CN106348403A - Modified quartz particle electrode with function of removing furan through electrocatalysis and preparation method thereof - Google Patents

Modified quartz particle electrode with function of removing furan through electrocatalysis and preparation method thereof Download PDF

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CN106348403A
CN106348403A CN201611039126.5A CN201611039126A CN106348403A CN 106348403 A CN106348403 A CN 106348403A CN 201611039126 A CN201611039126 A CN 201611039126A CN 106348403 A CN106348403 A CN 106348403A
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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
    • C02F2101/34—Organic compounds containing oxygen
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2305/00—Use of specific compounds during water treatment
    • C02F2305/02—Specific form of oxidant
    • C02F2305/023—Reactive oxygen species, singlet oxygen, OH radical

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Engineering & Computer Science (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Organic Chemistry (AREA)
  • Catalysts (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)

Abstract

The invention discloses a modified quartz particle electrode with a function of removing furan through electrocatalysis and a preparation method thereof. Quartz, trichloromethane and ethyl alcohol are prepared into a substance A; the substance A is prepared into a substance E through modifying mixed liquid prepared from silver nitrate, platinum nitrate, diethyl ether and Bi(NO3)3; the substance E is prepared into a substance H through modifying mixed liquid prepared from Pb(NO3)2, ethyl alcohol, CeCl3, ZrCl4, MgCl2 and CdCl2; the substance H is prepared into a substance K through modifying mixed liquid prepared from lauryl sodium sulfate, normal hexane, normal butanol, ammonium metavanadate, sodium citrate, MgCl2 and CdCl2; the substance K is prepared into a substance through modifying mixed liquid prepared from polyvinyl alcohol and HAuCl4, and the substance is the modified quartz particle electrode with the function of removing furan through electrocatalysis.

Description

There is modified quartz particles electrode and the preparation method that electro-catalysis removes furan 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 quartz particles electrode removing furan 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 furan 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 quartz particles electrode and the preparation that electro-catalysis removes furan function Method, the specifically comprising the following steps that of its preparation method
(1) put in 500ml beaker after the 98g quartz particles 1000ml deionized water wash being 2～4mm by particle diameter, Add the hydrochloric acid solution that 300ml molar concentration is 0.1mol/l and soak 0.5h, remove liquid after filtration and obtain material a01, will Material a01 is added to the agno that 250ml molar concentration is 1.66mol/l3In solution, temperature be 65 DEG C shaking table in shake 15 Minute, it is filtered to remove liquid after being cooled to room temperature and obtains material a02, material a02 is 95% through 900ml mass percent concentration Place 1.5h in 85 DEG C of drying baker after washing with alcohol, be subsequently placed in Muffle furnace roasting 1h under the conditions of 480 DEG C, obtain thing Matter a1；
(2) 8.34 grams of platinum nitrates and 750ml deionized water being added to volume is in 1000ml conical flask, in 1000r/ Stir 3 minutes under the conditions of min, add 15ml concentrated nitric acid, after shaking up, be divided into 3 parts of equivalent, obtain mixed liquor k1, mixed liquor k2, mix Close liquid k3；
(3) by 817 milligrams of bi (no3)3It is the agno of 0.44mol/l with 37ml molar concentration3Solution is added to mixed liquor k1 In, stir 3 minutes under the conditions of 1000r/min, obtain mixed liquor l1；
(4) material a1 is added in mixed liquor l1, temperature be 45 DEG C shaking table in shake 15 minutes, be cooled to room temperature After be filtered to remove liquid and obtain material a2, material a2 is after the washing with alcohol that 100ml mass percent concentration is 93% at 88 DEG C Drying baker in place 112 minutes, be subsequently placed in Muffle furnace roasting 58 minutes under the conditions of 508 DEG C, obtain material a3；
(5) by 847 milligrams of bi (no3)3It is the agno of 0.64mol/l with 67ml molar concentration3Solution is added to mixed liquor k2 In, stir 3 minutes under the conditions of 1000r/min, obtain mixed liquor l2；
(6) material a3 is added in mixed liquor l2, temperature be 45 DEG C shaking table in shake 15 minutes, be cooled to room temperature After be filtered to remove liquid and obtain material a4, material a4 is after the washing with alcohol that 100ml mass percent concentration is 93% at 88 DEG C Drying baker in place 112 minutes, be subsequently placed in Muffle furnace roasting 58 minutes under the conditions of 508 DEG C, obtain material a5；
(7) by 877 milligrams of bi (no3)3It is the agno of 0.84mol/l with 97ml molar concentration3Solution is added to mixed liquor k3 In, stir 3 minutes under the conditions of 1000r/min, obtain mixed liquor l3；
(8) material a5 is added in mixed liquor l3, temperature be 45 DEG C shaking table in shake 15 minutes, be cooled to room temperature After be filtered to remove liquid and obtain material a6, material a6 is after the washing with alcohol that 100ml mass percent concentration is 93% at 88 DEG C Drying baker in place 112 minutes, be subsequently placed in Muffle furnace roasting 58 minutes under the conditions of 508 DEG C, obtain material a；
(9) by 5.29 grams of agno3Being added to volume with 750ml ether is in 1000ml conical flask, in 1000r/min condition Lower stirring 3 minutes, is divided into 3 parts of equivalent, obtains mixed liquor m1, mixed liquor m2, mixed liquor m3 after shaking up；
(10) by 228 milligrams of agno3It is the bi (no of 0.49mol/l with 46ml molar concentration3)3Solution is added to mixed liquor In m1, stir 3 minutes under the conditions of 1000r/min, obtain mixed liquor n1；
(11) material a is added in mixed liquor n1, temperature be 45 DEG C shaking table in shake 15 minutes, be cooled to room temperature After be filtered to remove liquid and obtain material b, material b is after the washing with alcohol that 100ml mass percent concentration is 93% at 88 DEG C Place 112 minutes in drying baker, be subsequently placed in Muffle furnace roasting 58 minutes under the conditions of 508 DEG C, obtain material b1；
