CN106430459A - Modified activated carbon particle electrode with function using electro-catalysis to remove indole and preparation method - Google Patents

Modified activated carbon particle electrode with function using electro-catalysis to remove indole and preparation method Download PDF

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CN106430459A
CN106430459A CN201611043591.6A CN201611043591A CN106430459A CN 106430459 A CN106430459 A CN 106430459A CN 201611043591 A CN201611043591 A CN 201611043591A CN 106430459 A CN106430459 A CN 106430459A
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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
    • C02F1/467—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
    • 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
    • C02F1/46104—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

Abstract

The invention discloses a modified activated carbon particle electrode with a function using electro-catalysis to remove indole and a preparation method. The preparation method includes: preparing activated carbon particles, trichloromethane and ethanol into a substance A; by the substance A, modifying mixed liquid prepared by AgNO3, ethyl ether and PtCl4 to prepare a substance E; by the substance E, modifying mixed liquid prepared by Ce(NO3)2, ethanol, Fe(NO3)3, sodium citrate, CoCl2 and NiCl2 to prepare a substance H; by the substance H, modifying mixed liquid prepared by lauryl sodium sulfate, n-hexane, 2-methyl-2-butanol, sodium metavanadate, sodium citrate, CoCl2 and NiCl2 to prepare a substance K; by the substance K, modifying mixed liquid prepared by N-vinyl caprolactam and HAuCl4 to obtain a substance, namely the modified activated carbon particle electrode with the function using electro-catalysis to remove indole.

Description

There is modified activated carbon granule electrode and the preparation method that electro-catalysis removes indole function
Technical field
The invention belongs to organic wastewater with difficult degradation thereby Electrocatalytic Oxidation processing technology field, particularly to one kind, there is electricity and urge Change the modified activated carbon granule electrode removing indole function and preparation method.
Background technology
Electro-catalytic oxidation technology is the very promising water technology of the one kind gradually growing up in recent years, mainly The active group by producing hydroxyl radical free radical etc. with strong oxidizing property carries out oxidative degradation to the organic pollution in waste water, can So that hardly degraded organic substance or bio-toxicity pollutant be converted into biodegradable or innocuous substance, that improves waste water can be biochemical Property, thus beneficial to follow-up biological treatment.Therefore, electrocatalytic oxidation water technology is processing high concentration, bio-refractory work Industry waste water aspect has the features such as 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 of electro-catalytic oxidation technology and operating cost, because This exploration and the electrocatalysis material preparing good combination property are the research emphasis of current electro-catalytic oxidation technology.But traditional electrode The resistance of material is larger, conductivity is low so that its current efficiency is low in the treatment of waste water, stability not, short life, electrode material Material is relatively costly, limits popularization and application in water process for the electro-catalytic oxidation technology and development, so new electrode materials Research also needs to strengthen further with preparation.Also lack at present and there is to indole specific pollutants efficient electric catalytic elimination function Electrode material and preparation method.
Content of the invention
It is an object of the invention to provide a kind of have modified activated carbon granule electrode and the system that electro-catalysis removes indole function Preparation Method, the comprising the following steps that of its preparation method：
(1) the activated carbon granule 1000mL deionized water wash for 4-6mm by 150g particle diameter, is then placed in 500mL tri- Soak 8h in chloromethanes, after taking-up, use 1000mL deionized water wash, then the second being 95% with 1000mL mass percent concentration Place 2h in 85 DEG C of drying baker after alcohol washing, obtain substance A；
(2) by 1.23 grams of AgNO3Being added to volume with 800mL ether is in 1000mL conical flask, in 1000r/min condition Lower stirring 5 minutes, is divided into 4 parts of equivalent, obtains mixed liquor M1, mixed liquor M2, mixed liquor M3, mixed liquor M4 after shaking up；
(3) by 262 milligrams of PtCl4It is added in mixed liquor M1, stir 5 minutes under the conditions of 1000r/min, mixed Liquid N1；
(4) AgNO for 0.5mol/L by 10mL mixed liquor N1 and 10mL molar concentration3Solution is added in mixed liquor M2, Stir 5 minutes under the conditions of 1000r/min, obtain mixed liquor N2；
(5) substance A is added in mixed liquor N2, temperature be 40 DEG C shaking table in shake 0.5h, after being cooled to room temperature It is filtered to remove liquid and obtains substance B, substance B is dry at 82 DEG C after the washing with alcohol that 500mL mass percent concentration is 95% Place 115 minutes in dry case, be subsequently placed in Muffle furnace roasting 78 minutes under the conditions of 489 DEG C, obtain substance C；
(6) by 486 milligrams of PtCl4It is added in mixed liquor M3, stir 5 minutes under the conditions of 1000r/min, mixed Liquid N3；
(7) AgNO for 0.45mol/L by 10mL mixed liquor N3 and 10mL molar concentration3Solution is added to mixed liquor M4 In, stir 5 minutes under the conditions of 1000r/min, obtain mixed liquor N4；
