CN109608688A - A kind of preparation method of the graphene sponge of high efficiency oil-water separation - Google Patents
A kind of preparation method of the graphene sponge of high efficiency oil-water separation Download PDFInfo
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Abstract
A kind of preparation method of the graphene sponge of high efficiency oil-water separation, includes the following steps: the polyurethane sponge of (1) cleaning；(2) preparation of graphene oxide；(3) preparation of graphene oxide dispersion；(4) configuration of 2mg/ml graphene oxide alcohol suspension；(5) the clean melamine sponge that addition hydrazine hydrate and step 1 obtain into the graphene oxide alcohol suspension that step 4 obtains, it is placed in microwave chemical reactor, 30-60min is reacted in microwave heating, it is subsequently placed in ultrasonic cleaning machine ultrasonic disperse 30-50min, increase the distributing homogeneity of graphene oxide, sponge is taken out, is washed with deionized, is put into 80-100 DEG C of oven drying；(6) dimethyl silicone polymer/hexane solution preparation；(7) preparation of the graphene sponge of high efficiency oil-water separation.The present invention has excellent absorption property and good hydrophobicity.
Description
Technical field
The present invention relates to polymeric material fields, and in particular to a kind of preparation side of the graphene sponge of high efficiency oil-water separation
Method.
Background technique
With the fast development of the modern industry, the increasingly deficient of land resources increases energy demand rapidly with the mankind,
Shallow sea petroleum resources are continually developed.But with the exploitation of submarine oil and crude oil etc., product is also constantly at sea transported
Defeated, this just inevitably produces many marine oil pollution events, the leakage thing of gas blowout accident and Transport Oiler Ship when such as developing
Therefore it waits.Deepwater oil leaks and not only has brought tremendous economic losses to us, it is often more important that the marine eco-environment and
Periphery seashore causes great pollution.Firstly, petroleum can seriously endanger the existence of aquatile, the intake of ocean mammal
After oil spilling, viscera function is damaged, and certain petroleum components can make lactation animal and free mushroom to the consciousness of chemical stimulation
Imbalance, and the chemical information between aqueous bio is hindered to transmit；Greasy dirt can make the feather of aquatic bird lose thermal insulating and water-proof effect, and wing is viscous
There is greasy dirt to be also difficult to fly.As long as will significantly change sunlight, air to water studies have shown that: the water surface has very thin oil film
" input " of body, thus the death of the seaweed and other lower hydrobionts of causing birds edible.In addition the toxicity of oil product, is caused
Ecological environment sharply deteriorates, or even can induce marine red tide.It is reported that in the past 50 years because oily pollution has more than 1000 kinds of sea lifes
Omnicide, marine organisms have reduced 40%；In addition, oil spilling also generates important influence to human health.Comet passes through examination
Test the intracorporal poisonous substance accumulation of shellfish analyzed by oil spill, it was found that certain density polycyclic aromatic hydrocarbon (PAH), people
If eaten absorb petroleum fish and shellfish, the long-acting poisonous substance such as carcinogenic substance in petroleum will be brought into vivo.Furthermore petroleum
The organic steam that volatilization is formed, which is diffused into atmosphere, can also pollute atmospheric environment, cause photochemical fog, equally understand stimulating human
Vision, the organic matter in damage to the environment causes plant necrosis etc..
In order to administer petroleum pollution in ocean, its harm is reduced to greatest extent, and lot of domestic and foreign scholar has carried out various
Research.And administering method common at present has Mechanical Method, combustion method, biological restoration, material absorption process etc..Machinery physically
Absorption method not only solves oil slick problem on ocean, also by the energy recycling do not waste, but the oil fence cannot ensure it is fast
Speed, the trend of fully control oil diffusion, therefore it still has certain limitation.It is simplest method that combustion method, which seems, still
Product after burning can cause secondary pollution to environment, therefore up to the present all high sea oil leak events did not all use
This kind of method.What biological restoration mostly used is surfactant to realize, especially biosurfactant combines surface
The hydrophobicity of activating agent and the degradation function of microorganism can achieve efficient, nontoxic, antibacterial, economy, degradable and without secondary dirt
The advantages that dye, it is contemplated that industrial cost, the problems such as ecological balance and time are longer, are not also commonly used at oil spill
Reason.Material absorption process at present, due to it efficiently, quickly, do not generate secondary pollution, and the advantages that can be carried out recycling, become
The prefered method of oil spill processing.The type of absorbent has polymeric type absorbent, natural material absorbent and fiber now
Material absorbent etc., wherein graphene is due to its unique two-dimensional structure and its special hydrophobic oleophilic oil characteristic, as a kind of
Coating material has become the hot spot of oil absorption material research.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation methods of the graphene sponge of high efficiency oil-water separation, have excellent
Absorption property and good hydrophobicity.
