CN107185411A - It is a kind of in method of the metal cation crosslinking-oxidization graphene nanometer sheet to ultrafiltration membrane modifying - Google Patents
It is a kind of in method of the metal cation crosslinking-oxidization graphene nanometer sheet to ultrafiltration membrane modifying Download PDFInfo
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- CN107185411A CN107185411A CN201710355225.2A CN201710355225A CN107185411A CN 107185411 A CN107185411 A CN 107185411A CN 201710355225 A CN201710355225 A CN 201710355225A CN 107185411 A CN107185411 A CN 107185411A
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- ultrafiltration membrane
- nanometer sheet
- graphene
- metal cation
- stannic oxide
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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
- B01D67/0081—After-treatment of organic or inorganic membranes
- B01D67/0088—Physical treatment with compounds, e.g. swelling, coating or impregnation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
- B01D61/14—Ultrafiltration; Microfiltration
- B01D61/145—Ultrafiltration
-
- 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
- B01D69/02—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor characterised by their properties
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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
- C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
- C02F1/444—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis by ultrafiltration or microfiltration
Abstract
It is disclosed by the invention a kind of in method of the metal cation crosslinking-oxidization graphene nanometer sheet to ultrafiltration membrane modifying, it is related to a kind of method with to ultrafiltration membrane modifying, belongs to environmentally friendly water treatment field.The present invention comprises the following steps：Stannic oxide/graphene nano piece is dissolved into solvent, then cationic cross linking agent is being added；It is to be mixed it is uniform after, under constant-pressure conditions, the stannic oxide/graphene nano piece stacked in multi-layers in solution is loaded into ultrafiltration membrane surface.The stannic oxide/graphene nano piece of the ultrafiltration membrane surface pre-deposition of the present invention retains pollutant by size selection effect, reduces fouling membrane, improves the service life of film, improves water treatment efficiency.The inventive method is simple to operation and is easy to scale and uses, beneficial to popularization.
Description
Technical field
The present invention relates to a kind of in method of the metal cation crosslinking-oxidization graphene nanometer sheet to ultrafiltration membrane modifying, belong to
Environmentally friendly water treatment field.
Background technology
Membrane technology is a kind of water technology of simple and effective, environmentally friendly water treatment field application more and more extensively and by
One of the basis of step as world's strategy of sustainable development.Membrane technology is widely used in every field with its wide applicability
Water process, however, fouling membrane remain hinder membrane technology popularization and application major obstacle.Early stage reduces the main side of fouling membrane
Method is that sewage is carried out a preprocessing process to reduce fouling membrane, and main also most traditional preprocessing process is that chemistry is mixed
It is solidifying.Ultrasound, backwash are carried out to film in addition, also having, the method that the pretreatments such as electric flocculation, electric coagulation are carried out to sewage.But ultrasound is only
Some materials of film adsorption can be removed, and the contaminant particle adsorbed in fenestra can not be removed；Backwash has than super
The more preferable removal efficiency of sound, can remove the particle adsorbed in fenestra, though and chemical flocculation, electric flocculation and electric these methods of coagulation
Fouling membrane can be so reduced to a certain extent, but the chemical reagent added can all cause fouling membrane.Stannic oxide/graphene nano
Piece is employed for membrane modifying as nano material and shows good performance, but traditional utilizes stannic oxide/graphene nano piece to carry out
Membrane modifying, its preparation technology is often extremely complex, long preparation period and cost high, seriously limits stannic oxide/graphene nano piece and exists
Application in terms of membrane modifying.
The content of the invention
The invention aims to the process for solving existing ultrafiltration membrane modifying it is more complicated the problem of there is provided one kind with gold
Belong to method of the cationic crosslinked stannic oxide/graphene nano piece to ultrafiltration membrane modifying.This method exists using metal cation as crosslinking agent
One layer of stannic oxide/graphene nano piece of ultrafiltration membrane surface pre-deposition is as pretreatment, for retaining and adsorbing the pollutant in water, with
The pollution of film is reduced to greatest extent.
The purpose of the present invention is achieved through the following technical solutions.
It is a kind of in method of the metal cation crosslinking-oxidization graphene nanometer sheet to ultrafiltration membrane modifying, graphene oxide is received
Rice piece is dissolved in solvent, then adds crosslinking agent, after being well mixed, obtains solution；Under constant-pressure conditions, by solution
Stannic oxide/graphene nano piece loads to ultrafiltration membrane surface；Solute addition quality and the addition of stannic oxide/graphene nano piece in crosslinking agent
The ratio of quality is 10-13500.
