CN110194449A - A method of graphene is prepared using graphene quantum dot mechanical stripping - Google Patents

A method of graphene is prepared using graphene quantum dot mechanical stripping Download PDF

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Publication number
CN110194449A
CN110194449A CN201910393605.4A CN201910393605A CN110194449A CN 110194449 A CN110194449 A CN 110194449A CN 201910393605 A CN201910393605 A CN 201910393605A CN 110194449 A CN110194449 A CN 110194449A
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CN
China
Prior art keywords
graphene
raw material
quantum dot
solution
mechanical stripping
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CN201910393605.4A
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Chinese (zh)
Inventor
王群力
王平
王江
张伟
俞祖英
王洪杰
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SICHUAN OUXUN ENERGY ENGINEERING TECHNOLOGY Co Ltd
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SICHUAN OUXUN ENERGY ENGINEERING TECHNOLOGY Co Ltd
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Priority to CN201910393605.4A priority Critical patent/CN110194449A/en
Publication of CN110194449A publication Critical patent/CN110194449A/en
Pending legal-status Critical Current

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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00Carbon; Compounds thereof
    • C01B32/15Nano-sized carbon materials
    • C01B32/182Graphene
    • C01B32/184Preparation
    • C01B32/19Preparation by exfoliation

Abstract

The invention discloses a kind of methods for preparing graphene using graphene quantum dot mechanical stripping, the following steps are included: graphene raw material is taken to be slowly added in 30% sodium bicarbonate solution, after stirring 1h -2h, graphene raw material is taken out and is cleaned using clear water, it is polished using edges and corners of the grinding device to graphene raw material, the graphene particles after polishing are collected simultaneously, the beneficial effects of the present invention are: the invention is a kind of method for preparing graphene using graphene quantum dot mechanical stripping, it is lower to solve controllability in the prior art, it is difficult to realize the problem of synthesizing on a large scale, using the new process to graphene oxide solution temperature test, and original graphene raw material is polished, again resulting particle is used to test, save raw material, improve product yield and production efficiency, substantially increase production capacity, Reduce costs, can mass production, benefit is evident.

