CN106693444A - Preparing method of reproducible super-hydrophobic graphite alkenyl oil absorption sponge - Google Patents
Preparing method of reproducible super-hydrophobic graphite alkenyl oil absorption sponge Download PDFInfo
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- CN106693444A CN106693444A CN201611221938.1A CN201611221938A CN106693444A CN 106693444 A CN106693444 A CN 106693444A CN 201611221938 A CN201611221938 A CN 201611221938A CN 106693444 A CN106693444 A CN 106693444A
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D17/00—Separation of liquids, not provided for elsewhere, e.g. by thermal diffusion
- B01D17/02—Separation of non-miscible liquids
- B01D17/0202—Separation of non-miscible liquids by ab- or adsorption
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Abstract
The invention discloses a preparing method of a reproducible super-hydrophobic graphite alkenyl oil absorption sponge. The method comprises the steps of soaking a melamine sponge into a graphene oxide suspension liquid, and conducting ultrasonic dispersion treatment; taking the sponge out, putting the sponge into a vacuum drying oven to be subjected to a thermal reductive reaction after remnant liquid is squeezed out; soaking the obtained sponge into an alcohol diluent of a silane coupling agent to be subjected to a thorough reaction; taking the sponge out, and putting the sponge into the vacuum drying oven when no liquid flows to dried to obtain the reproducible super-hydrophobic graphite alkenyl oil absorption sponge. The graphite alkenyl oil absorption sponge has super-hydrophobicity (a contact angle reaches 159.6 degrees), the saturated adsorption capacity to oil and organic solvents reaches 50-120 g/g, the mechanical stability is good, the porosity is high, the graphene coating does not shed from a sponge skeleton easily, and the sponge has good reproducible ability and can effectively separate the oil and the organic solvents in water. The reproducible super-hydrophobic graphite alkenyl oil absorption sponge is simple in process, low in cost and environmentally friendly, can be produced on a large scale, and has a big application potential in the fields of oil spill treatment and organic solvent recovery.
Description
Technical field
The present invention relates to a kind of preparation method of reproducible super-hydrophobic graphene-based oil suction sponge, belong to functional material
And water-oil separating field.
Background technology
With the fast development of petroleum chemical industry, a large amount of oils that the process such as oil exploitation, refining, oil product transport is produced
Leakage and industrial organic solvent pollution cause serious destruction to water ecological environment.Or traditional oil absorption material energy of adsorption
Power is low, poor selectivity, otherwise preparation technology is complicated, it is expensive, it is impossible to meet the need of extensive waste oil recovery and environmental improvement
Will.Therefore, exploitation cleaning, oil absorption material economic, efficient, can be recycled turn into recent research focus.
In recent years, researcher is applied in oils using the good characteristic that Graphene specific surface area is big, hydrophobicity is strong
And Adsorption of Organic field, develop many graphene-based materials with high oil absorption amount, including spongy graphene
(Spongy graphene), graphene-based sponge (Graphene based sponge) and carbon aerogels (Carbon
Aerogels) etc..These three-dimensional porous sponges have very high absorption capacity and selectivity, but its pore structure is unstable, easily
It is damaged, and preparation cost is higher, severe reaction conditions, limits its application in water-oil separating field.Porous polymer sea
Big, the elastic good, porosity of continuous intensity is high, density is low, cheap, is the good matrix for preparing oil absorption material.However, this kind of sea
It is continuous that generally there is hydrophily, it is impossible to realize water-oil separating.At present, using porous polymer sponge as base material, using graphite
The special surface property of ene coatings, hydrophobically modified is carried out to its surface, and the graphene-based oil suction sponge that hydrophobic oleophilic oil is obtained is one
Big research direction.But current graphene-based oil suction sponge is present, and mechanical strength is weaker, adsorption capacity is relatively low, water-oil separating performance
The problems such as poor, limited regeneration capability and graphite ene coatings easy to fall off；Additionally, commonly using hydration in Graphene reduction process
The poisonous reducing agent such as hydrazine, ethylenediamine, not only technique is cumbersome, and harm environment.
