JPS63159212A - Production of interlaminar compound of graphite - Google Patents
Production of interlaminar compound of graphiteInfo
- Publication number
- JPS63159212A JPS63159212A JP61307545A JP30754586A JPS63159212A JP S63159212 A JPS63159212 A JP S63159212A JP 61307545 A JP61307545 A JP 61307545A JP 30754586 A JP30754586 A JP 30754586A JP S63159212 A JPS63159212 A JP S63159212A
- Authority
- JP
- Japan
- Prior art keywords
- graphite
- hydrogen peroxide
- sulfuric acid
- hydroxyquinoline
- peroxide water
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 72
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 58
- 239000010439 graphite Substances 0.000 title claims abstract description 58
- 150000001875 compounds Chemical class 0.000 title claims abstract description 38
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 11
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 28
- MCJGNVYPOGVAJF-UHFFFAOYSA-N quinolin-8-ol Chemical compound C1=CN=C2C(O)=CC=CC2=C1 MCJGNVYPOGVAJF-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000005725 8-Hydroxyquinoline Substances 0.000 claims abstract description 14
- 229960003540 oxyquinoline Drugs 0.000 claims abstract description 14
- 239000002002 slurry Substances 0.000 claims abstract description 10
- 238000000034 method Methods 0.000 claims abstract description 6
- 238000009830 intercalation Methods 0.000 claims description 34
- 230000002687 intercalation Effects 0.000 claims description 34
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 29
- 238000000354 decomposition reaction Methods 0.000 abstract description 6
- QOSATHPSBFQAML-UHFFFAOYSA-N hydrogen peroxide;hydrate Chemical group O.OO QOSATHPSBFQAML-UHFFFAOYSA-N 0.000 abstract 6
- 238000006243 chemical reaction Methods 0.000 description 7
- 239000010410 layer Substances 0.000 description 6
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- 229910052799 carbon Inorganic materials 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 239000000376 reactant Substances 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 239000011229 interlayer Substances 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 239000003381 stabilizer Substances 0.000 description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 239000013626 chemical specie Substances 0.000 description 2
- 229910052736 halogen Inorganic materials 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 229910017604 nitric acid Inorganic materials 0.000 description 2
- 239000007800 oxidant agent Substances 0.000 description 2
- 238000012856 packing Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- QLOKJRIVRGCVIM-UHFFFAOYSA-N 1-[(4-methylsulfanylphenyl)methyl]piperazine Chemical compound C1=CC(SC)=CC=C1CN1CCNCC1 QLOKJRIVRGCVIM-UHFFFAOYSA-N 0.000 description 1
- XTEGARKTQYYJKE-UHFFFAOYSA-M Chlorate Chemical class [O-]Cl(=O)=O XTEGARKTQYYJKE-UHFFFAOYSA-M 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- ZCDOYSPFYFSLEW-UHFFFAOYSA-N chromate(2-) Chemical class [O-][Cr]([O-])(=O)=O ZCDOYSPFYFSLEW-UHFFFAOYSA-N 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 210000004709 eyebrow Anatomy 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000005755 formation reaction Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- -1 halogen oxygen salts Chemical class 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- XEMZLVDIUVCKGL-UHFFFAOYSA-N hydrogen peroxide;sulfuric acid Chemical compound OO.OS(O)(=O)=O XEMZLVDIUVCKGL-UHFFFAOYSA-N 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical class OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 description 1
- VKJKEPKFPUWCAS-UHFFFAOYSA-M potassium chlorate Chemical compound [K+].[O-]Cl(=O)=O VKJKEPKFPUWCAS-UHFFFAOYSA-M 0.000 description 1
- 239000012286 potassium permanganate Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Landscapes
- Carbon And Carbon Compounds (AREA)
Abstract
Description
【発明の詳細な説明】
（産業上の利用分野）
本発明はガスケット、パツキンなどく使用される可撓性
黒鉛製品の材料となる黒鉛層間化合物の製造法に関する
。DETAILED DESCRIPTION OF THE INVENTION (Industrial Application Field) The present invention relates to a method for producing a graphite intercalation compound which is a material for flexible graphite products used such as gaskets and packing.
