CN110124529A - A kind of preparation method and application of graphene oxide/MXene composite membrane - Google Patents

A kind of preparation method and application of graphene oxide/MXene composite membrane Download PDF

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Publication number
CN110124529A
CN110124529A CN201910453450.9A CN201910453450A CN110124529A CN 110124529 A CN110124529 A CN 110124529A CN 201910453450 A CN201910453450 A CN 201910453450A CN 110124529 A CN110124529 A CN 110124529A
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mxene
graphene oxide
composite membrane
solution
preparation
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刘婷
刘晓燕
孙克宁
田隆
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Beijing Institute of Technology BIT
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Beijing Institute of Technology BIT
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
    • B01D67/0079—Manufacture of membranes comprising organic and inorganic components
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
    • B01D69/12—Composite membranes; Ultra-thin membranes
    • 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
    • B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
    • B01J20/0248—Compounds of B, Al, Ga, In, Tl
    • 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
    • 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
    • B01J20/28033—Membrane, sheet, cloth, pad, lamellar or mat
    • 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
    • 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
    • C02F1/288—Treatment of water, waste water, or sewage by sorption using composite sorbents, e.g. coated, impregnated, multi-layered
    • 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
    • C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
    • 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
    • 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
    • C02F2101/308—Dyes; Colorants; Fluorescent agents

Abstract

The present invention provides a kind of graphene oxide/MXene composite membrane preparation method and applications, by graphene oxide solution and MXene solution is proportional is mixed into mixed solution, ultrasound is poured into and is placed in the bottle,suction of microfiltration membranes, by the method for vacuum filter by both two-dimensional material composite loads to micro-filtration film surface to get composite membrane.The pure water flux of graphene oxide (GO)/MXene composite membrane prepared by the present invention is much larger than the flux of pure zirconia graphene film, and with increasing for MXene doping ratio, flux is in increasing trend；And 99.5% or more is up to for the removal rate of the small molecule dyes in water；Method is simple to operation and is easy to scale use, is conducive to promote.