The technical solution adopted by the present invention to solve the technical problems is: a kind of graphene sponge of high efficiency oil-water separation
Preparation method includes the following steps:
(1) polyurethane sponge is placed in ethyl alcohol and cleans 10-20min, be placed in a vacuum drying oven drying, obtain cleaning
Polyurethane sponge；
(2) preparation of graphene oxide: flaky graphite is added in the mixture of sodium nitrate and the concentrated sulfuric acid, in ice bath
Under the conditions of uniform magnetic agitation；Potassium permanganate is slowly added in mixed solution, control mixed solution temperature is lower than 20 DEG C and magnetic
Power stirs 1-3h, and it is 35-45 DEG C and magnetic agitation 1-2h that mixed solution temperature is then controlled under condition of ice bath；It is molten to mixing again
It is 70 DEG C of deionized waters that temperature is added in liquid, obtains bright orange color contamination liquid after being eventually adding the hydrogen peroxide that mass fraction concentration is 30%
Solution obtains graphene oxide after being 6-7 with deionized water centrifuge washing to pH；
(3) graphene oxide for obtaining step 2 is added in ethyl alcohol, ultrasonic disperse 1-3h, obtains graphene oxide point
Dispersion liquid；
(4) coupling agent is add to deionized water, the pH value for adjusting the solution is 3-5, and stirring hydrolyzes 30-50min, so
It is slowly added into the graphene oxide dispersion that step 3 obtains, 60 DEG C of reaction 4h, is centrifugated afterwards, with ethanol washing, 80 DEG C
Lower drying for 24 hours, is then ground, and it is outstanding to be configured to 2mg/ml graphene oxide ethyl alcohol into ethanol solution for redisperse after grinding
Supernatant liquid, remain using；
(5) clean three that addition hydrazine hydrate and step 1 obtain into the graphene oxide alcohol suspension that step 4 obtains
Poly cyanamid sponge, is placed in microwave chemical reactor, and microwave heating reacts 30-60min, is subsequently placed in ultrasonic cleaning machine ultrasonic disperse
30-50min increases the distributing homogeneity of graphene oxide, takes out sponge, is washed with deionized, is put into 80-100 DEG C of baking oven
It is dry；
(6) dimethyl silicone polymer is added in n-hexane, ultrasonic disperse is uniform, obtains dimethyl silicone polymer/just
Hexane solution；
(7) sponge for drying step 5 is immersed in dimethyl silicone polymer/hexane solution that step 6 obtains, dipping
2-4h is reacted, the residual liquid in sponge gap is extracted, is placed in after 80-120 DEG C of oven drying to get high efficiency oil-water separation is arrived
Graphene sponge.
Preferably, in step 2, flaky graphite, sodium nitrate, the concentrated sulfuric acid, potassium permanganate, 70 DEG C of deionized waters, quality point
The mass ratio for the hydrogen peroxide that Particle density is 30% is 1-5:3-6:100-180:1-4:150-200:1-4.
Preferably, in step 3, graphene oxide, ethyl alcohol mass ratio be 1-5:50-150.
Preferably, in step 4, coupling agent, deionized water mass ratio be 1-3:50-100.
Preferably, in step 4, coupling agent is γ-glycidyl ether oxygen propyl trimethoxy silicane.
Preferably, in step 5, graphene oxide alcohol suspension, hydrazine hydrate mass ratio be 80-300:1-5.
Preferably, in step 6, dimethyl silicone polymer, n-hexane mass ratio be 1-5:50-200.