(12) by 258 milligrams of agno3It is the bi (no of 0.69mol/l with 66ml molar concentration3)3Solution is added to mixed liquor In m2, stir 3 minutes under the conditions of 1000r/min, obtain mixed liquor n2；
(13) material b1 is added in mixed liquor n2, temperature be 45 DEG C shaking table in shake 15 minutes, be cooled to room It is filtered to remove liquid after temperature and obtains material b2, material b2 is after the washing with alcohol that 100ml mass percent concentration is 93% 88 DEG C drying baker in place 112 minutes, be subsequently placed in Muffle furnace roasting 58 minutes under the conditions of 508 DEG C, obtain material c；
(14) by 288 milligrams of agno3It is the bi (no of 0.89mol/l with 86ml molar concentration3)3Solution is added to mixed liquor In m3, stir 3 minutes under the conditions of 1000r/min, obtain mixed liquor n3；
(15) material c is added in mixed liquor n3, temperature be 45 DEG C shaking table in shake 15 minutes, be cooled to room temperature After be filtered to remove liquid and obtain material d, material d is after the washing with alcohol that 100ml mass percent concentration is 93% at 88 DEG C Place 112 minutes in drying baker, be subsequently placed in Muffle furnace roasting 58 minutes under the conditions of 508 DEG C, obtain material e；
(16) by 6.98 grams of pb (no3)2Being added to volume with 850ml ethanol is in 1000ml conical flask, in 1000r/min Under the conditions of stir 3 minutes, add 5ml concentrated nitric acid, be divided into 5 parts of equivalent after shaking up, obtain mixed liquor p1, mixed liquor p2, mixed liquor P3, mixed liquor p4, mixed liquor p5；
(17) cecl for 0.77mol/l by 87ml molar concentration3Solution is added in mixed liquor p1, in 1000r/min Under the conditions of stir 3 minutes, obtain mixed liquor q1；
(18) material e is added in mixed liquor q1, temperature be 45 DEG C shaking table in shake 15 minutes, be cooled to room temperature After be filtered to remove liquid and obtain material f1, material f1 is after the washing with alcohol that 100ml mass percent concentration is 93% at 88 DEG C Drying baker in place 112 minutes, be subsequently placed in Muffle furnace roasting 58 minutes under the conditions of 508 DEG C, obtain material f2；
(19) pb (no for 0.86mol/l by 92ml molar concentration3)2Solution is added in mixed liquor p2, in 1000r/ Stir 3 minutes under the conditions of min, obtain mixed liquor q2；
(20) material f2 is added in mixed liquor q2, temperature be 45 DEG C shaking table in shake 15 minutes, be cooled to room It is filtered to remove liquid after temperature and obtains material f3, material f3 is after the washing with alcohol that 100ml mass percent concentration is 93% 88 DEG C drying baker in place 112 minutes, be subsequently placed in Muffle furnace roasting 58 minutes under the conditions of 508 DEG C, obtain material f4；
(21) cecl for 0.57mol/l by 67ml molar concentration3Solution is added in mixed liquor p3, in 1000r/min Under the conditions of stir 3 minutes, obtain mixed liquor q3；
(22) material f4 is added in mixed liquor q3, temperature be 45 DEG C shaking table in shake 15 minutes, be cooled to room It is filtered to remove liquid after temperature and obtains material f5, material f5 is after the washing with alcohol that 100ml mass percent concentration is 93% 88 DEG C drying baker in place 112 minutes, be subsequently placed in Muffle furnace roasting 58 minutes under the conditions of 508 DEG C, obtain material f6；
(23) pb (no for 0.66mol/l by 72ml molar concentration3)2Solution is added in mixed liquor p4, in 1000r/ Stir 3 minutes under the conditions of min, obtain mixed liquor q4；
(24) material f6 is added in mixed liquor q4, temperature be 45 DEG C shaking table in shake 15 minutes, be cooled to room It is filtered to remove liquid after temperature and obtains material f7, material f7 is after the washing with alcohol that 100ml mass percent concentration is 93% 88 DEG C drying baker in place 112 minutes, be subsequently placed in Muffle furnace roasting 58 minutes under the conditions of 508 DEG C, obtain material f8；
(25) cecl for 0.37mol/l by 47ml molar concentration3Solution and 52ml molar concentration are the pb of 0.46mol/l (no3)2Solution is added in mixed liquor p5, stirs 3 minutes, obtain mixed liquor q5 under the conditions of 1000r/min；
(26) material f8 is added in mixed liquor q5, temperature be 45 DEG C shaking table in shake 15 minutes, be cooled to room It is filtered to remove liquid after temperature and obtains material f9, material f9 is after the washing with alcohol that 100ml mass percent concentration is 93% 88 DEG C drying baker in place 112 minutes, be subsequently placed in Muffle furnace roasting 58 minutes under the conditions of 508 DEG C, obtain material f；
(27) by 5.98g zrcl4It is added to volume with the sodium citrate solution that 750ml mass percent concentration is 10% For, in 1000ml conical flask, stirring 3 minutes under the conditions of 1000r/min, being divided into 3 parts of equivalent after shaking up, obtain mixed liquor r1, mix Close liquid r2, mixed liquor r3；
(28) mgcl for 0.39mol/l by 35ml molar concentration2Solution and 65ml molar concentration are 0.84mol/l's cdcl2Solution is added in mixed liquor r1, stirs 3 minutes, obtain mixed liquor s1 under the conditions of 1000r/min；
(29) material f is added in mixed liquor s1, temperature be 45 DEG C shaking table in shake 15 minutes, be cooled to room temperature After be filtered to remove liquid and obtain material g1, material g1 is after the washing with alcohol that 100ml mass percent concentration is 93% at 88 DEG C Drying baker in place 112 minutes, be subsequently placed in Muffle furnace roasting 58 minutes under the conditions of 508 DEG C, obtain material h1；
(30) mgcl for 0.59mol/l by 55ml molar concentration2Solution and 45ml molar concentration are 0.64mol/l's cdcl2Solution is added in mixed liquor r2, stirs 3 minutes, obtain mixed liquor s2 under the conditions of 1000r/min；
(31) material h1 is added in mixed liquor s2, temperature be 45 DEG C shaking table in shake 15 minutes, be cooled to room It is filtered to remove liquid after temperature and obtains material g2, material g2 is after the washing with alcohol that 100ml mass percent concentration is 93% 88 DEG C drying baker in place 112 minutes, be subsequently placed in Muffle furnace roasting 58 minutes under the conditions of 508 DEG C, obtain material h2；