The patent of invention of the A of Application No. CN 102500133 discloses a kind of application process of graphene sponge, synthesis
Graphene sponge can be used for absorbing organic solvent or grease.The graphene sponge is obtained by self-assembling reaction, though to oils and
Organic solvent has good adsorption effect, but sponge intensity is not enough, and destructible sponge structure in extrusion process can only be used low
The method of pressure distillation, extraction or high temperature distillation, organic solvent or grease are removed from graphene sponge or reclaimed profit
With.
The patent of invention of the A of Application No. CN 103342827 discloses a kind of preparation of hydrophobic/lipophilpolyurethane polyurethane sponge
Method, expanded graphite is prepared first with crystalline flake graphite, and expanded graphite is flowed back 36h in concentrated nitric acid, and in ammoniacal liquor/ethanol mixing
Ultrasonically treated 3h in solution, then by gained material in ethanol solution ultrasound 90min, obtain few layer graphene nanoscale twins.Most
Polyurethane sponge is immersed in Graphene ethanol solution afterwards, hydrophobic oleophilic oil sponge is obtained after drying.Should sponge sucks in water multiplying power and suction
Oily multiplying power is respectively up to 0.04 and 43 times, and hydrophobic and oil absorbing effect is preferable.But the patent is both contacted not over the water of test sponge
Angle size carrys out the hydrophobic effect for expressing sponge directly perceived, does not also investigate the regenerability of sponge.
The patent of invention of the A of Application No. CN 104338519 disclose a kind of modified graphene load polyurethane sponge and
Its preparation method, by through on silane coupler modified Graphene coating load to polyurethane sponge, sponge is become by hydrophilic
Super-hydrophobic (contact angle is 161 °), oil absorption enhancing, the saturated extent of adsorption to diesel oil reaches 37.89g, but still in relatively low water
It is flat.
It is multiple that the patent of invention of the A of Application No. CN 105754144 discloses a kind of super-hydrophobic redox graphene/sponge
, with ethylenediamine as reducing agent, be reduced into graphene oxide also in microwave-ultrasonic reactor by condensation material and preparation method thereof
Former graphene oxide, and redox graphene is disperseed and is attached on commodity sponge under the sound wave effects such as hole, obtain
Redox graphene with super-hydrophobicity/sponge composite.The invention is simple to operate, gained sponge oleophilic drainage performance
Preferably, but from having strong basicity and corrosive ethylenediamine to carry out redox graphene, there is certain harm to environment；The patent
The regenerability of sponge is not investigated yet.
Patent of invention content
It is an object of the invention to provide a kind of preparation method of super-hydrophobic graphene-based oil suction sponge, the Graphene of gained
Base sponge can effectively in adsorbed water body oils and organic solvent, with mechanical flexibility it is good, power of regeneration is strong, technique is simple
Single, environment-friendly and with low cost advantage.
A kind of preparation method of reproducible super-hydrophobic graphene-based oil suction sponge, is specifically carried out as follows：
(1) clean melamine sponge is immersed in graphene oxide suspension, ultrasonic disperse makes graphene oxide uniform
Be attached on melamine sponge；
(2) step (1) gained sponge is taken out, extracts and be put into vacuum drying chamber after residual liquid and carry out thermal reduction reaction；
(3) step (2) gained sponge is immersed the ethanol dilution of silane coupler, impregnation takes out afterwards for a period of time
Sponge, is put into vacuum drying chamber drying target product after liquid no longer trickles.
Described clean melamine sponge carries out ultrasonic rinse successively by ethanol and pure water, is subsequently placed in 50~80 DEG C
Vacuum drying chamber drying to constant weight is obtained.
Described graphene oxide suspension is prepared by improved Hummer ' s methods；Described graphene oxide hangs
Supernatant liquid concentration is 2~4mg/L.
Described melamine sponge be immersed in the ultrasonic disperse time needed for graphene oxide suspension for 30~
60min, supersonic frequency is 25~80kHz, and ultrasonic power is 50~200W.
Described thermal reduction reaction temperature is 160~200 DEG C, and vacuum drying chamber vacuum is 1500~2000Pa, reaction
Time is 8~12h.
The volume fraction of ethanol dilution shared by described silane coupler is 2~5%.
