CN110152619A - A kind of preparation method of graphene oil suction sponge - Google Patents
A kind of preparation method of graphene oil suction sponge Download PDFInfo
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- CN110152619A CN110152619A CN201810326711.6A CN201810326711A CN110152619A CN 110152619 A CN110152619 A CN 110152619A CN 201810326711 A CN201810326711 A CN 201810326711A CN 110152619 A CN110152619 A CN 110152619A
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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
- B01J20/02—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
- 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
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
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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
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/24—Naturally occurring macromolecular compounds, e.g. humic acids or their derivatives
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/285—Treatment of water, waste water, or sewage by sorption using synthetic organic sorbents
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/286—Treatment of water, waste water, or sewage by sorption using natural organic sorbents or derivatives thereof
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/40—Devices for separating or removing fatty or oily substances or similar floating material
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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
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/46—Materials comprising a mixture of inorganic and organic materials
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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
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4806—Sorbents characterised by the starting material used for their preparation the starting material being of inorganic character
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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
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character
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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
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character
- B01J2220/4825—Polysaccharides or cellulose materials, e.g. starch, chitin, sawdust, wood, straw, cotton
Abstract
The present invention relates to a kind of preparation methods of graphene oil suction sponge, including chitosan sponge is immersed in deionized water, it is cleaned by ultrasonic in Vltrasonic device, take out sponge, sponge is immersed in dehydrated alcohol again and continues to be cleaned by ultrasonic, it dries after cleaning, finally sponge is further processed using the method for plasma treatment；Sponge is immersed in graphene oxide suspension, ultrasonic disperse is uniformly adhered to graphene oxide on chitosan sponge；Gained sponge is taken out, is put into vacuum oven progress thermal reduction reaction after extracting residual liquid；Octadecyl trichlorosilane alkane is dissolved in organic solution, sponge is immersed in the organic solution containing octadecyl trichlorosilane alkane, by clean sponge heating, drying, obtains graphene oil suction sponge.A kind of preparation method of graphene oil suction sponge of the invention, resulting graphene oil suction sponge can even underwater quick adsorption oils and various organic solvents on the water, realize efficient water-oil separation.
Description
Technical field
The present invention relates to a kind of preparation methods of oil suction sponge, and in particular to a kind of preparation side of graphene oil suction sponge
Method.
Background technique
With the development that petroleum industry and offshore oil are transported, oils leakage becomes the big serious problems for influencing ecological environment,
Sufficiently to cause the attention of the public.The large area oil film being consequently formed can not only obstruct normal also gas exchange process, make gas
Time is abnormal, and also will affect the circulation of food chain, to destroy the ecological balance of ocean.Since oils leakage accident can not be kept away
Exempt from, therefore efficient processing is particularly important in time after the accident.It is main to the processing mode of oils leakage problem at present
Based on adsorption treatment.However there are many disadvantages for current oil absorption material, at high cost such as preparation process complexity, grease selection
Property is poor, and oil absorption capacity is low etc..
Summary of the invention
The purpose of the present invention is to provide a kind of preparation method of graphene oil suction sponge, resulting graphene oil suction sponge
Can even underwater quick adsorption oils and various organic solvents on the water, realize efficient water-oil separation, the graphene oil suction
It is sponge preparation method strong operability, low in cost.
A kind of preparation method of graphene oil suction sponge, includes the following steps to carry out:
(1) chitosan sponge is immersed in deionized water first, 2h is cleaned by ultrasonic in Vltrasonic device, sea is taken out after cleaning
Silk floss, then sponge is immersed in dehydrated alcohol and continues to be cleaned by ultrasonic 2h, it is dried after cleaning, finally uses the side of plasma treatment
Method is further processed sponge；
(2) sponge obtained by step (1) is immersed in graphene oxide suspension, ultrasonic disperse keeps graphene oxide equably attached
On chitosan sponge；
(3) sponge obtained by step (2) is taken out, is put into vacuum oven progress thermal reduction reaction after extracting residual liquid；
(4) octadecyl trichlorosilane alkane is dissolved in organic solution, the weight ratio of octadecyl trichlorosilane alkane and organic solution is
1:100~1000, by sponge obtained by step (3) at moisture state, the moisture content of sponge is 1~2%, by sponge be immersed in containing
In the organic solution of octadecyl trichlorosilane alkane, reaction temperature is controlled within the scope of 5~30 DEG C, and the reaction time is 3~40min,
It is taken out after reflection, cleans unreacted octadecyl trichlorosilane with organic solvent, by clean sponge heating, drying, drying
Temperature is 105~120 DEG C, obtains graphene oil suction sponge.