(32) mgcl for 0.79mol/l by 75ml molar concentration2Solution and 25ml molar concentration are 0.44mol/l's cdcl2Solution is added in mixed liquor r3, stirs 3 minutes, obtain mixed liquor s3 under the conditions of 1000r/min；
(33) material h2 is added in mixed liquor s3, temperature be 45 DEG C shaking table in shake 15 minutes, be cooled to room It is filtered to remove liquid after temperature and obtains material g3, material g3 is after the washing with alcohol that 100ml mass percent concentration is 93% 88 DEG C drying baker in place 112 minutes, be subsequently placed in Muffle furnace roasting 58 minutes under the conditions of 508 DEG C, obtain material h；
(34) 4.55g sodium lauryl sulphate, 40ml normal hexane, 20 milliliters of n-butyl alcohol are added sequentially to volume and are In 250ml conical flask, add 8.31g ammonium 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；
(35) material i and sodium citrate solution that 800ml mass percent concentration is 15% being added to volume is In 1000ml conical flask, stir 3 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；
(36) mgcl for 0.41mol/l by 33ml molar concentration2Solution and 67ml molar concentration are 0.88mol/l's cdcl2Solution is added in mixed liquor t1, stirs 3 minutes, obtain mixed liquor u1 under the conditions of 1000r/min；
(37) material h is added in mixed liquor u1, temperature be 45 DEG C shaking table in shake 15 minutes, be cooled to room temperature After be filtered to remove liquid and obtain material j1, material j1 is after the washing with alcohol that 100ml mass percent concentration is 93% at 88 DEG C Drying baker in place 112 minutes, be subsequently placed in Muffle furnace roasting 58 minutes under the conditions of 508 DEG C, obtain material k1；
(38) mgcl for 0.51mol/l by 43ml molar concentration2Solution and 57ml molar concentration are 0.78mol/l's cdcl2Solution is added in mixed liquor t2, stirs 3 minutes, obtain mixed liquor u2 under the conditions of 1000r/min；
(39) material k1 is added in mixed liquor u2, temperature be 45 DEG C shaking table in shake 15 minutes, be cooled to room It is filtered to remove liquid after temperature and obtains material j2, material j2 is after the washing with alcohol that 100ml mass percent concentration is 93% 88 DEG C drying baker in place 112 minutes, be subsequently placed in Muffle furnace roasting 58 minutes under the conditions of 508 DEG C, obtain material k2；
(40) mgcl for 0.61mol/l by 53ml molar concentration2Solution and 47ml molar concentration are 0.68mol/l's cdcl2Solution is added in mixed liquor t3, stirs 3 minutes, obtain mixed liquor u3 under the conditions of 1000r/min；
(41) material k2 is added in mixed liquor u3, temperature be 45 DEG C shaking table in shake 15 minutes, be cooled to room It is filtered to remove liquid after temperature and obtains material j3, material j3 is after the washing with alcohol that 100ml mass percent concentration is 93% 88 DEG C drying baker in place 112 minutes, be subsequently placed in Muffle furnace roasting 58 minutes under the conditions of 508 DEG C, obtain material k3；
(42) mgcl for 0.71mol/l by 63ml molar concentration2Solution and 37ml molar concentration are 0.58mol/l's cdcl2Solution is added in mixed liquor t4, stirs 3 minutes, obtain mixed liquor u4 under the conditions of 1000r/min；
(43) material k3 is added in mixed liquor u4, temperature be 45 DEG C shaking table in shake 15 minutes, be cooled to room It is filtered to remove liquid after temperature and obtains material j4, material j4 is after the washing with alcohol that 100ml mass percent concentration is 93% 88 DEG C drying baker in place 112 minutes, be subsequently placed in Muffle furnace roasting 58 minutes under the conditions of 508 DEG C, obtain material k；
(44) 9.66g polyvinyl alcohol and 900ml deionized water being added to volume is in 1000ml conical flask, in 1000r/ Stir 3 minutes under the conditions of min, be divided into 3 parts of equivalent after shaking up, obtain mixed liquor v1, mixed liquor v2, mixed liquor v3；
(45) haucl for 0.96mol/l by 89ml molar concentration4Solution is added in mixed liquor v1, in 1000r/min Under the conditions of stir 3 minutes, obtain mixed liquor w1；
(46) material k is added in mixed liquor w1, temperature be 45 DEG C shaking table in shake 15 minutes, be cooled to room temperature After be filtered to remove liquid and obtain material l1, material l1 is after the washing with alcohol that 100ml mass percent concentration is 93% at 88 DEG C Drying baker in place 112 minutes, be subsequently placed in Muffle furnace roasting 58 minutes under the conditions of 508 DEG C, obtain material z1；
(47) haucl for 0.76mol/l by 69ml molar concentration4Solution is added in mixed liquor v2, in 1000r/min Under the conditions of stir 3 minutes, obtain mixed liquor w2；
(48) material z1 is added in mixed liquor w2, temperature be 45 DEG C shaking table in shake 15 minutes, be cooled to room It is filtered to remove liquid after temperature and obtains material l2, material l2 is after the washing with alcohol that 100ml mass percent concentration is 93% 88 DEG C drying baker in place 112 minutes, be subsequently placed in Muffle furnace roasting 58 minutes under the conditions of 508 DEG C, obtain material z2；
(49) haucl for 0.56mol/l by 49ml molar concentration4Solution is added in mixed liquor v3, in 1000r/min Under the conditions of stir 3 minutes, obtain mixed liquor w3；
(50) material z2 is added in mixed liquor w3, temperature be 45 DEG C shaking table in shake 15 minutes, be cooled to room It is filtered to remove liquid after temperature and obtains material l3, material l3 is after the washing with alcohol that 100ml mass percent concentration is 93% 88 DEG C drying baker in place 112 minutes, be subsequently placed in Muffle furnace roasting 58 minutes under the conditions of 508 DEG C, the material obtaining is Remove the modified quartz particles electrode of furan function for having electro-catalysis.
The invention has the beneficial effects as follows, the prepared modified quartz particles electrode with electro-catalysis removal furan function has Current efficiency is high, stability is strong, electrode life length, high to furan removal efficiency the features such as.
Specific embodiment
The present invention provides a kind of modified quartz particles electrode with electro-catalysis removal furan function and preparation method, below Illustrate in fact to apply process by an example.
Embodiment 1.
