CN111635540A - Preparation method of graphene oily slurry - Google Patents
Preparation method of graphene oily slurry Download PDFInfo
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- CN111635540A CN111635540A CN202010447822.XA CN202010447822A CN111635540A CN 111635540 A CN111635540 A CN 111635540A CN 202010447822 A CN202010447822 A CN 202010447822A CN 111635540 A CN111635540 A CN 111635540A
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- graphene
- resin
- oily slurry
- preparation
- stirring
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/20—Compounding polymers with additives, e.g. colouring
- C08J3/205—Compounding polymers with additives, e.g. colouring in the presence of a continuous liquid phase
- C08J3/2053—Compounding polymers with additives, e.g. colouring in the presence of a continuous liquid phase the additives only being premixed with a liquid phase
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2363/00—Characterised by the use of epoxy resins; Derivatives of epoxy resins
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2491/00—Characterised by the use of oils, fats or waxes; Derivatives thereof
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
- C08K3/042—Graphene or derivatives, e.g. graphene oxides
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/05—Alcohols; Metal alcoholates
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/05—Alcohols; Metal alcoholates
- C08K5/053—Polyhydroxylic alcohols
Abstract
A preparation method of graphene oily slurry comprises the steps of putting graphene into a mixing barrel, adding dispersion liquid, adding a mixed solution of two or more resin diluents, adding resin, and sanding at a high speed for a set time to obtain the graphene oily slurry with uniform dispersion. The graphene slurry obtained by the invention has the advantage of uniform dispersion, is a low-cost preparation method, and has a good application prospect.
Description
Technical Field
The invention relates to a preparation method of graphene oil slurry.
Background
Graphene is a sp2 hybridized two-dimensional material with close packed monolayer carbon atoms, and is widely researched due to the unique structure and excellent electrical, optical, mechanical and thermal properties. 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.
Disclosure of Invention
In order to solve the problems in the prior art, the invention aims to provide a preparation method of graphene oily slurry, and in order to prepare the graphene oily slurry, a large amount of experiments and researches prove that graphene is mixed with oily resin slurry by using a sand mill, so that the graphene can be more uniformly dispersed in the oily slurry, and the uniformly dispersed graphene oily slurry is obtained.
In order to solve the technical problems, the invention provides the following technical scheme:
a preparation method of graphene oily slurry comprises the steps of putting graphene into a mixing barrel, adding dispersion liquid, adding a mixed solution of two or more resin diluents, adding resin, and sanding at a high speed for a set time to obtain the graphene oily slurry with uniform dispersion.
Further, the resin diluent is ethylene glycol, glycerol, butanol and No. 1000 solvent oil.
The resin is epoxy resin.
Preferably, the graphene and the dispersing agent are uniformly dispersed in the diluent by mechanical stirring, the stirring time is 10-20 min, and the rotating speed is 400-600 rpm; and adding resin, and continuing stirring at the rotation speed of 1000-1500 rpm for 15-20 min. And starting the sand mill, wherein the set time of high-speed sanding of the sand mill is 20-25 min, and the rotating speed is 1000-1500 rpm.
In summary, the invention provides a preparation method of graphene oily slurry, which comprises the steps of firstly putting graphene into a mixing barrel, adding a dispersion liquid and a mixed liquid of two or more resin diluents, adding resin, and setting a period of time through a sand mill to obtain graphene oily slurry with uniform dispersion. The obtained graphene slurry has the advantage of uniform dispersion, is a low-cost preparation method, and has a good application prospect.
Detailed Description
The invention will now be further illustrated by the following examples, without limiting the scope of the invention thereto.
Example 1
The conditions adopted in this example: the rotation speed of the sand mill is 1500rpm, the consumption of zirconium beads is 2.0kg, and the time is 25 min.
Weighing 120g of graphene in a mixing barrel, adding 6g of dispersion liquid, adding 1.5kg of mixed solution of resin diluent, wherein the resin diluent is ethylene glycol and glycerol, stirring for 15min by using a stirring paddle at the rotation speed of 500rpm to better disperse the graphene in the mixed solution, adding 1.5kg of epoxy resin, and stirring for 20min at the rotation speed of 1000 rpm. The time of the sand mill is 25min, and the rotating speed of the sand mill is 1500rpm, so that the graphene oil-based slurry with uniform dispersion can be obtained.
Example 2
The conditions adopted in this example: the rotation speed of the sand mill is 1200rpm, the consumption of zirconium beads is 2.0kg, and the time is 20 min.
Weighing 200g of graphene in a mixing barrel, adding 10g of dispersion liquid, adding 2.5kg of mixed liquid of resin diluent, wherein the resin diluent is butanol and No. 1000 solvent oil, stirring for 20min by using a stirring paddle at the rotating speed of 400rpm to better disperse the graphene in the mixed liquid, adding 2.5kg of epoxy resin, and stirring for 18min at the rotating speed of 1200 rpm. The time of the sand mill is 20min, and the rotating speed of the sand mill is 1200rpm, so that the graphene oil-based slurry with uniform dispersion can be obtained.