The invention has the following advantages: the preparation side for the graphene sponge that a kind of high efficiency oil-water of the invention separates
Method has excellent absorption property and good hydrophobicity；γ-glycidyl ether oxygen propyl trimethoxy silicane can make oxygen
The dispersion of graphite alkene lamella becomes more uniformly, by γ-glycidyl ether oxygen propyl trimethoxy silicane to graphene oxide
Modified effect is very good；In the polyurethane sponge area load stone modified through γ-glycidyl ether oxygen propyl trimethoxy silicane
Black alkene, so that script had not only absorbed water but also the sponge of oil suction has good hydrophobicity and stronger oil absorption；Using poly dimethyl
Siloxanes changes the polyurethane sponge for the graphene that load has γ-glycidyl ether oxygen propyl trimethoxy silicane modified
Property, cause hydrophobic performance to greatly promote.
Specific embodiment
Embodiment 1
A kind of preparation method of the graphene sponge of high efficiency oil-water separation, includes the following steps:
(1) polyurethane sponge is placed in ethyl alcohol and cleans 10min, be placed in a vacuum drying oven drying, obtain clean gather
Urethane sponge；
(2) preparation of graphene oxide: flaky graphite is added in the mixture of sodium nitrate and the concentrated sulfuric acid, in ice bath
Under the conditions of uniform magnetic agitation；Potassium permanganate is slowly added in mixed solution, control mixed solution temperature is lower than 20 DEG C and magnetic
Power stirs 1h, and it is 35 DEG C and magnetic agitation 1h that mixed solution temperature is then controlled under condition of ice bath；Add again into mixed solution
Entering temperature is 70 DEG C of deionized waters, obtains bright orange color contamination liquor after being eventually adding the hydrogen peroxide that mass fraction concentration is 30%,
Graphene oxide is obtained after being 6 with deionized water centrifuge washing to pH；Flaky graphite, sodium nitrate, the concentrated sulfuric acid, potassium permanganate,
The mass ratio for the hydrogen peroxide that 70 DEG C of deionized waters, mass fraction concentration are 30% is 1:3:100:1:150:1；
(3) graphene oxide for obtaining step 2 is added in ethyl alcohol, ultrasonic disperse 1h, obtains graphene oxide dispersion
Liquid；Graphene oxide, ethyl alcohol mass ratio be 1:50；
(4) γ-glycidyl ether oxygen propyl trimethoxy silicane is add to deionized water, adjusts the pH value of the solution
It is 3, stirring hydrolysis 30min is then slowly added in the graphene oxide dispersion that step 3 obtains, 60 DEG C of reaction 4h, is centrifuged
Separation, with ethanol washing, at 80 DEG C it is dry for 24 hours, then ground, redisperse is configured into ethanol solution after grinding
2mg/ml graphene oxide alcohol suspension, remain using；γ-glycidyl ether oxygen propyl trimethoxy silicane, deionized water
Mass ratio be 1:50；
(5) clean three that addition hydrazine hydrate and step 1 obtain into the graphene oxide alcohol suspension that step 4 obtains
Poly cyanamid sponge, is placed in microwave chemical reactor, and microwave heating reacts 30min, is subsequently placed in ultrasonic cleaning machine ultrasonic disperse
30min increases the distributing homogeneity of graphene oxide, takes out sponge, is washed with deionized, is put into 80 DEG C of oven dryings；Oxygen
Graphite alkene alcohol suspension, hydrazine hydrate mass ratio be 80:1；
(6) dimethyl silicone polymer is added in n-hexane, ultrasonic disperse is uniform, obtains dimethyl silicone polymer/just
Hexane solution；Dimethyl silicone polymer, n-hexane mass ratio be 1:50；
(7) sponge for drying step 5 is immersed in dimethyl silicone polymer/hexane solution that step 6 obtains, dipping
2h is reacted, the residual liquid in sponge gap is extracted, is placed in after 80 DEG C of oven dryings to get the graphene separated to high efficiency oil-water
Sponge.