(8) substance C is added in mixed liquor N4, temperature be 40 DEG C shaking table in shake 0.5h, after being cooled to room temperature It is filtered to remove liquid and obtains material D, material D is dry at 82 DEG C after the washing with alcohol that 500mL mass percent concentration is 90% Place 115 minutes in dry case, be subsequently placed in Muffle furnace roasting 78 minutes under the conditions of 489 DEG C, obtain material E；
(9) by 2.69 grams of Ce (NO3)2Being added to volume with 800mL ethanol is in 1000mL conical flask, in 1000r/min bar Under part stir 5 minutes, add 5mL concentrated nitric acid, be divided into 4 parts of equivalent after shaking up, obtain mixed liquor P1, mixed liquor P2, mixed liquor P3, Mixed liquor P4；
(10) Fe (NO for 0.50mol/L by 15mL molar concentration3)3Solution is added in mixed liquor P1, in 1000r/ Stir 5 minutes under the conditions of min, obtain mixed liquor Q1；
(11) Ce (NO for 0.85mol/L by 15mL mixed liquor Q1 and 15mL molar concentration3)2Solution is added to mixed liquor In P2, stir 5 minutes under the conditions of 1000r/min, obtain mixed liquor Q2；
(12) Fe (NO for 0.45mol/L by 15mL mixed liquor Q2 and 15mL molar concentration3)3Solution is added to mixed liquor In P3, stir 5 minutes under the conditions of 1000r/min, obtain mixed liquor Q3；
(13) Ce (NO for 0.80mol/L by 15mL mixed liquor Q3 and 15mL molar concentration3)2Solution is added to mixed liquor In P4, stir 5 minutes under the conditions of 1000r/min, obtain mixed liquor Q4；
(14) mixed liquor Q4 is transferred in high-pressure digestion tank, be heated to 200 DEG C and insulation reaction 10h, be cooled to room temperature After be filtered to remove liquid and obtain material F1, material F1 is after the washing with alcohol that 500mL mass percent concentration is 95% at 85 DEG C Drying baker in place 2h, obtain material F；
(15) material F and sodium citrate solution that 800mL mass percent concentration is 10% being added to volume is In 1000mL conical flask, stir 5 minutes under the conditions of 1000r/min, be divided into 4 parts of equivalent after shaking up, obtain mixed liquor R1, mixing Liquid R2, mixed liquor R3, mixed liquor R4；
(16) CoCl for 0.45mol/L by 25mL molar concentration2Solution and 40mL molar concentration are 0.35mol/L's NiCl2Solution is added in mixed liquor R1, stirs 5 minutes, obtain mixed liquor S1 under the conditions of 1000r/min；
(17) material E is added in mixed liquor S1, temperature be 40 DEG C shaking table in shake 0.5h, after being cooled to room temperature It is filtered to remove liquid and obtains material G1, material G1 is after the washing with alcohol that 500mL mass percent concentration is 90% at 82 DEG C Place 115 minutes in drying baker, be subsequently placed in Muffle furnace roasting 78 minutes under the conditions of 489 DEG C, obtain material H1；
(18) CoCl for 0.40mol/L by 25mL molar concentration2Solution and 40mL molar concentration are 0.30mol/L's NiCl2Solution is added in mixed liquor R2, stirs 5 minutes, obtain mixed liquor S2 under the conditions of 1000r/min；
(19) material H1 is added in mixed liquor S2, temperature be 40 DEG C shaking table in shake 0.5h, be cooled to room temperature After be filtered to remove liquid and obtain material G2, material G2 is after the washing with alcohol that 500mL mass percent concentration is 90% at 82 DEG C Drying baker in place 115 minutes, be subsequently placed in Muffle furnace roasting 78 minutes under the conditions of 489 DEG C, obtain material H2；
(20) CoCl for 0.35mol/L by 25mL molar concentration2Solution and 40mL molar concentration are 0.25mol/L's NiCl2Solution is added in mixed liquor R3, stirs 5 minutes, obtain mixed liquor S3 under the conditions of 1000r/min；
(21) material H2 is added in mixed liquor S3, temperature be 40 DEG C shaking table in shake 0.5h, be cooled to room temperature After be filtered to remove liquid and obtain material G3, material G3 is after the washing with alcohol that 500mL mass percent concentration is 90% at 82 DEG C Drying baker in place 115 minutes, be subsequently placed in Muffle furnace roasting 78 minutes under the conditions of 489 DEG C, obtain material H3；
(22) CoCl for 0.30mol/L by 25mL molar concentration2Solution and 40mL molar concentration are 0.20mol/L's NiCl2Solution is added in mixed liquor R4, stirs 5 minutes, obtain mixed liquor S4 under the conditions of 1000r/min；
(23) material H3 is added in mixed liquor S4, temperature be 40 DEG C shaking table in shake 0.5h, be cooled to room temperature After be filtered to remove liquid and obtain material G4, material G4 is after the washing with alcohol that 500mL mass percent concentration is 90% at 82 DEG C Drying baker in place 115 minutes, be subsequently placed in Muffle furnace roasting 78 minutes under the conditions of 489 DEG C, obtain material H；
(24) 4.23g sodium lauryl sulphate, 35mL normal hexane, 15 milliliters of 2- methyl -2- butanol are added sequentially to hold Amass as in 250mL conical flask, adding 3.55g sodium metavanadate and 150mL deionized water, be placed in 70 DEG C of water-baths in 1000r/ Stir 1h under the conditions of min, be subsequently adding the hydrochloric acid solution that 25mL molar concentration is 2.40mol/L, the shaking table being 45 DEG C in temperature Middle shake 0.5h, is centrifuged 15min under the conditions of 7500r/min after being cooled to room temperature, removes supernatant, use 500mL percent mass Specific concentration is 95% washing with alcohol, obtains material I；
(25) material I and sodium citrate solution that 800mL mass percent concentration is 15% being added to volume is In 1000mL conical flask, stir 5 minutes under the conditions of 1000r/min, be divided into 4 parts of equivalent after shaking up, obtain mixed liquor T1, mixing Liquid T2, mixed liquor T3, mixed liquor T4；
