CN103768960A - Preparation method for graphene-based film and application of graphene-based film to oil-water separation - Google Patents
Preparation method for graphene-based film and application of graphene-based film to oil-water separation Download PDFInfo
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Abstract
The invention relates to a preparation method for a graphene-based film and application of the graphene-based film to oil-water separation. The graphene-based film is obtained by preparing gel from oxidized graphene and a crosslinking agent, drying the gel, compacting the gel under the pressure of 10-200 kPa, and reducing. The preparation method for the graphene-based oil-water separation film is simple, feasible and low in cost and can be applied to batch industrial production; the film is light in mass and stable and can be cyclically used at high efficiency; the graphene-based oil-water separation film material can separate oil from an oil-water mixture at high efficiency, low energy consumption and ultrahigh speed in various environments, the water content is lower than 200ppm, the minimum water concentration is up to 10ppm, and the water concentration is different slightly according to different oil phases.
Description
Technical field
The present invention relates to a kind of preparation method of Graphene basement membrane and the application in water-oil separating thereof, belong to functional material technology, membrane separation technique and environmental protection technical field.
Background technology
Oil extraction, offshore oil leaks, and industry, life oil-polluted water etc. bring great harm to environment and the ecological balance, make oily water separation technique enjoy people to pay close attention to.At present, membrane separation technique is the effective ways to oily waste water treatment, take organic microfiltration membranes and organic milipore filter as main.But poor due to its chemical stability, heat endurance, even there will be phenomenon swelling, that dissolve, so the use of this class film is very restricted.
The preparation method of the graphene-based oil suction foamed composite of a kind of magnetic that application number is 201310407309 Patent Application Publication, the method is peeled off graphite with improved Hummers method and is obtained graphite oxide; By obtaining graphite oxide aqueous solution after ultrasonic graphite oxide dispersion, in this solution, add CNT, and through suction filtration film forming; Obtain graphene-based foamed material by hydrothermal reduction method; Take graphene-based foam as carrier, prepare magnetic graphite thiazolinyl foamed composite by chemical method at its area load iron oxide.The magnetic graphite thiazolinyl foamed composite that adopts the method for the invention to obtain has good absorption property to oils and organic solvent, simultaneously Stability Analysis of Structures can adopt magnetism separate method to realize to the reusing of material, for graphene-based foamed material is laid a good foundation in the application in water-oil separating field.
Application number is the fast preparation method that 201110066634 patent application relates to a kind of graphene oxide film, take crystalline graphite powder as raw material, with flat glass for becoming membrane carrier, with sulfuric acid, sodium nitrate, potassium permanganate, hydrogen peroxide is preparation process material, deionized water is for preparing solvent, take nitrogen as protective gas, first in four-hole boiling flask, prepare graphene oxide solution, graphene oxide is flocculated with salpeter solution, then film forming on flat glass, obtain graphene oxide film through vacuum drying, film thickness is 1-2 μ m, intensity is good, toughness is large, anti-fracture strength is good, the method technological process is short, speed is fast, processing ease, can accomplish scale production.
The preparation method's of above-mentioned prior art technological process is all comparatively complicated, and cost is high, and the auxiliary agent adding is many, and above-mentioned preparation method can not carry out continuous water-oil separating operation, the not comprehensive investigation of its water-oil separating performance.
Summary of the invention
The object of the invention is to solve the problems of the prior art, prepare a kind of graphene-based water-oil separating film with economic, simple method, it forms gel by graphene oxide and crosslinking agent, dry, under 10 ~ 200 kPas of pressure, after compacting, reduces and obtains.
In a preferred embodiment of the invention, the preparation method of described graphene-based water-oil separating film comprises the steps:
(1) preparation of graphene oxide hydrogel: getting 10mL concentration is the graphene oxide solution of 1 ~ 100mg/mL, adds the crosslinking agent of 0.5mmol ~ 0.1mol at 60 ~ 150 ℃ of reaction 4 ~ 8h, obtains graphene oxide hydrogel;
(2) preparation of graphene oxide xerogel: the dry processing of graphene oxide hydrogel that step (1) is obtained, obtains graphene oxide xerogel;
(3) press mold: by graphene oxide xerogel compacting under 10 ~ 200 kPas of pressure of step (2) gained, maintain 5 ~ 50min;
(4) graphene film preparation: by the graphene oxide film reduction after the compacting of step (3) gained, obtain graphene film.
