CN104556007A - Equipment and process for producing graphene by spray drying and microwaves - Google Patents
Equipment and process for producing graphene by spray drying and microwaves Download PDFInfo
- Publication number
- CN104556007A CN104556007A CN201410846369.4A CN201410846369A CN104556007A CN 104556007 A CN104556007 A CN 104556007A CN 201410846369 A CN201410846369 A CN 201410846369A CN 104556007 A CN104556007 A CN 104556007A
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- microwave
- graphene
- spray drying
- kiln
- equipment
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 56
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 37
- 238000000034 method Methods 0.000 title claims abstract description 20
- 238000001694 spray drying Methods 0.000 title claims abstract description 10
- 239000000463 material Substances 0.000 claims abstract description 19
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 17
- 239000010439 graphite Substances 0.000 claims abstract description 17
- 239000007864 aqueous solution Substances 0.000 claims abstract description 5
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000002253 acid Substances 0.000 claims abstract description 4
- 230000000694 effects Effects 0.000 claims abstract description 4
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 4
- 239000007800 oxidant agent Substances 0.000 claims abstract description 4
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 claims abstract description 4
- 230000002572 peristaltic effect Effects 0.000 claims abstract description 4
- 238000005502 peroxidation Methods 0.000 claims abstract description 4
- 235000011149 sulphuric acid Nutrition 0.000 claims abstract description 4
- 238000005507 spraying Methods 0.000 claims description 24
- 238000004519 manufacturing process Methods 0.000 claims description 9
- 239000010431 corundum Substances 0.000 claims description 3
- 229910052593 corundum Inorganic materials 0.000 claims description 3
- 230000005518 electrochemistry Effects 0.000 claims description 3
- 239000012527 feed solution Substances 0.000 claims description 3
- 230000007062 hydrolysis Effects 0.000 claims description 3
- 238000006460 hydrolysis reaction Methods 0.000 claims description 3
- 238000012856 packing Methods 0.000 claims description 3
- 239000010453 quartz Substances 0.000 claims description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 2
- 238000001035 drying Methods 0.000 abstract 4
- 230000001590 oxidative effect Effects 0.000 abstract 1
- 238000004806 packaging method and process Methods 0.000 abstract 1
- 239000002994 raw material Substances 0.000 abstract 1
- 239000010410 layer Substances 0.000 description 4
- 229910052799 carbon Inorganic materials 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 230000033116 oxidation-reduction process Effects 0.000 description 3
- 239000013078 crystal Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 description 1
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 239000011149 active material Substances 0.000 description 1
- 125000004429 atom Chemical group 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000001721 carbon Chemical group 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical group FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- Carbon And Carbon Compounds (AREA)
Abstract
The invention relates to equipment and process for producing graphene by spray drying and microwaves. The equipment comprises a microwave oven cavity, a spray drying device, a cyclone collector, an air shutoff unloader and an air exhaust pipe, wherein the spray drying device is arranged in the microwave oven cavity and comprises an atomizer and a drying chamber; the atomizer is arranged at the upper part of the drying chamber; the cyclone collector is connected with the drying chamber through a connection pipe; the air shutoff unloader is arranged at the bottom of the cyclone collector; the air exhaust pipe is arranged at the top of the cyclone collector; graphite is hydrolyzed under the action of strong acid and a strong oxidant such as H2SO4, HNO3 and HClO4 or under the action of electrochemical peroxidation effect to prepare an oxidized graphite aqueous solution with the concentration of 0.1-50 percent; the oxidized graphite aqueous solution raw material enters the drying chamber through a peristaltic pump and the atomizer; atomized materials are dissociated through the microwaves and are reduced into flocculent graphene easy to fly; the reduced graphene enters the cyclone collection device along with the flowing air to be collected, and the materials are packaged into a packaging bag through the air shutoff unloader.
Description
Technical field
The present invention relates to graphene new material preparing technical field, be specifically related to a kind of equipment and technology utilizing spraying dry and microwave radiation suitability for industrialized production Graphene.
Background technology
Graphene (Graphene) is the carbon atomic layer of monoatomic thickness, is that carbon atom is with sp
2the thickness that hydbridized carbon atoms is formed is only the individual layer two dimensional crystal being arranged in honeycomb lattice (honeycomb crystal lattice) of the hexaplanar of individual layer atom.Graphene is one the thinnest in known materials, also unusual rigid; As simple substance, it at room temperature transmits the speed of electronics than known all conductors and semi-conductor all fast (in Graphene, the travelling speed of electronics reaches 1/300 of the light velocity).Meanwhile, as monolayer carbon atomic structure, the theoretical specific surface area of Graphene is up to 3000m
2/ g.So high specific surface area makes to become extremely promising energy storage active material based on the material of Graphene, in storage hydrogen, new type lithium ion battery, ultracapacitor or fuel cell etc., have good application prospect.
