CN1029693C - Expanding graphite made device and method thereof - Google Patents
Expanding graphite made device and method thereof Download PDFInfo
- Publication number
- CN1029693C CN1029693C CN92111135A CN92111135A CN1029693C CN 1029693 C CN1029693 C CN 1029693C CN 92111135 A CN92111135 A CN 92111135A CN 92111135 A CN92111135 A CN 92111135A CN 1029693 C CN1029693 C CN 1029693C
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- China
- Prior art keywords
- graphite
- electrochemical reaction
- negative electrode
- groove
- reaction groove
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- Expired - Fee Related
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/20—Graphite
- C01B32/21—After-treatment
- C01B32/23—Oxidation
Abstract
The present invention provides an expanding graphite preparing device and a method thereof. The device comprises an electrochemical reaction groove, wherein inserter solution is injected into the groove; an anode, a cathode and a permeable partition plate are correspondingly filled in the groove. The present invention is characterized in that the electrochemical reaction groove is slantwise installed on a transmission device, and rotates along with the rotation of the transmission device to form a uniform electrochemical reaction field; the concentration of the inserter solution is uniform. In this way, the present invention improves product quality, enhances the quantity of filling graphite in a single groove, shortens reaction time, and largely enhances a production rate. The present invention is also convenient for realizing mechanization.
Description
The present invention relates to method for making expansible graphite and device thereof.
Natural graphite is the netted plane of a carbon atom hexagonal overlay structure, a little less than the interlayer bonding force.With manual method can between graphite, insert foreign atom, ion, molecule, it combines with carbon atom and forms compound between graphite layers.If this intercalation compound belongs to heating and can decompose, moment becomes gas and loss, can produce 10～400 times expansion on graphite crystal C direction of principal axis, so be called expansible black lead.With it is raw material, makes soft graphite, can do sealing material or shielding material etc.Has good industrial use value.
Up to now, the manufacturing of expansible black lead is except that traditional chemical process, also developed electrochemical method, as the Japanese Patent spy open clear 55-62807 number put down in writing, natural graphite is inserted in the electrolytic bath, add electrode energising, carry out anodic oxidation treatment, with the reversal of current energising, carry out cathodic reduction and handle then, after repeated multiple times is carried out above-mentioned oxidation-reduction processing, graphite is taken out washing and drying, can obtain expansible black lead.In similar approach, 0.1～100Hz ac process is led in the employing that has, and replaces above-mentioned cathodic reduction to handle, the requirement that has add depress or whipped state under carry out anodic oxidation treatment (Fig. 2 a), this require special whipping appts certainly; The special reaction frame of the employing static state that has is shown in (Fig. 2 b), and the somebody proposes to strengthen the pole plate area or reduces pole distance recently, with the acquisition uniform electric field, thus the cancellation cathodic reduction stage etc.
Utilize above-mentioned existing manufacture method and device thereof that following weak point is arranged.
1, after the anodic oxidation, logical reversible circulation carries out cathodic reduction, and technology difficulty is big, the equipment complexity.
2, use static special reaction frame all maintained static because of pole plate and electrolysis wood, although it is even as far as possible that electric field can be done, be difficult to make the every residing environment of graphite just the same, electrochemistry liquid concentration just has difference, electrically contact also difficult the assurance, bring detrimentally affect to product performance.
3, above-mentioned two class methods, after the energising reaction, passivation very easily takes place in anode, reduces speed of response,
Thereby reduced production efficiency, and be difficult for realizing mechanize.
4, above-mentioned whipping appts be easy to generate stirring less than the dead angle, and be prone to graphite and do not contact with anode, be unfavorable for the anodic oxidation intercalation of graphite, this situation can be more obvious in big production.
The objective of the invention is at above-mentioned weak point, a kind of manufacture method and device thereof of improved expansible black lead is provided,, can reduce operation again simultaneously, be suitable for scale operation to guarantee to obtain superior prod.
For achieving the above object, improved expanding graphite made device comprises the electrochemical reaction groove, inject inset solution in the groove, and negative electrode, anode and porous spacer plate be housed, it is characterized in that said electrochemical reaction groove is contained on the transmission mechanism obliquely, rotates with transmission mechanism, anode is fixed on the electrochemical reaction cell wall, and negative electrode and anode are staggered relatively; Preferably the position is adjustable, and transmission mechanism drives the electrochemical reaction groove and rotates, and speed range is 0.1～15 rev/min, and optimum revolution is 1～3 rev/min.
The modified version method for making expansible graphite utilizes said apparatus, it is characterized in that, comprises the following steps:
(1) pending natural graphite flakes is packed into above-mentioned electrochemical reaction groove, and inject inset solution;
(2) load onto negative electrode, and suitably adjust negative electrode and anodic distance according to the natural graphite Intake Quantity;
(3) give negative electrode, anodal closure, carry out the anodic oxidation treatment of graphite, and start transmission mechanism simultaneously, rotate to drive the electrochemical reaction groove;
(4) take out the graphite of handling, washing, drying.
