CN104843690A - Method for preparing graphene by means of steam explosion method - Google Patents
Method for preparing graphene by means of steam explosion method Download PDFInfo
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- CN104843690A CN104843690A CN201510213046.6A CN201510213046A CN104843690A CN 104843690 A CN104843690 A CN 104843690A CN 201510213046 A CN201510213046 A CN 201510213046A CN 104843690 A CN104843690 A CN 104843690A
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Abstract
A method for preparing graphene by means of a steam explosion method comprises the following steps of 1 using graphene to prepare oxidized graphene, 2 mixing the prepared oxidized graphene and dispersion liquid and performing ultrasonic dispersion and stirring to obtain an oxidized graphene solution; 3 arranging the oxidized graphene solution in a steam explosion pressure relief valve, controlling temperature rising rate to be 5 DEG C/min-15 DEG C/min, rising the temperature to be 300 DEG-500 DEG C, keeping the temperature for 2-10 hours and then instantly releasing pressure to obtain a reaction product; 4 washing and drying the reaction product to obtain the graphene. The method is simple in operation, short in preparation time, free of pollution, low in cost and high in yield, can be used for lithium battery electrode materials and lubricating materials, can be also used for medicine, catalysis or special spraying materials and can be directly used as or synthesized into an abrasion-resisting material for an engine air cylinder.
Description
Technical field
The present invention relates to grapheme material field, particularly a kind of with the method for the quick-fried legal system of vapour for Graphene.
Background technology
Graphene be a kind of by carbon atom with sp
2hybridized orbital composition hexangle type be honeycomb lattice flat film, only have the two-dimensional material of a carbon atom thickness, be thin, the hardest nano material in known world.It is almost completely transparent, only absorbs the light of 2.3%; Thermal conductivity is up to 5300 W/mK, and higher than carbon nanotube and diamond, under normal temperature, its electronic mobility is more than 15000 cm
2/ Vs, again than CNT (carbon nano-tube) or silicon wafer height, and resistivity only about 10
-8Ω cm, than copper or silver lower, be the material that world resistivity is minimum, particularly there is the theoretical specific surface area 2630m of super large
2/ g.
Graphene has huge application prospect, and this finds a kind of quick, efficient, cheap preparation method to meet growing demand with regard to requiring.The situation ubiquity that Graphene production capacity is low, quality is unstable both at home and abroad at present, adopt chemical process to prepare Graphene mostly, this is very large to the performance impact of Graphene, and have that environmental pollution is serious, raw materials cost is high simultaneously, severe reaction conditions, the problem such as yield poorly, practicality is not strong.
CN201310262842.X discloses the method for a kind of foaming and intumescing legal system for Graphene, and it adopts graphene/polyurethane composite material to prepare Graphene, and preparation process does not use strong oxidizing property, strong and stimulating material; But the method operation introduces new chemical substance, increase cost, and preparation time is long, is unfavorable for that fast industrialization is produced.
Summary of the invention
The object of the invention is to overcome the above-mentioned deficiency of prior art and provide a kind of simple to operate, preparation time is short, pollution-free, and cost is low, output high with the method for the quick-fried legal system of vapour for Graphene.
Technical scheme of the present invention is:
With the quick-fried legal system of vapour for a method for Graphene, comprise the following steps:
(1) use graphite-made for graphene oxide;
(2) carry out ultrasonic disperse after being mixed with dispersion liquid by the graphene oxide prepared and stir, obtaining graphene oxide solution;
(3) graphene oxide solution is placed in the quick-fried pressure release valve of vapour, to control temperature rise rate be 5 DEG C/min ~ 15 DEG C/min, be warming up to 300 DEG C ~ 500 DEG C, moment release after insulation 2h ~ 10h, obtains reaction product;
(4) Graphene is obtained by after reaction product washing, drying.