Description

A method of graphene is prepared using graphene quantum dot mechanical stripping
Technical field
The present invention relates to a kind of difenoconazole purifying techniques, specially a kind of to utilize graphene quantum dot mechanical stripping system The method of standby graphene.
Background technique
Graphene have excellent optics, electricity, mechanical characteristic, materialogy, micro-nano technology, the energy, biomedicine and Drug delivery etc. is with important application prospects, it is considered to be a kind of future revolutionary material.Mechanical stripping method is benefit With the friction and relative motion between object and graphene, the method for obtaining graphene layer material.This method is easy to operate, Obtained graphene generally remains complete crystal structure.2004, two scientifical use adhesive tapes of Britain were to natural stone Ink carries out the method that removing obtains graphene layer by layer, is also classified as mechanical stripping method.
It is low that original this method had once been considered production efficiency, can not industrial volume production.Although this method can be prepared The graphene of micron size, but its controllability is lower, it is difficult to realize extensive synthesis, while resulting graphene can generate greatly The waste of amount.
Summary of the invention
The purpose of the present invention is to provide a kind of methods for preparing graphene using graphene quantum dot mechanical stripping, with solution Certainly the problems mentioned above in the background art.
The purpose of the present invention is be achieved by following technical proposals: a kind of to utilize graphene quantum dot mechanical stripping system The method of standby graphene, comprising the following steps:
1) it takes graphene raw material to be slowly added in 30% sodium bicarbonate solution, after stirring 1h -2h, graphene raw material is taken out and is used Clear water is cleaned, and is polished using edges and corners of the grinding device to graphene raw material, while to the graphene after polishing Grain is collected.
2) the graphene particles 10g after taking step 1) to polish is placed in 5% ammonium hydroxide, forms it into the oxygen of 0.25g/L ~ 1g/L Graphite alkene solution, while putting it into high-voltaghe compartment, reuses ultrasonic wave and is separated, and high-voltaghe compartment be warming up to 100 DEG C with On, and internal air pressure keeps its constant by adjusting, and keeps 0.5h, then again carries out graphene solution placement 1h -1.5h cold But, the extrudate and record in its solution are observed at different temperature.
3) take the temperature recorded in step 2 by calculating the high temperature production of selection yield, by the graphite after polishing Alkene raw material is decomposed using press machine, then it is uniformly layered on parcel shelf, is carried out in the environment of 100 DEG C -110 DEG C Then heating is cooled to room temperature and stands 0.5h, then heated in the environment of being warming up to 120 DEG C -130 DEG C, then internally lead to Enter HCL gas, stand 1h and be discharged, is finally down to normal temperature and pressure again, it will be resulting swollen using filter and resonance device Change product separation.
4) it takes step 3) to obtain resulting extruding product 10kg and alcoholic solution 2kg mixing, fills it using agitating device Divide mixing, then cool to -5 DEG C~0 DEG C, stand 1.5h, then extra alcoholic solution is discharged by filter, up to solid Body is precipitated, then is passed through clear water into solid and reaches room temperature, solid is successively washed and dried acquisition finished product.
HCL gas concentration in the step 3) is 45%, and HCL gas can also be used ammonia to be replaced.
The beneficial effects of the present invention are: the invention is a kind of side for preparing graphene using graphene quantum dot mechanical stripping It is lower to solve controllability in the prior art for method, it is difficult to the problem of realizing extensive synthesis, using to graphene oxide solution temperature The new process of test is spent, and original graphene raw material is polished, then resulting particle is used to test, raw material is saved, mentions High product yield and production efficiency, substantially increase production capacity, reduce costs, can mass production, benefit is evident.
Specific embodiment
Further instruction With reference to embodiment, but following detailed description should not be done and be managed Solution is the limitation invented ontology.Those of ordinary skill in the art can apparently make various on the basis of the present invention Change and change, it should within the scope of invention.
Embodiment 1:
A method of graphene is prepared using graphene quantum dot mechanical stripping, comprising the following steps:
1) it takes graphene raw material to be slowly added in 30% sodium bicarbonate solution, after stirring 1h -2h, graphene raw material is taken out and is used Clear water is cleaned, and is polished using edges and corners of the grinding device to graphene raw material, while to the graphene after polishing Grain is collected.
2) the graphene particles 10g after taking step 1) to polish is placed in 5% ammonium hydroxide, forms it into the oxygen of 0.25g/L ~ 1g/L Graphite alkene solution, while putting it into high-voltaghe compartment, reuses ultrasonic wave and is separated, and high-voltaghe compartment be warming up to 100 DEG C with On, and internal air pressure keeps its constant by adjusting, and keeps 0.5h, then again carries out graphene solution placement 1h -1.5h cold But, the extrudate and record in its solution are observed at different temperature.
3) take the temperature recorded in step 2 by calculating the high temperature production of selection yield, by the graphite after polishing Alkene raw material is decomposed using press machine, then it is uniformly layered on parcel shelf, is carried out in the environment of 100 DEG C -110 DEG C Then heating is cooled to room temperature and stands 0.5h, then heated in the environment of being warming up to 120 DEG C -130 DEG C, then internally lead to Enter HCL gas, stand 1h and be discharged, is finally down to normal temperature and pressure again, it will be resulting swollen using filter and resonance device Change product separation.
4) it takes step 3) to obtain resulting extruding product 10kg and alcoholic solution 2kg mixing, fills it using agitating device Divide mixing, then cool to -5 DEG C~0 DEG C, stand 1.5h, then extra alcoholic solution is discharged by filter, up to solid Body is precipitated, then is passed through clear water into solid and reaches room temperature, solid is successively washed and dried acquisition finished product.
HCL gas concentration in the step 3) is 45%, and HCL gas can also be used ammonia to be replaced.
Embodiment 2:
A method of graphene is prepared using graphene quantum dot mechanical stripping, comprising the following steps:
1) it takes graphene raw material to be slowly added in 50% sodium bicarbonate solution, after stirring 1h -1.5h, graphene raw material taking-up is made It is cleaned, is polished using edges and corners of the grinding device to graphene raw material, while to the graphene after polishing with clear water Particle is collected.
2) the graphene particles 20g after taking step 1) to polish is placed in 10% ammonium hydroxide, forms it into the oxygen of 0.25g/L ~ 1g/L Graphite alkene solution, while putting it into high-voltaghe compartment, reuses ultrasonic wave and is separated, and high-voltaghe compartment be warming up to 100 DEG C with On, and internal air pressure keeps its constant by adjusting, and keeps 0.5h, then again carries out graphene solution placement 1h -1.5h cold But, the extrudate and record in its solution are observed at different temperature.
3) take the temperature recorded in step 2 by calculating the high temperature production of selection yield, by the graphite after polishing Alkene raw material is decomposed using press machine, then it is uniformly layered on parcel shelf, is carried out in the environment of 130 DEG C -140 DEG C Then heating is cooled to room temperature and stands 0.5h, then heated in the environment of being warming up to 140 DEG C -150 DEG C, then internally lead to Enter HCL gas, stand 1h and be discharged, is finally down to normal temperature and pressure again, it will be resulting swollen using filter and resonance device Change product separation.
4) it takes step 3) to obtain resulting extruding product 20kg and alcoholic solution 4kg mixing, fills it using agitating device Divide mixing, then cool to -5 DEG C~0 DEG C, stand 1.5h, then extra alcoholic solution is discharged by filter, up to solid Body is precipitated, then is passed through clear water into solid and reaches room temperature, solid is successively washed and dried acquisition finished product.
HCL gas concentration in the step 3) is 35%, and HCL gas can also be used ammonia to be replaced.
Above description is only the preferred embodiment of the application and the explanation to institute's application technology principle.Those skilled in the art Member is it should be appreciated that invention scope involved in the application, however it is not limited to technology made of the specific combination of above-mentioned technical characteristic Scheme, while should also cover in the case where not departing from the inventive concept, it is carried out by above-mentioned technical characteristic or its equivalent feature Any combination and the other technical solutions formed.Such as features described above has similar function with (but being not limited to) disclosed herein Can technical characteristic replaced mutually and the technical solution that is formed.