Described silane coupler is γ aminopropyltriethoxy silane, γ-glycidyl ether oxygen propyl trimethoxy
Silane, γ-methacryloxypropyl trimethoxy silane, γ-mercaptopropyl trimethoxysilane, γ-ethoxy of mercapto propyl group three
One or more in base silane, ethylenediamine hydroxypropyl methyl dimethoxysilane, ethylenediaminepropyltriethoxysilane.
Described sponge is 2~8h, vacuum drying chamber drying temperature with the ethanol dilution reaction time of silane coupler
≤80℃。
Compared with prior art, the present invention has following distinguishing feature：
1. the melamine porous polymer substrate sponge good mechanical stability of selection, porosity are high, modified through Graphene
Turn into super-hydrophobic oleophylic sponge afterwards, there is good adsorbing separation ability to oils in water and organic solvent；
2. acted on using " molecular bridge " of silane coupler, by Graphene and melamine sponge skeleton in covalent bond form
Combine, even if extruding sponge repeatedly, graphene film also can be sticked to stably on sponge, difficult for drop-off, therefore sponge exists
Still there is stronger oil and water separation capability after recycling repeatedly；
3. preparation method selected by replaces the use of the poisonous reducing agents such as hydrazine hydrate, environment friend using thermal reduction Graphene method
Good, process is simple, it is with low cost, can mass produce, oil spill accident process have with organic solvent recycling field it is larger
Application potential.
Brief description of the drawings
Fig. 1 is the water drop static contact angle test chart of the graphene-based oil suction sponge that embodiment 1 is obtained；
Fig. 2 is that the graphene-based oil suction sponge that embodiment 2 is obtained is tried hard to the saturation energy of adsorption of oils, organic solvent；
Fig. 3 is the graphene-based oil suction sponge that obtains of embodiment 3 to oils, the regenerative adsorption lab diagram of organic solvent.
Fig. 4 is that the graphene-based oil suction sponge that embodiment 4 is obtained is connected by emulsion tube with vavuum pump, to the diesel oil in water
The lab diagram being continuously separated.
Specific embodiment
For convenience of the present invention is understood, this is with reference to the embodiment content that the present invention is furture elucidated, inventive technique scheme
It is not limited solely to the specific embodiment being set forth below.
Embodiment 1：
Dried 55 DEG C of vacuum drying chambers are placed in through the clean melamine sponge after ethanol and pure water successively ultrasonic rinse
To constant weight, then it is immersed in 2mg/mL graphene oxide suspensions, ultrasonic disperse 60min, supersonic frequency is 40kHz,
Ultrasonic power is 50W；Sponge is taken out, being put into 160 DEG C of vacuum drying chambers after extracting after residual liquid carries out thermal reduction reaction, vacuum
It is 2000Pa to spend, and the reaction time is 12h；By the γ aminopropyltriethoxy silane of gained sponge immersion volume fraction 2%
Ethanol dilution, reacts 8h；Sponge is taken out, vacuum drying chamber drying is put into after liquid no longer trickles.
As can be seen from Figure 1：Obtained graphene-based sponge has a super-hydrophobicity, the globule on its surface in spherical, it is quiet
State contact angle up to 159.6 °, with good hydrophobicity.
Embodiment 2：
Dried 50 DEG C of vacuum drying chambers are placed in through the clean melamine sponge after ethanol and pure water successively ultrasonic rinse
To constant weight, then it is immersed in 4mg/mL graphene oxide suspensions, ultrasonic disperse 45min, supersonic frequency is 40kHz,
Ultrasonic power is 150W；Sponge is taken out, to be extracted and be put into 180 DEG C of vacuum drying chambers after residual liquid and carry out thermal reduction reaction, vacuum
It is 1800Pa to spend, and the reaction time is 10h；Gained sponge is immersed the γ-methacryloxypropyl front three of volume fraction 2%
The ethanol dilution of TMOS, reacts 6h；Sponge is taken out, vacuum drying chamber drying is put into after liquid no longer trickles.
As can be seen from Figure 2：Obtained graphene-based oil suction sponge is to the saturated extent of adsorption of oils and organic solvent up to certainly
50~120 times of body quality, adsorption capacity is higher than the common sorbing material such as activated carbon.
