CN106423058A - Method for adsorbing heavy metals and organic matters in water by using graphene sheet-active alumina-carbon nanotube composites - Google Patents

Method for adsorbing heavy metals and organic matters in water by using graphene sheet-active alumina-carbon nanotube composites Download PDF

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Publication number
CN106423058A
CN106423058A CN201610894688.1A CN201610894688A CN106423058A CN 106423058 A CN106423058 A CN 106423058A CN 201610894688 A CN201610894688 A CN 201610894688A CN 106423058 A CN106423058 A CN 106423058A
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graphene film
activated alumina
graphene sheet
graphene
active alumina
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张梅
张一梅
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North China Electric Power University
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North China Electric Power University
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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
    • 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
    • B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
    • B01J20/205—Carbon nanostructures, e.g. nanotubes, nanohorns, nanocones, nanoballs
    • 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
    • B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
    • B01J20/08—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04 comprising aluminium oxide or hydroxide; comprising bauxite
    • 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
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/28—Treatment of water, waste water, or sewage by sorption
    • C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
    • 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
    • B01J2220/00—Aspects relating to sorbent materials
    • B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
    • B01J2220/42—Materials comprising a mixture of inorganic materials
    • 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
    • B01J2220/00—Aspects relating to sorbent materials
    • B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
    • B01J2220/48—Sorbents characterised by the starting material used for their preparation
    • B01J2220/4806—Sorbents characterised by the starting material used for their preparation the starting material being of inorganic character
    • 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 invention discloses a method for adsorbing heavy metals and organic matters in water by using graphene sheet-active alumina-carbon nanotube composites. The method comprises the following steps: a, taking active alumina as a matrix and then carrying out pretreatment; b, immersing the pretreated matrix in an ethanol solution containing silane coupling agents, and then adding the matrix to an organic solution containing graphene to obtain graphene sheet-active alumina composites; c, under ultrasonic vibration conditions, fully mixing the graphene sheet-active alumina composites obtained in the step b with carbon nanotubes in an organic solvent to form a graphene sheet-active alumina-carbon nanotube composite solution; d, adding the graphene sheet-active alumina-carbon nanotube composites to wastewater containing the heavy metal ions and the organic matters; e, separating out graphene sheet-carbon nanotube composites by an external magnetic field. By adopting the method for adsorbing the heavy metals and the organic matters in water by using the graphene sheet-active alumina-carbon nanotube composites, a variety of the heavy metal ions can be treated once, furthermore, organic pollutants in water can be further simultaneously treated.