Claims (2)

1. a kind of method for preparing graphene using graphene quantum dot mechanical stripping, which comprises the following steps:
1) it takes graphene raw material to be slowly added in 30% sodium bicarbonate solution, after stirring 1h -2h, graphene raw material is taken out and is used Clear water is cleaned, and is polished using edges and corners of the grinding device to graphene raw material, while to the graphene after polishing Grain is collected;
2) the graphene particles 10g after taking step 1) to polish is placed in 5% ammonium hydroxide, forms it into the oxidation stone of 0.25g/L ~ 1g/L Black alkene solution, while putting it into high-voltaghe compartment, reuses ultrasonic wave and is separated, and high-voltaghe compartment is warming up to 100 DEG C or more, and Internal air pressure keeps its constant by adjusting, and keeps 0.5h, then again cools down graphene solution placement 1h -1.5h, The extrudate and record in its solution are observed at a temperature of different;
3) take the temperature recorded in step 2 by calculating the high temperature production of selection yield, the graphene after polishing is former Material is decomposed using press machine, then it is uniformly layered on parcel shelf, is heated in the environment of 100 DEG C -110 DEG C, Then it is cooled to room temperature and stands 0.5h, then heated in the environment of being warming up to 120 DEG C -130 DEG C, be then internally passed through HCL Gas stands 1h and is simultaneously discharged, is finally down to normal temperature and pressure again, using filter and resonance device by resulting extruding product Separation;
4) it takes step 3) to obtain resulting extruding product 10kg and alcoholic solution 2kg mixing, keeps it sufficiently mixed using agitating device It closes, then cools to -5 DEG C~0 DEG C, stand 1.5h, then extra alcoholic solution is discharged by filter, until solid is analysed Out, then into solid it is passed through clear water and reaches room temperature, solid is successively washed and dried acquisition finished product.
2. a kind of method for preparing graphene using graphene quantum dot mechanical stripping as described in claim 1, feature exist In the HCL gas concentration in the step 3) is 45%, and HCL gas can also be used ammonia to be replaced.
CN201910393605.4A 2019-05-13 2019-05-13 A method of graphene is prepared using graphene quantum dot mechanical stripping Pending CN110194449A (en)

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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103935999A (en) * 2014-05-09 2014-07-23 中国科学院上海微系统与信息技术研究所 Preparation method of graphene
CN103950928A (en) * 2014-05-22 2014-07-30 苏州斯迪克新材料科技股份有限公司 Preparation method of graphene
CN105399090A (en) * 2015-12-22 2016-03-16 成都新柯力化工科技有限公司 Graphene preparation method by using graphene quantum point mechanical stripping
CN105439133A (en) * 2015-12-18 2016-03-30 浙江理工大学 Preparation method of electronegative monolayer graphene
WO2016045023A1 (en) * 2014-09-25 2016-03-31 深圳粤网节能技术服务有限公司 Method for grading and separating graphene material
US20160200581A1 (en) * 2013-08-21 2016-07-14 Hanwha Chemical Corporation Graphene, method and apparatus for preparing graphene

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20160200581A1 (en) * 2013-08-21 2016-07-14 Hanwha Chemical Corporation Graphene, method and apparatus for preparing graphene
CN103935999A (en) * 2014-05-09 2014-07-23 中国科学院上海微系统与信息技术研究所 Preparation method of graphene
CN103950928A (en) * 2014-05-22 2014-07-30 苏州斯迪克新材料科技股份有限公司 Preparation method of graphene
WO2016045023A1 (en) * 2014-09-25 2016-03-31 深圳粤网节能技术服务有限公司 Method for grading and separating graphene material
CN105439133A (en) * 2015-12-18 2016-03-30 浙江理工大学 Preparation method of electronegative monolayer graphene
CN105399090A (en) * 2015-12-22 2016-03-16 成都新柯力化工科技有限公司 Graphene preparation method by using graphene quantum point mechanical stripping

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Application publication date: 20190903