Embodiment 3：
Dried 60 DEG C of vacuum drying chambers are placed in through the clean melamine sponge after ethanol and pure water successively ultrasonic rinse
To constant weight, then it is immersed in 2.5mg/mL graphene oxide suspensions, ultrasonic disperse 30min, supersonic frequency is
40kHz, ultrasonic power is 100W；Sponge is taken out, is extracted and be put into after residual liquid 200 DEG C of vacuum drying chambers to carry out thermal reduction anti-
Should, vacuum is 1600Pa, and the reaction time is 8h；Gained sponge is immersed the γ-mercapto propyl trimethoxy silicon of volume fraction 3%
The ethanol dilution of alkane, reacts 4h；Sponge is taken out, vacuum drying chamber drying is put into after liquid no longer trickles.
As can be seen from Figure 3：Obtained graphene-based oil suction sponge is in the regenerative adsorption to different oils and organic solvent
In experiment, 3 times adsorption process, the saturation adsorption capacity of sponge slowly declines with the increase of regeneration times, hereafter adsorbance
It is held essentially constant, and there is not obscission in graphite ene coatings.Sponge saturation adsorption capacity still reaches after 10 circulation experiments
38~98 times, illustrate that obtained sponge has good renewable.
Embodiment 4：
Dried 50 DEG C of vacuum drying chambers are placed in through the clean melamine sponge after ethanol and pure water successively ultrasonic rinse
To constant weight, then it is immersed in 3.5mg/mL graphene oxide suspensions, ultrasonic disperse 60min, supersonic frequency is
40kHz, ultrasonic power is 50W；Sponge is taken out, to be extracted and be put into 185 DEG C of vacuum drying chambers after residual liquid and carry out thermal reduction reaction,
Vacuum is 1800Pa, and the reaction time is 12h；Gained sponge is immersed the γ-mercaptopropyl trimethoxysilane of volume fraction 3%
Ethanol dilution, react 4h；Sponge is taken out, vacuum drying chamber drying is put into after liquid no longer trickles.
As can be seen from Figure 4：Obtained graphene-based oil suction sponge (2.5 × 2.5 × 5cm3) pass through emulsion tube and vacuum
Pump is connected, and the diesel oil in diesel oil/water mixed system (diesel oil 100mL, pure water 300mL) is continuously adsorbed, the water surface after 35s
Diesel oil is all recycled in the flask in left side, and whole process beaker water level remains at 300mL graduation positions, illustrates to be obtained
Sponge possess good oil and water separation capability, there is larger application prospect in oil spilling recycling field.
Claims (9)
1. a kind of preparation method of reproducible super-hydrophobic graphene-based oil suction sponge, it is characterised in that reproducible super-hydrophobic
The preparation of graphene-based oil suction sponge is carried out as follows：
(1) clean melamine sponge is immersed in graphene oxide suspension, ultrasonic disperse makes graphene oxide equably attached
On melamine sponge；
(2) step (1) gained sponge is taken out, extracts and be put into vacuum drying chamber after residual liquid and carry out thermal reduction reaction；
(3) step (2) gained sponge is immersed the ethanol dilution of silane coupler, impregnation takes out sea afterwards for a period of time
Silk floss, is put into vacuum drying chamber drying target product after liquid no longer trickles.
2. the preparation method of reproducible super-hydrophobic graphene-based oil suction sponge according to claim 1, it is characterised in that
Clean melamine sponge described in step (1) carries out ultrasonic rinse successively by ethanol and pure water, is subsequently placed in 50~80
DEG C vacuum drying chamber drying to constant weight is obtained.
3. the preparation method of reproducible super-hydrophobic graphene-based oil suction sponge according to claim 1, it is characterised in that
Graphene oxide suspension described in step (1) is prepared by improved Hummer ' s methods；Described graphene oxide
Suspension concentration is 2~4mg/L.
