substance A 2, substance A 2 is Jing after the ethanol washing that 100mL mass percent concentrations are 95% at 85 DEG C Drying box in place 1.5h, be subsequently placed in Muffle furnace the roasting 1h under the conditions of 480 DEG C, obtain substance A 3；
(5) by 647 milligrams of Sb (NO3)3With the AgNO that 50mL molar concentrations are 0.54mol/L3Solution is added to mixed liquor K2 In, stir 3 minutes under the conditions of 1000r/min, obtain mixed liquor L2；
(6) substance A 3 is added in mixed liquor L2, is shaken 15 minutes in the shaking table that temperature is 45 DEG C, be cooled to room temperature After be filtered to remove liquid and obtain substance A 4, substance A 4 is Jing after the ethanol washing that 100mL mass percent concentrations are 95% at 85 DEG C Drying box in place 1.5h, be subsequently placed in Muffle furnace the roasting 1h under the conditions of 480 DEG C, obtain substance A 5；
(7) by 667 milligrams of Sb (NO3)3With the AgNO that 70mL molar concentrations are 0.64mol/L3Solution is added to mixed liquor K3 In, stir 3 minutes under the conditions of 1000r/min, obtain mixed liquor L3；
(8) substance A 5 is added in mixed liquor L3, is shaken 15 minutes in the shaking table that temperature is 45 DEG C, be cooled to room temperature After be filtered to remove liquid and obtain substance A 6, substance A 6 is Jing after the ethanol washing that 100mL mass percent concentrations are 95% at 85 DEG C Drying box in place 1.5h, be subsequently placed in Muffle furnace the roasting 1h under the conditions of 480 DEG C, obtain substance A 7；
(9) by 687 milligrams of Sb (NO3)3With the AgNO that 90mL molar concentrations are 0.74mol/L3Solution is added to mixed liquor K4 In, stir 3 minutes under the conditions of 1000r/min, obtain mixed liquor L4；
(10) substance A 7 is added in mixed liquor L4, is shaken 15 minutes in the shaking table that temperature is 45 DEG C, be cooled to room Liquid is filtered to remove after temperature and obtains substance A 8, substance A 8 is Jing after the ethanol washing that 100mL mass percent concentrations are 95% 85 DEG C drying box in place 1.5h, be subsequently placed in Muffle furnace the roasting 1h under the conditions of 480 DEG C, obtain substance A；
(11) by 6.59 grams of AgNO3It is in 1000mL conical flasks, in 1000r/min bars to be added to volume with 750mL ether Stir 3 minutes under part, 3 parts of equivalent is divided into after shaking up, obtain mixed liquor M1, mixed liquor M2, mixed liquor M3；
(12) by 329 milligrams of AgNO3With the Sb (NO that 30mL molar concentrations are 0.48mol/L3)3Solution is added to mixed liquor In M1, stir 3 minutes under the conditions of 1000r/min, obtain mixed liquor N1；
(13) substance A is added in mixed liquor N1, is shaken 15 minutes in the shaking table that temperature is 45 DEG C, be cooled to room temperature After be filtered to remove liquid and obtain substance B, substance B is Jing after the ethanol washing that 100mL mass percent concentrations are 95% at 85 DEG C 1.5h is placed in drying box, the roasting 1h under the conditions of 480 DEG C is subsequently placed in Muffle furnace, substance B 1 is obtained；
(14) by 359 milligrams of AgNO3With the Sb (NO that 60mL molar concentrations are 0.68mol/L3)3Solution is added to mixed liquor In M2, stir 3 minutes under the conditions of 1000r/min, obtain mixed liquor N2；
(15) substance B 1 is added in mixed liquor N2, is shaken 15 minutes in the shaking table that temperature is 45 DEG C, be cooled to room Liquid is filtered to remove after temperature and obtains substance B 2, substance B 2 is Jing after the ethanol washing that 100mL mass percent concentrations are 95% 85 DEG C drying box in place 1.5h, be subsequently placed in Muffle furnace the roasting 1h under the conditions of 480 DEG C, obtain substance C；
(16) by 389 milligrams of AgNO3With the Sb (NO that 90mL molar concentrations are 0.88mol/L3)3Solution is added to mixed liquor In M3, stir 3 minutes under the conditions of 1000r/min, obtain mixed liquor N3；
(17) substance C is added in mixed liquor N3, is shaken 15 minutes in the shaking table that temperature is 45 DEG C, be cooled to room temperature After be filtered to remove liquid and obtain material D, material D is Jing after the ethanol washing that 100mL mass percent concentrations are 95% at 85 DEG C 1.5h is placed in drying box, the roasting 1h under the conditions of 480 DEG C is subsequently placed in Muffle furnace, material E is obtained；
(18) by 7.58 grams of Pb (NO3)2It is in 1000mL conical flasks, in 1000r/min to be added to volume with 900mL ethanol Under the conditions of stir 3 minutes, add 5mL red fuming nitric acid (RFNA)s, 3 parts of equivalent is divided into after shaking up, obtain mixed liquor P1, mixed liquor P2, mixed liquor P3；
(19) by 85mL molar concentrations for 0.99mol/L AlCl3Solution is added in mixed liquor P1, in 1000r/min Under the conditions of stir 3 minutes, obtain mixed liquor Q1；
(20) material E is added in mixed liquor Q1, is shaken 15 minutes in the shaking table that temperature is 45 DEG C, be cooled to room temperature After be filtered to remove liquid and obtain material F1, material F1 is Jing after the ethanol washing that 100mL mass percent concentrations are 95% at 85 DEG C Drying box in place 1.5h, be subsequently placed in Muffle furnace the roasting 1h under the conditions of 480 DEG C, obtain material F2；
(21) by 75mL molar concentrations for 0.69mol/L Pb (NO3)2Solution is added in mixed liquor P2, in 1000r/ Stir 3 minutes under the conditions of min, obtain mixed liquor Q2；
(22) material F2 is added in mixed liquor Q2, is shaken 15 minutes in the shaking table that temperature is 45 DEG C, be cooled to room Liquid is filtered to remove after temperature and obtains material F3, material F3 is Jing after the ethanol washing that 100mL mass percent concentrations are 95% 85 DEG C drying box in place 1.5h, be subsequently placed in Muffle furnace the roasting 1h under the conditions of 480 DEG C, obtain material F4；
(23) by 55mL molar concentrations for 0.59mol/L AlCl3Solution is added in mixed liquor P3, in 1000r/min Under the conditions of stir 3 minutes, obtain mixed liquor Q3；
(24) material F4 is added in mixed liquor Q3, is shaken 15 minutes in the shaking table that temperature is 45 DEG C, be cooled to room Liquid is filtered to remove after temperature and obtains material F5, material F5 is Jing after the ethanol washing that 100mL mass percent concentrations are 95% 85 DEG C drying box in place 1.5h, be subsequently placed in Muffle furnace the roasting 1h under the conditions of 480 DEG C, obtain material F；