Further, described use graphite-made comprises for the step of graphene oxide:
(1) add 300 ~ 500ml strong acid in a kettle., then add 6g graphite, normal temperature, stir 1 hour;
(2) add oxygenant 0 ~ 16g, stir 2 hours, obtain mixture;
(3) mixture is centrifugal, gained filter residue adopts pure water twice;
(4) in washed filter residue, hydrogen peroxide 5ml is added, the more also washing and filter pressing that stirs that adds water, obtain graphene oxide.
Further, described strong acid be sulfuric acid, chlorsulfonic acid, phosphoric acid, nitric acid, fluosulfonic acid one or more, acid concentration be not less than 50%.
Further, described oxygenant is one or more in potassium permanganate, Potassium Iodate, potassium ferrate.
Further, centrifugal speed when described mixture is centrifugal is 8000 ~ 10000rpm, and centrifugation time is 10 ~ 20min; The centrifugal centrifugate used of mixture is reusable.
Further, in step (2), the graphene oxide prepared is mixed with dispersion liquid and carries out ultrasonic disperse and stir 20min, obtain graphene oxide solution.
Further, the quick-fried pressure release valve of described vapour comprises valve seat, valve body and the valve gap installed successively from top to bottom, heated base is provided with between described valve seat and valve body, the top of described heated base is provided with piston-type flap, described piston-type flap connection valve bar, the end of described valve rod is connected stage clip through valve body with after valve gap.
Further, described graphene oxide solution enters from the entrance of heated base, to control temperature rise rate be 5 DEG C/min ~ 15 DEG C/min(is preferably 6 DEG C/min ~ 9 DEG C/min, be more preferably 10 DEG C/min ~ 14 DEG C/min), be warming up to 300 DEG C ~ 500 DEG C and (be preferably 350 DEG C ~ 400 DEG C, be more preferably 430 DEG C ~ 480 DEG C), the high pressure gas produced promote piston-type flap and move up, stage clip bends by valve rod, treat that insulation 2h ~ 10h(is preferably 3h ~ 5h, be more preferably 6h ~ 9h) after, release is carried out in the air outlet of opening valve body, namely in heated base, reaction product is obtained.
Further, describedly graphene oxide solution is placed in the quick-fried pressure release valve of vapour, to control temperature rise rate be 6 DEG C/min ~ 9 DEG C/min, be warming up to 350 DEG C ~ 400 DEG C, moment release after insulation 3h ~ 5h, obtains reaction product.
Further, describedly graphene oxide solution is placed in the quick-fried pressure release valve of vapour, to control temperature rise rate be 10 DEG C/min ~ 14 DEG C/min, be warming up to 430 DEG C ~ 480 DEG C, moment release after insulation 6h ~ 9h, obtains reaction product.
The present invention compared with prior art has following features: obtain graphene oxide by peeling off at a high speed graphite, utilize pressure expansion strip off graphene sheet layer, simple to operate, preparation time is short, pollution-free, cost is low, output is high, can be used for electrode material of lithium battery, lubricant, also can be used for medicine, catalysis or do extraordinary spray material (as non-stick cooker, glass with clean plated film etc.), also can directly or synthesis do the high-abrasive material etc. of engine cylinder.
Accompanying drawing explanation
Fig. 1 is the structural representation of embodiment of the present invention reactor;
Fig. 2 is the structural representation of embodiment of the present invention vapour quick-fried pressure release valve when not working;
Structural representation when Fig. 3 is the work of embodiment of the present invention vapour quick-fried pressure release valve;
Fig. 4 is the SEM electron microscopic picture of Graphene prepared by the embodiment of the present invention.
Embodiment
Below in conjunction with the drawings and specific embodiments, detailed construction of the present invention is further described.
Device embodiment:
Embodiment 1
Graphene oxide is prepared in reactor.As shown in Figure 1: reactor comprises container body 1, the side, upper end of container body 1 is provided with charging opening 11, and bottom is provided with discharge port 12, and middle part is provided with motor 2, and the bottom of motor 2 is provided with rotor 3, and the outside of rotor 3 is provided with stator 4.Run can peel off graphite fast by the high speed centrifugation of rotor 3, prepare graphene oxide, shorten preparation time.