Specifically, the chitosan sponge is prepared under the conditions of liquid nitrogen, -10 ~ -50 DEG C using freeze-drying.
Specifically, graphene oxide suspension described in step (2) is prepared by improved Hummer ' s hair；Institute
The graphene oxide suspension concentration stated is 3 ~ 10mg/L.
Specifically, the ultrasonic disperse time described in step (2) is 30~60min, and supersonic frequency is 25~80kHz, is surpassed
Acoustical power is 50~200W.
Specifically, thermal reduction reaction temperature described in step (3) be 150 ~ 180 DEG C, the thermal reduction reaction time be 6 ~
10h, vacuum oven vacuum degree are 1600 ~ 2000pa.
Specifically, organic solvent described in step (4) is that toluene, cyclooctane, hexadecane, carbon tetrachloride etc. can dissolve ten
The solvent of eight alkyltrichlorosilanes.
The invention has the following advantages: a kind of preparation method of graphene oil suction sponge of the invention, resulting stone
Black alkene oil suction sponge can even underwater quick adsorption oils and various organic solvents on the water, realize efficient water-oil separation,
It is the graphene oil suction sponge preparation method strong operability, low in cost；It is acted on using " molecular bridge " of silane coupling agent, by stone
Black alkene is combined in the form of covalent bond with chitosan sponge skeleton, even if repeatedly extruding sponge, graphene film also can be steadily
It is adhered on sponge, it is not easily to fall off, therefore sponge still has stronger oil and water separation capability after being recycled repeatedly.
Specific embodiment
Embodiment 1
A kind of preparation method of graphene oil suction sponge, includes the following steps to carry out:
(1) chitosan sponge is immersed in deionized water first, 2h is cleaned by ultrasonic in Vltrasonic device, sea is taken out after cleaning
Silk floss, then sponge is immersed in dehydrated alcohol and continues to be cleaned by ultrasonic 2h, it is dried after cleaning, finally uses the side of plasma treatment
Method is further processed sponge；
(2) sponge obtained by step (1) is immersed in 3mg/L graphene oxide suspension, ultrasonic disperse 30min, supersonic frequency is
25kHz, ultrasonic power 50W, is uniformly adhered to graphene oxide on chitosan sponge；
(3) sponge obtained by step (2) is taken out, is put into 150 DEG C of vacuum ovens progress thermal reduction reactions after extracting residual liquid,
Vacuum degree is 1600pa, and the thermal reduction reaction time is 7h.
(4) octadecyl trichlorosilane alkane is dissolved in toluene solution, weight ratio 1:150, by sponge obtained by step (3) at
Moisture content is that 1% sponge is impregnated in the above solution, reacts 20min at being 20 DEG C in temperature, after taking-up immediately by moisture state
Cleaning repeatedly is carried out to without octadecyl trichlorosilane alkane with toluene solvant, is put it into and is dried 1h in baking oven under the conditions of 105 DEG C,
Obtain graphene oil suction sponge.
Embodiment 2
A kind of preparation method of graphene oil suction sponge, includes the following steps to carry out:
(1) chitosan sponge is immersed in deionized water first, 2h is cleaned by ultrasonic in Vltrasonic device, sea is taken out after cleaning
Silk floss, then sponge is immersed in dehydrated alcohol and continues to be cleaned by ultrasonic 2h, it is dried after cleaning, finally uses the side of plasma treatment
Method is further processed sponge；
(2) sponge obtained by step (1) is immersed in 10mg/L graphene oxide suspension, ultrasonic disperse 60min, supersonic frequency is
80kHz, ultrasonic power 200W, is uniformly adhered to graphene oxide on chitosan sponge；
(3) sponge obtained by step (2) is taken out, is put into 180 DEG C of vacuum ovens progress thermal reduction reactions after extracting residual liquid,
Vacuum degree is 2000pa, and the thermal reduction reaction time is 10h.
