CN203794630U - Industrial device for continuously producing graphene powder - Google Patents
Industrial device for continuously producing graphene powder Download PDFInfo
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- CN203794630U CN203794630U CN201420166500.8U CN201420166500U CN203794630U CN 203794630 U CN203794630 U CN 203794630U CN 201420166500 U CN201420166500 U CN 201420166500U CN 203794630 U CN203794630 U CN 203794630U
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Abstract
The utility model discloses an industrial device for continuously producing graphene powder. The device comprises a liquid storage tank, a flow valve, a plurality of ultrasonic treaters, a microwave reaction kettle, a vibrating screen, a mixing tank, a reservoir, a booster pump, a spray drying tower and a cyclone centrifuge. The surface tension is adjusted by controlling the ratio of a dispersant; after the dispersant is mixed evenly with graphite, evenly dispersed graphene can be obtained under the synergistic action of continuous ultrasonic waves and microwaves; a bonding liquid is added to a graphene dispersion liquid to prepare a slurry; and a centrifugal spray drying apparatus is used for performing spray drying and granulation on the slurry. The industrial device is characterized in that large-scale production of the graphene is realized in a combined ultrasonic wave-microwave manner, the granulation of the graphene can be realized in combination with spray drying, the environmental pollution is reduced, and the obtained graphene powder is convenient to transport and use.
Description
Technical field
The utility model belongs to technical field of nano material, is specifically related to a kind of serialization and produces graphene powder full scale plant.
Background technology
Graphene (Graphene) is a kind of individual layer sheet structured material consisting of carbon atom, because the advantages such as its high strength, high heat conductance, high conductivity and high-specific surface area have been subject to investigator's extensive attention.At present, the method for preparing Graphene both at home and abroad mainly contains several as follows:
(1) micromechanics stripping method; The Graphene quality that this method makes is high, but can only obtain a limited number of graphene films, is only applicable to probe into as fundamental research the electrical properties of Graphene.
(2) epitaxial growth method; This method preparation condition is harsh, all require to carry out under the conditions such as high temperature high vacuum or certain particular atmosphere and single crystalline substrate, and the Graphene making is difficult for separating from substrate, can not prepare on a large scale Graphene.
(3) oxidation-reduction method; The method be at present comparatively common low-cost high-efficiency prepare the chemical process of big area Graphene layer material, but the Graphene obtaining contains a large amount of oxy radicals and defect, its conductivity is lower, and reductive agent major part is poisonous, makes preparation process have environmental pollution.
(4) chemical Vapor deposition process; This method can meet the requirement that high-quality graphene is prepared in mass-producing, but cost is higher, complex process.
(5) electrolytic process; This method can be synthesized a large amount of Graphenes, but the surface of the Graphene synthesizing is all with a large amount of positive ions, negative ion or organism.Aforesaid method respectively has limitation part, thus people urgently wish to develop a kind of environmental friendliness, technique simple, can less Graphene method and the device of large-scale production place defect.
Liquid phase ultrasonic stripping method is the crushing effect to powder by ultrasonic wave, in organic solvent, graphite flake layer is peeled off to the method (J.Mater.Chem.19,3367-3369,2009) of preparing Graphene.Organic solvent not only provides preparation place, and can play by control condition the effect that promotes graphite linings separation, dispersion, protection, isolation Graphene.The method not only can be carried out large volume preparation, and simultaneously owing to not introducing chemical process, Graphene crystalline structure has also obtained better protecting, the Graphene of availability excellence.But this method exists energy consumption high, inefficient defect.And microwave liquid phase stripping method is prepared Graphene, energy consumption is low, and product size is evenly distributed, and can stable suspersion in reaction solution.
China Patent No. CN 103253659 A disclose " a kind of ultrasonic wave is peeled off the method for preparing graphite alkene ", this method is evenly mixed powdered graphite and intercalator by a certain percentage in organic solvent, recycling ultrasound bath is peeled off certain hour, centrifugation, obtains grapheme material after filtration.It is high that the prepared Graphene of this method has quality, and excellent performance, defect are few, yet the method is periodical operation, and energy consumption is high, therefore cannot scale operation.
To sum up, the problem that how to solve high-quality graphene large-scale production becomes the hot issue of people's research.