(25) by 6.58g PtCl4Volume is added to the sodium citrate solution that 750mL mass percent concentrations are 10% In for 1000mL conical flasks, stir 3 minutes under the conditions of 1000r/min, 3 parts of equivalent is divided into after shaking up, obtain mixed liquor R1, mix Close liquid R2, mixed liquor R3；
(26) by 40mL molar concentrations for 0.38mol/L CdCl2Solution and 60mL molar concentrations are for 0.86mol/L's PdCl2Solution is added in mixed liquor R1, is stirred 3 minutes under the conditions of 1000r/min, obtains mixed liquor S1；
(27) material F is added in mixed liquor S1, is shaken 15 minutes in the shaking table that temperature is 45 DEG C, be cooled to room temperature After be filtered to remove liquid and obtain material G1, material G1 is Jing after the ethanol washing that 100mL mass percent concentrations are 95% at 85 DEG C Drying box in place 1.5h, be subsequently placed in Muffle furnace the roasting 1h under the conditions of 480 DEG C, obtain material H1；
(28) by 50mL molar concentrations for 0.58mol/L CdCl2Solution and 50mL molar concentrations are for 0.66mol/L's PdCl2Solution is added in mixed liquor R2, is stirred 3 minutes under the conditions of 1000r/min, obtains mixed liquor S2；
(29) material H1 is added in mixed liquor S2, is shaken 15 minutes in the shaking table that temperature is 45 DEG C, be cooled to room Liquid is filtered to remove after temperature and obtains material G2, material G2 is Jing after the ethanol washing that 100mL mass percent concentrations are 95% 85 DEG C drying box in place 1.5h, be subsequently placed in Muffle furnace the roasting 1h under the conditions of 480 DEG C, obtain material H2；
(30) by 60mL molar concentrations for 0.78mol/L CdCl2Solution and 40mL molar concentrations are for 0.46mol/L's PdCl2Solution is added in mixed liquor R3, is stirred 3 minutes under the conditions of 1000r/min, obtains mixed liquor S3；
(31) material H2 is added in mixed liquor S3, is shaken 15 minutes in the shaking table that temperature is 45 DEG C, be cooled to room Liquid is filtered to remove after temperature and obtains material G3, material G3 is Jing after the ethanol washing that 100mL mass percent concentrations are 95% 85 DEG C drying box in place 1.5h, be subsequently placed in Muffle furnace the roasting 1h under the conditions of 480 DEG C, obtain material H；
(32) 6.39g lauryl sodium sulfate, 40mL n-hexanes, 20 milliliters of n-butanols are added sequentially to volume and are In 250mL conical flasks, 11.28g ammonium metavanadates and 150mL deionized waters are added, be placed in 70 DEG C of water-baths in 1000r/min bars 1h is stirred under part, the hydrochloric acid solution that 25mL molar concentrations are 2.40mol/L is subsequently adding, is shaken in the shaking table that temperature is 45 DEG C 0.5h, is cooled to after room temperature under the conditions of 7500r/min and 15min is centrifuged, and removes supernatant, uses 500mL mass percent concentrations Ethanol for 95% is washed, and obtains material I；
(33) sodium citrate solution that material I and 800mL mass percent concentration is 15% is added to into volume is In 1000mL conical flasks, stir 3 minutes under the conditions of 1000r/min, 4 parts of equivalent is divided into after shaking up, obtain mixed liquor T1, mixing Liquid T2, mixed liquor T3, mixed liquor T4；
(34) by 35mL molar concentrations for 0.48mol/L CdCl2Solution and 65mL molar concentrations are for 0.99mol/L's PdCl2Solution is added in mixed liquor T1, is stirred 3 minutes under the conditions of 1000r/min, obtains mixed liquor U1；
(35) material H is added in mixed liquor U1, is shaken 15 minutes in the shaking table that temperature is 45 DEG C, be cooled to room temperature After be filtered to remove liquid and obtain material J1, material J1 is Jing after the ethanol washing that 100mL mass percent concentrations are 95% at 85 DEG C Drying box in place 1.5h, be subsequently placed in Muffle furnace the roasting 1h under the conditions of 480 DEG C, obtain material K1；
(36) by 45mL molar concentrations for 0.58mol/L CdCl2Solution and 55mL molar concentrations are for 0.79mol/L's PdCl2Solution is added in mixed liquor T2, is stirred 3 minutes under the conditions of 1000r/min, obtains mixed liquor U2；
(37) material K1 is added in mixed liquor U2, is shaken 15 minutes in the shaking table that temperature is 45 DEG C, be cooled to room Liquid is filtered to remove after temperature and obtains material J2, material J2 is Jing after the ethanol washing that 100mL mass percent concentrations are 95% 85 DEG C drying box in place 1.5h, be subsequently placed in Muffle furnace the roasting 1h under the conditions of 480 DEG C, obtain material K2；
(38) by 55mL molar concentrations for 0.68mol/L CdCl2Solution and 45mL molar concentrations are for 0.59mol/L's PdCl2Solution is added in mixed liquor T3, is stirred 3 minutes under the conditions of 1000r/min, obtains mixed liquor U3；
(39) material K2 is added in mixed liquor U3, is shaken 15 minutes in the shaking table that temperature is 45 DEG C, be cooled to room Liquid is filtered to remove after temperature and obtains material J3, material J3 is Jing after the ethanol washing that 100mL mass percent concentrations are 95% 85 DEG C drying box in place 1.5h, be subsequently placed in Muffle furnace the roasting 1h under the conditions of 480 DEG C, obtain material K3；
(40) by 65mL molar concentrations for 0.78mol/L CdCl2Solution and 35mL molar concentrations are for 0.39mol/L's PdCl2Solution is added in mixed liquor T4, is stirred 3 minutes under the conditions of 1000r/min, obtains mixed liquor U4；
(41) material K3 is added in mixed liquor U4, is shaken 15 minutes in the shaking table that temperature is 45 DEG C, be cooled to room Liquid is filtered to remove after temperature and obtains material J4, material J4 is Jing after the ethanol washing that 100mL mass percent concentrations are 95% 85 DEG C drying box in place 1.5h, be subsequently placed in Muffle furnace the roasting 1h under the conditions of 480 DEG C, obtain material K；
(42) 12.64g polyvinyl alcohol and 800mL deionized waters are added to into volume in 1000mL conical flasks, Stir 3 minutes under the conditions of 1000r/min, 4 parts of equivalent is divided into after shaking up, obtain mixed liquor V1, mixed liquor V2, mixed liquor V3, mixed Close liquid V4；
(43) by 95mL molar concentrations for 0.78mol/L HAuCl4Solution is added in mixed liquor V1, in 1000r/min Under the conditions of stir 3 minutes, obtain mixed liquor W1；