Embodiment 2
Graphene is prepared in the quick-fried pressure release valve of vapour.As shown in Figure 2: the quick-fried pressure release valve of vapour comprises valve seat 5, valve body 6 and the valve gap 7 installed successively from top to bottom, heated base 8 is provided with between valve seat 5 and valve body 6, the top of heated base 8 is provided with piston-type flap 61, piston-type flap 61 connects valve rod 62, and the end of valve rod 62 is connected stage clip 9 through valve body 6 with after valve gap 7.
During work, as shown in Figure 3: the ingress of graphene oxide solution from heated base 8 pumps into by the quick-fried pressure release valve of vapour, obtain High Temperature High Pressure through heating, and then promotion piston-type flap 61 moves upward, stage clip 9 bends by valve rod 62; Utilize pressure expansion strip off graphene sheet layer, after pushing aside completely, release is carried out in the air outlet of opening valve body 6, thus obtains Graphene.Adopt the quick-fried pressure release valve of vapour to prepare Graphene and can shorten preparation time, and form enclosed space in valve body 6 during work, safety coefficient is high, pollution-free, and prepared Graphene output is high.
Embodiment of the method:
Embodiment 1
(1) add in a kettle. 400ml, 98% sulfuric acid, add 6g graphite, normal temperature, stir 1 hour, then add potassium permanganate 12g, stir 2 hours; (2) with the centrifugal 20min of the rotating speed of 8000rpm, centrifugate is reusable, and centrifugal gained filter residue pure water twice, adds hydrogen peroxide 5ml in washed filter residue, the more also washing and filter pressing that stirs that adds water, and obtains graphene oxide; (3) carry out ultrasonic disperse after being mixed with dispersion liquid by graphene oxide and stir, obtaining graphene oxide solution; (4) proceed in the quick-fried pressure release valve of vapour, to control temperature rise rate be 5 DEG C/min ~ 10 DEG C/min, be warming up to 300 DEG C ~ 500 DEG C, moment release after insulation 2h ~ 4h, obtains reaction product; Graphene is obtained again, as shown in Figure 4 by after reaction product washing, drying.
Embodiment 2
The difference of the present embodiment and embodiment 1 is: to control temperature rise rate be 6 DEG C/and min ~ 15 DEG C/min, be warming up to 350 DEG C ~ 500 DEG C, insulation 2h ~ 4h.Other is identical with embodiment 1.
Embodiment 3
The difference of the present embodiment and embodiment 1 is: to control temperature rise rate be 6 DEG C/and min ~ 9 DEG C/min, be warming up to 350 DEG C ~ 400 DEG C, insulation 3h ~ 5h.Other is identical with embodiment 1.
Embodiment 4
The difference of the present embodiment and embodiment 1 is: to control temperature rise rate be 10 DEG C/and min ~ 14 DEG C/min, be warming up to 430 DEG C ~ 480 DEG C, insulation 6h ~ 9h.Other is identical with embodiment 1.
Embodiment 5
The present embodiment and specific embodiment 1 unlike: to control temperature rise rate be 8 DEG C/min ~ 10 DEG C/min, is warming up to 320 DEG C ~ 400 DEG C, insulation 3h ~ 6h.Other is identical with embodiment 1.
Embodiment 6
The present embodiment and specific embodiment 1 unlike: to control temperature rise rate be 7 DEG C/min ~ 12 DEG C/min, is warming up to 420 DEG C ~ 450 DEG C, insulation 3h ~ 5h.Other is identical with embodiment 1.
Embodiment 7
The present embodiment and specific embodiment 1 unlike: to control temperature rise rate be 7 DEG C/min ~ 14 DEG C/min, is warming up to 460 DEG C ~ 490 DEG C, insulation 2h ~ 3h.Other is identical with embodiment 1.
Embodiment 8
The present embodiment and specific embodiment 1 unlike: to control temperature rise rate be 9 DEG C/min ~ 12 DEG C/min, is warming up to 310 DEG C ~ 350 DEG C, insulation 2h.Other is identical with embodiment 1.
