CN106745527A - Modified Activated Carbon aerogel particles electrode and preparation method with electro-catalysis removal benzoquinones function - Google Patents

Modified Activated Carbon aerogel particles electrode and preparation method with electro-catalysis removal benzoquinones function Download PDF

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CN106745527A
CN106745527A CN201611055948.2A CN201611055948A CN106745527A CN 106745527 A CN106745527 A CN 106745527A CN 201611055948 A CN201611055948 A CN 201611055948A CN 106745527 A CN106745527 A CN 106745527A
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mixed liquor
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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
    • C02F2101/00—Nature of the contaminant
    • C02F2101/30—Organic compounds
    • C02F2101/34—Organic compounds containing oxygen

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Abstract

The invention discloses Modified Activated Carbon aerogel particles electrode and preparation method with electro-catalysis removal benzoquinones function.Charcoal-aero gel, chloroform, ethanol are prepared into substance A；Substance A is by by silver nitrate, platinum nitrate, ether, Al (NO3)3The mixed liquor of preparation is modified to be prepared into material E；Material E is by by Mn (NO3)2, ethanol, SbCl3、ZrCl4、NiCl2、PbCl2The mixed liquor of preparation is modified to be prepared into material H；Material H is by by lauryl sodium sulfate, n-hexane, n-butanol, ammonium metavanadate, sodium citrate, NiCl2、PbCl2The mixed liquor of preparation is modified to be prepared into material K；Material K is by by polyvinyl alcohol, HAuCl4The modified material that obtains of the mixed liquor of preparation is the Modified Activated Carbon aerogel particles electrode that benzoquinones function is removed with electro-catalysis.

Description

Modified Activated Carbon aerogel particles electrode and preparation with electro-catalysis removal benzoquinones function Method
Technical field
The invention belongs to organic wastewater with difficult degradation thereby Electrocatalytic Oxidation processing technology field, more particularly to one kind is urged with electricity Change the Modified Activated Carbon aerogel particles electrode and preparation method of removal benzoquinones 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 group with strong oxidizing property such as hydroxyl radical free radical, can Biodegradable or innocuous substance is converted into by hardly degraded organic substance or bio-toxicity pollutant, the biochemical of waste water is improved Property, so that beneficial to follow-up biological treatment.Therefore, electrocatalytic oxidation water technology is in treatment 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 current efficiency is low in the treatment of waste water, 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 lacking 1,4-benzoquinone specific pollutants has efficient electric catalytic elimination function at present Electrode material and preparation method.
The content of the invention
It is an object of the invention to provide it is a kind of with electro-catalysis removal benzoquinones function Modified Activated Carbon aerogel particles electrode and Preparation method, its preparation method is comprised the following steps that：
(1) the 94g carbon aerogel particles that particle diameter is 4~6mm are washed with 1000mL deionized waters, is then placed in 500mL 8h is soaked in chloroform, is washed with 1000mL deionized waters after taking-up, then be 95% with 1000mL mass percent concentrations 1.5h is placed in 85 DEG C of drying box after ethanol washing, substance A 1 is obtained；
(2) 8.29 grams of platinum nitrates and 800mL deionized waters are added to volume in 1000mL conical flasks, in 1000r/ Stirred 3 minutes under the conditions of min, add 15mL concentrated nitric acids, 4 parts of equivalent is divided into after shaking up, obtained mixed liquor K1, mixed liquor K2, mix Close liquid K3, mixed liquor K4；
(3) by 910 milligrams of Al (NO3)3It is the AgNO of 0.86mol/L with 85mL molar concentrations3Solution is added to mixed liquor K1 In, stirred 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 washed through the ethanol that 100mL mass percent concentrations are 84% after at 68 DEG C Drying box in place 156 minutes, be subsequently placed in Muffle furnace and be calcined 240 minutes under the conditions of 146 DEG C, obtain substance A 3；
(5) by 930 milligrams of Al (NO3)3It is the AgNO of 0.76mol/L with 75mL molar concentrations3Solution is added to mixed liquor K2 In, stirred 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 washed through the ethanol that 100mL mass percent concentrations are 84% after at 68 DEG C Drying box in place 156 minutes, be subsequently placed in Muffle furnace and be calcined 240 minutes under the conditions of 146 DEG C, obtain substance A 5；
(7) by 950 milligrams of Al (NO3)3It is the AgNO of 0.66mol/L with 65mL molar concentrations3Solution is added to mixed liquor K3 In, stirred 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 washed through the ethanol that 100mL mass percent concentrations are 84% after at 68 DEG C Drying box in place 156 minutes, be subsequently placed in Muffle furnace and be calcined 240 minutes under the conditions of 146 DEG C, obtain substance A 7；
(9) by 970 milligrams of Al (NO3)3It is the AgNO of 0.56mol/L with 55mL molar concentrations3Solution is added to mixed liquor K4 In, stirred 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 after the ethanol washing that 100mL mass percent concentrations are 84% 68 DEG C drying box in place 156 minutes, be subsequently placed in Muffle furnace and be calcined 240 minutes under the conditions of 146 DEG C, obtain substance A；
(11) by 4.37 grams of AgNO3Volume is added to in 1000mL conical flasks with 850mL ether, in 1000r/min bars Stirred 3 minutes under part, 5 parts of equivalent is divided into after shaking up, obtain mixed liquor M1, mixed liquor M2, mixed liquor M3, mixed liquor M4, mixing Liquid M5；
(12) by 218 milligrams of AgNO3It is the Al (NO of 0.95mol/L with 75mL molar concentrations3)3Solution is added to mixed liquor In M1, stirred 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 washed through the ethanol that 100mL mass percent concentrations are 84% after at 68 DEG C Placed 156 minutes in drying box, be subsequently placed in Muffle furnace and be calcined 240 minutes under the conditions of 146 DEG C, obtain substance B 1；
