CN107021475A - The method that ultraviolet light solidification prepares mesoporous graphene - Google Patents

The method that ultraviolet light solidification prepares mesoporous graphene Download PDF

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CN107021475A
CN107021475A CN201710166544.9A CN201710166544A CN107021475A CN 107021475 A CN107021475 A CN 107021475A CN 201710166544 A CN201710166544 A CN 201710166544A CN 107021475 A CN107021475 A CN 107021475A
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ultraviolet light
mesoporous graphene
nano
graphene
mesoporous
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CN107021475B (en
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张登松
施利毅
颜婷婷
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University of Shanghai for Science and Technology
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2204/00—Structure or properties of graphene
    • C01B2204/20—Graphene characterized by its properties
    • C01B2204/32—Size or surface area
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
    • C01P2002/82—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by IR- or Raman-data
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM

Abstract

The present invention relates to the method that a kind of solidification of ultraviolet light prepares mesoporous graphene.This method prepares mesoporous graphene presoma using UV-curing technology, and inorganic particulate is template, and metal salt is catalyst, carbonization, and template thing, which is removed, obtains mesoporous grapheme material, and the mesoporous grapheme material mesopore orbit of preparation enriches, and specific surface area is high.The preparation technology is quick, and simply, cost is low, can be mass.Mesoporous graphene prepared by the present invention can be widely applied to the fields such as ultracapacitor, structure capacitance desalination, lithium ion battery, sodium-ion battery.

