CN85103917A - Expansible black lead and manufacture method thereof - Google Patents
Expansible black lead and manufacture method thereof Download PDFInfo
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- CN85103917A CN85103917A CN198585103917A CN85103917A CN85103917A CN 85103917 A CN85103917 A CN 85103917A CN 198585103917 A CN198585103917 A CN 198585103917A CN 85103917 A CN85103917 A CN 85103917A CN 85103917 A CN85103917 A CN 85103917A
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Abstract
Expansible black lead and manufacture method thereof relate to expansible black lead and the method for manufacturing technology thereof with stable high expansioning multiple.Belong to the chemical treatment of graphite, it is little and unstable to have solved the prior art expansion multiple.And to problems such as graphite raw material granularity requirements height, adopt respectively and soak granular graphite with nitric acid and sulfuric acid successively, after water cleans low temperature dry by the fire to water content less than 10% after, adding lime powder handles and sieves, make the expansible black lead of making have stable high expansioning multiple, the end product of this expansible black lead has good physicals, is suitable for making various sealing members etc.
Description
The present invention relates to have the expansible black lead of stable high expansioning multiple, and the processing method of making this graphite, the chemical treatment of graphite belonged to.
Before the present invention makes, what the method for manufacturing technology of expanded graphite meterial was introduced as " electrical carbon " 1981 1 phases is more than 97% with purity, (international standard sieves is with number for granularity 50 orders, down together) above crystalline flake graphite is put into nitric acid and the sulfuric acid mixture liquid for preparing by a certain percentage, under the temperature of room temperature to 105 ℃, acidification was preferably 3-4 hour more than 1 minute, filtering acid solution is then dried under 105 ± 5 ℃ of temperature through the washing back." graphite crossed through this acidification then is expansible black lead." it is again through 800～1000 ℃ high temperature instantaneously heating, just can make to expand into originally more than 80 times on the C direction of principal axis of graphite-structure, makes expanded graphite meterial ".In addition just like disclosed in No. the 4146401st, the US Patent specification: " granular graphite is immersed in nitric acid and the vitriolic mixed solution; the granular graphite that acid soak is crossed cleans with the water of pH value 4-7; again the granular graphite that soaks into is put into phosphoric acid or the aqueous phosphatic that per kilogram contains 0.05～1.0 molconcentration; perhaps preferably soaked 0.5 to 10 hour; granular graphite is washed once more thereafter in aluminium phosphate aqueous solution; 800 ℃ of the granular graphite heating of the water content about 30% through handling like this, just may be expanded to 60 times of former granular graphite size, this expanded graphite meterial has stronger autohension and compressibility, can compression moulding under need not the situation of any tackiness agent ".
The producing and manufacturing technique of above-described expanded graphite meterial exists tangible deficiency: one, dry through 105 ℃ temperature after the granular graphite washing after the acidifying, its expansion multiple can obviously descend, thereby the autohension of expanded graphite meterial and compressibility are reduced, directly have influence on the physicals of end product.Its two, if make graphite after the acidifying washing as a kind of intermediates-expansible black lead, its water content is big, especially the expansion multiple instability all makes troubles for packing, accumulating and use.Its three, above-mentioned technology only is applicable to the graphite of the above granularity of 50 orders, to less than 50 purpose graphite, especially the following granular graphite of 100 orders is poor for applicability, this proposes certain requirement to the graphite raw material granularity, and the utilization of graphite resource is restricted.At above deficiency, the present invention has overcome these defectives.
The purpose of this invention is to provide and a kind ofly have the stable high expansioning multiple and the expansible black lead of low water content, and the method for manufacturing technology of this expansible black lead, this processing method also is applicable to greater than 200 purpose crystalline flake graphites.
The method of manufacturing technology of expansible black lead of the present invention is: " greater than 97%, granularity is put into salpeter solution earlier greater than 200 purpose crystalline flake graphites with carbon content, and the temperature of keeping room temperature to 100 ℃ is more than 1 minute, and 4～6 hours better.The weight ratio of granular graphite and nitric acid is (0.1～3): 1, and better with 2: 1.The concentration of nitric acid is not less than 60%.Again it is taken out filtering acid solution and puts into sulphuric acid soln, keep the temperature one minute to 12 hours of room temperature to 100 ℃, with 2-8 hour for well.Graphite and vitriolic weight ratio are (0.1～3): 1, with 0.5: 1 better, vitriolic concentration is not less than 90%.The granular graphite that successively soaked through twice acid solution is taken out, the filtering acid solution, cleaning to pH value with the water of pH value 5～6 is that this pH value of 3(is that to put into 20 parts of pH values be 7 clear water institute measured value to 1 part of graphite, down together), empty then solid carbon dioxide part be not more than dry by the fire under 100 ℃ the temperature to water content less than 10%, add lime powder, placed 1～24 hour the back that stirs, the weight of calcium oxide is advisable with the 2-10% of granular graphite weight, and granularity is less than graphite particle size.The granular graphite that will add at last after calcium oxide is handled sieves, and removes the calcium oxide composition.Then the process for making of whole expansible black lead is finished.