(14) by 238 milligrams of AgNO3It is the Al (NO of 0.85mol/L with 65mL molar concentrations3)3Solution is added to mixed liquor In M2, stirred 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 after the ethanol washing that 100mL mass percent concentrations are 84% 68 DEG C drying box in place 156 minutes, be subsequently placed in Muffle furnace and be calcined 240 minutes under the conditions of 146 DEG C, obtain substance B 3；
(16) by 258 milligrams of AgNO3It is the Al (NO of 0.75mol/L with 55mL molar concentrations3)3Solution is added to mixed liquor In M3, stirred 3 minutes under the conditions of 1000r/min, obtain mixed liquor N3；
(17) substance B 3 is added in mixed liquor N3, 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 4, substance B 4 is after the ethanol washing that 100mL mass percent concentrations are 84% 68 DEG C drying box in place 156 minutes, be subsequently placed in Muffle furnace and be calcined 240 minutes under the conditions of 146 DEG C, obtain substance B 5；
(18) by 278 milligrams of AgNO3It is the Al (NO of 0.65mol/L with 45mL molar concentrations3)3Solution is added to mixed liquor In M4, stirred 3 minutes under the conditions of 1000r/min, obtain mixed liquor N4；
(19) substance B 5 is added in mixed liquor N4, 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 6, substance B 6 is after the ethanol washing that 100mL mass percent concentrations are 84% 68 DEG C drying box in place 156 minutes, be subsequently placed in Muffle furnace and be calcined 240 minutes under the conditions of 146 DEG C, obtain substance C；
(20) by 298 milligrams of AgNO3It is the Al (NO of 0.55mol/L with 35mL molar concentrations3)3Solution is added to mixed liquor In M5, stirred 3 minutes under the conditions of 1000r/min, obtain mixed liquor N5；
(21) substance C is added in mixed liquor N5, 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 washed through the ethanol that 100mL mass percent concentrations are 84% after at 68 DEG C Placed 156 minutes in drying box, be subsequently placed in Muffle furnace and be calcined 240 minutes under the conditions of 146 DEG C, obtain material E；
(22) by 6.33 grams of Mn (NO3)2Volume is added to in 1000mL conical flasks with 850mL ethanol, in 1000r/min Under the conditions of stir 3 minutes, add 5mL concentrated nitric acids, 5 parts of equivalent is divided into after shaking up, obtain mixed liquor P1, mixed liquor P2, mixed liquor P3, mixed liquor P4, mixed liquor P5；
(23) it is the SbCl of 0.69mol/L by 95mL molar concentrations3Solution is added in mixed liquor P1, in 1000r/min Under the conditions of stir 3 minutes, obtain mixed liquor Q1；
(24) 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 washed through the ethanol that 100mL mass percent concentrations are 84% after at 68 DEG C Drying box in place 156 minutes, be subsequently placed in Muffle furnace and be calcined 240 minutes under the conditions of 146 DEG C, obtain material F2；
(25) it is the Mn (NO of 0.92mol/L by 80mL molar concentrations3)2Solution is added in mixed liquor P2, in 1000r/ Stirred 3 minutes under the conditions of min, obtain mixed liquor Q2；
(26) 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 after the ethanol washing that 100mL mass percent concentrations are 84% 68 DEG C drying box in place 156 minutes, be subsequently placed in Muffle furnace and be calcined 240 minutes under the conditions of 146 DEG C, obtain material F4；
(27) it is the SbCl of 0.59mol/L by 80mL molar concentrations3Solution is added in mixed liquor P3, in 1000r/min Under the conditions of stir 3 minutes, obtain mixed liquor Q3；
(28) 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 after the ethanol washing that 100mL mass percent concentrations are 84% 68 DEG C drying box in place 156 minutes, be subsequently placed in Muffle furnace and be calcined 240 minutes under the conditions of 146 DEG C, obtain material F6；
(29) it is the Mn (NO of 0.72mol/L by 60mL molar concentrations3)2Solution is added in mixed liquor P4, in 1000r/ Stirred 3 minutes under the conditions of min, obtain mixed liquor Q4；
(30) material F6 is added in mixed liquor Q4, 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 F7, material F7 is after the ethanol washing that 100mL mass percent concentrations are 84% 68 DEG C drying box in place 156 minutes, be subsequently placed in Muffle furnace and be calcined 240 minutes under the conditions of 146 DEG C, obtain material F8；
(31) it is the SbCl of 0.49mol/L by 65mL molar concentrations3Solution and 40mL molar concentrations are the Mn of 0.52mol/L (NO3)2Solution is added in mixed liquor P5, is stirred 3 minutes under the conditions of 1000r/min, obtains mixed liquor Q5；
(32) material F8 is added in mixed liquor Q5, 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 F9, material F9 is after the ethanol washing that 100mL mass percent concentrations are 84% 68 DEG C drying box in place 156 minutes, be subsequently placed in Muffle furnace and be calcined 240 minutes under the conditions of 146 DEG C, obtain material F；
(33) by 6.57g ZrCl4Volume is added to the sodium citrate solution that 750mL mass percent concentrations are 10% In for 1000mL conical flasks, stirred 3 minutes under the conditions of 1000r/min, 3 parts of equivalent is divided into after shaking up, obtained mixed liquor R1, mix Close liquid R2, mixed liquor R3；
(34) it is the NiCl of 0.38mol/L by 40mL molar concentrations2Solution and 60mL molar concentrations are 0.84mol/L's PbCl2Solution is added in mixed liquor R1, is stirred 3 minutes under the conditions of 1000r/min, obtains mixed liquor S1；
(35) 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 washed through the ethanol that 100mL mass percent concentrations are 84% after at 68 DEG C Drying box in place 156 minutes, be subsequently placed in Muffle furnace and be calcined 240 minutes under the conditions of 146 DEG C, obtain material H1；
(36) it is the NiCl of 0.58mol/L by 50mL molar concentrations2Solution and 50mL molar concentrations are 0.64mol/L's PbCl2Solution is added in mixed liquor R2, is stirred 3 minutes under the conditions of 1000r/min, obtains mixed liquor S2；
(37) 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 after the ethanol washing that 100mL mass percent concentrations are 84% 68 DEG C drying box in place 156 minutes, be subsequently placed in Muffle furnace and be calcined 240 minutes under the conditions of 146 DEG C, obtain material H2；
