CN110203917B - Graphene hyperdispersant, preparation method thereof and application thereof in graphene - Google Patents
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 70
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 70
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 239000006185 dispersion Substances 0.000 claims abstract description 21
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims abstract description 18
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000003999 initiator Substances 0.000 claims abstract description 14
- 239000002994 raw material Substances 0.000 claims abstract description 12
- 239000003960 organic solvent Substances 0.000 claims abstract description 11
- 125000003903 2-propenyl group Chemical group [H]C([*])([H])C([H])=C([H])[H] 0.000 claims abstract description 9
- 229920002503 polyoxyethylene-polyoxypropylene Polymers 0.000 claims abstract description 9
- 229920005552 sodium lignosulfonate Polymers 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
- OMIGHNLMNHATMP-UHFFFAOYSA-N 2-hydroxyethyl prop-2-enoate Chemical compound OCCOC(=O)C=C OMIGHNLMNHATMP-UHFFFAOYSA-N 0.000 claims abstract description 8
- DXPPIEDUBFUSEZ-UHFFFAOYSA-N 6-methylheptyl prop-2-enoate Chemical compound CC(C)CCCCCOC(=O)C=C DXPPIEDUBFUSEZ-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910052708 sodium Inorganic materials 0.000 claims abstract description 8
- 239000011734 sodium Substances 0.000 claims abstract description 8
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 claims abstract description 8
- 239000007788 liquid Substances 0.000 claims description 9
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 8
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 6
- 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 4
- 235000019400 benzoyl peroxide Nutrition 0.000 claims description 4
- LSXWFXONGKSEMY-UHFFFAOYSA-N di-tert-butyl peroxide Chemical compound CC(C)(C)OOC(C)(C)C LSXWFXONGKSEMY-UHFFFAOYSA-N 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
- DKPFZGUDAPQIHT-UHFFFAOYSA-N Butyl acetate Natural products CCCCOC(C)=O DKPFZGUDAPQIHT-UHFFFAOYSA-N 0.000 claims description 3
- FUZZWVXGSFPDMH-UHFFFAOYSA-N hexanoic acid Chemical compound CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 claims description 3
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 3
- 238000009210 therapy by ultrasound Methods 0.000 claims description 2
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims 1
- 238000006243 chemical reaction Methods 0.000 abstract description 27
- 230000000977 initiatory effect Effects 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 21
- 238000003756 stirring Methods 0.000 description 15
- 238000001035 drying Methods 0.000 description 14
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 12
- 238000001816 cooling Methods 0.000 description 12
- 239000011259 mixed solution Substances 0.000 description 12
- 239000002270 dispersing agent Substances 0.000 description 10
- FYGHSUNMUKGBRK-UHFFFAOYSA-N 1,2,3-trimethylbenzene Chemical compound CC1=CC=CC(C)=C1C FYGHSUNMUKGBRK-UHFFFAOYSA-N 0.000 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 description 6
- 238000001914 filtration Methods 0.000 description 6
- 239000000047 product Substances 0.000 description 6
- 238000005303 weighing Methods 0.000 description 6
- 238000000034 method Methods 0.000 description 5
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 239000002244 precipitate Substances 0.000 description 4
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 3
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 3
- 235000011114 ammonium hydroxide Nutrition 0.000 description 3
- 239000011248 coating agent Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 description 3
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 description 3
- 229920000036 polyvinylpyrrolidone Polymers 0.000 description 3
- 239000001267 polyvinylpyrrolidone Substances 0.000 description 3
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 description 3
- 239000006228 supernatant Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 239000008096 xylene Substances 0.000 description 3
- 239000004593 Epoxy Substances 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 2
- 239000011701 zinc Substances 0.000 description 2
- 229910052725 zinc Inorganic materials 0.000 description 2
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 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
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 150000001721 carbon Chemical group 0.000 description 1
- 125000004432 carbon atom Chemical group C* 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
- 230000032798 delamination Effects 0.000 description 1
- 239000010408 film Substances 0.000 description 1
- 235000019253 formic acid Nutrition 0.000 description 1
- 230000036571 hydration Effects 0.000 description 1
- 238000006703 hydration reaction Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 230000033116 oxidation-reduction process Effects 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000011164 primary particle Substances 0.000 description 1
- 230000008569 process Effects 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
- 238000011160 research Methods 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 238000013517 stratification Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000010409 thin film Substances 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
The invention discloses a graphene hyperdispersant, a preparation method thereof and application thereof in graphene, wherein the graphene hyperdispersant is prepared from styrene, allyl polyoxyethylene polyoxypropylene ether, N-allyl imidazole, styrene-4-sodium sulfonate, hydroxyethyl acrylate, isooctyl acrylate, an initiator, sodium lignosulfonate and an organic solvent, the graphene hyperdispersant is prepared by taking the styrene and the allyl polyoxyethylene polyoxypropylene ether as basic raw materials and initiating a reaction by using the initiator, and the graphene hyperdispersant with good dispersibility and high dispersion stability is finally prepared.