(1) put in 500ml beaker after the 98g quartz particles 1000ml deionized water wash being 2～4mm by particle diameter, Add the hydrochloric acid solution that 300ml molar concentration is 0.1mol/l and soak 0.5h, remove liquid after filtration and obtain material a01, will Material a01 is added to the agno that 250ml molar concentration is 1.66mol/l3In solution, temperature be 65 DEG C shaking table in shake 15 Minute, it is filtered to remove liquid after being cooled to room temperature and obtains material a02, material a02 is 95% through 900ml mass percent concentration Place 1.5h in 85 DEG C of drying baker after washing with alcohol, be subsequently placed in Muffle furnace roasting 1h under the conditions of 480 DEG C, obtain thing Matter a1；
(2) 8.34 grams of platinum nitrates and 750ml deionized water being added to volume is in 1000ml conical flask, in 1000r/ Stir 3 minutes under the conditions of min, add 15ml concentrated nitric acid, after shaking up, be divided into 3 parts of equivalent, obtain mixed liquor k1, mixed liquor k2, mix Close liquid k3；
(3) by 817 milligrams of bi (no3)3It is the agno of 0.44mol/l with 37ml molar concentration3Solution is added to mixed liquor k1 In, stir 3 minutes under the conditions of 1000r/min, obtain mixed liquor l1；
(4) material a1 is added in mixed liquor l1, temperature be 45 DEG C shaking table in shake 15 minutes, be cooled to room temperature After be filtered to remove liquid and obtain material a2, material a2 is after the washing with alcohol that 100ml mass percent concentration is 93% at 88 DEG C Drying baker in place 112 minutes, be subsequently placed in Muffle furnace roasting 58 minutes under the conditions of 508 DEG C, obtain material a3；
(5) by 847 milligrams of bi (no3)3It is the agno of 0.64mol/l with 67ml molar concentration3Solution is added to mixed liquor k2 In, stir 3 minutes under the conditions of 1000r/min, obtain mixed liquor l2；
(6) material a3 is added in mixed liquor l2, temperature be 45 DEG C shaking table in shake 15 minutes, be cooled to room temperature After be filtered to remove liquid and obtain material a4, material a4 is after the washing with alcohol that 100ml mass percent concentration is 93% at 88 DEG C Drying baker in place 112 minutes, be subsequently placed in Muffle furnace roasting 58 minutes under the conditions of 508 DEG C, obtain material a5；
(7) by 877 milligrams of bi (no3)3It is the agno of 0.84mol/l with 97ml molar concentration3Solution is added to mixed liquor k3 In, stir 3 minutes under the conditions of 1000r/min, obtain mixed liquor l3；
(8) material a5 is added in mixed liquor l3, temperature be 45 DEG C shaking table in shake 15 minutes, be cooled to room temperature After be filtered to remove liquid and obtain material a6, material a6 is after the washing with alcohol that 100ml mass percent concentration is 93% at 88 DEG C Drying baker in place 112 minutes, be subsequently placed in Muffle furnace roasting 58 minutes under the conditions of 508 DEG C, obtain material a；
(9) by 5.29 grams of agno3Being added to volume with 750ml ether is in 1000ml conical flask, in 1000r/min condition Lower stirring 3 minutes, is divided into 3 parts of equivalent, obtains mixed liquor m1, mixed liquor m2, mixed liquor m3 after shaking up；
(10) by 228 milligrams of agno3It is the bi (no of 0.49mol/l with 46ml molar concentration3)3Solution is added to mixed liquor In m1, stir 3 minutes under the conditions of 1000r/min, obtain mixed liquor n1；
(11) material a is added in mixed liquor n1, temperature be 45 DEG C shaking table in shake 15 minutes, be cooled to room temperature After be filtered to remove liquid and obtain material b, material b is after the washing with alcohol that 100ml mass percent concentration is 93% at 88 DEG C Place 112 minutes in drying baker, be subsequently placed in Muffle furnace roasting 58 minutes under the conditions of 508 DEG C, obtain material b1；
(12) by 258 milligrams of agno3It is the bi (no of 0.69mol/l with 66ml molar concentration3)3Solution is added to mixed liquor In m2, stir 3 minutes under the conditions of 1000r/min, obtain mixed liquor n2；
(13) material b1 is added in mixed liquor n2, temperature be 45 DEG C shaking table in shake 15 minutes, be cooled to room It is filtered to remove liquid after temperature and obtains material b2, material b2 is after the washing with alcohol that 100ml mass percent concentration is 93% 88 DEG C drying baker in place 112 minutes, be subsequently placed in Muffle furnace roasting 58 minutes under the conditions of 508 DEG C, obtain material c；
(14) by 288 milligrams of agno3It is the bi (no of 0.89mol/l with 86ml molar concentration3)3Solution is added to mixed liquor In m3, stir 3 minutes under the conditions of 1000r/min, obtain mixed liquor n3；
(15) material c is added in mixed liquor n3, temperature be 45 DEG C shaking table in shake 15 minutes, be cooled to room temperature After be filtered to remove liquid and obtain material d, material d is after the washing with alcohol that 100ml mass percent concentration is 93% at 88 DEG C Place 112 minutes in drying baker, be subsequently placed in Muffle furnace roasting 58 minutes under the conditions of 508 DEG C, obtain material e；
(16) by 6.98 grams of pb (no3)2Being added to volume with 850ml ethanol is in 1000ml conical flask, in 1000r/min Under the conditions of stir 3 minutes, add 5ml concentrated nitric acid, be divided into 5 parts of equivalent after shaking up, obtain mixed liquor p1, mixed liquor p2, mixed liquor P3, mixed liquor p4, mixed liquor p5；
(17) cecl for 0.77mol/l by 87ml molar concentration3Solution is added in mixed liquor p1, in 1000r/min Under the conditions of stir 3 minutes, obtain mixed liquor q1；
(18) material e is added in mixed liquor q1, temperature be 45 DEG C shaking table in shake 15 minutes, be cooled to room temperature After be filtered to remove liquid and obtain material f1, material f1 is after the washing with alcohol that 100ml mass percent concentration is 93% at 88 DEG C Drying baker in place 112 minutes, be subsequently placed in Muffle furnace roasting 58 minutes under the conditions of 508 DEG C, obtain material f2；
(19) pb (no for 0.86mol/l by 92ml molar concentration3)2Solution is added in mixed liquor p2, in 1000r/ Stir 3 minutes under the conditions of min, obtain mixed liquor q2；
(20) material f2 is added in mixed liquor q2, temperature be 45 DEG C shaking table in shake 15 minutes, be cooled to room It is filtered to remove liquid after temperature and obtains material f3, material f3 is after the washing with alcohol that 100ml mass percent concentration is 93% 88 DEG C drying baker in place 112 minutes, be subsequently placed in Muffle furnace roasting 58 minutes under the conditions of 508 DEG C, obtain material f4；
(21) cecl for 0.57mol/l by 67ml molar concentration3Solution is added in mixed liquor p3, in 1000r/min Under the conditions of stir 3 minutes, obtain mixed liquor q3；
(22) material f4 is added in mixed liquor q3, temperature be 45 DEG C shaking table in shake 15 minutes, be cooled to room It is filtered to remove liquid after temperature and obtains material f5, material f5 is after the washing with alcohol that 100ml mass percent concentration is 93% 88 DEG C drying baker in place 112 minutes, be subsequently placed in Muffle furnace roasting 58 minutes under the conditions of 508 DEG C, obtain material f6；
(23) pb (no for 0.66mol/l by 72ml molar concentration3)2Solution is added in mixed liquor p4, in 1000r/ Stir 3 minutes under the conditions of min, obtain mixed liquor q4；
(24) material f6 is added in mixed liquor q4, temperature be 45 DEG C shaking table in shake 15 minutes, be cooled to room It is filtered to remove liquid after temperature and obtains material f7, material f7 is after the washing with alcohol that 100ml mass percent concentration is 93% 88 DEG C drying baker in place 112 minutes, be subsequently placed in Muffle furnace roasting 58 minutes under the conditions of 508 DEG C, obtain material f8；
(25) cecl for 0.37mol/l by 47ml molar concentration3Solution and 52ml molar concentration are the pb of 0.46mol/l (no3)2Solution is added in mixed liquor p5, stirs 3 minutes, obtain mixed liquor q5 under the conditions of 1000r/min；
