CN108212083A - A kind of oil suction carbon sponge and preparation method thereof - Google Patents
A kind of oil suction carbon sponge and preparation method thereof Download PDFInfo
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- CN108212083A CN108212083A CN201711458354.0A CN201711458354A CN108212083A CN 108212083 A CN108212083 A CN 108212083A CN 201711458354 A CN201711458354 A CN 201711458354A CN 108212083 A CN108212083 A CN 108212083A
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- sponge
- graphene
- graphene oxide
- melamine
- oil suction
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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
-
- 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
-
- 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
- B01J20/205—Carbon nanostructures, e.g. nanotubes, nanohorns, nanocones, nanoballs
-
- 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
-
- 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
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/32—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating
- B01J20/3231—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating characterised by the coating or impregnating layer
- B01J20/3234—Inorganic material layers
- B01J20/324—Inorganic material layers containing free carbon, e.g. activated carbon
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/36—After-treatment
- C08J9/365—Coating
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K3/00—Materials not provided for elsewhere
- C09K3/32—Materials not provided for elsewhere for absorbing liquids to remove pollution, e.g. oil, gasoline, fat
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2361/00—Characterised by the use of condensation polymers of aldehydes or ketones; Derivatives of such polymers
- C08J2361/20—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen
- C08J2361/26—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes with heterocyclic compounds
- C08J2361/28—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes with heterocyclic compounds with melamine
Abstract
The present invention provides a kind of oil suction carbon sponge and preparation method thereof, and this method includes:Sponge is put into the graphene oxide of known concentration, ultrasonic disperse, obtains the melamine sponge of graphene oxide cladding;The melamine sponge of graphene oxide cladding is freeze-dried;The freeze-drying includes:Subzero 70 DEG C, the melamine sponge that graphene oxide coats all is frozen into ice, is put it under the vacuum condition of 1pa later, is dried in vacuo 36~72h;The calcining for carrying out 1 5h under reducing atmosphere at 150~400 DEG C obtains graphene-based carbon sponge.The present invention obtains super-hydrophobic graphene-based carbon sponge using graphene oxide modification melamine carbon sponge, the dosage of graphene oxide is not only reduced so as to reduce production cost, it is and simple for process, obtained graphene carbon sponge more effectively combines the advantages of graphene and three-dimensional macro business sponge, there is better absorption property, excellent mechanical performance and superior hydrophobic property.
Description
Technical field
The present invention relates to field of material technology more particularly to a kind of oil suction carbon sponge and preparation method thereof.
Background technology
The exploitation and utilization of oil, industrial production and sanitary waste all inevitably bring water environment a series of tight
The pollution problem of weight, water pollution etc. as caused by crude oil leakage leads to water pollution, industrial waste oil and organic solvent.Numerous
In water pollution, Crude Oil at Sea leakage is that current harm is maximum, degree is most deep, administers one of pollution being most difficult to, this is because marine
Crude oil leakage can not only directly affect the marine eco-environment, and can involve eventually terrestrial environment for the survival of mankind and itself
Safety.The processing key of leaked offshore oil is the promptness handled, extensive property, high efficiency and recycling property.It compares
Compared with for, physical absorption not only can fast and effeciently adsorb grease, grease can also be recycled, and do not cause two
Secondary pollution has become one of Main way of the area research at present.Therefore, research and development are with high efficiency of additive capability, simple for process
Oil absorption material become and solve the problems, such as the key of marine oil spill and aqueous pollution remediation problem.
Graphene aerogel have ultralight density, the specific surface area of superelevation, good mechanical strength, hydrophobic oleophilic oil and
Good electric conductivity, therefore extensive concern and the research in the world are caused in recent years.But simple graphene aerogel application
In water remediation, but its shortcoming but also it is very prominent, not only of high cost, poor toughness, utilization ratio be not high because its shape hold
Easy destroyed, difficult reuse.How the good characteristic of graphene is utilized, and overcome its own expensive and cyclicity difference
Problem.
