CN108722347A - A kind of preparation of graphene oil suction sponge - Google Patents
A kind of preparation of graphene oil suction sponge Download PDFInfo
- Publication number
- CN108722347A CN108722347A CN201710263799.7A CN201710263799A CN108722347A CN 108722347 A CN108722347 A CN 108722347A CN 201710263799 A CN201710263799 A CN 201710263799A CN 108722347 A CN108722347 A CN 108722347A
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- graphene
- sponge
- oil suction
- graphene oxide
- oil
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- 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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- B—PERFORMING OPERATIONS; TRANSPORTING
- 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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- 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
- B01J20/28—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
- B01J20/28042—Shaped bodies; Monolithic structures
- B01J20/28045—Honeycomb or cellular structures; Solid foams or sponges
Abstract
The invention discloses a kind of preparations of graphene oil suction sponge, include the following steps：1) graphene oxide powder is added to the water, ultrasonic disperse obtains graphene oxide water solution；2) a certain amount of gamma-aminopropyl-triethoxy-silane, gamma-methyl allyl acyloxypropyl trimethoxysilane, boron nitride, butyl titanate oleyl amine, 3-mercaptopropyi trimethoxy silane modifying agent is added, after stirring, 80~100 DEG C are warming up to, graft modification is carried out to graphene oxide；3) polyurethane sponge, melamine sponge are impregnated in graphene oxide solution after modification；4) sponge being soaked for a period of time is pulled out, and is dried to get to graphene oil suction sponge at 100~200 DEG C.Graphene oil suction sponge prepared by the present invention has an oil suction and does not absorb water, and oil absorption is up to hundreds times of dead weight, the recyclable absorption oil product by way of simply squeezing.Graphene oil suction sponge prepared by the present invention has at low cost, easy to operate, the good feature of reusability.It is had potential application in fields such as the removing of water body oil pollutant, oil exploitation, industrial oil pollutant separation.
Description
Technical field
The present invention relates to technical fields prepared by oil suction sponge, are related specifically to a kind of system of graphene oil suction sponge
It is standby.
Background technology
Since 20th century, with the prosperity in international trade market, sea transport industry has obtained significant progress, is sent out in economy
While exhibition, marine oil overflow pollution is also more serious, and the extensive oil spill accident caused by the contingency of marine ships is repeatly
See not fresh.Oil, which enters sea, can absorb dissolved oxygen of seawater, lead to seawater anoxic, and marine organisms are dead, serious to destroy sea
The foreign ecological balance.Currently, marine eco-environment crisis has been put into 21 examination century, ten overall situation crisis, marine pollution matter is solved
It is very urgent.
Currently used oil slick processing method such as physical treatment process, using the oil fence, spiral vortex type sea cleaner etc.,
Project scale is great, of high cost.And method of chemical treatment uses sprinkling dispersant, detergent and other surfaces activating agent etc. by sea
Oil slick is dispersed into atomic small particle, so that it is emulsified in the seawater, disperse, dissolving or being deposited to seabed, and can draw in the seawater
Enter other pollutants.
Graphene has large specific surface area, has the characteristics that excellent absorption property, modified to have oleophilic drainage performance,
It is carried on sponge again, obtains graphene oil suction sponge, can conveniently and efficiently absorb and swim in the oil on sea, and drop significantly
Low cost.However the method for most of preparation oil suction sponges is cumbersome at present, reuse rate is low.Such as patent
A kind of 201310027624.8 methods preparing hydrophobic graphene sponge, by graphene oxide in water ultrasonic disperse, freeze-drying,
Then calcination obtains the graphene sponge with the super oleophylic of super-hydrophobic to high-temperature process in flame again.Graphene sea prepared by the method
Silk floss has low-down density by raw material of graphene oxide, but preparation process is complicated, and oil absorption is limited and cannot reuse.
Invention content
The purpose of the present invention is to provide a kind of preparation of graphene oil suction sponge, with the suctions such as conventional adsorbent such as activated carbon
Attached greasy dirt is compared, adsorption efficiency higher, and service life cycle is longer.