（従来の技術）
一般に黒鉛は炭素六員環網状平面が積み重りた層状構造
を有し１層平面の結合は強く緻密な網平面を形成してい
るが１層平面と直角な方向での結合は弱く９層間に相対
的に広い空間を有している。(Prior art) In general, graphite has a layered structure in which six-membered carbon ring network planes are piled up, and the bonds between the planes of one layer are strong and form a dense network plane, but the bonds are in the direction perpendicular to the plane of the first layer. is weak and has a relatively wide space between the nine layers.
このため適当な条件下でａ！、アルカリ金属、ハロゲン
等が容易に黒鉛層間に挿入され黒鉛層間化合物となる。Therefore, under appropriate conditions, a! , alkali metals, halogens, etc. are easily inserted between graphite layers to form a graphite intercalation compound.
この黒鉛層間化合物を適当な温度に加熱すると化合物は
瞬間的に分解し、侵入化学種は蒸気となって散逸し、黒
鉛は結晶のＣ軸方向く１０〜４００倍に膨張する。この
膨張黒鉛を原料として、単独に、または適当な結合材と
ともに圧縮、成形すると可撓性に富んだ黒鉛のシート、
テープ等が得られ、各種ガスケット、パツキン等に幅広
く利用されている。また黒鉛層間化合物単独においても
侵入化学種およびそれの黒鉛層間への挿入量を調整する
ことによシ導電性材料、電池部材、気体吸蔵分離材料と
して幅広い応用が期待されている。When this graphite intercalation compound is heated to an appropriate temperature, the compound decomposes instantaneously, the invading chemical species become vapor and dissipate, and the graphite expands 10 to 400 times in the C-axis direction of the crystal. When this expanded graphite is used as a raw material and compressed and molded alone or with a suitable binder, it becomes a highly flexible graphite sheet.
Tapes are obtained and are widely used in various gaskets, packings, etc. In addition, graphite intercalation compounds alone are expected to have a wide range of applications as conductive materials, battery components, and gas storage and separation materials by adjusting the invading chemical species and the amount of them inserted between graphite layers.
黒鉛層間化合物を形成させるための反応剤としては濃硫
酸と硝酸、塩素酸カリウム、過マンガン酸カリウム、ク
ロム酸カリウムなど濃硫酸と強酸化剤の多くの組み合わ
せが知られている。Many combinations of concentrated sulfuric acid and strong oxidizing agents are known as reactants for forming graphite intercalation compounds, such as concentrated sulfuric acid and nitric acid, potassium chlorate, potassium permanganate, and potassium chromate.
（発明が解決しようとする問題点）
上記中、硝酸または硝酸塩を使用する黒鉛層関化合物の
製造法においては１反応に際し濃厚なＮＯｘが発生しや
すく作業環境を悪化させるだけでなく、公害対策面にお
いても大きな問題を４！、たらす。一方塩素酸塩、過塩
素陵塩、クロム酸塩、過マンガン酸塩等ハロゲンの酸素
塩９重金属の酸化物の使用においても、腐食性がはげし
く、自然発火性や爆発性を呈するばかりでなく廃水など
く混入して公害をひき起こす危険性があり、これらの公
害防止に多大の設備と費用を要し好ましくない。(Problems to be Solved by the Invention) Among the above, in the method for producing a graphite layered compound using nitric acid or nitrate, a large amount of NOx is likely to be generated during one reaction, which not only worsens the working environment but also poses problems in terms of pollution control. There are also 4 major problems! , Tarasu. On the other hand, when using halogen oxygen salts such as chlorates, perchlorates, chromates, and permanganates, they are not only highly corrosive, spontaneously flammable, and explosive, but also waste water. There is a danger that such substances may be mixed in and cause pollution, and preventing such pollution requires a large amount of equipment and expense, which is undesirable.
