CN107585765A - A kind of preparation method of graphene or graphene oxide - Google Patents
A kind of preparation method of graphene or graphene oxide Download PDFInfo
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- CN107585765A CN107585765A CN201710945511.4A CN201710945511A CN107585765A CN 107585765 A CN107585765 A CN 107585765A CN 201710945511 A CN201710945511 A CN 201710945511A CN 107585765 A CN107585765 A CN 107585765A
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- graphene
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Abstract
The invention discloses the preparation method of a kind of graphene or graphene oxide to be：The preparation of graphene oxide：Reaction is mixed evenly in graphite raw material, solvent and oxidant mixed material, decompression, filters, after washing, carries out the vacuum drying and grinding of material；The graphite oxide olefinic substance of preparation adds reducing agent, reaction, heating, stirring, suspension separating-purifying is carried out after multiplicating, is positioned over ionized water drying；Dry graphene oxide and graphite olefinic substance is in drying process once again under certain temperature, and carry out the collection of later stage material.The preparation method of the graphene or graphene oxide; technique is simple and easily operated; the selection of supplementary material is relatively common; it is adapted to large-scale production; by further carrying out the interim time to its process, effect refines, and more its process is easy to grasp, using two-stage oxidation; ensure that effect is more preferable, obtain the graphene and graphene oxide of higher degree.
Description
Technical field
The present invention relates to the preparing technical field of graphene associated materials, specially a kind of graphene or graphene oxide
Preparation method.
Background technology
Graphene be it is a kind of only an atomic thickness two-dimentional carbon film, be people find so far it is unique one kind by individual layer
The material of atomic building, hexagonal network is connected into by chemical bond between carbon atom in carbon film, due to the chemical bond between carbon atom
It is made up of SP2 hybridized orbits, therefore graphene is very indomitable, possesses bent, electric conductivity is strong, mechanical strength is good, translucency is good etc.
The good characteristic that other new materials do not possess.Graphene possesses extraordinary electric conductivity, and resistivity very little, electronics can pole
Efficiently migrate, this respect performance is more much higher than traditional conductor and semiconductor；Electronics is migrated in graphene in the absence of electricity
The collision of son and atom, can greatly reduce energy loss；Graphene possesses fabulous translucency, but airtight, Ke Yiyong
To develop protective layer material of new generation, and can be used for developing transparent electron product and wearable electronic product.
The preparation method of graphene product is various, but some drawbacks be present, is difficult to control especially in preparation process
Product quality and yield, the change of the processing conditions slight variation such as temperature and time in production process, the matter of product will be given
Amount and yield bring very big influence, and therefore, it is difficult to realize prepare with scale.
The content of the invention
It is an object of the invention to provide the preparation method of a kind of graphene or graphene oxide, to solve above-mentioned background skill
The problem of being proposed in art.
To achieve the above object, the present invention provides following technical scheme：A kind of preparation side of graphene or graphene oxide
The preparation process of method, described graphene or graphene oxide is：
（1）, graphene oxide preparation：Reaction is mixed evenly in graphite raw material, solvent and oxidant mixed material, is subtracted
Pressure, filter, after washing, carry out the vacuum drying and grinding of material；
（2）, re-oxidation process：Will（1）The graphite oxide olefinic substance of middle preparation adds reducing agent, and reaction, heating, stirring are more
Suspension separating-purifying is carried out after secondary repetition, is positioned over ionized water drying；
（3）, oxidation-reduction process：Will（2）In ionized water in dry graphene experience washing and dry；
（4）, redrying collect：Will（3）In drying graphene oxide and graphite olefinic substance be under certain temperature and do once again
Dry processing, and carry out the collection of later stage material.
Preferably, in graphene oxide preparation process（1）In mixing temperature range be 50-100 DEG C, and stir anti-
It is 2-4h between seasonable.
Preferably, in graphene oxide preparation process（2）In reaction time be 2-3h, temperature rises to 25-35 by 0-2 DEG C
DEG C, the stirring reaction time is 1-2h after heating.
Preferably, in graphene oxide preparation process（4）In certain temperature be 25-30 DEG C, and the collection ring of dried object
Border is germ-free condition.
