CN105439135A - Method for preparing graphene from lignin - Google Patents
Method for preparing graphene from lignin Download PDFInfo
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Abstract
The invention discloses a method for preparing graphene from lignin. The method comprises steps as follows: a, lignin and aqueous alkali are mixed in a volume ratio of solid to liquid being 1:(5-10), the solution is heated to the temperature of 70-100 DEG C, and the insulation treatment time is 1-3 h; b, a material treated by alkali is filtered and washed, an obtained solid is dried at the temperature of 60-80 DEG C, and pretreated lignin is obtained; c, a catalyst is added to the pretreated lignin obtained in Step b, the mixture is fully mixed by a high-pressure homogenizer, non-homogenous lignin is homogenized and split, and cracked carbon and the catalyst are homogenized to be in a high energy obtaining state; d, the mixture is placed in an autoclave, inert gas is introduced, the pressure is increased at the speed of 0.1-1 MPa/s to 20-50 MPa, the mixture is heated to 500-800 DEG C and cooled to the normal temperature and pressure after being treated, and graphene is obtained. The lignin is decomposed at the high temperature and under the high pressure, high-energy carbon atoms are obtained, graphene grows under the action of the catalyst, with the adoption of the method, the preparation temperature of the graphene is reduced, and the preparation technology is simple, economical, environment-friendly and suitable for industrial production.
Description
Technical field
The present invention relates to technical field of nanometer material preparation, particularly a kind of graphene preparation method.
Background technology
Within 2004, grapheme material is successfully prepared, and has caused the upsurge of a new ripple carbon materials research since then.The planar carbon nano material that Graphene is made up of one deck carbon atom, be the thinnest known two-dimensional material at present, its thickness is only 0.335nm, and it is made up of hexagonal lattice.Connected by σ key between carbon atom in Graphene, impart the extremely excellent mechanical property of Graphene and structure rigidity.And in Graphene, each carbon atom has the p electronics of a non-Cheng Jian, and these p electronics can move freely in crystal, and movement velocity is up to 1/300 of the light velocity, impart the electroconductibility that Graphene is good.In optics, Graphene is almost completely transparent, only absorbs the light of 2.3%.By means of these peculiar mechanics, electrical and optical properties, Graphene has very vast potential for future development.
In order to allow outstanding grapheme material realize suitability for industrialized production and application, a kind of can be mass-produced and the number of plies and the controlled preparation method of size just must be developed.The preparation method of current Graphene has mechanical stripping method, epitaxial growth method, oxidation reduction process, ultrasonic stripping method, organic synthesis method, solvent-thermal method, chemical Vapor deposition process etc.In these methods, in these methods, mechanically peel method and epitaxial growth method preparation efficiency very low, be difficult to satisfied large-scale needs.Although chemical Vapor deposition process can obtain large size continuous print graphene film, be applicable to electron device or transparent conductive film, the demand of scale operation can not be met.Oxidation reduction process is prepared the with low cost of grapheme material powder and is easily realized, but can produce a large amount of waste liquids, causes severe contamination to environment, limits the extensive industrialized development of Graphene.These methods are all using graphite ore as former material, and this Mineral resources are not recyclable regeneratives, are unfavorable for the scale operation of Graphene.
Xylogen is a kind of natural reproducible resource, has many excellent properties, has high potential using value in modern chemical industry.Its output is huge, but application is extremely low.Analyze from its chemical composition, in xylogen nearly 65% carbon, have great potential preparing in carbon material.
It take xylogen as the method that Graphene prepared by raw material that China Patent Publication No. 103466613A discloses a kind of.First the porcelain example boat that xylogen and catalyzer are housed is put into hinge tube furnace by the method; at the uniform velocity pass into inert protective gas; in stove, with constant temperature rise rate, sample is heated to target temperature from room temperature simultaneously; and keep under target temperature; when sample temperature is down to room temperature; sample is taken out, after deionized water wash, vacuum filtration, oven drying at low temperature, obtains Graphene.Preparation technology of the present invention is easy, and gained quality of graphene is excellent, and productive rate is considerable.But the method adopts anaerobic sintering, and sintering temperature reaches 1500 DEG C, high to equipment requirements, and equipment preparation cost improves, and can not be applied to scale operation.
