CN108607526A - It is a kind of to utilize coal ash for manufacturing for SiO2The method of the cuprous adsorbent of gel combined oxidation - Google Patents

It is a kind of to utilize coal ash for manufacturing for SiO2The method of the cuprous adsorbent of gel combined oxidation Download PDF

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Publication number
CN108607526A
CN108607526A CN201810460706.4A CN201810460706A CN108607526A CN 108607526 A CN108607526 A CN 108607526A CN 201810460706 A CN201810460706 A CN 201810460706A CN 108607526 A CN108607526 A CN 108607526A
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Prior art keywords
sio
gel
adsorbent
cuprous
filter residue
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CN201810460706.4A
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Chinese (zh)
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张庆
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Wuhu Baoyi Amusement Equipment Co Ltd
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Wuhu Baoyi Amusement Equipment Co Ltd
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Priority to CN201810460706.4A priority Critical patent/CN108607526A/en
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
    • B01J13/0052—Preparation of gels
    • B01J13/0056—Preparation of gels containing inorganic material and water
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
    • B01J20/103—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate comprising silica
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
    • B01J20/28047—Gels
    • 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
    • C02F1/28—Treatment of water, waste water, or sewage by sorption
    • C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
    • 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
    • C02F2101/10—Inorganic compounds
    • C02F2101/20—Heavy metals or heavy metal compounds

Abstract

The present invention disclose it is a kind of using coal ash for manufacturing for SiO2The method of the cuprous adsorbent of gel combined oxidation makes SiO using flyash as raw material through pickling, alkali carries2Leaching prepares water glass solution, remaining filter residue obtains the manosil AS mineral of porous structure after calcining, there is excellent absorption property to heavy metal ion such as copper, lead in waste water, flyash filter residue after calcining is added during water glass solution forms gel later, obtains the SiO of doping porous mineral particle2Gel；Later using gel rubber system as carrier, cuprous oxide catalysis agent is loaded, microgel three-dimensional network polymer has been synthesized, has improved Cu2O realizes Cu in the dispersion effect and stability of entire sorbent systems2The excellent adsorptivity of gel rubber system is combined with the visible light catalysis activity of cuprous oxide, improves the adsorption capacity and rate to Organic Pollutants in Wastewater, have good removal effect to heavy metal ion and waste water from dyestuff by the recycling of O.

