CN110152502A - A kind of novel environment friendly graphene oxide membrane and preparation method - Google Patents
A kind of novel environment friendly graphene oxide membrane and preparation method Download PDFInfo
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- CN110152502A CN110152502A CN201910213030.3A CN201910213030A CN110152502A CN 110152502 A CN110152502 A CN 110152502A CN 201910213030 A CN201910213030 A CN 201910213030A CN 110152502 A CN110152502 A CN 110152502A
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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
- B01D67/0039—Inorganic membrane manufacture
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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
- B01D67/0079—Manufacture of membranes comprising organic and inorganic components
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- 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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/02—Inorganic material
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Abstract
The present invention provides a kind of novel environment friendly graphene oxide membrane and preparation methods, include: S1, mix graphene oxide according to a certain percentage with solvent, graphene oxide dispersion is obtained by ultrasonic treatment: S2, isolating the unstripped big thickness graphite flake opened, and obtaining supernatant is thin graphene piece dispersion liquid；S3, thin graphene piece dispersion liquid is subjected to centrifugal treating, obtains large scale thin graphene nanometer sheet；S4, by ultrasonic treatment, obtain large scale thin graphene nanometer sheet dispersion liquid；S5, large scale thin graphene nanometer sheet dispersion liquid is combined to the membrane material of high molecular polymer filter membrane or the formation of inorganic filter membrane surface with graphene oxide separating layer.Novel environment friendly graphene oxide membrane and preparation method of the present invention prepare graphene oxide membrane material using large scale thin graphene nanometer sheet, and process is simple and easy to do and environmentally protective, and can pass through the thickness of adjusting raw material usage amount direct regulation and control membrane material.
Description
Technical field
The invention belongs to technical field of graphene, more particularly, to a kind of novel environment friendly graphene oxide membrane and preparation side
Method.
Background technique
With the rapid development of modern industry, produce largely containing various persistent organic pollutants and metal ion
Waste water.Persistent organic pollutants such as phenols, nitrobenzene, phenyl amines, chlorobenzene class, Polychlorinated biphenyls, multiring aromatic hydrocarbon etc. are led to
It is often the very big substance of toxicity, there is certain carcinogenic, teratogenesis, mutagenesis.Contain these persistent organic pollutants
Organic wastewater usually has the characteristics that as follows: high organic content, coloration are big, strong toxicity, salinity are high, pH amplitude of variation is big, at
Divide complexity, microbial nutrition element ratio numerous imbalances, biodegradability poor.Wastewater in waters containing heavy metal equally have compared with
Big harm.Waste water containing persistent organic pollutants and heavy metal is handled using conventional biological method, it is generally difficult to realize
Effluent quality qualified discharge, the advanced treating containing persistent organic pollutants and heavy metal wastewater thereby are one and urgently to be resolved ask
Topic.In addition, being even more a technical problem for the removal of light concentration organic pollutant in drinking water.
Traditional water treatment technology be largely faced with low separation efficiency, energy consumption is high, to water temperature require it is stringent, adapt to
The disadvantages of range is small.
Summary of the invention
In view of this, the present invention is directed to propose a kind of novel environment friendly graphene oxide membrane and preparation method, to solve tradition
Water treatment technology low separation efficiency, energy consumption is high, requires the problems such as stringent, adaptation range is small to water temperature.
In order to achieve the above objectives, the technical scheme of the present invention is realized as follows:
A kind of novel environment friendly graphene oxide membrane preparation method, comprising:
S1, graphene oxide is mixed according to a certain percentage with solvent, obtains graphene oxide dispersion by ultrasonic treatment
Liquid:
S2, graphene oxide dispersion obtained in step S1 is subjected to centrifugal treating, isolates the unstripped big thickness opened
Graphite flake is spent, obtaining supernatant is thin graphene piece dispersion liquid；
S3, thin graphene piece dispersion liquid is subjected to centrifugal treating, obtains large scale thin graphene nanometer sheet；
S4, large scale thin graphene nanometer sheet is mixed according to a certain percentage with solvent, by ultrasonic treatment, is obtained big
Size thin graphene nanometer sheet dispersion liquid；
S5, large scale thin graphene nanometer sheet dispersion liquid is combined to high molecular polymer filter membrane or inorganic filter membrane table
Face forms the membrane material with graphene oxide separating layer.