China Patent Publication No. 103935986A discloses a kind of method preparing Graphene with biological carbon source material high yield, comprise the steps: that biological carbon source material joins in acid solution after microwave treatment, again through washing, drying treatment, obtain pretreated biological carbon source material; By pretreated biological carbon source material and catalyst mix, 600-1600 DEG C, shielding gas exist under calcine 1-12h, obtain described Graphene after cooling.The method significantly reduces production cost, achieves the large-scale industrial production of Graphene.But used some noble metal catalysts in the method, not only cost improves, and the Graphene area of preparation is little, and crystallization is poor, is unfavorable for the industrialized development of Graphene.
In sum, now existing utilize xylogen to prepare in the method for Graphene also not have a kind of particular requirement be there is no to production unit, be applicable to scale operation, the preparation method of low production cost.
Summary of the invention
In order to solve deficiency and the defect of aforesaid method, the present invention develops a kind of method utilizing xylogen to prepare Graphene, adopts High Temperature High Pressure to decompose xylogen, obtains high-octane carbon atom, growing graphene under the effect of catalyzer.The invention provides aforesaid method and not only reduce Graphene preparation temperature, and preparation process is simple, economic environmental protection, is suitable for industrial production.
The invention provides a kind of method utilizing xylogen to prepare Graphene, it is characterized in that, said method comprising the steps of:
A. be 1:5-10 by xylogen with alkaline solution mixing solid-liquid volume ratio, heated solution temperature is to 70-100 DEG C, and the isothermal holding time is 1-3 hour;
B. the material after alkaline purification carried out filtering, wash and obtain solid and liquid, solid drying at 60-80 DEG C is obtained pre-treatment xylogen;
C. catalyzer is added by the pre-treatment xylogen of b step gained, high pressure homogenizer is utilized fully to mix, clarifixator up time pressure reaches 20-100MPa, material is by after high-pressure homogeneous nozzle head-on collision, collect the homogenizing valve flowing to slit, make non-homogeneous xylogen homogenizing and cracking, make cracking carbon and catalyzer homogenizing be in acquisition higher-energy state;
D. the mixture obtained in step c is put into autoclave, pour rare gas element, pressure is increased to 20-50MPa with the speed of 0.1-1MPa/s, sample is heated to 500 DEG C-800 DEG C from room temperature with the fixing temperature rise rate of 30-60 DEG C/min by mixture, and keep 30-120min at this temperature, be down to normal temperature and pressure through process, obtain Graphene.
Preferably, described alkaline solution is the aqueous solution of at least one in sodium hydroxide, potassium hydroxide, ammoniacal liquor.
Preferably, described alkaline solution alkali charge is the 10-30% of the weight of xylogen.
Preferably, described catalyzer is at least one in iron powder, nickel powder, copper powder, nickelous nitrate, ferric oxide.
Preferably, described high pressure homogenizer operating pressure parameter is 80MPa.
Preferably, described rare gas element is at least one in argon gas, helium, nitrogen.
Above-mentioned one or more technical scheme in the embodiment of the present application, at least has one or more technique effects following:
1, the present invention adopts High Temperature High Pressure to decompose xylogen, obtains high-octane carbon atom, growing graphene under the effect of catalyzer.The invention provides aforesaid method and not only reduce Graphene preparation temperature, and preparation process is simple.
2, the present invention adopts plain metal and metal ion compound as catalyzer, and safety non-toxic is with low cost.
3, the present invention adopts xylogen as carbon source, draws materials extensively, is conducive to reducing production cost, is conducive in industrial production.
Embodiment
By embodiment, the present invention is described in further detail, but this should be interpreted as scope of the present invention is only limitted to following example.When not departing from aforesaid method thought of the present invention, the various replacement made according to ordinary skill knowledge and customary means or change, all should be within the scope of the present invention.