Preferably, in graphene oxide preparation process（2）Centrifugal separation method is taken in middle suspension separation, and centrifugal rotational speed is
4800-6500r/min, and the time for carrying out continuous centrifugal rotation is 4-10min.
Preferably, in graphene oxide preparation process（2）Constituent is NaOH, KOH and hydrazine hydrate inside middle reducing agent.
Preferably, graphene oxide preparation process（2）Middle purification purity value scope is 88%-98%.
Compared with prior art, the beneficial effects of the invention are as follows：The preparation method of the graphene or graphene oxide, technique
Simple and easily operated, the selection of supplementary material is relatively common, is adapted to large-scale production, by further being carried out to its process
The time of stage, effect refinement, more are easy to grasp to its process, using two-stage oxidation, ensure that effect is more preferable, obtain higher
The graphene and graphene oxide of purity.
Embodiment
It is clearly and completely described below in conjunction with the technical scheme in the embodiment of the present invention, it is clear that described reality
It is only part of the embodiment of the present invention to apply example, rather than whole embodiments.It is general based on the embodiment in the present invention, this area
The every other embodiment that logical technical staff is obtained under the premise of creative work is not made, belong to what the present invention protected
Scope.
, it is necessary to explanation in description of the invention, the orientation of instruction such as term " vertical ", " on ", " under ", " level " or
Person's position relationship is for only for ease of the description present invention and simplifies description, rather than instruction either implies signified device or member
Part must have specific orientation, with specific azimuth configuration and operation, therefore be not considered as limiting the invention.This
Outside, " first ", " second ", " the 3rd ", " the 4th " are only used for describing purpose, and it is not intended that indicating or implying relatively important
Property.In description of the invention, it is also necessary to explanation, unless otherwise clear and definite regulation and limitation, term " setting ", " installation ",
" connected ", " connection ", it should be interpreted broadly, for example, it may be connecting or being fixedly connected or detachably connect
Connect, or integrally connected, it can be mechanical connection or electrical connection, can be directly connected to or by middle matchmaker
It is situated between and is connected, can is the connection of two element internals.For the ordinary skill in the art, can be as the case may be
Understand the concrete meaning of above-mentioned term in the present invention.
The present invention provides a kind of technical scheme：A kind of preparation method of graphene or graphene oxide, described graphene
Or the preparation process of graphene oxide is：
（1）, graphene oxide preparation：Reaction is mixed evenly in graphite raw material, solvent and oxidant mixed material, is subtracted
Pressure, filter, after washing, carry out the vacuum drying and grinding of material；
（2）, re-oxidation process：Will（1）The graphite oxide olefinic substance of middle preparation adds reducing agent, and reaction, heating, stirring are more
Suspension separating-purifying is carried out after secondary repetition, is positioned over ionized water drying；
（3）, oxidation-reduction process：Will（2）In ionized water in dry graphene experience washing and dry；
（4）, redrying collect：Will（3）In drying graphene oxide and graphite olefinic substance be under certain temperature and do once again
Dry processing, and carry out the collection of later stage material.
Preferably, in graphene oxide preparation process（1）In mixing temperature range be 50-100 DEG C, and stir anti-
It is 2-4h between seasonable.
Preferably, in graphene oxide preparation process（2）In reaction time be 2-3h, temperature rises to 25-35 by 0-2 DEG C
DEG C, the stirring reaction time is 1-2h after heating.
Preferably, in graphene oxide preparation process（4）In certain temperature be 25-30 DEG C, and the collection ring of dried object
Border is germ-free condition.
Preferably, in graphene oxide preparation process（2）Centrifugal separation method is taken in middle suspension separation, and centrifugal rotational speed is
4800-6500r/min, and the time for carrying out continuous centrifugal rotation is 4-10min.
Preferably, in graphene oxide preparation process（2）Constituent is NaOH, KOH and hydrazine hydrate inside middle reducing agent.
Preferably, graphene oxide preparation process（2）Middle purification purity value scope is 88%-98%.
