CN113184841A - Method for enhancing dispersibility of low-oxygen-content graphene - Google Patents
Method for enhancing dispersibility of low-oxygen-content graphene Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 71
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 59
- 238000000034 method Methods 0.000 title claims abstract description 33
- 230000002708 enhancing effect Effects 0.000 title claims abstract description 18
- 238000006243 chemical reaction Methods 0.000 claims abstract description 40
- 238000005303 weighing Methods 0.000 claims abstract description 31
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 27
- 239000006185 dispersion Substances 0.000 claims abstract description 24
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 23
- 239000007788 liquid Substances 0.000 claims abstract description 18
- 238000003756 stirring Methods 0.000 claims abstract description 18
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 16
- 239000001301 oxygen Substances 0.000 claims abstract description 16
- 239000000843 powder Substances 0.000 claims abstract description 12
- 239000008367 deionised water Substances 0.000 claims abstract description 8
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 8
- 238000010438 heat treatment Methods 0.000 claims abstract description 7
- 239000003960 organic solvent Substances 0.000 claims abstract description 5
- 239000000463 material Substances 0.000 claims description 29
- 239000004721 Polyphenylene oxide Substances 0.000 claims description 8
- 229920000570 polyether Polymers 0.000 claims description 8
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 7
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 7
- 239000003999 initiator Substances 0.000 claims description 7
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 claims description 6
- 239000012986 chain transfer agent Substances 0.000 claims description 6
- 239000003638 chemical reducing agent Substances 0.000 claims description 6
- XFTALRAZSCGSKN-UHFFFAOYSA-M sodium;4-ethenylbenzenesulfonate Chemical compound [Na+].[O-]S(=O)(=O)C1=CC=C(C=C)C=C1 XFTALRAZSCGSKN-UHFFFAOYSA-M 0.000 claims description 6
- 239000002253 acid Substances 0.000 claims description 5
- FWDBOZPQNFPOLF-UHFFFAOYSA-N ethenyl(triethoxy)silane Chemical compound CCO[Si](OCC)(OCC)C=C FWDBOZPQNFPOLF-UHFFFAOYSA-N 0.000 claims description 2
- NKSJNEHGWDZZQF-UHFFFAOYSA-N ethenyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)C=C NKSJNEHGWDZZQF-UHFFFAOYSA-N 0.000 claims description 2
- 238000001694 spray drying Methods 0.000 claims description 2
- WKRJCCZAZDZNJL-UHFFFAOYSA-N 2-methoxyethoxysilicon Chemical compound COCCO[Si] WKRJCCZAZDZNJL-UHFFFAOYSA-N 0.000 claims 1
- 238000007865 diluting Methods 0.000 claims 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims 1
- 229920002554 vinyl polymer Polymers 0.000 claims 1
- 230000000694 effects Effects 0.000 description 5
- 238000007306 functionalization reaction Methods 0.000 description 5
- 230000009471 action Effects 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- 239000011203 carbon fibre reinforced carbon Substances 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 238000010526 radical polymerization reaction Methods 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000006482 condensation reaction Methods 0.000 description 2
- 239000007822 coupling agent Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 230000018044 dehydration Effects 0.000 description 2
- 238000006297 dehydration reaction Methods 0.000 description 2
- 238000006116 polymerization reaction Methods 0.000 description 2
- SCPYDCQAZCOKTP-UHFFFAOYSA-N silanol Chemical compound [SiH3]O SCPYDCQAZCOKTP-UHFFFAOYSA-N 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 238000006557 surface reaction Methods 0.000 description 2
- 238000005821 Claisen rearrangement reaction Methods 0.000 description 1
- 238000006959 Williamson synthesis reaction Methods 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 238000005917 acylation reaction Methods 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 239000002612 dispersion medium Substances 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000005886 esterification reaction Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 150000003254 radicals Chemical class 0.000 description 1
- 239000012429 reaction media Substances 0.000 description 1
- MNCGMVDMOKPCSQ-UHFFFAOYSA-M sodium;2-phenylethenesulfonate Chemical compound [Na+].[O-]S(=O)(=O)C=CC1=CC=CC=C1 MNCGMVDMOKPCSQ-UHFFFAOYSA-M 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- UKRDPEFKFJNXQM-UHFFFAOYSA-N vinylsilane Chemical compound [SiH3]C=C UKRDPEFKFJNXQM-UHFFFAOYSA-N 0.000 description 1
Classifications
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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
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/194—After-treatment
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
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- Nanotechnology (AREA)
- Inorganic Chemistry (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The invention discloses a method for enhancing the dispersibility of low-oxygen graphene, which comprises the following steps: s1, weighing 0.1-1 part by mass of graphene powder, stirring with 90-99.9 parts by mass of deionized water, and dispersing under an ultrasonic condition; s2, placing the treated dispersion liquid into a reaction kettle, stirring, and heating in a water bath to 60-80 ℃; s3, weighing 0.1-3 parts by mass of silane coupling agent, and adding the silane coupling agent into the reaction kettle in a dropwise manner for 0.5-1.5 hours; the method has mild reaction conditions, does not need or only needs a small amount of organic solvent, has low requirements on equipment, can effectively solve the problem of dispersion of the graphene in large-scale application, and reduces the dispersion cost.