Embodiment 9
The present embodiment and specific embodiment 1 unlike: to control temperature rise rate be 10 DEG C/min ~ 12 DEG C/min, is warming up to 360 DEG C ~ 400 DEG C, insulation 4h.Other is identical with embodiment 1.
Embodiment 10
The present embodiment and specific embodiment 1 unlike: to control temperature rise rate be 13 DEG C/min ~ 15 DEG C/min, is warming up to 410 DEG C ~ 450 DEG C, insulation 5h.Other is identical with embodiment 1.
The output adopting the Graphene prepared by method of the present embodiment 1 ~ 10 is 5g ~ 6g.
These are only the preferred embodiments of the present invention, be not limited to the present invention, obviously, those skilled in the art can carry out various change, modification and do not depart from the spirit and scope of the present invention to the present invention.If belong within the scope of the claims in the present invention and equivalent technologies thereof these amendments of the present invention and modification, all belong to protection scope of the present invention.
Claims (10)
1. with the quick-fried legal system of vapour for a method for Graphene, it is characterized in that: comprise the following steps:
(1) use graphite-made for graphene oxide;
(2) carry out ultrasonic disperse after being mixed with dispersion liquid by the graphene oxide prepared and stir, obtaining graphene oxide solution;
(3) graphene oxide solution is placed in the quick-fried pressure release valve of vapour, to control temperature rise rate be 5 DEG C/min ~ 15 DEG C/min, be warming up to 300 DEG C ~ 500 DEG C, moment release after insulation 2h ~ 10h, obtains reaction product;
(4) Graphene is obtained by after reaction product washing, drying.
2. according to claim 1 with the quick-fried legal system of vapour for the method for Graphene, it is characterized in that: described use graphite-made comprises for the step of graphene oxide:
(1) add 300 ~ 500ml strong acid in a kettle., then add 6g graphite, normal temperature, stir 1 hour;
(2) add oxygenant 0 ~ 16g, stir 2 hours, obtain mixture;
(3) mixture is centrifugal, gained filter residue adopts pure water twice;
(4) in washed filter residue, hydrogen peroxide 5ml is added, the more also washing and filter pressing that stirs that adds water, obtain graphene oxide.
3. according to claim 2 with the quick-fried legal system of vapour for the method for Graphene, it is characterized in that: described strong acid be sulfuric acid, chlorsulfonic acid, phosphoric acid, nitric acid, fluosulfonic acid one or more, acid concentration be not less than 50%.
4. according to Claims 2 or 3 with the quick-fried legal system of vapour for the method for Graphene, it is characterized in that: described oxygenant is one or more in potassium permanganate, Potassium Iodate, potassium ferrate.
5. according to Claims 2 or 3 with the quick-fried legal system of vapour for the method for Graphene, it is characterized in that: centrifugal speed when described mixture is centrifugal is 8000 ~ 10000rpm, centrifugation time is 10 ~ 20min; The centrifugal centrifugate used of mixture is reusable.
6. according to claim 1 with the quick-fried legal system of vapour for the method for Graphene, it is characterized in that: in step (2), the graphene oxide prepared mixed with dispersion liquid and carries out ultrasonic disperse and stir 20min, obtain graphene oxide solution.
7. according to claim 1 or 2 or 3 with the method for the quick-fried legal system of vapour for Graphene, it is characterized in that: the quick-fried pressure release valve of described vapour comprises valve seat, valve body and the valve gap installed successively from top to bottom, heated base is provided with between described valve seat and valve body, the top of described heated base is provided with piston-type flap, described piston-type flap connection valve bar, the end of described valve rod is connected stage clip through valve body with after valve gap.
8. according to claim 7 with the method for the quick-fried legal system of vapour for Graphene, it is characterized in that: described graphene oxide solution enters from the entrance of heated base, to control temperature rise rate be 5 DEG C/min ~ 15 DEG C/min, be warming up to 300 DEG C ~ 500 DEG C, the high pressure gas produced promote piston-type flap and move up, and stage clip bends by valve rod, after insulation 2h ~ 10h, release is carried out in the air outlet of opening valve body, namely in heated base, obtains reaction product.
