CN1102444A - Method preparation of expansible black lead and its apparatus - Google Patents
Method preparation of expansible black lead and its apparatus Download PDFInfo
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- CN1102444A CN1102444A CN 94115576 CN94115576A CN1102444A CN 1102444 A CN1102444 A CN 1102444A CN 94115576 CN94115576 CN 94115576 CN 94115576 A CN94115576 A CN 94115576A CN 1102444 A CN1102444 A CN 1102444A
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Abstract
The process for preparing expansible graphite features use of electrolyte. During preparing, the electrolyte for anode oxidation is circulating between electrochemical reaction bath and liquid storage tank to increase the active utilization rate of solution and current, slow the polarization of auxiliary anode plate, speed up reaction and shorten oxidation time.
Description
The present invention relates to a kind of novel method and device thereof for preparing expansible black lead, belong to material science.Patent with the electrochemical production expansible black lead is existing several, as Chinese patent CN 1061387A, and CN 1061388A, CN 1068086A, CN 1068151A, CN 1070889A, CN 1068152A and U.S. Pat 03323869 etc.The ultimate principle of these methods all is identical, is anode with graphite and supplementary anode, utilizes electrolytic solution that graphite is carried out anodic oxidation, obtains expansible black lead, as C
n +(HSO4)
-
Expansible black lead is under the condition of high-temperature heat treatment, and the inset of graphite layers is separated out from graphite layers with the form of volatile gases, and makes laminate graphite expand tens times to hundred times along the C axle, the quasiflake graphite that forms expanded.The soft graphite product is then made in following process and compression moulding to graphite worm, and present widespread use is the covering slag in sealing material, the metallurgical industry, and can be used as senior catalyst, sorbing material, extinction material, electro-conductive material and magnetic shielding material etc.
Method in the above-mentioned patent is had nothing in common with each other, but the following shortcoming of ubiquity:
1. most of process using vitriol oils carry out anodic oxidation, but high temperature puffing can not effectively be removed the sulphur content in the expansible black lead, also are sulphur content in the limited minimizing expansible black lead even fully wash before expanded.And sulphur is to cause flexible graphite sealing material that equipment is carried out the corrosive principal element.
2. all have the problem of electrolyte flow difference in these technologies, this causes the effective rate of utilization of electrolytic solution low, the utilization ratio of electric current is low, be easy to polarization and cause electrolyte temperature rising, reaction effect variation so that can not carry out.Adopt ultrasonic wave among the patent CN 1068151A, but its labor condition is poor; Though it is fully mobile that electrolytic solution is obtained, its synthetic method is still chemical oxidization method in essence, and with so passing to direct current in reaction process, but graphite raw material is not to be in anode and just to be dipped among the sulphuric acid soln.
3. most of technologies all adopt corrodibility strong acid, and as the vitriol oil, concentrated nitric acid, difficult processing of its waste liquid and labor condition are poor.
The objective of the invention is provides a kind of novel electrolyte, and technological process is improved, with improve production efficiency and product quality at the weak point in the existing preparation expansible black lead technology.
Content of the present invention is that the new method of preparation expansible black lead comprises the following steps:
1. sample pretreatment comprises washing, oil removing to sample,
2. carry out anodic oxidation in electrolyzer, used electrolytic solution is NH
4NO
3The aqueous solution, concentration are 7.5wt%～40wt%, 15 ℃～60 ℃ of electrolyte temperatures, and current density is 25mA/cm
2～70mA/cm
2, 100A hour/kilogram～300A of energising amount hour/kilogram,
3. in the anodised while, electrolytic solution is circulated between electrolyzer and liquid-storing box,
4. the graphite to the oxidation gained carries out drying treatment, comprises the removal and the oven dry of electrolytic solution, 40 ℃～70 ℃ of bake out temperatures,
5. under 500 ℃～1000 ℃ graphite is carried out puffing, the time is 2 seconds～10 seconds
The device that electrolytic solution is circulated between electrolyzer and liquid-storing box is illustrated in accompanying drawing 1, and accompanying drawing 2 is the sectional view of A-A section.
This device comprises (1) electrolyzer, (2) negative plate, (3) electrolytic solution, (4) plastic silk screen hopper, (5) graphite, (6) positive plate, (7) conduit, (8) pump, (9) strainer, (10) liquid-collecting box etc.