In a preferred embodiment of the invention, described crosslinking agent is ethylenediamine, diethylenetriamine, triethylene tetramine, N-hydroxyethyl-ethylenediamine, polymine, dithioglycol, dimercaptopropane, 1,6-ethanthiol or 2,3-diaminopropionic acid.
In a preferred embodiment of the invention, described method of reducing is any one in following two kinds:
(1), under one or more reducing agent effects in hydrazine hydrate or hydroiodic acid, vitamin C, sodium borohydride, iron chloride of the xerogel after compacting, at 0 ~ 100 ℃, reduce 1 ~ 120min; Or,
(2) xerogel after compacting, under inert gas shielding effect, 100 ~ 800w microwave reduction, 5 ~ 300s.
The present invention also protects this application of Graphene basement membrane in water-oil separating.Wherein, profit comprises oil phase and water.
In a preferred embodiment of the invention, oil phase is the mixing of one or more components in oil, rape oil, gasoline, diesel oil, benzinum, cyclohexane, normal heptane, normal octane, ethyl acetate, benzene,toluene,xylene, carrene, chloroform; Wherein, oil phase accounts for 10 ~ 99.9% of oil phase and water mixed volume.
In a preferred embodiment of the invention, water is water, or the aqueous solution of one or more solutes in hydrochloric acid, sulfuric acid, nitric acid, phosphoric acid, NaOH, potassium hydroxide, sodium chloride, potassium chloride, copper chloride, iron chloride, copper sulphate, wherein in the aqueous solution, the mass fraction of total soluble matters is 0.1 ~ 90%.
In a preferred embodiment of the invention, in oil water mixture, contain one or more surfactants in span 80, this dish 60, this dish 20, Tween 80, polysorbate60, polysorbas20, neopelex, S-170.
The preparation method of this graphene-based water-oil separating film is simple, easily capable, with low cost, can mass industrialized production, and this is membranous light stable, can efficient circulation use.This graphene-based water-oil separating membrane material is can be under multiple environment efficient, low energy consumption, ultrahigh speed ground separating oil aqueous mixtures obtain oil content wherein, and water content is lower than 200ppm, and minimum water concentration can reach 10ppm, slightly variant according to different oil phases.
Accompanying drawing explanation
Below in conjunction with accompanying drawing, the present invention is further described
Fig. 1: the graphene-based water-oil separating film preparing in the embodiment of the present invention 2;
Fig. 2: the stereoscan photograph on the graphene-based water-oil separating film surface preparing in the embodiment of the present invention 2, can clearly see this very polishing of film surface;
Fig. 3 (a): the graphene-based water-oil separating film obtaining in the embodiment of the present invention 2 contact angle photo to oil droplet in air, contact angle is close to 0
o, confirm it and in air, there is super-oleophilic matter;
Fig. 3 (b): the graphene-based water-oil separating film obtaining in the embodiment of the present invention 2 contact angle photo to water droplet in air, contact angle approximately 95
o, confirm its tool hydrophobic property in air.
The specific embodiment
Below by embodiment, the present invention will be further described:
Embodiment 1
100 microlitre dithioglycols are joined in 10mL graphite oxide aqueous solution (80mg/mL), stir rear 70 ℃ of reaction 4h and obtain graphene oxide hydrogel, after hydrogel is dry, obtain graphene oxide xerogel; Under 50 kPas of pressure, by the compacting of graphene oxide xerogel, maintain 5min, subsequently xerogel is immersed in 85% hydrazine hydrate, 100 ℃ of reaction 30min, obtain Graphene basement membrane material; Finally, the graphene film material obtaining Soxhlet in the aqueous solution is extracted to 5h, 60 ℃ of oven dry can be directly used in water-oil separating.
Embodiment 2
100 microlitre ethylenediamines are joined in 10mL graphite oxide aqueous solution (50mg/mL), stir rear 100 ℃ of reaction 4h and obtain graphene oxide hydrogel, after hydrogel is dry, obtain graphene oxide xerogel; Under 80 kPas of pressure, by the compacting of graphene oxide xerogel, maintain 10min, subsequently xerogel is immersed in 55% hydroiodic acid, 90 ℃ of reaction 30min, obtain Graphene basement membrane material; Finally, the graphene film material obtaining Soxhlet in the aqueous solution is extracted to 5h, 60 ℃ of oven dry can be directly used in water-oil separating.
