CN105752964A - High-temperature high-pressure bursting method for producing graphene and equipment - Google Patents
High-temperature high-pressure bursting method for producing graphene and equipment Download PDFInfo
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- CN105752964A CN105752964A CN201610049559.2A CN201610049559A CN105752964A CN 105752964 A CN105752964 A CN 105752964A CN 201610049559 A CN201610049559 A CN 201610049559A CN 105752964 A CN105752964 A CN 105752964A
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Abstract
The invention provides a high-temperature high-pressure bursting method for producing graphene and equipment.The equipment comprises a high-pressure kettle and at least two stages of collecting covers, wherein every collecting cover is of a barrel-shaped structure with the top open, the collecting covers are distributed concentrically, and the high-pressure kettle is positioned in the centers of the collecting covers.
Description
Technical field
The present invention relates to Graphene production field, especially relate to produce High Temperature High Pressure decrepitation method and the production equipment of Graphene.
Background technology
Graphene (Graphene) is the two dimensional crystal of the only one layer of atomic thickness being stripped out from graphite material, being made up of carbon atom.2004, Univ Manchester UK physicist An Deliegaimu and Constantine's Nuo Woxiao love, Graphene is isolated in success from graphite, it was demonstrated that it can individualism, therefore two people also obtain Nobel Prize in physics in 2010 jointly.
Graphene is the thinnest material, is also the most tough material, more taller than best steel 200 times of fracture strength.It has again good elasticity simultaneously, and stretch range can reach the 20% of own dimensions.It is the material that current nature is the thinnest, intensity is the highest, if making hammock with the Graphene of one piece of area 1 square metre, weight own just can bear the cat of a kilogram less than 1 milligram.
The current most potential application of Graphene is the succedaneum becoming silicon, manufactures superminiature transistor, is used for producing the supercomputer in future.Replacing silicon with Graphene, the speed of service of computer processor will hundreds times soon.
It addition, Graphene is almost fully transparent, only absorb the light of 2.3%.On the other hand, it is very fine and close, even minimum gas atom (helium atom) also cannot penetrate.These features make it be highly suitable as the raw material of transparent electron product, such as transparent touch display screen, luminous plaque and solar panel.
As the thinnest, a kind of novel nano-material that maximum intensity, electrical and thermal conductivity performance are the strongest that have now been found that, Graphene is referred to as " dark fund ", is " king of new material ", and scientist even foretells that Graphene " will thoroughly change 21 century ".Very likely start a subversiveness new technique new industrial revolution have swept the globe, but batch production high-quality Graphene is the bottleneck of this new material business development application.
The production method of existing Graphene industrially mainly uses acidleach to send out, and acidleach is entered between the molecular layer of graphite, is washed out afterwards, prepare Graphene, but in this kind of method, acid is not easily cleaned, cause for this in subsequent step, between Graphene, leave impurity, affect subsequent production and use；
Graphene is to be formed by adhesive tape sticky paper in the lab, does not have impurity, but yield is very little in Graphene prepared by this kind of method, is simply applicable to the use of laboratory small batch.
Summary of the invention
It is an object of the invention to provide a kind of for the method that efficiently batch prepares high-quality Graphene, and realize the equipment of this method, be especially suitable in industry production Graphene.
The technical scheme is that
A kind of High Temperature High Pressure decrepitation method for producing Graphene,
S1, admixed graphite, liquid nitrogen and penetration aid, in reactor, form homogeneous mixture；
S2, closed reaction still；
S3, heat described mixture；
S4, expose described mixture at ambient pressure；
S5, collection Graphene.
Further, in S1, the volume ratio of described graphite and described liquid nitrogen is 1:3.
Further, in S3, the speed of described heating is at the uniform velocity.
Further, described penetration aid is hydrogen peroxide.
Further, when reacting kettle inner pressure is 40MPa, temperature in the kettle controls at 400 DEG C
Further, in S3, after heating, make reacting kettle inner pressure between 3.4～40.0MPa.
Further, one is used for including autoclave and at least two-stage pressure-bearing collecting hood；
Described pressure-bearing collecting hood is the barrel-like structure of open-top, and at least the described pressure-bearing collecting hood of two-stage is arranged with one heart, and described autoclave is positioned at the center of described collecting hood；Described autoclave is provided with attemperating unit and pressure control device.