Description

A kind of preparation method and application of graphene oxide/MXene composite membrane
Technical field
The invention belongs to composite membrane technology fields, more particularly, to a kind of graphene oxide/MXene composite membrane preparation side Method and application.
Background technique
The water quality and water of global water resources are worsening, and membrane technology has been to be concerned by more and more people.In water process side Face, main membrane technology to be used include micro-filtration (MF), ultrafiltration (UF), nanofiltration (NF), reverse osmosis (RO) and just permeate (FO), this A little films be mostly use organic high molecular polymer to prepare, but these films water treatment field be still faced with some problems and Challenge, for example pollutant rejection is low, film bad mechanical property, energy consumption are high, some membrane materials not chlorine-resistant etc..Graphene oxide conduct A kind of novel two-dimensional material has superpower elasticity, chemical stability and mechanical strength due to its special molecular structure, Its superior filming performance has potential application in field of membrane material.But it in the nanochannel of graphene oxide, is dispersed with Oxide regions and pure graphene region, hydrone are forming hydrogen bond by oxide regions Shi Huiyu oxygen-containing group, are increasing the stream of water Dynamic resistance causes pure water flux small, it is therefore desirable to find new preparation method to improve the flux of graphene oxide membrane.
Summary of the invention
In view of this, the problem that the present invention is directed to have flux small for existing graphene oxide membrane, proposes a kind of use MXene and graphene oxide is compound prepares graphene oxide (the GO)/MXene composite membrane with high-throughput and high rejection Method, this method remove graphite oxidation at graphene oxide, Ti3AlC2Etching removing passes through the side of vacuum filter at MXene Method is by both two-dimensional material composite loads to 0.45 μm of micro-filtration film surface, for retaining and adsorbing the dyestuff in water.
In order to achieve the above objectives, the technical scheme of the present invention is realized as follows:
A kind of preparation method of graphene oxide/MXene composite membrane, by graphene oxide solution and MXene solution at than Example is mixed into mixed solution, and ultrasound is poured into and is placed in the bottle,suction of microfiltration membranes, by the method for vacuum filter by both two Dimension Material cladding loads to micro-filtration film surface to get composite membrane.
Further, the mass ratio of graphene oxide and MXene are 0.25~4:1 in the mixed solution.
Further, the mass ratio of graphene oxide and MXene are 4:1 or 2:1 or 1:1 or 0.5 in the mixed solution: 1 or 0.25:1.
Further, the preparation of the graphene oxide solution includes the following steps:
To NaNO3In, pour into dense H2SO4, it is placed in water-bath and stirs, crystalline flake graphite is then added, is cooled to 0~10 DEG C； KMnO is added4；React 2h after then heating to 35 DEG C again, be added deionized water, reaction temperature in 98 DEG C of 15~30min of reaction, It is eventually adding hydrogen peroxide and reacts 15~30min, by the centrifugation of obtained product, freezing ultrasound, freeze-drying is solid at graphene oxide Body takes graphene oxide solid to be dissolved in deionized water, is configured to graphene oxide solution.
Graphene oxide is prepared by the method in following document:
Processable aqueous dispersions of graphene nanosheets,Nature Nanotechnology,3(2008)101。
W.S.Hummers,R.E.Offeman,Preparation of Graphitic Oxide,Journal of the American Chemical Society,80(1958)1339-1339。
Further, the preparation of the MXene solution includes the following steps:
It takes LiF to be added in HCl solution, stirs 5~15min, be slowly added to Ti3AlC2, reacted at 35 DEG C for 24 hours, finally Centrifugation obtains Ti3C2TX, single layer MXene nanometer sheet is obtained in ice bath middle probe ultrasound, in freeze-drying at solid, takes MXene solid Body powder is dissolved in deionized water, is configured to MXene solution.
MXene is prepared by the method in following document:
Guidelines for Synthesis and Processing of Two-Dimensional Titanium Carbide(Ti3C2Tx MXene),Chemistry of Materials,29。
Further, the mesh number of the crystalline flake graphite is 200~400 mesh.
Further, the Ti3AlC2Mesh number be 200~400 mesh.
Further, the graphene oxide is first cleaned with 5%HCl solution, and the centrifugal rotational speed time is elder generation 4000rpm centrifugation 8min tri- to four times, supernatant is outwelled, then cleaned with deionized water, the centrifugal rotational speed time is that 8000rpm is centrifuged 8min two to three It is secondary until pH is neutrality, outwell supernatant, last 11800~12000rpm centrifugation 10min takes upper solution.
Further, the MXene is cleaned with deionized water, and the centrifugal rotational speed time is that 3500rpm is centrifuged 5min tri- to four It is secondary, supernatant is outwelled, last 3500rpm is centrifuged 1h.
Further, the graphene oxide freezing ultrasonic time is 1~2h, and MXene is in ice bath middle probe ultrasonic time For 0.5~1h.
The present invention also provides a kind of graphene oxide/application of the MXene composite membrane in sewage treatment, especially cutting Stay and adsorb the application in the dyestuff in water.
The flux of graphene oxide membrane is small, but removal rate is high, and the flux of MXene film is big, and removal rate is relatively low, by the two In conjunction with rear, the flux of composite membrane is big, removal rate is high.On the one hand the addition of MXene makes the interlamellar spacing of film become larger, on the other hand compound The oxygen-containing functional group of film is few, to the drag reduction of water flowing, so that flux increases.