Description
Technical Field
The invention relates to the technical field of graphene dispersion, in particular to a method for enhancing the dispersibility of low-oxygen-content graphene.
Background
The problem exists in the application process of graphene, that is, in the dispersion process of graphene, since graphene with a complete structure consists of benzene six-membered rings containing stable bonds, the chemical stability is high, the surface is in an inert state, the interaction with other media is weak, and strong intermolecular force exists among the sheets of graphene, the sheets are very easy to stack together and are difficult to disperse, and the sheets are difficult to dissolve in a solvent and difficult to uniformly compound with other organic or inorganic materials. This causes great difficulty in further research and application of graphene, and thus improving the dispersibility of graphene and its compatibility with various solvents and materials becomes a problem to be solved urgently in expanding the application field of graphene.
One effective way to solve the above problem is to functionalize the surface. The graphene surface functionalization is that a specific functional group is introduced at a defect position of an imperfect graphene surface through covalent bond and non-covalent bond connection, so that certain properties of the graphene surface are changed. The method can achieve the following effects: improving the dispersibility of graphene; the surface activity of the material is improved; endows the material with new physical and chemical properties; improving the compatibility of graphene with other substances. At present, the research on graphene surface functionalization is in a development stage, and from the viewpoint of a functionalization method, the method is mainly divided into two types: (1) covalent bond functionalization; (2) non-covalent bond functionalization. Functionalization is an important means for realizing dispersion, dissolution and molding processing of graphene, and the research progress of the two functionalization methods at home and abroad will be specifically described below.
The defects of the prior art are mainly reflected in that: non-covalently modified graphene dispersions often require expensive organic solvents as dispersants and water as the dispersion medium lacks dispersion stability. The covalent modification conditions of graphene are harsh, reactions for commonly modifying graphene and graphene oxide by covalent mainly include esterification reaction, acylation reaction, Williamson reaction, Claisen rearrangement reaction and the like, and these reactions usually have higher requirements on reaction conditions such as reaction medium, reaction temperature, reaction vessel and the like, and in large-scale application, these requirements can greatly increase production cost and are not favorable for application of graphene. Therefore, a method for enhancing the dispersibility of the low-oxygen graphene is provided.
Disclosure of Invention
The present invention aims to provide a method for enhancing dispersibility of low-oxygen content graphene, so as to solve the problems in the background art.
In order to achieve the purpose, the invention provides the following technical scheme: a method for enhancing dispersibility of low-oxygen content graphene comprises the following steps:
s1, weighing 0.1-1 part by mass of graphene powder, stirring with 90-99.9 parts by mass of deionized water, and dispersing under an ultrasonic condition;
s2, placing the treated dispersion liquid into a reaction kettle, stirring, and heating in a water bath to 60-80 ℃;
s3, weighing 0.1-3 parts by mass of silane coupling agent, and adding the silane coupling agent into the reaction kettle in a dropwise manner for 0.5-1.5 hours;
s4, placing 40-60 parts by mass of the modified graphene dispersion liquid obtained in the S3, 20-30 parts by mass of the polyether macromonomer and 0.1-1 part by mass of the initiator in a reaction kettle for stirring at the rotating speed of 200-400 r/min;
s5, weighing 2-6 parts by mass of acrylic acid or methacrylic acid, 1-3 parts by mass of sodium p-styrene sulfonate, and weighing 2-6 parts by mass of water to prepare solution A;
s6, weighing 0.1-1 part by mass of reducing agent, weighing 0.1-1 part by mass of chain transfer agent, and preparing liquid B;
and S7, after the base material is uniformly stirred, adding A, B material dropwise, wherein the material A is added dropwise for 2-3.5 hours, the material B is added dropwise for 0.5 hour on the basis of the material A, and finally, water is supplemented until the mass fraction of the reaction system is 100.
Preferably, the silane coupling agent has an unsaturated carbon-carbon double bond.
Preferably, the silane coupling agent is one of vinyltriethoxysilane, vinyltrimethoxysilane and vinyltri-beta-methoxyethoxysilane.
Preferably, the silane coupling agent is solubilized by an organic solvent having properties similar to those of the organic terminal.
Preferably, in S1, the graphene powder and the deionized water are dispersed for 1 to 4 hours under ultrasonic conditions, the dispersion time depends on the dispersion state of the graphene, and generally, the ultrasonically dispersed graphene can maintain stability for a certain time.
