CN1030535C - Process and equipments for production of expandable graphite - Google Patents
Process and equipments for production of expandable graphite Download PDFInfo
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- CN1030535C CN1030535C CN 91111825 CN91111825A CN1030535C CN 1030535 C CN1030535 C CN 1030535C CN 91111825 CN91111825 CN 91111825 CN 91111825 A CN91111825 A CN 91111825A CN 1030535 C CN1030535 C CN 1030535C
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- graphite
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- frame
- plate
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Abstract
The present invention provides a process and equipment for the preparation of expandable graphite. The equipment comprises an electrochemical reaction trough; electrochemical solution and an electrode are filled in the trough; a frame prepared from a leak proper plate is filled on one side near an anode; graphite to be treated is filled in the frame; a cathode plate and an anode plate are parallel; the rate of plate spacing to the dimension of the short edge lines of the cathode plate and the anode plate is smaller than 0.35. In the process, direct current is led for oxidizing the anode; the graphite is not pressurized, stirred, etc. The present invention simplifies a technology and ensures the quality.
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.Can insert foreign atom, ion, molecule in graphite layers with manual method, 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 be as sealing material or shielding material etc.
Up to now, the manufacture method of expansible black lead is except traditional chemical method, also developed electrochemical method, the Japanese Patent spy opens that clear 55-62807 grade disclosed, and natural graphite is inserted in the electrolytic bath, by two electrifying electrodes, 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, drying, can obtain expansible black lead.In similar method, 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; What have also will make electrode with the platinum silk screen.
Above-mentioned existing manufacture method and device thereof have following shortcoming:
1. need logical reversible circulation carry out cathodic reduction after the anodic oxidation, make the equipment complexity, and during cathodic reduction, very easy polarization, thereby technology difficulty is big.
2. increase and stir and pressurizing device, increased the difficulty of cost and technology.
Purpose of the present invention just is, a kind of manufacture method and device thereof of expansible black lead is provided, and is guaranteeing under the product quality premise that simplified apparatus is simplified technology greatly.
In order to achieve the above object, the method for making expansible graphite that proposes among the present invention comprises the following steps:
1. in filling the electrochemical reaction groove of electrolytic solution, proximal pole anomaly column electrode plate is set, anode and cathode apart from the ratio of the linear dimension of pole plate minor face less than 0.35, to form in a big way electrochemical field uniformly.
2. natural graphite is put into the permeable barrier frame, again the dividing plate frame is put into electrochemical reaction groove anode side.
3. logical direct current carries out anodic oxidation treatment to graphite.
4. graphite is taken out washing, drying.
To achieve the above object, expanding graphite made device provided by the invention, form by following several parts:
The electrochemical reaction groove of inset solution is housed; Negative electrode, the anode electrode compatible with above-mentioned inset solution are housed in the groove; In anode side the permeable frame of above-mentioned solution is housed, pending natural graphite is housed in the frame, it is characterized in that two electrodes are parallel, the ratio of cathode and anode spacing and the linear dimension of pole plate minor face is less than 0.35.
Utilize above-mentioned device, mainly be because shortened interpole gap relatively, add the relatively large-area battery lead plate of employing, between two-plate, formed uniform electrochemical field in a big way, in this electrochemical field, make all pending graphite particles all have the reaction conditions that is equal to, speed of response is identical.This just provides good precondition for simplifying technology, for example, there is no need by stirring, technologies such as pressurization are improved the homogenizing condition of particle reaction, since and reaction is uniformly, thereby just do not need after anodic oxidation, again current reversal carried out cathodic reduction and handle.This can not only simplify the difficulty of technology and operation greatly, and can ensure the quality of products, and obtains that quality is good, the uniform expansible black lead of performance.
Introduce an embodiment in detail below in conjunction with accompanying drawing:
Accompanying drawing 1 is the expanding graphite made device sectional view
Fig. 1 (a) is the front section view of this device
Fig. 2 (b) is the AA ' sectional view of this device
Accompanying drawing 2 is existing device diagrammatic cross-section
Fig. 2 (a) is with pressurizing device
Fig. 2 (b) is with whipping appts
Nomenclature:
1. electrochemical reaction groove
2. positive plate
3. negative plate
4. porous spacer plate framework
5. graphite
6. electrolytic solution
7. direct supply
8. pressurization weight
9. agitator
In the middle of the electrochemical reaction groove, a planar anode plate of being made by stainless steel is housed, near two negative plates of being made by stainless material of reactive tank two walls, it is parallel relative with above-mentioned positive plate in the positive plate both sides, and the area of each pole plate is 50 * 40cm
2, anode and cathode spacing are 7.5cm.Inject sulphuric acid soln in reactive tank, concentration is higher for well, adopts 14～18.2 mol in the present embodiment.