The stannic oxide/graphene nano piece includes：In single-layer graphene oxide nanometer sheet, multilayer graphene oxide nanometer sheet
One or more.
The crosslinking agent is aluminum sulfate, aluminium chloride, aluminum nitrate, ferric sulfate, ferric trichloride, frerrous chloride/potassium manganate, sulfuric acid
Ferrous iron/potassium manganate, frerrous chloride/potassium permanganate or ferrous sulfate/potassium permanganate, and above-mentioned all substances any combination.
The solvent includes deionized water and ethanol.
Preferably, the load capacity of the stannic oxide/graphene nano piece is 20mg/m2-7000mg/m2。
Preferably, the concentration of described crosslinking agent is 0.0001-0.1M (mol/L)；
Preferably, described stannic oxide/graphene nano piece is 1-100 layers
Preferably, described constant pressure is 0.05-0.4MPa.
Beneficial effect
1), on the premise of the treatment effeciency and antifouling property of modified milipore filter is ensured, it enormously simplify system
Standby process, reduces the cost of raw material making.
2), the stannic oxide/graphene nano piece formation nanochannel of ultrafiltration membrane surface pre-deposition, is intercepted dirty by size exclusion
Contaminate thing and reduce fouling membrane.The service life of film is improved, water treatment efficiency is improved.
3), metal cation crosslinking agent strengthens the adhesion between stannic oxide/graphene nano piece by electrostatic force, improves
Stability of the stannic oxide/graphene nano piece in water, is difficult to be dissolved.
4), the inventive method is simple to operation and is easy to scale and uses, beneficial to popularization.
Brief description of the drawings
Fig. 1, on PVDF membrane surface using aluminium ion as crosslinking agent pre-deposition 0.1mg stannic oxide/graphene nano pieces
Scanning electron microscope diagram (SEM), upper strata is the stannic oxide/graphene nano piece of load, and lower floor is PVDF membrane；
In Fig. 2, case study on implementation one PVDF membrane surface through pre-deposition using 0.0001mol/L aluminium ions as crosslinking
To the absorption flux decline figure of organic matter bovine serum albumin (BSA) solution after agent pre-deposition 0.1mg stannic oxide/graphene nano pieces；
In Fig. 3, case study on implementation two PVDF membrane surface through pre-deposition using 0.001mol/L iron ions as crosslinking
To the absorption flux decline figure of organic matter sodium humate (HS) solution after agent pre-deposition 1mg stannic oxide/graphene nano pieces；
In Fig. 4, case study on implementation three on PVDF membrane surface through pre-deposition with 0.05mol/L aluminium ions and
0.05mol/L iron ions be crosslinking agent pre-deposition 15mg stannic oxide/graphene nano pieces after after to organic matter sodium alginate (SA) solution
Absorption flux decline figure；
In Fig. 5, case study on implementation four on PVDF membrane surface through pre-deposition with 0.05mol/L aluminium ions and
0.05mol/L iron ions be crosslinking agent pre-deposition 30mg stannic oxide/graphene nano pieces after after to organic matter sodium alginate (SA) solution
Absorption flux decline figure.
Embodiment
The inventive method is described further with case study on implementation below in conjunction with the accompanying drawings.It should be understood that these cases are only limitted to
Illustrate the inventive method, rather than limitation use scope of the invention.
Embodiment 1
1), 0.1 milligram 1 layer of stannic oxide/graphene nano piece is added in 100 ml deionized waters, then will
2.415mg Aluminium chloride hexahydrate is added in other 100 ml deionized water, and two kinds of solution are well mixed.Afterwards super
Film is placed in filter bowl, then pours mixed solution into ultrafiltration cup, filtered 2-5 minutes under the conditions of constant pressure 0.05MPa
Stannic oxide/graphene nano piece is successfully loaded to polyvinylidene fluoride ultrafiltration film surface by work(, and the film after load is as shown in Figure 1.
2), 1 milliliter of 1g/L bovine serum albumin (BSA) storing solution is added in 100 ml deionized waters, by the BSA
Solution above-mentioned steps 1) in pre-deposition the polyvinylidene fluoride ultrafiltration film ultrafiltration of 0.1mg stannic oxide/graphene nano pieces, electricity consumption
Sub- day flushconnection data display equipment gathered data, inquires into the change of membrane flux.As shown in Fig. 2 the rate of decay of membrane flux is notable
Reduce, 75% or so flux can be still kept after such as figure a period of time.