(26) material f8 is added in mixed liquor q5, temperature be 45 DEG C shaking table in shake 15 minutes, be cooled to room It is filtered to remove liquid after temperature and obtains material f9, material f9 is after the washing with alcohol that 100ml mass percent concentration is 93% 88 DEG C drying baker in place 112 minutes, be subsequently placed in Muffle furnace roasting 58 minutes under the conditions of 508 DEG C, obtain material f；
(27) by 5.98g zrcl4It is added to volume with the sodium citrate solution that 750ml mass percent concentration is 10% For, in 1000ml conical flask, stirring 3 minutes under the conditions of 1000r/min, being divided into 3 parts of equivalent after shaking up, obtain mixed liquor r1, mix Close liquid r2, mixed liquor r3；
(28) mgcl for 0.39mol/l by 35ml molar concentration2Solution and 65ml molar concentration are 0.84mol/l's cdcl2Solution is added in mixed liquor r1, stirs 3 minutes, obtain mixed liquor s1 under the conditions of 1000r/min；
(29) material f is added in mixed liquor s1, temperature be 45 DEG C shaking table in shake 15 minutes, be cooled to room temperature After be filtered to remove liquid and obtain material g1, material g1 is after the washing with alcohol that 100ml mass percent concentration is 93% at 88 DEG C Drying baker in place 112 minutes, be subsequently placed in Muffle furnace roasting 58 minutes under the conditions of 508 DEG C, obtain material h1；
(30) mgcl for 0.59mol/l by 55ml molar concentration2Solution and 45ml molar concentration are 0.64mol/l's cdcl2Solution is added in mixed liquor r2, stirs 3 minutes, obtain mixed liquor s2 under the conditions of 1000r/min；
(31) material h1 is added in mixed liquor s2, temperature be 45 DEG C shaking table in shake 15 minutes, be cooled to room It is filtered to remove liquid after temperature and obtains material g2, material g2 is after the washing with alcohol that 100ml mass percent concentration is 93% 88 DEG C drying baker in place 112 minutes, be subsequently placed in Muffle furnace roasting 58 minutes under the conditions of 508 DEG C, obtain material h2；
(32) mgcl for 0.79mol/l by 75ml molar concentration2Solution and 25ml molar concentration are 0.44mol/l's cdcl2Solution is added in mixed liquor r3, stirs 3 minutes, obtain mixed liquor s3 under the conditions of 1000r/min；
(33) material h2 is added in mixed liquor s3, temperature be 45 DEG C shaking table in shake 15 minutes, be cooled to room It is filtered to remove liquid after temperature and obtains material g3, material g3 is after the washing with alcohol that 100ml mass percent concentration is 93% 88 DEG C drying baker in place 112 minutes, be subsequently placed in Muffle furnace roasting 58 minutes under the conditions of 508 DEG C, obtain material h；
(34) 4.55g sodium lauryl sulphate, 40ml normal hexane, 20 milliliters of n-butyl alcohol are added sequentially to volume and are In 250ml conical flask, add 8.31g ammonium 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；
(35) material i and sodium citrate solution that 800ml mass percent concentration is 15% being added to volume is In 1000ml conical flask, stir 3 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；
(36) mgcl for 0.41mol/l by 33ml molar concentration2Solution and 67ml molar concentration are 0.88mol/l's cdcl2Solution is added in mixed liquor t1, stirs 3 minutes, obtain mixed liquor u1 under the conditions of 1000r/min；
(37) material h is added in mixed liquor u1, temperature be 45 DEG C shaking table in shake 15 minutes, be cooled to room temperature After be filtered to remove liquid and obtain material j1, material j1 is after the washing with alcohol that 100ml mass percent concentration is 93% at 88 DEG C Drying baker in place 112 minutes, be subsequently placed in Muffle furnace roasting 58 minutes under the conditions of 508 DEG C, obtain material k1；
(38) mgcl for 0.51mol/l by 43ml molar concentration2Solution and 57ml molar concentration are 0.78mol/l's cdcl2Solution is added in mixed liquor t2, stirs 3 minutes, obtain mixed liquor u2 under the conditions of 1000r/min；
(39) material k1 is added in mixed liquor u2, temperature be 45 DEG C shaking table in shake 15 minutes, be cooled to room It is filtered to remove liquid after temperature and obtains material j2, material j2 is after the washing with alcohol that 100ml mass percent concentration is 93% 88 DEG C drying baker in place 112 minutes, be subsequently placed in Muffle furnace roasting 58 minutes under the conditions of 508 DEG C, obtain material k2；
(40) mgcl for 0.61mol/l by 53ml molar concentration2Solution and 47ml molar concentration are 0.68mol/l's cdcl2Solution is added in mixed liquor t3, stirs 3 minutes, obtain mixed liquor u3 under the conditions of 1000r/min；
(41) material k2 is added in mixed liquor u3, temperature be 45 DEG C shaking table in shake 15 minutes, be cooled to room It is filtered to remove liquid after temperature and obtains material j3, material j3 is after the washing with alcohol that 100ml mass percent concentration is 93% 88 DEG C drying baker in place 112 minutes, be subsequently placed in Muffle furnace roasting 58 minutes under the conditions of 508 DEG C, obtain material k3；
(42) mgcl for 0.71mol/l by 63ml molar concentration2Solution and 37ml molar concentration are 0.58mol/l's cdcl2Solution is added in mixed liquor t4, stirs 3 minutes, obtain mixed liquor u4 under the conditions of 1000r/min；
(43) material k3 is added in mixed liquor u4, temperature be 45 DEG C shaking table in shake 15 minutes, be cooled to room It is filtered to remove liquid after temperature and obtains material j4, material j4 is after the washing with alcohol that 100ml mass percent concentration is 93% 88 DEG C drying baker in place 112 minutes, be subsequently placed in Muffle furnace roasting 58 minutes under the conditions of 508 DEG C, obtain material k；
(44) 9.66g polyvinyl alcohol and 900ml deionized water being added to volume is in 1000ml conical flask, in 1000r/ Stir 3 minutes under the conditions of min, be divided into 3 parts of equivalent after shaking up, obtain mixed liquor v1, mixed liquor v2, mixed liquor v3；
(45) haucl for 0.96mol/l by 89ml molar concentration4Solution is added in mixed liquor v1, in 1000r/min Under the conditions of stir 3 minutes, obtain mixed liquor w1；
(46) material k is added in mixed liquor w1, temperature be 45 DEG C shaking table in shake 15 minutes, be cooled to room temperature After be filtered to remove liquid and obtain material l1, material l1 is after the washing with alcohol that 100ml mass percent concentration is 93% at 88 DEG C Drying baker in place 112 minutes, be subsequently placed in Muffle furnace roasting 58 minutes under the conditions of 508 DEG C, obtain material z1；
(47) haucl for 0.76mol/l by 69ml molar concentration4Solution is added in mixed liquor v2, in 1000r/min Under the conditions of stir 3 minutes, obtain mixed liquor w2；
(48) material z1 is added in mixed liquor w2, temperature be 45 DEG C shaking table in shake 15 minutes, be cooled to room It is filtered to remove liquid after temperature and obtains material l2, material l2 is after the washing with alcohol that 100ml mass percent concentration is 93% 88 DEG C drying baker in place 112 minutes, be subsequently placed in Muffle furnace roasting 58 minutes under the conditions of 508 DEG C, obtain material z2；
(49) haucl for 0.56mol/l by 49ml molar concentration4Solution is added in mixed liquor v3, in 1000r/min Under the conditions of stir 3 minutes, obtain mixed liquor w3；
(50) material z2 is added in mixed liquor w3, temperature be 45 DEG C shaking table in shake 15 minutes, be cooled to room It is filtered to remove liquid after temperature and obtains material l3, material l3 is after the washing with alcohol that 100ml mass percent concentration is 93% 88 DEG C drying baker in place 112 minutes, be subsequently placed in Muffle furnace roasting 58 minutes under the conditions of 508 DEG C, the material obtaining is Remove the modified quartz particles electrode of furan function for having electro-catalysis.