For this purpose, the present invention uses following technical scheme：
A kind of preparation of graphene oil suction sponge, includes the following steps：
1) graphene oxide powder is added to the water, ultrasonic disperse obtains graphene oxide water solution；
2) modifying agent is added in graphene oxide water solution, is heated after stirring, graft modification is carried out to graphene oxide；
3) sponge is impregnated in graphene oxide solution after modification；
4) sponge being immersed in graphene oxide solution is pulled out, high temperature reduction drying.
Preferably, the graphene oxide is the product that the oxidized stripping of graphite obtains；The side of the graphite oxidation stripping
Formula is one kind in Hummers methods, Brodie methods or Staudenmaier methods.
Preferably, the modifying agent is gamma-aminopropyl-triethoxy-silane, gamma-methyl allyl acyloxypropyl trimethoxy
One or more of silane, boron nitride, butyl titanate oleyl amine, 3-mercaptopropyi trimethoxy silane, wherein graphite oxide
The mass ratio of alkene and modifying agent is 0.1~10.
Preferably, the heating temperature is 80~100 DEG C, and heating time is 0.5~4h.
Preferably, the sponge is one kind in porosity polyurethane sponge or melamine sponge.
Preferably, the sponge size is 0.1 × 0.1 × 0.1cm~1 × 1 × 1m, such as 0.5 × 0.5 × 0.5cm, 0.6
× 0.2 × 0.1cm, 0.9 × 0.9 × 1cm.
Preferably, the soaking time is 0.5~20h.
Preferably, the drying temperature is 100~200 DEG C, and the time is 2~20h.
Preferably, the graphene oil suction sponge oil suction type is light oil, heavy oil, crude oil.
The present invention uses above technical scheme, using gamma-aminopropyl-triethoxy-silane, gamma-methyl allyl acyloxypropyl
Trimethoxy silane, boron nitride, butyl titanate, oleyl amine, 3-mercaptopropyi trimethoxy silane modifying agent are to graphene oxide
It is modified grafting, increases the contact area of graphene oxide and sponge and the adhesive force on sponge, while adding dry
Graphene oxide is reduced into graphene in the process of heat, and making it, only oil suction does not absorb water, and oil absorption passes through letter up to hundreds times of dead weight
The recyclable absorption oil product of mode singly squeezed.Graphene oil suction sponge prepared by the present invention has at low cost, easy to operate, repetition
The good feature of usability.Have in fields such as the removing of water body oil pollutant, oil exploitation, industrial oil pollutant separation potential
Application value.
Specific implementation mode
In order to keep objects, features and advantages of the present invention more clear, following embodiment, the specific implementation to the present invention
Mode makes more detailed description, in the following description, elaborates many concrete details in order to adequately understand this
Invention, but the present invention can be implemented with being much different from the other modes of description.Therefore, the present invention is not by following discloses
The limitation of specific implementation.
A kind of preparation of graphene oil suction sponge, includes the following steps：
1) graphene oxide powder is added to the water, ultrasonic disperse obtains graphene oxide water solution；
2) modifying agent is added in graphene oxide water solution, is heated after stirring, graft modification is carried out to graphene oxide；
3) sponge is impregnated in graphene oxide solution after modification；
4) sponge being immersed in graphene oxide solution is pulled out, high temperature reduction drying.
Wherein, the graphene oxide is the product that the oxidized stripping of graphite obtains；The mode of the graphite oxidation stripping
For one kind in Hummers methods, Brodie methods or Staudenmaier methods.
Wherein, the modifying agent is gamma-aminopropyl-triethoxy-silane, gamma-methyl allyl acyloxypropyl trimethoxy silicon
One or more of alkane, boron nitride, butyl titanate oleyl amine, 3-mercaptopropyi trimethoxy silane, wherein graphene oxide
Mass ratio with modifying agent is 0.1~10.
Wherein, the heating temperature is 80~100 DEG C, and heating time is 0.5~4h.