(4) octadecyl trichlorosilane alkane is dissolved in cyclooctane solution, weight ratio 1:200, by sponge obtained by step (3)
At moisture state, it is that 2% sponge is impregnated in the above solution by moisture content, reacts 20min at being 30 DEG C in temperature, stood after taking-up
Cleaning repeatedly is carried out to without octadecyl trichlorosilane alkane with cyclooctane solvent, is put it into baking oven and is done under the conditions of 120 DEG C
Dry 1h obtains graphene oil suction sponge.
Embodiment 3
A kind of preparation method of graphene oil suction sponge, includes the following steps to carry out:
(1) chitosan sponge is immersed in deionized water first, 2h is cleaned by ultrasonic in Vltrasonic device, sea is taken out after cleaning
Silk floss, then sponge is immersed in dehydrated alcohol and continues to be cleaned by ultrasonic 2h, it is dried after cleaning, finally uses the side of plasma treatment
Method is further processed sponge；
(2) sponge obtained by step (1) is immersed in 5mg/L graphene oxide suspension, ultrasonic disperse 40min, supersonic frequency is
35kHz, ultrasonic power 80W, is uniformly adhered to graphene oxide on chitosan sponge；
(3) sponge obtained by step (2) is taken out, is put into 160 DEG C of vacuum ovens progress thermal reduction reactions after extracting residual liquid,
Vacuum degree is 1800pa, and the thermal reduction reaction time is 6h.
(4) octadecyl trichlorosilane alkane is dissolved in hexadecane solution, weight ratio 1:100, by sponge obtained by step (3)
At moisture state, it is that 1% sponge is impregnated in the above solution by moisture content, reacts 25min at being 25 DEG C in temperature, stood after taking-up
Cleaning repeatedly is carried out to without octadecyl trichlorosilane alkane with hexadecane solvent, is put it into baking oven and is done under the conditions of 110 DEG C
Dry 1h obtains graphene oil suction sponge.
Embodiment 4
A kind of preparation method of graphene oil suction sponge, includes the following steps to carry out:
(1) chitosan sponge is immersed in deionized water first, 2h is cleaned by ultrasonic in Vltrasonic device, sea is taken out after cleaning
Silk floss, then sponge is immersed in dehydrated alcohol and continues to be cleaned by ultrasonic 2h, it is dried after cleaning, finally uses the side of plasma treatment
Method is further processed sponge；
(2) sponge obtained by step (1) is immersed in 8mg/L graphene oxide suspension, ultrasonic disperse 50min, supersonic frequency is
80kHz, ultrasonic power 180W, is uniformly adhered to graphene oxide on chitosan sponge；
(3) sponge obtained by step (2) is taken out, is put into 170 DEG C of vacuum ovens progress thermal reduction reactions after extracting residual liquid,
Vacuum degree is 1900pa, and the thermal reduction reaction time is 5h.
(4) octadecyl trichlorosilane alkane is dissolved in carbon tetrachloride solution, weight ratio 1:200, by sea obtained by step (3)
Moisture content is that 2% sponge is impregnated in the above solution, 30min is reacted at being 20 DEG C in temperature, after taking-up by silk floss at moisture state
Cleaning repeatedly is carried out to without octadecyl trichlorosilane alkane with carbon tetrachloride solvent immediately, puts it into 120 DEG C of conditions in baking oven
Lower dry 1h obtains graphene oil suction sponge.
Claims (6)
1. a kind of preparation method of graphene oil suction sponge, which is characterized in that include the following steps to carry out:
(1) chitosan sponge is immersed in deionized water first, 2h is cleaned by ultrasonic in Vltrasonic device, sea is taken out after cleaning
Silk floss, then sponge is immersed in dehydrated alcohol and continues to be cleaned by ultrasonic 2h, it is dried after cleaning, finally uses the side of plasma treatment
Method is further processed sponge；
(2) sponge obtained by step (1) is immersed in graphene oxide suspension, ultrasonic disperse keeps graphene oxide equably attached
On chitosan sponge；
(3) sponge obtained by step (2) is taken out, is put into vacuum oven progress thermal reduction reaction after extracting residual liquid；
(4) octadecyl trichlorosilane alkane is dissolved in organic solution, the weight ratio of octadecyl trichlorosilane alkane and organic solution is
1:100~1000, by sponge obtained by step (3) at moisture state, the moisture content of sponge is 1~2%, by sponge be immersed in containing
In the organic solution of octadecyl trichlorosilane alkane, reaction temperature is controlled within the scope of 5~30 DEG C, and the reaction time is 3~40min,
It is taken out after reflection, cleans unreacted octadecyl trichlorosilane with organic solvent, by clean sponge heating, drying, drying
Temperature is 105~120 DEG C, obtains graphene oil suction sponge.
