CN102553521B - A kind of preparation method of magnetic graphite - Google Patents
A kind of preparation method of magnetic graphite Download PDFInfo
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- CN102553521B CN102553521B CN201010613011.9A CN201010613011A CN102553521B CN 102553521 B CN102553521 B CN 102553521B CN 201010613011 A CN201010613011 A CN 201010613011A CN 102553521 B CN102553521 B CN 102553521B
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Abstract
The invention belongs to technical field of inorganic material, disclose a kind of preparation method of magnetic graphite, the method comprises the following steps: graphite oxide disperses in a solvent by (1), concentration is 0.1 ~ 5wt%, ultrasonic disperse 1 ~ 10 hour, obtain graphite oxide colloid suspension, be heated to boiling, inflated with nitrogen keeps away oxygen; (2) by tri-iron tetroxide particle dispersion in the solvent identical with step (1), concentration is 0.1 ~ 5wt%, ultrasonic disperse 1 ~ 10 hour, obtains finely dispersed tri-iron tetroxide suspension; (3) the tri-iron tetroxide suspension that step (2) obtains being joined step (1) temperature is in the graphite oxide suspension of 50 ~ 80 DEG C, tri-iron tetroxide mass particle and the middle graphite oxide mass ratio of step (1) are 0.1: 1 ~ 2: 1, be uniformly mixed, backflow 30 ~ 120min, naturally cooling, filtration, vacuum drying, keep away oxygen storage, namely obtain magnetic graphite.Magnetic graphite prepared by the inventive method, can be easy to be dispersed in water.
Description
Technical field
The invention belongs to technical field of inorganic material, be specifically related to a kind of preparation method of magnetic graphite.
Background technology
Along with global economic development, more and more large to the demand of oil equal energy source raw material, due to shipping work in world wide and marine incident, especially the sporadic accident such as oil carrier accident and oil platform, store oil and oil transportation facility is increasing, and environment waters oil pollution is also more and more serious.Therefore, control and administer oil pollution of waters dye and the leakage of oil of recovery accident extremely urgent, key technology is the efficient oil suction of developmental research, be easy to the novel environmental functional material reclaiming comprehensive utilization.Expanded graphite becomes the study hotspot of water body greasy dirt in recent years with the advantage of uniqueness, and it has flourishing network-like pore structure.Specific area is large, and hole forms primarily of macropore, has good absorption property.The group on expanded graphite surface is mainly non-polar group, thus for the hydrophobic substance in the aqueous solution, there is good absorption property, especially for oil pollutant, there is high absorption property, there is low-density, high chemical stability, nontoxic and cyclic utilization rate high, be considered to the ideal material of very promising improvement sea oil spill.But due to shortcomings such as expanded graphite light weight, property compatible with water differences, and marine weather condition is complicated, affects wayward by wave, sea wind and reclaims, and is unfavorable for practical application.Therefore, find or synthesize a kind of water-soluble, be easy to control graphite material have important application value.
Summary of the invention
The object of this invention is to provide a kind of preparation method of magnetic graphite.
Technical scheme of the present invention is as follows:
The invention provides a kind of preparation method of magnetic graphite, the method comprises the following steps:
(1) by graphite oxide dispersion in a solvent, concentration is 0.1 ~ 5wt%, ultrasonic disperse 1 ~ 10 hour, obtains graphite oxide colloid suspension, and be heated to boiling, inflated with nitrogen keeps away oxygen;
(2) by tri-iron tetroxide particle dispersion in the solvent identical with step (1), concentration is 0.1 ~ 5wt%, ultrasonic disperse 1 ~ 10 hour, obtains finely dispersed tri-iron tetroxide suspension;
(3) the tri-iron tetroxide suspension that step (2) obtains being joined step (1) temperature is in the graphite oxide suspension of 50 ~ 80 DEG C, tri-iron tetroxide mass particle and the middle graphite oxide mass ratio of step (1) are 0.1: 1 ~ 2: 1, be uniformly mixed, backflow 30 ~ 120min, naturally cooling, filtration, vacuum drying, keep away oxygen storage, namely obtain magnetic graphite.
The preparation method of described graphite oxide is selected from the one in Brodie method, Staudenmaier method or Hummers method.
