CN110203917A - A kind of graphene hyper-dispersant and preparation method thereof and the application in graphene - Google Patents
A kind of graphene hyper-dispersant and preparation method thereof and the application in graphene Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 74
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 67
- 239000002270 dispersing agent Substances 0.000 title claims abstract description 41
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 claims abstract description 24
- 238000006243 chemical reaction Methods 0.000 claims abstract description 24
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000003999 initiator Substances 0.000 claims abstract description 15
- 229910052708 sodium Inorganic materials 0.000 claims abstract description 15
- 239000011734 sodium Substances 0.000 claims abstract description 15
- 239000002994 raw material Substances 0.000 claims abstract description 13
- 239000003960 organic solvent Substances 0.000 claims abstract description 12
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 claims abstract description 12
- 125000003903 2-propenyl group Chemical group [H]C([*])([H])C([H])=C([H])[H] 0.000 claims abstract description 9
- XLXCHZCQTCBUOX-UHFFFAOYSA-N 1-prop-2-enylimidazole Chemical compound C=CCN1C=CN=C1 XLXCHZCQTCBUOX-UHFFFAOYSA-N 0.000 claims abstract description 8
- DXPPIEDUBFUSEZ-UHFFFAOYSA-N 6-methylheptyl prop-2-enoate Chemical group CC(C)CCCCCOC(=O)C=C DXPPIEDUBFUSEZ-UHFFFAOYSA-N 0.000 claims abstract description 8
- YDEXUEFDPVHGHE-GGMCWBHBSA-L disodium;(2r)-3-(2-hydroxy-3-methoxyphenyl)-2-[2-methoxy-4-(3-sulfonatopropyl)phenoxy]propane-1-sulfonate Chemical compound [Na+].[Na+].COC1=CC=CC(C[C@H](CS([O-])(=O)=O)OC=2C(=CC(CCCS([O-])(=O)=O)=CC=2)OC)=C1O YDEXUEFDPVHGHE-GGMCWBHBSA-L 0.000 claims abstract description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- 238000003756 stirring Methods 0.000 claims description 15
- 150000001336 alkenes Chemical class 0.000 claims description 13
- 229910002804 graphite Inorganic materials 0.000 claims description 12
- 239000010439 graphite Substances 0.000 claims description 12
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 8
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical group CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 8
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 7
- -1 hydroxyl ethyl Chemical group 0.000 claims description 7
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 6
- 230000003068 static effect Effects 0.000 claims description 6
- OZAIFHULBGXAKX-UHFFFAOYSA-N 2-(2-cyanopropan-2-yldiazenyl)-2-methylpropanenitrile Chemical compound N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 claims description 4
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 4
- 239000000908 ammonium hydroxide Substances 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- GJBRNHKUVLOCEB-UHFFFAOYSA-N tert-butyl benzenecarboperoxoate Chemical compound CC(C)(C)OOC(=O)C1=CC=CC=C1 GJBRNHKUVLOCEB-UHFFFAOYSA-N 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 claims description 3
- 239000004342 Benzoyl peroxide Substances 0.000 claims description 3
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical compound C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 claims description 3
- DKPFZGUDAPQIHT-UHFFFAOYSA-N Butyl acetate Natural products CCCCOC(C)=O DKPFZGUDAPQIHT-UHFFFAOYSA-N 0.000 claims description 3
- 235000019400 benzoyl peroxide Nutrition 0.000 claims description 3
- LSXWFXONGKSEMY-UHFFFAOYSA-N di-tert-butyl peroxide Chemical compound CC(C)(C)OOC(C)(C)C LSXWFXONGKSEMY-UHFFFAOYSA-N 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- FUZZWVXGSFPDMH-UHFFFAOYSA-N hexanoic acid Chemical compound CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 claims description 3
- 229920005610 lignin Polymers 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 239000003002 pH adjusting agent Substances 0.000 claims description 3
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 3
- 238000011017 operating method Methods 0.000 claims description 2
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims 3