(26) CoCl for 0.75mol/L by 30mL molar concentration2Solution and 40mL molar concentration are 0.55mol/L's NiCl2Solution is added in mixed liquor T1, stirs 5 minutes, obtain mixed liquor U1 under the conditions of 1000r/min；
(27) material H is added in mixed liquor U1, temperature be 40 DEG C shaking table in shake 0.5h, after being cooled to room temperature It is filtered to remove liquid and obtains material J1, material J1 is after the washing with alcohol that 500mL mass percent concentration is 90% at 82 DEG C Place 115 minutes in drying baker, be subsequently placed in Muffle furnace roasting 78 minutes under the conditions of 489 DEG C, obtain material K1；
(28) CoCl for 0.65mol/L by 30mL molar concentration2Solution and 40mL molar concentration are 0.45mol/L's NiCl2Solution is added in mixed liquor T2, stirs 5 minutes, obtain mixed liquor U2 under the conditions of 1000r/min；
(29) material K1 is added in mixed liquor U2, temperature be 40 DEG C shaking table in shake 0.5h, be cooled to room temperature After be filtered to remove liquid and obtain material J2, material J2 is after the washing with alcohol that 500mL mass percent concentration is 95% at 85 DEG C Drying baker in place 1h, be subsequently placed in Muffle furnace roasting 1h under the conditions of 500 DEG C, obtain material K2；
(30) CoCl for 0.60mol/L by 30mL molar concentration2Solution and 40mL molar concentration are 0.40mol/L's NiCl2Solution is added in mixed liquor T3, stirs 5 minutes, obtain mixed liquor U3 under the conditions of 1000r/min；
(31) material K2 is added in mixed liquor U3, temperature be 40 DEG C shaking table in shake 0.5h, be cooled to room temperature After be filtered to remove liquid and obtain material J3, material J3 is after the washing with alcohol that 500mL mass percent concentration is 95% at 85 DEG C Drying baker in place 1h, be subsequently placed in Muffle furnace roasting 1h under the conditions of 500 DEG C, obtain material K3；
(32) CoCl for 0.55mol/L by 30mL molar concentration2Solution and 40mL molar concentration are 0.35mol/L's NiCl2Solution is added in mixed liquor T4, stirs 5 minutes, obtain mixed liquor U4 under the conditions of 1000r/min；
(33) material K3 is added in mixed liquor U4, temperature be 40 DEG C shaking table in shake 0.5h, be cooled to room temperature After be filtered to remove liquid and obtain material J4, material J4 is after the washing with alcohol that 500mL mass percent concentration is 95% at 85 DEG C Drying baker in place 1h, be subsequently placed in Muffle furnace roasting 1h under the conditions of 500 DEG C, obtain material K；
(34) 2.94g poly-N-vinylcaprolactam and 800mL deionized water being added to volume is 1000mL conical flask In, stir 5 minutes under the conditions of 1000r/min, be divided into 4 parts of equivalent after shaking up, obtain mixed liquor V1, mixed liquor V2, mixed liquor V3, mixed liquor V4；
(35) HAuCl for 0.70mol/L by 10mL molar concentration4Solution is added in mixed liquor V1, in 1000r/min Under the conditions of stir 5 minutes, obtain mixed liquor W1；
(36) material K is added in mixed liquor W1, temperature be 40 DEG C shaking table in shake 0.5h, after being cooled to room temperature It is filtered to remove liquid and obtains material L1, material L1 is after the washing with alcohol that 500mL mass percent concentration is 90% at 82 DEG C Place 115 minutes in drying baker, be subsequently placed in Muffle furnace roasting 78 minutes under the conditions of 489 DEG C, obtain material Z1；
(37) HAuCl for 0.65mol/L by 10mL molar concentration4Solution is added in mixed liquor V2, in 1000r/min Under the conditions of stir 5 minutes, obtain mixed liquor W2；
(38) material Z1 is added in mixed liquor W2, temperature be 40 DEG C shaking table in shake 0.5h, be cooled to room temperature After be filtered to remove liquid and obtain material L2, material L2 is after the washing with alcohol that 500mL mass percent concentration is 90% at 82 DEG C Drying baker in place 115 minutes, be subsequently placed in Muffle furnace roasting 78 minutes under the conditions of 489 DEG C, obtain material Z2；
(39) HAuCl for 0.60mol/L by 10mL molar concentration4Solution is added in mixed liquor V3, in 1000r/min Under the conditions of stir 5 minutes, obtain mixed liquor W3；
(40) material Z2 is added in mixed liquor W3, temperature be 40 DEG C shaking table in shake 0.5h, be cooled to room temperature After be filtered to remove liquid and obtain material L3, material L3 is after the washing with alcohol that 500mL mass percent concentration is 90% at 82 DEG C Drying baker in place 115 minutes, be subsequently placed in Muffle furnace roasting 78 minutes under the conditions of 489 DEG C, obtain material Z3；
(41) HAuCl for 0.55mol/L by 10mL molar concentration4Solution is added in mixed liquor V4, in 1000r/min Under the conditions of stir 5 minutes, obtain mixed liquor W4；
(42) material Z3 is added in mixed liquor W4, temperature be 40 DEG C shaking table in shake 0.5h, be cooled to room temperature After be filtered to remove liquid and obtain material L4, material L4 is after the washing with alcohol that 500mL mass percent concentration is 90% at 82 DEG C Drying baker in place 115 minutes, be subsequently placed in Muffle furnace roasting 78 minutes under the conditions of 489 DEG C, the material obtaining is There is the modified activated carbon granule electrode that electro-catalysis removes indole function.
The invention has the beneficial effects as follows, prepared has the modified activated carbon granule electrode tool that electro-catalysis removes indole function Have that current efficiency is high, stability is strong, electrode life length, high to indole removal efficiency the features such as.
Specific embodiment
The present invention provides a kind of modified activated carbon granule electrode with electro-catalysis removal indole function and preparation method, under Face illustrates in fact to apply process by an example.
Embodiment 1.