Further, described autoclave includes pressure reducing sleeve, temperature and pressure inner bag two parts；
Described temperature and pressure inner bag is embedded inside described pressure reducing sleeve, is rotatably connected with described pressure reducing sleeve；Described temperature and pressure inner bag is provided with heating wire.
At least one mutually corresponding discharge opening is all offered on described pressure reducing sleeve, on described temperature and pressure inner bag.
Further, the outside of described pressure reducing sleeve is equipped with ring gear, and the side of described ring gear is provided with the driving gear cooperated with described ring gear, and described driving gear is fixing with the outfan of motor to be connected.
Further, the top of described pressure-bearing collecting hood is provided with collected overhead cover, and described collected overhead cover is the ring wall tilted to described collecting hood center.
The present invention has the advantage that and has the benefit effect that owing to adopting technique scheme, present invention have the advantage that
The problem solving Graphene large-scale production, use the liquids such as liquid nitrogen, distilled water or hydrogen peroxide, afterwards by heating the pattern of supercharging, graphite is fully infiltrated, fast decompression afterwards, it is positioned at the rapid expanding blastings of liquid such as the liquid nitrogen between graphitic molecules, distilled water, hydrogen peroxide, prepares Graphene with this.
Accompanying drawing explanation
Fig. 1 is the schematic cross-section producing Graphene equipment of the present invention.
In figure:
1, pressure reducing sleeve 2, temperature and pressure inner bag 3, autoclave
4,5, two grades of pressure-bearing collecting hoods 6, discharge openings of one-level pressure-bearing collecting hood
7, driving gear 8, ring gear 9, collected overhead cover
Detailed description of the invention
By particular specific embodiment, embodiments of the present invention being described below, those skilled in the art the content disclosed by this specification can understand other advantages and effect of the present invention easily.
Notice, the structure of this specification institute accompanying drawings depicted, ratio, size etc., all only in order to coordinate the disclosed content of description, understand for those skilled in the art and read, it is not limited to the enforceable qualifications of the present invention, therefore do not have technical essential meaning, the adjustment of the modification of any structure, the change of proportionate relationship or size, under not affecting effect that the present invention can be generated by and the purpose that can reach, all should still drop on disclosed technology contents and obtain in the scope that can contain.Simultaneously, in this specification cited as " on ", D score, "left", "right", " centre " etc. term, it is merely convenient to understanding of narration, and it is not used to limit the enforceable scope of the present invention, the change of its relativeness or adjustment, changing under technology contents without essence, when being also considered as the enforceable category of the present invention.
A kind of High Temperature High Pressure decrepitation method for producing Graphene,
S1, admixed graphite, liquid nitrogen and penetration aid, in reactor, form homogeneous mixture；
Graphite porosity 75%, with 1:3 ratio admixed graphite and liquid nitrogen, distilled water or hydrogen peroxide isoperm is strong, the coefficient of expansion big, the liquid of easily diffusion, under high pressure make the liquids such as liquid nitrogen, distilled water or hydrogen peroxide be fully infiltrated into graphite wafer interlayer, make mixture.
S2, closed reaction still；
S3, heat described mixture；
The mixture constant-speed heating of the liquids such as saturated liquid nitrogen, distilled water or hydrogen peroxide, intrinsic pressure to increase；
S4, expose described mixture at ambient pressure；
Suddenly decompression exposes described mixture at ambient pressure, so that the unexpected expanding blasting of liquid that graphite layers is saturated, causes graphite wafer to be separated into single-layer wafers, namely produces Graphene.
S5, collection Graphene.
In S1, the volume ratio of described graphite and described liquid nitrogen is 1:3.
In S3, the speed of described heating is at the uniform velocity.
Described penetration aid is hydrogen peroxide.
In S3, after heating, make reacting kettle inner pressure between 3.4～40.0MPa.
Implementation as said method is more optimized:
S1, admixed graphite, liquid nitrogen and penetration aid, in reactor, form homogeneous mixture；
Graphite porosity 75%, with 1:3 ratio admixed graphite and liquid nitrogen, distilled water or hydrogen peroxide isoperm is strong, the coefficient of expansion big, the liquid of easily diffusion, under high pressure make the liquids such as liquid nitrogen, distilled water or hydrogen peroxide be fully infiltrated into graphite wafer interlayer, make mixture.