It is presented herein below and exist with the modified quartz particles electrode with electro-catalysis removal furan function that the inventive method is obtained In electric catalysis reactor, Electro-catalytic Oxidation Process test is carried out to the waste water containing furan, further illustrated the present invention.
The modified quartz particles electrode with electro-catalysis removal furan function that the inventive method is obtained is seated in electricity and urges Change in reactor, Degrading experiment has been carried out to the waste water containing furan, result shows the electric catalysis reactor being loaded by this electrode The furan in waste water can efficiently be removed, when the furan concentration in waste water is 37.7mg/l, be 5.0 in ph, voltage is 14v, Under the conditions of process time is 45min, the furan concentration in water outlet after process is reduced to 1.6mg/l.

Claims (1)

1. a kind of have electro-catalysis remove furan function modified quartz particles electrode preparation method it is characterised in that the party The specifically comprising the following steps that of method
(1) put in 500ml beaker after the 98g quartz particles 1000ml deionized water wash being 2～4mm by particle diameter, add 300ml molar concentration is the hydrochloric acid solution of 0.1mol/l and soaks 0.5h, removes liquid and obtain material a01, by material after filtration A01 is added to the agno that 250ml molar concentration is 1.66mol/l3In solution, temperature be 65 DEG C shaking table in shake 15 points Clock, is filtered to remove liquid and obtains material a02, the second that material a02 is 95% through 900ml mass percent concentration after being cooled to room temperature Place 1.5h in 85 DEG C of drying baker after alcohol washing, be subsequently placed in Muffle furnace roasting 1h under the conditions of 480 DEG C, obtain material a1；
(2) 8.34 grams of platinum nitrates and 750ml deionized water being added to volume is in 1000ml conical flask, in 1000r/min bar Stir 3 minutes under part, add 15ml concentrated nitric acid, be divided into 3 parts of equivalent after shaking up, obtain mixed liquor k1, mixed liquor k2, mixed liquor k3；
(3) by 817 milligrams of bi (no3)3It is the agno of 0.44mol/l with 37ml molar concentration3Solution is added in mixed liquor k1, Stir 3 minutes under the conditions of 1000r/min, obtain mixed liquor l1；
(4) material a1 is added in mixed liquor l1, temperature be 45 DEG C shaking table in shake 15 minutes, be cooled to mistake after room temperature Filter liquid and obtain material a2, material a2 is dry at 88 DEG C after the washing with alcohol that 100ml mass percent concentration is 93% Place 112 minutes in dry case, be subsequently placed in Muffle furnace roasting 58 minutes under the conditions of 508 DEG C, obtain material a3；
(5) by 847 milligrams of bi (no3)3It is the agno of 0.64mol/l with 67ml molar concentration3Solution is added in mixed liquor k2, Stir 3 minutes under the conditions of 1000r/min, obtain mixed liquor l2；
(6) material a3 is added in mixed liquor l2, temperature be 45 DEG C shaking table in shake 15 minutes, be cooled to mistake after room temperature Filter liquid and obtain material a4, material a4 is dry at 88 DEG C after the washing with alcohol that 100ml mass percent concentration is 93% Place 112 minutes in dry case, be subsequently placed in Muffle furnace roasting 58 minutes under the conditions of 508 DEG C, obtain material a5；
(7) by 877 milligrams of bi (no3)3It is the agno of 0.84mol/l with 97ml molar concentration3Solution is added in mixed liquor k3, Stir 3 minutes under the conditions of 1000r/min, obtain mixed liquor l3；
(8) material a5 is added in mixed liquor l3, temperature be 45 DEG C shaking table in shake 15 minutes, be cooled to mistake after room temperature Filter liquid and obtain material a6, material a6 is dry at 88 DEG C after the washing with alcohol that 100ml mass percent concentration is 93% Place 112 minutes in dry case, be subsequently placed in Muffle furnace roasting 58 minutes under the conditions of 508 DEG C, obtain material a；
(9) by 5.29 grams of agno3Being added to volume with 750ml ether is in 1000ml conical flask, stirs under the conditions of 1000r/min Mix 3 minutes, after shaking up, be divided into 3 parts of equivalent, obtain mixed liquor m1, mixed liquor m2, mixed liquor m3；
(10) by 228 milligrams of agno3It is the bi (no of 0.49mol/l with 46ml molar concentration3)3Solution is added in mixed liquor m1, Stir 3 minutes under the conditions of 1000r/min, obtain mixed liquor n1；
(11) material a is added in mixed liquor n1, temperature be 45 DEG C shaking table in shake 15 minutes, be cooled to mistake after room temperature Filter liquid and obtain material b, material b is after the washing with alcohol that 100ml mass percent concentration is 93% in 88 DEG C of drying Place 112 minutes in case, be subsequently placed in Muffle furnace roasting 58 minutes under the conditions of 508 DEG C, obtain material b1；
(12) by 258 milligrams of agno3It is the bi (no of 0.69mol/l with 66ml molar concentration3)3Solution is added in mixed liquor m2, Stir 3 minutes under the conditions of 1000r/min, obtain mixed liquor n2；
(13) material b1 is added in mixed liquor n2, temperature be 45 DEG C shaking table in shake 15 minutes, after being cooled to room temperature It is filtered to remove liquid and obtains material b2, material b2 is after the washing with alcohol that 100ml mass percent concentration is 93% at 88 DEG C Place 112 minutes in drying baker, be subsequently placed in Muffle furnace roasting 58 minutes under the conditions of 508 DEG C, obtain material c；
(14) by 288 milligrams of agno3It is the bi (no of 0.89mol/l with 86ml molar concentration3)3Solution is added in mixed liquor m3, Stir 3 minutes under the conditions of 1000r/min, obtain mixed liquor n3；
(15) material c is added in mixed liquor n3, temperature be 45 DEG C shaking table in shake 15 minutes, be cooled to mistake after room temperature Filter liquid and obtain material d, material d is after the washing with alcohol that 100ml mass percent concentration is 93% in 88 DEG C of drying Place 112 minutes in case, be subsequently placed in Muffle furnace roasting 58 minutes under the conditions of 508 DEG C, obtain material e；