Embodiment 3
200 microlitre diethylenetriamines are joined in 10mL graphite oxide aqueous solution (20mg/mL), stir rear 120 ℃ of reaction 6h and obtain graphene oxide hydrogel, after hydrogel is dry, obtain graphene oxide xerogel; Under 80 kPas of pressure, by the compacting of graphene oxide xerogel, maintain 5min, subsequently xerogel is immersed in 85% hydrazine hydrate solution, 90 ℃ of reaction 10min, obtain Graphene basement membrane material; Finally, the graphene film material obtaining Soxhlet in the aqueous solution is extracted to 5h, 60 ℃ of oven dry can be directly used in water-oil separating.
Embodiment 4
50 microlitre polymines are joined in 10mL graphite oxide aqueous solution (5mg/mL), stir rear 70 ℃ of reaction 4h and obtain graphene oxide hydrogel, after hydrogel is dry, obtain graphene oxide xerogel; Under 50 kPas of pressure, by the compacting of graphene oxide xerogel, maintain 5min, xerogel 800w microwave 60 seconds under nitrogen protection, obtains Graphene basement membrane material and can be directly used in water-oil separating subsequently.
Embodiment 5
100 microlitre dimercaptopropanes are joined in 10mL graphite oxide aqueous solution (6mg/mL), stir rear 95 ℃ of reaction 4h and obtain graphene oxide hydrogel, after hydrogel is dry, obtain graphene oxide xerogel; Under 80 kPas of pressure, by the compacting of graphene oxide xerogel, maintain 10min, subsequently xerogel is immersed in 50mM sodium borohydride aqueous solution, 90 ℃ of reaction 30min, obtain Graphene basement membrane material; Finally, the graphene film material obtaining Soxhlet in the aqueous solution is extracted to 5h, 60 ℃ of oven dry can be directly used in water-oil separating.
Embodiment 6
Getting the graphene-based water-oil separating film that embodiment 2 prepares is fixed in filter; 90mL isooctane and 10mL water are mixed to form to suspension, pour on the separator of putting up, by diffusion barrier, water is trapped isooctane.Finally measuring water content in the isooctane obtaining is 10ppm.
Embodiment 7
Getting the graphene-based water-oil separating film that embodiment 2 prepares is fixed in filter; 50mL diesel oil and 50mL water are mixed to form to suspension, pour on the separator of putting up, by diffusion barrier, water is trapped diesel oil.Finally measuring water content in the diesel oil obtaining is 15ppm.
Embodiment 8
Getting the graphene-based water-oil separating film that embodiment 3 prepares is fixed in filter; 90mL toluene and 10mL8M sodium hydrate aqueous solution are mixed to form to suspension, pour on the separator of putting up, by diffusion barrier, sodium hydrate aqueous solution is trapped toluene.Finally measuring water content in the toluene obtaining is 80ppm.
Embodiment 9
Getting the graphene-based water-oil separating film that embodiment 5 prepares is fixed in filter; 40mL toluene, 40mL benzinum and 20mL water are mixed to form to suspension, pour on the separator of putting up, the aqueous solution is trapped by diffusion barrier for toluene and benzinum mixed solution.In the toluene that finally mensuration obtains and benzinum mixed solution, water content is 85ppm.
Embodiment 10
Getting the graphene-based water-oil separating film that embodiment 4 prepares is fixed in filter; 40mL toluene, 10mg S-170 and 60mL water are mixed to form to suspension, pour on the separator of putting up, by diffusion barrier, the aqueous solution is trapped toluene.Finally measuring water content in the toluene solution obtaining is 100ppm.
Embodiment 11
Getting the graphene-based water-oil separating film that embodiment 2 prepares is fixed in filter; 80mL ethyl acetate, 10mg neopelex and 20mL water are mixed to form to suspension, pour on the separator of putting up, by diffusion barrier, the aqueous solution is trapped ethyl acetate.Finally measuring water content in the ethyl acetate solution obtaining is 50ppm.