(38) it is the NiCl of 0.78mol/L by 60mL molar concentrations2Solution and 40mL molar concentrations are 0.44mol/L's PbCl2Solution is added in mixed liquor R3, is stirred 3 minutes under the conditions of 1000r/min, obtains mixed liquor S3；
(39) 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 after the ethanol washing that 100mL mass percent concentrations are 84% 68 DEG C drying box in place 156 minutes, be subsequently placed in Muffle furnace and be calcined 240 minutes under the conditions of 146 DEG C, obtain material H；
(40) 3.28g lauryl sodium sulfate, 40mL n-hexanes, 20 milliliters of n-butanols are added sequentially to volume and are In 250mL conical flasks, 7.49g 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, shaken in the shaking table that temperature is 45 DEG C 0.5h, 15min is centrifuged after being cooled to room temperature under the conditions of 7500r/min, removes supernatant, uses 500mL mass percent concentrations Ethanol for 95% is washed, and obtains material I；
(41) sodium citrate solution that material I and 850mL mass percent concentration is 15% is added into volume is In 1000mL conical flasks, stirred 3 minutes under the conditions of 1000r/min, 5 parts of equivalent is divided into after shaking up, obtain mixed liquor T1, mixing Liquid T2, mixed liquor T3, mixed liquor T4, mixed liquor T5；
(42) it is the NiCl of 0.76mol/L by 70mL molar concentrations2Solution and 30mL molar concentrations are 0.47mol/L's PbCl2Solution is added in mixed liquor T1, is stirred 3 minutes under the conditions of 1000r/min, obtains mixed liquor U1；
(43) 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 washed through the ethanol that 100mL mass percent concentrations are 84% after at 68 DEG C Drying box in place 156 minutes, be subsequently placed in Muffle furnace and be calcined 240 minutes under the conditions of 146 DEG C, obtain material K1；
(44) it is the NiCl of 0.66mol/L by 60mL molar concentrations2Solution and 40mL molar concentrations are 0.57mol/L's PbCl2Solution is added in mixed liquor T2, is stirred 3 minutes under the conditions of 1000r/min, obtains mixed liquor U2；
(45) 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 after the ethanol washing that 100mL mass percent concentrations are 84% 68 DEG C drying box in place 156 minutes, be subsequently placed in Muffle furnace and be calcined 240 minutes under the conditions of 146 DEG C, obtain material K2；
(46) it is the NiCl of 0.56mol/L by 50mL molar concentrations2Solution and 50mL molar concentrations are 0.67mol/L's PbCl2Solution is added in mixed liquor T3, is stirred 3 minutes under the conditions of 1000r/min, obtains mixed liquor U3；
(47) 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 after the ethanol washing that 100mL mass percent concentrations are 84% 68 DEG C drying box in place 156 minutes, be subsequently placed in Muffle furnace and be calcined 240 minutes under the conditions of 146 DEG C, obtain material K3；
(48) it is the NiCl of 0.46mol/L by 40mL molar concentrations2Solution and 60mL molar concentrations are 0.77mol/L's PbCl2Solution is added in mixed liquor T4, is stirred 3 minutes under the conditions of 1000r/min, obtains mixed liquor U4；
(49) 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 after the ethanol washing that 100mL mass percent concentrations are 84% 68 DEG C drying box in place 156 minutes, be subsequently placed in Muffle furnace and be calcined 240 minutes under the conditions of 146 DEG C, obtain material K4；
(50) it is the NiCl of 0.36mol/L by 30mL molar concentrations2Solution and 70mL molar concentrations are 0.87mol/L's PbCl2Solution is added in mixed liquor T5, is stirred 3 minutes under the conditions of 1000r/min, obtains mixed liquor U5；
(51) material K4 is added in mixed liquor U5, 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 J5, material J5 is after the ethanol washing that 100mL mass percent concentrations are 84% 68 DEG C drying box in place 156 minutes, be subsequently placed in Muffle furnace and be calcined 240 minutes under the conditions of 146 DEG C, obtain material K；
(52) 9.66g polyvinyl alcohol and 900mL deionized waters are added to volume in 1000mL conical flasks, in 1000r/ Stirred 3 minutes under the conditions of min, 3 parts of equivalent is divided into after shaking up, obtain mixed liquor V1, mixed liquor V2, mixed liquor V3；
(53) it is the HAuCl of 0.89mol/L by 95mL molar concentrations4Solution is added in mixed liquor V1, in 1000r/min Under the conditions of stir 3 minutes, obtain mixed liquor W1；
(54) 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 washed through the ethanol that 100mL mass percent concentrations are 84% after at 68 DEG C Drying box in place 156 minutes, be subsequently placed in Muffle furnace and be calcined 240 minutes under the conditions of 146 DEG C, obtain material Z1；
(55) it is the HAuCl of 0.69mol/L by 65mL molar concentrations4Solution is added in mixed liquor V2, in 1000r/min Under the conditions of stir 3 minutes, obtain mixed liquor W2；
(56) 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 after the ethanol washing that 100mL mass percent concentrations are 84% 68 DEG C drying box in place 156 minutes, be subsequently placed in Muffle furnace and be calcined 240 minutes under the conditions of 146 DEG C, obtain material Z2；
(57) it is the HAuCl of 0.49mol/L by 35mL molar concentrations4Solution is added in mixed liquor V3, in 1000r/min Under the conditions of stir 3 minutes, obtain mixed liquor W3；
(58) 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 after the ethanol washing that 100mL mass percent concentrations are 84% 68 DEG C drying box in place 156 minutes, be subsequently placed in Muffle furnace and be calcined 240 minutes under the conditions of 146 DEG C, the material for obtaining is i.e. It is the Modified Activated Carbon aerogel particles electrode that benzoquinones function is removed with electro-catalysis.
The beneficial effects of the invention are as follows the obtained Modified Activated Carbon aerogel particles electrode that benzoquinones function is removed with electro-catalysis With current efficiency it is high, stability is strong, electrode life is long, 1,4-benzoquinone removal efficiency is high the features such as.
Specific embodiment
The present invention provides a kind of Modified Activated Carbon aerogel particles electrode with electro-catalysis removal benzoquinones function and preparation method, Illustrate to apply process in fact below by an example.
Embodiment 1.