Utilize the expansible black lead of prepared of the present invention, the expansion multiple height, sulphur content significantly is lower than prior art.Because improved the flowability of solution effectively, the effective rate of utilization and the current utilization rate of electrolytic solution are improved, and can slow down the polarization trend of positive plate, help improving the quality of expansible black lead.And do not contain strong acid in the used electrolytic solution, working conditions improves, and waste liquid is easy to handle, and helps environment protection.
Below be embodiments of the invention.In an embodiment, adopt ore deposit, Xinghe, the Inner Mongol 595 natural flake graphites, carbon content 95%, order several 50.Example weight 60g, 30 ℃ of electrolyte temperatures, 2 liters of electrolyzer volumes; 45 ℃ of drying temperatures, the beasurement base GB10698-89 of puffing and other parameter.
Embodiment sees Table:
| Nitric acid ammonia wt% | Anodic oxidation condition | Expansion rate ml/g | Sulphur content wt% | Ash content % | Volatile matter % | ||
| i?mA/ | T minute | ||||||
| 1 | 10 | 70 | 70 | 330 | 0.0606 | 2.77 | 8.19 |
| 2 | 30 | 60 | 85 | 230 | 0.0743 | 2.67 | 4.42 |
Claims (2)
1, a kind of manufacture method of expansible black lead is characterized in that the preparation method comprises the following steps:
(1) the sample desire is handled, and comprises the washing to sample, oil removing,
(2) carry out anodic oxidation in electrolyzer, used electrolytic solution is NH
4NO
3The aqueous solution, concentration are 7.5wt%～40wt%, 15 ℃～60 ℃ of electrolyte temperatures, and current density is 25mA/cm
2～70mA/cm
2, 100A hour/kilogram～300A of energising amount hour/kilogram,
(3) in the anodised while, electrolytic solution is circulated between electrolyzer and liquid-storing box,
(4) oxidation gained graphite is carried out drying treatment, comprise the removal and the oven dry of electrolytic solution, 40 ℃～60 ℃ of bake out temperatures,
(5) under 500 ℃～1000 ℃ graphite is carried out puffing, the time is 2 seconds～10 seconds.
2, a kind of preparation method as claimed in claim 1 and device thereof, mainly form by direct supply and line, electrolyzer, negative plate, supplementary anode plate, pump etc., oxidation electrolytic solution is housed in the electrolyzer, the groove inwall is a negative electrode, hopper is made by the common plastics silk screen and is placed therebetween, the supplementary anode plate closely contacts with graphite in the middle of hopper, it is characterized in that: electrolytic solution flows out through pump, strainer, reservoir from bottom of electrolytic tank and drenches down and inject groove by drain pipe materials supplied by customers box top to graphite.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 94115576 CN1102444A (en) | 1994-09-02 | 1994-09-02 | Method preparation of expansible black lead and its apparatus |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 94115576 CN1102444A (en) | 1994-09-02 | 1994-09-02 | Method preparation of expansible black lead and its apparatus |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1102444A true CN1102444A (en) | 1995-05-10 |
Family
ID=5037603
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 94115576 Pending CN1102444A (en) | 1994-09-02 | 1994-09-02 | Method preparation of expansible black lead and its apparatus |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1102444A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102286753A (en) * | 2011-05-30 | 2011-12-21 | 黑龙江科技学院 | Method for preparing high-purity low-sulphur expanded graphite |
| CN104789981A (en) * | 2015-03-31 | 2015-07-22 | 清华大学 | Preparation method for expanded graphite |
| CN109790640A (en) * | 2016-08-08 | 2019-05-21 | 得克萨斯州A&M大学系统 | The material and reactor and its manufacturing method of electrochemistry extension |
-
1994
- 1994-09-02 CN CN 94115576 patent/CN1102444A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102286753A (en) * | 2011-05-30 | 2011-12-21 | 黑龙江科技学院 | Method for preparing high-purity low-sulphur expanded graphite |
| CN104789981A (en) * | 2015-03-31 | 2015-07-22 | 清华大学 | Preparation method for expanded graphite |
| CN109790640A (en) * | 2016-08-08 | 2019-05-21 | 得克萨斯州A&M大学系统 | The material and reactor and its manufacturing method of electrochemistry extension |
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