(44) material K is added in mixed liquor W1, is shaken 15 minutes in the shaking table that temperature is 45 DEG C, be cooled to room temperature After be filtered to remove liquid and obtain material L1, material L1 is Jing after the ethanol washing that 100mL mass percent concentrations are 95% at 85 DEG C Drying box in place 1.5h, be subsequently placed in Muffle furnace the roasting 1h under the conditions of 480 DEG C, obtain material Z1；
(45) by 75mL molar concentrations for 0.68mol/L HAuCl4Solution is added in mixed liquor V2, in 1000r/min Under the conditions of stir 3 minutes, obtain mixed liquor W2；
(46) material Z1 is added in mixed liquor W2, is shaken 15 minutes in the shaking table that temperature is 45 DEG C, be cooled to room Liquid is filtered to remove after temperature and obtains material L2, material L2 is Jing after the ethanol washing that 100mL mass percent concentrations are 95% 85 DEG C drying box in place 1.5h, be subsequently placed in Muffle furnace the roasting 1h under the conditions of 480 DEG C, obtain material Z2；
(47) by 55mL molar concentrations for 0.58mol/L HAuCl4Solution is added in mixed liquor V3, in 1000r/min Under the conditions of stir 3 minutes, obtain mixed liquor W3；
(48) material Z2 is added in mixed liquor W3, is shaken 15 minutes in the shaking table that temperature is 45 DEG C, be cooled to room Liquid is filtered to remove after temperature and obtains material L3, material L3 is Jing after the ethanol washing that 100mL mass percent concentrations are 95% 85 DEG C drying box in place 1.5h, be subsequently placed in Muffle furnace the roasting 1h under the conditions of 480 DEG C, obtain material Z3；
(49) by 35mL molar concentrations for 0.48mol/L HAuCl4Solution is added in mixed liquor V4, in 1000r/min Under the conditions of stir 3 minutes, obtain mixed liquor W4；
(50) material Z3 is added in mixed liquor W4, is shaken 15 minutes in the shaking table that temperature is 45 DEG C, be cooled to room Liquid is filtered to remove after temperature and obtains material L4, material L4 is Jing after the ethanol washing that 100mL mass percent concentrations are 95% 85 DEG C drying box in place 1.5h, be subsequently placed in Muffle furnace the roasting 1h under the conditions of 480 DEG C, the material for obtaining as has electricity The modified carbon fiber granule electrode of catalytic elimination carbazole function.
The invention has the beneficial effects as follows, the obtained modified carbon fiber granule electrode tool that carbazole function is removed with electro-catalysis Have that current efficiency is high, stability is strong, electrode life length, it is high to carbazole removal efficiency the features such as.
Specific embodiment
The present invention provides a kind of modified carbon fiber granule electrode and preparation method that carbazole function is removed with electro-catalysis, under Face illustrates to apply process in fact by an example.
Embodiment 1.
(1) 500mL beakers are put into after are washed with 1000mL deionized waters the 133g carbon fiber particles that particle diameter is 4～6mm In, 300mL molar concentrations are added for the hydrochloric acid solution of 0.1mol/L and soak 0.5h, liquid is removed after filtration and obtains substance A 01, Substance A 01 is added to into the AgNO that 250mL molar concentrations are 1.84mol/L3In solution, shake in the shaking table that temperature is 65 DEG C 15 minutes, it is cooled to after room temperature and is filtered to remove liquid and obtains substance A 02, the Jing 900mL mass percent concentrations of substance A 02 is 95% Ethanol washing after place 1.5h in 85 DEG C of drying box, be subsequently placed in Muffle furnace the roasting 1h under the conditions of 480 DEG C, obtain Substance A 1；
(2) it is in 1000mL conical flasks, in 1000r/ 8.99 grams of platinum nitrates and 800mL deionized waters to be added to into volume Stir 3 minutes under the conditions of min, add 15mL red fuming nitric acid (RFNA)s, 4 parts of equivalent is divided into after shaking up, obtain mixed liquor K1, mixed liquor K2, mix Close liquid K3, mixed liquor K4；
(3) by 627 milligrams of Sb (NO3)3With the AgNO that 30mL molar concentrations are 0.44mol/L3Solution is added to mixed liquor K1 In, stir 3 minutes under the conditions of 1000r/min, obtain mixed liquor L1；
(4) substance A 1 is added in mixed liquor L1, is shaken 15 minutes in the shaking table that temperature is 45 DEG C, be cooled to room temperature After be filtered to remove liquid and obtain substance A 2, substance A 2 is Jing after the ethanol washing that 100mL mass percent concentrations are 95% at 85 DEG C Drying box in place 1.5h, be subsequently placed in Muffle furnace the roasting 1h under the conditions of 480 DEG C, obtain substance A 3；
(5) by 647 milligrams of Sb (NO3)3With the AgNO that 50mL molar concentrations are 0.54mol/L3Solution is added to mixed liquor K2 In, stir 3 minutes under the conditions of 1000r/min, obtain mixed liquor L2；
(6) substance A 3 is added in mixed liquor L2, is shaken 15 minutes in the shaking table that temperature is 45 DEG C, be cooled to room temperature After be filtered to remove liquid and obtain substance A 4, substance A 4 is Jing after the ethanol washing that 100mL mass percent concentrations are 95% at 85 DEG C Drying box in place 1.5h, be subsequently placed in Muffle furnace the roasting 1h under the conditions of 480 DEG C, obtain substance A 5；
(7) by 667 milligrams of Sb (NO3)3With the AgNO that 70mL molar concentrations are 0.64mol/L3Solution is added to mixed liquor K3 In, stir 3 minutes under the conditions of 1000r/min, obtain mixed liquor L3；
(8) substance A 5 is added in mixed liquor L3, is shaken 15 minutes in the shaking table that temperature is 45 DEG C, be cooled to room temperature After be filtered to remove liquid and obtain substance A 6, substance A 6 is Jing after the ethanol washing that 100mL mass percent concentrations are 95% at 85 DEG C Drying box in place 1.5h, be subsequently placed in Muffle furnace the roasting 1h under the conditions of 480 DEG C, obtain substance A 7；
(9) by 687 milligrams of Sb (NO3)3With the AgNO that 90mL molar concentrations are 0.74mol/L3Solution is added to mixed liquor K4 In, stir 3 minutes under the conditions of 1000r/min, obtain mixed liquor L4；
(10) substance A 7 is added in mixed liquor L4, is shaken 15 minutes in the shaking table that temperature is 45 DEG C, be cooled to room Liquid is filtered to remove after temperature and obtains substance A 8, substance A 8 is Jing after the ethanol washing that 100mL mass percent concentrations are 95% 85 DEG C drying box in place 1.5h, be subsequently placed in Muffle furnace the roasting 1h under the conditions of 480 DEG C, obtain substance A；
