High-dispersion graphene solution prepared by virtue of one-step method and preparation method of high-dispersion graphene solution

A graphene solution, high dispersion technology, applied in the direction of coating, etc., can solve the problems of poor dispersion of graphene and polymer, discount of excellent performance of graphene, application restrictions, etc., and achieve convenient method, low cost and good applicability Effect

Inactive Publication Date: 2019-03-19

NANJING FORESTRY UNIV

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Problems solved by technology

[0005] Generally, graphene is stripped from graphite, the cost is high, and the dispersion of graphene and polymer is poor. Due to the interaction of Van der Waals force between the sheets, it is easy to aggregate during the application process, and usually needs to be dispersed. In solvents, but because graphene is insoluble in water and non-lipophilic, its application is limited, so the ...

Abstract

The invention relates to a high-dispersion graphene solution prepared by virtue of a one-step method and a preparation method of the high-dispersion graphene solution. The high-dispersion graphene solution contains suspension liquid consisting of flake graphite and cellulose nanocrystals, wherein the mass ratio of flake graphite to cellulose nanocrystal in cellulose nanocrystal/flake graphite suspension liquid is (1-3) to 100. The preparation method compriss the following steps: (1) preparing the cellulose nanocrystal/flake graphite suspension liquid; (2) centrifuging the suspension liquid; (3) carrying out dialysis on the suspension liquid; and (4) carrying out ultrasonic treatment formation on the suspension liquid. The high-dispersion graphene solution has the advantages that (1) by preparing through the one-step method, the principle is simple, the operation is convenient, and the method is convenient, fast and suitable for industrial production; (2) hydroxide radicals on the surfaces of the cellulose nanocrystals can adequately react with surface active groups on the surface of a graphene slice layer, so that the graphene can be highly and uniformly dispersed; and (3) the high-dispersion graphene solution is low in cost, wide in source, controllable in process and good in applicability.

Application Domain

Coatings

Technology Topic

Cvd grapheneFlake graphite +5

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Examples

Experimental program(6)

Example Embodiment

[0038] Example 1

[0039] One-step preparation of highly dispersed graphene solution, which is characterized by comprising a suspension of cellulose nanocrystals/graphene flakes; among them, a suspension of graphene flakes and cellulose nanocrystals in a cellulose nanocrystal/graphene flake suspension The mass ratio is 1-3:100.

[0040] The modifier nanocellulose is a suspension of cellulose nanocrystals/sheet-like graphene, the amount of dry matter after blending the two ranges from 20.2-20.6g, and the preparation method is: treating with sulfuric acid with a concentration of 64% Microcrystalline cellulose Microcrystalline cellulose, the ratio of microcrystalline cellulose: H 2 SO 4 =1g:9.8ml, add a certain amount of flake graphene material and microcrystalline cellulose and concentrated sulfuric acid in proportion, acidolysis temperature is 45℃, time is 60min-120min; add deionized water to terminate the acidolysis reaction, then Carry out centrifugal washing, centrifugal speed 4000rpm, time 5min, number of times 6-8 times; then conduct dialysis to remove acid radical ions, 30% power ultrasonic treatment for 30min; cellulose nanocrystal/graphene composite material.

[0041] The one-step method for preparing highly dispersed graphene solution includes the following steps:

[0042] (1) Treat microcrystalline cellulose microcrystalline cellulose with a concentration of 64% sulfuric acid, with a ratio of microcrystalline cellulose: H 2 SO 4 =1g:9.8ml, 0.2g graphene material and 20g microcrystalline cellulose and concentrated sulfuric acid mixed solution, acidolysis temperature is 45℃, time is 60min-120min; add deionized water to terminate the acidolysis reaction;

[0043] (2) Centrifugal washing: Centrifugal washing the solution after termination of the reaction, the centrifugal speed is 4000 rpm, the time is 5 min, and the number of times is 6-8;

[0044] (3) Dialysis: Dialysis to remove acid radical ions, use 8000-10000 molecular weight dialysis bag for dialysis, keep flowing water, dialysis for 3-4 days;

[0045] (4) Ultrasonic treatment: Ultrasonic treatment for 30 minutes under 30% power condition to obtain modifier cellulose nanocrystal/sheet-like graphene suspension.

Example Embodiment

[0046] Example 2

[0047] One-step preparation of highly dispersed graphene solution, which is characterized by comprising a suspension of cellulose nanocrystals/graphene flakes; among them, a suspension of graphene flakes and cellulose nanocrystals in a cellulose nanocrystal/graphene flake suspension The mass ratio is 1-3:100.