Further, in the step S1, the mass parts ratio of graphene oxide and solvent is 1 than 10-1000, in 10-
0.2-10min is ultrasonically treated under the power of 400W；
Preferably, in the step S1, the mass parts ratio of graphene oxide and solvent is 1 to 100, in the power of 300W
Lower ultrasonic treatment 3-6min.
Further, in the step S2, the graphene oxide dispersion that step S1 is obtained is in 3000 r/min conditions
Lower centrifugation 10 minutes.
Further, in the step S3, by thin graphene piece dispersion liquid obtained in step S2 in 12000r/min
Under the conditions of be centrifuged 5-100min, the thin graphene nanometer sheet of small size and large-sized thin graphene nanometer sheet are separated,
Obtain large scale thin graphene nanometer sheet；
Preferably, in the step S3, by thin graphene piece dispersion liquid obtained in step S2 in 12000r/min item
It is centrifuged 20min under part, the thin graphene nanometer sheet of small size and large-sized thin graphene nanometer sheet are separated, is obtained big
Size thin graphene nanometer sheet.
Further, in the step S4, the mass parts ratio of large scale thin graphene nanometer sheet and solvent is 1 ratio
100-100000, and it is ultrasonically treated 0.2-10min under the power of 10-400W, obtain large scale thin graphene nanometer sheet point
Dispersion liquid.
Further, in the step S5, by large scale thin graphene nanometer sheet dispersion liquid through suction filtration, spin coating, spraying
Or the mode brushed is combined to high molecular polymer filter membrane or inorganic filter membrane surface, being formed has graphene oxide separating layer
Membrane material.
Further, the solvent includes water, ethyl alcohol, methanol, dimethyl sulfoxide, acetone, dimethylformamide, dimethyl
Acetamide, N- methyl adjoin pyrrolidone, gamma-valerolactone one or more kinds of solution compounding.
Further, in the step S5, the high molecular polymer filter membrane is to be trapped in 0.1-0.5 μm of particle section
Nylon microfiltration membranes, poly- sough microfiltration membranes, polyethers sough microfiltration membranes, polytetrafluoroethylene (PTFE), polyvinylidene fluoride microporous filtering film.
Further, in the step S5, inorganic filter membrane is aluminium oxide, zirconium oxide, zirconia-silica, hafnium oxide
Sodium, alumina-titania material.
A kind of novel environment friendly graphene oxide membrane, by the described in any item novel environment friendly graphite oxides of claim 1-9
Alkene membrane preparation method is prepared.
Compared with the existing technology, novel environment friendly graphene oxide membrane preparation method of the present invention has the advantage that
(1) novel environment friendly graphene oxide membrane preparation method of the present invention uses large scale (8-25 μm) thin layer stone
Black alkene nanometer sheet prepares graphene oxide membrane material, and process is simple and easy to do and environmentally protective, and can be made by adjusting raw material
The thickness of dosage direct regulation and control membrane material.
(2) graphene oxide membrane prepared by novel environment friendly graphene oxide membrane preparation method of the present invention has water
There is good permeability, the efficient selective that organic matter may be implemented in the thickness by adjusting membrane material penetrates and retention, is having
The fields such as the isolating and purifying of machine object, wastewater treatment and drink water purifying have huge application prospect.
Specific embodiment
It should be noted that in the absence of conflict, the feature in embodiment and embodiment in the present invention can phase
Mutually combination.
In the description of the present invention, it should be noted that unless otherwise clearly defined and limited, term " installation ", " phase
Even ", " connection " shall be understood in a broad sense, for example, it may be being fixedly connected, may be a detachable connection, or be integrally connected；It can
To be mechanical connection, it is also possible to be electrically connected；It can be directly connected, can also can be indirectly connected through an intermediary
Connection inside two elements.For the ordinary skill in the art, above-mentioned term can be understood by concrete condition
Concrete meaning in the present invention.
Below in conjunction with embodiment, the present invention will be described in detail.