At present, prepare this special MATERIALS METHODS of Graphene to comprise: slight rubbing manipulation or tear tape method (pasting HOPG), heating SiC method, metal substrate chemical Vapor deposition process, oxidation reduction process etc.First three methods is due to the reason not suitable for mass production Graphene such as productive rate is low or apparatus expensive, process be loaded down with trivial details.The advantage that oxidation reduction process has productive rate higher because of it is more suitable for scale operation comparatively speaking.
But the chemical reducing agent (as hydrazine hydrate) that traditional oxidation reduction process adopts has very large toxicity, to such an extent as to this method of reducing constitutes larger threat to health of human body and environment protection.Thermal reduction method has fast and reduction ratio advantage more thoroughly; But generally need to carry out under the high temperature more than 1000 DEG C owing to heating, add the energy consumption of whole process.And this method needs the costly equipment such as high-temperature heater.It is fast that microwave exposure heating has speed, and cost is low, uses the features such as simple.Irradiation oxidation graphite granule can obtain the fluffy graphene powder of black within one minute.But the material that common microwave exposure adds must be powder, and the process of dry graphite oxide loaded down with trivial details and power consumption higher.And the Graphene loft that microwave exposure obtains very high (can reach 100L/g), light weight easily flies upward, and is difficult to collect.These problems become the obstacle of microwave radiation method suitability for industrialized production Graphene.
Summary of the invention
For solving deficiency of the prior art, the object of the present invention is to provide a kind of cost is low, production capacity is high, Graphene collects the Graphene of microwave production easily equipment and production technique thereof.
For reaching above object, the technical scheme that the present invention takes is:
A kind of equipment utilizing spraying dry and microwave to produce Graphene, it is characterized in that, comprise microwave cavity, spray drying unit, rotoclone collector, pass wind dumper and vapor pipe, described spray drying unit is arranged in microwave cavity, described spray drying unit comprises spraying gun and kiln, described spraying gun is arranged at kiln top, described rotoclone collector is connected with kiln through pipe connecting, the bottom of described rotoclone collector is provided with closes wind dumper, and the top of described rotoclone collector is provided with vapor pipe.
Further, any two opposite faces in described microwave cavity are provided with multiple microwave launcher.
Further, described microwave cavity inwall and pipe connecting are equipped with polytetrafluoroethyllining lining layer.
Again further, described spraying gun and kiln material are quartz, corundum or pottery.
Spraying dry and microwave is utilized to produce a production technique for Graphene, by graphite under the effect of the strong acid such as H2SO4, HNO3, HClO4 and strong oxidizer, or under electrochemistry peroxidation, after hydrolysis, form the graphite oxide aqueous solution that concentration is 0.1-50%; Graphite oxide aqueous feed solution enters in kiln by peristaltic pump through spraying gun, the material of atomizing state dissociates through microwave, material is reduced to the cotton-shaped Graphene easily flown upward, Graphene after reduction enters tornado collection device with fluidizing air and collects, and material loads in packing bag by closing wind dumper.
After taking above technical scheme, beneficial effect of the present invention is:
Spraying gun is utilized to spray into kiln by graphite oxide water, graphite oxide is dispersed open after, with microwave equipment, graphite oxide heat is reduced again, produce fluidizing air with tornado collection device and collection is guided to cotton-shaped Graphene, through closing the discharging of wind dumper after completing, whole process completes at enclosed space, device structure is simple, easy to operate, safety non-pollution, achieve the continuous prodution of graphene product, improve product yield.
Accompanying drawing explanation
Fig. 1 is structural representation of the present invention;
In figure: spraying gun 1, kiln 2, microwave cavity 3, porthole 4, rotoclone collector 5, closes wind dumper 6, vapor pipe 7, pipe connecting 8.
Embodiment
Below in conjunction with accompanying drawing, the specific embodiment of the present invention is further described:
As shown in the figure, a kind of equipment utilizing spraying dry and microwave to produce Graphene, comprises spraying gun 1, kiln 2, microwave cavity 3, porthole 4, rotoclone collector 5, closes wind dumper 6 and vapor pipe 7.The top with kiln 2 inner chamber installed by described spraying gun 1, and the bottom of described kiln 2 connects the head of rotoclone collector 5 through pipe connecting 8; Described kiln 2 is arranged in microwave cavity 3, two in described microwave cavity 3 relative inwalls are provided with multiple microwave emitter, described microwave cavity 3 and pipe connecting 8 be stainless steel and all in be lined with tetrafluoroethylene, described spraying gun 1 and kiln 2 material be quartzy, corundum or pottery; The top of described rotoclone collector 5 is provided with vapor pipe 7, is provided with and closes wind dumper 6 bottom it.
Take the technical program to produce the technique of Graphene to be: graphite under the effect of the strong acid such as H2SO4, HNO3, HClO4 and strong oxidizer, or under electrochemistry peroxidation, forms the graphite oxide aqueous solution that concentration is 0.1-50% after hydrolysis; Graphite oxide aqueous feed solution enters in kiln by peristaltic pump through spraying gun, the material of atomizing state dissociates through microwave, material is reduced to the cotton-shaped Graphene easily flown upward, Graphene after reduction enters tornado collection device with fluidizing air and collects, and material loads in packing bag by closing wind dumper.
