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Preparation method and application of easy-to-disperse graphene slurry
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A graphene, easy-to-disperse technology, applied in the field of graphene, can solve problems such as inability, insoluble, and preparation of graphene dispersions
Active Publication Date: 2022-05-13
ZHEJIANG MARINE DEV RES INST +1
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However, the team of the present invention found after research that the perylenediimide graphene dispersants reported in the above two patents are insoluble in dibasic acid ester mixtures, so they cannot be used to prepare graphite in dibasic acid ester mixtures. olefin dispersion
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[0037] A preparation method for easily dispersible graphene slurry, comprising the following steps:
[0038] (1) Preparation of graphene dispersant: add perylenetetracarboxylic dianhydride, polyether monoamine and imidazole to the reaction vessel at a mass ratio of 10: (35-60): (50-80), under the protection of an inert gas Heating and reacting at 120-160° C. for 4-12 hours; transferring the obtained product to ice water, stirring and cooling for 0-40 minutes, suction filtering, washing, and drying to obtain a graphene dispersant.
[0039] (2) According to the mass ratio of 10: (250-350): (0.5-1.5). After the expandable graphite, the dibasic acid ester mixture and the graphene dispersant are mixed, pre-disperse for 0.5-1.5h to obtain the expandable graphite dispersion; the chemical structural formula of the graphene dispersant is as follows:
[0040]
[0041] Wherein, m=1-20, n=1-10.
[0042] (3) Exfoliate the expandable graphite dispersion in a colloid mill cycle for 2-4 ...
preparation Embodiment 1
[0050] In the reaction flask, add 10 grams of perylenetetracarboxylic dianhydride, 35 grams of polyether monoamine (Jeffamine M-600), 50 grams of imidazole, nitrogen protection, 140 degrees, react for 8 hours, pour 200 grams of ice water, stirred for 30 minutes, suction filtered, washed with water, and dried to obtain 38 grams of graphene dispersion agent 1.
[0055] In the reaction flask, add 10 grams of perylenetetracarboxylic dianhydride, 58 grams of polyether monoamine (Jeffamine M-1000), 60 grams of imidazole, nitrogen protection, 140 degrees, react for 10 hours, pour 300 grams of ice water, stirred for 30 minutes, suction filtered, washed with water, and dried to obtain 57 grams of graphene dispersant 2.
[0059] 10 grams of expandable graphite, 300 grams of mixed dibasic acid ester (DBE), 0.7 gram of graphene dispersant 1 pre-dispersed 1 hour in a high-speed disperser, and the gained expandable graphite dispersion was transferred to a high-speed colloid mill Stripping, cyclic stripping for 3 hours, and then removing a small amount of unstripped expandable graphite by a continuous centrifuge to obtain 290 grams of graphene content of 2.5% graphene slurry 1. TEM test ( figure 2 ), shown as predominantly few-layer graphene. Graphene...
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Abstract
The invention relates to the field of graphene, and discloses a preparation method and application of easy-to-disperse grapheneslurry, the preparation method comprises the following steps: (1) mixing expandable graphite, a dibasic acid ester mixture and a graphene dispersant, and then pre-dispersing to obtain an expandable graphite dispersion liquid; and (2) circularly stripping the expandable graphite dispersion liquid by using a colloid mill, and centrifuging to remove the unstripped expandable graphite to obtain the graphene slurry. By optimizing the graphene dispersing agent and the solvent, when the graphene slurry is prepared by stripping, the graphene slurry with stable dispersity is directly obtained, and the graphene slurry can be used for preparing graphene-containing products such as graphene heavy anti-corrosion coatings and graphene heat-conducting slurry only through dilution preparation.
Description
technical field [0001] The invention relates to the field of graphene, in particular to a preparation method and application of an easily dispersible graphene slurry. Background technique [0002] Graphene is a flake nanomaterial. In the solvent, adding an appropriate graphene dispersant, the few-layer graphene prepared by mechanically exfoliating graphite contains neither oxide nor structural defects, and keeps the graphene intact. Physical properties, with the characteristics of unrestricted application. Therefore, mechanical exfoliation of graphite is the main method for the industrial production of few-layer graphene. Commonly used solvents include alcohol-containing aqueous solutions and organic solvents. Usually, the graphite powder needs to be mechanically peeled off in an alcohol-containing aqueous solution or an organic solvent, separated and dried to obtain a few-layer graphene powder, and then dispersed in an appropriate organic solvent to prepare a stable graph...
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