Wherein, the sponge is one kind in porosity polyurethane sponge or melamine sponge.
Wherein, the sponge size is 0.1 × 0.1 × 0.1cm~1 × 1 × 1m, such as 0.5 × 0.5 × 0.5cm, 0.6 ×
0.2 × 0.1cm, 0.9 × 0.9 × 1cm.
Wherein, the soaking time is 0.5~20h.
Wherein, the drying temperature is 100~200 DEG C, and the time is 2~20h.
Embodiment one
A kind of preparation of graphene oil suction sponge, includes the following steps：
1) 1g graphene oxide powders are added in 100 water, ultrasonic disperse 1h obtains graphene oxide water solution；
2) boron nitride 0.5g, gamma-methyl allyl acyloxypropyl front three are added in scattered graphene oxide water solution
Oxysilane 2ml is sufficiently mixed uniformly, and 90 DEG C of heating reaction 2h obtain modified graphene oxide mixed solution；
3) the melamine sponge of 5 × 5 × 1cm is immersed in graphene oxide mixed solution 3h, graphene oxide is made to fill
Divide and be adsorbed on sponge, obtains graphene oxide sponge；
4) by the graphene oxide sponge as in baking oven, 120 DEG C of high temperature reduction 5h, graphene oxide is reduced into graphite
Alkene obtains graphene sponge.
Experiment measures CA=172 ° of the contact angle of graphene sponge and water, roll angle=13 °, oil absorption 88mg/mg, weight
Relapse oil 60 times after, oil absorption 68mg/mg.
Embodiment two
1) 0.5g graphene oxide powders are added in 100 water, it is water-soluble to obtain graphene oxide by ultrasonic disperse 0.5h
Liquid；
2) boron nitride 0.1g, 3-mercaptopropyi trimethoxy silane are added in scattered graphene oxide water solution
1ml is sufficiently mixed uniformly, and 90 DEG C of heating reaction 1h obtain modified graphene oxide mixed solution；
3) the melamine sponge of 3 × 5 × 0.5cm is soaked in graphene oxide mixed solution 3h, makes graphene oxide
It is fully adsorbed on sponge, obtains graphene oxide sponge；
4) by the graphene oxide sponge as in baking oven, 120 DEG C of high temperature reduction 10h, graphene oxide is reduced into stone
Black alkene, obtains graphene sponge.
Experiment measures CA=162 ° of the contact angle of graphene sponge and water, roll angle=12 °, oil absorption 78mg/mg, weight
Relapse oil 60 times after, oil absorption 61mg/mg.
Embodiment three
1) 2g graphene oxide powders are added in 500 water, ultrasonic disperse 2h obtains graphene oxide water solution；
2) boron nitride 0.2g, oleyl amine 0.5ml are added in scattered graphene oxide water solution, is sufficiently mixed uniformly,
120 DEG C of heating reaction 0.5h, obtain modified graphene oxide mixed solution；
3) the melamine sponge of 3 × 5 × 1cm is soaked in graphene oxide mixed solution 5h, graphene oxide is made to fill
Divide and be adsorbed on sponge, obtains graphene oxide sponge；
4) by the graphene oxide sponge as in baking oven, 120 DEG C of high temperature reduction 15h, graphene oxide is reduced into stone
Black alkene, obtains graphene sponge.
Experiment measures CA=170 ° of the contact angle of graphene sponge and water, roll angle=10 °, oil absorption 90mg/mg, weight
Relapse oil 60 times after, oil absorption 70mg/mg.
The graphene oil suction sponge prepared using method of the present invention has excellent hydrophobic performance and lipophile
Can, and can reuse, reduce cost.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
All any modification, equivalent and improvement etc., should all be included in the protection scope of the present invention made by within refreshing and principle.