(11) by 6.59 grams of AgNO3It is in 1000mL conical flasks, in 1000r/min bars to be added to volume with 750mL ether Stir 3 minutes under part, 3 parts of equivalent is divided into after shaking up, obtain mixed liquor M1, mixed liquor M2, mixed liquor M3；
(12) by 329 milligrams of AgNO3With the Sb (NO that 30mL molar concentrations are 0.48mol/L3)3Solution is added to mixed liquor In M1, stir 3 minutes under the conditions of 1000r/min, obtain mixed liquor N1；
(13) substance A is added in mixed liquor N1, is shaken 15 minutes in the shaking table that temperature is 45 DEG C, be cooled to room temperature After be filtered to remove liquid and obtain substance B, substance B is Jing after the ethanol washing that 100mL mass percent concentrations are 95% at 85 DEG C 1.5h is placed in drying box, the roasting 1h under the conditions of 480 DEG C is subsequently placed in Muffle furnace, substance B 1 is obtained；
(14) by 359 milligrams of AgNO3With the Sb (NO that 60mL molar concentrations are 0.68mol/L3)3Solution is added to mixed liquor In M2, stir 3 minutes under the conditions of 1000r/min, obtain mixed liquor N2；
(15) substance B 1 is added in mixed liquor N2, is shaken 15 minutes in the shaking table that temperature is 45 DEG C, be cooled to room Liquid is filtered to remove after temperature and obtains substance B 2, substance B 2 is Jing after the ethanol washing that 100mL mass percent concentrations are 95% 85 DEG C drying box in place 1.5h, be subsequently placed in Muffle furnace the roasting 1h under the conditions of 480 DEG C, obtain substance C；
(16) by 389 milligrams of AgNO3With the Sb (NO that 90mL molar concentrations are 0.88mol/L3)3Solution is added to mixed liquor In M3, stir 3 minutes under the conditions of 1000r/min, obtain mixed liquor N3；
(17) substance C is added in mixed liquor N3, is shaken 15 minutes in the shaking table that temperature is 45 DEG C, be cooled to room temperature After be filtered to remove liquid and obtain material D, material D is Jing after the ethanol washing that 100mL mass percent concentrations are 95% at 85 DEG C 1.5h is placed in drying box, the roasting 1h under the conditions of 480 DEG C is subsequently placed in Muffle furnace, material E is obtained；
(18) by 7.58 grams of Pb (NO3)2It is in 1000mL conical flasks, in 1000r/min to be added to volume with 900mL ethanol Under the conditions of stir 3 minutes, add 5mL red fuming nitric acid (RFNA)s, 3 parts of equivalent is divided into after shaking up, obtain mixed liquor P1, mixed liquor P2, mixed liquor P3；
(19) by 85mL molar concentrations for 0.99mol/L AlCl3Solution is added in mixed liquor P1, in 1000r/min Under the conditions of stir 3 minutes, obtain mixed liquor Q1；
(20) material E is added in mixed liquor Q1, is shaken 15 minutes in the shaking table that temperature is 45 DEG C, be cooled to room temperature After be filtered to remove liquid and obtain material F1, material F1 is Jing after the ethanol washing that 100mL mass percent concentrations are 95% at 85 DEG C Drying box in place 1.5h, be subsequently placed in Muffle furnace the roasting 1h under the conditions of 480 DEG C, obtain material F2；
(21) by 75mL molar concentrations for 0.69mol/L Pb (NO3)2Solution is added in mixed liquor P2, in 1000r/ Stir 3 minutes under the conditions of min, obtain mixed liquor Q2；
(22) material F2 is added in mixed liquor Q2, is shaken 15 minutes in the shaking table that temperature is 45 DEG C, be cooled to room Liquid is filtered to remove after temperature and obtains material F3, material F3 is Jing after the ethanol washing that 100mL mass percent concentrations are 95% 85 DEG C drying box in place 1.5h, be subsequently placed in Muffle furnace the roasting 1h under the conditions of 480 DEG C, obtain material F4；
(23) by 55mL molar concentrations for 0.59mol/L AlCl3Solution is added in mixed liquor P3, in 1000r/min Under the conditions of stir 3 minutes, obtain mixed liquor Q3；
(24) material F4 is added in mixed liquor Q3, is shaken 15 minutes in the shaking table that temperature is 45 DEG C, be cooled to room Liquid is filtered to remove after temperature and obtains material F5, material F5 is Jing after the ethanol washing that 100mL mass percent concentrations are 95% 85 DEG C drying box in place 1.5h, be subsequently placed in Muffle furnace the roasting 1h under the conditions of 480 DEG C, obtain material F；
(25) by 6.58g PtCl4Volume is added to the sodium citrate solution that 750mL mass percent concentrations are 10% In for 1000mL conical flasks, stir 3 minutes under the conditions of 1000r/min, 3 parts of equivalent is divided into after shaking up, obtain mixed liquor R1, mix Close liquid R2, mixed liquor R3；
(26) by 40mL molar concentrations for 0.38mol/L CdCl2Solution and 60mL molar concentrations are for 0.86mol/L's PdCl2Solution is added in mixed liquor R1, is stirred 3 minutes under the conditions of 1000r/min, obtains mixed liquor S1；
(27) material F is added in mixed liquor S1, is shaken 15 minutes in the shaking table that temperature is 45 DEG C, be cooled to room temperature After be filtered to remove liquid and obtain material G1, material G1 is Jing after the ethanol washing that 100mL mass percent concentrations are 95% at 85 DEG C Drying box in place 1.5h, be subsequently placed in Muffle furnace the roasting 1h under the conditions of 480 DEG C, obtain material H1；
(28) by 50mL molar concentrations for 0.58mol/L CdCl2Solution and 50mL molar concentrations are for 0.66mol/L's PdCl2Solution is added in mixed liquor R2, is stirred 3 minutes under the conditions of 1000r/min, obtains mixed liquor S2；
(29) material H1 is added in mixed liquor S2, is shaken 15 minutes in the shaking table that temperature is 45 DEG C, be cooled to room Liquid is filtered to remove after temperature and obtains material G2, material G2 is Jing after the ethanol washing that 100mL mass percent concentrations are 95% 85 DEG C drying box in place 1.5h, be subsequently placed in Muffle furnace the roasting 1h under the conditions of 480 DEG C, obtain material H2；
(30) by 60mL molar concentrations for 0.78mol/L CdCl2Solution and 40mL molar concentrations are for 0.46mol/L's PdCl2Solution is added in mixed liquor R3, is stirred 3 minutes under the conditions of 1000r/min, obtains mixed liquor S3；
(31) material H2 is added in mixed liquor S3, is shaken 15 minutes in the shaking table that temperature is 45 DEG C, be cooled to room Liquid is filtered to remove after temperature and obtains material G3, material G3 is Jing after the ethanol washing that 100mL mass percent concentrations are 95% 85 DEG C drying box in place 1.5h, be subsequently placed in Muffle furnace the roasting 1h under the conditions of 480 DEG C, obtain material H；
