CN104944420A - Interlaminar intercalation graphite preparation equipment - Google Patents
Interlaminar intercalation graphite preparation equipment Download PDFInfo
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- CN104944420A CN104944420A CN201510372161.8A CN201510372161A CN104944420A CN 104944420 A CN104944420 A CN 104944420A CN 201510372161 A CN201510372161 A CN 201510372161A CN 104944420 A CN104944420 A CN 104944420A
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Abstract
The invention discloses interlaminar intercalation graphite preparation equipment. A frame is provided with a connecting pipe with a bottom opening; the connecting pipe is internally provided with a horizontal regulating roller; a combined type anode is arranged on the frame, the combined type anode is insulated with the frame, and the combined type anode is a blade type electrode and comprises a plurality of knife type electrodes; a porous cathode is horizontally arranged on the frame and positioned below the combined type anode, and the combined type anode and the porous cathode are separated through a mobile type separator; and the mobile type separator is a closed type conveying belt with a tile edge and a cross section, the bottom opening of the connecting pipe is formed above the cross section of the mobile type separator, two ends of the mobile type separator are respectively provided with a driving roller and a tension roller, a conveying belt positioned above the mobile type separator is positioned on the surface of the porous cathode, washing machines are positioned on two sides of the conveying belt positioned below the mobile type separator, material receiving grooves are arranged below the washing machines, and the side edges of the material receiving grooves are limiting side walls. The interlaminar intercalation graphite preparation equipment disclosed by the invention has the beneficial effects of high manufacturing efficiency and low energy consumption.
Description
Technical field
The invention belongs to chemical technology field, relate to a kind of interlayer intercalated graphite preparation apparatus.
Background technology
Interlayer intercalated graphite some compounds is inserted the product of original graphite crystal, is the intermediate materials produced in thermal expansion graphite technology and utilize its goods.Usually liquid phase chemical oxidation style is adopted to produce interlayer intercalated graphite, the method strong oxidizer and interlayer thing process graphite in the industry.
The oxygenant that chemical oxidization method uses generally has solid oxidizing agent to have solid oxidizing agent and liquid oxidizer two class.Solid oxidizing agent has KMnO
4, KClO
4, NaC1O
3, (NH
4)
2s
2o
7deng, liquid oxidizer has H
2sO
4, HNO
3, HCIO
4, H
2o
2deng.Solid oxidizing agent General reactions is violent, dangerous property, and price is high, and product ash content is large, and contaminate environment.Liquid oxidizer H
2sO
4, HNO
3deng degradation manipulation environment, polluted water; H
2o
2reaction temperature and, pollute little.Intercalation thing material chooses sulfuric acid, nitric acid, perchloric acid, phosphoric acid, some organic acid and organic acid anhydride class, although this kind of method is simple, acid consumption is large, is unfavorable for recycling of acid solution.In preparation process, certain chemical factor is difficult to control insert at interlayer skewness, constant product quality difference and have the pollution of obnoxious flavour or heavy metal ion in production process.More economical effective means is that electrochemical oxidation process produces interlayer intercalated graphite, electrochemical oxidation process has series of advantages, under controlled operating mode, realize synthesis interlayer intercalated graphite, obtain the product of specified performance [Stoyan Apostolov. С. П., Peter Krass promise husband. В. В., Fei Nanyenuofu. А. И. constant potential electrochemical oxidation process synthetic graphite hydrosulfate // applied chemistry (crow)]-1997.-Т .70.4.-С .602-607 rolls up].According to Faraday's law, contriver calculate graphite oxide matrix must theoretical capacity, being 93Ah/kg when producing interlayer intercalated graphite the stage 1, is 46.5Ah/kg during production stage 2, average out to 69.75Ah/kg when production stage 1+ the stage 2.Like this, theoretical production stage 1 interlayer intercalated graphite, time voltage 4-8 (V), every 1kg graphite consumes power 0.372 – 0.744 kilowatt-hour.But existingly produce interlayer intercalated graphite electrochemical oxidation process and produce interlayer intercalated graphite plant efficiency low, and electric quantity consumption will far beyond calculated value (more than 200Ah/kg).Similar approach shortcoming is also had to be: use poisonous in a large number and have the reagent of explosion hazard, consume energy high, power consumption is for being 200 А h/kg graphite.
Summary of the invention
The object of the present invention is to provide a kind of interlayer intercalated graphite preparation apparatus, solve existing preparation method when using sulfuric acid, electrolytic solution consumption is large, and the problem that power consumption is large.
The technical solution adopted in the present invention comprises pipe connecting graphite mixture being carried out to stirring and smooth thickness; The Combined anode of direct current positive pole can be connected and the porous cathode of direct current negative pole can be connected; Between Combined anode and porous cathode, carrying and mobile graphite mixture and suspension liquid, and make suspension liquid contact the movable separator of Combined anode.