Description

It is a kind of to utilize coal ash for manufacturing for SiO2The method of the cuprous adsorbent of gel combined oxidation
Technical field
The invention belongs to technical field of waste water processing, more particularly, it relates to a kind of standby using coal ash for manufacturing SiO2The method of the cuprous adsorbent of gel combined oxidation.
Technical background
In numerous semiconductor light-catalysts studied, cuprous oxide（Cu2O）It is that last decade carrys out visible light catalytic Research hotspot.Its energy gap is only 2.17eV, can generate photo-generate electron-hole pair by excited by visible light, i.e., in sunlight Irradiation under can cause light-catalyzed reaction, therefore have in terms of visible light photocatalytic degradation of organic pollutants prodigious latent Power.However Cu2After O itself there is also photo-quantum efficiencies relatively low, catalytic degradation waste water the shortcomings of difficult recycling.By being made into load Load type photochemical catalyst or composite photocatalyst are considered as effective method.As activated carbon-loaded cuprous oxide photocatalyst, The cuprous visible light catalyst of carbon nanotube combined oxidation, tripolite loading cuprous oxide catalysis agent etc..
Currently, common adsorbent is some natural or industrial solid adsorbents in wastewater treatment absorption method, as activated carbon, Clay, flyash, Wheat Straw etc..Flyash is the tiny incombustible dissolved that coal is formed in combustion, on surface Usual particle spherical in shape under the action of power.In its forming process, it is quickly cooled down and makes it have very high chemical interior energy, therefore powder Coal ash has preferable chemical reactivity, can be applied to the removal of heavy metal ion and cationic surface active agent in water, But the processing of waste water from dyestuff is reported less.
Invention content
The present invention provides a kind of using coal ash for manufacturing for SiO2The method of the cuprous adsorbent of gel combined oxidation, using this Performance of the adsorbent prepared by inventive method is stablized, and light-catalyzed reaction is efficient.
The present invention uses following technical scheme：
It is a kind of to utilize coal ash for manufacturing for SiO2The method of the cuprous adsorbent of gel combined oxidation, is as follows：
（1）Flyash pickling processes：
Flyash is placed in Muffle furnace and at 550-650 DEG C roast 1.5-3h, takes the flyash after calcining and 4-7mol/L Hydrochloric acid solution is stirred to react, and is reacted 4-6h at 95-100 DEG C, is filtered to reaction solution, filtrate be in light green color, then spend from After sub- water cleaning filter residue 3-5 times, for use；
（2）Alkali carries：
According to solid-to-liquid ratio 1:3-8 takes above-mentioned filter residue to react 4-6h at 95-100 DEG C with the sodium hydroxide solution of 6-10mol/L, Then it is that the mixed liquor of waterglass and sodium hydroxide is placed in after filter residue washing in Muffle furnace to use NaOH weak solution leachings, filtrate 1.5-3h is calcined at 650-800 DEG C, is retained after grinding for use；
（3）SiO2The preparation of gel：
The waterglass and sodium hydroxide mixed liquor for taking above-mentioned preparation, are first added dropwise dilute H of a small amount of 1-3mol/L2SO4, then add Enter filter residue after above-mentioned calcining, stirring makes filter residue be uniformly dispersed in the solution, dilute H is then added dropwise again2SO4, while being stirred with magnetic force Device stirring is mixed, the SiO of doping filter residue is obtained2Colloidal sol impregnates 6-12h with deionized water after colloidal sol gelling, water one is changed every 1-2h It is secondary, soaked in absolute ethyl alcohol is then added and places 3-6h, to replace the aqueous solvent removed in gel, is freeze-dried, obtains later SiO2Gel；
（4）The preparation of adsorbent：
1-5g gels obtained above are immersed to the Cu of a concentration of 0.4-1.0mol/L of 300mL2+Until absorption is flat in aqueous solution Weighing apparatus adds the glucose of a concentration of 0.8-2.0mol/L of 400mL after the NaOH solution of a concentration of 1-3mol/L of 300mL is added Solution, after 40-70 DEG C of water-bath 40-100min, solid is taken out in filtering, is freeze-dried after water washing, obtains SiO2 The cuprous adsorbent of gel combined oxidation.
Wherein, the flyash is the waste of coal-burning power plant's pulverized coal friring discharge, with SiO2And Al2O3Based on, ingredient Account for 70-80%.
Wherein, the Cu2+Aqueous solution refers to copper nitrate or copper sulfate solution.
Wherein, the step（4）Gel immerses Cu2+It is adsorbed using vacuum suck method in aqueous solution, while immersion By container vacuum-pumping, 10-20min, then slow pressure release are kept, keeps 10-20min, then vacuumized, is repeated 3-6 times, until inhaling Attached balance.
The SiO obtained such as above-mentioned preparation method2The cuprous adsorbent of gel combined oxidation can be used for containing organic pollution, again The processing of metallic wastewater.
Compared with prior art, the present invention has the following advantages：
The present invention is using flyash as raw material, the flyash filter residue after pickling, containing active larger SiO2, make SiO through alkali carries2 Leaching prepares water glass solution, and remaining filter residue obtains the manosil AS mineral of porous structure after calcining, to copper, the lead in waste water Etc. heavy metal ion have excellent absorption property, later select sulphur acid as catalyst, water glass solution formed gel mistake Flyash filter residue after calcining is added in journey, after freeze-dried, obtains the SiO of doping porous mineral particle2Gel obtains SiO2Gel has higher porosity and specific surface area, while the carboxyl of gel rubber system is excellent to the absorption property of organic dyestuff It is different, it is greatly improved to the adsorption treatment of heavy metal, organic dye waste water；Later using gel rubber system as carrier, load Cuprous oxide catalysis agent has synthesized microgel three-dimensional network polymer, has improved Cu2O is imitated in the dispersion of entire sorbent systems Fruit and stability, realize Cu2The recycling of O, by the visible light catalytic of gel rubber system excellent adsorptivity and cuprous oxide Activity is combined, and improves adsorption capacity and rate to Organic Pollutants in Wastewater, equal to heavy metal ion and waste water from dyestuff There is good removal effect, realizes the purpose of " treatment of wastes with processes of wastes against one another ".
Specific implementation mode
Embodiment 1
（1）Flyash pickling processes：
Flyash is placed in Muffle furnace and roasts 3h at 600 DEG C, the hydrochloric acid solution of flyash and 6mol/L after calcining is taken to stir It mixes and reacts 5h at 100 DEG C of reaction, reaction solution is filtered, filtrate is in light green color, then cleans filter residue 4 times with deionized water Afterwards, for use；
（2）Alkali carries：
According to solid-to-liquid ratio 1:5, it takes above-mentioned filter residue to react 5h at 100 DEG C with the sodium hydroxide solution of 8mol/L, then uses NaOH Weak solution leaching, filtrate are that the mixed liquor of waterglass and sodium hydroxide is placed in Muffle furnace after filter residue washing at 680 DEG C 2h is calcined, is retained after grinding for use；
（3）SiO2The preparation of gel：
The waterglass and sodium hydroxide mixed liquor for taking above-mentioned preparation, are first added dropwise dilute H of a small amount of 2mol/L2SO4, then it is added Filter residue after above-mentioned calcining, stirring make filter residue be uniformly dispersed in the solution, dilute H are then added dropwise again2SO4, while using magnetic agitation Device stirs, and obtains the SiO of doping filter residue2Colloidal sol, impregnates 12h after colloidal sol gelling with deionized water, and it is primary to change water every 2h, then Soaked in absolute ethyl alcohol is added and places 5h, to replace the aqueous solvent removed in gel, is freeze-dried later, obtains SiO2Gel；
（4）The preparation of adsorbent：
1-5g gels obtained above are immersed in the copper nitrate aqueous solution of 300mL a concentration of 1.0mol/L, immersion while will Container vacuum-pumping keeps 20min, then slow pressure release, keeps 10min, then vacuumized, is repeated 5 times, until adsorption equilibrium, adds After the NaOH solution for entering a concentration of 2mol/L of 300mL, the glucose solution of a concentration of 1.0mol/L of 400mL is added, then at 60 After DEG C water-bath 90min, solid is taken out in filtering, is freeze-dried after water washing, obtains SiO2The cuprous suction of gel combined oxidation Attached dose.

