CN105036119A - Preparing method of interlayer intercalation graphite - Google Patents
Preparing method of interlayer intercalation graphite Download PDFInfo
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- CN105036119A CN105036119A CN201510372162.2A CN201510372162A CN105036119A CN 105036119 A CN105036119 A CN 105036119A CN 201510372162 A CN201510372162 A CN 201510372162A CN 105036119 A CN105036119 A CN 105036119A
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Abstract
The invention discloses a preparing method of interlayer intercalation graphite. The method comprises the steps of stirring graphite and sulfuric acid to prepare a mixture, placing the mixture into a connecting pipe for bearing, entering the transverse section of a mobile separator, leveling and adjusting the thickness of the mixture by using a horizontal adjustment roller, adding graphite suspension into the connecting pipe, and along with the movement of the mobile separator, enabling a mixture layer to move to a position below a combined type anode to enable a graphite suspension layer to contact with the combined type anode to switch on direct current, wherein the current density is 25 to 42 Ma/cm<2>, and the current passes through a graphite and sulfuric acid solution mixture layer, along with the consumption of the graphite suspension, new graphite suspension needs to be supplemented into the connecting pipeline to ensure the continuous operation of a flow for preparing the intercalation graphite, and when the mobile separator moves between the combined type anode and a porous cathode, the graphite suspension and the mixture are changed into the intercalation graphite under the effect of the direct current. The preparation method provided 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 method.
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 adopt liquid chemical method to produce interlayer intercalated graphite in the industry, method comprises with strong oxidizer and interlayer thing process graphite.Oxygenant comprises: potassium bichromate, nitric acid, ammonium persulphate, hydrogen peroxide, chromic oxide (VI) (anhydrous chromic acid) etc.Intercalation thing material chooses sulfuric acid, nitric acid, phosphoric acid, some salt, and this kind of method exists very serious shortcoming, and precondition uses strong oxidizer and concentrated acid.It is a kind of more economical effective means that electrochemical oxidation method produces interlayer intercalated graphite.Electrochemical oxidation method 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 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 method 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 method, solve existing preparation method and use high-concentration sulfuric acid, electrolytic solution consumption is large, and the problem that power consumption is large.
The technical solution adopted in the present invention is that the sulfuric acid of 30%-94% is according to (0.5 – 1.0 с m by graphite and concentration
3): 1g stirs, make mixture, mixture is put into the pipe connecting of carrying, enter on the transverse section of movable separator, flatten with horizontal adjustment roller and adjust the thickness of mixture, graphite suspension is added in pipe connecting, along with movable separator moves, mixture layer moves to below Combined anode, and graphite suspension layer is encountered Combined anode, connect direct current, current density 25 – 42m А/с m
2electric current is by graphite and sulphuric acid soln mixture layer, along with the consumption of graphite suspension, new graphite suspension to be supplemented in pipe connecting, ensure that the flow process producing interlayer graphite runs without interruption, when movable separator moves between Combined anode and porous cathode, graphite suspension and mixture are transformed into interlayer graphite under direct current effect.
Further, described mixture preparation, adopt 98% concentration sulphuric acid and the 50kg-100kg deionized water and stirring of 50kg-100kg, the sulphuric acid soln generating 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.
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: 98% concentration sulphuric acid and the 50kg-100kg deionized water and stirring that adopt 50kg-100kg, generate the sulphuric acid soln of 20%-50% concentration, the crystalline flake graphite 80-100kg getting 50-100L and carbon content 99% stirs, make the mixture that density is the pulpous state of 1.72g/cm3, 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, graphite suspension is added in pipe connecting 2, along with movable separator 13 moves, mixture layer moves to below Combined anode 4, graphite suspension layer is encountered Combined anode 4, connect 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 (2)
1. an interlayer intercalated graphite preparation method, is characterized in that, carries out according to following steps: be that the sulfuric acid of 30%-94% is according to (0.5-1.0cm by graphite and concentration
3): 1g stirs, make mixture, mixture is put into the pipe connecting of carrying, enter on the transverse section of movable separator, flatten with horizontal adjustment roller and adjust the thickness of mixture, graphite suspension is added in pipe connecting, along with movable separator moves, mixture layer moves to below Combined anode, and graphite suspension layer is encountered Combined anode, connect direct current, current density 25-42mA/ с m
2electric current is by graphite and sulphuric acid soln mixture layer, along with the consumption of graphite suspension, new graphite suspension to be supplemented in pipe connecting, ensure that the flow process producing interlayer graphite runs without interruption, when movable separator moves between Combined anode and porous cathode, graphite suspension and mixture are transformed into interlayer graphite under direct current effect.
2. according to interlayer intercalated graphite preparation method a kind of described in claim 1, it is characterized in that: described mixture preparation, adopt 98% concentration sulphuric acid and the 50kg-100kg deionized water and stirring of 50kg-100kg, generate the sulphuric acid soln of 20%-50% concentration, get 50-100L, stir with the crystalline flake graphite 80-100kg of carbon content 99%, make the mixture that density is the pulpous state of 1.72g/cm3.
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| CN105036119B CN105036119B (en) | 2017-05-03 |
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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)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN1189141A (en) * | 1995-04-28 | 1998-07-29 | V·V·阿吾迪夫 | Process and device for obtaining oxidised graphite |
-
2015
- 2015-06-30 CN CN201510372162.2A patent/CN105036119B/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 |
| CN1189141A (en) * | 1995-04-28 | 1998-07-29 | V·V·阿吾迪夫 | Process and device for obtaining oxidised graphite |
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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