Further, described Combined anode is paddle electrode, is made up of some blade electrodes, and blade electrode to each other distance is 10-25mm;
Further, described pipe connecting is arranged on framework, pipe connecting bottom opening, horizontal adjustment roller is installed in pipe connecting, the mixture of graphite and sulphuric acid soln enters in pipe connecting, horizontal adjustment roller adjusts mixture thickness and makes mixture smooth, Combined anode is arranged on framework, Combined anode and frame insulation, porous cathode level is arranged on framework, and be positioned at below Combined anode, kept apart by movable separator between Combined anode and porous cathode, Combined anode distance moving separator distance is 4-14mm, movable separator is the closed travelling belt with watt edge and transverse section, the bottom opening of pipe connecting is positioned at above the transverse section of movable separator, movable separator two ends are respectively fitted with drive roll and tension drum, tension drum is furnished with take-up device, be used for straining travelling belt, drive roll is furnished with drive roll transmission mechanism, travelling belt above movable separator is positioned at porous cathode surface, washing machine is arranged on framework, be positioned at the travelling belt both sides below movable separator, be used for cleaning movable separator, below washing machine, receiving vat is installed, receiving vat side is restriction sidewall.
Further, described receiving vat is inclined and mounted on framework, and current flow out from washing machine, and interlayer graphite pours in outside suction filter along tilting receiving vat by current.
Further, described movable separator speed is 1-18cm/min.
Further, described transverse section is provided with some uniform projections, and transverse section is divided into some grooves, and when movable separator moves, the mixture flowed down from pipe connecting and graphite suspension lay respectively in some grooves.
The invention has the beneficial effects as follows that manufacture efficiency is high, energy consumption is low.
Accompanying drawing explanation
Fig. 1 is preparation method's schematic diagram of graphite mixture of the present invention;
Fig. 2 is the equipment side schematic view that interlayer intercalated graphite of the present invention produces use;
Fig. 3 is the equipment vertical view that interlayer intercalated graphite of the present invention produces use.
In figure, 1-framework; 2-pipe connecting; 3-horizontal adjustment roller; 4-Combined anode; 5-porous cathode; 6-drive roll; 7-drive roll transmission mechanism; 8-tension drum; 9-take-up device; 10-washing machine; 11-receiving vat; 12-limits sidewall; 13-movable separator; 14-corrugation limit; 15-transverse section; 16-is protruding.
Embodiment
Below in conjunction with embodiment, the present invention is described in detail.
Graphite and concentration are that the sulfuric acid of 30%-94% is according to (0.5 – 1.0cm by interlayer intercalated graphite preparation method of the present invention
3): 1g stirs, and makes mixture.As shown in Figure 1, for preferred preparation method of mixture: adopt 98% concentration sulphuric acid of 50kg-100kg and 50kg-100kg deionized water and stirring, the sulphuric acid soln of generation 20%-50% concentration, gets 50-100L, stir with the crystalline flake graphite 80-100kg of carbon content 99%, making density is 1.72g/cm
3the mixture of pulpous state, mixture is put into the pipe connecting 2 of carrying, enter on the transverse section of movable separator 13, flatten with horizontal adjustment roller 3 and adjust the thickness of mixture, in pipe connecting 2, adding graphite suspension, along with movable separator 13 moves, mixture layer moves to below Combined anode 4, graphite suspension layer is encountered Combined anode 4, connects direct current, current density 25 – 42mA/cm
2, electric current, by graphite and sulphuric acid soln mixture layer, along with the consumption of graphite suspension, will supplement new graphite suspension, ensure that the flow process producing interlayer graphite runs without interruption in pipe connecting 2.When movable separator 13 moves between Combined anode 4 and porous cathode, graphite suspension and mixture are transformed into interlayer graphite under direct current effect.
Graphite suspension in strong acid electrolyte is delivered to reaction zone between anode and negative electrode by the inventive method, discharges by suspension subsequently, intercalated graphite between anodic oxidation graphite generation layer.Electrochemical process will consume suspension, carries out anodic oxidation, without the need to graphite is expressed to anode in without too much electrolytic solution situation.