Claims (5)

1. a kind of utilize coal ash for manufacturing for SiO2The method of the cuprous adsorbent of gel combined oxidation, which is characterized in that specific steps are such as Under：
（1）Flyash pickling processes：
Flyash is placed in Muffle furnace and at 550-650 DEG C roast 1.5-3h, takes the flyash after calcining and 4-7mol/L Hydrochloric acid solution is stirred to react, and is reacted 4-6h at 95-100 DEG C, is filtered to reaction solution, filtrate be in light green color, then spend from After sub- water cleaning filter residue 3-5 times, for use；
（2）Alkali carries：
According to solid-to-liquid ratio 1:3-8 takes above-mentioned filter residue to react 4-6h at 95-100 DEG C with the sodium hydroxide solution of 6-10mol/L, Then it is that the mixed liquor of waterglass and sodium hydroxide is placed in after filter residue washing in Muffle furnace to use NaOH weak solution leachings, filtrate 1.5-3h is calcined at 650-800 DEG C, is retained after grinding for use；
（3）SiO2The preparation of gel：
The waterglass and sodium hydroxide mixed liquor for taking above-mentioned preparation, are first added dropwise dilute H of a small amount of 1-3mol/L2SO4, then add Enter filter residue after above-mentioned calcining, stirring makes filter residue be uniformly dispersed in the solution, dilute H is then added dropwise again2SO4, while being stirred with magnetic force Device stirring is mixed, the SiO of doping filter residue is obtained2Colloidal sol impregnates 6-12h with deionized water after colloidal sol gelling, water one is changed every 1-2h It is secondary, soaked in absolute ethyl alcohol is then added and places 3-6h, to replace the aqueous solvent removed in gel, is freeze-dried, obtains later SiO2Gel；
（4）The preparation of adsorbent：
1-5g gels obtained above are immersed to the Cu of a concentration of 0.4-1.0mol/L of 300mL2+Until absorption is flat in aqueous solution Weighing apparatus adds the glucose of a concentration of 0.8-2.0mol/L of 400mL after the NaOH solution of a concentration of 1-3mol/L of 300mL is added Solution, after 40-70 DEG C of water-bath 40-100min, solid is taken out in filtering, is freeze-dried after water washing, obtains SiO2 The cuprous adsorbent of gel combined oxidation.
2. a kind of utilization coal ash for manufacturing according to claim 1, is for SiO2The method of the cuprous adsorbent of gel combined oxidation, It is characterized in that, the flyash is the waste of coal-burning power plant's pulverized coal friring discharge, with SiO2And Al2O3Based on, ingredient accounts for 70-80%。
3. a kind of utilization coal ash for manufacturing according to claim 1, is for SiO2The method of the cuprous adsorbent of gel combined oxidation, It is characterized in that, the Cu2+Aqueous solution refers to copper nitrate or copper sulfate solution.
4. a kind of utilization coal ash for manufacturing according to claim 1, is for SiO2The method of the cuprous adsorbent of gel combined oxidation, It is characterized in that, the step（4）Gel immerses Cu2+It is adsorbed using vacuum suck method in aqueous solution, it will while immersion Container vacuum-pumping keeps 10-20min, then slow pressure release, keeps 10-20min, then vacuumized, and repeats 3-6 times, until absorption Balance.
5. the SiO that the preparation method as described in claim 1-4 is any obtains2The cuprous adsorbent of gel combined oxidation, feature exist In can be used for the processing containing organic pollution, heavy metal wastewater thereby.
CN201810460706.4A 2018-05-15 2018-05-15 It is a kind of to utilize coal ash for manufacturing for SiO2The method of the cuprous adsorbent of gel combined oxidation Withdrawn CN108607526A (en)