Claims (5)
1. the equipment utilizing spraying dry and microwave to produce Graphene, it is characterized in that, comprise microwave cavity, spray drying unit, rotoclone collector, pass wind dumper and vapor pipe, described spray drying unit is arranged in microwave cavity, described spray drying unit comprises spraying gun and kiln, described spraying gun is arranged at kiln top, described rotoclone collector is connected with kiln through pipe connecting, the bottom of described rotoclone collector is provided with closes wind dumper, and the top of described rotoclone collector is provided with vapor pipe.
2. a kind of equipment utilizing spraying dry and microwave to produce Graphene according to claim 1, it is characterized in that, any two opposite faces in described microwave cavity are provided with multiple microwave launcher.
3. a kind of equipment utilizing spraying dry and microwave to produce Graphene according to claim 1 and 2, it is characterized in that, described microwave cavity inwall and pipe connecting are equipped with polytetrafluoroethyllining lining layer.
4. a kind of equipment utilizing spraying dry and microwave to produce Graphene according to claim 1, it is characterized in that, described spraying gun and kiln material are quartz, corundum or pottery.
5. the production technique utilizing spraying dry and microwave to produce Graphene, it is characterized in that, by graphite under the effect of the strong acid such as H2SO4, HNO3, HClO4 and strong oxidizer, or under electrochemistry peroxidation, after hydrolysis, form the graphite oxide aqueous solution that concentration is 0.1-50%; Graphite oxide aqueous feed solution enters in kiln by peristaltic pump through spraying gun, the material of atomizing state dissociates through microwave, material is reduced to the cotton-shaped Graphene easily flown upward, Graphene after reduction enters tornado collection device with fluidizing air and collects, and material loads in packing bag by closing wind dumper.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410846369.4A CN104556007A (en) | 2014-12-31 | 2014-12-31 | Equipment and process for producing graphene by spray drying and microwaves |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410846369.4A CN104556007A (en) | 2014-12-31 | 2014-12-31 | Equipment and process for producing graphene by spray drying and microwaves |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN104556007A true CN104556007A (en) | 2015-04-29 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410846369.4A Pending CN104556007A (en) | 2014-12-31 | 2014-12-31 | Equipment and process for producing graphene by spray drying and microwaves |
Country Status (1)
| Country | Link |
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| CN (1) | CN104556007A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105819437A (en) * | 2016-05-06 | 2016-08-03 | 成都新柯力化工科技有限公司 | Method for large-scale clean graphene preparation |
| CN107362978A (en) * | 2016-05-12 | 2017-11-21 | 新疆隆平红安生物科技有限责任公司 | A kind of bipolar sedimentation capsicum cleaning equipment |
| CN107539978A (en) * | 2017-10-13 | 2018-01-05 | 南京旭羽睿材料科技有限公司 | A kind of graphene production equipment |
| CN113003569A (en) * | 2021-04-28 | 2021-06-22 | 南京工业大学 | Method for preparing reduced graphene oxide powder with high specific surface area |
| CN113443619A (en) * | 2021-08-13 | 2021-09-28 | 中国科学院城市环境研究所 | Device system for preparing single-layer graphene, single-layer graphene and preparation method of single-layer graphene |
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2014
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Patent Citations (4)
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105819437A (en) * | 2016-05-06 | 2016-08-03 | 成都新柯力化工科技有限公司 | Method for large-scale clean graphene preparation |
| CN105819437B (en) * | 2016-05-06 | 2018-01-30 | 成都新柯力化工科技有限公司 | A kind of method that scale cleaning prepares graphene |
| CN107362978A (en) * | 2016-05-12 | 2017-11-21 | 新疆隆平红安生物科技有限责任公司 | A kind of bipolar sedimentation capsicum cleaning equipment |
| CN107539978A (en) * | 2017-10-13 | 2018-01-05 | 南京旭羽睿材料科技有限公司 | A kind of graphene production equipment |
| CN113003569A (en) * | 2021-04-28 | 2021-06-22 | 南京工业大学 | Method for preparing reduced graphene oxide powder with high specific surface area |
| CN113003569B (en) * | 2021-04-28 | 2021-10-29 | 南京工业大学 | Method for preparing reduced graphene oxide powder with high specific surface area |
| CN113443619A (en) * | 2021-08-13 | 2021-09-28 | 中国科学院城市环境研究所 | Device system for preparing single-layer graphene, single-layer graphene and preparation method of single-layer graphene |
| CN113443619B (en) * | 2021-08-13 | 2023-02-17 | 中国科学院城市环境研究所 | Device system for preparing single-layer graphene, single-layer graphene and preparation method of single-layer graphene |
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Application publication date: 20150429 |