Description

One kind is using weight in graphene film-activated alumina-carbon mano-tube composite absorption water Metal and the method for organic matter
Technical field
The present invention relates to a kind of using graphene film-activated alumina-carbon mano-tube composite adsorbing heavy metal in water and The method of organic matter, belongs to the water treatment field in environmental protection.
Background technology
The toxicity of metal ion is big, distribution is wide, content is low, not degradable, and dispersion exists in the environment for a long time, eventually through The passive plant absorption of bioconcentration, enters human body by food chain, existence and health to the mankind produce serious influence. Therefore, in complex sample, the advanced treating of heavy metal ion just seems very meaningful.
The method removing heavy metal ion in water has ion reduction, co-precipitation, piece filtration, ion exchange and absorption etc..? In these methods absorption method due to have the advantages that relatively low cost, simple to operate, do not produce secondary pollution, regenerating easily, Thus application is than wide.And the performance of adsorbent determines the effect of advanced treating, its selection is key factor therein. Carbon-based sorbing material has stronger adsorption capacity, is widely used in terms of environmental contaminants absorption.Graphene is A kind of carbon-based sorbing material of rising in recent years, it is the periodicity honeybee being formed with hexagonal array by the carbon atom of sp2 hydridization Nest shape two dimension carbonaceous new material, its thickness only has 0.335 nm.In recent years, gradually Graphene was used as adsorption material both at home and abroad Material, uses it for the separation and concentration of environmental contaminants and mensure in aqueous phase, achieves fruitful result, grapheme material exists Substitute traditional adsorbent aspect and present good application prospect.But Graphene is as nano material, in Adsorption of Heavy Metals During ion may itself can cause secondary pollution, be unfavorable for water purification, nano material due to its in subsequent treatment can not Control property, is difficult to apply on a large scale.It is difficult to remove in water body by the use of Graphene as adsorbent in prior art simultaneously simultaneously Simultaneous contents of many kinds of heavy metal ion and organic pollution.
Content of the invention
It is an object of the invention to provide a kind of can achieve removes contents of many kinds of heavy metal ion and the suction of organic pollution simultaneously Attached purification method, and process efficient, quick, simple, pollution-free, thus overcoming deficiency of the prior art.
For achieving the above object, present invention employs following technical scheme：
The present invention provides a kind of using graphene film-activated alumina-carbon mano-tube composite adsorbing heavy metal in water and organic The method of thing, comprises the steps：
A, with activated alumina as matrix, add it in the middle of the organic solution of polyvinyl alcohol, under lasting stirring action, 120 DEG C of reaction 2-5h, are placed in after being dried in baking oven, obtain pretreated matrix, stand-by；
B, by the immersion of pretreated matrix containing the ethanol solution for 0.1-10% silane coupler for the volumetric concentration in the middle of, 20-50 At DEG C, under lasting stirring action, react 1-10h, take out matrix, after drying, then add it to containing 0.1%-10wt% stone In the middle of the organic solution of black alkene, 50-100 DEG C of reaction 1-10h, that is, obtain graphene film-activated alumina compound；
C, under the conditions of sonic oscillation, graphene film-activated alumina compound that step b is obtained is with CNT organic It is sufficiently mixed in solvent, form graphene film-activated alumina-carbon mano-tube composite solution；
D, by graphene film -- activated alumina-carbon mano-tube composite adds in the sewage containing heavy metal ion and organic matter, It is continuously stirred at room temperature, until the hybrid reaction system being formed reaches adsorption equilibrium state, then will be quiet for this hybrid reaction system Put；
E, isolate graphene film-carbon mano-tube composite with externally-applied magnetic field, realize to dirty water purification；
Described graphene film is any one or two in modified redox graphene piece and modified graphene oxide sheet More than kind；Described modified redox graphene piece and modified graphene oxide sheet surface active groups include carboxyl, ring In epoxide, acid chloride group, hydroxyl, sulfydryl, amino and polyethylene glycol any one or two or more；
Described CNT is selected from SWCN, multi-walled carbon nano-tubes, oxidation SWCN, oxidation multi-wall carbon nano-tube In pipe, modified rear oxidation SWCN and modified oxidation multi-wall carbon nano-tube tube any one or two or more.
Organic solvent described in step c is selected from methyl alcohol, ethanol, oxolane, acetone, DMAC N,N' dimethyl acetamide, N- methyl Pyrrolidones, N,N-dimethylformamide any one or two or more.