Embodiment 1:
The graphene oxide dispersion for forming that concentration is 0.05mg/mL is added graphene oxide into water.In the function of 20W
It is ultrasonically treated 3min under rate, obtains graphene oxide dispersion.By above-mentioned graphene oxide dispersion under the conditions of 3000r/min
Centrifugation isolates the unstripped larger graphite flake of the thickness opened in 10 minutes, obtains thin graphene piece dispersion liquid.By above-mentioned thin layer stone
Black alkene piece dispersion liquid is centrifuged 20min under the conditions of 12000r/min, and the thin graphene nanometer sheet of small size is retained in supernatant
In, obtain large scale thin graphene nanometer sheet；The large scale thin graphene nanometer sheet that 200mL concentration is 10mg/L is dispersed
Liquid is ultrasonically treated 10min under the power of 400W, obtains large scale thin graphene nanometer sheet dispersion liquid.By large scale thin layer stone
Black alkene nanometer sheet dispersion liquid is poured into the bottle,suction that polytetrafluoroethylene (PTFE) microfiltration membranes are support membrane, is then filtered by vacuum, and pressure is filtered
Power is 0.1MPa, and the membrane material with graphene oxide, drying at room temperature or the preservation in aqueous solvent are obtained after draining.Support
Film is the polytetrafluoroethylene (PTFE) microfiltration membranes of diameter 50mm, 0.45 μm of aperture.Graphene oxide membrane obtained with a thickness of 8.7nm, just oneself
The permeability 144n ml m of alkane-2h-1bar-1, and the retention rate of methylene blue is 95% or more.
Wherein, the calculation formula of permeability are as follows: permeability=Q/ (Δ PA)
In formula, Q is flow, and unit is n mL/h；The sectional area of A graphene film, unit m2；Δ P is that liquid passes through stone
Pressure difference before and after black alkene film, unit bar.
The retention rate calculation formula of methyl blue are as follows: methylene blue retention rate=(C0-C1)/C0
In formula, C0And C1It is original concentration, concentration after filtering respectively.
The permeability of n-hexane and the retention rate of methylene blue, the two numerical value are all measured values, basis after needing to measure
Formula calculates.
Embodiment 2:
The graphene oxide dispersion for forming that concentration is 0.05mg/mL is added graphene oxide into water.In the function of 20W
It is ultrasonically treated 3min under rate, obtains graphene oxide dispersion.By above-mentioned graphene oxide dispersion under the conditions of 3000r/min
Centrifugation isolates the unstripped larger graphite flake of the thickness opened in 10 minutes, obtains thin graphene piece dispersion liquid.By above-mentioned thin layer stone
Black alkene piece dispersion liquid is centrifuged 20min under the conditions of 12000r/min, and the thin graphene nanometer sheet of small size is retained in supernatant
In, obtain large scale thin graphene nanometer sheet；The large scale thin graphene nanometer sheet that 500mL concentration is 10mg/L is dispersed
Liquid is ultrasonically treated 10min under the power of 400W, obtains large scale thin graphene nanometer sheet dispersion liquid.By large scale thin layer stone
Black alkene nanometer sheet dispersion liquid is poured into the bottle,suction that polytetrafluoroethylene (PTFE) microfiltration membranes are support membrane, is then filtered by vacuum, and pressure is filtered
Power is 0.1MPa, and the membrane material with graphene oxide, drying at room temperature or the preservation in aqueous solvent are obtained after draining.Support
Film is diameter 50mm, the polytetrafluoroethylene (PTFE) microfiltration membranes in 0.45 μm of aperture.Graphene oxide membrane obtained with a thickness of 17.1nm, just oneself
The permeability 20n ml m of alkane-2h-1bar-1, and the retention rate of rhodamine is 98% or more.
Wherein, the calculation formula of permeability are as follows: permeability=Q/ (Δ PA)
In formula, Q is flow, and unit is n mL/h；The sectional area of A graphene film, unit m2；Δ P is that liquid passes through stone
Pressure difference before and after black alkene film, unit bar.