(1) the activated carbon granule 1000mL deionized water wash for 4-6mm by 150g particle diameter, is then placed in 500mL tri- Soak 8h in chloromethanes, after taking-up, use 1000mL deionized water wash, then the second being 95% with 1000mL mass percent concentration Place 2h in 85 DEG C of drying baker after alcohol washing, obtain substance A；
(2) by 1.23 grams of AgNO3Being added to volume with 800mL ether is in 1000mL conical flask, in 1000r/min condition Lower stirring 5 minutes, is divided into 4 parts of equivalent, obtains mixed liquor M1, mixed liquor M2, mixed liquor M3, mixed liquor M4 after shaking up；
(3) by 262 milligrams of PtCl4It is added in mixed liquor M1, stir 5 minutes under the conditions of 1000r/min, mixed Liquid N1；
(4) AgNO for 0.5mol/L by 10mL mixed liquor N1 and 10mL molar concentration3Solution is added in mixed liquor M2, Stir 5 minutes under the conditions of 1000r/min, obtain mixed liquor N2；
(5) substance A is added in mixed liquor N2, temperature be 38 DEG C shaking table in shake 28 minutes, be cooled to room temperature After be filtered to remove liquid and obtain substance B, substance B is after the washing with alcohol that 500mL mass percent concentration is 95% at 82 DEG C Place 115 minutes in drying baker, be subsequently placed in Muffle furnace roasting 78 minutes under the conditions of 489 DEG C, obtain substance C；
(6) by 486 milligrams of PtCl4It is added in mixed liquor M3, stir 5 minutes under the conditions of 1000r/min, mixed Liquid N3；
(7) AgNO for 0.45mol/L by 10mL mixed liquor N3 and 10mL molar concentration3Solution is added to mixed liquor M4 In, stir 5 minutes under the conditions of 1000r/min, obtain mixed liquor N4；
(8) substance C is added in mixed liquor N4, temperature be 40 DEG C shaking table in shake 0.5h, after being cooled to room temperature It is filtered to remove liquid and obtains material D, material D is dry at 82 DEG C after the washing with alcohol that 500mL mass percent concentration is 90% Place 115 minutes in dry case, be subsequently placed in Muffle furnace roasting 78 minutes under the conditions of 489 DEG C, obtain material E；
(9) by 2.69 grams of Ce (NO3)2Being added to volume with 800mL ethanol is in 1000mL conical flask, in 1000r/min bar Under part stir 5 minutes, add 5mL concentrated nitric acid, be divided into 4 parts of equivalent after shaking up, obtain mixed liquor P1, mixed liquor P2, mixed liquor P3, Mixed liquor P4；
(10) Fe (NO for 0.50mol/L by 15mL molar concentration3)3Solution is added in mixed liquor P1, in 1000r/ Stir 5 minutes under the conditions of min, obtain mixed liquor Q1；
(11) Ce (NO for 0.85mol/L by 15mL mixed liquor Q1 and 15mL molar concentration3)2Solution is added to mixed liquor In P2, stir 5 minutes under the conditions of 1000r/min, obtain mixed liquor Q2；
(12) Fe (NO for 0.45mol/L by 15mL mixed liquor Q2 and 15mL molar concentration3)3Solution is added to mixed liquor In P3, stir 5 minutes under the conditions of 1000r/min, obtain mixed liquor Q3；
(13) Ce (NO for 0.80mol/L by 15mL mixed liquor Q3 and 15mL molar concentration3)2Solution is added to mixed liquor In P4, stir 5 minutes under the conditions of 1000r/min, obtain mixed liquor Q4；
(14) mixed liquor Q4 is transferred in high-pressure digestion tank, be heated to 200 DEG C and insulation reaction 10h, be cooled to room temperature After be filtered to remove liquid and obtain material F1, material F1 is after the washing with alcohol that 500mL mass percent concentration is 95% at 85 DEG C Drying baker in place 2h, obtain material F；
(15) material F and sodium citrate solution that 800mL mass percent concentration is 10% being added to volume is In 1000mL conical flask, stir 5 minutes under the conditions of 1000r/min, be divided into 4 parts of equivalent after shaking up, obtain mixed liquor R1, mixing Liquid R2, mixed liquor R3, mixed liquor R4；
(16) CoCl for 0.45mol/L by 25mL molar concentration2Solution and 40mL molar concentration are 0.35mol/L's NiCl2Solution is added in mixed liquor R1, stirs 5 minutes, obtain mixed liquor S1 under the conditions of 1000r/min；
(17) material E is added in mixed liquor S1, temperature be 40 DEG C shaking table in shake 0.5h, after being cooled to room temperature It is filtered to remove liquid and obtains material G1, material G1 is after the washing with alcohol that 500mL mass percent concentration is 90% at 82 DEG C Place 115 minutes in drying baker, be subsequently placed in Muffle furnace roasting 78 minutes under the conditions of 489 DEG C, obtain material H1；
(18) CoCl for 0.40mol/L by 25mL molar concentration2Solution and 40mL molar concentration are 0.30mol/L's NiCl2Solution is added in mixed liquor R2, stirs 5 minutes, obtain mixed liquor S2 under the conditions of 1000r/min；
(19) material H1 is added in mixed liquor S2, temperature be 40 DEG C shaking table in shake 0.5h, be cooled to room temperature After be filtered to remove liquid and obtain material G2, material G2 is after the washing with alcohol that 500mL mass percent concentration is 90% at 82 DEG C Drying baker in place 115 minutes, be subsequently placed in Muffle furnace roasting 78 minutes under the conditions of 489 DEG C, obtain material H2；
(20) CoCl for 0.35mol/L by 25mL molar concentration2Solution and 40mL molar concentration are 0.25mol/L's NiCl2Solution is added in mixed liquor R3, stirs 5 minutes, obtain mixed liquor S3 under the conditions of 1000r/min；
(21) material H2 is added in mixed liquor S3, temperature be 40 DEG C shaking table in shake 0.5h, be cooled to room temperature After be filtered to remove liquid and obtain material G3, material G3 is after the washing with alcohol that 500mL mass percent concentration is 90% at 82 DEG C Drying baker in place 115 minutes, be subsequently placed in Muffle furnace roasting 78 minutes under the conditions of 489 DEG C, obtain material H3；
(22) CoCl for 0.30mol/L by 25mL molar concentration2Solution and 40mL molar concentration are 0.20mol/L's NiCl2Solution is added in mixed liquor R4, stirs 5 minutes, obtain mixed liquor S4 under the conditions of 1000r/min；
(23) material H3 is added in mixed liquor S4, temperature be 40 DEG C shaking table in shake 0.5h, be cooled to room temperature After be filtered to remove liquid and obtain material G4, material G4 is after the washing with alcohol that 500mL mass percent concentration is 90% at 82 DEG C Drying baker in place 115 minutes, be subsequently placed in Muffle furnace roasting 78 minutes under the conditions of 489 DEG C, obtain material H；