Compared with the existing technology, graphene oxide of the present invention/MXene composite membrane preparation method and application has Following advantage:
Graphene oxide of the present invention/MXene composite membrane preparation method,
1) graphene oxide (the GO)/MXene composite membrane pure water flux prepared is logical much larger than pure zirconia graphene film Amount, with increasing for MXene doping ratio, flux is in increasing trend；
2) graphene oxide (the GO)/MXene composite membrane prepared is up to the removal rate of the small molecule dyes in water 99.5% or more；
3) the method for the present invention is simple to operation and is easy to scale use, is conducive to promote.
Detailed description of the invention
Fig. 1, preparation graphene oxide (GO)/MXene film, compositely proportional be 1:1 scanning electron microscope diagram (SEM)；
Fig. 2, graphene oxide (GO)/MXene film pure water flux figure that load quality is 1mg；
Graphene oxide (GO)/MXene film XRD diagram of Fig. 3, different composite ratio；
The infrared figure of graphene oxide (GO)/MXene film of Fig. 4, different composite ratio；
Figure 5-8, different composite ratio graphene oxide (GO)/MXene film respectively to small molecule dyes (CG, NR, MB, CV) removal rate figure.
Specific embodiment
In addition to being defined, technical term used in following embodiment has universal with those skilled in the art of the invention The identical meanings of understanding.Test reagent used in following embodiment is unless otherwise specified conventional biochemical reagent；It is described Experimental method is unless otherwise specified conventional method.
Below with reference to examples and drawings, the present invention will be described in detail.
Embodiment 1
Graphene oxide (GO)/MXene compositely proportional is the preparation of the film of 1:1
Take 1g NaNO3It is added in beaker, pours into the dense H of 46mL2SO4, it is placed in water-bath and stirs, 2g mesh number is then added For the crystalline flake graphite of 325 mesh, it is cooled to 5 DEG C of stirring 1h；It is slowly added to 6g KMnO4, 1h is added in batches；Then heat to 35 DEG C It reacts 2h again afterwards, is slowly added to 92mL deionized water, it is anti-to be eventually adding appropriate hydrogen peroxide in 98 DEG C of reaction 15min for reaction temperature 30min is answered, obtained product is centrifuged, is first cleaned with 5%HCl solution, the centrifugal rotational speed time is that 4000rpm is centrifuged 8min tri- It is secondary, outwell supernatant, then cleaned with deionized water, the centrifugal rotational speed time be 8000rpm centrifugation 8min three times until pH be it is neutral, Supernatant is outwelled, last 12000rpm centrifugation 10min takes upper solution, and ultrasonic 1h is freeze-dried into solid, 100mg is taken to aoxidize Graphene solid powder is dissolved in 100mL deionized water, is configured to the solution of 1mg/mL.
It takes 1g LiF to be added in 10mL 9M HCl solution, stirs 10min, being slowly added to 0.5g mesh number is 400 purposes Ti3AlC2, react at 35 DEG C for 24 hours, be finally centrifuged, cleaned with deionized water, the centrifugal rotational speed time is that 3500rpm is centrifuged 5min Three times, supernatant is outwelled, last 3500rpm is centrifuged 1h, obtains Ti3C2TX, in ice bath middle probe ultrasound 0.5h, obtain single layer MXene nanometer sheet, then it is freeze-dried into solid, it takes 100mg MXene solid powder to be dissolved in 100mL deionized water, is configured to The solution of 1mg/mL.
The MXene solution of the graphene oxide solution and 0.5mL 1mg/L that take 0.5mL 1mg/L is added to the deionization of 50mL In water, ultrasonic 10min pours into bottle,suction, by the method for vacuum filter by both two-dimensional material composite loads to 0.45 μm Micro-filtration film surface.The film that graphene oxide (GO)/MXene compositely proportional is 1:1 is prepared according to aforesaid operations, as shown in Figure 1, The composite membrane of preparation is stacked in multi-layers, and the thickness of film is about 550nm.
Compositely proportional is 1:0,4:1,2:1,0.5:1,0.25:1, and 0:1 is prepared according to aforesaid operations.
The mechanism of action: the addition of MXene makes the interlamellar spacing of composite membrane become larger, and can be seen that interlamellar spacing from the XRD diagram of Fig. 3 Increase with MXene content and increase, so that pure water flux increases, on the other hand, it can be seen that MXene from the infrared figure of Fig. 4 Addition reduce the amount of the oxygen-containing functional group of composite membrane, thus to the drag reduction of water flowing, so that pure water flux increases.
Experiment:
Filtration of demineralized water is carried out with graphene oxide (GO)/MXene composite membrane, while connecting data display equipment with electronic balance Data are acquired, pure water flux is calculated, as shown in Fig. 2, graphene oxide (GO)/MXene composite membrane pure water of preparation is logical Amount is much larger than the flux of pure zirconia graphene film, and with increasing for MXene doping ratio, flux is also gradually increased.
With graphene oxide (GO)/MXene composite membrane to small molecule dyes Basic Orange (CG), dimethyl diaminophenazine chloride (NR), methylene Blue (MB), crystal violet (CV) solution filtering, solution carries out ultraviolet-uisible spectrophotometer test after taking filter preceding and filter, is calculated Removal rate, as shown in Figure 5-Figure 8, graphene oxide (GO)/MXene composite membrane of preparation are gone for the small molecule dyes in water Except rate is up to 99.5% or more.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention Within mind and principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.