S2, closed reaction still；
S3, heat described mixture；
The mixture constant-speed heating of the liquids such as saturated liquid nitrogen, distilled water or hydrogen peroxide, intrinsic pressure to increase；
S4, expose described mixture at ambient pressure；
Suddenly decompression exposes described mixture at ambient pressure, so that the unexpected expanding blasting of liquid that graphite layers is saturated, causes graphite wafer to be separated into single-layer wafers, namely produces Graphene.
S5, collection Graphene.
In S1, the volume ratio of described graphite and described liquid nitrogen is 1:3.
In S3, the speed of described heating is at the uniform velocity.
Described penetration aid is hydrogen peroxide.
In S3, after heating, making reacting kettle inner pressure to 40.0MPa, heating temperatures is to 400 DEG C.
40.0MPa supercritical pressure when being add hydrothermal solution to 400 DEG C, it also it is the safe pressure of heating autoclave.The fluid of above-critical state has better mass-transfer performance, it is possible to more quick by graphite infiltration.
As it is shown in figure 1, a kind of equipment of High Temperature High Pressure decrepitation method realizing producing Graphene, including autoclave 3 and at least two-stage pressure-bearing collecting hood；
Described pressure-bearing collecting hood is the barrel-like structure of open-top, and at least the described pressure-bearing collecting hood of two-stage is arranged with one heart, and described autoclave 3 is positioned at the center of described collecting hood；Described autoclave 3 is provided with attemperating unit and pressure control device.
Described autoclave 3 includes pressure reducing sleeve 1, temperature and pressure inner bag 2 two parts；
Described temperature and pressure inner bag 2 is embedded inside described pressure reducing sleeve 1, is rotatably connected with described pressure reducing sleeve 1；Described temperature and pressure inner bag 2 is provided with heating wire.
At least one mutually corresponding discharge opening 6 is all offered on described pressure reducing sleeve 1, on described temperature and pressure inner bag 22.
The outside of described pressure reducing sleeve 1 is equipped with ring gear 8, and the side of described ring gear 8 is provided with the driving gear 7 cooperated with described ring gear 8, and described driving gear 7 is fixing with the outfan of motor to be connected.
The top of described pressure-bearing collecting hood is provided with collected overhead cover 9, and described collected overhead cover 9 is the ring wall tilted to described collecting hood center.
As shown in fig. 1, pressure-bearing collecting hood includes the first pressure-bearing collecting hood 4 and the second pressure-bearing collecting hood 5, and two pressure-bearing collecting hoods are nested together each other, are provided with distilled water between two pressure-bearing mobile phone covers, for the Graphene of mobile phone ejection.
Above one embodiment of the present of invention is described in detail, but described content has been only presently preferred embodiments of the present invention, it is impossible to be considered the practical range for limiting the present invention.All equalizations made according to the present patent application scope change and improvement etc., all should still belong within the patent covering scope of the present invention.
Claims (10)
1. the High Temperature High Pressure decrepitation method being used for producing Graphene, it is characterised in that:
S1, admixed graphite, liquid nitrogen and penetration aid, in reactor, form homogeneous mixture；
S2, closed reaction still；
S3, heat described mixture；
S4, expose described mixture at ambient pressure；
S5, collection Graphene.
2. the High Temperature High Pressure decrepitation method of production Graphene according to claim 1, it is characterised in that: in S1, the volume ratio of described graphite and described liquid nitrogen is 1:3.
3. the High Temperature High Pressure decrepitation method of production Graphene according to claim 2, it is characterised in that: in S3, the speed of described heating is at the uniform velocity.
4. the High Temperature High Pressure decrepitation method of production Graphene according to claim 3, it is characterised in that: described penetration aid is the liquefied mixture of hydrogen peroxide and water.
5. the High Temperature High Pressure decrepitation method of production Graphene according to claim 4, it is characterised in that: in S3, after heating, make reacting kettle inner pressure between 3.4～40.0MPa.
6. the High Temperature High Pressure decrepitation method of production Graphene according to claim 4, it is characterised in that: when reacting kettle inner pressure is 40MPa, temperature in the kettle controls at 400 DEG C.