(24) 4.23g sodium lauryl sulphate, 35mL normal hexane, 15 milliliters of 2- methyl -2- butanol are added sequentially to hold Amass as in 250mL conical flask, adding 3.55g sodium metavanadate and 150mL deionized water, be placed in 70 DEG C of water-baths in 1000r/ Stir 1h under the conditions of min, be subsequently adding the hydrochloric acid solution that 25mL molar concentration is 2.40mol/L, the shaking table being 45 DEG C in temperature Middle shake 0.5h, is centrifuged 15min under the conditions of 7500r/min after being cooled to room temperature, removes supernatant, use 500mL percent mass Specific concentration is 95% washing with alcohol, obtains material I；
(25) material I and sodium citrate solution that 800mL mass percent concentration is 15% being added to volume is In 1000mL conical flask, stir 5 minutes under the conditions of 1000r/min, be divided into 4 parts of equivalent after shaking up, obtain mixed liquor T1, mixing Liquid T2, mixed liquor T3, mixed liquor T4；
(26) CoCl for 0.75mol/L by 30mL molar concentration2Solution and 40mL molar concentration are 0.55mol/L's NiCl2Solution is added in mixed liquor T1, stirs 5 minutes, obtain mixed liquor U1 under the conditions of 1000r/min；
(27) material H is added in mixed liquor U1, temperature be 40 DEG C shaking table in shake 0.5h, after being cooled to room temperature It is filtered to remove liquid and obtains material J1, material J1 is after the washing with alcohol that 500mL mass percent concentration is 90% at 82 DEG C Place 115 minutes in drying baker, be subsequently placed in Muffle furnace roasting 78 minutes under the conditions of 489 DEG C, obtain material K1；
(28) CoCl for 0.65mol/L by 30mL molar concentration2Solution and 40mL molar concentration are 0.45mol/L's NiCl2Solution is added in mixed liquor T2, stirs 5 minutes, obtain mixed liquor U2 under the conditions of 1000r/min；
(29) material K1 is added in mixed liquor U2, temperature be 40 DEG C shaking table in shake 0.5h, be cooled to room temperature After be filtered to remove liquid and obtain material J2, material J2 is after the washing with alcohol that 500mL mass percent concentration is 95% at 85 DEG C Drying baker in place 1h, be subsequently placed in Muffle furnace roasting 1h under the conditions of 500 DEG C, obtain material K2；
(30) CoCl for 0.60mol/L by 30mL molar concentration2Solution and 40mL molar concentration are 0.40mol/L's NiCl2Solution is added in mixed liquor T3, stirs 5 minutes, obtain mixed liquor U3 under the conditions of 1000r/min；
(31) material K2 is added in mixed liquor U3, temperature be 40 DEG C shaking table in shake 0.5h, be cooled to room temperature After be filtered to remove liquid and obtain material J3, material J3 is after the washing with alcohol that 500mL mass percent concentration is 95% at 85 DEG C Drying baker in place 1h, be subsequently placed in Muffle furnace roasting 1h under the conditions of 500 DEG C, obtain material K3；
(32) CoCl for 0.55mol/L by 30mL molar concentration2Solution and 40mL molar concentration are 0.35mol/L's NiCl2Solution is added in mixed liquor T4, stirs 5 minutes, obtain mixed liquor U4 under the conditions of 1000r/min；
(33) material K3 is added in mixed liquor U4, temperature be 40 DEG C shaking table in shake 0.5h, be cooled to room temperature After be filtered to remove liquid and obtain material J4, material J4 is after the washing with alcohol that 500mL mass percent concentration is 95% at 85 DEG C Drying baker in place 1h, be subsequently placed in Muffle furnace roasting 1h under the conditions of 500 DEG C, obtain material K；
(34) 2.94g poly-N-vinylcaprolactam and 800mL deionized water being added to volume is 1000mL conical flask In, stir 5 minutes under the conditions of 1000r/min, be divided into 4 parts of equivalent after shaking up, obtain mixed liquor V1, mixed liquor V2, mixed liquor V3, mixed liquor V4；
(35) HAuCl for 0.70mol/L by 10mL molar concentration4Solution is added in mixed liquor V1, in 1000r/min Under the conditions of stir 5 minutes, obtain mixed liquor W1；
(36) material K is added in mixed liquor W1, temperature be 40 DEG C shaking table in shake 0.5h, after being cooled to room temperature It is filtered to remove liquid and obtains material L1, material L1 is after the washing with alcohol that 500mL mass percent concentration is 90% at 82 DEG C Place 115 minutes in drying baker, be subsequently placed in Muffle furnace roasting 78 minutes under the conditions of 489 DEG C, obtain material Z1；
(37) HAuCl for 0.65mol/L by 10mL molar concentration4Solution is added in mixed liquor V2, in 1000r/min Under the conditions of stir 5 minutes, obtain mixed liquor W2；
(38) material Z1 is added in mixed liquor W2, temperature be 40 DEG C shaking table in shake 0.5h, be cooled to room temperature After be filtered to remove liquid and obtain material L2, material L2 is after the washing with alcohol that 500mL mass percent concentration is 90% at 82 DEG C Drying baker in place 115 minutes, be subsequently placed in Muffle furnace roasting 78 minutes under the conditions of 489 DEG C, obtain material Z2；
(39) HAuCl for 0.60mol/L by 10mL molar concentration4Solution is added in mixed liquor V3, in 1000r/min Under the conditions of stir 5 minutes, obtain mixed liquor W3；
(40) material Z2 is added in mixed liquor W3, temperature be 40 DEG C shaking table in shake 0.5h, be cooled to room temperature After be filtered to remove liquid and obtain material L3, material L3 is after the washing with alcohol that 500mL mass percent concentration is 90% at 82 DEG C Drying baker in place 115 minutes, be subsequently placed in Muffle furnace roasting 78 minutes under the conditions of 489 DEG C, obtain material Z3；
(41) HAuCl for 0.55mol/L by 10mL molar concentration4Solution is added in mixed liquor V4, in 1000r/min Under the conditions of stir 5 minutes, obtain mixed liquor W4；
(42) material Z3 is added in mixed liquor W4, temperature be 40 DEG C shaking table in shake 0.5h, be cooled to room temperature After be filtered to remove liquid and obtain material L4, material L4 is after the washing with alcohol that 500mL mass percent concentration is 90% at 82 DEG C Drying baker in place 115 minutes, be subsequently placed in Muffle furnace roasting 78 minutes under the conditions of 489 DEG C, the material obtaining is There is the modified activated carbon granule electrode that electro-catalysis removes indole function.