Embodiment 2
A kind of preparation method of the graphene sponge of high efficiency oil-water separation, includes the following steps:
(1) polyurethane sponge is placed in ethyl alcohol and cleans 20min, be placed in a vacuum drying oven drying, obtain clean gather
Urethane sponge；
(2) preparation of graphene oxide: flaky graphite is added in the mixture of sodium nitrate and the concentrated sulfuric acid, in ice bath
Under the conditions of uniform magnetic agitation；Potassium permanganate is slowly added in mixed solution, control mixed solution temperature is lower than 20 DEG C and magnetic
Power stirs 1-3h, and it is 35-45 DEG C and magnetic agitation 1-2h that mixed solution temperature is then controlled under condition of ice bath；It is molten to mixing again
It is 70 DEG C of deionized waters that temperature is added in liquid, obtains bright orange color contamination liquid after being eventually adding the hydrogen peroxide that mass fraction concentration is 30%
Solution obtains graphene oxide after being 6-7 with deionized water centrifuge washing to pH；Flaky graphite, sodium nitrate, the concentrated sulfuric acid, height
The mass ratio for the hydrogen peroxide that potassium manganate, 70 DEG C of deionized waters, mass fraction concentration are 30% is 5:6:180:4:200:4；
(3) graphene oxide for obtaining step 2 is added in ethyl alcohol, ultrasonic disperse 3h, obtains graphene oxide dispersion
Liquid；Graphene oxide, ethyl alcohol mass ratio be 5:150；
(4) γ-glycidyl ether oxygen propyl trimethoxy silicane is add to deionized water, adjusts the pH value of the solution
It is 5, stirring hydrolysis 50min is then slowly added in the graphene oxide dispersion that step 3 obtains, 60 DEG C of reaction 4h, is centrifuged
Separation, with ethanol washing, at 80 DEG C it is dry for 24 hours, then ground, redisperse is configured into ethanol solution after grinding
2mg/ml graphene oxide alcohol suspension, remain using；γ-glycidyl ether oxygen propyl trimethoxy silicane, deionized water
Mass ratio be 3:100；
(5) clean three that addition hydrazine hydrate and step 1 obtain into the graphene oxide alcohol suspension that step 4 obtains
Poly cyanamid sponge, is placed in microwave chemical reactor, and microwave heating reacts 60min, is subsequently placed in ultrasonic cleaning machine ultrasonic disperse
50min increases the distributing homogeneity of graphene oxide, takes out sponge, is washed with deionized, is put into 100 DEG C of oven dryings；Oxygen
Graphite alkene alcohol suspension, hydrazine hydrate mass ratio be 300:5；
(6) dimethyl silicone polymer is added in n-hexane, ultrasonic disperse is uniform, obtains dimethyl silicone polymer/just
Hexane solution；Dimethyl silicone polymer, n-hexane mass ratio be 5:200；
(7) sponge for drying step 5 is immersed in dimethyl silicone polymer/hexane solution that step 6 obtains, dipping
4h is reacted, the residual liquid in sponge gap is extracted, is placed in after 120 DEG C of oven dryings to get the graphite separated to high efficiency oil-water
Alkene sponge.
Embodiment 3
A kind of preparation method of the graphene sponge of high efficiency oil-water separation, includes the following steps:
(1) polyurethane sponge is placed in ethyl alcohol and cleans 14min, be placed in a vacuum drying oven drying, obtain clean gather
Urethane sponge；
(2) preparation of graphene oxide: flaky graphite is added in the mixture of sodium nitrate and the concentrated sulfuric acid, in ice bath
Under the conditions of uniform magnetic agitation；Potassium permanganate is slowly added in mixed solution, control mixed solution temperature is lower than 20 DEG C and magnetic
Power stirs 1-3h, and it is 35-45 DEG C and magnetic agitation 1-2h that mixed solution temperature is then controlled under condition of ice bath；It is molten to mixing again
It is 70 DEG C of deionized waters that temperature is added in liquid, obtains bright orange color contamination liquid after being eventually adding the hydrogen peroxide that mass fraction concentration is 30%
Solution obtains graphene oxide after being 6-7 with deionized water centrifuge washing to pH；Flaky graphite, sodium nitrate, the concentrated sulfuric acid, height
The mass ratio for the hydrogen peroxide that potassium manganate, 70 DEG C of deionized waters, mass fraction concentration are 30% is 2:4:140:2:175:2；
(3) graphene oxide for obtaining step 2 is added in ethyl alcohol, ultrasonic disperse 2h, obtains graphene oxide dispersion
Liquid；Graphene oxide, ethyl alcohol mass ratio be 2:80；