(32) 6.39g lauryl sodium sulfate, 40mL n-hexanes, 20 milliliters of n-butanols are added sequentially to volume and are In 250mL conical flasks, 11.28g ammonium metavanadates and 150mL deionized waters are added, be placed in 70 DEG C of water-baths in 1000r/min bars 1h is stirred under part, the hydrochloric acid solution that 25mL molar concentrations are 2.40mol/L is subsequently adding, is shaken in the shaking table that temperature is 45 DEG C 0.5h, is cooled to after room temperature under the conditions of 7500r/min and 15min is centrifuged, and removes supernatant, uses 500mL mass percent concentrations Ethanol for 95% is washed, and obtains material I；
(33) sodium citrate solution that material I and 800mL mass percent concentration is 15% is added to into volume is In 1000mL conical flasks, stir 3 minutes under the conditions of 1000r/min, 4 parts of equivalent is divided into after shaking up, obtain mixed liquor T1, mixing Liquid T2, mixed liquor T3, mixed liquor T4；
(34) by 35mL molar concentrations for 0.48mol/L CdCl2Solution and 65mL molar concentrations are for 0.99mol/L's PdCl2Solution is added in mixed liquor T1, is stirred 3 minutes under the conditions of 1000r/min, obtains mixed liquor U1；
(35) material H is added in mixed liquor U1, is shaken 15 minutes in the shaking table that temperature is 45 DEG C, be cooled to room temperature After be filtered to remove liquid and obtain material J1, material J1 is Jing after the ethanol washing that 100mL mass percent concentrations are 95% at 85 DEG C Drying box in place 1.5h, be subsequently placed in Muffle furnace the roasting 1h under the conditions of 480 DEG C, obtain material K1；
(36) by 45mL molar concentrations for 0.58mol/L CdCl2Solution and 55mL molar concentrations are for 0.79mol/L's PdCl2Solution is added in mixed liquor T2, is stirred 3 minutes under the conditions of 1000r/min, obtains mixed liquor U2；
(37) material K1 is added in mixed liquor U2, is shaken 15 minutes in the shaking table that temperature is 45 DEG C, be cooled to room Liquid is filtered to remove after temperature and obtains material J2, material J2 is Jing after the ethanol washing that 100mL mass percent concentrations are 95% 85 DEG C drying box in place 1.5h, be subsequently placed in Muffle furnace the roasting 1h under the conditions of 480 DEG C, obtain material K2；
(38) by 55mL molar concentrations for 0.68mol/L CdCl2Solution and 45mL molar concentrations are for 0.59mol/L's PdCl2Solution is added in mixed liquor T3, is stirred 3 minutes under the conditions of 1000r/min, obtains mixed liquor U3；
(39) material K2 is added in mixed liquor U3, is shaken 15 minutes in the shaking table that temperature is 45 DEG C, be cooled to room Liquid is filtered to remove after temperature and obtains material J3, material J3 is Jing after the ethanol washing that 100mL mass percent concentrations are 95% 85 DEG C drying box in place 1.5h, be subsequently placed in Muffle furnace the roasting 1h under the conditions of 480 DEG C, obtain material K3；
(40) by 65mL molar concentrations for 0.78mol/L CdCl2Solution and 35mL molar concentrations are for 0.39mol/L's PdCl2Solution is added in mixed liquor T4, is stirred 3 minutes under the conditions of 1000r/min, obtains mixed liquor U4；
(41) material K3 is added in mixed liquor U4, is shaken 15 minutes in the shaking table that temperature is 45 DEG C, be cooled to room Liquid is filtered to remove after temperature and obtains material J4, material J4 is Jing after the ethanol washing that 100mL mass percent concentrations are 95% 85 DEG C drying box in place 1.5h, be subsequently placed in Muffle furnace the roasting 1h under the conditions of 480 DEG C, obtain material K；
(42) 12.64g polyvinyl alcohol and 800mL deionized waters are added to into volume in 1000mL conical flasks, Stir 3 minutes under the conditions of 1000r/min, 4 parts of equivalent is divided into after shaking up, obtain mixed liquor V1, mixed liquor V2, mixed liquor V3, mixed Close liquid V4；
(43) by 95mL molar concentrations for 0.78mol/L HAuCl4Solution is added in mixed liquor V1, in 1000r/min Under the conditions of stir 3 minutes, obtain mixed liquor W1；
(44) material K is added in mixed liquor W1, is shaken 15 minutes in the shaking table that temperature is 45 DEG C, be cooled to room temperature After be filtered to remove liquid and obtain material L1, material L1 is Jing after the ethanol washing that 100mL mass percent concentrations are 95% at 85 DEG C Drying box in place 1.5h, be subsequently placed in Muffle furnace the roasting 1h under the conditions of 480 DEG C, obtain material Z1；
(45) by 75mL molar concentrations for 0.68mol/L HAuCl4Solution is added in mixed liquor V2, in 1000r/min Under the conditions of stir 3 minutes, obtain mixed liquor W2；
(46) material Z1 is added in mixed liquor W2, is shaken 15 minutes in the shaking table that temperature is 45 DEG C, be cooled to room Liquid is filtered to remove after temperature and obtains material L2, material L2 is Jing after the ethanol washing that 100mL mass percent concentrations are 95% 85 DEG C drying box in place 1.5h, be subsequently placed in Muffle furnace the roasting 1h under the conditions of 480 DEG C, obtain material Z2；
(47) by 55mL molar concentrations for 0.58mol/L HAuCl4Solution is added in mixed liquor V3, in 1000r/min Under the conditions of stir 3 minutes, obtain mixed liquor W3；
(48) material Z2 is added in mixed liquor W3, is shaken 15 minutes in the shaking table that temperature is 45 DEG C, be cooled to room Liquid is filtered to remove after temperature and obtains material L3, material L3 is Jing after the ethanol washing that 100mL mass percent concentrations are 95% 85 DEG C drying box in place 1.5h, be subsequently placed in Muffle furnace the roasting 1h under the conditions of 480 DEG C, obtain material Z3；
(49) by 35mL molar concentrations for 0.48mol/L HAuCl4Solution is added in mixed liquor V4, in 1000r/min Under the conditions of stir 3 minutes, obtain mixed liquor W4；
(50) material Z3 is added in mixed liquor W4, is shaken 15 minutes in the shaking table that temperature is 45 DEG C, be cooled to room Liquid is filtered to remove after temperature and obtains material L4, material L4 is Jing after the ethanol washing that 100mL mass percent concentrations are 95% 85 DEG C drying box in place 1.5h, be subsequently placed in Muffle furnace the roasting 1h under the conditions of 480 DEG C, the material for obtaining as has electricity The modified carbon fiber granule electrode of catalytic elimination carbazole function.