Embodiment 2
1), 1 milligram 60 layers of stannic oxide/graphene nano piece is added in 100 milliliters of ethanol, then by the six of 27.05mg
Ferric Chloride Hydrated is added in other 100 ml deionized water, and two kinds of solution are well mixed.Placed afterwards in ultrafiltration cup
Film, then pour mixed solution into ultrafiltration cup, 2-5 minutes are filtered under the conditions of constant pressure 0.2MPa i.e. successfully by graphene oxide
Nanometer sheet successfully loads to polyvinylidene fluoride ultrafiltration film surface.
2), 1 milliliter of 3g/L sodium humate (HS) storing solution is added in 300 ml deionized waters, by the HS solution
With above-mentioned steps 1) in the pre-deposition polyvinylidene fluoride ultrafiltration film ultrafiltration of 1mg stannic oxide/graphene nano pieces, use electronic balance
Data display equipment gathered data is connected, the change of membrane flux is inquired into.As shown in Figure 3.Membrane flux stability is greatly improved, by such as
75% or so flux can be still kept after figure a period of time.
Embodiment 3
1), 15 milligrams 100 layers of stannic oxide/graphene nano piece is added in 100 ml deionized waters, then will
1666.1mg Patent alum and 974.8mg ferric sulfate hydrate are added in other 100 ml deionized water, by two
Solution is planted to be well mixed.Film is placed in ultrafiltration cup afterwards, then pours mixed solution into ultrafiltration cup, in constant pressure 0.4MPa
Under the conditions of filtering 2-5 minute be stannic oxide/graphene nano piece is successfully successfully loaded into polyvinylidene fluoride ultrafiltration film surface.
2), 1 milliliter of 1g/L sodium alginate (SA) storing solution is added in 100 ml deionized waters, by the SA solution
With above-mentioned steps 1) in the pre-deposition polyvinylidene fluoride ultrafiltration film ultrafiltration of 15mg stannic oxide/graphene nano pieces, use electronic balance
Data display equipment gathered data is connected, the change of membrane flux is inquired into.As shown in Figure 4.The decay of membrane flux is greatly reduced, is passed through
Such as scheme still keep 75% or so flux after a period of time.
Embodiment 4
1), 30 milligrams 60 layers of stannic oxide/graphene nano piece is added in 100 milliliters of ethanol, then by 1352.5mg's
Ferric chloride hexahydrate and 1207.5mg Aluminium chloride hexahydrate are added in other 100 ml deionized water, and two kinds of solution are mixed
Close uniform.Film is placed in ultrafiltration cup afterwards, then pours mixed solution into ultrafiltration cup, the mistake under the conditions of constant pressure 0.4MPa
Stannic oxide/graphene nano piece is successfully successfully loaded to polyvinylidene fluoride ultrafiltration film surface in 2-5 minutes by filter.
2) 1 milliliter of 1g/L sodium alginate (SA) storing solution is added in 100 ml deionized waters, the SA solution is used
Above-mentioned steps 1) in the pre-deposition polyvinylidene fluoride ultrafiltration film ultrafiltration of 30mg stannic oxide/graphene nano pieces, connected with electronic balance
Data display equipment gathered data is connect, the change of membrane flux is inquired into.As shown in Figure 4.As shown in Figure 5.Graphene oxide has been loaded to receive
The milipore filter of rice piece can greatly reduce fouling membrane, put forward high-throughout stability.
Above-described to specifically describe, purpose, technical scheme and beneficial effect to invention have been carried out further specifically
It is bright, the specific embodiment that the foregoing is only the present invention is should be understood that, for explaining the present invention, is not used to limit this
The protection domain of invention, within the spirit and principles of the invention, any modification, equivalent substitution and improvements done etc. all should
Within protection scope of the present invention.
Claims (8)
1. it is a kind of in method of the metal cation crosslinking-oxidization graphene nanometer sheet to ultrafiltration membrane modifying, it is characterised in that：By oxygen
Graphite alkene nanometer sheet is dissolved in solvent, then adds crosslinking agent, after being well mixed, obtains solution；Under constant-pressure conditions,
Stannic oxide/graphene nano piece in solution is loaded into ultrafiltration membrane surface；Solute addition quality is received with graphene oxide in crosslinking agent
The ratio of the addition quality of rice piece is 10-13500.
