CN112408374A - Method for reducing graphene agglomeration - Google Patents
Method for reducing graphene agglomeration Download PDFInfo
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- CN112408374A CN112408374A CN202011353717.6A CN202011353717A CN112408374A CN 112408374 A CN112408374 A CN 112408374A CN 202011353717 A CN202011353717 A CN 202011353717A CN 112408374 A CN112408374 A CN 112408374A
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- 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
Abstract
The invention provides a method for reducing graphene agglomeration, which comprises the steps of adding a modifier into graphene powder, adding water, uniformly stirring, homogenizing by a homogenizer, and spray-drying the obtained turbid liquid to obtain the required graphene; the graphene obtained by the treatment of the method has the advantage of low agglomeration, and meanwhile, the method is a low-cost preparation method and has a good application prospect.
Description
Technical Field
The invention relates to the technical field of graphene, in particular to a method for reducing graphene agglomeration.
Background
Graphene is a two-dimensional material which is formed by carbon atoms in a planar hybrid orbit into a hexagonal honeycomb structure and has the thickness of only a single carbon atom, and is one of the thinnest and hardest nano materials known in the world.
Graphene has a huge application prospect, so that a method which is high in quality, less in pollution and easy to prepare is urgently needed to be found to meet the application requirement of the currently vigorously developed graphene, the current method for producing graphene on a large scale at home and abroad mainly adopts a chemical method and a physical method, and the graphene is easy to agglomerate due to the fact that the graphene has a large specific surface area. The physical and chemical properties of the material are much smaller than the theoretical value, and the application of the material in practice is limited.
Disclosure of Invention
Aiming at the problem that the graphene is easy to agglomerate in the preparation process, the invention aims to provide a method for reducing the agglomeration of the graphene. After a large amount of experimental exploration, the invention discovers that the low-aggregation graphene can be obtained by effectively improving the aggregation of the graphene by mixing the graphene with the modifier.
The technical scheme of the invention is as follows:
a method for reducing graphene agglomeration, the method comprising:
mixing graphene powder, a modifier and water, stirring uniformly, homogenizing by a homogenizer, and then carrying out spray drying to obtain finished product powder;
the mass ratio of the graphene powder to the modifier to the water is 1: 0.01-0.1: 20-100 parts of;
the modifier is selected from: (E) -cyclooct-2-en-1-yl (4-nitrophenyl) carbonate, 2-bromobicyclo [2,2,1] heptane, potassium pentyltrichloroborate, n-butyl thiophosphoric triamide, aminotrimethylene phosphonic acid, antioxidant 702, benzyltrimethylsilane, 3' -dithiobis (propan-1-ol), tetraisopropyl methylenediphosphate, cyanomethylene tri-n-butylphosphine, or a mixture of two or more thereof in any proportion;
the graphene powder can be prepared by a known high-pressure liquid phase stripping method, and the preparation method of the graphene powder is not limited;
preferably, when the graphene powder, the modifier and water are mixed, the modifier is added into the graphene powder, and then the water is added for mixing; preferably, the modifier is dissolved in ethanol first and then fed;
mixing the graphene powder, the modifier and water, and stirring at the speed of 300-800 rpm/min for 3-40 min;
the working parameters of the homogenizer are as follows: the pressure is 550-650 bar, the preferable number of times of homogenization is 1-3 times, and each time lasts for 5-10 min;
the working parameters of the spray drying are as follows: the inlet temperature is 130-190 ℃, and the wind speed is 60-200 m2The peristaltic speed is 300-800 ml/h.
The invention has the beneficial effects that:
the invention provides a method for reducing graphene agglomeration, which comprises the steps of adding a modifier into graphene powder, adding water, uniformly stirring, homogenizing by a homogenizer, and spray-drying the obtained turbid liquid to obtain the required graphene. The graphene obtained by the treatment of the method has the advantage of low agglomeration, and meanwhile, the method is a low-cost preparation method and has a good application prospect.
Drawings
FIG. 1: SEM image of the powder obtained in example 1.
FIG. 2: SEM image of the powder obtained in example 2.
FIG. 3: SEM image of the powder obtained in comparative example 1.
Detailed Description
The invention is further described below by means of specific examples, without restricting its scope to these.
Example 1
(1) Weighing 25g of powder graphene obtained by a high-pressure liquid phase stripping method, weighing 0.75g of antioxidant 702 in a small beaker, adding 10mL of ethanol for dissolving, and adding the obtained solution into the powder graphene.
(2) 975g of water is weighed and added into the graphene, and the graphene is stirred at a constant speed by a stirrer, wherein the rotating speed is 450rpm/min, and the time is 5 min.
(3) The stirred suspension was poured into a homogenizer set at a pressure of 600bar for two cycles of approximately 15 min.
