CN105384166A - Graphene microsphere preparation method - Google Patents
Graphene microsphere preparation method Download PDFInfo
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- CN105384166A CN105384166A CN201510960743.8A CN201510960743A CN105384166A CN 105384166 A CN105384166 A CN 105384166A CN 201510960743 A CN201510960743 A CN 201510960743A CN 105384166 A CN105384166 A CN 105384166A
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Abstract
The present invention discloses a graphene microsphere preparation method, which comprises: carrying out ultrasonic dispersion on sheet-like or powdery graphene in water or alcohol, wherein the concentration is 1-3 mg/mL; after uniform dispersion, dripping the graphene solution on paper with a surface sizing agent coated on the surface through a drip tube, placing into an oven, drying, and controlling the drying temperature at 50-52 DEG C until completely drying; and peeling off the dried graphene from the paper, and granulating to obtain the graphene microspheres. According to the present invention, the structure of the prepared graphene microsphere is uniform, the diameter can be controlled through the granulating, the surface sizing agent does not provide wettability for graphene so as to make the graphene can be subjected to self-agglomeration during the drying process, and finally the granulating is performed to obtain the graphene microsphere.
Description
Technical field
The present invention relates to new material technology field, particularly a kind of method preparing Graphene microsphere.
Background technology
The research of people to the self-assembly aspect of Graphene mainly concentrates on two-dimensional material aspect, as graphene transparent conductive film, graphene membrane electrode, Graphene polymer or nano composite material etc.And it is fewer for the research of graphite three-dimensional group package material (i.e. Graphene microsphere).The special construction of Graphene microsphere makes it have a lot of excellent performance, as unreactiveness, high-bulk-density, excellent conduction and thermal conductivity etc., the aspects such as high-density high-strength material, high-performance liquid chromatography filler, support of the catalyst, drug delivery, activated carbon with high specific surface area, ion secondary battery cathode material lithium and ultracapacitor can be used as.And rarely have report so far about the preparation method of Graphene microsphere.
Summary of the invention
The present invention, in order to overcome the deficiency of above-mentioned technical problem, provides a kind of method preparing Graphene microsphere, can solve the problems of the technologies described above completely.
The technical scheme solved the problems of the technologies described above is as follows:
Prepare a method for Graphene microsphere, comprise the following steps:
By sheet or powdered graphite alkene ultrasonic disperse in water or alcohol, concentration is 1 ~ 3mg/mL, being dripped by graphene solution dropper after being uniformly dispersed scribbles on the paper of Surface Size in surface, put into baking oven, dry, drying temperature is controlled at 50 ~ 52 DEG C, till oven dry, again the Graphene of drying is peeled off from paper, carry out granulation, obtain Graphene microsphere.
Described Surface Size is become by following components in mass portion array: alkyl ketene dimer 12-18 part, dimethyl diallyl ammonium chloride 20-30 part, rosin 5-10 part, sodium hydroxide 2-4 part, oxidic polyethylene 8-20 part, silver suboxide 1-2 part, calcium oxide 2-5 part, zinc oxide 4-7 part, starch 3-7 part.
Graphene microsphere structure prepared by the present invention is even, and diameter controls by granulation, because Surface Size has not wetting property to Graphene, makes Graphene in drying process, can reunite voluntarily, namely obtain Graphene microsphere finally by granulation.Do not need to recombinate to graphene molecules structure as oxide-reduction method before and after preparation, security is high, and method is simple and reliable, and energy consumption is low.
Embodiment
Below in conjunction with embodiment, the present invention is further detailed explanation.
Embodiment 1:
Prepare a method for Graphene microsphere, comprise the following steps:
By sheet or powdered graphite alkene ultrasonic disperse in water or alcohol, concentration is 1mg/mL, being dripped by graphene solution dropper after being uniformly dispersed scribbles on the paper of Surface Size in surface, put into baking oven, dry, drying temperature is controlled at 50 ~ 52 DEG C, till oven dry, again the Graphene of drying is peeled off from paper, carry out granulation, obtain Graphene microsphere.
Described Surface Size is become by following components in mass portion array: alkyl ketene dimer 12 parts, dimethyl diallyl ammonium chloride 20 parts, rosin 5 parts, 2 parts, sodium hydroxide, oxidic polyethylene 8 parts, silver suboxide 1 part, 2 parts, calcium oxide, 4 parts, zinc oxide, starch 3 parts.
Embodiment 2:
Prepare the method for Graphene microsphere, comprise the following steps:
By sheet or powdered graphite alkene ultrasonic disperse in water or alcohol, concentration is 3mg/mL, being dripped by graphene solution dropper after being uniformly dispersed scribbles on the paper of Surface Size in surface, put into baking oven, dry, drying temperature is controlled at 50 ~ 52 DEG C, till oven dry, again the Graphene of drying is peeled off from paper, carry out granulation, obtain Graphene microsphere.
Described Surface Size is become by following components in mass portion array: alkyl ketene dimer 18 parts, dimethyl diallyl ammonium chloride 30 parts, rosin 10 parts, 4 parts, sodium hydroxide, oxidic polyethylene 20 parts, silver suboxide 2 parts, 5 parts, calcium oxide, 7 parts, zinc oxide, starch 7 parts.