Described solvent is selected from the one in DMF (DMF) or DMA (DMAC).
The tri-iron tetroxide that described tri-iron tetroxide particle is selected from unmodified or the one organised in the tri-iron tetroxide of modification.
Compared with the existing technology, tool has the following advantages and beneficial effect in the present invention:
Expansible graphite strong acid and strong oxidizer are oxidized to graphite oxide by the present invention, and graphite oxide interlayer has the functional group such as hydroxyl or carboxyl, substantially improve the microenvironment of graphite linings.Magnetic ferroferric oxide particle is easy to and graphite oxide intercalation synthesis, prepare the material of the magnetic absorption greasy dirt of tool, graphite oxide interlayer contains polar group, can be easy to be dispersed in water, so that realize can either efficient adsorption oil pollution of waters, being convenient to again control and reclaim, providing new method for administering water environment oil pollution.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is further illustrated.
Embodiment 1
(1) be dispersed in 100mlDMAC by 1g by the graphite oxide that Brodie legal system is standby, ultrasonic disperse 5 hours, obtain graphite oxide colloid suspension, be heated to boiling, inflated with nitrogen keeps away oxygen;
(2) by the tri-iron tetroxide particle dispersion of 0.5g unmodified in 50mlDMAC solvent, ultrasonic disperse 5 hours, obtains finely dispersed tri-iron tetroxide suspension;
(3) the tri-iron tetroxide suspension that step (2) obtains being joined step (1) temperature is in the graphite oxide suspension of 60 DEG C, be uniformly mixed, backflow 30min, cooling naturally, filtration, vacuum drying, keep away oxygen storage, namely obtain magnetic graphite.
Embodiment 2
(1) be dispersed in 100mlDMF by 1g by the graphite oxide that Staudenmaier legal system is standby, ultrasonic disperse 5 hours, obtain graphite oxide colloid suspension, be heated to boiling, inflated with nitrogen keeps away oxygen;
(2) the tri-iron tetroxide particle dispersion of modifying that organised by 0.5g is in 50mlDMF solvent, and ultrasonic disperse 5 hours, obtains finely dispersed tri-iron tetroxide suspension;
(3) the tri-iron tetroxide suspension that step (2) obtains being joined step (1) temperature is in the graphite oxide suspension of 70 DEG C, be uniformly mixed, backflow 30min, cooling naturally, filtration, vacuum drying, keep away oxygen storage, namely obtain magnetic graphite.
Embodiment 3
(1) be dispersed in 100mlDMAC by 1.5g by the graphite oxide that Hummers legal system is standby, ultrasonic disperse 5 hours, obtain graphite oxide colloid suspension, be heated to boiling, inflated with nitrogen keeps away oxygen;
(2) by the tri-iron tetroxide particle dispersion of 1.5g unmodified in 100mlDMAC solvent, ultrasonic disperse 5 hours, obtains finely dispersed tri-iron tetroxide suspension;
(3) the tri-iron tetroxide suspension that step (2) obtains being joined step (1) temperature is in the graphite oxide suspension of 80, be uniformly mixed, backflow 1.5h, cooling naturally, filtration, vacuum drying, keep away oxygen storage, namely obtain magnetic graphite.
Embodiment 4
(1) be dispersed in 100mlDMF by 2g by the graphite oxide that Hummers legal system is standby, ultrasonic disperse 10 hours, obtain graphite oxide colloid suspension, be heated to boiling, inflated with nitrogen keeps away oxygen;
(2) the tri-iron tetroxide particle dispersion of modifying that organised by 4g is in 100mlDMF solvent, and ultrasonic disperse 10 hours, obtains finely dispersed tri-iron tetroxide suspension;
(3) the tri-iron tetroxide suspension that step (2) obtains being joined step (1) temperature is in the graphite oxide suspension of 70 DEG C, be uniformly mixed, backflow 1.5h, cooling naturally, filtration, vacuum drying, keep away oxygen storage, namely obtain magnetic graphite.
Above-mentioned is can understand and apply the invention for ease of those skilled in the art to the description of embodiment.Person skilled in the art obviously easily can make various amendment to these embodiments, and General Principle described herein is applied in other embodiments and need not through performing creative labour.Therefore, the invention is not restricted to embodiment here, those skilled in the art, according to announcement of the present invention, do not depart from improvement that scope makes and amendment all should within protection scope of the present invention.