Embodiment 12
Getting the graphene-based water-oil separating film that embodiment 2 prepares is fixed in filter; 30mL ethyl acetate, 30mL normal octane, 10mg neopelex, 10mg Span80 and 40mL water are mixed to form to suspension, pour on the separator of putting up, the aqueous solution is trapped by diffusion barrier for ethyl acetate and normal octane mixed solution.In the ethyl acetate that finally mensuration obtains and normal octane mixed solution, water content is 90ppm.
Above embodiment shows and has described basic principle of the present invention and principal character and advantage of the present invention.The technical staff of the industry should understand; the present invention is not restricted to the described embodiments; that in above-described embodiment and description, describes just illustrates principle of the present invention; rather than limit the scope of the invention by any way; without departing from the scope of the invention; the present invention also has various changes and modifications, and these changes and improvements all fall in claimed scope.
Claims (9)
1. a preparation method for Graphene basement membrane, is characterized in that, forms gel by graphene oxide and crosslinking agent, dry, under 10 ~ 200 kPas of pressure, after compacting, reduces and obtains.
2. preparation method according to claim 1, is characterized in that specifically comprising the steps:
(1) preparation of graphene oxide hydrogel: getting 10mL concentration is the graphene oxide solution of 1 ~ 100mg/mL, adds the crosslinking agent of 0.5mmol ~ 0.1mol at 60 ~ 150 ℃ of reaction 4 ~ 8h, obtains graphene oxide hydrogel;
(2) preparation of graphene oxide xerogel: the dry processing of graphene oxide hydrogel that step (1) is obtained, obtains graphene oxide xerogel;
(3) press mold: by graphene oxide xerogel compacting under 10 ~ 200 kPas of pressure of step (2) gained, maintain 5 ~ 50min;
(4) graphene film preparation: by the graphene oxide film reduction after the compacting of step (3) gained, obtain Graphene basement membrane.
3. preparation method according to claim 2, it is characterized in that, described crosslinking agent is ethylenediamine, diethylenetriamine, triethylene tetramine, N-hydroxyethyl-ethylenediamine, polymine, dithioglycol, dimercaptopropane, 1,6-ethanthiol or 2,3-diaminopropionic acid.
4. preparation method according to claim 2, is characterized in that, described method of reducing is any one in following two kinds:
(1), under one or more reducing agent effects in hydrazine hydrate or hydroiodic acid, vitamin C, sodium borohydride, iron chloride of the xerogel after compacting, at 0 ~ 100 ℃, reduce 1 ~ 120min; Or,
(2) xerogel after compacting, under inert gas shielding effect, 100 ~ 800w microwave reduction, 5 ~ 300s.
5. the Graphene basement membrane preparing according to the preparation method one of claim 1-4 Suo Shu.
6. the application of Graphene basement membrane according to claim 5 in water-oil separating.
7. application according to claim 6, it is characterized in that, profit comprises oil phase and water, and wherein oil phase is the mixing of one or more components in oil, rape oil, gasoline, diesel oil, benzinum, cyclohexane, normal heptane, normal octane, ethyl acetate, benzene,toluene,xylene, carrene, chloroform; Oil phase accounts for 10 ~ 99.99% of oil phase and water mixed volume.
8. application according to claim 7, it is characterized in that, water is water, or the aqueous solution of one or more solutes in hydrochloric acid, sulfuric acid, nitric acid, phosphoric acid, NaOH, potassium hydroxide, sodium chloride, potassium chloride, copper chloride, iron chloride, copper sulphate, wherein in the aqueous solution, the mass fraction of total soluble matters is 0.1 ~ 90%.
9. according to the application one of claim 6-8 Suo Shu, it is characterized in that, in oil water mixture, contain one or more surfactants in span 80, this dish 60, this dish 20, Tween 80, polysorbate60, polysorbas20, neopelex, S-170.
