CN206911273U - Graphene peels off tri compound plant equipment - Google Patents

Graphene peels off tri compound plant equipment Download PDF

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Publication number
CN206911273U
CN206911273U CN201720708305.7U CN201720708305U CN206911273U CN 206911273 U CN206911273 U CN 206911273U CN 201720708305 U CN201720708305 U CN 201720708305U CN 206911273 U CN206911273 U CN 206911273U
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tank
stripping
equipment
ultrasonic
peels
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CN201720708305.7U
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肖彦社
万振涛
杨树斌
武卫明
商红岩
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Beijing Huake Xunneng Graphene New Technology Research Institute Co ltd
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Beijing Huakexun To Graphene New Technology Research Institute Co Ltd
Beihang University
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Abstract

The utility model proposes a kind of graphene to peel off tri compound plant equipment, including emulsification shearing equipment, ultrasonic peel-off device and agitation mixer;The emulsification shearing equipment includes shearing cutter head, and the ultrasonic peel-off device includes ultrasonic probe, and the shearing cutter head and the ultrasonic probe may be contained within peeling off in tank;The agitation mixer includes blending tank, and the tank bottom of the blending tank connects the blending tank higher than the top for peeling off tank, the stripping tank by pipeline.The utility model proposes equipment, the advantages of combining mechanical stripping, ultrasound stripping and stirring, can be by mechanically pulling off, the compound action of ultrasound and stirring efficiently, quickly peels off layered solid powder two-dimension nano materials into high quality, and there is no the discharge of dust, waste liquid, waste gas in stripping process.