Embodiment one
The present embodiment comprises the steps:
Get 1kg xylogen and put into 10kg sodium hydroxide solution, containing sodium hydroxide quality in sodium hydroxide solution is 0.1kg, heated solution temperature to 70 DEG C, the isothermal holding time is 1 hour, is next carried out by the material after sodium hydroxide solution process filtering, washing the solid matter dry 20 hours acquisition pre-treatment xylogen at 60 DEG C obtained.12g iron powder is added by pre-treatment xylogen, high pressure homogenizer operating pressure is set to 20MPa, material is by after high-pressure homogeneous nozzle head-on collision, collect the homogenizing valve flowing to slit, make non-homogeneous xylogen homogenizing and cracking, cracking carbon and catalyzer homogenizing is made to be in acquisition higher-energy state, the abundant acquisition pretreated xylogen of mixing and iron mixture, the mixture of acquisition is put into autoclave, be filled with nitrogen, pressure is increased to 20MPa with the speed of 0.1MPa/s, mixture is heated to 500 DEG C with the fixing temperature rise rate of 30 DEG C/min from room temperature, and 30min is kept at 500 DEG C, normal temperature and pressure is down to through process, obtain Graphene.After testing, the mean thickness of the graphene sheet layer prepared in embodiment one is 0.82nm, and productive rate is 3.9%.
Embodiment two
The present embodiment comprises the steps:
Get 1kg xylogen and put into 10kg sodium hydroxide solution, containing sodium hydroxide quality in sodium hydroxide solution is 0.1kg, heated solution temperature to 70 DEG C, the isothermal holding time is 1 hour, is next carried out by the material after sodium hydroxide solution process filtering, washing the solid matter dry 20 hours acquisition pre-treatment xylogen at 60 DEG C obtained.100g iron powder is added by pre-treatment xylogen, high pressure homogenizer operating pressure is set to 20MPa, material is by after high-pressure homogeneous nozzle head-on collision, collect the homogenizing valve flowing to slit, make non-homogeneous xylogen homogenizing and cracking, cracking carbon and catalyzer homogenizing is made to be in acquisition higher-energy state, the abundant acquisition pretreated xylogen of mixing and iron mixture, the mixture of acquisition is put into autoclave, be filled with nitrogen, pressure is increased to 20MPa with the speed of 0.1MPa/s, mixture is heated to 500 DEG C with the fixing temperature rise rate of 30 DEG C/min from room temperature, and 30min is kept at 500 DEG C, normal temperature and pressure is down to through process, obtain Graphene.After testing, the mean thickness of the graphene sheet layer prepared in embodiment two is 0.72nm, and productive rate is 4.7%.
Embodiment three
The present embodiment comprises the steps:
Get 1kg xylogen and put into 10kg potassium hydroxide solution, containing potassium hydroxide quality in potassium hydroxide solution is 0.1kg, heated solution temperature to 85 DEG C, the isothermal holding time is 1 hour, is next carried out by the material after potassium hydroxide solution process filtering, washing the solid matter dry 20 hours acquisition pre-treatment xylogen at 60 DEG C obtained.100g iron powder is added by pre-treatment xylogen, high pressure homogenizer operating pressure is set to 40MPa, material is by after high-pressure homogeneous nozzle head-on collision, collect the homogenizing valve flowing to slit, make non-homogeneous xylogen homogenizing and cracking, cracking carbon and catalyzer homogenizing is made to be in acquisition higher-energy state, the abundant acquisition pretreated xylogen of mixing and iron mixture, the mixture of acquisition is put into autoclave, be filled with nitrogen, pressure is increased to 20MPa with the speed of 0.1MPa/s, mixture is heated to 500 DEG C with the fixing temperature rise rate of 30 DEG C/min from room temperature, and 30min is kept at 500 DEG C, normal temperature and pressure is down to through process, obtain Graphene.After testing, the mean thickness of the graphene sheet layer prepared in embodiment three is 0.58nm, and productive rate is 6.1%.