The retention rate calculation formula of methyl blue are as follows: methylene blue retention rate=(C0-C1)/C0
In formula, C0And C1It is original concentration, concentration after filtering respectively.
The permeability of n-hexane and the retention rate of methylene blue, the two numerical value are all measured values, basis after needing to measure
Formula calculates.
Embodiment 3:
The graphene oxide dispersion for forming that concentration is 0.05mg/mL is added graphene oxide into water.In the function of 20W
It is ultrasonically treated 3min under rate, obtains graphene oxide dispersion.By above-mentioned graphene oxide dispersion under the conditions of 3000r/min
Centrifugation isolates the unstripped larger graphite flake of the thickness opened in 10 minutes, obtains thin graphene piece dispersion liquid.By above-mentioned thin layer stone
Black alkene piece dispersion liquid is centrifuged 20min under the conditions of 12000r/min, and the thin graphene nanometer sheet of small size is retained in supernatant
In, obtain large scale thin graphene nanometer sheet；By the large scale thin graphene nanometer sheet point that 4000mL concentration is 10mg/L
Dispersion liquid is ultrasonically treated 10min under the power of 400W, obtains large scale thin graphene nanometer sheet dispersion liquid.By large scale thin layer
Graphene nanometer sheet dispersion liquid pours into the bottle,suction that polytetrafluoroethylene (PTFE) microfiltration membranes are support membrane, is then filtered by vacuum, and filters
Pressure is 0.1MPa, and the membrane material with graphene oxide, drying at room temperature or the preservation in aqueous solvent are obtained after draining.Branch
Support film is diameter 50mm, the polytetrafluoroethylene (PTFE) microfiltration membranes in 0.45 μm of aperture.Graphene oxide membrane obtained with a thickness of 40nm, just oneself
The permeability 1n ml m of alkane-2h-1bar-1, and the retention rate of methylene blue is 95% or more.
Wherein, the calculation formula of permeability are as follows: permeability=Q/ (Δ PA)
In formula, Q is flow, and unit is n mL/h；The sectional area of A graphene film, unit m2；Δ P is that liquid passes through stone
Pressure difference before and after black alkene film, unit bar.
The retention rate calculation formula of methyl blue are as follows: methylene blue retention rate=(C0-C1)/C0
In formula, C0And C1It is original concentration, concentration after filtering respectively.
The permeability of n-hexane and the retention rate of methylene blue, the two numerical value are all measured values, basis after needing to measure
Formula calculates.
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 novel environment friendly graphene oxide membrane preparation method characterized by comprising
S1, graphene oxide is mixed according to a certain percentage with solvent, obtains graphene oxide dispersion by ultrasonic treatment:
S2, graphene oxide dispersion obtained in step S1 is subjected to centrifugal treating, isolates the unstripped big thickness stone opened
Ink sheet, obtaining supernatant is thin graphene piece dispersion liquid；
S3, thin graphene piece dispersion liquid is subjected to centrifugal treating, obtains large scale thin graphene nanometer sheet；
S4, large scale thin graphene nanometer sheet is mixed according to a certain percentage with solvent, by ultrasonic treatment, obtains large scale
Thin graphene nanometer sheet dispersion liquid；
S5, large scale thin graphene nanometer sheet dispersion liquid is combined to high molecular polymer filter membrane or inorganic filter membrane surface shape
At the membrane material with graphene oxide separating layer.
2. novel environment friendly graphene oxide membrane preparation method according to claim 1, it is characterised in that: the step S1
In, the mass parts ratio of graphene oxide and solvent is 1 than 10-1000, is ultrasonically treated 0.2- under the power of 10-400W
10min；
Preferably, in the step S1, the mass parts ratio of graphene oxide and solvent is 1 to 100, is surpassed under the power of 300W
Sonication 3-6min.
3. novel environment friendly graphene oxide membrane preparation method according to claim 1, it is characterised in that: the step S2
In, the graphene oxide dispersion that step S1 is obtained is centrifuged 10 minutes under the conditions of 3000r/min.