The preparation method of the graphene or graphene oxide, technique is simple and easily operated, and the selection of supplementary material is compared
It is common, it is adapted to large-scale production, by further carrying out the interim time to its process, effect refines, more to its mistake
Journey is easy to grasp, and using two-stage oxidation, ensures that effect is more preferable, obtains the graphene and graphene oxide of higher degree.
Although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with
A variety of changes, modification can be carried out to these embodiments, replace without departing from the principles and spirit of the present invention by understanding
And modification, the scope of the present invention is defined by the appended.
Claims (7)
- A kind of 1. preparation method of graphene or graphene oxide, it is characterised in that：Described graphene or graphene oxide Preparation process is：, graphene oxide preparation：Reaction is mixed evenly in graphite raw material, solvent and oxidant mixed material, depressurizes, take out After filter, washing, the vacuum drying and grinding of material are carried out；, re-oxidation process：Will（1）The graphite oxide olefinic substance of middle preparation adds reducing agent, reaction, heating, stirring, multiple weight Suspension separating-purifying is carried out after multiple, is positioned over ionized water drying；, oxidation-reduction process：Will（2）In ionized water in dry graphene experience washing and dry；, redrying collect：Will（3）In drying graphene oxide and graphite olefinic substance be under certain temperature once again dry at Reason, and carry out the collection of later stage material.
- 2. the preparation method of a kind of graphene according to claim 1 or graphene oxide, it is characterised in that：Graphite oxide In alkene preparation process（1）In mixing temperature range be 50-100 DEG C, and the stirring reaction time is 2-4h.
- 3. the preparation method of a kind of graphene according to claim 1 or graphene oxide, it is characterised in that：Graphite oxide In alkene preparation process（2）In reaction time be 2-3h, temperature rises to 25-35 DEG C by 0-2 DEG C, after heating the stirring reaction time be 1-2h。
- 4. the preparation method of a kind of graphene according to claim 1 or graphene oxide, it is characterised in that：Graphite oxide In alkene preparation process（4）In certain temperature be 25-30 DEG C, and the collection environment of dried object is germ-free condition.
- 5. the preparation method of a kind of graphene according to claim 1 or graphene oxide, it is characterised in that：Graphite oxide In alkene preparation process（2）Centrifugal separation method, centrifugal rotational speed 4800-6500r/min are taken in middle suspension separation, and are connected The time of continuous centrifugal rotation is 4-10min.
- 6. the preparation method of a kind of graphene according to claim 1 or graphene oxide, it is characterised in that：Graphite oxide In alkene preparation process（2）Constituent is NaOH, KOH and hydrazine hydrate inside middle reducing agent.
- 7. the preparation method of a kind of graphene according to claim 1 or graphene oxide, it is characterised in that：Graphite oxide Alkene preparation process（2）Middle purification purity value scope is 88%-98%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201710945511.4A CN107585765A (en) | 2017-10-12 | 2017-10-12 | A kind of preparation method of graphene or graphene oxide |
Applications Claiming Priority (1)
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| CN201710945511.4A CN107585765A (en) | 2017-10-12 | 2017-10-12 | A kind of preparation method of graphene or graphene oxide |
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| CN201710945511.4A Pending CN107585765A (en) | 2017-10-12 | 2017-10-12 | A kind of preparation method of graphene or graphene oxide |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101575095A (en) * | 2009-05-26 | 2009-11-11 | 北京大学 | Method for preparing graphene |
| CN104386679A (en) * | 2014-11-13 | 2015-03-04 | 苏州经贸职业技术学院 | Method for preparing graphene oxide and graphene |
-
2017
- 2017-10-12 CN CN201710945511.4A patent/CN107585765A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101575095A (en) * | 2009-05-26 | 2009-11-11 | 北京大学 | Method for preparing graphene |
| CN104386679A (en) * | 2014-11-13 | 2015-03-04 | 苏州经贸职业技术学院 | Method for preparing graphene oxide and graphene |
Non-Patent Citations (1)
| Title |
|---|
| XIAOBIN FAN ET AL.: "Deoxygenation of exfoliated graphite oxide under alkaline conditions:A green route to graphene preparation", 《ADVANCED MATERIALS》 * |
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Application publication date: 20180116 |