Description
Technical Field
The invention relates to the technical field of dispersants, and particularly relates to a graphene hyperdispersant, a preparation method thereof and application thereof in graphene.
Background
Graphene is a two-dimensional material having a single-layer sheet structure, and is a planar thin film having a hexagonal honeycomb lattice formed by carbon atoms in sp2 hybridized orbitals, and has a thickness of only one carbon atom. Graphene is the thinnest and toughest nano material known at present, and the breaking strength of the graphene is 200 times higher than that of the best steel; its thermal conductivity coefficient is as high as 5300W/m.K, and its electron mobility is over 15000cm at normal temp2V.s, and a resistivity of only about 10-6Omega cm; in addition, graphene is also oversizedThe coating has the advantages of specific surface area, excellent permeability resistance, high thermal stability, high chemical stability and the like, and the characteristics enable the coating to have great application potential in the aspects of improving the mechanical property and the corrosion resistance of the coating. The graphene is added into the epoxy zinc-rich primer, so that on one hand, the graphene can replace part of zinc powder in the epoxy zinc-rich primer so as to reduce the using amount of the zinc powder and reduce the cost, and on the other hand, the shielding performance of a paint film can be improved.
However, strong van der waals forces and high specific surface area make graphene easy to aggregate together, and the fundamental reason for using graphene is its excellent properties, which can be reflected only on single sheets/primary particles to a great extent, while the properties of the aggregated graphene are greatly reduced or even completely lost, thus limiting the wide use of graphene,
researches show that the graphene can be modified and dispersed by adopting various methods, for example, the graphene surface can be modified by an oxidation-reduction method to achieve the purpose of dispersion. However, in the process of modifying the graphene aqueous solution by using the redox method, the application effect of the graphene is often affected due to poor dispersion effect of the graphene or too short anti-settling time. The existing graphene hyperdispersant comprises: sodium Dodecyl Benzene Sulfonate (SDBS), 1-pyrene formic acid, 1-pyrene sulfonic acid and the like, arabic gum, polyvinylpyrrolidone (PVP) and the like, and some synthesized complex organic molecules exist, but the graphene hyperdispersant has very limited capability of dispersing graphene in an aqueous solution, poor dispersing performance, low graphene concentration and poor dispersion stability.
Therefore, it is an urgent problem to be solved by those skilled in the art to provide a graphene hyperdispersant having good dispersibility and high dispersion stability.
Disclosure of Invention
In view of the above, the invention provides a graphene hyperdispersant, a preparation method thereof and an application thereof in graphene, wherein the graphene hyperdispersant can rapidly disperse graphene without agglomeration for a long time, and a dispersion liquid has excellent stability.
In order to achieve the purpose, the invention adopts the following technical scheme:
the graphene hyperdispersant is prepared from the following raw materials in parts by weight: 30-45 parts of styrene, 20-45 parts of allyl polyoxyethylene polyoxypropylene ether, 2-8 parts of N-allyl imidazole, 1-5 parts of styrene-4-sodium sulfonate, 2-5 parts of hydroxyethyl acrylate, 5-10 parts of isooctyl acrylate, 1-5 parts of an initiator, 1-5 parts of sodium lignosulfonate and 60-100 parts of an organic solvent.