Description

The method that ultraviolet light solidification prepares mesoporous graphene
Technical field
The present invention relates to the method that a kind of solidification of ultraviolet light prepares mesoporous graphene.
Background technology
Graphene is as a kind of carbon material of new bi-dimensional cellular shape structure, and it has good electric conductivity（ 7200 S/ m）, larger theoretical specific surface area (2600 m2/ g), the superior performance such as high mechanical stability, therefore cause extensive Concern.Preparing the method for graphene at present mainly has：（ 1）The graceful Chester university An Deli of micromechanics stripping method, such as Britain People prepares graphene using adhesive tape method, though this method can obtain the higher few layer graphene of quality, yield is relatively low, process is numerous Trivial, size is whard to control to be limited it and uses；（ 2）Chemical vapour deposition technique, this method is with the anti-of catalyst substrate Answer in device, deposition growing is into graphene on substrate for carbon atom, (Jia-Le Shi, Cheng Tang, Hong-Jie Peng, Lin Zhu, Qiang Zhang, 3D Mesoporous Graphene: CVD Self-Assembly on Porous Oxide Templates and Applications in High-Stable Li-S Batteries. small 2015,39 (11), 5243), this method can produce substantial amounts of graphene, but the severe reaction conditions of graphene, cost Also it is higher.（ 3）Oxidation-reduction method, this method is that graphite aoxidizes to form graphite oxide through strong oxidizer, then is reduced with reducing agent Obtain graphene.（ Dreyer, D. R.; Murali, S.; Zhu, Y.; Ruoff, R. S.; Bielawski, C. W., Reduction of graphite oxide using alcohols. J Mater Chem 2011, 21 (10), 3443）Chemical reduction method is considered as a large amount of effective ways for preparing graphene, but the defect destruction that oxidation-reduction method is produced The electronic structure and perfection of crystal of graphene, and the high toxicity of conventional reducing agent such as hydrazine hydrate, hydroquinones, it is right Environment and human body have great harm, limit it and use.
The content of the invention
An object of the present invention is to overcome the complexity of technical matters present in prior art, preparation time longer, has There is provided the method that a kind of solidification of ultraviolet light prepares mesoporous graphene for the problem of effect specific surface area is low.
To reach above-mentioned purpose, the present invention is adopted the following technical scheme that：
Method that a kind of solidification of ultraviolet light prepares mesoporous graphene, it is characterised in that this method is concretely comprised the following steps：
A. the dispersion liquid for being 25~40 wt% by the scattered solid content of formation in a solvent of inorganic oxide nanoparticles, is added The mass ratio of surfactant, wherein inorganic oxide nanoparticles and surfactant is 1：（0.2~0.5）, it is uniformly dispersed To modified inorganic oxide nanoparticles solution；
B. prepolymer, diluent are dispersed in modified inorganic oxide nanoparticles solution, add catalyst, Cationic curing dose, it is coated on aluminium foil, is volatilized completely to solvent after being uniformly dispersed, obtains transparent after solidifying using ultraviolet light Film, as mesoporous graphene presoma；Described prepolymer, diluent, the inorganic oxide nanoparticles of modification, catalyst Mass ratio with cationic curing dose is 1：（0.5~1）：（1~5）：（1~4）：（0.01~0.09）；
C. mesoporous graphene presoma obtained by step b is calcined into carbonization under an inert atmosphere, gained compound 3-6 after carbonization Mol/L HCl solution or HF solution etches inorganic particulate templates, filtering, fully washing filtration cakes torrefaction obtains mesoporous graphene material Material.
Above-mentioned inorganic oxide nanoparticles be nano silicon oxide, nano-sized iron oxide or nano zine oxide, particle diameter be 5~ 50 nm。
Above-mentioned catalyst is at least one of ferrocene, dicyclopentadienyl nickel, basic nickel carbonate and nickel nitrate.
Above-mentioned surface modifier is 3- glycidylpropyls trimethoxy silane, 3-（Methacryloxy）Propyl group three Methoxy silane, 3-（Acryloxypropyl）Trimethoxy silane, 3-（Methacryloxy）The TMOS of propyl group three At least one of.
Above-mentioned prepolymer is bisphenol A epoxy acrylate, bisphenol-A liquid epoxy resin, aliphatic polyurethane propylene At least one of acid esters.
Above-mentioned diluent is hexanediyl ester or 1,4- butanediol diglycidyl ethers.
What the calcining in above-mentioned step C was carbonized concretely comprises the following steps：Inert gas flow velocity is 40~150 mL/min；Heating Speed is 1~5 DEG C/min, is warming up to 300~400 DEG C, is incubated 1~3 h, then heating rate is 1~5 DEG C/min, is warming up to 800~1400oC calcines 2~4 h.
Above-mentioned inorganic nano-particle particle diameter is between 5-50 nm, particle diameter is too small, and grapheme material is based on micropore, grain Footpath is excessive, and the material of preparation just belongs to large pore material.The different adjustment of template particle diameter prepare mesoporous grapheme material aperture and Specific surface area, so that for various applications.