It is presented herein below, with what the inventive method was obtained, there is the modified activated carbon granule electrode that electro-catalysis removes indole function In electric catalysis reactor, Electro-catalytic Oxidation Process test is carried out to the waste water containing indole, further illustrated the present invention.
The modified activated carbon granule electrode with electro-catalysis removal indole function that the inventive method is obtained is seated in electricity In catalytic reactor, Degrading experiment is carried out to the waste water containing indole, result shows the electrocatalytic reaction being loaded by this electrode Device can efficiently remove the indole in waste water, when the indole concentration in waste water is 42.3mg/L, is 5.0 in pH, voltage is 14V, under the conditions of process time is 45min, the indole concentration in water outlet after process is reduced to 2.6mg/L, and treatment effeciency reaches 93.86%.

Claims (1)

1. a kind of preparation method of the modified activated carbon granule electrode with electro-catalysis removal indole function is it is characterised in that be somebody's turn to do The comprising the following steps that of method：
(1) the activated carbon granule 1000mL deionized water wash for 4-6mm by 150g particle diameter, is then placed in 500mL tri- chloromethane Soak 8h in alkane, use 1000mL deionized water wash after taking-up, then washed with the ethanol that 1000mL mass percent concentration is 95% Place 2h in 85 DEG C of drying baker after washing, obtain substance A；
(2) by 1.23 grams of AgNO3Being added to volume with 800mL ether is in 1000mL conical flask, stirs under the conditions of 1000r/min Mix 5 minutes, after shaking up, be divided into 4 parts of equivalent, obtain mixed liquor M1, mixed liquor M2, mixed liquor M3, mixed liquor M4；
(3) by 262 milligrams of PtCl4It is added in mixed liquor M1, stir 5 minutes under the conditions of 1000r/min, obtain mixed liquor N1；
(4) AgNO for 0.5mol/L by 10mL mixed liquor N1 and 10mL molar concentration3Solution is added in mixed liquor M2, Stir 5 minutes under the conditions of 1000r/min, obtain mixed liquor N2；
(5) substance A is added in mixed liquor N2, temperature be 40 DEG C shaking table in shake 0.5h, be cooled to and filter after room temperature Remove liquid and obtain substance B, substance B is after the washing with alcohol that 500mL mass percent concentration is 90% in 82 DEG C of drying baker Middle place 115 minutes, be subsequently placed in Muffle furnace roasting 78 minutes under the conditions of 489 DEG C, obtain substance C；
(6) by 486 milligrams of PtCl4It is added in mixed liquor M3, stir 5 minutes under the conditions of 1000r/min, obtain mixed liquor N3；
(7) AgNO for 0.45mol/L by 10mL mixed liquor N3 and 10mL molar concentration3Solution is added in mixed liquor M4, Stir 5 minutes under the conditions of 1000r/min, obtain mixed liquor N4；
(8) substance C is added in mixed liquor N4, temperature be 40 DEG C shaking table in shake 0.5h, be cooled to and filter after room temperature Remove liquid and obtain material D, material D is after the washing with alcohol that 500mL mass percent concentration is 90% in 82 DEG C of drying baker Middle place 115 minutes, be subsequently placed in Muffle furnace roasting 78 minutes under the conditions of 489 DEG C, obtain material E；
(9) by 2.69 grams of Ce (NO3)2Being added to volume with 800mL ethanol is in 1000mL conical flask, under the conditions of 1000r/min Stirring 5 minutes, adds 5mL concentrated nitric acid, is divided into 4 parts of equivalent, obtains mixed liquor P1, mixed liquor P2, mixed liquor P3, mixing after shaking up Liquid P4；
(10) Fe (NO for 0.50mol/L by 15mL molar concentration3)3Solution is added in mixed liquor P1, in 1000r/min bar Stir 5 minutes under part, obtain mixed liquor Q1；
(11) Ce (NO for 0.85mol/L by 15mL mixed liquor Q1 and 15mL molar concentration3)2Solution is added in mixed liquor P2, Stir 5 minutes under the conditions of 1000r/min, obtain mixed liquor Q2；
(12) Fe (NO for 0.45mol/L by 15mL mixed liquor Q2 and 15mL molar concentration3)3Solution is added in mixed liquor P3, Stir 5 minutes under the conditions of 1000r/min, obtain mixed liquor Q3；
(13) Ce (NO for 0.80mol/L by 15mL mixed liquor Q3 and 15mL molar concentration3)2Solution is added in mixed liquor P4, Stir 5 minutes under the conditions of 1000r/min, obtain mixed liquor Q4；
(14) mixed liquor Q4 is transferred in high-pressure digestion tank, be heated to 200 DEG C and insulation reaction 10h, be cooled to mistake after room temperature Filter liquid and obtain material F1, material F1 is dry at 85 DEG C after the washing with alcohol that 500mL mass percent concentration is 95% Place 2h in dry case, obtain material F；
(15) material F and sodium citrate solution that 800mL mass percent concentration is 10% are added to volume to bore for 1000mL In shape bottle, stir 5 minutes under the conditions of 1000r/min, after shaking up, be divided into 4 parts of equivalent, obtain mixed liquor R1, mixed liquor R2, mix Close liquid R3, mixed liquor R4；