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims 1
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims 1
- 125000002252 acyl group Chemical group 0.000 claims 1
- 239000003795 chemical substances by application Substances 0.000 claims 1
- 239000000843 powder Substances 0.000 claims 1
- 239000006185 dispersion Substances 0.000 abstract description 15
- OMIGHNLMNHATMP-UHFFFAOYSA-N 2-hydroxyethyl prop-2-enoate Chemical compound OCCOC(=O)C=C OMIGHNLMNHATMP-UHFFFAOYSA-N 0.000 abstract description 7
- 230000006641 stabilisation Effects 0.000 abstract description 3
- 238000011105 stabilization Methods 0.000 abstract description 3
- 239000002244 precipitate Substances 0.000 abstract description 2
- 230000000977 initiatory effect Effects 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 24
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 15
- 238000000034 method Methods 0.000 description 7
- FYGHSUNMUKGBRK-UHFFFAOYSA-N 1,2,3-trimethylbenzene Chemical compound CC1=CC=CC(C)=C1C FYGHSUNMUKGBRK-UHFFFAOYSA-N 0.000 description 6
- 239000000047 product Substances 0.000 description 6
- 239000007788 liquid Substances 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000002604 ultrasonography Methods 0.000 description 3
- KAESVJOAVNADME-UHFFFAOYSA-N Pyrrole Chemical compound C=1C=CNC=1 KAESVJOAVNADME-UHFFFAOYSA-N 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 150000001721 carbon Chemical group 0.000 description 2
- 230000033116 oxidation-reduction process Effects 0.000 description 2
- 150000002978 peroxides Chemical class 0.000 description 2
- 230000001376 precipitating effect Effects 0.000 description 2
- 230000001737 promoting effect Effects 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 239000004593 Epoxy Substances 0.000 description 1
- 101710171229 Peroxidase 12 Proteins 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 238000005411 Van der Waals force Methods 0.000 description 1
- 235000010489 acacia gum Nutrition 0.000 description 1
- 239000001785 acacia senegal l. willd gum Substances 0.000 description 1
- WURBFLDFSFBTLW-UHFFFAOYSA-N benzil Chemical group C=1C=CC=CC=1C(=O)C(=O)C1=CC=CC=C1 WURBFLDFSFBTLW-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 229920006316 polyvinylpyrrolidine Polymers 0.000 description 1
- 239000011164 primary particle Substances 0.000 description 1
- DLOBKMWCBFOUHP-UHFFFAOYSA-N pyrene-1-sulfonic acid Chemical compound C1=C2C(S(=O)(=O)O)=CC=C(C=C3)C2=C2C3=CC=CC2=C1 DLOBKMWCBFOUHP-UHFFFAOYSA-N 0.000 description 1
- 150000003254 radicals Chemical class 0.000 description 1
- HFQQZARZPUDIFP-UHFFFAOYSA-M sodium;2-dodecylbenzenesulfonate Chemical compound [Na+].CCCCCCCCCCCCC1=CC=CC=C1S([O-])(=O)=O HFQQZARZPUDIFP-UHFFFAOYSA-M 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
Classifications
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
- C08F283/06—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals
- C08F283/065—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals on to unsaturated polyethers, polyoxymethylenes or polyacetals
Abstract
Application the invention discloses a kind of graphene hyper-dispersant and preparation method thereof and in graphene, the graphene hyper-dispersant uses styrene, allyl polyethenoxy polyethenoxy ether, N- allyl imidazole, styrene -4- sodium sulfonate, hydroxy-ethyl acrylate, Isooctyl acrylate monomer, initiator, sodium lignin sulfonate and organic solvent are prepared, the present invention is with styrene, allyl polyethenoxy polyethenoxy ether is as basic raw material, using initiator initiation reaction, it is good that dispersion performance finally has been prepared, the high graphene hyper-dispersant of dispersion stabilization, the graphene hyper-dispersant that the present invention is prepared can improve graphene dispersing solution concentration to 65mg/ml, graphene dispersing solution is able to maintain 72h or more stabilization and does not precipitate.
Description
Technical field
The present invention relates to dispersing agent technical field, relate particularly to a kind of graphene hyper-dispersant and preparation method thereof and
Application in graphene.