Claims (1)
1. a preparation method for magnetic graphite, is characterized in that: the method comprises the following steps,
(1) by graphite oxide dispersion in a solvent, concentration is 1.1wt% or 1.6wt% or 2.1%, ultrasonic disperse 5 or 10 hours, obtains graphite oxide colloid suspension, and be heated to boiling, inflated with nitrogen keeps away oxygen;
(2) by tri-iron tetroxide particle dispersion in the solvent identical with step (1), concentration is 1.1wt% or 1.6wt% or 4.2wt%, ultrasonic disperse 5 or 10 hours, obtains finely dispersed tri-iron tetroxide suspension;
(3) the tri-iron tetroxide suspension that step (2) obtains being joined step (1) temperature is in the graphite oxide suspension of 60 or 70 or 80 DEG C, tri-iron tetroxide mass particle and the middle graphite oxide mass ratio of step (1) are 0.5:1 or 1:1 or 2:1, be uniformly mixed, backflow 30 or 90min, naturally cooling, filtration, vacuum drying, keep away oxygen storage, namely obtain magnetic graphite;
Described solvent is selected from the one in DMF or DMA;
The preparation method of described graphite oxide is selected from the one in Brodie method, Staudenmaier method or Hummers method;
The tri-iron tetroxide that described tri-iron tetroxide particle is selected from unmodified or the one organised in the tri-iron tetroxide of modification.
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| CN201010613011.9A CN102553521B (en) | 2010-12-29 | 2010-12-29 | A kind of preparation method of magnetic graphite |
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| CN102553521B true CN102553521B (en) | 2015-09-09 |
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| CN108558231B (en) * | 2018-04-26 | 2021-04-09 | 山西奇宇环保新材料研究院有限公司 | Preparation method of magnetic graphite oxide composite membrane |
| CN110980724B (en) * | 2019-12-31 | 2022-11-25 | 东华大学 | Magnetic graphite oxide and preparation method and application thereof |
Citations (4)
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| CN1837148A (en) * | 2006-04-07 | 2006-09-27 | 华侨大学 | Process for making graphite powder with electromagnetic property |
| CN101279730A (en) * | 2008-05-20 | 2008-10-08 | 厦门大学 | Preparation for aminated magnetic carbon tube and application thereof to biosensor |
| CN101474406A (en) * | 2008-12-19 | 2009-07-08 | 天津医科大学 | Mono-layer oxidized mineral carbon and ferriferrous oxide composite material as well as preparation and application |
| CN101525436A (en) * | 2009-03-20 | 2009-09-09 | 西北师范大学 | Polypyrrole/Fe*O*/nanometer graphite sheet composite material and preparation method thereof |
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2010
- 2010-12-29 CN CN201010613011.9A patent/CN102553521B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1837148A (en) * | 2006-04-07 | 2006-09-27 | 华侨大学 | Process for making graphite powder with electromagnetic property |
| CN101279730A (en) * | 2008-05-20 | 2008-10-08 | 厦门大学 | Preparation for aminated magnetic carbon tube and application thereof to biosensor |
| CN101474406A (en) * | 2008-12-19 | 2009-07-08 | 天津医科大学 | Mono-layer oxidized mineral carbon and ferriferrous oxide composite material as well as preparation and application |
| CN101525436A (en) * | 2009-03-20 | 2009-09-09 | 西北师范大学 | Polypyrrole/Fe*O*/nanometer graphite sheet composite material and preparation method thereof |
Non-Patent Citations (2)
| Title |
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| Water-Soluble Magnetic-Functionalized Reduced Graphene Oxide Sheets: In situ Synthesis and Magnetic Resonance Imaging Applications;Huai-Ping Cong，Jia-Jun He，Yang Lu，Shu-Hong Yu;《small》;20091102;第6卷(第2期);全文 * |
| Xiaoying Yang,Xiaoyan Zhang,Yanfeng Ma,Yi Huang,Yinsong Wang.Superparamagnetic graphene oxide–Fe3O4 nanoparticles hybrid for controlled targeted drug carriers.《Journal of Materials Chemistry》.2009,第19卷2710-2714. * |
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