CN109046043B - Graphene oxide/chrome black T composite membrane and preparation method thereof - Google Patents
Graphene oxide/chrome black T composite membrane and preparation method thereof Download PDFInfo
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- B01D69/12—Composite membranes; Ultra-thin membranes
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- 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
- B01D61/147—Microfiltration
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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
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- 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
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- 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
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
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- 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
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- 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
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- C02F1/00—Treatment of water, waste water, or sewage
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
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- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/34—Organic compounds containing oxygen
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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
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/38—Organic compounds containing nitrogen
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Abstract
The invention discloses a graphene oxide/chrome black T composite membrane and a preparation method thereof, wherein the graphene oxide/chrome black T composite membrane consists of a base membrane and a filter layer attached to the base membrane; the main components of the filter layer are composed of graphene oxide and chrome black T. The preparation method comprises the following steps: grinding graphene oxide with pure water until the particle size is uniformly dispersed, adding the pure water under the stirring condition, diluting to 5-20 mu g/mL, continuously stirring, then performing ultrasonic treatment at 300-500 w for 10-60 min, adding chrome black T, and stirring until the mixture is uniformly mixed to obtain a membrane preparation solution; adding a proper amount of membrane making liquid into a sand core funnel, wherein a base membrane is laid in the sand core funnel in advance; and carrying out vacuum filtration and drying to obtain the graphene oxide/chrome black T composite membrane. The preparation method is simple, efficient, low in cost and high in repeatability; the obtained product can greatly improve the retention rate of the dye.
Description
Technical Field
The invention relates to the technical field of films, in particular to a graphene oxide/chrome black T composite film and a preparation method thereof.
Background
Graphene, a carbon-based material, is prepared from sp2The formed single-atom thickness two-dimensional layered material hybridizes carbon atoms. Graphene oxide (abbreviated as GO) is one of its main derivatives, having a two-dimensional planar structure similar to graphene. GO introduces the above 3 polar oxygen-containing functional groups on the surface of the carbon skeleton due to oxidation. The structure enables the GO membrane to have extremely strong hydrophilicity, so that the GO membrane has good stability and dispersibility in an aqueous solution, and the GO membrane has a special zigzag water molecule transmission channel, so that the prepared GO membrane has good permeability. Therefore, engineering applications of GO membranes are of more realistic significance. The existing GO membrane has low retention rate when treating dye wastewater, and greatly limits the further waste printing and dyeingApplication in the field of water treatment.
Disclosure of Invention
In order to solve the technical problems, the invention provides the graphene oxide/chrome black T composite membrane and the preparation method thereof, the obtained graphene oxide/chrome black T composite membrane can greatly improve the retention rate of the dye, has stable performance when used in water for a long time, is simple and efficient in preparation method, low in cost and high in repeatability, can greatly reduce the cost of treating dye wastewater, and has wide market application prospect.
Therefore, the technical scheme of the invention is as follows:
a graphene oxide/chrome black T composite membrane is composed of a base membrane and a filter layer attached to the base membrane; the main components of the filter layer are composed of graphene oxide and chrome black T.
Further, the basement membrane is a microfiltration membrane.
Further, the base membrane is a polyamide microfiltration membrane, a polyether sulfone microfiltration membrane, a polyvinylidene fluoride microfiltration membrane, a polytetrafluoroethylene microfiltration membrane or a mixed cellulose microfiltration membrane.
A preparation method of a graphene oxide/chrome black T composite film comprises the following steps:
1) adding pure water into graphene oxide, grinding until the particle size is uniformly dispersed, adding pure water under the stirring condition, diluting to 5-20 mu g/mL, and continuously stirring to obtain a graphene oxide suspension;
2) performing ultrasonic treatment on the graphene oxide suspension at 300-500 w for 10-60 min to obtain a uniformly dispersed graphene oxide aqueous solution;
3) adding chromium black T into the graphene oxide aqueous solution, and stirring until the chromium black T and the graphene oxide aqueous solution are uniformly mixed to obtain a membrane preparation solution; wherein the graphene oxide accounts for 0.0005-0.001% of the total mass of the membrane-forming solution, and the chrome black T accounts for 1 × 10 of the total mass of the membrane-forming solution-6％～1×10-4％；
4) Adding a proper amount of the membrane making solution into a sand core funnel, wherein a base membrane is laid in the sand core funnel in advance; and carrying out vacuum filtration and drying to obtain the graphene oxide/chrome black T composite membrane.
Further, the chrome black T occupies1.5 multiplied by 10 of the total mass of the membrane-forming liquid-5％～3.0×10-5％。
Further, the drying in the step 4) is room temperature drying or freeze drying.
