CN111826054A

CN111826054A - Preparation method of low-fineness graphene oil-based resin slurry

Info

Publication number: CN111826054A
Application number: CN202010710846.XA
Authority: CN
Inventors: 张�诚; 罗俊涛; 刘军磊; 许林铁
Original assignee: Zhejiang University of Technology ZJUT
Current assignee: Zhejiang University of Technology ZJUT
Priority date: 2020-07-22
Filing date: 2020-07-22
Publication date: 2020-10-27

Abstract

The invention relates to a preparation method of low-fineness graphene oil resin slurry, which comprises the following steps: and uniformly mixing the resin diluent according to a ratio, sequentially adding the graphene, the resin and the concentrated solution, and performing low-speed sanding on the obtained mixed solution for 5-20 min at 800-1600 rpm and then performing high-speed sanding at 1800-2700 rpm for 20-45 min by using a sanding machine to obtain the low-fineness graphene oleoresin slurry. The invention has the following beneficial effects: the invention provides a preparation method of low-fineness graphene oil-based resin slurry, and the obtained graphene slurry is uniform in dispersion, low in fineness, simple to operate, low in auxiliary agent consumption, low in cost and good in application prospect.

Description

Preparation method of low-fineness graphene oil-based resin slurry

(I) technical field

The invention relates to a preparation method of low-fineness graphene oil-based resin slurry.

(II) background of the invention

Graphene is a sp2 hybridized two-dimensional crystal material with tightly packed single-layer carbon atoms, and has a unique structure, so that excellent electrical, optical, mechanical and thermal properties become important for many researches.

The particle size of graphene is small, and the lamellae are extremely easy to stack and difficult to disperse uniformly due to the strong van der Waals acting force formed by the conjugated structure among the lamellae. When the organic compound is attached to the surface of the graphene, the surface energy of the graphene can be reduced, so that the agglomeration of the graphene is reduced. The preparation of the graphene slurry is a good industrial application approach, and can improve the dispersibility of graphene in various systems and enhance the comprehensive properties of various materials, such as electric conduction, heat conduction, mechanics and the like.

Disclosure of the invention

The invention aims to provide a preparation method of low-fineness graphene oil-based resin slurry.

The technical scheme adopted by the invention is as follows:

a method of preparing a low-fineness graphene oil-based resin slurry, the method comprising: and uniformly mixing the resin diluent according to a ratio, sequentially adding the graphene, the resin and the concentrated solution, and performing low-speed sanding on the obtained mixed solution for 5-20 min at 800-1600 rpm and then performing high-speed sanding at 1800-2700 rpm for 20-45 min by using a sanding machine to obtain the low-fineness graphene oleoresin slurry.

The inventor finds that the fineness of the graphene oleoresin slurry can be effectively reduced by mixing the graphene with the oleoresin slurry through a sand mill and alternately sanding at a low speed and a high speed through the sand mill, so that the graphene oleoresin slurry with the low fineness is obtained.

Preferably, the resin diluent is a mixture of two or more of the following: butanol, No. 1000 solvent oil, methanol, ethyl acetate and toluene. More preferably, the resin diluent is a mixture of butanol and No. 1000 solvent oil in a mass ratio of 1: 0.5-1: 4 in the presence of a solvent.

Specifically, the amount of zirconium beads used in the sand mill is 2-3.5 kg.

Preferably, the resin is an epoxy resin.

Specifically, the graphene is uniformly dispersed in the diluent by mechanical stirring, the stirring time is 2-7 min, and the rotating speed is 400-1100 rpm; adding resin, and continuing stirring at the rotation speed of 800-2000 rpm for 10-25 min; and finally, adding the concentrated solution under stirring at 800-2000 rpm (the adding time is 2-5 min).

The concentrated solution is prepared by dissolving one or more of antioxidant 702, 3-bithiophene, EDOT, n-dodecyl p-hydroxybenzoate and sodium dodecyl sulfate as solutes in a mixed solution of one or more of methanol, toluene, ethanol, ethylene glycol, glycerol, butanol and No. 1000 solvent naphtha, wherein the mass ratio of the solutes to the solvents is 1: 3-8.