Description

Graphene peels off tri compound plant equipment
Technical field
The utility model belongs to field of energy source materials, and in particular to a kind of to shear, be ultrasonic, stirring compound plant equipment.
Background technology
Two-dimension nano materials include graphene, boron nitride, molybdenum disulfide, black phosphorus nano flake etc., wherein two dimension is single former Sublayer graphite-graphene, because it has a very high specific surface area, excellent chemistry, heat endurance and are led at good electric conductivity The property such as hot property, excellent mechanical performance, there is great answer in fields such as catalysis, electronics, the energy, biological medicine, materials Use prospect.Meanwhile class graphene two-dimension nano materials, such as molybdenum disulfide nano thin slice, black phosphorus nano flake, because with good Catalytic hydrogen evolution activity and storage lithium performance, also have potential application value in catalysis and energy storage field.
Graphene or class grapheme two-dimension material can be prepared by a variety of methods, be broadly divided into Physical and chemistry Method, wherein Physical can be divided into the methods of micromechanics is peeled off, liquid/vapor is directly peeled off, and chemical method can be divided into chemical gas Mutually the methods of deposition (CVD), oxidation-reduction method.CVD method is to be deposited on solid film substrate by gas phase reaction under high temperature The method of upper graphene, this method can prepare the graphene of high quality, large area, but higher cost, complicated technique with And harsh process regulation conditionality its development.Presently the most conventional oxide-reduction method, passes through strong protonic acid Graphite is handled, forms compound between graphite layers, strong oxidizer is then added and it is aoxidized, form graphene oxide, pass through Further reduction can obtain redox graphene, but the method has used in process of production has deep-etching to chemical industry equipment Property, the strong acid and strong oxidizer of strong oxidizing property, have larger harm to environment, and formed graphene electronic structure and crystal it is complete For whole property by serious destruction, electrical conductivity has obvious reduction, limits its application and industry in the energy, electronic applications Change development.The method of liquid phase mechanical stripping can prepare the graphene and class graphene two-dimension nano materials of high quality, but Typically peeled off by single mechanical stripping or ultrasonication, it is less efficient, and yield is also than relatively low.
The device that the present invention develops acts on mechanical shearing, ultrasonic release effect and stirring action combine, can The layered solid dusty material in liquid phase is prepared into two-dimensional nano sheet material with efficient, cleaning, such as graphene, curing Molybdenum, black phosphorus nano flake, and the two-dimension nano materials separated by the equipment have that thickness of thin, specific surface area be big, crystal knot The advantages that structure is complete, and the size adjustable of two-dimensional nano piece is controllable, avoid using the harshness such as strong acid and strong base and HTHP Process conditions, graphene or class graphene two-dimension nano materials suitable for prepare with scale high quality.
Utility model content
In order to efficiently, cleaning, prepare at low cost with the graphene that crystal structure is complete, specific surface area is big and Class graphene two-dimension nano materials, the purpose of this utility model be to provide a kind of equipment that can prepare two-dimension nano materials, The equipment is by mechanical shearing, ultrasound is peeled off and three kinds of compound actions of mechanical agitation, can clean, efficiently, it is stable will point The layered solid dusty material dissipated in liquid solution is peeled off into two-dimensional nano sheet material.
The technical scheme for realizing the utility model purpose is:
A kind of graphene peels off tri compound plant equipment, including emulsification shearing equipment, ultrasonic peel-off device and stirring mix Close equipment;
The emulsification shearing equipment includes shearing cutter head, and the ultrasonic peel-off device includes ultrasonic probe, the shear knife Head and the ultrasonic probe may be contained within peeling off in tank;The agitation mixer includes blending tank, the tank bottom of the blending tank Higher than the top of the stripping tank, the stripping tank connects the blending tank by pipeline.
Wherein, the shearing cutter head includes the stator and rotor being coaxially nested with, and rotor is connected with buncher;Shearing cutter head Highly locate to peel off tank 1/4-1/2 apart from tank bottom.
Wherein, the ultrasonic probe is connected with supersonic generator, a diameter of 6-40mm of ultrasonic probe;The ultrasound is visited Head is highly located apart from tank bottom to peel off tank 1/4-3/4.
Wherein, the blending tank is provided with chuck, and the chuck is connected with cooling water water pipe;Stirring is provided with blending tank Oar, the agitating paddle are that blending tank 1/3-1/2 highly locates apart from tank bottom.
Preferably, the stripping tank tank bottom is provided with material outlet, and material outlet connects the blending tank by pipeline, pipe Impeller pump and valve are provided with road;The mixing pot bottom connects the stripping tank, the return line by return line On be provided with valve.
The utility model has advantages below:
The utility model avoids individually or is used in combination emulsification cutting and led with ultrasonic device by mass transfer is uneven The charge stripping efficiency of cause is relatively low and the problem of peeled off two-dimension nano materials thickness evenness difference, can without using strong acid and Cleaned in the case of severe corrosive chemical reagent, efficiently separate high income, thickness of thin and uniformly, crystal structure is complete, compares table Area is big and the adjustable controllable graphene of area and class graphene two-dimension nano materials.The utility model proposes equipment, The advantages of combining mechanical stripping, ultrasound stripping and stirring, it can be by mechanically pulling off, ultrasonic and stirring compound action Layered solid powder efficiently, is quickly peeled off to the two-dimension nano materials into high quality, and do not have in stripping process dust, The discharge of waste liquid, waste gas.
1. the utility model proposes equipment, be compounded with mechanical shearing, ultrasound peel off and mechanical agitation three effect, Greatly improve the charge stripping efficiency of stratiform powder body material.
2. an equipment efficient under liquid-phase condition, cleaning can be peeled off layered solid material into two-dimension nano materials.
3. the two-dimension nano materials thickness of thin that is separated by this equipment and uniformly, it is controllable that area is adjustable, and crystal structure is complete The advantages that whole.
4. a device structure has the advantages that simple, cost is relatively low, energy consumption is small, suitable for commercial application.
Brief description of the drawings