(4) γ-glycidyl ether oxygen propyl trimethoxy silicane is add to deionized water, adjusts the pH value of the solution
It is 4, stirring hydrolysis 36min is then slowly added in the graphene oxide dispersion that step 3 obtains, 60 DEG C of reaction 4h, is centrifuged
Separation, with ethanol washing, at 80 DEG C it is dry for 24 hours, then ground, redisperse is configured into ethanol solution after grinding
2mg/ml graphene oxide alcohol suspension, remain using；γ-glycidyl ether oxygen propyl trimethoxy silicane, deionized water
Mass ratio be 2:80；
(5) clean three that addition hydrazine hydrate and step 1 obtain into the graphene oxide alcohol suspension that step 4 obtains
Poly cyanamid sponge, is placed in microwave chemical reactor, and microwave heating reacts 40min, is subsequently placed in ultrasonic cleaning machine ultrasonic disperse
36min increases the distributing homogeneity of graphene oxide, takes out sponge, is washed with deionized, is put into 88 DEG C of oven dryings；Oxygen
Graphite alkene alcohol suspension, hydrazine hydrate mass ratio be 200:3；
(6) dimethyl silicone polymer is added in n-hexane, ultrasonic disperse is uniform, obtains dimethyl silicone polymer/just
Hexane solution；Dimethyl silicone polymer, n-hexane mass ratio be 2:90；
(7) sponge for drying step 5 is immersed in dimethyl silicone polymer/hexane solution that step 6 obtains, dipping
3h is reacted, the residual liquid in sponge gap is extracted, is placed in after 90 DEG C of oven dryings to get the graphene separated to high efficiency oil-water
Sponge.
Embodiment 4
A kind of preparation method of the graphene sponge of high efficiency oil-water separation, includes the following steps:
(1) polyurethane sponge is placed in ethyl alcohol and cleans 28min, be placed in a vacuum drying oven drying, obtain clean gather
Urethane sponge；
(2) preparation of graphene oxide: flaky graphite is added in the mixture of sodium nitrate and the concentrated sulfuric acid, in ice bath
Under the conditions of uniform magnetic agitation；Potassium permanganate is slowly added in mixed solution, control mixed solution temperature is lower than 20 DEG C and magnetic
Power stirs 1-3h, and it is 35-45 DEG C and magnetic agitation 1-2h that mixed solution temperature is then controlled under condition of ice bath；It is molten to mixing again
It is 70 DEG C of deionized waters that temperature is added in liquid, obtains bright orange color contamination liquid after being eventually adding the hydrogen peroxide that mass fraction concentration is 30%
Solution obtains graphene oxide after being 6-7 with deionized water centrifuge washing to pH；Flaky graphite, sodium nitrate, the concentrated sulfuric acid, height
The mass ratio for the hydrogen peroxide that potassium manganate, 70 DEG C of deionized waters, mass fraction concentration are 30% is 4:5:160:3:180:3；
(3) graphene oxide for obtaining step 2 is added in ethyl alcohol, ultrasonic disperse 2h, obtains graphene oxide dispersion
Liquid；Graphene oxide, ethyl alcohol mass ratio be 4:130；
(4) γ-glycidyl ether oxygen propyl trimethoxy silicane is add to deionized water, adjusts the pH value of the solution
It is 4, stirring hydrolysis 48min is then slowly added in the graphene oxide dispersion that step 3 obtains, 60 DEG C of reaction 4h, is centrifuged
Separation, with ethanol washing, at 80 DEG C it is dry for 24 hours, then ground, redisperse is configured into ethanol solution after grinding
2mg/ml graphene oxide alcohol suspension, remain using；γ-glycidyl ether oxygen propyl trimethoxy silicane, deionized water
Mass ratio be 2:90；
(5) clean three that addition hydrazine hydrate and step 1 obtain into the graphene oxide alcohol suspension that step 4 obtains
Poly cyanamid sponge, is placed in microwave chemical reactor, and microwave heating reacts 57min, is subsequently placed in ultrasonic cleaning machine ultrasonic disperse
47min increases the distributing homogeneity of graphene oxide, takes out sponge, is washed with deionized, is put into 95 DEG C of oven dryings；Oxygen
Graphite alkene alcohol suspension, hydrazine hydrate mass ratio be 270:4；
(6) dimethyl silicone polymer is added in n-hexane, ultrasonic disperse is uniform, obtains dimethyl silicone polymer/just
Hexane solution；Dimethyl silicone polymer, n-hexane mass ratio be 4:170；
(7) sponge for drying step 5 is immersed in dimethyl silicone polymer/hexane solution that step 6 obtains, dipping
3h is reacted, the residual liquid in sponge gap is extracted, is placed in after 110 DEG C of oven dryings to get the graphite separated to high efficiency oil-water
Alkene sponge.