Embodiment 3:
Prepare the method for Graphene microsphere, comprise the following steps:
By sheet or powdered graphite alkene ultrasonic disperse in water or alcohol, concentration is 2mg/mL, being dripped by graphene solution dropper after being uniformly dispersed scribbles on the paper of Surface Size in surface, put into baking oven, dry, drying temperature is controlled at 50 ~ 52 DEG C, till oven dry, again the Graphene of drying is peeled off from paper, carry out granulation, obtain Graphene microsphere.
Described Surface Size is become by following components in mass portion array: alkyl ketene dimer 15 parts, dimethyl diallyl ammonium chloride 25 parts, rosin 7 parts, 3 parts, sodium hydroxide, oxidic polyethylene 14 parts, silver suboxide 1.5 parts, 3 parts, calcium oxide, 5 parts, zinc oxide, starch 6 parts.
Graphene microsphere structure prepared by the present invention is even, and diameter controls by granulation, because Surface Size has not wetting property to Graphene, makes Graphene in drying process, can reunite voluntarily, namely obtain Graphene microsphere finally by granulation.Do not need to recombinate to graphene molecules structure as oxide-reduction method before and after preparation, security is high, and method is simple and reliable, and energy consumption is low.
The above is only preferred embodiment of the present invention, not does any pro forma restriction to the present invention, every according in technical spirit of the present invention to any simple modification, equivalent variations that above embodiment is done, all fall within protection scope of the present invention.
Claims (2)
1. prepare a method for Graphene microsphere, it is characterized in that, comprise the following steps:
By sheet or powdered graphite alkene ultrasonic disperse in water or alcohol, concentration is 1 ~ 3mg/mL, being dripped by graphene solution dropper after being uniformly dispersed scribbles on the paper of Surface Size in surface, put into baking oven, dry, drying temperature is controlled at 50 ~ 52 DEG C, till oven dry, again the Graphene of drying is peeled off from paper, carry out granulation, obtain Graphene microsphere.
2. a kind of method preparing Graphene microsphere according to claim 1, it is characterized in that, described Surface Size is become by following components in mass portion array: alkyl ketene dimer 12-18 part, dimethyl diallyl ammonium chloride 20-30 part, rosin 5-10 part, sodium hydroxide 2-4 part, oxidic polyethylene 8-20 part, silver suboxide 1-2 part, calcium oxide 2-5 part, zinc oxide 4-7 part, starch 3-7 part.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510960743.8A CN105384166A (en) | 2015-12-21 | 2015-12-21 | Graphene microsphere preparation method |
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| CN201510960743.8A CN105384166A (en) | 2015-12-21 | 2015-12-21 | Graphene microsphere preparation method |
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| CN105384166A true CN105384166A (en) | 2016-03-09 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106185904A (en) * | 2016-07-15 | 2016-12-07 | 浙江大学 | A kind of high fold graphene paper |
| CN106185906A (en) * | 2016-07-15 | 2016-12-07 | 浙江大学 | A kind of Graphene elastic film and preparation method thereof |
| CN107651672A (en) * | 2017-10-13 | 2018-02-02 | 杭州高烯科技有限公司 | A kind of preparation method of Ultralight graphene microballoon for solar absorption |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102515152A (en) * | 2011-12-23 | 2012-06-27 | 深圳市贝特瑞纳米科技有限公司 | Method for preparing spheroidal graphene |
| CN102815697A (en) * | 2012-08-28 | 2012-12-12 | 中国科学院过程工程研究所 | Preparation method of graphene oxide microspheres |
| KR20140085870A (en) * | 2012-12-28 | 2014-07-08 | 전자부품연구원 | Graphene composite for water treatment |
| CN104372713A (en) * | 2013-08-13 | 2015-02-25 | 陆伟明 | High efficient surface sizing agent |
-
2015
- 2015-12-21 CN CN201510960743.8A patent/CN105384166A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102515152A (en) * | 2011-12-23 | 2012-06-27 | 深圳市贝特瑞纳米科技有限公司 | Method for preparing spheroidal graphene |
| CN102815697A (en) * | 2012-08-28 | 2012-12-12 | 中国科学院过程工程研究所 | Preparation method of graphene oxide microspheres |
| KR20140085870A (en) * | 2012-12-28 | 2014-07-08 | 전자부품연구원 | Graphene composite for water treatment |
| CN104372713A (en) * | 2013-08-13 | 2015-02-25 | 陆伟明 | High efficient surface sizing agent |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106185904A (en) * | 2016-07-15 | 2016-12-07 | 浙江大学 | A kind of high fold graphene paper |
| CN106185906A (en) * | 2016-07-15 | 2016-12-07 | 浙江大学 | A kind of Graphene elastic film and preparation method thereof |
| CN106185906B (en) * | 2016-07-15 | 2019-01-01 | 浙江大学 | A kind of graphene elastic film and preparation method thereof |
| CN107651672A (en) * | 2017-10-13 | 2018-02-02 | 杭州高烯科技有限公司 | A kind of preparation method of Ultralight graphene microballoon for solar absorption |
| CN107651672B (en) * | 2017-10-13 | 2019-11-22 | 杭州高烯科技有限公司 | A kind of preparation method of the Ultralight graphene microballoon for solar absorption |
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Application publication date: 20160309 |