Coupling agent described in step b is γ-aminopropyl trimethoxysilane, gamma-aminopropyl-triethoxy-silane, 3- Aminopropyl trimethoxysilane, N- β-aminoethyl-γ-aminopropyltriethoxy dimethoxysilane, N- (β-aminoethyl)-γ-ammonia third Ethyl triethoxy silicane alkane, N- β-(aminoethyl)-γ aminopropyl trimethoxysilane, N- (β-aminoethyl)-γ-aminopropyl three ethoxy In base silane, γ-aminopropyltriethoxy diethoxy silane any one or two or more.
Contained graphene film-activated alumina in described graphene film-activated alumina-carbon mano-tube composite solution- The concentration of carbon mano-tube composite is about 10g/L-30g/L.
Described heavy metal ion is Au3+、Fe3+、Ni2+、Cu2+、Mn2+、Cd2+、Pt2+、Cr3+And Pb2+In any one Or it is two or more.
The concentration of heavy metal ion described in step d is 0.05mg/L-200mg/L, the concentration of organic matter described in step d For 50 mg/L -200 mg/L.
Proposed by the present invention using graphene film-activated alumina-carbon mano-tube composite Adsorption of Heavy Metal Ions and having The method of machine thing is a kind of to be suitable for processing the new method of complicated pollutant waste water.Activated alumina has larger specific surface Long-pending, being capable of organic matter in adsorbed water body.Graphene film and CNT are respectively provided with preferable heavy metal adsorption, Graphene Piece, with its huge specific surface area, abundant surface functional group advantage, can be had with heavy metal ions in sewage and difficult degradation Machine thing is fully contacted and adsorbs.CNT plays support effect in system, prevents the reunion of Graphene so that system is abundant Dispersion, simultaneously itself also can Adsorption of Heavy Metal Ions, this composite construction is more beneficial for heavy metal ions in sewage in complex Enrichment in system, precipitation, absorption or complexing.CNT passes through physics from graphene film and chemical mode adsorbs different metals Ion, is suitable for processing the sewage containing contents of many kinds of heavy metal ion, and it is three-dimensional with CNT to have processed the graphene film of sewage Compound can be reclaimed by magnetic field and be reused.
Therefore compared with prior art, outside the features such as present invention has nontoxic, non-secondary pollution, also have and once can process Contents of many kinds of heavy metal ion, process heavy metal ion species is many, and clearance is 99% with first-class advantage.The present invention can also be simultaneously simultaneously Process the organic pollution in water body, clearance is more than 95%.And graphene film-activated alumina-carbon mano-tube composite is also Can be reclaimed by magnetic field and reuse, with low cost.
Specific embodiment
With reference to embodiments technical scheme is described further.
Embodiment 1
A, with activated alumina as matrix, add it in the middle of the organic solution of polyvinyl alcohol, under lasting stirring action, 120 DEG C of reaction 4h, are placed in after being dried in baking oven, obtain pretreated matrix, stand-by；
B, the ethanol solution of the 3- aminopropyl trimethoxysilane being 5% containing volumetric concentration by the immersion of pretreated matrix are worked as In, at 40 DEG C, under lasting stirring action, react 5h, take out matrix, after drying, then add it to containing 6wt% Graphene Organic solution in the middle of, 100 DEG C reaction 4h, that is, obtain graphene film-activated alumina compound；
C, under the conditions of sonic oscillation, add graphene film-activated alumina compound of obtaining of 5g step b, 95ml tetrahydrochysene furan Mutter, constantly stir, be simultaneously introduced the oxidation SWCN tetrahydrofuran solution of 100ml 10g/L, after adding, continue to stir Mix and be sufficiently mixed under 20min, room temperature, form compound；
D, the complex solution obtaining step c are added to 1L and contain Au3+、Fe3+、Ni2+、Cu2+、Mn2+、Cd2+、Pt2+、Cr3+And Pb2+ Each ion concentration is 50mg/L, in the sewage containing 80 mg/L pentachlorophenols, after process 1h is stirred at room temperature, stands 30min, makes to reach To adsorption equilibrium；
E, with magnetic field collect compound after, take the atomic absorption spectrum of the sewage after process detect each heavy metal ion content, send out Existing clearance is attained by more than 99%；
Table 1 is graphene film-activated alumina-carbon mano-tube composite described in embodiment 1 to Au3+、Fe3+、Ni2+、Cu2+、 Mn2+、Cd2+、Pt2+、Cr3+And Pb2+And the clearance data of pentachlorophenol.As seen from the table graphene film-activated alumina- Carbon mano-tube composite is to Au3+、Fe3+、Ni2+、Cu2+、Mn2+、Cd2+、Pt2+、Pb2+And Cr3+Clearance be respectively 99.5%, 99.2%th, 99.1%, 99.5%, 99.2%, 99.5%, 99.1%, 99.3%, 99.6%, the clearance to pentachlorophenol is 95.0%
The clearance to 6 heavy metal species ions for the table 1. graphene-carbon nano tube three-dimensional composite system
Ion Au3+ Fe3+ Ni2+ Cu2+ Mn2+ Cd2+ Pt2+ Pb2+ Cr3+ Pentachlorophenol
Clearance 99.5% 99.2% 99.1% 99.5% 99.2% 99.5% 99.1% 99.3% 99.6% 95.0%