Embodiment four
The present embodiment comprises the steps:
Get 1kg xylogen and put into 10kg potassium hydroxide solution, containing potassium hydroxide quality in potassium hydroxide solution is 0.1kg, heated solution temperature to 85 DEG C, the isothermal holding time is 3 hours, is next carried out by the material after potassium hydroxide solution process filtering, washing the solid matter dry 10 hours acquisition pre-treatment xylogen at 80 DEG C obtained.80g nickel powder is added by pre-treatment xylogen, high pressure homogenizer operating pressure is set to 40MPa, material is by after high-pressure homogeneous nozzle head-on collision, collect the homogenizing valve flowing to slit, make non-homogeneous xylogen homogenizing and cracking, cracking carbon and catalyzer homogenizing is made to be in acquisition higher-energy state, the abundant acquisition pretreated xylogen of mixing and nickel powder mixture, the mixture of acquisition is put into autoclave, be filled with nitrogen, pressure is increased to 35MPa with the speed of 0.5MPa/s, mixture is heated to 600 DEG C with the fixing temperature rise rate of 50 DEG C/min from room temperature, and 60min is kept at 600 DEG C, normal temperature and pressure is down to through process, obtain Graphene.After testing, the mean thickness of the graphene sheet layer prepared in embodiment four is 0.78nm, and productive rate is 5.6%.
Embodiment five
The present embodiment comprises the steps:
Get 3kg xylogen and put into 10kg potassium hydroxide solution, containing potassium hydroxide quality in potassium hydroxide solution is 0.25kg, heated solution temperature to 100 DEG C, the isothermal holding time is 2 hours, is next carried out by the material after potassium hydroxide solution process filtering, washing the solid matter dry 15 hours acquisition pre-treatment xylogen at 80 DEG C obtained.10g nickelous nitrate powder will be added in pre-treatment xylogen, high pressure homogenizer operating pressure is set to 80MPa, material is by after high-pressure homogeneous nozzle head-on collision, collect the homogenizing valve flowing to slit, make non-homogeneous xylogen homogenizing and cracking, cracking carbon and catalyzer homogenizing is made to be in acquisition higher-energy state, the abundant acquisition pretreated xylogen of mixing and nickelous nitrate powdered mixture, the mixture of acquisition is put into autoclave, be filled with nitrogen, pressure is increased to 50MPa with the speed of 1MPa/s, mixture is heated to 800 DEG C with the fixing temperature rise rate of 60 DEG C/min from room temperature, and 120min is kept at 800 DEG C, normal temperature and pressure is down to through process, obtain Graphene.After testing, the mean thickness of the graphene sheet layer prepared in embodiment five is 0.68nm, and productive rate is 6.9%.
Embodiment six
The present embodiment comprises the steps:
Get 5kg xylogen and put into 10kg potassium hydroxide solution, containing potassium hydroxide quality in potassium hydroxide solution is 1.3kg, heated solution temperature to 100 DEG C, the isothermal holding time is 2 hours, is next carried out by the material after potassium hydroxide solution process filtering, washing the solid matter dry 15 hours acquisition pre-treatment xylogen at 80 DEG C obtained.50g nickel powder is added by pre-treatment xylogen, high pressure homogenizer operating pressure is set to 80MPa, material is by after high-pressure homogeneous nozzle head-on collision, collect the homogenizing valve flowing to slit, make non-homogeneous xylogen homogenizing and cracking, cracking carbon and catalyzer homogenizing is made to be in acquisition higher-energy state, the abundant acquisition pretreated xylogen of mixing and nickel powder mixture, the mixture of acquisition is put into autoclave, be filled with nitrogen, pressure is increased to 50MPa with the speed of 1MPa/s, mixture is heated to 800 DEG C with the fixing temperature rise rate of 60 DEG C/min from room temperature, and 120min is kept at 800 DEG C, normal temperature and pressure is down to through process, obtain Graphene.After testing, the mean thickness of the graphene sheet layer prepared in embodiment six is 0.63nm, and productive rate is 7.6%.
Although describe the preferred embodiments of the present invention, those skilled in the art once obtain the basic creative concept of cicada, then can make other change and amendment to these embodiments.So claims are intended to be interpreted as comprising preferred embodiment and falling into all changes and the amendment of the scope of the invention.