4. the preparation method of reproducible super-hydrophobic graphene-based oil suction sponge according to claim 1, it is characterised in that
Ultrasonic disperse time described in step (1) is 30~60min, and supersonic frequency is 25~80kHz, ultrasonic power is 50~
200W。
5. the preparation method of reproducible super-hydrophobic graphene-based oil suction sponge according to claim 1, it is characterised in that
Thermal reduction reaction temperature described in step (2) is 160~200 DEG C, and vacuum drying chamber vacuum is 1500~2000Pa.
6. the preparation method of reproducible super-hydrophobic graphene-based oil suction sponge according to claim 1, it is characterised in that
The thermal reduction reaction time described in step (2) is 8~12h.
7. the preparation method of reproducible super-hydrophobic graphene-based oil suction sponge according to claim 1, it is characterised in that
The volume fraction of ethanol dilution shared by silane coupler described in step (3) is 2~5%.
8. the preparation method of reproducible super-hydrophobic graphene-based oil suction sponge according to claim 1, it is characterised in that
Silane coupler described in step (3) is γ aminopropyltriethoxy silane, γ-glycidyl ether oxygen propyl trimethoxy
Base silane, γ-methacryloxypropyl trimethoxy silane, γ-mercaptopropyl trimethoxysilane, γ-second of mercapto propyl group three
One or more in TMOS, ethylenediamine hydroxypropyl methyl dimethoxysilane, ethylenediaminepropyltriethoxysilane.
9. the preparation method of reproducible super-hydrophobic graphene-based oil suction sponge according to claim 1, it is characterised in that
The impregnation time described in step (3) is 2~8h, vacuum drying chamber drying temperature≤80 DEG C.
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Cited By (18)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107876033A (en) * | 2017-11-16 | 2018-04-06 | 武汉工程大学 | The method that solution dipping method prepares the hydrophobic oleophilic oil melamine sponge of carbon nano-tube modification |
| CN108744606A (en) * | 2018-07-13 | 2018-11-06 | 北京欧美中科学技术研究院 | The preparation method of graphene sponge for water-oil separating |
| CN108854162A (en) * | 2018-07-13 | 2018-11-23 | 北京欧美中科学技术研究院 | A kind of preparation method of the graphene composite material for water process |
| CN108854977A (en) * | 2018-07-31 | 2018-11-23 | 李忠 | A kind of hydrophobic oil suction modified sponge composite material and preparation method |
| CN108854261A (en) * | 2018-07-09 | 2018-11-23 | 山东佳星环保科技有限公司 | The preparation method of graphene high-efficiency filtering material for air purifying |
| CN108997607A (en) * | 2018-07-12 | 2018-12-14 | 山东佳星环保科技有限公司 | The preparation method of the hydrophobic oil suction sponge of graphene |
| CN110090631A (en) * | 2019-05-27 | 2019-08-06 | 深圳市辉翰科技发展有限公司 | A kind of large area charing sponge and preparation method thereof that the graphene of modifying super hydrophobicity is modified |
| CN110152619A (en) * | 2018-04-12 | 2019-08-23 | 济南开发区星火科学技术研究院 | A kind of preparation method of graphene oil suction sponge |
| CN110183723A (en) * | 2019-06-27 | 2019-08-30 | 中素新科技有限公司 | Graphene-based oil suction sponge and its preparation method and application |
| CN110237830A (en) * | 2019-06-19 | 2019-09-17 | 南京林业大学 | A kind of mild preparation method of environmental protection of hydrophobic oleophilic oil sponge |
| CN110947359A (en) * | 2018-09-26 | 2020-04-03 | 中国石油天然气股份有限公司 | Low-density high-elasticity hydrophobic/oleophylic carbon sponge and preparation method and application thereof |
| WO2020080922A1 (en) * | 2018-10-16 | 2020-04-23 | Ecole Supérieure Des Industries Du Textile Et De L'habillement | Device for separating immiscible liquids using a textile membrane functionalised by ionic liquids |
| CN111073031A (en) * | 2018-10-22 | 2020-04-28 | 中国石油化工股份有限公司 | Preparation method of hydrophobically modified melamine sponge |