(16) CoCl for 0.45mol/L by 25mL molar concentration2Solution and 40mL molar concentration are the NiCl of 0.35mol/L2Molten Liquid is added in mixed liquor R1, stirs 5 minutes, obtain mixed liquor S1 under the conditions of 1000r/min；
(17) material E is added in mixed liquor S1, temperature be 40 DEG C shaking table in shake 0.5h, be cooled to and filter after room temperature Remove liquid and obtain material G1, material G1 is after the washing with alcohol that 500mL mass percent concentration is 90% in 82 DEG C of drying Place 115 minutes in case, be subsequently placed in Muffle furnace roasting 78 minutes under the conditions of 489 DEG C, obtain material H1；
(18) CoCl for 0.40mol/L by 25mL molar concentration2Solution and 40mL molar concentration are the NiCl of 0.30mol/L2Molten Liquid is added in mixed liquor R2, stirs 5 minutes, obtain mixed liquor S2 under the conditions of 1000r/min；
(19) material H1 is added in mixed liquor S2, temperature be 40 DEG C shaking table in shake 0.5h, be cooled to mistake after room temperature Filter liquid and obtain material G2, material G2 is dry at 82 DEG C after the washing with alcohol that 500mL mass percent concentration is 90% Place 115 minutes in dry case, be subsequently placed in Muffle furnace roasting 78 minutes under the conditions of 489 DEG C, obtain material H2；
(20) CoCl for 0.35mol/L by 25mL molar concentration2Solution and 40mL molar concentration are the NiCl of 0.25mol/L2Molten Liquid is added in mixed liquor R3, stirs 5 minutes, obtain mixed liquor S3 under the conditions of 1000r/min；
(21) material H2 is added in mixed liquor S3, temperature be 40 DEG C shaking table in shake 0.5h, be cooled to mistake after room temperature Filter liquid and obtain material G3, material G3 is dry at 82 DEG C after the washing with alcohol that 500mL mass percent concentration is 90% Place 115 minutes in dry case, be subsequently placed in Muffle furnace roasting 78 minutes under the conditions of 489 DEG C, obtain material H3；
(22) CoCl for 0.30mol/L by 25mL molar concentration2Solution and 40mL molar concentration are the NiCl of 0.20mol/L2Molten Liquid is added in mixed liquor R4, stirs 5 minutes, obtain mixed liquor S4 under the conditions of 1000r/min；
(23) material H3 is added in mixed liquor S4, temperature be 40 DEG C shaking table in shake 0.5h, be cooled to mistake after room temperature Filter liquid and obtain material G4, material G4 is dry at 82 DEG C after the washing with alcohol that 500mL mass percent concentration is 90% Place 115 minutes in dry case, be subsequently placed in Muffle furnace roasting 78 minutes under the conditions of 489 DEG C, obtain material H；
(24) 4.23g sodium lauryl sulphate, 35mL normal hexane, 15 milliliters of 2- methyl -2- butanol are added sequentially to volume and are In 250mL conical flask, add 3.55g sodium metavanadate and 150mL deionized water, be placed in 70 DEG C of water-baths in 1000r/min bar Under part stir 1h, be subsequently adding 25mL molar concentration be 2.40mol/L hydrochloric acid solution, temperature be 45 DEG C shaking table in shake 0.5h, is centrifuged 15min under the conditions of 7500r/min after being cooled to room temperature, removes supernatant, use 500mL mass percent concentration Washing with alcohol for 95%, obtains material I；
(25) material I and sodium citrate solution that 800mL mass percent concentration is 15% are added to volume to bore for 1000mL In shape bottle, stir 5 minutes under the conditions of 1000r/min, after shaking up, be divided into 4 parts of equivalent, obtain mixed liquor T1, mixed liquor T2, mix Close liquid T3, mixed liquor T4；
(26) CoCl for 0.75mol/L by 30mL molar concentration2Solution and 40mL molar concentration are the NiCl of 0.55mol/L2Molten Liquid is added in mixed liquor T1, stirs 5 minutes, obtain mixed liquor U1 under the conditions of 1000r/min；
(27) material H is added in mixed liquor U1, temperature be 40 DEG C shaking table in shake 0.5h, be cooled to and filter after room temperature Remove liquid and obtain material J1, material J1 is after the washing with alcohol that 500mL mass percent concentration is 90% in 82 DEG C of drying Place 115 minutes in case, be subsequently placed in Muffle furnace roasting 78 minutes under the conditions of 489 DEG C, obtain material K1；
(28) CoCl for 0.65mol/L by 30mL molar concentration2Solution and 40mL molar concentration are the NiCl of 0.45mol/L2Molten Liquid is added in mixed liquor T2, stirs 5 minutes, obtain mixed liquor U2 under the conditions of 1000r/min；
(29) material K1 is added in mixed liquor U2, temperature be 40 DEG C shaking table in shake 0.5h, be cooled to mistake after room temperature Filter liquid and obtain material J2, material J2 is dry at 85 DEG C after the washing with alcohol that 500mL mass percent concentration is 95% Place 1h in dry case, be subsequently placed in Muffle furnace roasting 1h under the conditions of 500 DEG C, obtain material K2；
(30) CoCl for 0.60mol/L by 30mL molar concentration2Solution and 40mL molar concentration are the NiCl of 0.40mol/L2Molten Liquid is added in mixed liquor T3, stirs 5 minutes, obtain mixed liquor U3 under the conditions of 1000r/min；