Claims (7)
1. a kind of preparation method of the graphene sponge of high efficiency oil-water separation, which comprises the steps of:
(1) polyurethane sponge is placed in ethyl alcohol and cleans 10-20min, be placed in a vacuum drying oven drying, obtain clean poly- ammonia
Ester sponge；
(2) preparation of graphene oxide: flaky graphite is added in the mixture of sodium nitrate and the concentrated sulfuric acid, in condition of ice bath
Uniform magnetic agitation down；Potassium permanganate is slowly added in mixed solution, control mixed solution temperature is lower than 20 DEG C and magnetic force stirs
1-3h is mixed, it is 35-45 DEG C and magnetic agitation 1-2h that mixed solution temperature is then controlled under condition of ice bath；Again into mixed solution
Addition temperature is 70 DEG C of deionized waters, and it is molten to obtain bright orange color contamination liquid after 30% hydrogen peroxide to be eventually adding mass fraction concentration
Liquid obtains graphene oxide after being 6-7 with deionized water centrifuge washing to pH；
(3) graphene oxide for obtaining step 2 is added in ethyl alcohol, and ultrasonic disperse 1-3h obtains graphene oxide dispersion；
(4) coupling agent is add to deionized water, the pH value for adjusting the solution is 3-5, then stirring hydrolysis 30-50min delays
Slowly it is added in the graphene oxide dispersion that step 3 obtains, 60 DEG C of reaction 4h, is centrifugated, with ethanol washing, done at 80 DEG C
Dry then to be ground for 24 hours, redisperse is configured to 2mg/ml graphene oxide alcohol suspension into ethanol solution after grinding,
Remain using；
(5) the clean melamine that addition hydrazine hydrate and step 1 obtain into the graphene oxide alcohol suspension that step 4 obtains
Amine sponge, is placed in microwave chemical reactor, and microwave heating reacts 30-60min, is subsequently placed in ultrasonic cleaning machine ultrasonic disperse 30-
50min increases the distributing homogeneity of graphene oxide, takes out sponge, is washed with deionized, and it is dry to be put into 80-100 DEG C of baking oven
It is dry；
(6) dimethyl silicone polymer is added in n-hexane, ultrasonic disperse is uniform, obtains dimethyl silicone polymer/n-hexane
Solution；
(7) sponge for drying step 5 is immersed in dimethyl silicone polymer/hexane solution that step 6 obtains, impregnation
2-4h extracts the residual liquid in sponge gap, is placed in after 80-120 DEG C of oven drying to get the graphite separated to high efficiency oil-water
Alkene sponge.
2. a kind of preparation method of the graphene sponge of high efficiency oil-water separation according to claim 1, which is characterized in that step
In rapid 2, flaky graphite, sodium nitrate, the concentrated sulfuric acid, potassium permanganate, 70 DEG C of deionized waters, the dioxygen that mass fraction concentration is 30%
The mass ratio of water is 1-5:3-6:100-180:1-4:150-200:1-4.
3. a kind of preparation method of the graphene sponge of high efficiency oil-water separation according to claim 1, which is characterized in that step
In rapid 3, graphene oxide, ethyl alcohol mass ratio be 1-5:50-150.
4. a kind of preparation method of the graphene sponge of high efficiency oil-water separation according to claim 1, which is characterized in that step
In rapid 4, coupling agent, deionized water mass ratio be 1-3:50-100.
5. a kind of preparation method of the graphene sponge of high efficiency oil-water separation according to claim 1, which is characterized in that step
In rapid 4, coupling agent is γ-glycidyl ether oxygen propyl trimethoxy silicane.
6. a kind of preparation method of the graphene sponge of high efficiency oil-water separation according to claim 1, which is characterized in that step
In rapid 5, graphene oxide alcohol suspension, hydrazine hydrate mass ratio be 80-300:1-5.
7. a kind of preparation method of the graphene sponge of high efficiency oil-water separation according to claim 1, which is characterized in that step
In rapid 6, dimethyl silicone polymer, n-hexane mass ratio be 1-5:50-200.