9. according to claim 1 or 2 or 3 with the method for the quick-fried legal system of vapour for Graphene, it is characterized in that: describedly graphene oxide solution is placed in the quick-fried pressure release valve of vapour, to control temperature rise rate be 6 DEG C/min ~ 9 DEG C/min, be warming up to 350 DEG C ~ 400 DEG C, moment release after insulation 3h ~ 5h, obtains reaction product.
10. according to claim 1 or 2 or 3 with the method for the quick-fried legal system of vapour for Graphene, it is characterized in that: describedly graphene oxide solution is placed in the quick-fried pressure release valve of vapour, to control temperature rise rate be 10 DEG C/min ~ 14 DEG C/min, be warming up to 430 DEG C ~ 480 DEG C, moment release after insulation 6h ~ 9h, obtains reaction product.
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Cited By (7)
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| CN105752964A (en) * | 2016-01-25 | 2016-07-13 | 肖荣阁 | High-temperature high-pressure bursting method for producing graphene and equipment |
| CN106517168A (en) * | 2016-11-10 | 2017-03-22 | 中国石油大学(北京) | Device and method for preparing graphene by exfoliating graphite through quick pressure relief |
| CN107032338A (en) * | 2017-06-19 | 2017-08-11 | 成都新柯力化工科技有限公司 | A kind of method of continuous discharge-induced explosion parallel off preparing graphite alkene |
| CN110156002A (en) * | 2019-06-04 | 2019-08-23 | 新疆弘瑞达纤维有限公司 | A kind of preparation method of graphene oxide composite material |
| CN111498838A (en) * | 2020-05-12 | 2020-08-07 | 山东领军科技集团有限公司 | Graphene wet-process air pressure stripping method |
| CN115124033A (en) * | 2022-06-30 | 2022-09-30 | 哈尔滨石油学院 | Graphene stripping device and graphene preparation method |
| CN115536016A (en) * | 2022-10-12 | 2022-12-30 | 三门峡芳瑞杜仲产业技术研究院有限公司 | Physical graphene stripping method |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105752964A (en) * | 2016-01-25 | 2016-07-13 | 肖荣阁 | High-temperature high-pressure bursting method for producing graphene and equipment |
| CN106517168A (en) * | 2016-11-10 | 2017-03-22 | 中国石油大学(北京) | Device and method for preparing graphene by exfoliating graphite through quick pressure relief |
| CN107032338A (en) * | 2017-06-19 | 2017-08-11 | 成都新柯力化工科技有限公司 | A kind of method of continuous discharge-induced explosion parallel off preparing graphite alkene |
| CN107032338B (en) * | 2017-06-19 | 2018-03-09 | 成都新柯力化工科技有限公司 | A kind of method of continuous discharge-induced explosion parallel off preparing graphite alkene |
| CN110156002A (en) * | 2019-06-04 | 2019-08-23 | 新疆弘瑞达纤维有限公司 | A kind of preparation method of graphene oxide composite material |
| CN110156002B (en) * | 2019-06-04 | 2023-02-10 | 新疆弘瑞达纤维有限公司 | Preparation method of graphene oxide material |
| CN111498838A (en) * | 2020-05-12 | 2020-08-07 | 山东领军科技集团有限公司 | Graphene wet-process air pressure stripping method |
| CN115124033A (en) * | 2022-06-30 | 2022-09-30 | 哈尔滨石油学院 | Graphene stripping device and graphene preparation method |
| CN115124033B (en) * | 2022-06-30 | 2024-03-29 | 哈尔滨石油学院 | Graphene stripping device and graphene preparation method |
| CN115536016A (en) * | 2022-10-12 | 2022-12-30 | 三门峡芳瑞杜仲产业技术研究院有限公司 | Physical graphene stripping method |
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