The equipment that preparation method of the present invention uses as shown in Figures 2 and 3, comprise framework 1, framework 1 is provided with the pipe connecting 2 of bottom opening, horizontal adjustment roller 3 is installed in pipe connecting 2, the mixture of graphite and sulphuric acid soln enters in pipe connecting 2, horizontal adjustment roller 3 pairs of mixture thickness adjust and make mixture smooth, Combined anode 4 is arranged on framework 1, Combined anode 4 and framework 1 insulate, Combined anode 4 is paddle electrode, be made up of some blade electrodes, blade electrode to each other distance is 10-25mm, porous cathode 5 level is arranged on framework 1, and be positioned at below Combined anode 4, kept apart by movable separator 13 between Combined anode 4 and porous cathode 5, Combined anode 4 distance moving separator 13 is apart from being 4-14mm, movable separator 13 is the closed travelling belts with watt edge 14 and transverse section 15, the bottom opening of pipe connecting 2 is positioned at above the transverse section 15 of movable separator 13, movable separator 13 two ends are respectively fitted with drive roll 6 and tension drum 8, tension drum 8 is furnished with take-up device 9, be used for straining travelling belt, drive roll 6 is furnished with drive roll transmission mechanism 7, travelling belt above movable separator 13 is positioned at porous cathode 5 surface, washing machine 10 is arranged on framework 1, be positioned at the travelling belt both sides below movable separator 13, be used for cleaning movable separator 13, receiving vat 11 is installed below washing machine 10, receiving vat 11 side is restriction sidewall 12.
Receiving vat 11 preferred angled is arranged on framework 1, and current flow out from washing machine 10, and interlayer graphite pours in outside suction filter along tilting receiving vat 11 by current.
Movable separator 13 speed is 1-18cm/min,
Transverse section 15 is provided with some uniform protruding 16, and transverse section 15 is divided into some grooves, and when movable separator 13 moves, the mixture flowed down from pipe connecting 2 and graphite suspension lay respectively in some grooves.
Movable separator 13 moves back and forth at the periphery of drive roll 6 and tension drum 8, when movable separator 13 moves along drive roll 6 and tension drum 8 cylinder top layer, graphite and sulfuric acid mixture there will be nonwoven fabric from filaments, when separator starts back to move, graphite and sulfuric acid mixture generating portion are shed in receiving vat 11.
During work, movable separator 13 starts counterclockwise running.Meanwhile, graphite suspension is filled in the transverse section 15 of movable separator 13 evenly to formulate thickness, and then, in movable separator 13 moving process, graphite suspension enters the region between Combined anode 4 and porous cathode 5.Then, movable separator 13 moves along drive roll 6 cylinder top layer, is back to tension drum 8, close to pipe connecting 2.Like this, graphite suspension separates with movable separator 13, enter in receiving vat 11, current flow out from washing machine 10, clean graphite suspension and resistates, and the product of electro-chemical machining is flushed in external filter along receiving vat 11, the interlayer graphite produced is developed, carries out heating power processing.
Following table 1 is according to the inventive method, changes the preparation result that different parameters carries out interlayer intercalated graphite.Wherein, in sample 3 and 6, sulfuric acid concentration is 94%, and anode and negative electrode are made up of stainless steel.In sample 2-8, in form, list the design parameter value of method, and generate the coefficient of expansion of product.
Table 1
The present invention in the method producing interlayer graphite and equipment thereof, by changing parameter, can also add and supplementing technique, and change the convenience of device structure, under guarantee interlayer graphite produces the high expanded graphite condition of use properties, raise the efficiency, simplified construction.The present invention produces interlayer graphite method and equipment can also in fields such as production atom, chemical industry, heat energy, metallurgy.
The above is only to better embodiment of the present invention, not any pro forma restriction is done to the present invention, every any simple modification done above embodiment according to technical spirit of the present invention, equivalent variations and modification, all belong in the scope of technical solution of the present invention.
Claims (6)
1. an interlayer intercalated graphite preparation apparatus, is characterized in that: comprise pipe connecting graphite mixture being carried out to stirring and smooth thickness; The Combined anode of direct current positive pole can be connected and the porous cathode of direct current negative pole can be connected; Between Combined anode and porous cathode, carrying and mobile graphite mixture and suspension liquid, and make suspension liquid contact the movable separator of Combined anode.
2. according to interlayer intercalated graphite preparation apparatus a kind of described in claim 1, it is characterized in that: described Combined anode is paddle electrode, be made up of some blade electrodes, blade electrode to each other distance is 10-25mm.
3. according to interlayer intercalated graphite preparation apparatus a kind of described in claim 1, it is characterized in that: described pipe connecting is arranged on framework, pipe connecting bottom opening, horizontal adjustment roller is installed in pipe connecting, the mixture of graphite and sulphuric acid soln enters in pipe connecting, horizontal adjustment roller adjusts mixture thickness and makes mixture smooth, Combined anode is arranged on framework, Combined anode and frame insulation, porous cathode level is arranged on framework, and be positioned at below Combined anode, kept apart by movable separator between Combined anode and porous cathode, Combined anode distance moving separator distance is 4-14mm, movable separator is the closed travelling belt with watt edge and transverse section, the bottom opening of pipe connecting is positioned at above the transverse section of movable separator, movable separator two ends are respectively fitted with drive roll and tension drum, tension drum is furnished with take-up device, be used for straining travelling belt, drive roll is furnished with drive roll transmission mechanism, travelling belt above movable separator is positioned at porous cathode surface, washing machine is arranged on framework, be positioned at the travelling belt both sides below movable separator, be used for cleaning movable separator, below washing machine, receiving vat is installed, receiving vat side is restriction sidewall.