(31) material K2 is added in mixed liquor U3, temperature be 40 DEG C shaking table in shake 0.5h, be cooled to mistake after room temperature Filter liquid and obtain material J3, material J3 is dry at 85 DEG C after the washing with alcohol that 500mL mass percent concentration is 95% Place 1h in dry case, be subsequently placed in Muffle furnace roasting 1h under the conditions of 500 DEG C, obtain material K3；
(32) CoCl for 0.55mol/L by 30mL molar concentration2Solution and 40mL molar concentration are the NiCl of 0.35mol/L2Molten Liquid is added in mixed liquor T4, stirs 5 minutes, obtain mixed liquor U4 under the conditions of 1000r/min；
(33) material K3 is added in mixed liquor U4, temperature be 40 DEG C shaking table in shake 0.5h, be cooled to mistake after room temperature Filter liquid and obtain material J4, material J4 is dry at 85 DEG C after the washing with alcohol that 500mL mass percent concentration is 95% Place 1h in dry case, be subsequently placed in Muffle furnace roasting 1h under the conditions of 500 DEG C, obtain material K；
(34) 2.94g poly-N-vinylcaprolactam and 800mL deionized water being added to volume is in 1000mL conical flask, Stir 5 minutes under the conditions of 1000r/min, after shaking up, be divided into 4 parts of equivalent, obtain mixed liquor V1, mixed liquor V2, mixed liquor V3, mix Close liquid V4；
(35) HAuCl for 0.70mol/L by 10mL molar concentration4Solution is added in mixed liquor V1, in 1000r/min condition Lower stirring 5 minutes, obtains mixed liquor W1；
(36) material K is added in mixed liquor W1, temperature be 40 DEG C shaking table in shake 0.5h, be cooled to and filter after room temperature Remove liquid and obtain material L1, material L1 is after the washing with alcohol that 500mL mass percent concentration is 90% in 82 DEG C of drying Place 115 minutes in case, be subsequently placed in Muffle furnace roasting 78 minutes under the conditions of 489 DEG C, obtain material Z1；
(37) HAuCl for 0.65mol/L by 10mL molar concentration4Solution is added in mixed liquor V2, in 1000r/min condition Lower stirring 5 minutes, obtains mixed liquor W2；
(38) material Z1 is added in mixed liquor W2, temperature be 40 DEG C shaking table in shake 0.5h, be cooled to mistake after room temperature Filter liquid and obtain material L2, material L2 is dry at 82 DEG C after the washing with alcohol that 500mL mass percent concentration is 90% Place 115 minutes in dry case, be subsequently placed in Muffle furnace roasting 78 minutes under the conditions of 489 DEG C, obtain material Z2；
(39) HAuCl for 0.60mol/L by 10mL molar concentration4Solution is added in mixed liquor V3, in 1000r/min condition Lower stirring 5 minutes, obtains mixed liquor W3；
(40) material Z2 is added in mixed liquor W3, temperature be 40 DEG C shaking table in shake 0.5h, be cooled to mistake after room temperature Filter liquid and obtain material L3, material L3 is dry at 82 DEG C after the washing with alcohol that 500mL mass percent concentration is 90% Place 115 minutes in dry case, be subsequently placed in Muffle furnace roasting 78 minutes under the conditions of 489 DEG C, obtain material Z3；
(41) HAuCl for 0.55mol/L by 10mL molar concentration4Solution is added in mixed liquor V4, in 1000r/min condition Lower stirring 5 minutes, obtains mixed liquor W4；
(42) material Z3 is added in mixed liquor W4, temperature be 40 DEG C shaking table in shake 0.5h, be cooled to mistake after room temperature Filter liquid and obtain material L4, material L4 is dry at 82 DEG C after the washing with alcohol that 500mL mass percent concentration is 90% Place 115 minutes in dry case, be subsequently placed in Muffle furnace roasting 78 minutes under the conditions of 489 DEG C, the material obtaining as has Electro-catalysis removes the modified activated carbon granule electrode of indole function.
CN201611043591.6A 2016-11-21 2016-11-21 Modified activated carbon particle electrode with function using electro-catalysis to remove indole and preparation method Withdrawn CN106430459A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108083393A (en) * 2017-12-28 2018-05-29 光合强化（北京）生物科技有限公司 The graphite electrode modified based on PbO-NiO-MgO and thiophene
CN108163931A (en) * 2017-12-28 2018-06-15 光合强化（北京）生物科技有限公司 The graphite electrode modified based on CeO-ZrO-NiO and pyrazine
CN108178247A (en) * 2017-12-28 2018-06-19 光合强化（北京）生物科技有限公司 The graphite electrode modified based on CrO-FeO-PbO and quinoline
CN108178248A (en) * 2017-12-28 2018-06-19 光合强化（北京）生物科技有限公司 The graphite electrode modified based on CuO-CoO-ZnO and pyridine

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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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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108083393A (en) * 2017-12-28 2018-05-29 光合强化（北京）生物科技有限公司 The graphite electrode modified based on PbO-NiO-MgO and thiophene
CN108163931A (en) * 2017-12-28 2018-06-15 光合强化（北京）生物科技有限公司 The graphite electrode modified based on CeO-ZrO-NiO and pyrazine
CN108178247A (en) * 2017-12-28 2018-06-19 光合强化（北京）生物科技有限公司 The graphite electrode modified based on CrO-FeO-PbO and quinoline
CN108178248A (en) * 2017-12-28 2018-06-19 光合强化（北京）生物科技有限公司 The graphite electrode modified based on CuO-CoO-ZnO and pyridine

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