It is presented herein below with the modified carbon fiber granule electrode obtained in the inventive method with electro-catalysis removal carbazole function Electro-catalytic Oxidation Process test has been carried out to the waste water containing carbazole in electric catalysis reactor, the present invention has been further illustrated.
Electricity is seated in by having the modified carbon fiber granule electrode that electro-catalysis removes carbazole function obtained in the inventive method In catalytic reactor, Degrading experiment is carried out to the waste water containing carbazole, as a result shown the electrocatalytic reaction loaded by the electrode Device can efficiently remove the carbazole in waste water, be 5.0 in pH when the carbazole concentration in waste water is 55.4mg/L, and voltage is 14V, process time is that the carbazole concentration after process in water outlet is reduced to 0.6mg/L under the conditions of 45min.

Claims (1)

1. it is a kind of with electro-catalysis remove carbazole function modified carbon fiber granule electrode preparation method, it is characterised in that should Method is comprised the following steps that：
(1) it is put in 500mL beakers after are washed with 1000mL deionized waters the 133g carbon fiber particles that particle diameter is 4～6mm, plus Enter 300mL molar concentrations be 0.1mol/L hydrochloric acid solution and soak 0.5h, after filtration remove liquid obtain substance A 01, by thing Matter A01 is added to the AgNO that 250mL molar concentrations are 1.84mol/L3In solution, 15 points are shaken in the shaking table that temperature is 65 DEG C Clock, is cooled to after room temperature and is filtered to remove liquid and obtains substance A 02, and the Jing 900mL mass percent concentrations of substance A 02 are 95% second 1.5h is placed in 85 DEG C of drying box after alcohol washing, the roasting 1h under the conditions of 480 DEG C is subsequently placed in Muffle furnace, material is obtained A1；
(2) it is in 1000mL conical flasks, in 1000r/min bars 8.99 grams of platinum nitrates and 800mL deionized waters to be added to into volume Stir 3 minutes under part, add 15mL red fuming nitric acid (RFNA)s, 4 parts of equivalent is divided into after shaking up, obtain mixed liquor K1, mixed liquor K2, mixed liquor K3, mixed liquor K4；
(3) by 627 milligrams of Sb (NO3)3With the AgNO that 30mL molar concentrations are 0.44mol/L3Solution is added in mixed liquor K1, Stir 3 minutes under the conditions of 1000r/min, obtain mixed liquor L1；
(4) substance A 1 is added in mixed liquor L1, is shaken 15 minutes in the shaking table that temperature is 45 DEG C, be cooled to mistake after room temperature Filter liquid and obtain substance A 2, substance A 2 is dry at 85 DEG C Jing after the ethanol washing that 100mL mass percent concentrations are 95% 1.5h is placed in dry case, the roasting 1h under the conditions of 480 DEG C is subsequently placed in Muffle furnace, substance A 3 is obtained；
(5) by 647 milligrams of Sb (NO3)3With the AgNO that 50mL molar concentrations are 0.54mol/L3Solution is added in mixed liquor K2, Stir 3 minutes under the conditions of 1000r/min, obtain mixed liquor L2；
(6) substance A 3 is added in mixed liquor L2, is shaken 15 minutes in the shaking table that temperature is 45 DEG C, be cooled to mistake after room temperature Filter liquid and obtain substance A 4, substance A 4 is dry at 85 DEG C Jing after the ethanol washing that 100mL mass percent concentrations are 95% 1.5h is placed in dry case, the roasting 1h under the conditions of 480 DEG C is subsequently placed in Muffle furnace, substance A 5 is obtained；
(7) by 667 milligrams of Sb (NO3)3With the AgNO that 70mL molar concentrations are 0.64mol/L3Solution is added in mixed liquor K3, Stir 3 minutes under the conditions of 1000r/min, obtain mixed liquor L3；
(8) substance A 5 is added in mixed liquor L3, is shaken 15 minutes in the shaking table that temperature is 45 DEG C, be cooled to mistake after room temperature Filter liquid and obtain substance A 6, substance A 6 is dry at 85 DEG C Jing after the ethanol washing that 100mL mass percent concentrations are 95% 1.5h is placed in dry case, the roasting 1h under the conditions of 480 DEG C is subsequently placed in Muffle furnace, substance A 7 is obtained；
(9) by 687 milligrams of Sb (NO3)3With the AgNO that 90mL molar concentrations are 0.74mol/L3Solution is added in mixed liquor K4, Stir 3 minutes under the conditions of 1000r/min, obtain mixed liquor L4；
(10) substance A 7 is added in mixed liquor L4, is shaken 15 minutes in the shaking table that temperature is 45 DEG C, after being cooled to room temperature It is filtered to remove liquid and obtains substance A 8, substance A 8 is Jing after the ethanol washing that 100mL mass percent concentrations are 95% at 85 DEG C 1.5h is placed in drying box, the roasting 1h under the conditions of 480 DEG C is subsequently placed in Muffle furnace, substance A is obtained；
(11) by 6.59 grams of AgNO3With 750mL ether volume is added in 1000mL conical flasks, to stir under the conditions of 1000r/min Mix 3 minutes, 3 parts of equivalent is divided into after shaking up, obtain mixed liquor M1, mixed liquor M2, mixed liquor M3；
(12) by 329 milligrams of AgNO3With the Sb (NO that 30mL molar concentrations are 0.48mol/L3)3Solution is added in mixed liquor M1, Stir 3 minutes under the conditions of 1000r/min, obtain mixed liquor N1；
(13) substance A is added in mixed liquor N1, is shaken 15 minutes in the shaking table that temperature is 45 DEG C, be cooled to mistake after room temperature Filter liquid and obtain substance B, substance B is Jing after the ethanol washing that 100mL mass percent concentrations are 95% in 85 DEG C of drying 1.5h is placed in case, the roasting 1h under the conditions of 480 DEG C is subsequently placed in Muffle furnace, substance B 1 is obtained；
(14) by 359 milligrams of AgNO3With the Sb (NO that 60mL molar concentrations are 0.68mol/L3)3Solution is added in mixed liquor M2, Stir 3 minutes under the conditions of 1000r/min, obtain mixed liquor N2；
(15) substance B 1 is added in mixed liquor N2, is shaken 15 minutes in the shaking table that temperature is 45 DEG C, after being cooled to room temperature It is filtered to remove liquid and obtains substance B 2, substance B 2 is Jing after the ethanol washing that 100mL mass percent concentrations are 95% at 85 DEG C 1.5h is placed in drying box, the roasting 1h under the conditions of 480 DEG C is subsequently placed in Muffle furnace, substance C is obtained；