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Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109354029A (en) * 2018-11-22 2019-02-19 山西大学 A method of by coal ash for manufacturing for mesopore silicon oxide
CN110302742A (en) * 2019-08-13 2019-10-08 河南昶宜检测技术研究院有限公司 A kind of preparation of the nano material of selective absorption heavy metal and application method
CN110316785A (en) * 2019-07-19 2019-10-11 深圳市深港产学研环保工程技术股份有限公司 Water remediation agent for controlling cyanobacterial bloom and preparation method thereof and eutrophic water body repairing method
CN110590014A (en) * 2019-09-17 2019-12-20 济南大学 Method for purifying electroplating wastewater and application of obtained xerogel in glass
CN111375374A (en) * 2018-12-29 2020-07-07 中国石油化工股份有限公司 Load type copper-based adsorbent and preparation method thereof
CN112408401A (en) * 2020-10-29 2021-02-26 中国建筑材料科学研究总院有限公司 Method for preparing silicon dioxide aerogel by utilizing industrial solid waste fly ash and silicon dioxide aerogel prepared by method
CN112624166A (en) * 2020-12-16 2021-04-09 东南大学 Preparation method of silicon-aluminum-based aerogel and application of prepared silicon-aluminum-based aerogel in aspect of adsorbing heavy metal gas
CN114180985A (en) * 2021-10-11 2022-03-15 河南兴安新型建筑材料有限公司 Ultralow-heat-conductivity autoclaved aerated concrete aerogel composite insulation board and preparation method thereof
CN114349207A (en) * 2021-12-17 2022-04-15 中煤科工集团西安研究院有限公司 Zero-emission high-salt and high-fluorine mine water purification system and process
CN116020398A (en) * 2023-02-22 2023-04-28 西华师范大学 Cuprous cation hydrogel composite adsorbent and preparation method and application thereof

Cited By (15)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109354029A (en) * 2018-11-22 2019-02-19 山西大学 A method of by coal ash for manufacturing for mesopore silicon oxide
CN109354029B (en) * 2018-11-22 2022-03-18 山西大学 Method for preparing mesoporous silicon oxide from fly ash
CN111375374A (en) * 2018-12-29 2020-07-07 中国石油化工股份有限公司 Load type copper-based adsorbent and preparation method thereof
CN110316785B (en) * 2019-07-19 2022-02-11 深圳市深港产学研环保工程技术股份有限公司 Water body repairing agent for controlling cyanobacterial bloom, preparation method thereof and eutrophic water body repairing method
CN110316785A (en) * 2019-07-19 2019-10-11 深圳市深港产学研环保工程技术股份有限公司 Water remediation agent for controlling cyanobacterial bloom and preparation method thereof and eutrophic water body repairing method
CN110302742A (en) * 2019-08-13 2019-10-08 河南昶宜检测技术研究院有限公司 A kind of preparation of the nano material of selective absorption heavy metal and application method
CN110302742B (en) * 2019-08-13 2022-07-01 河南昶宜检测技术研究院有限公司 Preparation and application method of nano material for selectively adsorbing heavy metals
CN110590014A (en) * 2019-09-17 2019-12-20 济南大学 Method for purifying electroplating wastewater and application of obtained xerogel in glass
CN112408401A (en) * 2020-10-29 2021-02-26 中国建筑材料科学研究总院有限公司 Method for preparing silicon dioxide aerogel by utilizing industrial solid waste fly ash and silicon dioxide aerogel prepared by method
CN112624166A (en) * 2020-12-16 2021-04-09 东南大学 Preparation method of silicon-aluminum-based aerogel and application of prepared silicon-aluminum-based aerogel in aspect of adsorbing heavy metal gas
CN112624166B (en) * 2020-12-16 2023-11-17 东南大学 Preparation method of silicon-aluminum-based aerogel and application of prepared silicon-aluminum-based aerogel in heavy metal gas adsorption
CN114180985A (en) * 2021-10-11 2022-03-15 河南兴安新型建筑材料有限公司 Ultralow-heat-conductivity autoclaved aerated concrete aerogel composite insulation board and preparation method thereof
CN114349207A (en) * 2021-12-17 2022-04-15 中煤科工集团西安研究院有限公司 Zero-emission high-salt and high-fluorine mine water purification system and process
CN114349207B (en) * 2021-12-17 2022-11-01 中煤科工集团西安研究院有限公司 Zero-emission-oriented high-salinity and high-fluorine mine water purification system and process
CN116020398A (en) * 2023-02-22 2023-04-28 西华师范大学 Cuprous cation hydrogel composite adsorbent and preparation method and application thereof

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