Further, the initiator is composed of one or more of benzoyl peroxide, tert-butyl peroxybenzoate, di-tert-butyl peroxide, azobisisobutyronitrile and azobisisoheptonitrile.
The further beneficial effect is that the initiator adopted by the invention can cause the cross-linking reaction among the raw materials to release free radicals, so that the reaction of the raw materials is promoted and the function of preventing the graphene from agglomerating is also realized.
Further, the organic solvent is one or more of xylene, trimethylbenzene, butyl acetate, isopropanol, tetrahydrofuran and 2-butanone.
Compared with the prior art, the invention has the beneficial effects that: the hyper-dispersant prepared by the invention has excellent hydration capability and thermal stability, the special structure increases the space barrier effect among graphene particles, the dispersion effect is more efficient, and the hyper-dispersant has good dispersion performance and high dispersion stability. The graphene hyper-dispersant prepared by the invention is applied to graphene, and the dispersibility of the graphene can be obviously improved, so that the concentration of a graphene dispersion liquid is improved.
The invention also provides a preparation method of the graphene hyperdispersant, which comprises the following operation steps:
(1) weighing the raw materials in parts by weight, dissolving the initiator in the organic solvent, and stirring to fully dissolve the raw materials and the initiator to obtain a mixed solution;
(2) reacting the mixed solution obtained in the step (1) at a set temperature, and standing and cooling to room temperature after the reaction is completed;
(3) adjusting the pH value of the cooling solution obtained in the step (2) to 9-10 by adopting a pH regulator, slowly adding weighed sodium lignosulfonate, and continuously stirring until complete reaction;
(4) and after the reaction is finished, filtering, concentrating the reaction solution, purifying and separating a product, and drying in vacuum to constant weight to obtain the graphene dispersant.
Further, the stirring speed in the step (1) is 300-600r/min, and the stirring time is 20-40 min.
Further, the pH regulator in the step (3) is a dilute solution of sodium hydroxide or ammonia water.
Furthermore, the stirring speed in the step (3) is 200-400 r/min.
Further, in the step (4), the drying temperature is 80-130 ℃, the drying times are 2-5 times, and the drying time is 20-40min each time.
The invention also provides a preparation method of the graphene ultra-dispersion liquid, which comprises the following steps: and dissolving the graphene hyperdispersant and graphene in water, and putting the solution into an ultrasonic machine for ultrasonic treatment for 18-36 hours to obtain the graphene dispersion solution.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and 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 1
Graphene hyperdispersant:
(1) accurately weighing 30g of styrene, 20g of allyl polyoxyethylene polyoxypropylene ether, 2g of N-allyl imidazole, 1g of styrene-4-sodium sulfonate, 2g of hydroxyethyl acrylate, 10g of isooctyl acrylate, 30g of xylene and 30g of isopropanol, dissolving 1g of dibenzoyl peroxide and 1g of azobisisobutyronitrile in an organic solvent, and stirring at the rotating speed of 300r/min for 40min to fully dissolve raw materials and an initiator to obtain a mixed solution;
(2) continuously reacting the mixed solution obtained in the step (1) at 80 ℃ for 4h, and standing and cooling to room temperature after the reaction is completed;
(3) adjusting the pH value of the cooling solution obtained in the step (2) to 10 by adopting a dilute solution of sodium hydroxide, slowly adding 1g of sodium lignosulfonate, and stirring at the rotating speed of 400r/min until complete reaction;
(4) and after the reaction is finished, filtering, concentrating the reaction solution, purifying and separating a product, drying at 130 ℃ for 20min in vacuum, and repeatedly drying for 5 times until the weight is constant to obtain the graphene dispersant.