(1) the 94g carbon aerogel particles that particle diameter is 4~6mm are washed with 1000mL deionized waters, is then placed in 500mL 8h is soaked in chloroform, is washed with 1000mL deionized waters after taking-up, then be 95% with 1000mL mass percent concentrations 1.5h is placed in 85 DEG C of drying box after ethanol washing, substance A 1 is obtained；
(2) 8.29 grams of platinum nitrates and 800mL deionized waters are added to volume in 1000mL conical flasks, in 1000r/ Stirred 3 minutes under the conditions of min, add 15mL concentrated nitric acids, 4 parts of equivalent is divided into after shaking up, obtained mixed liquor K1, mixed liquor K2, mix Close liquid K3, mixed liquor K4；
(3) by 910 milligrams of Al (NO3)3It is the AgNO of 0.86mol/L with 85mL molar concentrations3Solution is added to mixed liquor K1 In, stirred 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 washed through the ethanol that 100mL mass percent concentrations are 84% after at 68 DEG C Drying box in place 156 minutes, be subsequently placed in Muffle furnace and be calcined 240 minutes under the conditions of 146 DEG C, obtain substance A 3；
(5) by 930 milligrams of Al (NO3)3It is the AgNO of 0.76mol/L with 75mL molar concentrations3Solution is added to mixed liquor K2 In, stirred 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 washed through the ethanol that 100mL mass percent concentrations are 84% after at 68 DEG C Drying box in place 156 minutes, be subsequently placed in Muffle furnace and be calcined 240 minutes under the conditions of 146 DEG C, obtain substance A 5；
(7) by 950 milligrams of Al (NO3)3It is the AgNO of 0.66mol/L with 65mL molar concentrations3Solution is added to mixed liquor K3 In, stirred 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 washed through the ethanol that 100mL mass percent concentrations are 84% after at 68 DEG C Drying box in place 156 minutes, be subsequently placed in Muffle furnace and be calcined 240 minutes under the conditions of 146 DEG C, obtain substance A 7；
(9) by 970 milligrams of Al (NO3)3It is the AgNO of 0.56mol/L with 55mL molar concentrations3Solution is added to mixed liquor K4 In, stirred 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 after the ethanol washing that 100mL mass percent concentrations are 84% 68 DEG C drying box in place 156 minutes, be subsequently placed in Muffle furnace and be calcined 240 minutes under the conditions of 146 DEG C, obtain substance A；
(11) by 4.37 grams of AgNO3Volume is added to in 1000mL conical flasks with 850mL ether, in 1000r/min bars Stirred 3 minutes under part, 5 parts of equivalent is divided into after shaking up, obtain mixed liquor M1, mixed liquor M2, mixed liquor M3, mixed liquor M4, mixing Liquid M5；
(12) by 218 milligrams of AgNO3It is the Al (NO of 0.95mol/L with 75mL molar concentrations3)3Solution is added to mixed liquor In M1, stirred 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 washed through the ethanol that 100mL mass percent concentrations are 84% after at 68 DEG C Placed 156 minutes in drying box, be subsequently placed in Muffle furnace and be calcined 240 minutes under the conditions of 146 DEG C, obtain substance B 1；
(14) by 238 milligrams of AgNO3It is the Al (NO of 0.85mol/L with 65mL molar concentrations3)3Solution is added to mixed liquor In M2, stirred 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 after the ethanol washing that 100mL mass percent concentrations are 84% 68 DEG C drying box in place 156 minutes, be subsequently placed in Muffle furnace and be calcined 240 minutes under the conditions of 146 DEG C, obtain substance B 3；
(16) by 258 milligrams of AgNO3It is the Al (NO of 0.75mol/L with 55mL molar concentrations3)3Solution is added to mixed liquor In M3, stirred 3 minutes under the conditions of 1000r/min, obtain mixed liquor N3；
(17) substance B 3 is added in mixed liquor N3, 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 4, substance B 4 is after the ethanol washing that 100mL mass percent concentrations are 84% 68 DEG C drying box in place 156 minutes, be subsequently placed in Muffle furnace and be calcined 240 minutes under the conditions of 146 DEG C, obtain substance B 5；
(18) by 278 milligrams of AgNO3It is the Al (NO of 0.65mol/L with 45mL molar concentrations3)3Solution is added to mixed liquor In M4, stirred 3 minutes under the conditions of 1000r/min, obtain mixed liquor N4；
(19) substance B 5 is added in mixed liquor N4, 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 6, substance B 6 is after the ethanol washing that 100mL mass percent concentrations are 84% 68 DEG C drying box in place 156 minutes, be subsequently placed in Muffle furnace and be calcined 240 minutes under the conditions of 146 DEG C, obtain substance C；
(20) by 298 milligrams of AgNO3It is the Al (NO of 0.55mol/L with 35mL molar concentrations3)3Solution is added to mixed liquor In M5, stirred 3 minutes under the conditions of 1000r/min, obtain mixed liquor N5；
(21) substance C is added in mixed liquor N5, 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 washed through the ethanol that 100mL mass percent concentrations are 84% after at 68 DEG C Placed 156 minutes in drying box, be subsequently placed in Muffle furnace and be calcined 240 minutes under the conditions of 146 DEG C, obtain material E；
(22) by 6.33 grams of Mn (NO3)2Volume is added to in 1000mL conical flasks with 850mL ethanol, in 1000r/min Under the conditions of stir 3 minutes, add 5mL concentrated nitric acids, 5 parts of equivalent is divided into after shaking up, obtain mixed liquor P1, mixed liquor P2, mixed liquor P3, mixed liquor P4, mixed liquor P5；
(23) it is the SbCl of 0.69mol/L by 95mL molar concentrations3Solution is added in mixed liquor P1, in 1000r/min Under the conditions of stir 3 minutes, obtain mixed liquor Q1；
(24) 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 washed through the ethanol that 100mL mass percent concentrations are 84% after at 68 DEG C Drying box in place 156 minutes, be subsequently placed in Muffle furnace and be calcined 240 minutes under the conditions of 146 DEG C, obtain material F2；
(25) it is the Mn (NO of 0.92mol/L by 80mL molar concentrations3)2Solution is added in mixed liquor P2, in 1000r/ Stirred 3 minutes under the conditions of min, obtain mixed liquor Q2；
(26) 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 after the ethanol washing that 100mL mass percent concentrations are 84% 68 DEG C drying box in place 156 minutes, be subsequently placed in Muffle furnace and be calcined 240 minutes under the conditions of 146 DEG C, obtain material F4；