Invention content
It is an object of the invention to solve the problems of the above-mentioned prior art, provide that a kind of production cost is low, Er Qiegong
The graphene-based carbon sponge sorbing material of simple super-hydrophobic, the efficient oil suction of skill.In addition to this, due to graphene-based carbon sponge certainly
The specific surface area of height and abundant gap structure, graphene-based carbon sponge also have the applications such as adsorbed gas.
A kind of preparation method of oil suction carbon sponge, includes the following steps:
(1) sponge is put into the graphene oxide of known concentration, ultrasonic disperse, obtains the trimerization of graphene oxide cladding
Cyanamide sponge;
(2) the melamine sponge of graphene oxide cladding is freeze-dried;The freeze-drying includes:Subzero 70
DEG C, the melamine sponge that graphene oxide coats all is frozen into ice, is put it under the vacuum condition of 1pa later, very
Dry 36~the 72h of sky;
(3) calcining for carrying out 1-5h under reducing atmosphere at 150~400 DEG C obtains graphene-based oil suction carbon sponge.
Further, method as described above, in step (1), the concentration of the graphene oxide dispersion is configured to
0.5~5mg mL-1。
Further, method as described above, in step (1), the supersonic frequency during condition of the ultrasonic disperse:
59kHz;Temperature:Room temperature.
Further, method as described above, before step (1), further include the step of being cleaned to sponge and
Sponge after cleaning is cleaned by ultrasonic with ethanol solution, the step of drying.
The oil suction carbon sponge being prepared according to as above either method.
The present invention obtains oil suction carbon sponge using graphene oxide modification melamine sponge, not only reduces graphite oxide
The dosage of alkene is and simple for process so as to reduce production cost, and obtained graphene carbon sponge more effectively combines graphene
The advantages of with three-dimensional macro business sponge, there are better absorption property, excellent mechanical performance and superior hydrophobic property.
Different according to the density of adsorbate to the absorption multiple of the organic matters such as n-hexane, chloroform, toluene and pumping fluid, adsorbance exists
80-165 times;Itself original shape still can be restored to after repeatedly squeezing;It and can be static and agitation
Selection absorption grease, realizes efficient, quick water-oil separating in oil water mixture.Towards the efficient, inexpensive of solution sea pollution
Oil absorption material, it will as solve this world-class problem key.This is applied to graphene-based sorbing material practical
Water-oil separating and water remediation are extremely important in life, and advocate energy-saving and environment-friendly big policy energetically in country
Under, there is also the extremely wide market spaces for this.
Description of the drawings
Fig. 1 is the SEM electron microscopes of oil suction carbon sponge prepared by the embodiment of the present invention, and the illustration in SEM figures is system of the present invention
For the pictorial diagram gone out;
Fig. 2 is the SEM electron microscopes that the embodiment of the present invention prepares graphene-based oil suction carbon sponge silk floss skeleton;
Fig. 3 is the hydrophobic angle figure of graphene-based oil suction carbon sponge prepared by the embodiment of the present invention;
Fig. 4 is the extruding figure of graphene-based oil suction carbon sponge prepared by the embodiment of the present invention;
Fig. 5 is the absorption figure of graphene-based oil suction carbon sponge absorption organic matter prepared by the embodiment of the present invention;
Fig. 6 is the absorption figure of the circulation absorption experiment of graphene-based oil suction carbon sponge prepared by present example;
Fig. 7 is the graphene-based oil suction carbon sponge of preparation of the embodiment of the present invention at (a in figure) without mixing and has stirring (in figure
B) efficient, the figure that continuously adsorbs in the case of.
Specific embodiment
To make the object, technical solutions and advantages of the present invention clearer, the technical solution below in the present invention carries out clear
Chu is fully described by, it is clear that described embodiment is part of the embodiment of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, those of ordinary skill in the art are obtained every other without creative efforts
Embodiment shall fall within the protection scope of the present invention.