(16) by 6.98 grams of pb (no3)2Being added to volume with 850ml ethanol is in 1000ml conical flask, in 1000r/min condition Lower stirring 3 minutes, adds 5ml concentrated nitric acid, is divided into 5 parts of equivalent after shaking up, and obtains mixed liquor p1, mixed liquor p2, mixed liquor p3, mixes Close liquid p4, mixed liquor p5；
(17) cecl for 0.77mol/l by 87ml molar concentration3Solution is added in mixed liquor p1, under the conditions of 1000r/min Stirring 3 minutes, obtains mixed liquor q1；
(18) material e is added in mixed liquor q1, temperature be 45 DEG C shaking table in shake 15 minutes, be cooled to mistake after room temperature Filter liquid and obtain material f1, material f1 is dry at 88 DEG C after the washing with alcohol that 100ml mass percent concentration is 93% Place 112 minutes in dry case, be subsequently placed in Muffle furnace roasting 58 minutes under the conditions of 508 DEG C, obtain material f2；
(19) pb (no for 0.86mol/l by 92ml molar concentration3)2Solution is added in mixed liquor p2, in 1000r/min bar Stir 3 minutes under part, obtain mixed liquor q2；
(20) material f2 is added in mixed liquor q2, temperature be 45 DEG C shaking table in shake 15 minutes, after being cooled to room temperature It is filtered to remove liquid and obtains material f3, material f3 is after the washing with alcohol that 100ml mass percent concentration is 93% at 88 DEG C Place 112 minutes in drying baker, be subsequently placed in Muffle furnace roasting 58 minutes under the conditions of 508 DEG C, obtain material f4；
(21) cecl for 0.57mol/l by 67ml molar concentration3Solution is added in mixed liquor p3, under the conditions of 1000r/min Stirring 3 minutes, obtains mixed liquor q3；
(22) material f4 is added in mixed liquor q3, temperature be 45 DEG C shaking table in shake 15 minutes, after being cooled to room temperature It is filtered to remove liquid and obtains material f5, material f5 is after the washing with alcohol that 100ml mass percent concentration is 93% at 88 DEG C Place 112 minutes in drying baker, be subsequently placed in Muffle furnace roasting 58 minutes under the conditions of 508 DEG C, obtain material f6；
(23) pb (no for 0.66mol/l by 72ml molar concentration3)2Solution is added in mixed liquor p4, in 1000r/min bar Stir 3 minutes under part, obtain mixed liquor q4；
(24) material f6 is added in mixed liquor q4, temperature be 45 DEG C shaking table in shake 15 minutes, after being cooled to room temperature It is filtered to remove liquid and obtains material f7, material f7 is after the washing with alcohol that 100ml mass percent concentration is 93% at 88 DEG C Place 112 minutes in drying baker, be subsequently placed in Muffle furnace roasting 58 minutes under the conditions of 508 DEG C, obtain material f8；
(25) cecl for 0.37mol/l by 47ml molar concentration3Solution and 52ml molar concentration are the pb of 0.46mol/l (no3)2Solution is added in mixed liquor p5, stirs 3 minutes, obtain mixed liquor q5 under the conditions of 1000r/min；
(26) material f8 is added in mixed liquor q5, temperature be 45 DEG C shaking table in shake 15 minutes, after being cooled to room temperature It is filtered to remove liquid and obtains material f9, material f9 is after the washing with alcohol that 100ml mass percent concentration is 93% at 88 DEG C Place 112 minutes in drying baker, be subsequently placed in Muffle furnace roasting 58 minutes under the conditions of 508 DEG C, obtain material f；
(27) by 5.98g zrcl4Being added to volume with the sodium citrate solution that 750ml mass percent concentration is 10% is In 1000ml conical flask, stir 3 minutes under the conditions of 1000r/min, be divided into 3 parts of equivalent after shaking up, obtain mixed liquor r1, mixing Liquid r2, mixed liquor r3；
(28) mgcl for 0.39mol/l by 35ml molar concentration2Solution and 65ml molar concentration are the cdcl of 0.84mol/l2Molten Liquid is added in mixed liquor r1, stirs 3 minutes, obtain mixed liquor s1 under the conditions of 1000r/min；
(29) material f is added in mixed liquor s1, temperature be 45 DEG C shaking table in shake 15 minutes, be cooled to mistake after room temperature Filter liquid and obtain material g1, material g1 is dry at 88 DEG C after the washing with alcohol that 100ml mass percent concentration is 93% Place 112 minutes in dry case, be subsequently placed in Muffle furnace roasting 58 minutes under the conditions of 508 DEG C, obtain material h1；
(30) mgcl for 0.59mol/l by 55ml molar concentration2Solution and 45ml molar concentration are the cdcl of 0.64mol/l2Molten Liquid is added in mixed liquor r2, stirs 3 minutes, obtain mixed liquor s2 under the conditions of 1000r/min；
(31) material h1 is added in mixed liquor s2, temperature be 45 DEG C shaking table in shake 15 minutes, after being cooled to room temperature It is filtered to remove liquid and obtains material g2, material g2 is after the washing with alcohol that 100ml mass percent concentration is 93% at 88 DEG C Place 112 minutes in drying baker, be subsequently placed in Muffle furnace roasting 58 minutes under the conditions of 508 DEG C, obtain material h2；
(32) mgcl for 0.79mol/l by 75ml molar concentration2Solution and 25ml molar concentration are the cdcl of 0.44mol/l2Molten Liquid is added in mixed liquor r3, stirs 3 minutes, obtain mixed liquor s3 under the conditions of 1000r/min；
(33) material h2 is added in mixed liquor s3, temperature be 45 DEG C shaking table in shake 15 minutes, after being cooled to room temperature It is filtered to remove liquid and obtains material g3, material g3 is after the washing with alcohol that 100ml mass percent concentration is 93% at 88 DEG C Place 112 minutes in drying baker, be subsequently placed in Muffle furnace roasting 58 minutes under the conditions of 508 DEG C, obtain material h；