Background technique
Graphene is the two-dimensional material with individual layer laminated structure, is that one kind by carbon atom forms six with sp2 hybridized orbit
The angular flat film in honeycomb lattice, the two-dimensional material of only one carbon atom thickness.Graphene is to be currently known most
Thin, most tough nano material, 200 times more taller than best steel of breaking strength；Its thermal coefficient is up to 5300W/
MK, its electron mobility is more than 15000cm under room temperature2/ Vs, and resistivity about 10-6Ω·cm；In addition to this, graphite
Alkene also has many advantages, such as specific surface area, excellent permeability resistance, high thermal stability and the chemical stability of super large, these characteristics
It is set to have huge application potential in terms of the mechanical property and Corrosion Protection for promoting coating.Graphene is added to epoxy
In zinc rich primer, one side graphene can replace part zinc powder therein to reduce the dosage of zinc powder and reduce cost, another
Aspect can also be improved the shielding properties of paint film.
But powerful Van der Waals force and high-specific surface area is easily clumped together graphene, uses graphene
Basic reason is its excellent performance, these excellent properties can only be largely embodied on monolithic/primary particle, and
Graphene its performance after reunion is had a greatly reduced quality, can even be completely lost, therefore limits graphene and be widely used,
It is modified and dispersed graphite alkene studies have shown that a variety of methods can be used, such as oxidation-reduction method is to graphite
Alkene surface is modified the purpose that can reach dispersion.However, being modified process to graphene aqueous solution using oxidation-reduction method
In, the application effect of graphene is often influenced due to graphene dispersion is ineffective or the anti-settling time is too short.Existing graphite
Alkene hyper-dispersant includes: neopelex (SDBS), 1- pyrene formic acid, 1- pyrene sulfonic acid etc., Arabic gum, polyvinyl pyrrole
Alkanone (PVP) etc., there are also the complicated organic molecules of synthesis, but these graphene hyper-dispersants disperse in aqueous solution
The ability of graphene is very limited, and dispersion performance is bad, graphene concentration is lower, dispersion stability is poor.
Therefore, how to provide the high graphene hyper-dispersant of a kind of good dispersion property, dispersion stability is this field
The problem of technical staff's urgent need to resolve.
Summary of the invention
In view of this, the present invention provides a kind of graphene hyper-dispersant and preparation method thereof and answering in graphene
Dispersed graphite alkene and it can not reunited for a long time rapidly with, the dispersing agent, dispersion stability is outstanding.
To achieve the goals above, the present invention adopts the following technical scheme:
Graphene hyper-dispersant is prepared by the raw material of following parts by weight: 30-45 parts of styrene, allyl polyoxy second
20-45 parts of alkene polyethenoxy ether, 2-8 parts of N- allyl imidazole, 1-5 parts of styrene -4- sodium sulfonate, 2-5 parts of hydroxy-ethyl acrylate,
5-10 parts of Isooctyl acrylate monomer, 1-5 parts of initiator, 1-5 parts of sodium lignin sulfonate, 60-100 parts of organic solvent.
Further, above-mentioned initiator by benzoyl peroxide, peroxidized t-butyl perbenzoate, di-tert-butyl peroxide,
One of azodiisobutyronitrile, azobisisoheptonitrile or a variety of compositions.
It is using above-mentioned further beneficial effect, the initiator that the present invention uses, which can have, to be caused between each raw material
Cross-linking reaction releases free radical, and can also play while promoting raw material of the present invention reaction prevents graphene from reuniting
Effect.
Further, above-mentioned organic solvent is dimethylbenzene, in trimethylbenzene, butyl acetate, isopropanol, tetrahydrofuran, 2- butanone
One or more compositions.
The beneficial effects of the present invention are: hyper-dispersants prepared by the present invention to have splendid aquation compared with prior art
Ability and thermal stability, special structure increase the effect of the steric restriction between graphene particle, and dispersion effect is more efficient, and
Dispersion performance is good, dispersion stabilization is high.Graphene hyper-dispersant prepared by the present invention is applied in graphene, can significantly be mentioned
The dispersibility of high graphene, to improve the concentration of graphene dispersing solution.
The present invention also provides the preparation methods of above-mentioned graphene hyper-dispersant, including following operating procedure:
(1) weigh each raw material in parts by weight, then initiator be dissolved in organic solvent and be stirred, make raw material and
Initiator, which sufficiently dissolves, obtains mixed liquor；
(2) it is reacted to mixed liquor obtained in step (1), after fully reacting, is carried out quiet at a set temperature
Only it is cooled to room temperature；
(3) cooling pH value of solution will be obtained using pH adjusting agent in step (2) and be adjusted to 9-10, be slowly added to weigh up wooden
Plain sodium sulfonate, and continue stirring to complete reaction；
(4) it filters after reaction, concentration of reaction solution is isolated and purified with product, and it is super up to graphite to be dried under vacuum to constant weight
Alkene dispersing agent.