Utility model content
The purpose of this utility model is to propose a kind of serialization to produce graphene powder full scale plant; there is uninterrupted continuous production, and equipment is simple, operation simple and feasible; easily be automated and suitability for industrialized production, and can solve the problem of high-quality graphene large-scale production.
For achieving the above object, solution of the present utility model is:
A graphene powder full scale plant is produced in serialization, and it comprises the stationary tank being connected successively by pipeline, multistage microwave reaction kettle, reservoir, spray-drying tower and cyclone centrifugal device, is respectively equipped with flow valve between each several part; On reservoir, be connected with tempering tank, between reservoir and spray-drying tower, be provided with topping-up pump; Rapid stirring oar is installed respectively in stationary tank, tempering tank and reservoir; Microwave reaction kettles at different levels are provided with processor for ultrasonic wave, and microwave reaction kettle is temperature control microwave hydrothermal reaction kettle, separately between the pipeline opening of microwave reaction kettles at different levels, are provided with vibration screen, and vibration screen both sides are provided with the blade of horizontal rapid stirring.
Described processor for ultrasonic wave is energy gathering type ultrasound probe, and ultrasonic frequency is in 20kHz-80kHz.
Microwave heating has selectivity, instantaneity, high efficiency, controls suitable microwave condition and can promote the pulverizing of graphite to peel off.Microwave is a kind of non-ionising radiation energy that is caused molecular motion by ion migration and dipole rotation, when being subject to microwave electromagnetic field action, polar molecule just can produce instantaneous polarization, and do at a terrific speed reversal of pole campaign, thereby produce key motion, tear and particle between phase mutual friction, collision, promote molecular polarity part better contact and reaction, produce rapidly a large amount of heat energy simultaneously, impel graphite to pulverize, peel off; Secondly, graphite is a kind of good microwave absorbing medium, and by microwave treatment, graphite can absorb microwave fast and produce huge heat, and graphite layers can produce huge thermal stresses, can make effectively peeling off between layers of graphite.
The synergy that the utility model makes full use of hyperacoustic mechanical dispersion effect, ultrasonic cavitation effect, microwave homogeneous heating effect and produces between them, strengthening graphite stripping process, thereby realize Graphene efficiently, fast preparation.
Feature of the present utility model and beneficial effect:
(1) this device adopts continuous ultrasound mechanically peel graphite acquisition Graphene to belong to physical method, and the structure of not destroying Graphene can obtain good, the flawless Graphene of quality, and in device, adopts a plurality of energy gathering types probes can realize continuous large-scale production;
(2) adopt microwave simultaneously, can utilize the variation rapid heating of Electric and magnetic fields, Reaction time shorten, can reduce energy consumption to a great extent greatly, improves preparation efficiency;
(3) vibration screen that connects the install pipeline of microwave reaction kettle can be controlled the product size that every first order reaction still leads to next stage reactor, avoids the waste of energy can guarantee again the quality of the product that obtains simultaneously;
(4) be combined with centrifugal spray drying, can in the process of producing, avoid environmental pollution, after Direct spraying is dry, granulation can facilitate using and transporting of later stage.
Accompanying drawing explanation
Fig. 1 is the schematic diagram that graphene powder full scale plant is produced in the utility model serialization.
Embodiment
In order better to understand the utility model, below in conjunction with embodiment, further illustrate content of the present utility model, but the utility model content is not only confined to following specific embodiment.
As shown in Figure 1, the utility model has disclosed a kind of serialization and has produced graphene powder full scale plant, it comprises stationary tank 1, multistage microwave reaction kettle 4, reservoir 7, spray-drying tower 9 and the cyclone centrifugal device 10 being connected successively by pipeline, is respectively equipped with flow valve 2 between each several part; On reservoir 7, be also connected with tempering tank 6, between reservoir 7 and spray-drying tower 9, be provided with topping-up pump 8; The interior rapid stirring oar of installing respectively of stationary tank 1, tempering tank 6 and reservoir 7; Microwave reaction kettles 4 at different levels are provided with processor for ultrasonic wave 3, microwave reaction kettle 4 is temperature control microwave hydrothermal reaction kettle, the another vibration screen 5 that is provided with between the pipeline opening of microwave reaction kettles 4 at different levels, this screen cloth can be controlled the graphite size that enters next stage microwave reaction kettle, and vibration screen both sides are provided with the blade of horizontal rapid stirring, can pulverize large-sized graphite and prevent screen plugging.This processor for ultrasonic wave is that energy gathering type ultrasound probe and ultrasonic frequency are in 20kHz-80kHz.