2. the preparation method of graphene oil suction sponge according to claim 1, which is characterized in that the chitosan sponge is adopted
Prepared under the conditions of liquid nitrogen, -10~-50 DEG C with freeze-drying.
3. the preparation method of graphene oil suction sponge according to claim 1, which is characterized in that described in step (2)
Graphene oxide suspension is prepared by improved Hummer ' s hair；The graphene oxide suspension concentration be 3~
10mg/L。
4. the preparation method of graphene oil suction sponge according to claim 1, which is characterized in that described in step (2)
The ultrasonic disperse time is 30~60min, and supersonic frequency is 25~80kHz, and ultrasonic power is 50~200W.
5. the preparation method of graphene oil suction sponge according to claim 1, which is characterized in that described in step (3)
Thermal reduction reaction temperature be 150~180 DEG C, the thermal reduction reaction time be 6~10h, vacuum oven vacuum degree be 1600~
2000pa。
6. the preparation method of graphene oil suction sponge according to claim 1, which is characterized in that described in step (4)
Organic solvent is the solvent of the dissolvable octadecyl trichlorosilane alkanes such as toluene, cyclooctane, hexadecane, carbon tetrachloride.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810326711.6A CN110152619A (en) | 2018-04-12 | 2018-04-12 | A kind of preparation method of graphene oil suction sponge |
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| CN201810326711.6A CN110152619A (en) | 2018-04-12 | 2018-04-12 | A kind of preparation method of graphene oil suction sponge |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104629079A (en) * | 2014-12-05 | 2015-05-20 | 武汉工程大学 | Elastic superhydrophobic chitosan oil-absorption sponge as well as preparation method and application thereof |
| US20150194667A1 (en) * | 2014-01-08 | 2015-07-09 | Gordon Chiu | Hydrophobic and oleophilic sponge-like compositions |
| CN105694092A (en) * | 2016-02-01 | 2016-06-22 | 东南大学 | Preparation method of super-hydrophobic graphene sponge |
| CN106693444A (en) * | 2016-12-27 | 2017-05-24 | 西南石油大学 | Preparing method of reproducible super-hydrophobic graphite alkenyl oil absorption sponge |
| US20170182474A1 (en) * | 2015-12-28 | 2017-06-29 | Aruna Zhamu | Integral 3D graphene-carbon hybrid foam and devices containing same |
| CN107570127A (en) * | 2017-09-08 | 2018-01-12 | 浙江工业大学 | A kind of graphene-based water-oil separating foamed material and its preparation method and application |
-
2018
- 2018-04-12 CN CN201810326711.6A patent/CN110152619A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20150194667A1 (en) * | 2014-01-08 | 2015-07-09 | Gordon Chiu | Hydrophobic and oleophilic sponge-like compositions |
| CN104629079A (en) * | 2014-12-05 | 2015-05-20 | 武汉工程大学 | Elastic superhydrophobic chitosan oil-absorption sponge as well as preparation method and application thereof |
| US20170182474A1 (en) * | 2015-12-28 | 2017-06-29 | Aruna Zhamu | Integral 3D graphene-carbon hybrid foam and devices containing same |
| CN105694092A (en) * | 2016-02-01 | 2016-06-22 | 东南大学 | Preparation method of super-hydrophobic graphene sponge |
| CN106693444A (en) * | 2016-12-27 | 2017-05-24 | 西南石油大学 | Preparing method of reproducible super-hydrophobic graphite alkenyl oil absorption sponge |
| CN107570127A (en) * | 2017-09-08 | 2018-01-12 | 浙江工业大学 | A kind of graphene-based water-oil separating foamed material and its preparation method and application |
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