| CN111167421A (en) * | 2020-01-16 | 2020-05-19 | 南通纺织丝绸产业技术研究院 | Graphene-loaded polyurethane sponge adsorption material and preparation method thereof |
| CN108160036B (en) * | 2018-01-29 | 2020-11-24 | 重庆工商大学 | Preparation method and application of super-hydrophobic magnetic foam material |
| CN115193409A (en) * | 2022-07-15 | 2022-10-18 | 中国石油大学(华东) | Photo-thermal adsorption heavy oil material based on modified melamine sponge, and preparation and application thereof |
| CN115364811A (en) * | 2022-08-24 | 2022-11-22 | 榆林学院 | Petroleum asphalt nano sponge base macroporous carbon and preparation method and application thereof |
| WO2023080352A1 (en) * | 2021-11-03 | 2023-05-11 | 한남대학교 산학협력단 | Method for preparing oil absorbent using polyurethane sponge |
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| CN107876033A (en) * | 2017-11-16 | 2018-04-06 | 武汉工程大学 | The method that solution dipping method prepares the hydrophobic oleophilic oil melamine sponge of carbon nano-tube modification |
| CN108160036B (en) * | 2018-01-29 | 2020-11-24 | 重庆工商大学 | Preparation method and application of super-hydrophobic magnetic foam material |
| CN110152619A (en) * | 2018-04-12 | 2019-08-23 | 济南开发区星火科学技术研究院 | A kind of preparation method of graphene oil suction sponge |
| CN108854261A (en) * | 2018-07-09 | 2018-11-23 | 山东佳星环保科技有限公司 | The preparation method of graphene high-efficiency filtering material for air purifying |
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| CN108744606A (en) * | 2018-07-13 | 2018-11-06 | 北京欧美中科学技术研究院 | The preparation method of graphene sponge for water-oil separating |
| CN108854162A (en) * | 2018-07-13 | 2018-11-23 | 北京欧美中科学技术研究院 | A kind of preparation method of the graphene composite material for water process |
| CN108854977A (en) * | 2018-07-31 | 2018-11-23 | 李忠 | A kind of hydrophobic oil suction modified sponge composite material and preparation method |
| CN110947359A (en) * | 2018-09-26 | 2020-04-03 | 中国石油天然气股份有限公司 | Low-density high-elasticity hydrophobic/oleophylic carbon sponge and preparation method and application thereof |
| WO2020080922A1 (en) * | 2018-10-16 | 2020-04-23 | Ecole Supérieure Des Industries Du Textile Et De L'habillement | Device for separating immiscible liquids using a textile membrane functionalised by ionic liquids |
| CN111073031A (en) * | 2018-10-22 | 2020-04-28 | 中国石油化工股份有限公司 | Preparation method of hydrophobically modified melamine sponge |
| CN111073031B (en) * | 2018-10-22 | 2022-07-12 | 中国石油化工股份有限公司 | Preparation method of hydrophobically modified melamine sponge |
| CN110090631A (en) * | 2019-05-27 | 2019-08-06 | 深圳市辉翰科技发展有限公司 | A kind of large area charing sponge and preparation method thereof that the graphene of modifying super hydrophobicity is modified |
| CN110237830A (en) * | 2019-06-19 | 2019-09-17 | 南京林业大学 | A kind of mild preparation method of environmental protection of hydrophobic oleophilic oil sponge |
| CN110183723A (en) * | 2019-06-27 | 2019-08-30 | 中素新科技有限公司 | Graphene-based oil suction sponge and its preparation method and application |
| CN111167421A (en) * | 2020-01-16 | 2020-05-19 | 南通纺织丝绸产业技术研究院 | Graphene-loaded polyurethane sponge adsorption material and preparation method thereof |
| CN111167421B (en) * | 2020-01-16 | 2021-09-17 | 南通纺织丝绸产业技术研究院 | Graphene-loaded polyurethane sponge adsorption material and preparation method thereof |
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| CN115193409A (en) * | 2022-07-15 | 2022-10-18 | 中国石油大学(华东) | Photo-thermal adsorption heavy oil material based on modified melamine sponge, and preparation and application thereof |
| CN115364811A (en) * | 2022-08-24 | 2022-11-22 | 榆林学院 | Petroleum asphalt nano sponge base macroporous carbon and preparation method and application thereof |
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Application publication date: 20170524 |