And utilize this full scale plant specifically to produce the method for graphene powder, its step comprises:
Step 1: by graphite, dispersion agent is placed in stationary tank, wherein graphite is expanded graphite or graphite oxide, and dispersion agent is selected from water, ammoniacal liquor, ethanol, Virahol, acetone, ethylene glycol, N-Methyl pyrrolidone, dimethyl formamide, tetrahydrofuran (THF), dimethyl formamide, orthodichlorobenzene, acetonitrile, 1, 2-ethylene dichloride and sodium lauryl sulphate, Sodium dodecylbenzene sulfonate, a kind of or at least two or more combination in Trisodium Citrate, preferably from polar solvent, special further preferred ammoniacal liquor, ethanol, Sodium dodecylbenzene sulfonate, sodium lauryl sulphate, Trisodium Citrate, the combination that N-Methyl pyrrolidone is a kind of or at least two or more, stir, the proportioning of controlling dispersion agent obtains the graphite premix that surface tension is 30-50mN/m, wherein the graphite concentration in graphite premix is 0.1-3%, simultaneously in tempering tank 6, prepare slurry, tackiness agent comprises more than one the solution in hydrocarbon, thermoplastic resin and thermosetting resin,
Step 2: control flow valve, above-mentioned premix is flowed into microwave reaction kettle 4 by pipeline, take to control the output rating of energy gathering type ultrasound probe number, ultrasonic frequency, microwave reaction kettle, obtain graphene dispersing solution in reservoir 7; Wherein control energy gathering type ultrasound probe ultrasonic frequency for graphite raw material being carried out to ultrasonic mechanically peel with frequency or mixing with any power; Described with being same ultrasonic wave frequently, be mixed down two or more ultrasonic wave;
Step 3: control the flow valve of tempering tank 6, slurry is mixed with graphene dispersing solution, obtain Graphene slurry;
Step 4: adopt centrifugal spray drying mode, reach granulation object by adjusting rotary speed in cyclone centrifugal device 10, thereby obtain Graphene particle.
Case study on implementation one
Step 1: expanded graphite, ethanol, water, Sodium dodecylbenzene sulfonate are placed in to stationary tank 1, Sodium dodecylbenzene sulfonate content 0.01%, content of graphite 1%, the proportioning of water and ethanol is 3:1, above-mentioned substance is carried out fully stirring and obtain even graphite premix, in tempering tank 6, prepare Microcrystalline Cellulose slurry, concentration is 0.01% simultaneously;
Step 2: control flow valve, above-mentioned premix is flowed into microwave reaction kettle 4 with the speed of 100L/h by pipeline, open 8 energy gathering type ultrasound probe participation work, adopt identical frequency process to peel off graphite, frequency is that low frequency 20kH, the output rating of adjusting microwave reaction kettle are 200W, in reservoir 7, obtains graphene dispersing solution;
Step 3: the flow velocity of controlling the flow valve of tempering tank 6 is 100L/h, opens rapid stirring oar, stirs slurry fully to mix with graphene dispersing solution, obtains Graphene slurry;
Step 4: it is 150 ℃ that drying machine with centrifugal spray temperature in is set, and temperature out is 80 ℃, liquid ejection speed is 150L/h.After sample drying, in cyclone centrifugal device 10, by adjusting rotary speed, reach granulation object, thereby obtain Graphene particle.
Above-mentioned Graphene is added in polypropylene (PP), take polypropylene as base material, prepared the matrix material (respectively with PP, 1-PP10,1-PP15,1-PP20 represent) of Graphene content for difference 0%, 10%, 15,20%.
Above-mentioned materials is carried out to strength test, and each sample test 4 times, averages.Strength test the results are shown in Table 1.