The graphitization of carbon material is the solid phase reaction that a kind of amorphous state changes to crystalline state, and steering resistance is larger, easily forms sub- Stable state, is difficult to graphitization, by adding catalyst in heating process, can be less than required by usual graphitization Graphitization reaction, most of sp are carried out under temperature conditionss3The carbon conversion of hydridization is sp2The graphite of structure is so as to obtain higher stone Mo Huadu.
Above-mentioned surface modifier is silane coupler, and hydrolyzable one end can exist with inorganic nano-particle reactive grafting Particle surface, organic chain one end is conducive to inorganic particulate template to disperse in carbon organic precursor.
The preparation method technique of the present invention is quick, simply, can be mass, the mesoporous graphene mesopore orbit of preparation is rich Richness, specific surface area is high, can be widely applied to the neck such as ultracapacitor, structure capacitance desalination, lithium ion battery, sodium-ion battery Domain.
Brief description of the drawings
Fig. 1 is the high resolution transmission electron microscopy photo of mesoporous grapheme material prepared by the embodiment of the present invention 1.
Fig. 2 is the Raman spectrogram of the mesoporous grapheme material prepared by the embodiment of the present invention 1.
Fig. 3 is nitrogen adsorption/desorption curve of the mesoporous grapheme material prepared by the embodiment of the present invention 1.
Embodiment
After now the specific embodiment of the present invention is described in.
Embodiment 1
By the ZnO that particle diameter is 16 nm2Nano-particle is scattered to form the dispersion liquid that solid content is 40 wt% in a solvent, adds Surfactant 3-（Acryloxypropyl）Trimethoxy silane, wherein ZnO2Nano-particle and 3-（Acryloxypropyl） The mass ratio of trimethoxy silane is 1：0.3, it is uniformly dispersed and obtains modified ZnO2Nano-particle solution；By bisphenol-A epoxy third Olefin(e) acid ester, 1,4- butanediol diglycidyl ethers are dispersed in modified ZnO2In nano-particle solution, add ferrocene, Cationic curing dose, it is coated on aluminium foil, is volatilized completely to solvent after being uniformly dispersed, obtains transparent after solidifying using ultraviolet light Film, as mesoporous graphene presoma；Described bisphenol A epoxy acrylate, 1,4- butanediol diglycidyl ethers, modification ZnO2Nano-particle, ferrocene and cationic curing dose of mass ratio are 1：0.5：3：2：0.07；By above-mentioned mesoporous stone Black alkene presoma is placed in tube furnace, under an argon atmosphere calcining carbonization, and gas flow rate is 40mL/min.Temperature control speed is 1oC/ Min, room temperature to 400oC is incubated 2h, then temperature control speed is 1oC/min, is warming up to 1200 DEG C of calcining 2h.Compound after carbonization ZnO is etched with 3 mol/L HCl solution2The compound of template and iron, filtering, fully washing filtration cakes torrefaction obtains mesoporous graphene Material.
Test the specific surface area of above-mentioned mesoporous grapheme material.Using Full-automatic gas adsorption instrument ASIQ, sample before test Product degassing process under vacuum condition, 493K, and calculated using BET models.The specific surface area for measuring mesoporous grapheme material is 1082m2/g。
Embodiment 2
By the ZnO that particle diameter is 22 nm2Nano-particle is scattered to form the dispersion liquid that solid content is 40 wt% in a solvent, adds Surfactant 3-（Acryloxypropyl）Trimethoxy silane, wherein ZnO2Nano-particle and 3-（Acryloxypropyl） The mass ratio of trimethoxy silane is 1：0.5, it is uniformly dispersed and obtains modified ZnO2Nano-particle solution；By bisphenol-A liquid Epoxy resin, 1,4- butanediol diglycidyl ethers are dispersed in modified ZnO2In nano-particle solution, nitric acid is added Nickel, cationic curing dose, be coated on aluminium foil, volatilized completely to solvent after being uniformly dispersed, obtained after being solidified using ultraviolet light Transparent membrane, as mesoporous graphene presoma；Described bisphenol-A liquid epoxy resin, 1,4- butanediol 2-glycidyls Ether, the ZnO of modification2Nano-particle, nickel nitrate and cationic curing dose of mass ratio are 1：0.5：3：2：0.07；Will be above-mentioned Mesoporous graphene presoma is placed in tube furnace, under an argon atmosphere calcining carbonization, and gas flow rate is 40mL/min.Temperature control speed is 1oC/min, room temperature to 400oC is incubated 2h, then temperature control speed is 1oC/min, is warming up to 1200 DEG C of calcining 2h.It is multiple after carbonization Compound etches ZnO with 3 mol/L HCl solution2The compound of template and nickel, filtering, fully washing filtration cakes torrefaction obtains mesoporous stone Black alkene material.
Test the specific surface area of above-mentioned mesoporous grapheme material.Using Full-automatic gas adsorption instrument ASIQ, sample before test Product degassing process under vacuum condition, 493K, and calculated using BET models.The specific surface area for measuring mesoporous grapheme material is 862m2/g。
Embodiment 3