Through the expansible black lead that above-mentioned technological process is made, its pH value is 3, and water content is not more than 5%, and expansion multiple is more than 450 times, and places its expansion multiple for a long time and change and be not more than 5%.With this expansible black lead through 400～1000 ℃ of pyritous instantaneously heatings, resulting expanded graphite meterial is compared with the expanded graphite meterial that prior art produces, have stronger autohension and compressibility, the various physicalies of the end product made from this expanded graphite meterial all are better than the goods of prior art.
Said expansion multiple is meant expansible black lead after heat among the present invention, its volume (Cm
3) with the ratio of weight (g).
Main points of the present invention are graphite is used nitric acid and sulfuric acid immersion treatment respectively successively, the temperature of oven dry is not more than 100 ℃ after water cleans, and when the water content of graphite adds lime powder less than 10% the time, placed 1-24 hour the back that stirs, at last again through screening.
Compared with the prior art the present invention has following significant advantage, one, and the expansible black lead water content that this technological process is made is low, and expansion multiple is high and stablize.Its two, be suitable for the above crystalline flake graphite of 200 orders, this processing method is simple in addition, is easy to grasp.
Now with following specific embodiment, the present invention is further elaborated, used graphite is natural flake graphite in the example, and carbon content is greater than 97%, granularity 100 orders.
100 gram graphite are immersed in the 40 gram concentrated nitric acids, keep room temperature to 100 ℃, soaked 30 minutes.Filtering acid solution is then put into the 150 gram vitriol oils, soaks pull out after 2 hours, empty dry acid liquid, put into pH value and be 6 water and clean, being washed till pH value is taking-up in 3 o'clock.Under 60 ℃ temperature, dry to water content and be not more than 10%, add 7 grams, 200 purpose lime powders.Stir and placed 24 hours, then, the sieving separating lime powder.
Claims (9)
1, a kind of use nitric acid.Sulfuric acid soaks granular graphite, through the processing method of washing and oven dry manufacturing expansible black lead.It is characterized in that soaking granular graphite with nitric acid and sulfuric acid successively respectively, the oven dry after the washing is to carry out in the temperature below 100 ℃.Dry by the fire to water content less than after 10%, handle granular graphite with lime powder, then screening.
2, according to the processing method of the described manufacturing expansible black lead of claim 1, it is characterized in that saidly soaking with nitric acid and sulfuric acid successively respectively that granular graphite is performed such: graphite is put into salpeter solution earlier, keep the temperature of room temperature to 100 ℃, more than 1 minute, 4-6 hour better.Again granular graphite is taken out the filtering acid solution and puts into sulphuric acid soln, keep the temperature one minute to 12 hours of room temperature to 100 ℃, with 2-8 hour for well.
3, according to the processing method of the described manufacturing expansible black lead of claim 1, it is characterized in that handling that graphite is performed such with lime powder: dry through 100 ℃ of following temperature to water content less than 10% granular graphite adding lime powder, stir, placed 1-24 hour.
4,, it is characterized in that said screening is that the granular graphite that will add calcium oxide sieves again, separates granular graphite with lime powder according to the processing method of the described manufacturing expansible black lead of claim 1.
5, according to the processing method of the described manufacturing expansible black lead of claim 1, it is characterized in that granular graphite can be carbon content greater than 97%, granularity is not less than 200 purpose crystalline flake graphites.
6, according to the processing method of claim 1,2 described manufacturing expansible black leads, it is characterized in that the weight ratio of graphite and nitric acid is better with 2: 1, the concentration of nitric acid is not less than 60%.
7, according to the processing method of claim 1,2 described manufacturing expansible black leads, it is characterized in that graphite and vitriolic weight ratio are better with 0.5: 1, vitriolic concentration is not less than 90%.
8, according to the processing method of claim 1,3 described manufacturing expansible black leads, it is characterized in that the weight of lime powder is 2～10% of graphite weight, granularity is less than graphite particle size.
9, a kind of expansible black lead according to claim 1,2,3,4,5 described processing method manufacturings.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN198585103917A CN85103917A (en) | 1985-05-03 | 1985-05-03 | Expansible black lead and manufacture method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN198585103917A CN85103917A (en) | 1985-05-03 | 1985-05-03 | Expansible black lead and manufacture method thereof |
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| Publication Number | Publication Date |
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| CN85103917A true CN85103917A (en) | 1986-10-29 |
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| CN198585103917A Pending CN85103917A (en) | 1985-05-03 | 1985-05-03 | Expansible black lead and manufacture method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102244153A (en) * | 2011-04-19 | 2011-11-16 | 梁胜光 | Preparation method of graphite heat radiation fin |
| CN108190882A (en) * | 2018-02-26 | 2018-06-22 | 乌兰察布市大盛石墨新材料股份有限公司 | Conductive graphite paper and preparation method thereof |
-
1985
- 1985-05-03 CN CN198585103917A patent/CN85103917A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102244153A (en) * | 2011-04-19 | 2011-11-16 | 梁胜光 | Preparation method of graphite heat radiation fin |
| CN108190882A (en) * | 2018-02-26 | 2018-06-22 | 乌兰察布市大盛石墨新材料股份有限公司 | Conductive graphite paper and preparation method thereof |
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