Embodiment:
Commercialization sponge, that is, melamine sponge is cut into suitable size first, is then cleaned by ultrasonic trimerization with ultra-pure water
Cyanamide sponge 3~5 times;
Specifically, the purpose of ultrasonic cleaning is to wash off the dust and impurity of commercialization sponge surface, allows graphene oxide more
Good is supported on sponge;
It is cleaned by ultrasonic with ethanol solution, is dried;
Specifically, it is with the purpose that ethyl alcohol cleans:
(1) in order to dissolve the impurity of some organics;
(2) for sponge after the washing, water is replaced with alcohol solvent, sponge is made to dry faster.
The concentration of graphene oxide is transferred to OK range:0.5~5mg mL-1;
The sponge of drying is put into the graphene oxide of known concentration, ultrasonic disperse (supersonic frequency:59kHz;Temperature:
Room temperature;Time:Half an hour), obtain the melamine sponge of graphene oxide cladding;
The melamine sponge of graphene oxide cladding in lyophilized preparation is freeze-dried later, sample is put
Enter to subzero 70 DEG C, (pre-coo time is adjusted according to the size of sponge, until sample is all frozen within 2~5 hours for precooling
Ice), sample is put under vacuum condition (1pa) later, 36~72h is dried in vacuo, so as to obtain graphene oxide/melamine
Sponge.
Specifically, this step is the microcellular structure in order to keep sponge and graphene oxide, the compactness of connection and sponge
Flexibility.If without freeze-drying, if the method with 60 ° of drying, the shape of sponge can find to change, sponge meeting
It is hardened, graphene oxide and sponge cannot closely, uniformly combine.
High temperature cabonization is carried out to graphene oxide/melamine sponge:Under reducing atmosphere 1-5h is carried out at 150~400 DEG C
Calcining obtain graphene-based carbon sponge.
The present invention is waved the moisture in the melamine sponge impregnated of graphene oxide using the method for freeze-drying
Hair obtains the melamine sponge of dry graphene oxide cladding, graphene oxide is made closely to be coated on melamine bone
On frame, and the toughness of melamine sponge and the integrality of structure are remain, be sufficiently reserved the characteristic of each material.It avoids
In baking oven drying course, to the destruction impregnated of graphene oxide melamine sponge structure.
Fig. 1 is the SEM electron microscopes of graphene-based oil suction carbon sponge manufactured in the present embodiment, and the illustration in SEM figures is this hair
The bright pictorial diagram prepared, Fig. 2 are the SEM electron microscopes of graphene-based oil suction carbon sponge skeleton prepared by the embodiment of the present invention, from
Graphene has been loaded on the skeleton of it can be seen from the figure that sponge;Fig. 3 is graphene-based oil suction carbon sea prepared by the embodiment of the present invention
Continuous hydrophobic angle figure, wherein contact angle are up to 153 °, are demonstrated by the super-hydrophobicity of graphene-based carbon sponge.Fig. 4 is real for the present invention
The extruding figure of the graphene-based oil suction carbon sponge of example preparation is applied, it can be seen from the figure that graphene-based sponge after pressing may be used
With the shape before restoring completely;The absorption of graphene-based oil suction carbon sponge absorption organic matter prepared by Fig. 5 embodiment of the present invention
Figure;Fig. 6 is the absorption figure of the circulation absorption experiment of graphene-based oil suction carbon sponge prepared by present example;Fig. 7 is the present invention
The graphene-based oil suction carbon sponge prepared is in efficient, the figure that continuously adsorbs without mixing and in the case of having stirring.From Fig. 6, Fig. 7
In as can be seen that using the method for the present invention prepare graphene-based oil suction carbon sponge have good mechanical performance, cycle characteristics,
The characteristic of super-hydrophobic and efficient oil suction.
Finally it should be noted that:The above embodiments are merely illustrative of the technical solutions of the present invention, rather than its limitations;Although
The present invention is described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that:It still may be used
To modify to the technical solution recorded in foregoing embodiments or carry out equivalent replacement to which part technical characteristic;
And these modification or replace, various embodiments of the present invention technical solution that it does not separate the essence of the corresponding technical solution spirit and
Range.