By the Fe that particle diameter is 16 nm3O4Nano-particle is scattered to form the dispersion liquid that solid content is 30 wt% in a solvent, adds Surfactant 3-（Acryloxypropyl）Trimethoxy silane, wherein Fe3O4Nano-particle and 3-（Acryloxypropyl） The mass ratio of trimethoxy silane is 1：0.4, it is uniformly dispersed and obtains modified Fe3O4Nano-particle solution；By bisphenol-A liquid Epoxy resin, 1,4- butanediol diglycidyl ethers are dispersed in modified Fe3O4In nano-particle solution, alkali formula is added Nickelous carbonate, cationic curing dose, be coated on aluminium foil, volatilized completely to solvent, after being solidified using ultraviolet light after being uniformly dispersed Transparent membrane is obtained, as mesoporous graphene presoma；Described bisphenol-A liquid epoxy resin, 1,4- butanediols two shrink Glycerin ether, the Fe of modification3O4Nano-particle, basic nickel carbonate and cationic curing dose of mass ratio are 1：0.8：3：3：0.06； Above-mentioned mesoporous graphene presoma is placed in tube furnace, under an argon atmosphere calcining carbonization, gas flow rate is 40mL/min.Control Warm speed is 1oC/min, room temperature to 400oC is incubated 2h, then temperature control speed is 1oC/min, is warming up to 1200 DEG C of calcining 2h. Compound etches Fe with 3 mol/L HCl solution after carbonization3O4The compound of template and nickel, filtering, fully washs filtration cakes torrefaction Obtain mesoporous grapheme material.
Test the specific surface area of above-mentioned mesoporous grapheme material.Using Full-automatic gas adsorption instrument ASIQ, sample before test Product degassing process under vacuum condition, 493K, and calculated using BET models.The specific surface area for measuring mesoporous grapheme material is 1147m2/g。
Embodiment 4
By the Fe that particle diameter is 7 nm3O4Nano-particle is scattered to form the dispersion liquid that solid content is 30 wt% in a solvent, adds Surfactant 3-（Acryloxypropyl）Trimethoxy silane, wherein Fe3O4Nano-particle and 3-（Acryloxypropyl） The mass ratio of trimethoxy silane is 1：0.4, it is uniformly dispersed and obtains modified Fe3O4Nano-particle solution；By aliphatic polyurethane Acrylate, hexanediyl ester are dispersed in modified Fe3O4In nano-particle solution, add dicyclopentadienyl nickel, sun from Subtype curing agent, is coated on aluminium foil after being uniformly dispersed, and is volatilized completely to solvent, and thin transparent is obtained after solidifying using ultraviolet light Film, as mesoporous graphene presoma；Described aliphatic urethane acrylate, hexanediyl ester, modification Fe3O4Nano-particle, dicyclopentadienyl nickel and cationic curing dose of mass ratio are 1：0.8：3：3：0.06；By above-mentioned mesoporous graphite Alkene presoma is placed in tube furnace, under an argon atmosphere calcining carbonization, and gas flow rate is 40mL/min.Temperature control speed is 1oC/min, Room temperature is to 400oC is incubated 2h, then temperature control speed is 1oC/min, is warming up to 1200 DEG C of calcining 2h.Compound uses 3 after carbonization Mol/L HCl solution etching Fe3O4The compound of template and nickel, filtering, fully washing filtration cakes torrefaction obtains mesoporous graphene material Material.
Test the specific surface area of above-mentioned mesoporous grapheme material.Using Full-automatic gas adsorption instrument ASIQ, sample before test Product degassing process under vacuum condition, 493K, and calculated using BET models.The specific surface area for measuring mesoporous grapheme material is 1350m2/g。
Embodiment 5
By the SiO that particle diameter is 16 nm2Nano-particle is scattered to form the dispersion liquid that solid content is 30 wt% in a solvent, adds Surfactant 3-（Acryloxypropyl）Trimethoxy silane, wherein SiO2Nano-particle and 3-（Acryloxypropyl） The mass ratio of trimethoxy silane is 1：0.3, it is uniformly dispersed and obtains modified SiO2Nano-particle solution；By bisphenol-A liquid Epoxy resin, 1,4- butanediol diglycidyl ethers are dispersed in modified SiO2In nano-particle solution, nitric acid is added Nickel, cationic curing dose, be coated on aluminium foil, volatilized completely to solvent after being uniformly dispersed, obtained after being solidified using ultraviolet light Transparent membrane, as mesoporous graphene presoma；Described bisphenol-A liquid epoxy resin, 1,4- butanediol 2-glycidyls Ether, the SiO of modification2Nano-particle, nickel nitrate and cationic curing dose of mass ratio are 1：0.5：3：2：0.09；Will be above-mentioned Mesoporous graphene presoma is placed in tube furnace, under an argon atmosphere calcining carbonization, and gas flow rate is 40mL/min.Temperature control speed is 1oC/min, room temperature to 400oC is incubated 2h, then temperature control speed is 1oC/min, is warming up to 1200 DEG C of calcining 2h.It is multiple after carbonization 3 mol/L of compound HF solution etches SiO2The compound of template and nickel, filtering, fully washing filtration cakes torrefaction obtains mesoporous stone Black alkene material.
Test the specific surface area of above-mentioned mesoporous grapheme material.Using Full-automatic gas adsorption instrument ASIQ, sample before test Product degassing process under vacuum condition, 493K, and calculated using BET models.The specific surface area for measuring mesoporous grapheme material is 1232m2/g。