Obviously, those skilled in the art can carry out various change and modification to the present invention and not depart from the spirit and scope of the present invention.Like this, if these amendments of the present invention and modification belong within the scope of the claims in the present invention and equivalent technologies thereof, then the present invention is also intended to comprise these change and modification.
Claims (6)
1. utilize xylogen to prepare a method for Graphene, it is characterized in that, said method comprising the steps of:
A. be 1:5-10 by xylogen with alkaline solution mixing solid-liquid volume ratio, heated solution temperature is to 70-100 DEG C, and the isothermal holding time is 1-3 hour;
B. the material after alkaline purification is carried out filtering, washing, the drying at 60-80 DEG C of the solid of acquisition is obtained pre-treatment xylogen;
C. catalyzer is added by the pre-treatment xylogen of b step gained, high pressure homogenizer is utilized fully to mix, clarifixator up time pressure reaches 20-100MPa, material is by after high-pressure homogeneous nozzle head-on collision, collect the homogenizing valve flowing to slit, make non-homogeneous xylogen homogenizing and cracking, make cracking carbon and catalyzer homogenizing be in acquisition higher-energy state;
D. the mixture obtained in step c is put into autoclave, be filled with rare gas element, pressure is increased to 20-50MPa with the speed of 0.1-1MPa/s, mixture is heated to 500-800 DEG C with the fixing temperature rise rate of 30-60 DEG C/min from room temperature, and keep 30-120min at this temperature, be down to normal temperature and pressure through process, obtain Graphene.
2. a kind of method utilizing xylogen to prepare Graphene according to claim 1, it is characterized in that, described alkaline solution is the aqueous solution of at least one in sodium hydroxide, potassium hydroxide, ammoniacal liquor.
3. a kind of method utilizing xylogen to prepare Graphene according to claim 1, it is characterized in that, described alkaline solution alkalinity is the 10-30% of lignin quality.
4. a kind of method utilizing xylogen to prepare Graphene according to claim 1, it is characterized in that, described catalyzer is at least one in iron powder, nickel powder, copper powder, nickelous nitrate, ferric oxide, and described catalyzer and lignin quality are than being 0.01-0.1:10.
5. a kind of method utilizing xylogen to prepare Graphene according to claim 1, is characterized in that, described high pressure homogenizer operating pressure parameter is 80MPa.
6. a kind of method utilizing xylogen to prepare Graphene according to claim 1, it is characterized in that, described rare gas element is at least one in argon gas, helium, nitrogen.
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106241780A (en) * | 2016-07-19 | 2016-12-21 | 华南理工大学 | A kind of method preparing Graphene for raw material with lignin |
| CN106256761A (en) * | 2015-06-16 | 2016-12-28 | 宋玉军 | A kind of batch prepares the method for Graphene and doped graphene |
| CN106495132A (en) * | 2016-09-27 | 2017-03-15 | 济南米铎碳新能源科技有限公司 | The method that lignin prepares Graphene |
| CN106564874A (en) * | 2016-10-18 | 2017-04-19 | 宁波工程学院 | Lignin-based two-dimensional carbon nano-material as well as preparing method and application thereof |
| CN107235484A (en) * | 2017-08-03 | 2017-10-10 | 中南林业科技大学 | A kind of method that utilization black liquor rugose wood element prepares graphene |
| CN108751171A (en) * | 2018-06-15 | 2018-11-06 | 广西大学 | A method of preparing graphene film using lignin |
| CN109205603A (en) * | 2017-06-30 | 2019-01-15 | 中国科学院宁波材料技术与工程研究所 | The dispersing method of graphene |
| CN109437168A (en) * | 2019-01-03 | 2019-03-08 | 兖矿集团有限公司 | A kind of graphene hydrogel and preparation method thereof |