Claims (5)
1. a kind of preparation method of oil suction carbon sponge, which is characterized in that include the following steps:
(1) sponge is put into the graphene oxide of known concentration, ultrasonic disperse, obtains the melamine of graphene oxide cladding
Sponge;
(2) the melamine sponge of graphene oxide cladding is freeze-dried;The freeze-drying includes:Subzero 70 DEG C,
The melamine sponge that graphene oxide coats all is frozen into ice, is put it under the vacuum condition of 1pa later, vacuum is done
Dry 36~72h;
(3) calcining for carrying out 1-5h under reducing atmosphere at 150~400 DEG C obtains graphene-based oil suction carbon sponge.
2. according to the method described in claim 1, it is characterized in that, in step (1), the graphene oxide dispersion it is dense
Degree is configured to 0.5~5mg mL-1。
3. according to the method described in claim 1, it is characterized in that, in step (1), the ultrasound during condition of the ultrasonic disperse
Frequency:59kHz;Temperature:Room temperature.
4. according to the method described in claim 1, it is characterized in that, before step (1), further include what sponge was cleaned
Step and the sponge after cleaning is cleaned by ultrasonic with ethanol solution, the step of drying.
5. the oil suction carbon sponge being prepared according to claim 1-4 either method.
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Cited By (9)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
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 |
CN110124629A (en) * | 2019-04-08 | 2019-08-16 | 华南师范大学 | A kind of melamine sponge-graphene oxide adsorbent material and its preparation method and application |
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 |
CN111229168A (en) * | 2020-02-14 | 2020-06-05 | 上海第二工业大学 | Method for recovering high-viscosity leaked crude oil by using graphene-based material |
CN113072677A (en) * | 2021-03-26 | 2021-07-06 | 西南石油大学 | Composite polyurethane foam emulsion separation material, preparation method and application thereof |
CN113667291A (en) * | 2021-08-23 | 2021-11-19 | 华南理工大学 | Super-hydrophobic material, preparation method thereof and sensor |
CN113736133A (en) * | 2021-09-24 | 2021-12-03 | 北京美斯顿科技开发有限公司 | Graphene-based sponge and preparation method and application thereof |
CN114832781A (en) * | 2022-04-28 | 2022-08-02 | 西南石油大学 | Super-hydrophobic/super-oleophylic sponge oil-water separation material and preparation method 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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Cited By (12)
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CN110124629A (en) * | 2019-04-08 | 2019-08-16 | 华南师范大学 | A kind of melamine sponge-graphene oxide adsorbent material and its preparation method and application |
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 |
CN111229168A (en) * | 2020-02-14 | 2020-06-05 | 上海第二工业大学 | Method for recovering high-viscosity leaked crude oil by using graphene-based material |
CN113072677A (en) * | 2021-03-26 | 2021-07-06 | 西南石油大学 | Composite polyurethane foam emulsion separation material, preparation method and application thereof |
CN113072677B (en) * | 2021-03-26 | 2022-03-01 | 西南石油大学 | Composite polyurethane foam emulsion separation material, preparation method and application thereof |
CN113667291A (en) * | 2021-08-23 | 2021-11-19 | 华南理工大学 | Super-hydrophobic material, preparation method thereof and sensor |
CN113667291B (en) * | 2021-08-23 | 2022-08-12 | 华南理工大学 | Super-hydrophobic material, preparation method thereof and sensor |
CN113736133A (en) * | 2021-09-24 | 2021-12-03 | 北京美斯顿科技开发有限公司 | Graphene-based sponge and preparation method and application thereof |
CN114832781A (en) * | 2022-04-28 | 2022-08-02 | 西南石油大学 | Super-hydrophobic/super-oleophylic sponge oil-water separation material and preparation method thereof |
CN114832781B (en) * | 2022-04-28 | 2023-06-06 | 西南石油大学 | Super-hydrophobic/super-oleophylic sponge oil-water separation material and preparation method 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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