(27) it is the SbCl of 0.59mol/L by 80mL molar concentrations3Solution is added in mixed liquor P3, in 1000r/min Under the conditions of stir 3 minutes, obtain mixed liquor Q3；
(28) 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 after the ethanol washing that 100mL mass percent concentrations are 84% 68 DEG C drying box in place 156 minutes, be subsequently placed in Muffle furnace and be calcined 240 minutes under the conditions of 146 DEG C, obtain material F6；
(29) it is the Mn (NO of 0.72mol/L by 60mL molar concentrations3)2Solution is added in mixed liquor P4, in 1000r/ Stirred 3 minutes under the conditions of min, obtain mixed liquor Q4；
(30) material F6 is added in mixed liquor Q4, 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 F7, material F7 is after the ethanol washing that 100mL mass percent concentrations are 84% 68 DEG C drying box in place 156 minutes, be subsequently placed in Muffle furnace and be calcined 240 minutes under the conditions of 146 DEG C, obtain material F8；
(31) it is the SbCl of 0.49mol/L by 65mL molar concentrations3Solution and 40mL molar concentrations are the Mn of 0.52mol/L (NO3)2Solution is added in mixed liquor P5, is stirred 3 minutes under the conditions of 1000r/min, obtains mixed liquor Q5；
(32) material F8 is added in mixed liquor Q5, 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 F9, material F9 is after the ethanol washing that 100mL mass percent concentrations are 84% 68 DEG C drying box in place 156 minutes, be subsequently placed in Muffle furnace and be calcined 240 minutes under the conditions of 146 DEG C, obtain material F；
(33) by 6.57g ZrCl4Volume is added to the sodium citrate solution that 750mL mass percent concentrations are 10% In for 1000mL conical flasks, stirred 3 minutes under the conditions of 1000r/min, 3 parts of equivalent is divided into after shaking up, obtained mixed liquor R1, mix Close liquid R2, mixed liquor R3；
(34) it is the NiCl of 0.38mol/L by 40mL molar concentrations2Solution and 60mL molar concentrations are 0.84mol/L's PbCl2Solution is added in mixed liquor R1, is stirred 3 minutes under the conditions of 1000r/min, obtains mixed liquor S1；
(35) 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 washed through the ethanol that 100mL mass percent concentrations are 84% after at 68 DEG C Drying box in place 156 minutes, be subsequently placed in Muffle furnace and be calcined 240 minutes under the conditions of 146 DEG C, obtain material H1；
(36) it is the NiCl of 0.58mol/L by 50mL molar concentrations2Solution and 50mL molar concentrations are 0.64mol/L's PbCl2Solution is added in mixed liquor R2, is stirred 3 minutes under the conditions of 1000r/min, obtains mixed liquor S2；
(37) 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 after the ethanol washing that 100mL mass percent concentrations are 84% 68 DEG C drying box in place 156 minutes, be subsequently placed in Muffle furnace and be calcined 240 minutes under the conditions of 146 DEG C, obtain material H2；
(38) it is the NiCl of 0.78mol/L by 60mL molar concentrations2Solution and 40mL molar concentrations are 0.44mol/L's PbCl2Solution is added in mixed liquor R3, is stirred 3 minutes under the conditions of 1000r/min, obtains mixed liquor S3；
(39) 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 after the ethanol washing that 100mL mass percent concentrations are 84% 68 DEG C drying box in place 156 minutes, be subsequently placed in Muffle furnace and be calcined 240 minutes under the conditions of 146 DEG C, obtain material H；
(40) 3.28g lauryl sodium sulfate, 40mL n-hexanes, 20 milliliters of n-butanols are added sequentially to volume and are In 250mL conical flasks, 7.49g 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, shaken in the shaking table that temperature is 45 DEG C 0.5h, 15min is centrifuged after being cooled to room temperature under the conditions of 7500r/min, removes supernatant, uses 500mL mass percent concentrations Ethanol for 95% is washed, and obtains material I；
(41) sodium citrate solution that material I and 850mL mass percent concentration is 15% is added into volume is In 1000mL conical flasks, stirred 3 minutes under the conditions of 1000r/min, 5 parts of equivalent is divided into after shaking up, obtain mixed liquor T1, mixing Liquid T2, mixed liquor T3, mixed liquor T4, mixed liquor T5；
(42) it is the NiCl of 0.76mol/L by 70mL molar concentrations2Solution and 30mL molar concentrations are 0.47mol/L's PbCl2Solution is added in mixed liquor T1, is stirred 3 minutes under the conditions of 1000r/min, obtains mixed liquor U1；
(43) 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 washed through the ethanol that 100mL mass percent concentrations are 84% after at 68 DEG C Drying box in place 156 minutes, be subsequently placed in Muffle furnace and be calcined 240 minutes under the conditions of 146 DEG C, obtain material K1；
(44) it is the NiCl of 0.66mol/L by 60mL molar concentrations2Solution and 40mL molar concentrations are 0.57mol/L's PbCl2Solution is added in mixed liquor T2, is stirred 3 minutes under the conditions of 1000r/min, obtains mixed liquor U2；
(45) 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 after the ethanol washing that 100mL mass percent concentrations are 84% 68 DEG C drying box in place 156 minutes, be subsequently placed in Muffle furnace and be calcined 240 minutes under the conditions of 146 DEG C, obtain material K2；
(46) it is the NiCl of 0.56mol/L by 50mL molar concentrations2Solution and 50mL molar concentrations are 0.67mol/L's PbCl2Solution is added in mixed liquor T3, is stirred 3 minutes under the conditions of 1000r/min, obtains mixed liquor U3；
(47) 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 after the ethanol washing that 100mL mass percent concentrations are 84% 68 DEG C drying box in place 156 minutes, be subsequently placed in Muffle furnace and be calcined 240 minutes under the conditions of 146 DEG C, obtain material K3；
(48) it is the NiCl of 0.46mol/L by 40mL molar concentrations2Solution and 60mL molar concentrations are 0.77mol/L's PbCl2Solution is added in mixed liquor T4, is stirred 3 minutes under the conditions of 1000r/min, obtains mixed liquor U4；
(49) 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 after the ethanol washing that 100mL mass percent concentrations are 84% 68 DEG C drying box in place 156 minutes, be subsequently placed in Muffle furnace and be calcined 240 minutes under the conditions of 146 DEG C, obtain material K4；