The invention has the following beneficial effects: the invention provides a preparation method of low-fineness graphene oil-based resin slurry, and the obtained graphene slurry is uniform in dispersion, low in fineness, simple to operate, less in auxiliary agent material consumption, low in cost and good in application prospect.

(IV) description of the drawings

FIG. 1 is a schematic flow chart of the present invention.

(V) detailed description of the preferred embodiments

The invention will be further described with reference to specific examples, but the scope of the invention is not limited thereto:

example 1:

the conditions adopted in this example: the setting time of the low-speed sanding of the sand mill is 10min, the rotating speed is 1000rpm, the setting time of the high-speed sanding of the sand mill is 35min, and the rotating speed is 2400 rpm. The amount of zirconium beads was 2 kg.

Referring to fig. 1, 0.75kg of butanol and 0.75kg of solvent oil No. 1000 (shanghai refinery chemical limited) are weighed into a charging bucket, 120g of graphene is added, and the mixture is stirred with a stirring paddle for 3min at a rotation speed of 700rpm, so that the graphene is well dispersed in the mixed solution. Then adding 1.5kg of epoxy resin, stirring with a stirring paddle for 15min at the rotation speed of 1000rpm, continuing stirring, and adding 26g of concentrated solution (prepared by dissolving 3.6g of antioxidant 702 (Taishiai (Shanghai) chemical industry development Co., Ltd.) in 11.2g of butanol and 7.9g of No. 1000 solvent oil) during stirring (the adding time of the concentrated solution is about 2 min). And starting a sand mill, firstly carrying out low-rotation-speed sanding at the rotation speed of 1000rpm for 10min, and then carrying out high-rotation-speed sanding at the rotation speed of 2400rpm for 35min to obtain the low-fineness graphene slurry.

Example 2:

the conditions adopted in this example: the setting time of the low-speed sanding of the sand mill is 12min, the rotating speed is 1200rpm, the setting time of the high-speed sanding of the sand mill is 30min, and the rotating speed is 2100 rpm. The amount of zirconium beads was 2.4 kg.

Weighing 0.75kg of butanol and 0.75kg of No. 1000 solvent oil into a feeding barrel, adding 120g of graphene, stirring for 5min by using a stirring paddle at the rotating speed of 900rpm, and well dispersing the graphene in the mixed solution. Adding 1.5kg epoxy resin, stirring with stirring slurry at 1400rpm for 20min, stirring, and slowly adding 26g concentrated solution (prepared by dissolving 3.6g antioxidant 702 in 11.2g butanol and 7.9g No. 1000 solvent oil) while stirring. And starting the sand mill, and performing low-speed sanding at the rotation speed of 1200rpm for 12 min. And then sanding at a high rotating speed of 2100rpm for 30min to obtain the low-fineness graphene slurry.

Example 3:

the conditions adopted in this example: the setting time of the low-speed sanding of the sand mill is 12min, the rotating speed is 1300rpm, the setting time of the high-speed sanding of the sand mill is 30min, and the rotating speed is 2450 rpm. The amount of zirconium beads was 2.3 kg.

Weighing 1.5kg of butanol and 1.5kg of No. 1000 solvent oil into a feeding barrel, adding 140g of graphene, and stirring for 5min by using a stirring paddle at the rotating speed of 900rpm to better disperse the graphene in the mixed solution. Adding 0.5kg epoxy resin, stirring with stirring slurry at 1400rpm for 20min, stirring, and adding 20g concentrated solution (prepared by dissolving 4.2g antioxidant 702 in 7.9g butanol and 7.9g No. 1000 solvent oil) while stirring. And starting the sand mill, and performing low-speed sanding at the rotation speed of 1200rpm for 12 min. And then sanding at a high rotating speed of 2100rpm for 30min to obtain the low-fineness graphene slurry.