5kg puts into the frame of being made by permeable separator with 599 pending natural flake graphites (carbon amount 99%, median size 0.30mm), then frame is inserted above-mentioned positive plate both sides, that is to say that positive plate inserts in the above-mentioned frame.Permeable separator is graphite to be isolated in the positive column and the impurity such as gas that produce in solution and the reaction are permeable, is compiled into by plastic tape here.After said apparatus is ready,, answer control current density at 5～50 milliamperes/cm to the pole plate energising
2(pressing the positive plate area calculates) elects 15mA/cm as in the present embodiment
2For expansion multiplying power is the graphite of 70～300ml/g, handles the electric quantity density of graphite and is advisable at 20～70Ahr/kg.Be that 3.5 volts of electric currents are that oxidation treatment time is elected 3 hours as under 60 amperes the situation at voltage in the present embodiment, then electric quantity density is 45Ahr/kg.
After the anodic oxidation treatment, graphite is taken out washing, drying from frame.Expansible black lead finished product S＜2.5%, volatile matter＜12%, 950 ℃ allowance for expansion 210ml/g places after three months allowance for expansion reduced rate＜15%.Make 1000mm * 0.38mm rolling flexible graphite paper, its density 1.01g/cm
3The time, tensile strength reaches 5.0MPa, S＜1000ppm.
The electrolytic solution that present method is used removes H
2SO
4, also can use HNO
3, H
3PO
4And some metal salt solution or organic solution, also can be at H
2SO
4Add small amount of H NO in the solution
3, H
2O
2, NaNO
3Deng.
The two ends of electrochemical reaction groove of this device and isolation frame also can be openings, and an end pushes graphite, and the graphite that the other end is crossed anodic oxidation treatment is released, and like this, can realize continuous production.
Utilize these apparatus and method, make device simply not need special electrode, needn't pressurize or whipping appts, because interpolar forms uniform electrochemical field in a big way, all graphite particles all are under the electrochemical conditions that is equal to, and speed of response is the same, the degree of each zone reaction is all identical, do not need to carry out cathodic reduction again and handle, technology is easy to control, is convenient to industrial-scale production.Moreover, when simplifying technology, also improved the quality of product, have the characteristics of low-sulfur, low volatile, and product performance have been more even.Work simplification in addition, just easier realization serialization industrial production.
Claims (3)
1, a kind of manufacturing installation of expansible black lead, comprise the electrochemical reaction groove, electrochemical solution is housed in the groove, electrode is housed in the reactive tank, and anode and negative electrode are equipped with the frame that the infiltration plate is made by anode one side between the two poles of the earth, the pending graphite of packing in the frame, it is characterized in that above-mentioned pole plate is what be parallel to each other, the ratio of interpole gap and pole plate minor face linear dimension is less than 0.35.
2, the device of putting down in writing according to claim 1 is characterized in that said electrochemical reaction groove and frame are the two ends weapons, and an end pushes pending graphite, and an end is released the graphite of having handled well.
3, a kind of manufacture method of expansible black lead is characterized in that this method comprises the following steps:
(1) in filling the electrochemical reaction groove of electrolytic solution, proximal pole anomaly column electrode plate is set, anode and cathode compares less than 0.35 apart from the size with the pole plate minor face;
(2) natural graphite is put into the permeable barrier frame, again the dividing plate frame is put into electrochemical cell near anode one side;
(3) logical direct current carries out anodic oxidation to graphite;
(4) graphite is taken out washing, drying.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 91111825 CN1030535C (en) | 1991-12-26 | 1991-12-26 | Process and equipments for production of expandable graphite |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 91111825 CN1030535C (en) | 1991-12-26 | 1991-12-26 | Process and equipments for production of expandable graphite |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1061387A CN1061387A (en) | 1992-05-27 |
| CN1030535C true CN1030535C (en) | 1995-12-20 |
Family
ID=4910886
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 91111825 Expired - Fee Related CN1030535C (en) | 1991-12-26 | 1991-12-26 | Process and equipments for production of expandable graphite |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1030535C (en) |
Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE69606529T2 (en) * | 1995-04-28 | 2000-08-31 | Avdeev Viktor Vasilievic | METHOD AND DEVICE FOR PRODUCING OXIDIZED GRAPHITE |
| CN1297475C (en) * | 2004-06-30 | 2007-01-31 | 深圳大学 | Process for preparing expanded graphite |
| CN100545321C (en) * | 2007-11-05 | 2009-09-30 | 攀钢集团攀枝花钢铁研究院 | Graphite felt surface modifying method and modified graphite felt |
| TWI564244B (en) * | 2014-12-25 | 2017-01-01 | 國立臺灣師範大學 | Equipment for making graphene and its making method |
| US11584650B2 (en) | 2015-12-14 | 2023-02-21 | Baoshan Iron & Steel Co., Ltd. | Graphene oxide and method of production thereof |
| CN109790640B (en) * | 2016-08-08 | 2021-11-02 | 得克萨斯州A&M大学*** | Electrochemically expanded materials and reactors and methods of making same |
| CN111453723A (en) * | 2020-05-28 | 2020-07-28 | 鹰领航空高端装备技术秦皇岛有限公司 | Expandable graphite preparation device and electrochemical intercalation method thereof |
| CN114105135A (en) * | 2021-12-24 | 2022-03-01 | 湖南大学 | Method for electrochemically assisting preparation of low-defect expanded graphite paper |
-
1991
- 1991-12-26 CN CN 91111825 patent/CN1030535C/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| CN1061387A (en) | 1992-05-27 |
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