The intensity contrast table of table 1 polypropylene and Graphene/polypropylene composite material thereof
Case study on implementation two
Step 1: expanded graphite, water, ethylene glycol, Trisodium Citrate are placed in to stationary tank 1, the content of sodium citrate 0.01%, content of graphite 1%, the proportioning of water and ethylene glycol is 4:1, above-mentioned substance is carried out fully stirring and obtain even graphite premix, in tempering tank 6, prepare carboxymethyl cellulose slurry, concentration is 0.01% simultaneously;
Step 2: control flow valve, above-mentioned premix is flowed into microwave reaction kettle with the speed of 150L/h by pipeline, open 8 energy gathering type ultrasound probe participation work, adopt mixing mode to peel off graphite, frequency is followed successively by 20kH, 30kH, 40kH, 50kH, 20kH, 30kH, 40kH, 50kH, the output rating of adjusting microwave reaction kettle is 300W, in reservoir 7, obtains graphene dispersing solution;
Step 3: the flow velocity of controlling the flow valve of tempering tank 6 is 150L/h, opens rapid stirring oar, stirs slurry fully to mix with graphene dispersing solution, obtains Graphene slurry;
Step 4: it is 200 ℃ that drying machine with centrifugal spray temperature in is set, and temperature out is 80 ℃, liquid ejection speed is 200L/h.After sample drying, in cyclone centrifugal device 10, by adjusting rotary speed, reach granulation object, thereby obtain Graphene particle.
Above-mentioned Graphene is added in polypropylene (PP), take polypropylene as base material, prepared the matrix material (respectively with PP, 2-PP10,2-PP15,2-PP20 represent) of Graphene content for difference 0%, 10%, 15,20%.
Above-mentioned materials is carried out to strength test, and each sample test 4 times, averages.Strength test the results are shown in Table 2.
The intensity contrast table of table 2 polypropylene and Graphene/polypropylene composite material thereof
Case study on implementation three
Step 1: expanded graphite, water, N-Methyl pyrrolidone, sodium lauryl sulphate are placed in to stationary tank 1, Sodium Dodecyl Sulfate 0.01%, content of graphite 2%, the proportioning of water and N-Methyl pyrrolidone is 4:1, above-mentioned substance is carried out fully stirring and obtain even graphite premix, in tempering tank 6, prepare polyacrylic resin slurry, concentration is 0.02% simultaneously;
Step 2: control flow valve, above-mentioned premix is flowed into microwave reaction kettle with the speed of 200L/h by pipeline, open 8 energy gathering type ultrasound probe participation work, adopt mixing mode to peel off graphite, frequency is followed successively by 20kH, 30kH, 40kH, 20kH, 30kH, 40kH, 20kH, 20kH, the output rating of adjusting microwave reaction kettle is 250W, in reservoir 7, obtains graphene dispersing solution;
Step 3: the flow velocity of controlling the flow valve of tempering tank 6 is 200L/h, opens rapid stirring oar, stirs slurry fully to mix with graphene dispersing solution, obtains Graphene slurry;
Step 4: it is 180 ℃ that drying machine with centrifugal spray temperature in is set, and temperature out is 80 ℃, liquid ejection speed is 300L/h.After sample drying, in cyclone centrifugal device 10, by adjusting rotary speed, reach granulation object, thereby obtain Graphene particle.
Above-mentioned Graphene is added in polypropylene (PP), take polypropylene as base material, prepared the matrix material (respectively with PP, 3-PP10,3-PP15,3-PP20 represent) of Graphene content for difference 0%, 10%, 15,20%.
Above-mentioned materials is carried out to strength test, and each sample test 4 times, averages.Strength test the results are shown in Table 3.
The intensity contrast table of table 3 polypropylene and Graphene/polypropylene composite material thereof
Conducting performance test
The product that case study on implementation one is obtained adds in polypropylene with 10%, 15% amount, called after 1PP-10, and 1PP-15, the product that case study on implementation two is obtained adds in polypropylene with 10%, 15%, called after 2PP-10,2PP-15; Moral is filled in admittedly to superconductive carbon black XE-2B simultaneously and add in polypropylene as a comparison samplely, add 10% called after XE-2B-PP10, add 15% called after XE-2B-PP15.Above-mentioned sample is carried out to conductive test.Test result is in Table 4:
Table 4 polypropylene/graphite performance
From the above results, can find out, the Graphene sample quality preparing by the utility model is good, can be used as enhancing, conductive filler material.