(16) by 389 milligrams of AgNO3With the Sb (NO that 90mL molar concentrations are 0.88mol/L3)3Solution is added in mixed liquor M3, Stir 3 minutes under the conditions of 1000r/min, obtain mixed liquor N3；
(17) substance C is added in mixed liquor N3, is shaken 15 minutes in the shaking table that temperature is 45 DEG C, be cooled to mistake after room temperature Filter liquid and obtain material D, material D is Jing after the ethanol washing that 100mL mass percent concentrations are 95% in 85 DEG C of drying 1.5h is placed in case, the roasting 1h under the conditions of 480 DEG C is subsequently placed in Muffle furnace, material E is obtained；
(18) by 7.58 grams of Pb (NO3)2It is in 1000mL conical flasks, in 1000r/min conditions to be added to volume with 900mL ethanol Lower stirring 3 minutes, adds 5mL red fuming nitric acid (RFNA)s, and 3 parts of equivalent is divided into after shaking up, and obtains mixed liquor P1, mixed liquor P2, mixed liquor P3；
(19) by 85mL molar concentrations for 0.99mol/L AlCl3Solution is added in mixed liquor P1, under the conditions of 1000r/min Stirring 3 minutes, obtains mixed liquor Q1；
(20) material E is added in mixed liquor Q1, is shaken 15 minutes in the shaking table that temperature is 45 DEG C, be cooled to mistake after room temperature Filter liquid and obtain material F1, material F1 is dry at 85 DEG C Jing after the ethanol washing that 100mL mass percent concentrations are 95% 1.5h is placed in dry case, the roasting 1h under the conditions of 480 DEG C is subsequently placed in Muffle furnace, material F2 is obtained；
(21) by 75mL molar concentrations for 0.69mol/L Pb (NO3)2Solution is added in mixed liquor P2, in 1000r/min bars Stir 3 minutes under part, obtain mixed liquor Q2；
(22) material F2 is added in mixed liquor Q2, is shaken 15 minutes in the shaking table that temperature is 45 DEG C, after being cooled to room temperature It is filtered to remove liquid and obtains material F3, material F3 is Jing after the ethanol washing that 100mL mass percent concentrations are 95% at 85 DEG C 1.5h is placed in drying box, the roasting 1h under the conditions of 480 DEG C is subsequently placed in Muffle furnace, material F4 is obtained；
(23) by 55mL molar concentrations for 0.59mol/L AlCl3Solution is added in mixed liquor P3, under the conditions of 1000r/min Stirring 3 minutes, obtains mixed liquor Q3；
(24) material F4 is added in mixed liquor Q3, is shaken 15 minutes in the shaking table that temperature is 45 DEG C, after being cooled to room temperature It is filtered to remove liquid and obtains material F5, material F5 is Jing after the ethanol washing that 100mL mass percent concentrations are 95% at 85 DEG C 1.5h is placed in drying box, the roasting 1h under the conditions of 480 DEG C is subsequently placed in Muffle furnace, material F is obtained；
(25) by 6.58g PtCl4Being added to volume with the sodium citrate solution that 750mL mass percent concentrations are 10% is In 1000mL conical flasks, stir 3 minutes under the conditions of 1000r/min, 3 parts of equivalent is divided into after shaking up, obtain mixed liquor R1, mixing Liquid R2, mixed liquor R3；
(26) by 40mL molar concentrations for 0.38mol/L CdCl2Solution and the PdCl that 60mL molar concentrations are 0.86mol/L2It is molten Liquid is added in mixed liquor R1, is stirred 3 minutes under the conditions of 1000r/min, obtains mixed liquor S1；
(27) material F is added in mixed liquor S1, is shaken 15 minutes in the shaking table that temperature is 45 DEG C, be cooled to mistake after room temperature Filter liquid and obtain material G1, material G1 is dry at 85 DEG C Jing after the ethanol washing that 100mL mass percent concentrations are 95% 1.5h is placed in dry case, the roasting 1h under the conditions of 480 DEG C is subsequently placed in Muffle furnace, material H1 is obtained；
(28) by 50mL molar concentrations for 0.58mol/L CdCl2Solution and the PdCl that 50mL molar concentrations are 0.66mol/L2It is molten Liquid is added in mixed liquor R2, is stirred 3 minutes under the conditions of 1000r/min, obtains mixed liquor S2；
(29) material H1 is added in mixed liquor S2, is shaken 15 minutes in the shaking table that temperature is 45 DEG C, after being cooled to room temperature It is filtered to remove liquid and obtains material G2, material G2 is Jing after the ethanol washing that 100mL mass percent concentrations are 95% at 85 DEG C 1.5h is placed in drying box, the roasting 1h under the conditions of 480 DEG C is subsequently placed in Muffle furnace, material H2 is obtained；
(30) by 60mL molar concentrations for 0.78mol/L CdCl2Solution and the PdCl that 40mL molar concentrations are 0.46mol/L2It is molten Liquid is added in mixed liquor R3, is stirred 3 minutes under the conditions of 1000r/min, obtains mixed liquor S3；
(31) material H2 is added in mixed liquor S3, is shaken 15 minutes in the shaking table that temperature is 45 DEG C, after being cooled to room temperature It is filtered to remove liquid and obtains material G3, material G3 is Jing after the ethanol washing that 100mL mass percent concentrations are 95% at 85 DEG C 1.5h is placed in drying box, the roasting 1h under the conditions of 480 DEG C is subsequently placed in Muffle furnace, material H is obtained；
(32) 6.39g lauryl sodium sulfate, 40mL n-hexanes, 20 milliliters of n-butanols are added sequentially to into volume for 250mL cones In shape bottle, 11.28g ammonium metavanadates and 150mL deionized waters are added, be placed in 70 DEG C of water-baths and stirred under the conditions of 1000r/min 1h is mixed, the hydrochloric acid solution that 25mL molar concentrations are 2.40mol/L is subsequently adding, in the shaking table that temperature is 45 DEG C 0.5h is shaken, It is cooled to after room temperature under the conditions of 7500r/min and 15min is centrifuged, remove supernatant, is 95% with 500mL mass percent concentrations Ethanol washing, obtain material I；
(33) sodium citrate solution that material I and 800mL mass percent concentration is 15% is added to into volume for 1000mL cones In shape bottle, stir 3 minutes under the conditions of 1000r/min, 4 parts of equivalent is divided into after shaking up, obtain mixed liquor T1, mixed liquor T2, mix Close liquid T3, mixed liquor T4；