Comparative example 1:

the conditions adopted in this comparative example were: stirring with stirring paddle at 1000rpm for 40 min.

Weighing 0.75kg of butanol and 0.75kg of No. 1000 solvent oil into a feeding barrel, adding 120g of graphene, stirring for 5min by using a stirring paddle at the rotating speed of 900rpm, and well dispersing the graphene in the mixed solution. Then adding 1.5kg of epoxy resin, stirring with a stirring paddle for 20min at the rotation speed of 1400rpm, continuing stirring, and adding 26g of concentrated solution (prepared by dissolving 4.2g of antioxidant 702 in 7.9g of butanol and 7.9g of No. 1000 solvent oil) during stirring. Stirring for 40 min.

Comparative example 2:

the conditions adopted in this comparative example were: the rotation speed of the sand mill is 1100rpm, the consumption of the zirconium beads is 2.0kg, and the time is 40 min.

Weighing 0.75kg of butanol and 0.75kg of No. 1000 solvent oil into a feeding barrel, adding 120g of graphene, stirring for 5min by using a stirring paddle at the rotating speed of 900rpm, and well dispersing the graphene in the mixed solution. Adding 1.5kg epoxy resin, stirring with stirring slurry at 1400rpm for 20min, stirring, and slowly adding 26g concentrated solution (prepared by dissolving 4.2g antioxidant 702 in 7.9g butanol and 7.9g No. 1000 solvent oil) while stirring. The sand mill was started and sanding was performed at 1600rpm for 40 min.

The mixed solution is alternately sanded at low speed and high speed, so that the dispersity of the graphene oily slurry can be effectively improved, the fineness of the graphene oily slurry obtained in the three previous embodiments is 25-35 mu m, and the fineness of the graphene oily slurry obtained in the comparative example 1 is more than 100 mu m by only using a stirring method and not performing high-speed sanding. The graphene oil-based slurry obtained by the method of comparative example 2 through sanding at only one rotating speed has fineness concentrated between 45 and 60 mu m. According to the invention, the fineness of the graphene oleoresin slurry can be effectively reduced by alternately sanding at low speed and high speed by the sand mill.

In the above embodiments, in order to verify the effect of the sanding method in reducing the fineness of the graphene slurry, any modification, equivalence, replacement and improvement, etc. in the material ratio and the process method according to the present invention should be included in the protection scope of the present invention.

Claims

1. A method of preparing a low-fineness graphene oil-based resin slurry, the method comprising: and uniformly mixing the resin diluent according to a ratio, sequentially adding the graphene, the resin and the concentrated solution, and performing low-speed sanding on the obtained mixed solution for 5-20 min at 800-1600 rpm and then performing high-speed sanding at 1800-2700 rpm for 20-45 min by using a sanding machine to obtain the low-fineness graphene oleoresin slurry.

2. The method according to claim 1, wherein the resin diluent is a mixture of two or more of: butanol, No. 1000 solvent oil, methanol, ethyl acetate and toluene.

3. The method according to claim 2, wherein the resin diluent is a mixture of butanol and 1000 # solvent oil in a mass ratio of 1: 0.5-1: 4.

4. The method of claim 1, wherein: the amount of zirconium beads used in the sand mill is 2-3.5 kg.

5. The method of claim 1, wherein the resin is an epoxy resin.

6. The method according to claim 1, wherein graphene is uniformly dispersed in the diluent by mechanical stirring, wherein the stirring time is 2-7 min, and the rotation speed is 400-1100 rpm; adding resin, and continuing stirring at the rotation speed of 800-2000 rpm for 10-25 min; and finally adding the concentrated solution while stirring at 800-2000 rpm.

7. The method of claim 1, wherein the concentrate is prepared by dissolving one or more of antioxidant 702, 3-bithiophene, EDOT, n-dodecyl p-hydroxybenzoate, and sodium dodecyl sulfate in a mixture of one or more of methanol, toluene, ethanol, ethylene glycol, glycerol, butanol, and No. 1000 mineral spirits.