(4) And (4) carrying out spray drying on the homogenized suspension to obtain the required graphene. During spray drying, the inlet temperature is 160 ℃, and the air speed is 120m2The peristaltic speed was 450 ml/h.
Example 2
(1) Weighing 25g of powder graphene obtained by a high-pressure liquid phase stripping method, weighing 1.25g of antioxidant 702 in a small beaker, adding 17mL of ethanol for dissolving, and adding the obtained solution into the powder graphene.
(2) 975g of water is weighed and added into the powder graphene, and the mixture is stirred at a constant speed of 450rpm/min for 5min by a stirrer.
(3) The stirred suspension was poured into a homogenizer set at a pressure of 600bar for about 8min for one cycle.
(4) And (4) carrying out spray drying on the homogenized suspension to obtain the required graphene. During spray drying, the inlet temperature is 160 degrees, and the wind speed is 120m2The peristaltic speed was 450 ml/h.
Comparative example 1: treatment of powdered graphene without addition of modifier
(1) Weighing 25g of powder graphene obtained by a high-pressure liquid phase stripping method, and weighing 10mL of ethanol solution to be added into the powder graphene.
(2) 975g of water is weighed and added into the powder graphene, and the mixture is stirred at a constant speed of 450rpm/min for 5min by a stirrer.
(3) And pouring the stirred suspension into a homogenizer, wherein the pressure of the homogenizer is set to be 600 bar. One cycle, approximately 8 min.
(4) And (4) carrying out spray drying on the homogenized suspension to obtain the required graphene. During spray drying, the inlet temperature is 160 degrees, and the wind speed is 120m2The peristaltic speed was 450 ml/h.
From the above examples, it can be found that the difference between the particle sizes of the graphene before and after drying is reduced and the agglomeration phenomenon of the graphene after drying is reduced by modifying the graphene, and the results are shown in the following table.
| Particle size of the slurry (μm) | Particle size of powder (mum) | Difference (μm) | |
| Example 1 | 5.260 | 5.500 | 0.240 |
| Example 2 | 6.023 | 6.235 | 0.212 |
| Comparative example 1 | 5.250 | 7.614 | 2.364 |
SEM comparative photographs of the powders obtained in example 1, example 2 and comparative example 1 are shown in figures 1 to 3.
In the above embodiments, any modification, equivalence, replacement improvement, etc. made within the scope of the material ratio and the process manner related to the present invention should be included in the protection scope of the present invention to verify the effect of the small molecule in improving the graphene.
Claims (5)
1. A method for reducing graphene agglomeration is characterized by comprising the following steps:
mixing graphene powder, a modifier and water, stirring uniformly, homogenizing by a homogenizer, and then carrying out spray drying to obtain finished product powder;
the mass ratio of the graphene powder to the modifier to the water is 1: 0.01-0.1: 20-100 parts of;
the modifier is selected from: (E) -cyclooct-2-en-1-yl (4-nitrophenyl) carbonate, 2-bromobicyclo [2,2,1] heptane, potassium pentyltrichloroborate, n-butyl thiophosphoric triamide, aminotrimethylene phosphonic acid, antioxidant 702, benzyltrimethylsilane, 3' -dithiobis (propan-1-ol), tetraisopropyl methylenediphosphate, cyanomethylene tri-n-butylphosphine, or a mixture of two or more thereof in any proportion.
2. The method for reducing graphene agglomeration according to claim 1, wherein when the graphene powder, the modifier and water are mixed, the modifier is dissolved in ethanol and then added into the graphene powder, and then the graphene powder is mixed with water.
3. The method for reducing graphene agglomeration according to claim 1, wherein the graphene powder, the modifier and water are mixed and then stirred at a speed of 300-800 rpm/min for 3-40 min.
4. The method of reducing graphene agglomeration according to claim 1, wherein the operating parameters of the homogenizer are: homogenizing for 1-3 times at 550-650 bar pressure for 5-10 min each time.
5. The method of reducing graphene agglomeration according to claim 1, wherein the operating parameters of the spray drying are: the inlet temperature is 130-190 ℃, and the wind speed is 60-200 m2The peristaltic speed is 300-800 ml/h.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113462202A (en) * | 2021-06-24 | 2021-10-01 | 浙江工业大学 | Method for improving dispersion effect of graphene in acrylic emulsion |
| CN113817369A (en) * | 2021-08-19 | 2021-12-21 | 杭州烯鲸新材料科技有限公司 | Preparation method and application of graphene-water-based acrylic acid anticorrosive coating |
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| CN113817369A (en) * | 2021-08-19 | 2021-12-21 | 杭州烯鲸新材料科技有限公司 | Preparation method and application of graphene-water-based acrylic acid anticorrosive coating |
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Application publication date: 20210226 |