The invention relates to a graphene oxide/chrome black T composite membrane obtained through p-p conjugation and a preparation method thereof, and the technical effects are as follows:
1. because the graphene oxide contains rich oxygen-containing functional groups, the prepared graphene oxide film has a special zigzag transmission channel, and the obtained composite film has good permeability;
2. because the graphene oxide and the chrome black T both have conjugated systems, a p-p conjugated composite film can be formed through blending, and the p-p conjugated effect enables the graphene oxide/chrome black T composite film to have good stability.
3. Because the chrome black T is inserted into the graphene oxide lamella in the blending process, the interlayer spacing of the graphene oxide can be effectively reduced through the conjugation, so that the retention rate of the obtained composite membrane on the dye is effectively improved, and the composite membrane has important significance in the field of treating dye wastewater.
Detailed Description
The following provides a detailed description of the technical solution of the present invention with reference to examples.
Examples 1 to 3
A preparation method of a graphene oxide/chrome black T composite film comprises the following steps:
adding 0.005g of lamellar graphene oxide into a mortar, dropwise adding 1mL of pure water, grinding for 5min, transferring the lamellar graphene oxide into a 500mL round-bottom flask, diluting the lamellar graphene oxide to 200mL with the pure water, mechanically stirring the lamellar graphene oxide at 25 ℃ for 5.5h, performing ultrasonic treatment until the lamellar graphene oxide is completely dispersed, and sealing and storing the lamellar graphene oxide in a low-temperature chamber to obtain a uniformly dispersed graphene oxide aqueous solution;
adding chromium black T powder with different amounts into the graphene oxide aqueous solution, and magnetically stirring for 24 hours to obtain a membrane preparation solution;
and paving a mixed cellulose microfiltration membrane as a base membrane in a sand core funnel in advance, performing vacuum filtration on 100mL of membrane preparation liquid under the condition of-0.1 Mpa to form a membrane, and drying at room temperature for 2 days to obtain the graphene oxide/chrome black T composite membrane, wherein the membrane is sealed and stored at low temperature.
The graphene oxide/chrome black T composite membrane obtained in the embodiment 1-3 is tested for the dye-trapping performance by adopting a cross-flow device, a methyl orange solution, a disperse black 9 solution and a rhodamine B solution with the concentration of 50ppm are respectively tested under 0.2Mpa, and after continuous testing for 5 hours, the obtained trapping rate data is as follows:
| example 1 | Example 2 | Example 3 | |
| Methyl orange solution | 96.78％ | 97.56％ | 98.75％ |
| Disperse Black 9 solution | 100％ | 100％ | 100％ |
| Rhodamine B solution | 86.73％ | 89.69％ | 90.73％ |
Comparative example 1
A preparation method of a graphene oxide/chrome black T composite film comprises the following steps:
adding 0.005g of lamellar graphene oxide into a 500mL round-bottom flask, diluting the lamellar graphene oxide to 300mL with pure water, mechanically stirring the mixture at 20 ℃ for 3.5 hours, performing ultrasonic treatment until the lamellar graphene oxide is completely dispersed, and then sealing and storing the mixture in a low-temperature chamber to obtain a uniformly dispersed graphene oxide aqueous solution;
adding 2X 10 of graphene oxide into aqueous solution-5wt.% of chrome black T powder, and magnetically stirring for 24 hours to obtain a membrane preparation liquid;
and paving a mixed cellulose microfiltration membrane as a base membrane in a sand core funnel in advance, performing vacuum filtration on 100mL of membrane preparation liquid under the condition of-0.1 Mpa to form a membrane, and drying at room temperature for 2 days to obtain the graphene oxide/chrome black T composite membrane, wherein the membrane is sealed and stored at low temperature.
The graphene oxide/chrome black T composite membrane obtained in the comparative example 1 is tested for the dye-trapping performance by adopting a cross-flow device, a methyl orange solution, a disperse black 9 solution and a rhodamine B solution with the concentration of 50ppm are respectively tested under 0.2Mpa, and after continuous testing for 5 hours, the obtained retention rate data is as follows:
| methyl orange solution | Disperse Black 9 solution | Rhodamine B solution | |
| InterceptionRate of change | 91.33％ | 95.79％ | 76.53％ |
Comparative example 2
A preparation method of a graphene oxide/chrome black T composite film comprises the following steps:
adding 0.005g of lamellar graphene oxide into a mortar, dropwise adding 1mL of pure water, grinding for 5min, transferring the mixture into a 500mL round-bottom flask, diluting the mixture to 300mL with the pure water, performing ultrasonic treatment until the mixture is completely dispersed, sealing and storing the mixture in a low-temperature chamber to obtain a uniformly dispersed graphene oxide aqueous solution;
adding 2X 10 of graphene oxide into aqueous solution-5wt.% of chrome black T powder, and magnetically stirring for 24 hours to obtain a membrane preparation liquid;
and paving a mixed cellulose microfiltration membrane as a base membrane in a sand core funnel in advance, performing vacuum filtration on 100mL of membrane preparation liquid under the condition of-0.1 Mpa to form a membrane, and drying at room temperature for 2 days to obtain the graphene oxide/chrome black T composite membrane, wherein the membrane is sealed and stored at low temperature.