(50) it is the NiCl of 0.36mol/L by 30mL molar concentrations2Solution and 70mL molar concentrations are 0.87mol/L's PbCl2Solution is added in mixed liquor T5, is stirred 3 minutes under the conditions of 1000r/min, obtains mixed liquor U5；
(51) material K4 is added in mixed liquor U5, 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 J5, material J5 is after the ethanol washing that 100mL mass percent concentrations are 84% 68 DEG C drying box in place 156 minutes, be subsequently placed in Muffle furnace and be calcined 240 minutes under the conditions of 146 DEG C, obtain material K；
(52) 9.66g polyvinyl alcohol and 900mL deionized waters are added to volume in 1000mL conical flasks, in 1000r/ Stirred 3 minutes under the conditions of min, 3 parts of equivalent is divided into after shaking up, obtain mixed liquor V1, mixed liquor V2, mixed liquor V3；
(53) it is the HAuCl of 0.89mol/L by 95mL molar concentrations4Solution is added in mixed liquor V1, in 1000r/min Under the conditions of stir 3 minutes, obtain mixed liquor W1；
(54) 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 washed through the ethanol that 100mL mass percent concentrations are 84% after at 68 DEG C Drying box in place 156 minutes, be subsequently placed in Muffle furnace and be calcined 240 minutes under the conditions of 146 DEG C, obtain material Z1；
(55) it is the HAuCl of 0.69mol/L by 65mL molar concentrations4Solution is added in mixed liquor V2, in 1000r/min Under the conditions of stir 3 minutes, obtain mixed liquor W2；
(56) 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 after the ethanol washing that 100mL mass percent concentrations are 84% 68 DEG C drying box in place 156 minutes, be subsequently placed in Muffle furnace and be calcined 240 minutes under the conditions of 146 DEG C, obtain material Z2；
(57) it is the HAuCl of 0.49mol/L by 35mL molar concentrations4Solution is added in mixed liquor V3, in 1000r/min Under the conditions of stir 3 minutes, obtain mixed liquor W3；
(58) 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 after the ethanol washing that 100mL mass percent concentrations are 84% 68 DEG C drying box in place 156 minutes, be subsequently placed in Muffle furnace and be calcined 240 minutes under the conditions of 146 DEG C, the material for obtaining is i.e. It is the Modified Activated Carbon aerogel particles electrode that benzoquinones function is removed with electro-catalysis.
Here is with the obtained Modified Activated Carbon aerogel particles electricity with electro-catalysis removal benzoquinones function of the inventive method Pole has carried out Electro-catalytic Oxidation Process experiment in electric catalysis reactor to the waste water containing benzoquinones, further illustrates the present invention.
The Modified Activated Carbon aerogel particles electrode will obtained in the inventive method with electro-catalysis removal benzoquinones function is seated in In electric catalysis reactor, Degrading experiment is carried out to the waste water containing benzoquinones, as a result shown that the electro-catalysis loaded by the electrode is anti- Answering device can efficiently remove the benzoquinones in waste water, be 5.0 in pH when the benzoquinones concentration in waste water is 44.9mg/L, and voltage is 14V, process time is under the conditions of 45min, the benzoquinones concentration after treatment in water outlet is reduced to 3.5mg/L, and treatment effeciency reaches 92.20%.

Claims (1)

1. it is a kind of with electro-catalysis removal benzoquinones function Modified Activated Carbon aerogel particles electrode preparation method, it is characterised in that The method is comprised the following steps that：
(1) the 94g carbon aerogel particles that particle diameter is 4~6mm are washed with 1000mL deionized waters, is then placed in 500mL trichlorines 8h is soaked in methane, is washed with 1000mL deionized waters after taking-up, then with the ethanol that 1000mL mass percent concentrations are 95% 1.5h is placed in 85 DEG C of drying box after washing, substance A 1 is obtained；
(2) 8.29 grams of platinum nitrates and 800mL deionized waters are added to volume in 1000mL conical flasks, in 1000r/min bars Stirred 3 minutes under part, add 15mL concentrated nitric acids, 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 910 milligrams of Al (NO3)3It is the AgNO of 0.86mol/L with 85mL molar concentrations3Solution is added in mixed liquor K1, Stirred 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 68 DEG C after being washed through the ethanol that 100mL mass percent concentrations are 84% Placed 156 minutes in dry case, be subsequently placed in Muffle furnace and be calcined 240 minutes under the conditions of 146 DEG C, obtain substance A 3；
(5) by 930 milligrams of Al (NO3)3It is the AgNO of 0.76mol/L with 75mL molar concentrations3Solution is added in mixed liquor K2, Stirred 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 68 DEG C after being washed through the ethanol that 100mL mass percent concentrations are 84% Placed 156 minutes in dry case, be subsequently placed in Muffle furnace and be calcined 240 minutes under the conditions of 146 DEG C, obtain substance A 5；
(7) by 950 milligrams of Al (NO3)3It is the AgNO of 0.66mol/L with 65mL molar concentrations3Solution is added in mixed liquor K3, Stirred 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 68 DEG C after being washed through the ethanol that 100mL mass percent concentrations are 84% Placed 156 minutes in dry case, be subsequently placed in Muffle furnace and be calcined 240 minutes under the conditions of 146 DEG C, obtain substance A 7；
(9) by 970 milligrams of Al (NO3)3It is the AgNO of 0.56mol/L with 55mL molar concentrations3Solution is added in mixed liquor K4, Stirred 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 after the ethanol washing that 100mL mass percent concentrations are 84% at 68 DEG C Placed 156 minutes in drying box, be subsequently placed in Muffle furnace and be calcined 240 minutes under the conditions of 146 DEG C, obtain substance A；
(11) by 4.37 grams of AgNO3Volume is added in 1000mL conical flasks, to be stirred under the conditions of 1000r/min with 850mL ether Mix 3 minutes, 5 parts of equivalent is divided into after shaking up, obtain mixed liquor M1, mixed liquor M2, mixed liquor M3, mixed liquor M4, mixed liquor M5；