Claims (7)

1. the method that a kind of solidification of ultraviolet light prepares mesoporous graphene, it is characterised in that this method is concretely comprised the following steps：
A. the dispersion liquid for being 25~40 wt% by the scattered solid content of formation in a solvent of inorganic oxide nanoparticles, is added The mass ratio of surfactant, wherein inorganic oxide nanoparticles and surfactant is 1：（0.2~0.5）, it is uniformly dispersed To modified inorganic oxide nanoparticles solution；Described surfactant is silane coupler；
B. prepolymer, diluent are dispersed in modified inorganic oxide nanoparticles solution, add catalyst, Cationic curing dose, it is coated on aluminium foil, is volatilized completely to solvent after being uniformly dispersed, obtains transparent after solidifying using ultraviolet light Film, as mesoporous graphene presoma；Described prepolymer, diluent, the inorganic oxide nanoparticles of modification, catalyst Mass ratio with cationic curing dose is 1：（0.5~1）：（1~5）：（1~4）：（0.01~0.09）；
C. mesoporous graphene presoma obtained by step b is calcined into carbonization under an inert atmosphere, gained compound 3-6 after carbonization Mol/L NaOH solution or HCl solution etching inorganic particulate template, filtering, fully washing filtration cakes torrefaction obtains mesoporous graphene material Material.
2. the method that ultraviolet light solidification according to claim 1 prepares mesoporous graphene, it is characterised in that described is inorganic Oxide nano-particles are nano silicon oxide, nano-sized iron oxide or nano zine oxide, and particle diameter is 5~50 nm.
3. the method that ultraviolet light solidification according to claim 1 prepares mesoporous graphene, it is characterised in that described catalysis Agent is at least one of ferrocene, dicyclopentadienyl nickel, basic nickel carbonate and nickel nitrate.
4. the method that ultraviolet light solidification according to claim 1 prepares mesoporous graphene, it is characterised in that described silane Coupling agent is 3- glycidylpropyls trimethoxy silane, 3-（Methacryloxy）Propyl trimethoxy silicane, 3-（Propylene Acryloxypropylethoxysilane）Trimethoxy silane, 3-（Methacryloxy）At least one of the TMOS of propyl group three.
5. the method that ultraviolet light solidification according to claim 1 prepares mesoporous graphene, it is characterised in that described pre-polymerization Thing is at least one of bisphenol A epoxy acrylate, bisphenol-A liquid epoxy resin, aliphatic urethane acrylate.
6. the method that ultraviolet light solidification according to claim 1 prepares mesoporous graphene, it is characterised in that diluent is for oneself Omega-diol diacrylate or 1,4- butanediol diglycidyl ethers.
7. the method that ultraviolet light solidification according to claim 1 prepares mesoporous graphene, it is characterised in that described step C In calcining carbonization concretely comprise the following steps：Inert gas flow velocity is 40~150 mL/min；Heating rate is 1~5 DEG C/min, is risen Temperature is incubated 1~3 h to 300~400 DEG C, then heating rate is 1~5 DEG C/min, is warming up to 800~1400oC calcinings 2~4 h。
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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102437320A (en) * 2011-11-21 2012-05-02 北京师范大学 Graphene-coated mesoporous metallic oxide, and preparation method and use thereof
CN102992308A (en) * 2012-11-21 2013-03-27 复旦大学 Graphene with high specific capacitance and preparation method thereof
CN103011138A (en) * 2012-11-09 2013-04-03 中国科学院宁波材料技术与工程研究所 Graphene with composite pore structure, preparation method thereof and application in super capacitor
CN105129771A (en) * 2015-09-09 2015-12-09 上海大学 Preparation method of mesoporous carbon with adjustable aperture
CN105293480A (en) * 2015-12-03 2016-02-03 青岛昊鑫新能源科技有限公司 Preparation method of two-dimension ordered mesopore graphene skeleton thin-film material
CN106467300A (en) * 2015-08-13 2017-03-01 中国科学院上海硅酸盐研究所 Three-dimensional grapheme material of micropore-mesopore-macropore multilevel hierarchy and its preparation method and application

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102437320A (en) * 2011-11-21 2012-05-02 北京师范大学 Graphene-coated mesoporous metallic oxide, and preparation method and use thereof
CN103011138A (en) * 2012-11-09 2013-04-03 中国科学院宁波材料技术与工程研究所 Graphene with composite pore structure, preparation method thereof and application in super capacitor
CN102992308A (en) * 2012-11-21 2013-03-27 复旦大学 Graphene with high specific capacitance and preparation method thereof
CN106467300A (en) * 2015-08-13 2017-03-01 中国科学院上海硅酸盐研究所 Three-dimensional grapheme material of micropore-mesopore-macropore multilevel hierarchy and its preparation method and application
CN105129771A (en) * 2015-09-09 2015-12-09 上海大学 Preparation method of mesoporous carbon with adjustable aperture
CN105293480A (en) * 2015-12-03 2016-02-03 青岛昊鑫新能源科技有限公司 Preparation method of two-dimension ordered mesopore graphene skeleton thin-film material

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