| CN109908750A (en) * | 2017-01-20 | 2019-06-21 | 杭州启澄科技有限公司 | A kind of catalysis high-pressure decomposing reactor handling industrial waste gas |
| CN111072014A (en) * | 2019-12-26 | 2020-04-28 | 安徽理工大学 | Preparation method of graphene |
| CN111454497A (en) * | 2019-01-22 | 2020-07-28 | 南京工业大学 | Graphene modified lignin enhanced polyolefin wood-plastic composite material and preparation method thereof |
| CN112607731A (en) * | 2020-12-24 | 2021-04-06 | 广东工业大学 | Device and method for preparing graphene powder |
| CN115463950A (en) * | 2022-09-13 | 2022-12-13 | 昆明理工大学 | High-pressure dehydration method for water-containing material |
| CN116100646A (en) * | 2023-02-22 | 2023-05-12 | 中南林业科技大学 | Modified wood loaded with imitated blade-shaped graphene layer, and preparation method and application thereof |
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| CN103466613A (en) * | 2013-10-11 | 2013-12-25 | 中南林业科技大学 | Method for preparing graphene from lignin |
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Patent Citations (1)
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| CN103466613A (en) * | 2013-10-11 | 2013-12-25 | 中南林业科技大学 | Method for preparing graphene from lignin |
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| CN106256761A (en) * | 2015-06-16 | 2016-12-28 | 宋玉军 | A kind of batch prepares the method for Graphene and doped graphene |
| CN106241780A (en) * | 2016-07-19 | 2016-12-21 | 华南理工大学 | A kind of method preparing Graphene for raw material with lignin |
| CN106241780B (en) * | 2016-07-19 | 2018-02-27 | 华南理工大学 | A kind of method that graphene is prepared using lignin as raw material |
| CN106495132A (en) * | 2016-09-27 | 2017-03-15 | 济南米铎碳新能源科技有限公司 | The method that lignin prepares Graphene |
| CN106564874B (en) * | 2016-10-18 | 2018-12-21 | 宁波工程学院 | A kind of lignin-base two dimension carbon nanomaterial and its preparation method and application |
| CN106564874A (en) * | 2016-10-18 | 2017-04-19 | 宁波工程学院 | Lignin-based two-dimensional carbon nano-material as well as preparing method and application thereof |
| CN109908750A (en) * | 2017-01-20 | 2019-06-21 | 杭州启澄科技有限公司 | A kind of catalysis high-pressure decomposing reactor handling industrial waste gas |
| CN109205603A (en) * | 2017-06-30 | 2019-01-15 | 中国科学院宁波材料技术与工程研究所 | The dispersing method of graphene |
| CN107235484A (en) * | 2017-08-03 | 2017-10-10 | 中南林业科技大学 | A kind of method that utilization black liquor rugose wood element prepares graphene |
| CN108751171A (en) * | 2018-06-15 | 2018-11-06 | 广西大学 | A method of preparing graphene film using lignin |
| CN109437168B (en) * | 2019-01-03 | 2021-11-05 | 兖矿集团有限公司 | Graphene hydrogel and preparation method thereof |
| CN109437168A (en) * | 2019-01-03 | 2019-03-08 | 兖矿集团有限公司 | A kind of graphene hydrogel and preparation method thereof |
| CN111454497A (en) * | 2019-01-22 | 2020-07-28 | 南京工业大学 | Graphene modified lignin enhanced polyolefin wood-plastic composite material and preparation method thereof |
| CN111454497B (en) * | 2019-01-22 | 2021-06-01 | 南京工业大学 | Graphene modified lignin enhanced polyolefin wood-plastic composite material and preparation method thereof |
| CN111072014A (en) * | 2019-12-26 | 2020-04-28 | 安徽理工大学 | Preparation method of graphene |
| CN112607731A (en) * | 2020-12-24 | 2021-04-06 | 广东工业大学 | Device and method for preparing graphene powder |
| CN112607731B (en) * | 2020-12-24 | 2021-08-10 | 广东工业大学 | Device and method for preparing graphene powder |
| CN115463950A (en) * | 2022-09-13 | 2022-12-13 | 昆明理工大学 | High-pressure dehydration method for water-containing material |
| CN116100646A (en) * | 2023-02-22 | 2023-05-12 | 中南林业科技大学 | Modified wood loaded with imitated blade-shaped graphene layer, and preparation method and application thereof |
| CN116100646B (en) * | 2023-02-22 | 2024-03-19 | 中南林业科技大学 | Modified wood loaded with imitated blade-shaped graphene layer, and preparation method and application thereof |
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