2. it is as claimed in claim 1 a kind of with side of the metal cation crosslinking-oxidization graphene nanometer sheet to ultrafiltration membrane modifying
Method, it is characterised in that：The stannic oxide/graphene nano piece includes：Single-layer graphene oxide nanometer sheet, multilayer graphene oxide are received
One or more in rice piece.
3. it is as claimed in claim 1 a kind of with side of the metal cation crosslinking-oxidization graphene nanometer sheet to ultrafiltration membrane modifying
Method, it is characterised in that：The crosslinking agent is aluminum sulfate, aluminium chloride, aluminum nitrate, ferric sulfate, ferric trichloride, frerrous chloride/mangaic acid
Potassium, ferrous sulfate/potassium manganate, frerrous chloride/potassium permanganate or ferrous sulfate/potassium permanganate, and above-mentioned all substances appoint
Meaning combination.
4. it is as claimed in claim 1 a kind of with side of the metal cation crosslinking-oxidization graphene nanometer sheet to ultrafiltration membrane modifying
Method, it is characterised in that：The solvent includes deionized water and ethanol.
5. it is as claimed in claim 1 or 2 it is a kind of with metal cation crosslinking-oxidization graphene nanometer sheet to ultrafiltration membrane modifying
Method, it is characterised in that：The load capacity of the stannic oxide/graphene nano piece is 20mg/m2-7000mg/m2。
6. a kind of as described in claim 1 or 3 is with metal cation crosslinking-oxidization graphene nanometer sheet to ultrafiltration membrane modifying
Method, it is characterised in that：The concentration of described crosslinking agent is 0.0001-0.1M.
7. it is as claimed in claim 1 or 2 it is a kind of with metal cation crosslinking-oxidization graphene nanometer sheet to ultrafiltration membrane modifying
Method, it is characterised in that：Stannic oxide/graphene nano piece is 1-100 layers.
8. it is as claimed in claim 1 a kind of with side of the metal cation crosslinking-oxidization graphene nanometer sheet to ultrafiltration membrane modifying
Method, it is characterised in that：Described constant pressure is 0.05-0.4MPa.
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| CN201710355225.2A CN107185411A (en) | 2017-05-19 | 2017-05-19 | It is a kind of in method of the metal cation crosslinking-oxidization graphene nanometer sheet to ultrafiltration membrane modifying |
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| CN109731482A (en) * | 2019-03-11 | 2019-05-10 | 南京工业大学 | A kind of seperation film and preparation method thereof based on graphene oxide |
| CN110292864A (en) * | 2019-06-12 | 2019-10-01 | 时代沃顿科技有限公司 | A kind of preparation method of composite nano materials hybridized film and the hybridized film thus prepared |
| CN110449032A (en) * | 2019-07-08 | 2019-11-15 | 西安建筑科技大学 | A kind of swelling resistance two dimension SA-MXene stratiform nanofiltration membrane, preparation and application |
| CN111346517A (en) * | 2020-03-17 | 2020-06-30 | 北京理工大学 | Composite crosslinked graphene oxide membrane, preparation method and application thereof |
| CN111533117A (en) * | 2020-05-13 | 2020-08-14 | 四川大学 | Metal ion crosslinked high-strength stable graphene oxide membrane and preparation method thereof |
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| CN109731482A (en) * | 2019-03-11 | 2019-05-10 | 南京工业大学 | A kind of seperation film and preparation method thereof based on graphene oxide |
| CN110292864A (en) * | 2019-06-12 | 2019-10-01 | 时代沃顿科技有限公司 | A kind of preparation method of composite nano materials hybridized film and the hybridized film thus prepared |
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| CN110449032B (en) * | 2019-07-08 | 2021-10-08 | 西安建筑科技大学 | Swelling-resistant two-dimensional SA-MXene layered nanofiltration membrane, and preparation and application thereof |
| CN111346517A (en) * | 2020-03-17 | 2020-06-30 | 北京理工大学 | Composite crosslinked graphene oxide membrane, preparation method and application thereof |
| CN111346517B (en) * | 2020-03-17 | 2021-06-11 | 北京理工大学 | Composite crosslinked graphene oxide membrane, preparation method and application thereof |
| CN111533117A (en) * | 2020-05-13 | 2020-08-14 | 四川大学 | Metal ion crosslinked high-strength stable graphene oxide membrane and preparation method thereof |
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Application publication date: 20170922 |