Claims (6)

1. a kind of method of utilization graphene film-activated alumina-carbon mano-tube composite adsorbing heavy metal in water and organic matter, It is characterized in that comprising the steps：
A, with activated alumina as matrix, add it in the middle of the organic solution of polyvinyl alcohol, under lasting stirring action, 120 DEG C of reaction 2-5h, are placed in after being dried in baking oven, obtain pretreated matrix, stand-by；
B, by the immersion of pretreated matrix containing the ethanol solution for 0.1-10% silane coupler for the volumetric concentration in the middle of, 20-50 At DEG C, under lasting stirring action, react 1-10h, take out matrix, after drying, then add it to containing 0.1%-10wt% stone In the middle of the organic solution of black alkene, 50-100 DEG C of reaction 1-10h, that is, obtain graphene film-activated alumina compound；
C, under the conditions of sonic oscillation, graphene film-activated alumina compound that step b is obtained is with CNT organic It is sufficiently mixed in solvent, form graphene film-activated alumina-carbon mano-tube composite solution；
D, by graphene film -- activated alumina-carbon mano-tube composite adds in the sewage containing heavy metal ion and organic matter, It is continuously stirred at room temperature, until the hybrid reaction system being formed reaches adsorption equilibrium state, then will be quiet for this hybrid reaction system Put；
E, isolate graphene film-carbon mano-tube composite with externally-applied magnetic field, realize to dirty water purification；
Described graphene film is any one or two in modified redox graphene piece and modified graphene oxide sheet More than kind；Described modified redox graphene piece and modified graphene oxide sheet surface active groups include carboxyl, ring In epoxide, acid chloride group, hydroxyl, sulfydryl, amino and polyethylene glycol any one or two or more；
Described CNT is selected from SWCN, multi-walled carbon nano-tubes, oxidation SWCN, oxidation multi-wall carbon nano-tube In pipe, modified rear oxidation SWCN and modified oxidation multi-wall carbon nano-tube tube any one or two or more.
2. the method for claim 1 it is characterised in that：Organic solvent described in step c is selected from methyl alcohol, ethanol, tetrahydrochysene furan Mutter, acetone, DMAC N,N' dimethyl acetamide, 1-METHYLPYRROLIDONE, N,N-dimethylformamide any one or two or more.
3. the method for claim 1 it is characterised in that：Coupling agent described in step b is γ-aminopropyl trimethoxy Base silane, gamma-aminopropyl-triethoxy-silane, 3- aminopropyl trimethoxysilane, N- β-aminoethyl-γ-aminopropyltriethoxy two Methoxy silane, N- (β-aminoethyl)-gamma-aminopropyl-triethoxy-silane, N- β-(aminoethyl)-γ aminopropyl trimethoxy silicon Any one in alkane, N- (β-aminoethyl)-gamma-aminopropyl-triethoxy-silane, γ-aminopropyltriethoxy diethoxy silane Or it is two or more.
4. the method for claim 1 it is characterised in that：Described graphene film-activated alumina-carbon mano-tube composite In solution, the concentration of contained graphene film-activated alumina-carbon mano-tube composite is about 10g/L-30g/L.
5. the either method as described in claim 1-4 it is characterised in that：Described heavy metal ion is Au3+、Fe3+、Ni2+、Cu2 +、Mn2+、Cd2+、Pt2+、Cr3+And Pb2+In any one or two or more.
6. method as claimed in claim 5 it is characterised in that：The concentration of heavy metal ion described in step d is 0.05mg/L- 200mg/L, the concentration of organic matter described in step d is 50 mg/L -200 mg/L.
CN201610894688.1A 2016-10-14 2016-10-14 Method for adsorbing heavy metals and organic matters in water by using graphene sheet-active alumina-carbon nanotube composites Pending CN106423058A (en)

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Cited By (7)

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CN106902762A (en) * 2017-03-31 2017-06-30 济南大学 A kind of preparation and application of magnetic aerobic particle mud graphene oxide multi-walled carbon nano-tubes compound adsorbent
CN107512917A (en) * 2017-08-24 2017-12-26 浙江科屹耐火材料有限公司 A kind of flame-retardant fibre board
CN108043366A (en) * 2017-12-29 2018-05-18 徐州得铸生物科技有限公司 The nanocomposite of calcium ions and magnesium ions in a kind of absorption water
CN108176356A (en) * 2017-12-31 2018-06-19 安徽万方织染有限公司 A kind of preparation process of environmentally protective high adsorption activity dyeing waste water adsorbent
CN110420622A (en) * 2019-08-01 2019-11-08 合肥学院 The preparation method of the graphene oxide hybridized film of copper ion in a kind of removing water
CN111514868A (en) * 2020-04-09 2020-08-11 华东师范大学 Magnetic nano carbon, preparation method thereof and application thereof in removing micro plastic in water
CN112209468A (en) * 2019-07-11 2021-01-12 宣城亨旺新材料有限公司 Method and device for collecting metal by using modified graphene

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Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106902762A (en) * 2017-03-31 2017-06-30 济南大学 A kind of preparation and application of magnetic aerobic particle mud graphene oxide multi-walled carbon nano-tubes compound adsorbent
CN107512917A (en) * 2017-08-24 2017-12-26 浙江科屹耐火材料有限公司 A kind of flame-retardant fibre board
CN108043366A (en) * 2017-12-29 2018-05-18 徐州得铸生物科技有限公司 The nanocomposite of calcium ions and magnesium ions in a kind of absorption water
CN108176356A (en) * 2017-12-31 2018-06-19 安徽万方织染有限公司 A kind of preparation process of environmentally protective high adsorption activity dyeing waste water adsorbent
CN112209468A (en) * 2019-07-11 2021-01-12 宣城亨旺新材料有限公司 Method and device for collecting metal by using modified graphene
CN110420622A (en) * 2019-08-01 2019-11-08 合肥学院 The preparation method of the graphene oxide hybridized film of copper ion in a kind of removing water
CN110420622B (en) * 2019-08-01 2021-12-07 合肥学院 Preparation method of graphene oxide hybrid membrane for removing copper ions in water
CN111514868A (en) * 2020-04-09 2020-08-11 华东师范大学 Magnetic nano carbon, preparation method thereof and application thereof in removing micro plastic in water

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Application publication date: 20170222