Further, stirring rate is 300-600r/min, mixing time 20-40min in above-mentioned steps (1).
Further, in above-mentioned steps (3) pH adjusting agent be sodium hydroxide or ammonium hydroxide weak solution.
Further, stirring rate described in above-mentioned steps (3) is 200-400r/min.
Further, drying temperature is 80-130 DEG C in above-mentioned steps (4), and dry number is 2-5 times, and each drying time is
20-40min。
The present invention also provides the preparation methods of above-mentioned graphene oversubscription dispersion liquid, and steps are as follows: by graphene hyper-dispersant
With graphene it is soluble in water after, be put into ultrasonic machine ultrasound 18-36h to get graphene dispersing solution.
Specific embodiment
The technical scheme in the embodiments of the invention will be clearly and completely described below, it is clear that described implementation
Example is only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, this field is common
Technical staff's every other embodiment obtained without making creative work belongs to the model that the present invention protects
It encloses.
Embodiment 1
Graphene hyper-dispersant:
(1) styrene 30g, allyl polyethenoxy polyethenoxy ether 20g, N- allyl imidazole 2g, benzene second are accurately weighed
Alkene -4- sodium sulfonate 1g, hydroxy-ethyl acrylate 2g, Isooctyl acrylate monomer 10g, dimethylbenzene 30g, isopropanol 30g, then by peroxidating
Dibenzoyl 1g and azodiisobutyronitrile 1g is dissolved in organic solvent and stirs 40min under the revolving speed of 300r/min, makes raw material
It is sufficiently dissolved with initiator and obtains mixed liquor；
(2) it to mixed liquor obtained in step (1) in 80 DEG C of successive reaction 4h, after fully reacting, carries out static cold
But to room temperature；
(3) cooling pH value of solution will be obtained using the weak solution of sodium hydroxide in step (2) and be adjusted to 10, be slowly added to wooden
Plain sodium sulfonate 1g, and stirring is reacted to complete under 400r/min revolving speed；
(4) it filters after reaction, concentration of reaction solution is isolated and purified with product, 20min is dried in vacuo at 130 DEG C, weight
5 times are dried again to constant weight, obtain the super alkene dispersing agent of graphite.
Embodiment 2
Graphene hyper-dispersant:
(1) styrene 45g, allyl polyethenoxy polyethenoxy ether 45g, N- allyl imidazole 4g, benzene second are accurately weighed
Alkene -4- sodium sulfonate 5g, hydroxy-ethyl acrylate 5g, Isooctyl acrylate monomer 5g, trimethylbenzene 50g, tetrahydrofuran 50g, then by peroxide
Change t-butyl perbenzoate 1g and azobisisoheptonitrile 3g to be dissolved in organic solvent and stir 40min under the revolving speed of 300r/min,
Dissolving raw material and initiator sufficiently, to obtain mixed liquor poly-；
(2) it to mixed liquor obtained in step (1) in 100 DEG C of successive reaction 2.5h, after fully reacting, carries out static
It is cooled to room temperature；
(3) cooling pH value of solution will be obtained using the weak solution of ammonium hydroxide in step (2) and be adjusted to 9, be slowly added to sulfomethylated lignin
Sour sodium 3g, and stirring is reacted to complete under 400r/min revolving speed；
(4) it filters after reaction, concentration of reaction solution is isolated and purified with product, 20min is dried in vacuo at 130 DEG C, weight
5 times are dried again to constant weight, obtain the super alkene dispersing agent of graphite.
Embodiment 3
Graphene hyper-dispersant:
(1) styrene 38g, allyl polyethenoxy polyethenoxy ether 30g, N- allyl imidazole 8g, benzene second are accurately weighed
Alkene -4- sodium sulfonate 4g, hydroxy-ethyl acrylate 3g, Isooctyl acrylate monomer 8g, 2- butanone 75g, then by di-tert-butyl peroxide
3g and azodiisobutyronitrile 2g is dissolved in organic solvent and stirs 40min under the revolving speed of 300r/min, makes raw material and initiator
Sufficiently dissolution obtains mixed liquor；
(2) it to mixed liquor obtained in step (1) in 95 DEG C of successive reaction 3h, after fully reacting, carries out static cold
But to room temperature；
(3) cooling pH value of solution will be obtained using the weak solution of sodium hydroxide in step (2) and be adjusted to 10, be slowly added to wooden
Plain sodium sulfonate 5g, and stirring is reacted to complete under 400r/min revolving speed；
(4) it filters after reaction, concentration of reaction solution is isolated and purified with product, 20min is dried in vacuo at 130 DEG C, weight
5 times are dried again to constant weight, obtain the super alkene dispersing agent of graphite.