(34) by 35mL molar concentrations for 0.48mol/L CdCl2Solution and the PdCl that 65mL molar concentrations are 0.99mol/L2It is molten Liquid is added in mixed liquor T1, is stirred 3 minutes under the conditions of 1000r/min, obtains mixed liquor U1；
(35) material H is added in mixed liquor U1, is shaken 15 minutes in the shaking table that temperature is 45 DEG C, be cooled to mistake after room temperature Filter liquid and obtain material J1, material J1 is dry at 85 DEG C Jing after the ethanol washing that 100mL mass percent concentrations are 95% 1.5h is placed in dry case, the roasting 1h under the conditions of 480 DEG C is subsequently placed in Muffle furnace, material K1 is obtained；
(36) by 45mL molar concentrations for 0.58mol/L CdCl2Solution and the PdCl that 55mL molar concentrations are 0.79mol/L2It is molten Liquid is added in mixed liquor T2, is stirred 3 minutes under the conditions of 1000r/min, obtains mixed liquor U2；
(37) material K1 is added in mixed liquor U2, is shaken 15 minutes in the shaking table that temperature is 45 DEG C, after being cooled to room temperature It is filtered to remove liquid and obtains material J2, material J2 is Jing after the ethanol washing that 100mL mass percent concentrations are 95% at 85 DEG C 1.5h is placed in drying box, the roasting 1h under the conditions of 480 DEG C is subsequently placed in Muffle furnace, material K2 is obtained；
(38) by 55mL molar concentrations for 0.68mol/L CdCl2Solution and the PdCl that 45mL molar concentrations are 0.59mol/L2It is molten Liquid is added in mixed liquor T3, is stirred 3 minutes under the conditions of 1000r/min, obtains mixed liquor U3；
(39) material K2 is added in mixed liquor U3, is shaken 15 minutes in the shaking table that temperature is 45 DEG C, after being cooled to room temperature It is filtered to remove liquid and obtains material J3, material J3 is Jing after the ethanol washing that 100mL mass percent concentrations are 95% at 85 DEG C 1.5h is placed in drying box, the roasting 1h under the conditions of 480 DEG C is subsequently placed in Muffle furnace, material K3 is obtained；
(40) by 65mL molar concentrations for 0.78mol/L CdCl2Solution and the PdCl that 35mL molar concentrations are 0.39mol/L2It is molten Liquid is added in mixed liquor T4, is stirred 3 minutes under the conditions of 1000r/min, obtains mixed liquor U4；
(41) material K3 is added in mixed liquor U4, is shaken 15 minutes in the shaking table that temperature is 45 DEG C, after being cooled to room temperature It is filtered to remove liquid and obtains material J4, material J4 is Jing after the ethanol washing that 100mL mass percent concentrations are 95% at 85 DEG C 1.5h is placed in drying box, the roasting 1h under the conditions of 480 DEG C is subsequently placed in Muffle furnace, material K is obtained；
(42) it is in 1000mL conical flasks, in 1000r/min 12.64g polyvinyl alcohol and 800mL deionized waters to be added to into volume Under the conditions of stir 3 minutes, 4 parts of equivalent is divided into after shaking up, obtain mixed liquor V1, mixed liquor V2, mixed liquor V3, mixed liquor V4；
(43) by 95mL molar concentrations for 0.78mol/L HAuCl4Solution is added in mixed liquor V1, in 1000r/min conditions Lower stirring 3 minutes, obtains mixed liquor W1；
(44) material K is added in mixed liquor W1, is shaken 15 minutes in the shaking table that temperature is 45 DEG C, be cooled to mistake after room temperature Filter liquid and obtain material L1, material L1 is dry at 85 DEG C Jing after the ethanol washing that 100mL mass percent concentrations are 95% 1.5h is placed in dry case, the roasting 1h under the conditions of 480 DEG C is subsequently placed in Muffle furnace, material Z1 is obtained；
(45) by 75mL molar concentrations for 0.68mol/L HAuCl4Solution is added in mixed liquor V2, in 1000r/min conditions Lower stirring 3 minutes, obtains mixed liquor W2；
(46) material Z1 is added in mixed liquor W2, is shaken 15 minutes in the shaking table that temperature is 45 DEG C, after being cooled to room temperature It is filtered to remove liquid and obtains material L2, material L2 is Jing after the ethanol washing that 100mL mass percent concentrations are 95% at 85 DEG C 1.5h is placed in drying box, the roasting 1h under the conditions of 480 DEG C is subsequently placed in Muffle furnace, material Z2 is obtained；
(47) by 55mL molar concentrations for 0.58mol/L HAuCl4Solution is added in mixed liquor V3, in 1000r/min conditions Lower stirring 3 minutes, obtains mixed liquor W3；
(48) material Z2 is added in mixed liquor W3, is shaken 15 minutes in the shaking table that temperature is 45 DEG C, after being cooled to room temperature It is filtered to remove liquid and obtains material L3, material L3 is Jing after the ethanol washing that 100mL mass percent concentrations are 95% at 85 DEG C 1.5h is placed in drying box, the roasting 1h under the conditions of 480 DEG C is subsequently placed in Muffle furnace, material Z3 is obtained；
(49) by 35mL molar concentrations for 0.48mol/L HAuCl4Solution is added in mixed liquor V4, in 1000r/min conditions Lower stirring 3 minutes, obtains mixed liquor W4；
(50) material Z3 is added in mixed liquor W4, is shaken 15 minutes in the shaking table that temperature is 45 DEG C, after being cooled to room temperature It is filtered to remove liquid and obtains material L4, material L4 is Jing after the ethanol washing that 100mL mass percent concentrations are 95% at 85 DEG C 1.5h is placed in drying box, the roasting 1h under the conditions of 480 DEG C is subsequently placed in Muffle furnace, the material for obtaining as has electro-catalysis Remove the modified carbon fiber granule electrode of carbazole function.
CN201611055946.3A 2016-11-21 2016-11-21 Modified carbon fiber electrode with function of removing carbazole through electrocatalysis and preparation method thereof Withdrawn CN106630023A (en)

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102173449A (en) * 2011-01-14 2011-09-07 同济大学 Method for preparing nanometer lead dioxide electrode
CN103539229A (en) * 2013-10-30 2014-01-29 北京师范大学 Particle electrode for efficiently removing various organic compounds and preparation method thereof

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102173449A (en) * 2011-01-14 2011-09-07 同济大学 Method for preparing nanometer lead dioxide electrode
CN103539229A (en) * 2013-10-30 2014-01-29 北京师范大学 Particle electrode for efficiently removing various organic compounds and preparation method thereof

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