The graphene oxide/chrome black T composite membrane obtained in the comparative example 2 is tested for the dye-trapping performance by adopting a cross-flow device, a methyl orange solution, a disperse black 9 solution and a rhodamine B solution with the concentration of 50ppm are respectively tested under 0.2Mpa, and after continuous testing for 5 hours, the obtained retention rate data is as follows:
| methyl orange solution | Disperse Black 9 solution | Rhodamine B solution | |
| Retention rate | 92.42％ | 95.99％ | 78.13％ |
Claims (6)
1. The utility model provides a graphite oxide alkene/chrome black T complex film, comprises basement membrane and the filter layer of attached to the basement membrane, its characterized in that: the main components of the filter layer are composed of graphene oxide and chrome black T; the chrome black T is inserted into the graphene oxide sheet layer.
2. The graphene oxide/chrome black T composite film of claim 1, wherein: the basement membrane is a microfiltration membrane.
3. The graphene oxide/chrome black T composite film of claim 1, wherein: the base membrane is a polyamide microfiltration membrane, a polyether sulfone microfiltration membrane, a polyvinylidene fluoride microfiltration membrane, a polytetrafluoroethylene microfiltration membrane or a mixed cellulose microfiltration membrane.
4. A preparation method of a graphene oxide/chrome black T composite film is characterized by comprising the following steps:
1) adding pure water into graphene oxide, grinding until the particle size is uniformly dispersed, adding pure water under the stirring condition, diluting to 5-20 mu g/mL, and continuously stirring to obtain a graphene oxide suspension;
2) performing ultrasonic treatment on the graphene oxide suspension at 300-500 w for 10-60 min to obtain a uniformly dispersed graphene oxide aqueous solution;
3) adding chromium black T into the graphene oxide aqueous solution, and stirring until the chromium black T and the graphene oxide aqueous solution are uniformly mixed to obtain a membrane preparation solution; wherein the graphene oxide accounts for 0.0005-0.001% of the total mass of the membrane-making solution, and the chrome blackT accounts for 1 multiplied by 10 of the total mass of the membrane-making liquid-6％～1×10-4％；
4) Adding a proper amount of the membrane making solution into a sand core funnel, wherein a base membrane is laid in the sand core funnel in advance; and carrying out vacuum filtration and drying to obtain the graphene oxide/chrome black T composite membrane.
5. The method for preparing the graphene oxide/chrome black T composite film according to claim 4, wherein the graphene oxide/chrome black T composite film comprises: the chrome black T accounts for 1.5 multiplied by 10 of the total mass of the membrane-making liquid-5％～3.0×10-5％。
6. The method for preparing the graphene oxide/chrome black T composite film according to claim 4, wherein the graphene oxide/chrome black T composite film comprises: the drying in the step 4) is room temperature drying or freeze drying.
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| CN103736400A (en) * | 2014-01-06 | 2014-04-23 | 中国海洋大学 | Preparation method of graphene oxide composite nano filter membrane |
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| CN103706264B (en) * | 2014-01-14 | 2016-01-27 | 中国海洋大学 | LBL self-assembly graphene oxide NF membrane and preparation method thereof |
| KR20160123190A (en) * | 2015-04-15 | 2016-10-25 | 한국화학연구원 | Polyacrylonitrile/chitosan composite nanofiltration membrane containing graphene oxide and preparation method thereof |
| KR20160123187A (en) * | 2015-04-15 | 2016-10-25 | 한국화학연구원 | Nanocomposite ultrafiltration membrane containing graphene oxide or reduced graphene oxide and preparation method thereof |
| CN107720886B (en) * | 2017-10-17 | 2020-05-19 | 山东大学 | Nano particle intercalation graphene oxide film, preparation method and application |
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| CN103736400A (en) * | 2014-01-06 | 2014-04-23 | 中国海洋大学 | Preparation method of graphene oxide composite nano filter membrane |
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| Tuning inter-layer spacing of graphene oxide laminates with solvent green to enhance its nanofiltration performance;Hongpan Shen等;《Journal of Membrane Science》;20170401;第527卷;"摘要"和第43-50页 * |
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