7. according to claim 1 a kind of for realizing producing the equipment of High Temperature High Pressure decrepitation method of Graphene, it is characterised in that: include autoclave and at least two-stage pressure-bearing collecting hood；
Described pressure-bearing collecting hood is the barrel-like structure of open-top, and at least the described pressure-bearing collecting hood of two-stage is arranged with one heart, and described autoclave is positioned at the center of described collecting hood；
Described autoclave is provided with attemperating unit and pressure control device.
8. according to claim 7 a kind of for realizing producing the equipment of the High Temperature High Pressure decrepitation method of Graphene, it is characterised in that:
Described autoclave includes pressure reducing sleeve, temperature and pressure inner bag two parts；
Described temperature and pressure inner bag is embedded inside described pressure reducing sleeve, is rotatably connected with described pressure reducing sleeve；Described temperature and pressure inner bag is provided with heating wire.
At least one mutually corresponding discharge opening is all offered on described pressure reducing sleeve, on described temperature and pressure inner bag.
9. according to claim 7 a kind of for realizing producing the equipment of the High Temperature High Pressure decrepitation method of Graphene, it is characterized in that: the outside of described pressure reducing sleeve is equipped with ring gear, the side of described ring gear is provided with the driving gear cooperated with described ring gear, and described driving gear is fixing with the outfan of motor to be connected.
10. according to claim 8 a kind of for realizing producing the equipment of the High Temperature High Pressure decrepitation method of Graphene, it is characterised in that:
The top of described collecting hood is provided with collected overhead cover, and described collected overhead cover is the ring wall tilted to described collecting hood center.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106744881A (en) * | 2016-12-27 | 2017-05-31 | 成都新柯力化工科技有限公司 | A kind of method that utilization ultrasonic continuous prepare Graphene |
| CN108394890A (en) * | 2017-02-06 | 2018-08-14 | 中金态和（武汉）石墨烯科技股份有限公司 | The method that compression ignition method prepares graphene |
| CN108622886A (en) * | 2017-03-17 | 2018-10-09 | 国家纳米科学中心 | A kind of liquid nitrogen auxiliary prepares the method for high-quality graphene and high-quality graphene obtained |
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| CN102491314A (en) * | 2011-11-24 | 2012-06-13 | 中国科学院化学研究所 | Method for preparing graphene |
| CN103787315A (en) * | 2013-12-26 | 2014-05-14 | 中山大学 | Preparation method of graphene sheets |
| KR20140112826A (en) * | 2013-03-14 | 2014-09-24 | 국립대학법인 울산과학기술대학교 산학협력단 | Expanded Graphite or Graphene Fabricated by Physical Process And Method for Fabricating the same |
| CN104843690A (en) * | 2015-04-30 | 2015-08-19 | 湖南元素密码石墨烯研究院（有限合伙） | Method for preparing graphene by means of steam explosion method |
| CN204699671U (en) * | 2015-06-11 | 2015-10-14 | 济宁学院 | Chemical laboratory reactor |
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Patent Citations (5)
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| CN102491314A (en) * | 2011-11-24 | 2012-06-13 | 中国科学院化学研究所 | Method for preparing graphene |
| KR20140112826A (en) * | 2013-03-14 | 2014-09-24 | 국립대학법인 울산과학기술대학교 산학협력단 | Expanded Graphite or Graphene Fabricated by Physical Process And Method for Fabricating the same |
| CN103787315A (en) * | 2013-12-26 | 2014-05-14 | 中山大学 | Preparation method of graphene sheets |
| CN104843690A (en) * | 2015-04-30 | 2015-08-19 | 湖南元素密码石墨烯研究院（有限合伙） | Method for preparing graphene by means of steam explosion method |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106744881A (en) * | 2016-12-27 | 2017-05-31 | 成都新柯力化工科技有限公司 | A kind of method that utilization ultrasonic continuous prepare Graphene |
| CN108394890A (en) * | 2017-02-06 | 2018-08-14 | 中金态和（武汉）石墨烯科技股份有限公司 | The method that compression ignition method prepares graphene |
| CN108622886A (en) * | 2017-03-17 | 2018-10-09 | 国家纳米科学中心 | A kind of liquid nitrogen auxiliary prepares the method for high-quality graphene and high-quality graphene obtained |
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