Embodiment 4
Graphene hyper-dispersant:
(1) styrene 42g, allyl polyethenoxy polyethenoxy ether 25g, N- allyl imidazole 6g, benzene second are accurately weighed
Alkene -4- sodium sulfonate 3g, hydroxy-ethyl acrylate 3g, Isooctyl acrylate monomer 6g, dimethylbenzene 30g, butyl acetate 45g, then by peroxide
Change t-butyl perbenzoate 4g and benzoyl peroxide 1g to be dissolved in organic solvent and stir 25min under the revolving speed of 300r/min,
Dissolving raw material and initiator sufficiently, to obtain mixed liquor poly-；
(2) it to mixed liquor obtained in step (1) in 130 DEG C of successive reaction 2h, after fully reacting, carries out static cold
But to room temperature；
(3) cooling pH value of solution will be obtained using the weak solution of ammonium hydroxide in step (2) and be adjusted to 9, be slowly added to sulfomethylated lignin
Sour sodium 2g, and stirring is reacted to complete under 400r/min revolving speed；
(4) it filters after reaction, concentration of reaction solution is isolated and purified with product, 20min is dried in vacuo at 130 DEG C, weight
5 times are dried again to constant weight, obtain the super alkene dispersing agent of graphite.
Embodiment 5
Graphene hyper-dispersant:
(1) styrene 35g, allyl polyethenoxy polyethenoxy ether 35g, N- allyl imidazole 5g, benzene second are accurately weighed
Alkene -4- sodium sulfonate 5g, hydroxy-ethyl acrylate 3g, Isooctyl acrylate monomer 10g, isopropanol 35g, trimethylbenzene 50g, then by two tertiary fourths
Base peroxidase 12 g and azobisisoheptonitrile 3g is dissolved in organic solvent and stirs 40min under the revolving speed of 300r/min, makes original
Material and initiator, which sufficiently dissolve, obtains mixed liquor；
(2) it to mixed liquor obtained in step (1) in 105 DEG C of successive reaction 3h, after fully reacting, carries out static cold
But to room temperature；
(3) cooling pH value of solution will be obtained using the weak solution of sodium hydroxide in step (2) and be adjusted to 10, be slowly added to wooden
Plain sodium sulfonate 1g, and stirring is reacted to complete under 400r/min revolving speed；
(4) it filters after reaction, concentration of reaction solution is isolated and purified with product, 20min is dried in vacuo at 130 DEG C, weight
5 times are dried again to constant weight, obtain the super alkene dispersing agent of graphite.
Performance test
Graphene hyper-dispersant, the commercially available graphene hyper-dispersant, polyvinylpyrrolidine that 1-5 of the embodiment of the present invention is obtained
Ketone, neopelex and graphene and water are dissolved by 1: 5: 50 weight ratio, and are carried out under ultrasound condition
Ultrasound procedure 24 hours, while water temperature is controlled no more than 60 DEG C, take supernatant up to graphene dispersing solution.Using spectrophotometer
Method measures the concentration of its dispersion liquid, and stands and then take the concentration of its upper liquid measurement upper liquid respectively, and test result is shown in Table 1.
1 embodiment and comparative example data test result of table
From the data in table 1, it can be seen that the graphene dispersing solution that maximum concentration reaches 43mg/ml is made in the prior art, but after standing 12h
Just there is a small amount of precipitating to generate, and with the extension of time of repose, precipitate yield and gradually increase, stability is poor, easily precipitating point
Layer, and graphene dispersing solution produced by the present invention is at concentrations up to 65mg/ml, and stand after 72h without precipitated and separated phenomenon；Comparison is existing
There is technology, graphene dispersing solution made from preparation method of the invention substantially increases the concentration of dispersion liquid, and is not easy to precipitate
Layering, stability are high.