(34) 4.55g sodium lauryl sulphate, 40ml normal hexane, 20 milliliters of n-butyl alcohol are added sequentially to volume and bore for 250ml In shape bottle, add 8.31g ammonium metavanadate and 150ml deionized water, be placed in 70 DEG C of water-baths and stir under the conditions of 1000r/min 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, cold But it is centrifuged 15min under the conditions of 7500r/min to after room temperature, remove supernatant, be 95% with 500ml mass percent concentration Washing with alcohol, obtains material i；
(35) 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 3 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；
(36) mgcl for 0.41mol/l by 33ml molar concentration2Solution and 67ml molar concentration are the cdcl of 0.88mol/l2Molten Liquid is added in mixed liquor t1, stirs 3 minutes, obtain mixed liquor u1 under the conditions of 1000r/min；
(37) material h is added in mixed liquor u1, temperature be 45 DEG C shaking table in shake 15 minutes, be cooled to mistake after room temperature Filter liquid and obtain material j1, material j1 is dry at 88 DEG C after the washing with alcohol that 100ml mass percent concentration is 93% Place 112 minutes in dry case, be subsequently placed in Muffle furnace roasting 58 minutes under the conditions of 508 DEG C, obtain material k1；
(38) mgcl for 0.51mol/l by 43ml molar concentration2Solution and 57ml molar concentration are the cdcl of 0.78mol/l2Molten Liquid is added in mixed liquor t2, stirs 3 minutes, obtain mixed liquor u2 under the conditions of 1000r/min；
(39) material k1 is added in mixed liquor u2, temperature be 45 DEG C shaking table in shake 15 minutes, after being cooled to room temperature It is filtered to remove liquid and obtains material j2, material j2 is after the washing with alcohol that 100ml mass percent concentration is 93% at 88 DEG C Place 112 minutes in drying baker, be subsequently placed in Muffle furnace roasting 58 minutes under the conditions of 508 DEG C, obtain material k2；
(40) mgcl for 0.61mol/l by 53ml molar concentration2Solution and 47ml molar concentration are the cdcl of 0.68mol/l2Molten Liquid is added in mixed liquor t3, stirs 3 minutes, obtain mixed liquor u3 under the conditions of 1000r/min；
(41) material k2 is added in mixed liquor u3, temperature be 45 DEG C shaking table in shake 15 minutes, after being cooled to room temperature It is filtered to remove liquid and obtains material j3, material j3 is after the washing with alcohol that 100ml mass percent concentration is 93% at 88 DEG C Place 112 minutes in drying baker, be subsequently placed in Muffle furnace roasting 58 minutes under the conditions of 508 DEG C, obtain material k3；
(42) mgcl for 0.71mol/l by 63ml molar concentration2Solution and 37ml molar concentration are the cdcl of 0.58mol/l2Molten Liquid is added in mixed liquor t4, stirs 3 minutes, obtain mixed liquor u4 under the conditions of 1000r/min；
(43) material k3 is added in mixed liquor u4, temperature be 45 DEG C shaking table in shake 15 minutes, after being cooled to room temperature It is filtered to remove liquid and obtains material j4, material j4 is after the washing with alcohol that 100ml mass percent concentration is 93% at 88 DEG C Place 112 minutes in drying baker, be subsequently placed in Muffle furnace roasting 58 minutes under the conditions of 508 DEG C, obtain material k；
(44) 9.66g polyvinyl alcohol and 900ml deionized water being added to volume is in 1000ml conical flask, in 1000r/min Under the conditions of stir 3 minutes, be divided into 3 parts of equivalent after shaking up, obtain mixed liquor v1, mixed liquor v2, mixed liquor v3；
(45) haucl for 0.96mol/l by 89ml molar concentration4Solution is added in mixed liquor v1, in 1000r/min condition Lower stirring 3 minutes, obtains mixed liquor w1；
(46) material k is added in mixed liquor w1, temperature be 45 DEG C shaking table in shake 15 minutes, be cooled to mistake after room temperature Filter liquid and obtain material l1, material l1 is dry at 88 DEG C after the washing with alcohol that 100ml mass percent concentration is 93% Place 112 minutes in dry case, be subsequently placed in Muffle furnace roasting 58 minutes under the conditions of 508 DEG C, obtain material z1；
(47) haucl for 0.76mol/l by 69ml molar concentration4Solution is added in mixed liquor v2, in 1000r/min condition Lower stirring 3 minutes, obtains mixed liquor w2；
(48) material z1 is added in mixed liquor w2, temperature be 45 DEG C shaking table in shake 15 minutes, after being cooled to room temperature It is filtered to remove liquid and obtains material l2, material l2 is after the washing with alcohol that 100ml mass percent concentration is 93% at 88 DEG C Place 112 minutes in drying baker, be subsequently placed in Muffle furnace roasting 58 minutes under the conditions of 508 DEG C, obtain material z2；
(49) haucl for 0.56mol/l by 49ml molar concentration4Solution is added in mixed liquor v3, in 1000r/min condition Lower stirring 3 minutes, obtains mixed liquor w3；
(50) material z2 is added in mixed liquor w3, temperature be 45 DEG C shaking table in shake 15 minutes, after being cooled to room temperature It is filtered to remove liquid and obtains material l3, material l3 is after the washing with alcohol that 100ml mass percent concentration is 93% at 88 DEG C Place 112 minutes in drying baker, be subsequently placed in Muffle furnace roasting 58 minutes under the conditions of 508 DEG C, the material obtaining is to be had Electro-catalysis is had to remove the modified quartz particles electrode of furan function.
CN201611039126.5A 2016-11-21 2016-11-21 Modified quartz particle electrode with function of removing furan through electrocatalysis and preparation method thereof Withdrawn CN106348403A (en)

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1526652A (en) * 2003-09-23 2004-09-08 中国科学院广州地球化学研究所 Continuous circular flow-type optoelectric catalytic fixed bed reactor with 3D electrodes and its organic sewage treating method
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
CN1526652A (en) * 2003-09-23 2004-09-08 中国科学院广州地球化学研究所 Continuous circular flow-type optoelectric catalytic fixed bed reactor with 3D electrodes and its organic sewage treating method
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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