Example 2
Graphene hyperdispersant:
(1) accurately weighing 45g of styrene, 45g of allyl polyoxyethylene polyoxypropylene ether, 4g of N-allyl imidazole, 5g of styrene-4-sodium sulfonate, 5g of hydroxyethyl acrylate, 5g of isooctyl acrylate, 50g of trimethylbenzene and 50g of tetrahydrofuran, dissolving 1g of tert-butyl peroxybenzoate and 3g of azobisisoheptonitrile in an organic solvent, and stirring at the rotating speed of 300r/min for 40min to fully dissolve raw materials and an initiator to obtain a mixed solution;
(2) continuously reacting the mixed solution obtained in the step (1) at 100 ℃ for 2.5h, standing and cooling to room temperature after the reaction is completed;
(3) adjusting the pH value of the cooling solution obtained in the step (2) to 9 by adopting a dilute solution of ammonia water, slowly adding 3g of sodium lignosulfonate, and stirring at the rotating speed of 400r/min until complete reaction;
(4) and after the reaction is finished, filtering, concentrating the reaction solution, purifying and separating a product, drying at 130 ℃ for 20min in vacuum, and repeatedly drying for 5 times until the weight is constant to obtain the graphene dispersant.
Example 3
Graphene hyperdispersant:
(1) accurately weighing 38g of styrene, 30g of allyl polyoxyethylene polyoxypropylene ether, 8g of N-allyl imidazole, 4g of styrene-4-sodium sulfonate, 3g of hydroxyethyl acrylate, 8g of isooctyl acrylate and 75g of 2-butanone, dissolving 3g of di-tert-butyl peroxide and 2g of azobisisobutyronitrile in an organic solvent, and stirring at the rotating speed of 300r/min for 40min to fully dissolve raw materials and an initiator to obtain a mixed solution;
(2) continuously reacting the mixed solution obtained in the step (1) at 95 ℃ for 3h, and standing and cooling to room temperature after the reaction is completed;
(3) adjusting the pH value of the cooling solution obtained in the step (2) to 10 by adopting a dilute solution of sodium hydroxide, slowly adding 5g of sodium lignosulfonate, and stirring at the rotating speed of 400r/min until complete reaction;
(4) and after the reaction is finished, filtering, concentrating the reaction solution, purifying and separating a product, drying at 130 ℃ for 20min in vacuum, and repeatedly drying for 5 times until the weight is constant to obtain the graphene dispersant.
Example 4
Graphene hyperdispersant:
(1) accurately weighing 42g of styrene, 25g of allyl polyoxyethylene polyoxypropylene ether, 6g of N-allyl imidazole, 3g of styrene-4-sodium sulfonate, 3g of hydroxyethyl acrylate, 6g of isooctyl acrylate, 30g of xylene and 45g of butyl acetate, dissolving 4g of tert-butyl peroxybenzoate and 1g of benzoyl peroxide in an organic solvent, and stirring at the rotating speed of 300r/min for 25min to fully dissolve raw materials and an initiator to obtain mixed solution;
(2) continuously reacting the mixed solution obtained in the step (1) at 130 ℃ for 2h, and standing and cooling to room temperature after the reaction is completed;
(3) adjusting the pH value of the cooling solution obtained in the step (2) to 9 by adopting a dilute solution of ammonia water, slowly adding 2g of sodium lignosulfonate, and stirring at the rotating speed of 400r/min until complete reaction;
(4) and after the reaction is finished, filtering, concentrating the reaction solution, purifying and separating a product, drying at 130 ℃ for 20min in vacuum, and repeatedly drying for 5 times until the weight is constant to obtain the graphene dispersant.