Preferably, the rotation speed of stirring the dispersion liquid treated in the S2 in the reaction kettle is 200-400 r/min.
Preferably, the polycarboxylic acid graft modified graphene with higher viscosity is diluted by water.
Preferably, the polycarboxylic acid graft modified graphene powder is prepared by a spray drying method.
Compared with the prior art, the invention has the beneficial effects that:
according to the invention, the silane coupling agent with unsaturated double bonds is used for covalently modifying the graphene with low oxygen content, so that the carbon-carbon double bonds with reaction activity are anchored on the graphene, and the acrylic acid, sodium styrene sulfonate and polyether monomer provide steric hindrance for the covalent modification of the graphene, thereby being beneficial to the dispersion of the graphene. The method has mild reaction conditions, does not need or only needs a small amount of organic solvent, has low requirements on equipment, and greatly reduces the cost of dispersing the graphene.
Detailed Description
The described embodiments are only some embodiments of the invention, not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example one
Providing a technical scheme that: a method for enhancing dispersibility of low-oxygen content graphene comprises the following steps:
s1, weighing 1 part by mass of graphene powder, stirring the graphene powder with 99 parts by mass of deionized water, and dispersing under an ultrasonic condition, wherein the step is as follows: uniformly dispersing graphene powder to ensure the homogeneity of a subsequent reaction system;
s2, placing the treated dispersion liquid into a reaction kettle, stirring, heating in a water bath to 60-80 ℃, and heating for the purpose of: providing enough reaction activation energy for the following silane coupling agent modified graphene;
s3, weighing 1 part by mass of silane coupling agent, and adding the silane coupling agent into a reaction kettle in a dropwise manner, wherein the dropwise addition time is 0.5-1.5 hours, and the dropwise addition aims at: the hydrolysis reaction of the silane coupling agent is controlled, the autogenous dehydration condensation reaction caused by overhigh concentration of the silane coupling agent is reduced, the reaction efficiency of the coupling agent and the graphene is improved, and more unsaturated double bonds are anchored on a graphene sheet layer; the principle of the reaction is as follows: the vinyl silane coupling agent is hydrolyzed in aqueous solution to generate silanol, the silanol and hydroxyl on the surface of GO generate dehydration condensation reaction to further generate-Si-O-C-, so that the coupling agent and GO generate stable covalent connection, and the reaction enables GO to have a certain number of carbon-carbon double bonds, so that GO can participate in free radical polymerization reaction of polycarboxylic acid synthesis;
s4, placing the modified graphene dispersion liquid obtained in the S3 of 45 parts by mass, the polyether macromonomer of 21 parts by mass and the initiator of 0.2 part by mass into a reaction kettle, stirring at the rotating speed of 200-400r/min, and taking the modified graphene and the polyether macromonomer as reaction bottom materials because the activity of the reaction is relatively low;
s5, weighing 2 parts by mass of acrylic acid or methacrylic acid and 0.5 part by mass of sodium p-styrenesulfonate, and then weighing 2 parts by mass of water to prepare solution A, wherein the acrylic acid or the methacrylic acid has high reaction activity and can generate free radical polymerization reaction with carbon-carbon double bonds anchored on graphene under the action of an initiator, the sodium p-styrenesulfonate provides certain rigidity for a polymerization chain, and a polyether macromonomer introduces a branched chain on the polymerization chain to provide steric hindrance for dispersion of the graphene;
s6, weighing 0.1 part by mass of reducing agent, and weighing 0.2 part by mass of chain transfer agent to prepare liquid B;
and S7, after the base material is uniformly stirred, adding A, B material dropwise, wherein the material A is added dropwise for 2-3.5 hours, the material B is added dropwise for 0.5 hour on the basis of the material A, and finally water is supplemented until the mass fraction of the reaction system is 100.
Example two
Providing a technical scheme that: a method for enhancing dispersibility of low-oxygen content graphene comprises the following steps:
s1, weighing 0.3 part by mass of graphene powder, stirring with 99.7 parts by mass of deionized water, and dispersing under an ultrasonic condition;
s2, placing the treated dispersion liquid into a reaction kettle, stirring, and heating in a water bath to 60-80 ℃;
s3, weighing 0.6 mass part of silane coupling agent, and adding the silane coupling agent into the reaction kettle in a dropwise manner for 0.5-1.5 hours;
s4, placing 50 parts by mass of the modified graphene dispersion liquid obtained in the S3, 25 parts by mass of the polyether macromonomer and 0.2 part by mass of the initiator into a reaction kettle, and stirring at the rotating speed of 200-400 r/min;
s5, weighing 4 parts by mass of acrylic acid or methacrylic acid and 1.5 parts by mass of sodium p-styrene sulfonate, and then weighing 4 parts by mass of water to prepare solution A;
s6, weighing 0.15 part by mass of reducing agent, weighing 0.2 part by mass of chain transfer agent, and preparing liquid B, wherein the reducing agent can react with an initiator at normal temperature to generate free radicals, and the chain transfer agent is used for terminating free radical polymerization to avoid generating polymers with overlarge molecular weight;
and S7, after the base material is uniformly stirred, adding A, B material dropwise, wherein the material A is added dropwise for 2-3.5 hours, the material B is added dropwise for 0.5 hour on the basis of the material A, and finally, water is supplemented until the mass fraction of the reaction system is 100.