Example 3
The conditions adopted in this example: the rotation speed of the sand mill is 1000rpm, the consumption of zirconium beads is 2.0kg, and the time is 22 min.
Weighing 200g of graphene in a mixing barrel, adding 10g of dispersion liquid, adding 2.5kg of mixed liquid of resin diluent, wherein the resin diluent is ethylene glycol, butanol and No. 1000 solvent oil, stirring for 10min by using a stirring paddle at the rotating speed of 600rpm to better disperse the graphene in the mixed liquid, adding 2.5kg of epoxy resin, and stirring for 15min at the rotating speed of 1500 rpm. The time of the sand mill is 25min, and the rotating speed of the sand mill is 1000rpm, so that the graphene oil-based slurry with uniform dispersion can be obtained.
Comparative example:
the conditions adopted in this comparative example were: stirring with a stirring paddle at 1500rpm for 40 min.
Weighing 120g of graphene in a mixing barrel, adding 6g of dispersion liquid, adding 1.5kg of resin diluent mixed liquid, stirring for 10min by using a stirring paddle at the rotating speed of 500rpm to better disperse the graphene in the mixed liquid, and adding 1.5kg of epoxy resin; stirring is carried out for 40min all the time, and the stirring speed is 1500 rpm. And obtaining the graphene oily slurry.
The mixed liquid is subjected to high-speed sanding, so that the dispersion degree of the graphene oily slurry can be effectively improved, the fineness of the graphene oily slurry obtained in the three previous examples is concentrated between 40 and 60 mu m, and the fineness of the graphene oily slurry obtained in the comparative example is more than 100 mu m by only using a stirring method and not subjected to high-speed sanding.
In the above embodiments, to verify the effect of the sanding method in preparing the graphene slurry, any modification, equivalence, replacement, and improvement on the material ratio and the process method related to the present invention should be included in the scope of the present invention.
Claims (5)
1. A preparation method of graphene oily slurry is characterized by firstly putting graphene into a mixing barrel, adding dispersion liquid, adding a mixed solution of two or more resin diluents, adding resin, and sanding at a high speed for a set time to obtain the graphene oily slurry with uniform dispersion.
2. The method of claim 1, wherein the resin diluent is selected from the group consisting of ethylene glycol, glycerol, butanol, and mineral spirits No. 1000.
3. The method for preparing graphene oily slurry according to claim 1 or 2, wherein the resin is an epoxy resin.
4. The preparation method of the graphene oily slurry as claimed in claim 1 or 2, wherein the graphene and the dispersant are uniformly dispersed in the diluent by mechanical stirring, the stirring time is 10-20 min, and the rotation speed is 400-600 rpm; and adding resin, and continuing stirring at the rotation speed of 1000-1500 rpm for 15-20 min.
5. The method for preparing graphene oily slurry according to claim 1 or 2, wherein the set time of high-speed sanding of a sanding machine is 20-25 min, and the rotating speed is 1000-1500 rpm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010447822.XA CN111635540A (en) | 2020-05-25 | 2020-05-25 | Preparation method of graphene oily slurry |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010447822.XA CN111635540A (en) | 2020-05-25 | 2020-05-25 | Preparation method of graphene oily slurry |
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| Publication Number | Publication Date |
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| CN111635540A true CN111635540A (en) | 2020-09-08 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN202010447822.XA Pending CN111635540A (en) | 2020-05-25 | 2020-05-25 | Preparation method of graphene oily slurry |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104163928A (en) * | 2014-08-25 | 2014-11-26 | 鸿纳（东莞）新材料科技有限公司 | Conductive heat-conductive graphene slurry and coating |
| CN105969024A (en) * | 2016-06-27 | 2016-09-28 | 上海多希石墨烯材料科技有限公司 | Heat conduction coating material with physically stripped graphene and method for preparing heat conduction coating material |
| CN107298924A (en) * | 2017-07-06 | 2017-10-27 | 深圳市国创珈伟石墨烯科技有限公司 | A kind of graphene conductive slurry and preparation method thereof, application process |
| WO2017219944A1 (en) * | 2016-06-20 | 2017-12-28 | 山东欧铂新材料有限公司 | Method for preparing graphene-epoxy resin composite material |
-
2020
- 2020-05-25 CN CN202010447822.XA patent/CN111635540A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104163928A (en) * | 2014-08-25 | 2014-11-26 | 鸿纳（东莞）新材料科技有限公司 | Conductive heat-conductive graphene slurry and coating |
| WO2017219944A1 (en) * | 2016-06-20 | 2017-12-28 | 山东欧铂新材料有限公司 | Method for preparing graphene-epoxy resin composite material |
| CN105969024A (en) * | 2016-06-27 | 2016-09-28 | 上海多希石墨烯材料科技有限公司 | Heat conduction coating material with physically stripped graphene and method for preparing heat conduction coating material |
| CN107298924A (en) * | 2017-07-06 | 2017-10-27 | 深圳市国创珈伟石墨烯科技有限公司 | A kind of graphene conductive slurry and preparation method thereof, application process |
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Application publication date: 20200908 |