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| CN111974365A (en) * | 2020-08-31 | 2020-11-24 | 湖北大学 | Preparation method of multifunctional super-hydrophobic conductive sponge for emulsion separation |
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| CN115448535A (en) * | 2021-10-08 | 2022-12-09 | 江苏一环集团有限公司 | Water purification method of integrated water purification device |
| CN117986877A (en) * | 2024-03-07 | 2024-05-07 | 上海天净新材料科技股份有限公司 | Fouling-free material based on lotus leaf bionics and preparation method thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104324524A (en) * | 2014-11-21 | 2015-02-04 | 中国科学院新疆理化技术研究所 | Preparation method of super-hydrophobic, super-oleophylic and ultralight sponge |
| CN104338519A (en) * | 2014-09-17 | 2015-02-11 | 上海大学 | Modified graphene-loaded polyurethane sponge and preparation method thereof |
| CN106084276A (en) * | 2016-06-13 | 2016-11-09 | 东南大学 | A kind of synthetic method of Graphene polydimethylsiloxane function sponge |
| WO2017015648A1 (en) * | 2015-07-23 | 2017-01-26 | Ozkan Cengiz S | Magnetic hydrophobic porous graphene sponge for environmental and biological/medical applications |
| CN108997608A (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 |
-
2019
- 2019-02-18 CN CN201910119914.2A patent/CN109608688A/en not_active Withdrawn
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104338519A (en) * | 2014-09-17 | 2015-02-11 | 上海大学 | Modified graphene-loaded polyurethane sponge and preparation method thereof |
| CN104324524A (en) * | 2014-11-21 | 2015-02-04 | 中国科学院新疆理化技术研究所 | Preparation method of super-hydrophobic, super-oleophylic and ultralight sponge |
| WO2017015648A1 (en) * | 2015-07-23 | 2017-01-26 | Ozkan Cengiz S | Magnetic hydrophobic porous graphene sponge for environmental and biological/medical applications |
| CN106084276A (en) * | 2016-06-13 | 2016-11-09 | 东南大学 | A kind of synthetic method of Graphene polydimethylsiloxane function sponge |
| CN108997608A (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 |
Non-Patent Citations (1)
| Title |
|---|
| 杜国勇等: "石墨烯复合改性海绵的制备及其吸油性能", 《环境工程学报》 * |
Cited By (13)
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|---|---|---|---|---|
| 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 |
| CN111302467A (en) * | 2020-04-08 | 2020-06-19 | 刘水平 | Flocculant capable of recovering dye, preparation method and application thereof |
| CN111302467B (en) * | 2020-04-08 | 2020-12-01 | 湖州达立智能设备制造有限公司 | Flocculant capable of recovering dye, preparation method and application thereof |
| CN111974365A (en) * | 2020-08-31 | 2020-11-24 | 湖北大学 | Preparation method of multifunctional super-hydrophobic conductive sponge for emulsion separation |
| CN113150369A (en) * | 2021-03-05 | 2021-07-23 | 福建省蓝深环保技术股份有限公司 | Preparation method of graphene oxide modification-based oil absorption sponge |
| CN115490394B (en) * | 2021-10-08 | 2023-06-16 | 江苏一环集团有限公司 | Water purifying device with low energy consumption |
| CN115448535A (en) * | 2021-10-08 | 2022-12-09 | 江苏一环集团有限公司 | Water purification method of integrated water purification device |
| CN115490394A (en) * | 2021-10-08 | 2022-12-20 | 江苏一环集团有限公司 | Water purification device of low energy consumption |
| CN115448535B (en) * | 2021-10-08 | 2023-06-20 | 江苏一环集团有限公司 | Water purifying method of integrated water purifying device |
| CN114656659A (en) * | 2022-04-20 | 2022-06-24 | 常州大学 | Polydimethylsiloxane/graphene oxide modified polyurethane and preparation method thereof |
| CN114907698A (en) * | 2022-07-01 | 2022-08-16 | 深圳清华大学研究院 | Modified graphene oxide heat-conducting silicone grease and preparation method thereof |
| CN114907698B (en) * | 2022-07-01 | 2023-08-15 | 深圳清华大学研究院 | Modified graphene oxide heat-conducting silicone grease and preparation method thereof |
| CN117986877A (en) * | 2024-03-07 | 2024-05-07 | 上海天净新材料科技股份有限公司 | Fouling-free material based on lotus leaf bionics and preparation method thereof |
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