(12) by 218 milligrams of AgNO3It is the Al (NO of 0.95mol/L with 75mL molar concentrations3)3Solution is added in mixed liquor M1, Stirred 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 washed through the ethanol that 100mL mass percent concentrations are 84% after in 68 DEG C of drying Placed 156 minutes in case, be subsequently placed in Muffle furnace and be calcined 240 minutes under the conditions of 146 DEG C, obtain substance B 1；
(14) by 238 milligrams of AgNO3It is the Al (NO of 0.85mol/L with 65mL molar concentrations3)3Solution is added in mixed liquor M2, Stirred 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 after the ethanol washing that 100mL mass percent concentrations are 84% at 68 DEG C Placed 156 minutes in drying box, be subsequently placed in Muffle furnace and be calcined 240 minutes under the conditions of 146 DEG C, obtain substance B 3；
(16) by 258 milligrams of AgNO3It is the Al (NO of 0.75mol/L with 55mL molar concentrations3)3Solution is added in mixed liquor M3, Stirred 3 minutes under the conditions of 1000r/min, obtain mixed liquor N3；
(17) substance B 3 is added in mixed liquor N3, 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 4, substance B 4 is after the ethanol washing that 100mL mass percent concentrations are 84% at 68 DEG C Placed 156 minutes in drying box, be subsequently placed in Muffle furnace and be calcined 240 minutes under the conditions of 146 DEG C, obtain substance B 5；
(18) by 278 milligrams of AgNO3It is the Al (NO of 0.65mol/L with 45mL molar concentrations3)3Solution is added in mixed liquor M4, Stirred 3 minutes under the conditions of 1000r/min, obtain mixed liquor N4；
(19) substance B 5 is added in mixed liquor N4, 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 6, substance B 6 is after the ethanol washing that 100mL mass percent concentrations are 84% at 68 DEG C Placed 156 minutes in drying box, be subsequently placed in Muffle furnace and be calcined 240 minutes under the conditions of 146 DEG C, obtain substance C；
(20) by 298 milligrams of AgNO3It is the Al (NO of 0.55mol/L with 35mL molar concentrations3)3Solution is added in mixed liquor M5, Stirred 3 minutes under the conditions of 1000r/min, obtain mixed liquor N5；
(21) substance C is added in mixed liquor N5, 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 washed through the ethanol that 100mL mass percent concentrations are 84% after in 68 DEG C of drying Placed 156 minutes in case, be subsequently placed in Muffle furnace and be calcined 240 minutes under the conditions of 146 DEG C, obtain material E；
(22) by 6.33 grams of Mn (NO3)2Volume is added to in 1000mL conical flasks with 850mL ethanol, in 1000r/min conditions Lower stirring 3 minutes, adds 5mL concentrated nitric acids, and 5 parts of equivalent is divided into after shaking up, and obtains mixed liquor P1, mixed liquor P2, mixed liquor P3, mixed Close liquid P4, mixed liquor P5；
(23) it is the SbCl of 0.69mol/L by 95mL molar concentrations3Solution is added in mixed liquor P1, under the conditions of 1000r/min Stirring 3 minutes, obtains mixed liquor Q1；
(24) 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 68 DEG C after being washed through the ethanol that 100mL mass percent concentrations are 84% Placed 156 minutes in dry case, be subsequently placed in Muffle furnace and be calcined 240 minutes under the conditions of 146 DEG C, obtain material F2；
(25) it is the Mn (NO of 0.92mol/L by 80mL molar concentrations3)2Solution is added in mixed liquor P2, in 1000r/min bars Stirred 3 minutes under part, obtain mixed liquor Q2；
(26) 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 after the ethanol washing that 100mL mass percent concentrations are 84% at 68 DEG C Placed 156 minutes in drying box, be subsequently placed in Muffle furnace and be calcined 240 minutes under the conditions of 146 DEG C, obtain material F4；
(27) it is the SbCl of 0.59mol/L by 80mL molar concentrations3Solution is added in mixed liquor P3, under the conditions of 1000r/min Stirring 3 minutes, obtains mixed liquor Q3；
(28) 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 after the ethanol washing that 100mL mass percent concentrations are 84% at 68 DEG C Placed 156 minutes in drying box, be subsequently placed in Muffle furnace and be calcined 240 minutes under the conditions of 146 DEG C, obtain material F6；
(29) it is the Mn (NO of 0.72mol/L by 60mL molar concentrations3)2Solution is added in mixed liquor P4, in 1000r/min bars Stirred 3 minutes under part, obtain mixed liquor Q4；
(30) material F6 is added in mixed liquor Q4, 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 F7, material F7 is after the ethanol washing that 100mL mass percent concentrations are 84% at 68 DEG C Placed 156 minutes in drying box, be subsequently placed in Muffle furnace and be calcined 240 minutes under the conditions of 146 DEG C, obtain material F8；
(31) it is the SbCl of 0.49mol/L by 65mL molar concentrations3Solution and 40mL molar concentrations are the Mn of 0.52mol/L (NO3)2Solution is added in mixed liquor P5, is stirred 3 minutes under the conditions of 1000r/min, obtains mixed liquor Q5；
(32) material F8 is added in mixed liquor Q5, 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 F9, material F9 is after the ethanol washing that 100mL mass percent concentrations are 84% at 68 DEG C Placed 156 minutes in drying box, be subsequently placed in Muffle furnace and be calcined 240 minutes under the conditions of 146 DEG C, obtain material F；
(33) by 6.57g ZrCl4Being added to volume with the sodium citrate solution that 750mL mass percent concentrations are 10% is In 1000mL conical flasks, stirred 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；
(34) it is the NiCl of 0.38mol/L by 40mL molar concentrations2Solution and 60mL molar concentrations are the PbCl of 0.84mol/L2It is molten Liquid is added in mixed liquor R1, is stirred 3 minutes under the conditions of 1000r/min, obtains mixed liquor S1；
(35) 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 68 DEG C after being washed through the ethanol that 100mL mass percent concentrations are 84% Placed 156 minutes in dry case, be subsequently placed in Muffle furnace and be calcined 240 minutes under the conditions of 146 DEG C, obtain material H1；
(36) it is the NiCl of 0.58mol/L by 50mL molar concentrations2Solution and 50mL molar concentrations are the PbCl of 0.64mol/L2It is molten Liquid is added in mixed liquor R2, is stirred 3 minutes under the conditions of 1000r/min, obtains mixed liquor S2；
(37) 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 after the ethanol washing that 100mL mass percent concentrations are 84% at 68 DEG C Placed 156 minutes in drying box, be subsequently placed in Muffle furnace and be calcined 240 minutes under the conditions of 146 DEG C, obtain material H2；