Fig. 1 is that graphene of the present utility model peels off tri compound plant equipment structure diagram.
In figure, 1 is emulsification shearing equipment, and 2 be ultrasonic peel-off device, and 3 be stripping tank, and 4 be impeller pump, and 5 be agitating paddle, 6 It is return line for blending tank, 601.
Embodiment
Following examples are used to illustrate the utility model, but are not limited to the scope of the utility model.
In embodiment, unless otherwise specified, method therefor and equipment are the conventional apparatus and method in this area.
Embodiment 1:
Such as Fig. 1, a kind of graphene peels off tri compound plant equipment, including emulsification shearing equipment 1, ultrasonic peel-off device 2 And agitation mixer;
The emulsification shearing equipment 1 includes shearing cutter head, and the ultrasonic peel-off device 2 includes ultrasonic probe, the shearing Cutter head and the ultrasonic probe may be contained within peeling off in tank 3;The agitation mixer includes blending tank 6, the blending tank Tank bottom connects the blending tank 3 higher than the top for peeling off tank, the stripping tank 6 by pipeline.Blending tank is located at eminence, molten Automatically flow into and peel off in tank by return line 601 from blending tank during agent circulating and recovering, and no longer need pump.
The shearing cutter head includes the stator and rotor being coaxially nested with, and rotor is connected with buncher.
Blending tank 6 is provided with chuck, and the chuck is connected with cooling water water pipe;Agitating paddle 5 is provided with blending tank, is peeled off The tank bottom of tank 3 is provided with material outlet, and material outlet connects the blending tank by pipeline, impeller pump 4 and valve are provided with pipeline Door;The mixing pot bottom connects the stripping tank by return line 601, and valve is provided with the return line.
In the present embodiment, a diameter of 8mm of shearing cutter head stator, a diameter of 12mm of rotor, between stator and rotor Radial distance is about 0.2mm, peels off the high 20cm of tank, the distance that cutter head distance peels off tank bottom is about 5cm, and the rotating speed of rotor is in 1- It is adjustable controllable between 18000 revs/min;Simultaneously by with ultrasonication titanium alloy probe be inserted into peel off tank in, probe it is straight Footpath is about 6mm, wherein the distance that probe distance from bottom peels off tank base is about 7cm, ultrasonic power adjustable is controllable, ultrasonic work( Rate is between 1-1000W.Connected by pipeline and impeller pump by tank is peeled off with blending tank, wherein residing for mixing pot bottom Height be higher than peel off tank top about 10cm, the flow of impeller pump is 0.3m3/ h, agitating paddle are in tank body apart from tank bottom 1/ At 3, it is controllable that mixing speed is adjustable, and rotating speed is at about 1-3000 revs/min.Solvent about 3L is added in tank to peeling off, natural graphite powder is about 300g, after stirring, mechanical shearing, ultrasound are peeled off and mixing apparatus unit is opened successively, wherein turn of mechanical shearing Speed is at 12000 revs/min, and the power of ultrasonic stripping unit maintains 900W, and the flow of impeller pump turns in 0.3m3/h, agitating paddle Speed is at 1000 revs/min, by the working process of about 6 hours, can successfully prepare thickness in 1-10nm and uniform graphene, And graphene crystal structure is complete, electrical conductivity is high, and high income is up to 20%.
Embodiment 2
In the present embodiment, a diameter of 12mm of shearing cutter head stator, a diameter of 16mm of rotor, between stator and rotor Radial distance is about 0.3mm, and the distance that cutter head distance peels off tank bottom is about 8cm, and the rotating speed of rotor is between 1-18000 revs/min It is adjustable controllable;The titanium alloy probe with ultrasonication is inserted into simultaneously and peeled off in tank body, a diameter of about 30mm of probe, its It is middle probe distance from bottom peel off pot bottom distance be about 12cm, ultrasonic power adjustable is controllable, ultrasonic power 1-2000W it Between;Connected by pipeline and impeller pump by tank is peeled off with blending tank, wherein the height residing for mixing pot bottom is higher than Peel off tank top about 15cm.Mechanical stirring device is located at the top of blending tank, and agitating paddle is in tank body at tank bottom 1/2. Other are set with embodiment 1.
Solvent about 5L, molybdenum disulfide powder about 500g are added into solvent tank body, mechanical shearing, ultrasound are peeled off and stirred Mixing equipment unit is opened successively, and wherein at 14000 revs/min, the power of ultrasonic stripping unit maintains the rotating speed of mechanical shearing 1500W, the flow of impeller pump is in 0.3m3/h, and the rotating speed of agitating paddle is at 2000 revs/min, at the Continuous machings of about 8 hours Reason, can successfully prepare the molybdenum disulfide two-dimension nano materials in uniform thickness in 1-10nm, and crystal structure is complete, yield About 15%.
Embodiment 3
In the present embodiment, a diameter of 12mm of shearing cutter head stator, a diameter of 16mm of rotor, between stator and rotor Radial distance is about 0.2mm, and distance of the cutter head apart from solvent tank bottom is about 8cm, and the rotating speed of rotor is between 1-18000 revs/min It is adjustable controllable;The titanium alloy probe with ultrasonication is inserted into tank body simultaneously, a diameter of about 40mm of probe, wherein visiting The distance of head distance from bottom tank base is about 15cm, mixes the height residing for pot bottom and is higher than stripping tank top about 12cm. Agitating paddle is in tank body at tank bottom 1/4.Other are set with embodiment 1.
The flow for adjusting impeller pump is 0.6m3/ h, solvent about 10L, expanded graphite powder about 600g are added in tank body to peeling off, After stirring, mechanical shearing, ultrasound are peeled off and mixing plant unit is opened successively, the rotating speed of wherein mechanical shearing exists 12000 revs/min, the power of ultrasonic stripping unit maintains 2200W, and the flow of impeller pump exists in 0.6m3/h, the rotating speed of agitating paddle 2000 revs/min, handled by the Continuous machings of about 12 hours, can successfully prepare the graphene in uniform thickness in 1-8nm, And crystal structure is complete, electrical conductivity is high, yield is about 32%.
Although content of the present utility model is discussed in detail by above-mentioned preferred embodiment, but it should be appreciated that above-mentioned Description be not considered as to limitation of the present utility model.It will be understood by those skilled in the art that in this patent design and specifically Under embodiment enlightenment, some that directly can be exported or associate from this patent disclosure and general knowledge deform, and this area is common Technical staff will recognize also use other method, or the replacement of prior art, and the equivalent change or modification of feature, or Mutually different combination between person's feature, the function and effect of this patent description can be realized, no longer one by one for example, belonging to this Scope of patent protection.