Claims (2)
1. a graphene powder full scale plant is produced in serialization, it is characterized in that: comprise the stationary tank being connected successively by pipeline, multistage microwave reaction kettle, reservoir, spray-drying tower and cyclone centrifugal device, be respectively equipped with flow valve between each several part; On reservoir, be connected with tempering tank, between reservoir and spray-drying tower, be provided with topping-up pump; Rapid stirring oar is installed respectively in stationary tank, tempering tank and reservoir; Microwave reaction kettles at different levels are provided with processor for ultrasonic wave, and microwave reaction kettle is temperature control microwave hydrothermal reaction kettle, separately between the pipeline opening of microwave reaction kettles at different levels, are provided with vibration screen, and vibration screen both sides are provided with the blade of horizontal rapid stirring.
2. graphene powder full scale plant is produced in a kind of serialization as claimed in claim 1, it is characterized in that: described processor for ultrasonic wave is energy gathering type ultrasound probe, and ultrasonic frequency is in 20kHz-80kHz.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201420166500.8U CN203794630U (en) | 2014-04-04 | 2014-04-04 | Industrial device for continuously producing graphene powder |
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| CN201420166500.8U CN203794630U (en) | 2014-04-04 | 2014-04-04 | Industrial device for continuously producing graphene powder |
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| CN203794630U true CN203794630U (en) | 2014-08-27 |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103880002A (en) * | 2014-04-04 | 2014-06-25 | 厦门凯纳石墨烯技术有限公司 | Industrial device for continuously producing graphene powder and method thereof |
| CN105061684A (en) * | 2015-07-31 | 2015-11-18 | 湖州杨氏塑料助剂有限公司 | Automatic production equipment for MBS production |
| CN105585003A (en) * | 2014-10-22 | 2016-05-18 | 北京化工大学 | Large-scale continuous preparation method of graphene oxide and graphene nanosheet and equipment thereof |
| CN106207145A (en) * | 2016-09-26 | 2016-12-07 | 冯军 | A kind of silicium cathode active substance and preparation method thereof and the silene lithium battery prepared |
| CN106544690A (en) * | 2017-01-21 | 2017-03-29 | 德阳烯碳科技有限公司 | Prepare the electrolysis reaction device of Graphene |
| CN107619037A (en) * | 2017-09-27 | 2018-01-23 | 刘道灵 | A kind of graphene preparation facilities |
| CN110182794A (en) * | 2019-07-05 | 2019-08-30 | 常州魔晶纳米科技有限公司 | A kind of equipment and preparation method thereof of batch making graphene quantum dot |
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2014
- 2014-04-04 CN CN201420166500.8U patent/CN203794630U/en not_active Withdrawn - After Issue
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103880002A (en) * | 2014-04-04 | 2014-06-25 | 厦门凯纳石墨烯技术有限公司 | Industrial device for continuously producing graphene powder and method thereof |
| CN103880002B (en) * | 2014-04-04 | 2015-12-16 | 厦门凯纳石墨烯技术股份有限公司 | A kind of continuous prodution graphene powder full scale plant and method thereof |
| CN105585003A (en) * | 2014-10-22 | 2016-05-18 | 北京化工大学 | Large-scale continuous preparation method of graphene oxide and graphene nanosheet and equipment thereof |
| CN105061684A (en) * | 2015-07-31 | 2015-11-18 | 湖州杨氏塑料助剂有限公司 | Automatic production equipment for MBS production |
| CN106207145A (en) * | 2016-09-26 | 2016-12-07 | 冯军 | A kind of silicium cathode active substance and preparation method thereof and the silene lithium battery prepared |
| CN106207145B (en) * | 2016-09-26 | 2019-06-07 | 冯军 | A kind of silicium cathode active material and preparation method thereof and silene lithium battery obtained |
| CN106544690A (en) * | 2017-01-21 | 2017-03-29 | 德阳烯碳科技有限公司 | Prepare the electrolysis reaction device of Graphene |
| CN106544690B (en) * | 2017-01-21 | 2018-03-13 | 德阳烯碳科技有限公司 | Prepare the electrolysis reaction device of graphene |
| CN107619037A (en) * | 2017-09-27 | 2018-01-23 | 刘道灵 | A kind of graphene preparation facilities |
| CN110182794A (en) * | 2019-07-05 | 2019-08-30 | 常州魔晶纳米科技有限公司 | A kind of equipment and preparation method thereof of batch making graphene quantum dot |
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Granted publication date: 20140827 Effective date of abandoning: 20151216 |
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| C25 | Abandonment of patent right or utility model to avoid double patenting |