[0048] The modifier nanocellulose is a suspension of cellulose nanocrystals/sheet-like graphene, the amount of dry matter after blending the two ranges from 20.2-20.6g, and the preparation method is: treating with sulfuric acid with a concentration of 64% Microcrystalline cellulose Microcrystalline cellulose, the ratio of microcrystalline cellulose: H 2 SO 4 =1g:9.8ml, add a certain amount of flake graphene material and microcrystalline cellulose and concentrated sulfuric acid in proportion, acidolysis temperature is 45℃, time is 60min-120min; add deionized water to terminate the acidolysis reaction, then Carry out centrifugal washing, centrifugal speed 4000rpm, time 5min, number of times 6-8 times; then conduct dialysis to remove acid radical ions, 30% power ultrasonic treatment for 30min; cellulose nanocrystal/graphene composite material.

[0049] The one-step method for preparing highly dispersed graphene solution includes the following steps:

[0050] (1) Treat microcrystalline cellulose microcrystalline cellulose with a concentration of 64% sulfuric acid, with a ratio of microcrystalline cellulose: H 2 SO 4 =1g:9.8ml, 0.3g graphene material and 20g microcrystalline cellulose and concentrated sulfuric acid mixed solution, acidolysis temperature is 45℃, time is 60min-120min; add deionized water to terminate the acidolysis reaction;

[0051] (2) Centrifugal washing: Centrifugal washing the solution after termination of the reaction, the centrifugal speed is 4000 rpm, the time is 5 min, and the number of times is 6-8;

[0052] (3) Dialysis: Dialysis to remove acid radical ions, use 8000-10000 molecular weight dialysis bag for dialysis, keep flowing water, dialysis for 3-4 days;

[0053] (4) Ultrasonic treatment: Ultrasonic treatment for 30 minutes under 30% power condition to obtain modifier cellulose nanocrystal/sheet-like graphene suspension.

Example Embodiment

[0054] Example 3

[0055] One-step preparation of highly dispersed graphene solution, which is characterized by comprising a suspension of cellulose nanocrystals/graphene flakes; among them, a suspension of graphene flakes and cellulose nanocrystals in a cellulose nanocrystal/graphene flake suspension The mass ratio is 1-3:100.

[0056] The modifier nanocellulose is a suspension of cellulose nanocrystals/sheet-like graphene, the amount of dry matter after blending the two ranges from 20.2-20.6g, and the preparation method is: treating with sulfuric acid with a concentration of 64% Microcrystalline cellulose Microcrystalline cellulose, the ratio of microcrystalline cellulose: H 2 SO 4 =1g:9.8ml, add a certain amount of flake graphene material and microcrystalline cellulose and concentrated sulfuric acid in proportion, acidolysis temperature is 45℃, time is 60min-120min; add deionized water to terminate the acidolysis reaction, then Carry out centrifugal washing, centrifugal speed 4000rpm, time 5min, number of times 6-8 times; then conduct dialysis to remove acid radical ions, 30% power ultrasonic treatment for 30min; cellulose nanocrystal/graphene composite material.

[0057] The one-step method for preparing highly dispersed graphene solution includes the following steps:

[0058] (1) Treat microcrystalline cellulose microcrystalline cellulose with a concentration of 64% sulfuric acid, with a ratio of microcrystalline cellulose: H 2 SO 4 =1g:9.8ml, 0.4g graphene material and 20g microcrystalline cellulose and concentrated sulfuric acid mixture, acidolysis temperature is 45℃, time is 60min-120min; add deionized water to terminate the acidolysis reaction;

[0059] (2) Centrifugal washing: Centrifugal washing the solution after termination of the reaction, the centrifugal speed is 4000 rpm, the time is 5 min, and the number of times is 6-8;

[0060] (3) Dialysis: Dialysis to remove acid radical ions, use 8000-10000 molecular weight dialysis bag for dialysis, keep flowing water, dialysis for 3-4 days;

[0061] (4) Ultrasonic treatment: Ultrasonic treatment for 30 minutes under 30% power condition to obtain modifier cellulose nanocrystal/sheet-like graphene suspension.

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easy to operate
The principle is simple

High-dispersion graphene solution prepared by virtue of one-step method and preparation method of high-dispersion graphene solution

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