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| CN104071785A (en) * | 2014-07-14 | 2014-10-01 | 中国科学院福建物质结构研究所 | Method for preparing graphene with three-dimensional macroscopic porous structure |
| CN104310389A (en) * | 2014-10-22 | 2015-01-28 | 福州大学 | Compressive graphene hydrogel and preparation method thereof |
| CN104857742A (en) * | 2015-05-28 | 2015-08-26 | 重庆理工大学 | Water removal method of dichloromethane |
| CN106115955A (en) * | 2016-08-12 | 2016-11-16 | 刘承建 | A kind of exhausting or trade effluent advanced treatment apparatus |
| CN107106991A (en) * | 2014-12-31 | 2017-08-29 | 乔治洛德方法研究和开发液化空气有限公司 | Carbon Molecular Sieve Membrane is manufactured using the pyrolysis atmosphere comprising sulfur-containing compound |
| CN107528052A (en) * | 2017-08-16 | 2017-12-29 | 南京师范大学 | Graphene derived from a kind of double-network hydrogel/tin-nickel alloy composite and its preparation method and application |
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| CN109292754A (en) * | 2018-08-07 | 2019-02-01 | 济南大学 | A kind of preparation method of polyethyleneimine-modified graphene aerogel |
| CN109292765A (en) * | 2018-12-07 | 2019-02-01 | 四川聚创石墨烯科技有限公司 | A method of preparing low layer number redox graphene |
| US10266413B2 (en) * | 2016-11-04 | 2019-04-23 | University Of Connecticut | Fractionation of graphene oxide through emulsion stabilization and graphene oxide produced thereby |
| CN109803750A (en) * | 2016-10-03 | 2019-05-24 | 日东电工株式会社 | The antimicrobial element of graphene oxide |
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| CN104071785A (en) * | 2014-07-14 | 2014-10-01 | 中国科学院福建物质结构研究所 | Method for preparing graphene with three-dimensional macroscopic porous structure |
| CN104071785B (en) * | 2014-07-14 | 2016-01-13 | 中国科学院福建物质结构研究所 | A kind of method preparing the Graphene with three-dimensional macro vesicular structure |
| CN104310389A (en) * | 2014-10-22 | 2015-01-28 | 福州大学 | Compressive graphene hydrogel and preparation method thereof |
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| CN107106991A (en) * | 2014-12-31 | 2017-08-29 | 乔治洛德方法研究和开发液化空气有限公司 | Carbon Molecular Sieve Membrane is manufactured using the pyrolysis atmosphere comprising sulfur-containing compound |
| CN107106991B (en) * | 2014-12-31 | 2021-02-19 | 乔治洛德方法研究和开发液化空气有限公司 | Production of carbon molecular sieve membranes using a pyrolysis atmosphere comprising a sulfur-containing compound |
| CN104857742A (en) * | 2015-05-28 | 2015-08-26 | 重庆理工大学 | Water removal method of dichloromethane |
| US10442709B2 (en) | 2015-12-17 | 2019-10-15 | Nitto Denko Corporation | Selectively permeable graphene oxide membrane |
| CN106115955A (en) * | 2016-08-12 | 2016-11-16 | 刘承建 | A kind of exhausting or trade effluent advanced treatment apparatus |
| CN109803750A (en) * | 2016-10-03 | 2019-05-24 | 日东电工株式会社 | The antimicrobial element of graphene oxide |
| US10266413B2 (en) * | 2016-11-04 | 2019-04-23 | University Of Connecticut | Fractionation of graphene oxide through emulsion stabilization and graphene oxide produced thereby |
| CN107528052B (en) * | 2017-08-16 | 2020-05-05 | 南京师范大学 | Graphene/tin-nickel alloy composite material derived from double-network hydrogel and preparation method and application thereof |
| CN107528052A (en) * | 2017-08-16 | 2017-12-29 | 南京师范大学 | Graphene derived from a kind of double-network hydrogel/tin-nickel alloy composite and its preparation method and application |
| CN108671764A (en) * | 2018-06-13 | 2018-10-19 | 洛阳纳诺环保科技有限公司 | A kind of method that one-step method prepares super hydrophilic/underwater superoleophobic water-oil separationg film |
| CN109292754A (en) * | 2018-08-07 | 2019-02-01 | 济南大学 | A kind of preparation method of polyethyleneimine-modified graphene aerogel |
| CN109292765A (en) * | 2018-12-07 | 2019-02-01 | 四川聚创石墨烯科技有限公司 | A method of preparing low layer number redox graphene |
| CN110394162A (en) * | 2019-07-10 | 2019-11-01 | 浙江海洋大学 | A kind of preparation method of environmentally friendly magnetic Nano compound oil absorption material |
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