4. according to interlayer intercalated graphite preparation apparatus a kind of described in claim 3, it is characterized in that: described receiving vat is inclined and mounted on framework, and current flow out from washing machine, interlayer graphite pours in outside suction filter along tilting receiving vat by current.
5., according to interlayer intercalated graphite preparation apparatus a kind of described in claim 3, it is characterized in that: described movable separator speed is 1-18cm/min.
6. according to interlayer intercalated graphite preparation apparatus a kind of described in claim 3, it is characterized in that: described transverse section is provided with some uniform projections, transverse section is divided into some grooves, and when movable separator moves, the mixture flowed down from pipe connecting and graphite suspension lay respectively in some grooves.
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| CN201510372161.8A CN104944420B (en) | 2015-06-30 | 2015-06-30 | Interlaminar intercalation graphite preparation equipment |
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| CN104944420B CN104944420B (en) | 2017-04-26 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113231023A (en) * | 2021-05-17 | 2021-08-10 | 黑龙江省科学院高技术研究院 | Preparation method and application of expanded graphite-based cobalt-indium bimetal hydroxide interlayer composite material |
Citations (3)
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| CN1094761A (en) * | 1993-05-05 | 1994-11-09 | 石家庄长城新技术公司 | The manufacture method of expansible black lead and device thereof |
| CN1097225A (en) * | 1993-04-26 | 1995-01-11 | 石家庄长城新技术公司 | Method for making expansible graphite and device thereof |
| CN1117021A (en) * | 1993-12-13 | 1996-02-21 | 朱庄德 | Anode oxidative treatment method and apparatus for producing expansible graphite |
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2015
- 2015-06-30 CN CN201510372161.8A patent/CN104944420B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1097225A (en) * | 1993-04-26 | 1995-01-11 | 石家庄长城新技术公司 | Method for making expansible graphite and device thereof |
| CN1094761A (en) * | 1993-05-05 | 1994-11-09 | 石家庄长城新技术公司 | The manufacture method of expansible black lead and device thereof |
| CN1117021A (en) * | 1993-12-13 | 1996-02-21 | 朱庄德 | Anode oxidative treatment method and apparatus for producing expansible graphite |
Non-Patent Citations (1)
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| 刘定福等: "可膨胀石墨电化学氧化法制备工艺研究进展", 《炭素技术》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113231023A (en) * | 2021-05-17 | 2021-08-10 | 黑龙江省科学院高技术研究院 | Preparation method and application of expanded graphite-based cobalt-indium bimetal hydroxide interlayer composite material |
| CN113231023B (en) * | 2021-05-17 | 2022-06-28 | 黑龙江省科学院高技术研究院 | Preparation method and application of expanded graphite-based cobalt-indium bimetal hydroxide interlayer composite material |
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Inventor after: Zhang Weijun Inventor after: Zhang Song Inventor after: Wei Jian Inventor after: Wang Yanli Inventor after: Semeni Yuri. Ivanovic Zoff. Inventor after: P Yount koves Ki. Mikhail. Anida Ibrahimovic Inventor after: Carle McNair. Nicola. Jimmy FEAU Ibrahimovic Inventor after: Fruit, Orleck. Yiouxi Bao's. Inventor after: Guinness. Sergei. Based on the fruit of Norwich mergie Inventor after: Zhang Xiaochen Inventor after: Liu Hongcheng Inventor after: Zhou Guojiang Inventor after: Li Zhe Inventor after: Ren Liwei Inventor after: Zhang Yuting Inventor after: Wang Jue Inventor after: Wang Xiubo Inventor before: Zhang Weijun Inventor before: Wei Jian Inventor before: Semeni Yuri. Ivanovic Zoff. Inventor before: P Yount koves Ki. Mikhail. Anida Ibrahimovic Inventor before: Carle McNair. Nicola. Jimmy FEAU Ibrahimovic Inventor before: Fruit, Orleck. Yiouxi Bao's. Inventor before: Guinness. Sergei. Based on the fruit of Norwich mergie Inventor before: Zhang Xiaochen Inventor before: Zhou Guojiang Inventor before: Li Zhe Inventor before: Liu Hongcheng Inventor before: Ren Liwei Inventor before: Zhang Yuting Inventor before: Wang Xiubo Inventor before: Zhang Song |
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