Claims (9)
1. the invention discloses a kind of preparations of graphene oil suction sponge, which is characterized in that include the following steps：
1) graphene oxide powder is added to the water, ultrasonic disperse obtains graphene oxide water solution；
2) modifying agent is added in graphene oxide water solution, is heated after stirring, graft modification is carried out to graphene oxide；
3) sponge is impregnated in graphene oxide solution after modification；
4) sponge being immersed in graphene oxide solution is pulled out, high temperature reduction drying.
2. a kind of preparation of graphene oil suction sponge according to claim 1, which is characterized in that the graphene oxide is
Graphite is oxidized to remove obtained product；The mode of graphite oxidation stripping be Hummers methods, Brodie methods or
One kind in Staudenmaier methods.
3. a kind of preparation of graphene oil suction sponge according to claim 1, which is characterized in that the modifying agent is γ-
Aminopropyl triethoxysilane, gamma-methyl allyl acyloxypropyl trimethoxysilane, boron nitride, butyl titanate oleyl amine, 3- mercaptos
The mass ratio of one or more of base propyl trimethoxy silicane, wherein graphene oxide and modifying agent is 0.1~10.
4. a kind of preparation of graphene oil suction sponge according to claim 1, which is characterized in that the heating temperature is 80
~100 DEG C, heating time is 0.5~4h.
5. a kind of preparation of graphene oil suction sponge according to claim 1, which is characterized in that the sponge is porosity
One kind in polyurethane sponge or melamine sponge.
6. a kind of preparation of graphene oil suction sponge according to claim 1, which is characterized in that the sponge size is
0.1 × 0.1 × 0.1cm~1 × 1 × 1m.
7. a kind of preparation of graphene oil suction sponge according to claim 1, which is characterized in that the soaking time is
0.5~20h.
8. a kind of preparation of graphene oil suction sponge according to claim 1, which is characterized in that the drying temperature is
100~200 DEG C, the time is 2~20h.
9. a kind of preparation of graphene oil suction sponge according to claim 1, which is characterized in that the graphene oil suction sea
Continuous oil suction type is light oil, heavy oil, crude oil.
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| CN201710263799.7A CN108722347A (en) | 2017-04-21 | 2017-04-21 | A kind of preparation of graphene oil suction sponge |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109453562A (en) * | 2018-11-12 | 2019-03-12 | 天津市职业大学 | The preparation method of the renewable fiber-ball filter media of oily waste water treatment |
| 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 |
| 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 |
| CN110193357A (en) * | 2019-06-27 | 2019-09-03 | 中素新科技有限公司 | Composite sponge and its preparation method and application containing modified graphene |
| CN111215029A (en) * | 2020-01-21 | 2020-06-02 | 中国科学院上海硅酸盐研究所 | Graphene sponge capable of being directly baked at high temperature and reused, and preparation method and application thereof |
| CN114316186A (en) * | 2022-01-29 | 2022-04-12 | 中海油天津化工研究设计院有限公司 | Graphene oleophylic and hydrophobic material and preparation method thereof |
| WO2023080352A1 (en) * | 2021-11-03 | 2023-05-11 | 한남대학교 산학협력단 | Method for preparing oil absorbent using polyurethane sponge |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109453562A (en) * | 2018-11-12 | 2019-03-12 | 天津市职业大学 | The preparation method of the renewable fiber-ball filter media of oily waste water treatment |
| 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 |
| 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 |
| CN110193357A (en) * | 2019-06-27 | 2019-09-03 | 中素新科技有限公司 | Composite sponge and its preparation method and application containing modified graphene |
| CN111215029A (en) * | 2020-01-21 | 2020-06-02 | 中国科学院上海硅酸盐研究所 | Graphene sponge capable of being directly baked at high temperature and reused, and preparation method and application thereof |
| WO2023080352A1 (en) * | 2021-11-03 | 2023-05-11 | 한남대학교 산학협력단 | Method for preparing oil absorbent using polyurethane sponge |
| CN114316186A (en) * | 2022-01-29 | 2022-04-12 | 中海油天津化工研究设计院有限公司 | Graphene oleophylic and hydrophobic material and preparation method thereof |
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