Claims (9)
1. a kind of graphene hyper-dispersant, which is characterized in that be prepared by the raw material of following parts by weight: 30-45 parts of styrene,
20-45 parts of allyl polyethenoxy polyethenoxy ether, 2-8 parts of N- allyl imidazole, 1-5 parts of styrene -4- sodium sulfonate, acrylic acid
2-5 parts of hydroxyl ethyl ester, 5-10 parts of Isooctyl acrylate monomer, 1-5 parts of sodium lignin sulfonate, 2-10 parts of N-Methyl pyrrolidone, initiator
1-5 parts, 60-100 parts of organic solvent.
2. a kind of graphene hyper-dispersant according to claim 1, which is characterized in that the initiator is by benzoyl peroxide first
One of acyl, peroxidized t-butyl perbenzoate, di-tert-butyl peroxide, azodiisobutyronitrile, azobisisoheptonitrile are more
Kind composition.
3. a kind of graphene hyper-dispersant according to claim 1, which is characterized in that the organic solvent is dimethylbenzene, three
One of toluene, butyl acetate, isopropanol, tetrahydrofuran, 2- butanone or a variety of compositions.
4. a kind of preparation method of graphene hyper-dispersant, which is characterized in that including following operating procedure:
(1) each raw material is weighed by the parts by weight of graphene hyper-dispersant described in claim any one of 1-3, then will caused
Agent is dissolved in organic solvent and is stirred, and dissolves raw material and initiator sufficiently and obtains mixed liquor；
(2) mixed liquor obtained in step (1) is reacted at a set temperature, after fully reacting, is carried out static cold
But to room temperature；
(3) cooling pH value of solution will be obtained using pH adjusting agent in step (2) and be adjusted to 9-10, be slowly added to the sulfomethylated lignin weighed up
Sour sodium, and continue stirring to complete reaction；
(4) it filters after reaction, concentration of reaction solution is isolated and purified with product, is dried under vacuum to constant weight up to graphite and surpasses alkene point
Powder.
5. a kind of preparation method of graphene hyper-dispersant according to claim 4, which is characterized in that described in step (1)
Stirring rate is 300-600r/min, mixing time 20-40min.
6. a kind of preparation method of graphene hyper-dispersant according to claim 4, which is characterized in that step (3) described pH
Regulator is the weak solution of sodium hydroxide or ammonium hydroxide.
7. a kind of preparation method of graphene hyper-dispersant according to claim 4, which is characterized in that step (3) is described to be stirred
Mixing rate is 200-400r/min.
8. a kind of preparation method of graphene hyper-dispersant according to claim 4, which is characterized in that step (4) is described dry
Dry temperature is 80-130 DEG C, and dry number is 2-5 times, and each drying time is 20-40min.
9. a kind of preparation method of graphene dispersing solution, which is characterized in that steps are as follows:
By any one of the claim 1-3 graphene hyper-dispersant and graphene it is soluble in water after, be put into ultrasonic machine surpass
Sound 18-36h is to get graphene dispersing solution.
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| CN111235659A (en) * | 2020-03-19 | 2020-06-05 | 当阳市鸿阳新材料科技有限公司 | Lyocell fiber with heat storage and insulation functions and preparation method thereof |
| CN114805683B (en) * | 2022-04-25 | 2023-04-21 | 常熟理工学院 | Polyion liquid-based composition and application thereof in graphene color paste |
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| CN104959050A (en) * | 2015-04-29 | 2015-10-07 | 北京天恒盛通科技发展有限公司 | Highly dispersed highly stable high concentration and high yield graphene dispersion liquid and preparation method thereof |
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| WO2014183243A1 (en) * | 2013-05-14 | 2014-11-20 | 中国科学院福建物质结构研究所 | Method for preparing graphene material and use thereof in chemical energy storage and/or conversion |
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| CN114805683B (en) * | 2022-04-25 | 2023-04-21 | 常熟理工学院 | Polyion liquid-based composition and application thereof in graphene color paste |
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Denomination of invention: A Graphene Superdispersant and Its Preparation Method and Application in Graphene Effective date of registration: 20231212 Granted publication date: 20210402 Pledgee: Anqing rural commercial bank Limited by Share Ltd. Pledgor: Anhui Baichen New Material Technology Co.,Ltd. Registration number: Y2023980070905 |