(38) it is the NiCl of 0.78mol/L by 60mL molar concentrations2Solution and 40mL molar concentrations are the PbCl of 0.44mol/L2It is molten Liquid is added in mixed liquor R3, is stirred 3 minutes under the conditions of 1000r/min, obtains mixed liquor S3；
(39) 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 after the ethanol washing that 100mL mass percent concentrations are 84% at 68 DEG C Placed 156 minutes in drying box, be subsequently placed in Muffle furnace and be calcined 240 minutes under the conditions of 146 DEG C, obtain material H；
(40) 3.28g lauryl sodium sulfate, 40mL n-hexanes, 20 milliliters of n-butanols are added sequentially to volume for 250mL is bored In shape bottle, 7.49g 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 subsequently adding the hydrochloric acid solution that 25mL molar concentrations are 2.40mol/L, and 0.5h is shaken in the shaking table that temperature is 45 DEG C, cold But to 15min is centrifuged after room temperature under the conditions of 7500r/min, supernatant is removed, is 95% with 500mL mass percent concentrations Ethanol is washed, and obtains material I；
(41) sodium citrate solution that material I and 850mL mass percent concentration is 15% is added to volume for 1000mL is bored In shape bottle, stirred 3 minutes under the conditions of 1000r/min, 5 parts of equivalent is divided into after shaking up, obtained mixed liquor T1, mixed liquor T2, mix Close liquid T3, mixed liquor T4, mixed liquor T5；
(42) it is the NiCl of 0.76mol/L by 70mL molar concentrations2Solution and 30mL molar concentrations are the PbCl of 0.47mol/L2It is molten Liquid is added in mixed liquor T1, is stirred 3 minutes under the conditions of 1000r/min, obtains mixed liquor U1；
(43) 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 68 DEG C after being washed through the ethanol that 100mL mass percent concentrations are 84% Placed 156 minutes in dry case, be subsequently placed in Muffle furnace and be calcined 240 minutes under the conditions of 146 DEG C, obtain material K1；
(44) it is the NiCl of 0.66mol/L by 60mL molar concentrations2Solution and 40mL molar concentrations are the PbCl of 0.57mol/L2It is molten Liquid is added in mixed liquor T2, is stirred 3 minutes under the conditions of 1000r/min, obtains mixed liquor U2；
(45) 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 after the ethanol washing that 100mL mass percent concentrations are 84% at 68 DEG C Placed 156 minutes in drying box, be subsequently placed in Muffle furnace and be calcined 240 minutes under the conditions of 146 DEG C, obtain material K2；
(46) it is the NiCl of 0.56mol/L by 50mL molar concentrations2Solution and 50mL molar concentrations are the PbCl of 0.67mol/L2It is molten Liquid is added in mixed liquor T3, is stirred 3 minutes under the conditions of 1000r/min, obtains mixed liquor U3；
(47) 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 after the ethanol washing that 100mL mass percent concentrations are 84% at 68 DEG C Placed 156 minutes in drying box, be subsequently placed in Muffle furnace and be calcined 240 minutes under the conditions of 146 DEG C, obtain material K3；
(48) it is the NiCl of 0.46mol/L by 40mL molar concentrations2Solution and 60mL molar concentrations are the PbCl of 0.77mol/L2It is molten Liquid is added in mixed liquor T4, is stirred 3 minutes under the conditions of 1000r/min, obtains mixed liquor U4；
(49) 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 after the ethanol washing that 100mL mass percent concentrations are 84% at 68 DEG C Placed 156 minutes in drying box, be subsequently placed in Muffle furnace and be calcined 240 minutes under the conditions of 146 DEG C, obtain material K4；
(50) it is the NiCl of 0.36mol/L by 30mL molar concentrations2Solution and 70mL molar concentrations are the PbCl of 0.87mol/L2It is molten Liquid is added in mixed liquor T5, is stirred 3 minutes under the conditions of 1000r/min, obtains mixed liquor U5；
(51) material K4 is added in mixed liquor U5, 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 J5, material J5 is after the ethanol washing that 100mL mass percent concentrations are 84% at 68 DEG C Placed 156 minutes in drying box, be subsequently placed in Muffle furnace and be calcined 240 minutes under the conditions of 146 DEG C, obtain material K；
(52) 9.66g polyvinyl alcohol and 900mL deionized waters are added to volume in 1000mL conical flasks, in 1000r/min Under the conditions of stir 3 minutes, 3 parts of equivalent is divided into after shaking up, obtain mixed liquor V1, mixed liquor V2, mixed liquor V3；
(53) it is the HAuCl of 0.89mol/L by 95mL molar concentrations4Solution is added in mixed liquor V1, in 1000r/min conditions Lower stirring 3 minutes, obtains mixed liquor W1；
(54) 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 68 DEG C after being washed through the ethanol that 100mL mass percent concentrations are 84% Placed 156 minutes in dry case, be subsequently placed in Muffle furnace and be calcined 240 minutes under the conditions of 146 DEG C, obtain material Z1；
(55) it is the HAuCl of 0.69mol/L by 65mL molar concentrations4Solution is added in mixed liquor V2, in 1000r/min conditions Lower stirring 3 minutes, obtains mixed liquor W2；
(56) 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 after the ethanol washing that 100mL mass percent concentrations are 84% at 68 DEG C Placed 156 minutes in drying box, be subsequently placed in Muffle furnace and be calcined 240 minutes under the conditions of 146 DEG C, obtain material Z2；
(57) it is the HAuCl of 0.49mol/L by 35mL molar concentrations4Solution is added in mixed liquor V3, in 1000r/min conditions Lower stirring 3 minutes, obtains mixed liquor W3；
(58) 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 after the ethanol washing that 100mL mass percent concentrations are 84% at 68 DEG C Placed 156 minutes in drying box, be subsequently placed in Muffle furnace and be calcined 240 minutes under the conditions of 146 DEG C, the material for obtaining is tool There is electro-catalysis to remove the Modified Activated Carbon aerogel particles electrode of benzoquinones function.
CN201611055948.2A 2016-11-21 2016-11-21 Modified Activated Carbon aerogel particles electrode and preparation method with electro-catalysis removal benzoquinones function Withdrawn CN106745527A (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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