Example 5
Graphene hyperdispersant:
(1) accurately weighing 35g of styrene, 35g of allyl polyoxyethylene polyoxypropylene ether, 5g of N-allyl imidazole, 5g of styrene-4-sodium sulfonate, 3g of hydroxyethyl acrylate, 10g of isooctyl acrylate, 35g of isopropanol and 50g of trimethylbenzene, dissolving 2g of di-tert-butyl peroxide and 3g of azobisisoheptonitrile in an organic solvent, and stirring at the rotating speed of 300r/min for 40min to fully dissolve raw materials and an initiator to obtain a mixed solution;
(2) continuously reacting the mixed solution obtained in the step (1) at 105 ℃ for 3h, and standing and cooling to room temperature after the reaction is completed;
(3) adjusting the pH value of the cooling solution obtained in the step (2) to 10 by adopting a dilute solution of sodium hydroxide, slowly adding 1g of sodium lignosulfonate, and stirring at the rotating speed of 400r/min until complete reaction;
(4) and after the reaction is finished, filtering, concentrating the reaction solution, purifying and separating a product, drying at 130 ℃ for 20min in vacuum, and repeatedly drying for 5 times until the weight is constant to obtain the graphene dispersant.
Performance testing
Dissolving the graphene hyperdispersant obtained in the embodiments 1-5 of the invention, the commercially available graphene hyperdispersant, polyvinylpyrrolidone, sodium dodecyl benzene sulfonate, graphene and water according to the weight ratio of 1: 5: 50, carrying out ultrasonic operation for 24 hours under the ultrasonic condition, controlling the water temperature not to exceed 60 ℃, and taking the supernatant to obtain the graphene dispersion liquid. The concentration of the dispersion was measured by a spectrophotometer method, and the dispersion was allowed to stand still and the supernatant was taken to measure the concentration of the supernatant, and the test results are shown in Table 1.
Table 1 examples and comparative examples data test results
As can be seen from the data in Table 1, the graphene dispersion liquid with the highest concentration of 43mg/ml is prepared in the prior art, but a small amount of precipitate is generated after standing for 12 hours, and the precipitate generation amount is gradually increased along with the prolonging of the standing time, so that the stability is poor, the precipitate is easy to stratify, while the graphene dispersion liquid prepared by the invention has the concentration of 65mg/ml, and has no precipitate stratification phenomenon after standing for 72 hours; compared with the prior art, the graphene dispersion liquid prepared by the preparation method disclosed by the invention has the advantages that the concentration of the dispersion liquid is greatly improved, the precipitation and delamination are not easy to occur, and the stability is high.
Claims (2)
1. The graphene hyperdispersant is characterized by being prepared from the following raw materials in parts by weight: 30-45 parts of styrene, 20-45 parts of allyl polyoxyethylene polyoxypropylene ether, 2-8 parts of N-allyl imidazole, 1-5 parts of styrene-4-sodium sulfonate, 2-5 parts of hydroxyethyl acrylate, 5-10 parts of isooctyl acrylate, 1-5 parts of sodium lignosulfonate, 2-10 parts of N-methyl pyrrolidone, 1-5 parts of an initiator and 60-100 parts of an organic solvent;
the initiator consists of one or more of benzoyl peroxide, tert-butyl peroxybenzoate and di-tert-butyl peroxide;
the organic solvent is one or more of butyl acetate, isopropanol, tetrahydrofuran and 2-butanone.
2. A preparation method of graphene dispersion liquid is characterized by comprising the following steps:
dissolving the graphene hyperdispersant of claim 1 and graphene in water, and putting the solution into an ultrasonic machine for ultrasonic treatment for 18-36h to obtain the graphene dispersion solution.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102712779A (en) * | 2009-12-22 | 2012-10-03 | 徐光锡 | Graphene dispersion and graphene-ionic liquid polymer compound material |
| 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 |
| 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 |
| CN106915740A (en) * | 2017-05-08 | 2017-07-04 | 同光（江苏）新材料科技有限公司 | A kind of preparation method of graphene dispersing solution |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102712779A (en) * | 2009-12-22 | 2012-10-03 | 徐光锡 | Graphene dispersion and graphene-ionic liquid polymer compound material |
| 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 |
| 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 |
| CN106915740A (en) * | 2017-05-08 | 2017-07-04 | 同光（江苏）新材料科技有限公司 | A kind of preparation method of graphene dispersing solution |
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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 |