Claims (5)

1. a kind of graphene peels off tri compound plant equipment, it is characterised in that including emulsification shearing equipment, ultrasonic peel-off device And agitation mixer;
The emulsification shearing equipment includes shearing cutter head, and the ultrasonic peel-off device includes ultrasonic probe, the shearing cutter head with The ultrasonic probe may be contained within peeling off in tank;The agitation mixer includes blending tank, and the tank bottom of the blending tank is higher than The top for peeling off tank, the stripping tank connect the blending tank by pipeline.
2. graphene according to claim 1 peels off tri compound plant equipment, it is characterised in that the shearing cutter head bag The stator and rotor being coaxially nested with are included, rotor is connected with buncher;Shearing cutter head is stripping tank 1/4-1/2 height apart from tank bottom Place.
3. graphene according to claim 1 peels off tri compound plant equipment, it is characterised in that the ultrasonic probe connects It is connected to supersonic generator, a diameter of 6-40mm of ultrasonic probe;The ultrasonic probe is high to peel off tank 1/4-3/4 apart from tank bottom At degree.
4. the graphene according to claim any one of 1-3 peels off tri compound plant equipment, it is characterised in that described mixed Close tank and be provided with chuck, the chuck is connected with cooling water water pipe;Agitating paddle is provided with blending tank, the agitating paddle is apart from tank Bottom is that blending tank 1/3-1/2 highly locates.
5. the graphene according to claim any one of 1-3 peels off tri compound plant equipment, it is characterised in that the stripping Tank tank bottom is provided with material outlet, material outlet connects the blending tank by pipeline, impeller pump and valve are provided with pipeline Door;The mixing pot bottom connects the stripping tank by return line, and valve is provided with the return line.
CN201720708305.7U 2017-06-16 2017-06-16 Graphene peels off tri compound plant equipment Active CN206911273U (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108816461A (en) * 2018-04-08 2018-11-16 江苏匠心信息科技有限公司 A kind of graphene finished product grinding device
CN109364806A (en) * 2018-11-12 2019-02-22 天津理工大学 It is a kind of to assist cutting to realize that two-dimensional material prepares the method and device thereof of mass production using ultrasonic wave
CN109502648A (en) * 2018-12-10 2019-03-22 中南大学 A kind of the molybdenum disulfide nano sheet physical separation methods and its device of ultrasonic wave added
CN111185120A (en) * 2020-01-09 2020-05-22 吕梁学院 High-efficient dispersion dosing unit of graphite alkene production usefulness
WO2021062940A1 (en) * 2019-09-30 2021-04-08 青岛创启新能催化科技有限公司 Continuous dispersion system, catalyst batch synthesis apparatus and method