EXAMPLE III
Providing a technical scheme that: a method for enhancing dispersibility of low-oxygen content graphene comprises the following steps:
s1, weighing 0.8 mass part of graphene powder, stirring with 99.2 mass parts of deionized water, and dispersing under an ultrasonic condition;
s2, placing the treated dispersion liquid into a reaction kettle, stirring, and heating in a water bath to 60-80 ℃;
s3, weighing 1.6 mass parts of silane coupling agent, and adding the silane coupling agent into the reaction kettle in a dropwise manner for 0.5-1.5 hours;
s4, placing 56 mass parts of modified graphene dispersion liquid obtained in S3, 28 mass parts of polyether macromonomer and 0.3 mass part of initiator into a reaction kettle for stirring, wherein the rotating speed is 200-400 r/min;
s5, weighing 4 parts by mass of acrylic acid or methacrylic acid and 1 part by mass of sodium p-styrene sulfonate, and weighing 4.5 parts by mass of water to prepare solution A;
s6, weighing 0.3 part by mass of reducing agent and 0.3 part by mass of chain transfer agent to prepare liquid B;
and S7, after the base material is uniformly stirred, adding A, B material dropwise, wherein the material A is added dropwise for 2-3.5 hours, the material B is added dropwise for 0.5 hour on the basis of the material A, and finally, water is supplemented until the mass fraction of the reaction system is 100.
It is noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (8)
1. A method for enhancing the dispersibility of low-oxygen graphene is characterized by comprising the following steps: the method comprises the following steps:
s1, weighing 0.1-1 part by mass of graphene powder, stirring with 90-99.9 parts by mass of deionized water, and dispersing under an ultrasonic condition;
s2, placing the treated dispersion liquid into a reaction kettle, stirring, and heating in a water bath to 60-80 ℃; s3, weighing 0.1-3 parts by mass of silane coupling agent, and adding the silane coupling agent into the reaction kettle in a dropwise manner for 0.5-1.5 hours;
s4, placing 40-60 parts by mass of the modified graphene dispersion liquid obtained in the S3, 20-30 parts by mass of the polyether macromonomer and 0.1-1 part by mass of the initiator in a reaction kettle for stirring at the rotating speed of 200-400 r/min;
s5, weighing 2-6 parts by mass of acrylic acid or methacrylic acid, 1-3 parts by mass of sodium p-styrene sulfonate, and weighing 2-6 parts by mass of water to prepare solution A;
s6, weighing 0.1-1 part by mass of reducing agent, weighing 0.1-1 part by mass of chain transfer agent, and preparing liquid B;
and S7, after the base material is uniformly stirred, adding A, B material dropwise, wherein the material A is added dropwise for 2-3.5 hours, the material B is added dropwise for 0.5 hour on the basis of the material A, and finally, water is supplemented until the mass fraction of the reaction system is 100.
2. The method for enhancing dispersibility of low-oxygen graphene according to claim 1, wherein: the silane coupling agent has an unsaturated carbon-carbon double bond.
3. The method for enhancing dispersibility of low-oxygen graphene according to claim 2, wherein: the silane coupling agent is one of vinyl triethoxysilane, vinyl trimethoxysilane and vinyl tri-beta methoxyethoxysilane.
4. The method for enhancing dispersibility of low-oxygen graphene according to claim 1, wherein: the silane coupling agent is dissolved by an organic solvent with similar property with the organic end.
5. The method for enhancing dispersibility of low-oxygen graphene according to claim 1, wherein: and dispersing the graphene powder in the S1 and deionized water for 1-4 hours under the ultrasonic condition.
6. The method for enhancing dispersibility of low-oxygen graphene according to claim 1, wherein: the dispersion liquid treated in the S2 is placed in a reaction kettle to be stirred at the rotating speed of 200-400 r/min.
7. The method for enhancing dispersibility of low-oxygen graphene according to claim 1, wherein: diluting the high-viscosity polycarboxylic acid grafted modified graphene with water.
8. The method for enhancing dispersibility of low-oxygen graphene according to claim 1, wherein: and preparing polycarboxylic acid grafted modified graphene powder by using a spray drying method.
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Application publication date: 20210730 |