Claims (10)

1. a kind of graphene oxide/MXene composite membrane preparation method, it is characterised in that: by graphene oxide solution and MXene Solution is proportional to be mixed into mixed solution, and ultrasound is poured into and is placed in the bottle,suction of microfiltration membranes, and the method for passing through vacuum filter will Both two-dimensional material composite loads are to micro-filtration film surface to get composite membrane.
2. graphene oxide according to claim 1/MXene composite membrane preparation method, it is characterised in that: mixed solution The mass ratio of middle graphene oxide and MXene are 0.25~4:1.
3. graphene oxide according to claim 2/MXene composite membrane preparation method, it is characterised in that: mixed solution The mass ratio of middle graphene oxide and MXene are 4:1 or 2:1 or 1:1 or 0.5:1 or 0.25:1.
4. graphene oxide according to claim 1/MXene composite membrane preparation method, it is characterised in that: graphite oxide The preparation of alkene solution includes the following steps:
To NaNO3In, pour into dense H2SO4, it is placed in water-bath and stirs, crystalline flake graphite is then added, is cooled to 0~10 DEG C；It is added KMnO4；React 2h after then heating to 35 DEG C again, be added deionized water, reaction temperature in 90~100 DEG C of 15~30min of reaction, It is eventually adding hydrogen peroxide and reacts 15~30min, by the centrifugation of obtained product, freezing ultrasound, freeze-drying is solid at graphene oxide Body takes graphene oxide solid to be dissolved in deionized water, is configured to graphene oxide solution.
5. graphene oxide according to claim 1/MXene composite membrane preparation method, it is characterised in that: MXene is molten The preparation of liquid includes the following steps:
It takes LiF to be added in HCl solution, stirs 5~15min, be slowly added to Ti3AlC2, react at 35 DEG C for 24 hours, be finally centrifuged Obtain Ti3C2TX, single layer MXene nanometer sheet is obtained in ice bath middle probe ultrasound, in freeze-drying at solid, takes MXene solid powder End is dissolved in deionized water, is configured to MXene solution.
6. graphene oxide according to claim 4/MXene composite membrane preparation method, it is characterised in that: crystalline flake graphite Mesh number be 200~400 mesh.
7. graphene oxide according to claim 5/MXene composite membrane preparation method, it is characterised in that: Ti3AlC2's Mesh number is 200~400 mesh.
8. graphene oxide according to claim 4/MXene composite membrane preparation method, it is characterised in that: graphite oxide Alkene is first cleaned with 5%HCl solution, and the centrifugal rotational speed time is that 4000rpm is centrifuged 8min tri- to four times, outwells supernatant, then spend Ionized water cleaning, the centrifugal rotational speed time be 8000rpm centrifugation 8min two to three times until pH be neutrality, outwell supernatant, finally 11800~12000rpm centrifugation 10min takes upper solution.
9. graphene oxide according to claim 5/MXene composite membrane preparation method, it is characterised in that: MXene is used Deionized water cleaning, centrifugal rotational speed time are that 3500rpm is centrifuged 5min tri- to four times, outwell supernatant, last 3500rpm centrifugation 1h。
10. a kind of graphene oxide as described in any one of claims 1-3/application of the MXene composite membrane in sewage treatment.
CN201910453450.9A 2019-05-28 2019-05-28 A kind of preparation method and application of graphene oxide/MXene composite membrane Pending CN110124529A (en)

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CN110559880A (en) * 2019-09-21 2019-12-13 盐城增材科技有限公司 MXene/polyaniline composite membrane for water treatment and preparation method thereof
CN110975655A (en) * 2019-11-22 2020-04-10 成都理工大学 Novel RGO/MXene composite membrane and preparation method thereof
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CN111215021A (en) * 2019-12-03 2020-06-02 中南大学 Titanium carbide/poly (m-phenylenediamine) composite material and preparation method and application thereof
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CN111533130A (en) * 2020-04-23 2020-08-14 厦门理工学院 Preparation method of anthraquinone modified MXene two-dimensional layered material, modified microfiltration membrane and application
CN111629575A (en) * 2020-04-16 2020-09-04 北京服装学院 MXene-based nano composite wave-absorbing material and preparation method thereof
CN112808024A (en) * 2021-01-06 2021-05-18 北京工业大学 MXene-CNT photo-thermal composite membrane for self-floating removal of organic dye and realization of clean water regeneration and preparation method thereof
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CN112999885A (en) * 2021-02-18 2021-06-22 上海工程技术大学 MXene-GO composite membrane with humidity response and preparation method and application thereof
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CN114367204A (en) * 2020-10-14 2022-04-19 天津大学 Graphene oxide-MXene blending cross-linked membrane and preparation method thereof
CN114914100A (en) * 2022-04-12 2022-08-16 武汉工程大学 graphene/MXene composite film and preparation method thereof
CN115259268A (en) * 2022-07-02 2022-11-01 河海大学 Evaporator based on sandwich structure film and preparation method and application thereof

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CN110559880A (en) * 2019-09-21 2019-12-13 盐城增材科技有限公司 MXene/polyaniline composite membrane for water treatment and preparation method thereof
CN110550632B (en) * 2019-09-29 2021-05-28 西南交通大学 MXene/GO hybrid aerogel microsphere wave absorbing agent and preparation method thereof
CN110550632A (en) * 2019-09-29 2019-12-10 西南交通大学 MXene/GO hybrid aerogel microsphere wave absorbing agent and preparation method thereof
CN110975655A (en) * 2019-11-22 2020-04-10 成都理工大学 Novel RGO/MXene composite membrane and preparation method thereof
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Application publication date: 20190816