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108816461A (en) * 2018-04-08 2018-11-16 江苏匠心信息科技有限公司 A kind of graphene finished product grinding device
CN109364806A (en) * 2018-11-12 2019-02-22 天津理工大学 It is a kind of to assist cutting to realize that two-dimensional material prepares the method and device thereof of mass production using ultrasonic wave
CN109502648A (en) * 2018-12-10 2019-03-22 中南大学 A kind of the molybdenum disulfide nano sheet physical separation methods and its device of ultrasonic wave added
CN109502648B (en) * 2018-12-10 2020-11-03 中南大学 Ultrasonic-assisted molybdenum disulfide nanosheet physical stripping method and device
WO2021062940A1 (en) * 2019-09-30 2021-04-08 青岛创启新能催化科技有限公司 Continuous dispersion system, catalyst batch synthesis apparatus and method
CN111185120A (en) * 2020-01-09 2020-05-22 吕梁学院 High-efficient dispersion dosing unit of graphite alkene production usefulness

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Effective date of registration: 20180517

Address after: 100024 Chaoyang District, Beijing, Chaoyang North Road, 1 D-2-8, Hong Chong International Cultural Innovation Park

Patentee after: Beijing huakexun to graphene New Technology Research Institute Co. Ltd.

Address before: 100035 No. 235 block A, 28 new street, new street, Xicheng District, Beijing.

Co-patentee before: Beihang University

Patentee before: Beijing huakexun to graphene New Technology Research Institute Co. Ltd.

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Effective date of registration: 20180824

Address after: 214100 Dongsheng Road, anzhen Street City Industrial Park, Xishan District, Wuxi, Jiangsu, China

Patentee after: YADEA TECHNIC GROUP CO.,LTD

Address before: 100024 Chaoyang District, Beijing, Chaoyang North Road, 1 D-2-8, Hong Chong International Cultural Innovation Park

Patentee before: Beijing huakexun to graphene New Technology Research Institute Co. Ltd.

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Effective date of registration: 20201118

Address after: Room 8, unit 1, building 39, Luozhuang street, Muye District, Xinxiang City, Henan Province

Patentee after: Li Ximei

Address before: 214100 Dongsheng Road, anzhen Street City Industrial Park, Xishan District, Wuxi, Jiangsu, China

Patentee before: YADEA SCIENCE & TECHNOLOGY GROUP Co.,Ltd.

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Effective date of registration: 20220126

Address after: 100020 d-2-8 (1-3 floors), Beijing Hongzhuang international cultural bonded Innovation Park, No.1, baijialou, Chaoyang North Road, Chaoyang District, Beijing

Patentee after: BEIJING HUAKE XUNNENG GRAPHENE NEW TECHNOLOGY RESEARCH INSTITUTE CO.,LTD.

Address before: 453002 No.8, unit 1, building 39, Luozhuang street, Muye District, Xinxiang City, Henan Province

Patentee before: Li Ximei