Utilize said apparatus and method, because the electrochemical reaction groove constantly rotates, this just makes two interelectrode pending graphite particles be in the reacting field that is equal to from whole insertion process, this comprises electric field and concentration field, promptly from the statistics viewpoint, it is identical that graphite particle is in electric field probability everywhere, level of response is even, speed of response is accelerated this can avoid in a large number the residual of " dead sheet ", (dead sheet is meant that entire reaction course is in the graphite flake in the unfavorable relatively place of electric field) because rotation is fully constantly flowed inset solution, eliminated concentration polarization simultaneously, can guarantee to obtain the measured expansible black lead of matter, also have in the anodic oxidation reactions process, a large amount of graphite particles contact with anode surface, and do relative fricting movement with the reactive tank rotation, can slow down anode passivation effectively, reduction obviously improves quality product because of the influence of passivation to speed of response, and improves pack into the quantity of graphite of single groove, shorten the reaction times, boost productivity greatly.Also be convenient to realize mechanize.
The simple declaration of accompanying drawing and accompanying drawing:
Fig. 1 is the constructed profile of improvement expanding graphite made device,
Fig. 2 is existing device constructed profile
Wherein Fig. 2 (a) has whipping appts
Fig. 2 (b) is static special reaction frame type device
Symbol is among the figure: 1. negative electrode
2. electrochemical reaction groove
3. inset solution
4. graphite
5. anode
6. porous spacer plate
7. agitator
8. transmission mechanism
Embodiment.
On the bottom face of the cartridge type electrochemical reaction groove of the 45 ° of placements of tilting, a stainless steel garden shape positive plate (5) is housed, with (4) 1 kilograms of pending " 599 " natural flake graphites reactive tank (2) of packing into, and contact with anode (5), inject sulphuric acid soln (3) to reactive tank again, strength of solution is selected in 14.0～18.2 mol, elect 18.2 mol in the present embodiment as, from reactive tank (2) the opening end negative electrode (1) of packing into, staggered relatively with positive plate (5), negative electrode and anodic distance are adjustable.After said apparatus was ready, to the pole plate energising, electric weight should be controlled in 1～100Ah/kg graphite scope, and optimum range is 8～40Ah/kg graphite, and present embodiment is a 20Ah/kg graphite.Transmission mechanism (8) begins to drive reactive tank (2) rotation simultaneously, and rotating speed is 1 rev/min, after waiting to handle, takes out, and cleans, and drying obtains qualified product, and expansion rate is 200 a milliliters/gram graphite.
Claims (4)
1, a kind of method for making expansible graphite is characterized in that, this method comprises the following steps:
(1) pending natural graphite flakes is packed into electrochemical reaction groove, and inject inset solution;
(2) load onto negative electrode, and suitably adjust negative electrode and anodic distance according to the natural graphite Intake Quantity;
(3) give negative electrode, anodal closure, carry out the anodic oxidation treatment of graphite, electric weight is in 1～100Ah/Kg graphite scope, and starts transmission mechanism simultaneously, rotates to drive the electrochemical reaction groove, and its rotating speed is 0.1～30 rev/min;
(4) take out the graphite of handling, washing, drying.
2, the manufacture method of putting down in writing according to claim 1 is characterized in that, said electric weight scope is 8～40Ah/Kg graphite.
3, a kind of special-purpose manufacturing installation of expansible black lead, comprise the electrochemical reaction groove, inject inset solution in the groove, and negative electrode, anode and porous spacer plate are housed, it is characterized in that said electrochemical reaction groove is contained on the transmission mechanism obliquely, reactive tank rotates with transmission mechanism, rotating speed is 0.1～30 rev/min, and said anode is fixed on the electrochemical reaction groove, and negative electrode and anode are staggered relatively.
4, the expanding graphite made device of putting down in writing according to claim 3 is characterized in that, said negative electrode position is adjustable, in order to select and the suitable distance of anodic.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN92111135A CN1029693C (en) | 1992-09-29 | 1992-09-29 | Expanding graphite made device and method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN92111135A CN1029693C (en) | 1992-09-29 | 1992-09-29 | Expanding graphite made device and method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1070889A CN1070889A (en) | 1993-04-14 |
| CN1029693C true CN1029693C (en) | 1995-09-06 |
Family
ID=4945168
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN92111135A Expired - Fee Related CN1029693C (en) | 1992-09-29 | 1992-09-29 | Expanding graphite made device and method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1029693C (en) |
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1992
- 1992-09-29 CN CN92111135A patent/CN1029693C/en not_active Expired - Fee Related
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| Publication number | Publication date |
|---|---|
| CN1070889A (en) | 1993-04-14 |
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