4. novel environment friendly graphene oxide membrane preparation method according to claim 1, it is characterised in that: the step S3
In, thin graphene piece dispersion liquid obtained in step S2 is centrifuged 5-100min under the conditions of 12000r/min, by small size
Thin graphene nanometer sheet and large-sized thin graphene nanometer sheet separation, obtain large scale thin graphene nanometer sheet；
Preferably, in the step S3, by thin graphene piece dispersion liquid obtained in step S2 under the conditions of 12000r/min
It is centrifuged 20min, the thin graphene nanometer sheet of small size and large-sized thin graphene nanometer sheet are separated, large scale is obtained
Thin graphene nanometer sheet.
5. novel environment friendly graphene oxide membrane preparation method according to claim 1, it is characterised in that: the step S4
In, the mass parts ratio of large scale thin graphene nanometer sheet and solvent is 1 than 100-100000, and in the power of 10-400W
Lower ultrasonic treatment 0.2-10min obtains large scale thin graphene nanometer sheet dispersion liquid.
6. novel environment friendly graphene oxide membrane preparation method according to claim 1, it is characterised in that: the step S5
In, large scale thin graphene nanometer sheet dispersion liquid is combined to high molecular polymerization through suction filtration, spin coating, spraying or the mode of brushing
Object filter membrane or inorganic filter membrane surface form the membrane material with graphene oxide separating layer.
7. -6 any novel environment friendly graphene oxide membrane preparation method according to claim 1, it is characterised in that: described molten
Agent include water, ethyl alcohol, methanol, dimethyl sulfoxide, acetone, dimethylformamide, dimethyl acetamide, N- methyl adjoin pyrrolidone,
The compounding of one or more kinds of solution of gamma-valerolactone.
8. novel environment friendly graphene oxide membrane preparation method according to claim 1, it is characterised in that: the step S5
In, the high molecular polymer filter membrane is the nylon microfiltration membranes for being trapped in 0.1-0.5 μm of particle section, poly- sough microfiltration membranes, polyethers
It soughs microfiltration membranes, polytetrafluoroethylene (PTFE), polyvinylidene fluoride microporous filtering film.
9. novel environment friendly graphene oxide membrane preparation method according to claim 1, it is characterised in that: the step S5
In, inorganic filter membrane is aluminium oxide, zirconium oxide, zirconia-silica, hafnium oxide sodium, alumina-titania material.
10. a kind of novel environment friendly graphene oxide membrane, it is characterised in that: it is by the described in any item Novel rings of claim 1-9
Graphene oxide membrane preparation method is protected to be prepared.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110772994A (en) * | 2019-11-08 | 2020-02-11 | 成都石大力盾科技有限公司 | Mixed graphene oxide nanofiltration membrane, preparation method and application thereof |
| CN110773000A (en) * | 2019-11-08 | 2020-02-11 | 成都石大力盾科技有限公司 | Efficient and anti-pollution carboxylated graphene oxide nanofiltration membrane, and preparation method and application thereof |
| CN111426667A (en) * | 2020-04-23 | 2020-07-17 | 天津科技大学 | Fluorescence method for β -lactoglobulin detection based on quantum dot-aptamer-graphene oxide |
| CN113522059A (en) * | 2021-07-02 | 2021-10-22 | 五邑大学 | Folded graphene oxide film and preparation method thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110772994A (en) * | 2019-11-08 | 2020-02-11 | 成都石大力盾科技有限公司 | Mixed graphene oxide nanofiltration membrane, preparation method and application thereof |
| CN110773000A (en) * | 2019-11-08 | 2020-02-11 | 成都石大力盾科技有限公司 | Efficient and anti-pollution carboxylated graphene oxide nanofiltration membrane, and preparation method and application thereof |
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| CN110773000B (en) * | 2019-11-08 | 2021-09-24 | 成都石大力盾科技有限公司 | Efficient and anti-pollution carboxylated graphene oxide nanofiltration membrane, and preparation method and application thereof |
| CN111426667A (en) * | 2020-04-23 | 2020-07-17 | 天津科技大学 | Fluorescence method for β -lactoglobulin detection based on quantum dot-aptamer-graphene oxide |
| CN113522059A (en) * | 2021-07-02 | 2021-10-22 | 五邑大学 | Folded graphene oxide film and preparation method thereof |
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