上記に対し濃硫酸と過酸化水素水を使用する黒鉛を層間
化合物の製造法は、４？開昭５４−３８２９２号公報に
示されているように環境上や安全上から好ましい。しか
しこの場合過酸化水素水は鉄等の不純物の存在、過酸化
水素水の温度、硫酸−黒鉛スラリーの温度、硫酸濃度等
の影響により、過酸化水素の分解が生じやすい。黒鉛層
間化合物の生成反応の進行にはこの様な用いる酸化剤の
安定性が大きな効果を有するため、過酸化水素水を用勝
て黒鉛層間化合物を製造する場合には、不純物の少ない
固定炭素分９８重量−以上の高純度黒鉛お船中の灰分に
より過酸化水素水の分解が促進され。In contrast to the above, the method for producing an interlayer compound of graphite using concentrated sulfuric acid and hydrogen peroxide is 4? As disclosed in Japanese Patent Application Laid-open No. 54-38292, it is preferable from the viewpoint of environment and safety. However, in this case, hydrogen peroxide tends to decompose due to the presence of impurities such as iron, the temperature of the hydrogen peroxide solution, the temperature of the sulfuric acid-graphite slurry, the sulfuric acid concentration, etc. The stability of the oxidizing agent used has a great effect on the progress of the graphite intercalation compound production reaction, so when using hydrogen peroxide to produce a graphite intercalation compound, a fixed carbon content of 98% with less impurities is recommended. The ash content in the high-purity graphite vessel, which weighs more than -, accelerates the decomposition of the hydrogen peroxide solution.
また過酸化水素水は硫酸濃度が高ければ高いほど安定に
作用し、低濃度の硫酸中では自ら分解する性質があるな
どの理由から安定した反応が行えずに、得られる黒鉛層
間化合物も低品質のものとなり易い。In addition, the higher the concentration of sulfuric acid in hydrogen peroxide, the more stably it acts, and in low concentration sulfuric acid, it has the property of decomposing itself, so a stable reaction cannot be carried out, and the graphite intercalation compound obtained is of low quality. It is easy to become the property of
本発明は上記の問題点を解決し安定した硫酸−過酸化水
素水による黒鉛層間化合物の製造法を提供することを目
的とする。An object of the present invention is to solve the above-mentioned problems and provide a method for producing a graphite intercalation compound using a stable sulfuric acid-hydrogen peroxide solution.
（問題点を解決するための手段）
本発明者らは、過酸化水素水の分解を抑制し黒鉛層間化
合物を安定化させるための安定化剤として８−ヒドロキ
シキノリンを添加することにより。(Means for Solving the Problems) The present inventors added 8-hydroxyquinoline as a stabilizer to suppress the decomposition of hydrogen peroxide and stabilize the graphite intercalation compound.
固定炭素分９８重量％以下の多少低純度の黒鉛および濃
度９７重量％以下のやや低濃度の硫酸を用いても、安定
して高品質の黒鉛層間化合物を製造しうろことを見出し
た。We have found that it is possible to stably produce a high-quality graphite intercalation compound even when using somewhat low-purity graphite with a fixed carbon content of 98% by weight or less and sulfuric acid with a slightly low concentration of 97% by weight or less.
本発明は、濃硫酸に黒鉛粉を分散させたスラリーと過酸
化水素水とを反応させて黒鉛層間化合物を製造する方法
において、あらかじめ前記スラリー又は過酸化水素水に
、過酸化水素に対して０．０１重量−以上の８−ヒドロ
キシキノリンを添加する黒鉛層間化合物の製造法に関す
る。The present invention provides a method for producing a graphite intercalation compound by reacting a slurry in which graphite powder is dispersed in concentrated sulfuric acid with a hydrogen peroxide solution. The present invention relates to a method for producing a graphite intercalation compound in which 8-hydroxyquinoline is added in an amount of .01 weight or more.
本発明に用いる黒鉛粉の黒鉛は、一般に知られている天
然鱗状黒鉛のほか、キツシ工黒鉛、熱分解黒鉛等も使用
できる。黒鉛粉の粒度は特に制限がない。As the graphite powder used in the present invention, in addition to generally known natural scale graphite, engineered graphite, pyrolytic graphite, etc. can also be used. There are no particular restrictions on the particle size of graphite powder.
過酸化水素水の濃度は１０〜４０重量％が好ましい。濃
度が小さいと層間化合物の生成量が小さくなり、大きす
ぎると爆発の危険が生ずる。The concentration of the hydrogen peroxide solution is preferably 10 to 40% by weight. If the concentration is low, the amount of intercalation compounds produced will be small; if the concentration is too high, there will be a risk of explosion.
８−ヒドロキシキノリンは市販のものを用い。A commercially available 8-hydroxyquinoline was used.
過酸化水素に対して０．０１重量−以上加える。Add at least 0.01 weight to hydrogen peroxide.
０．０１重量−未満では効果がない、黒鉛層間化合物は
、＃硫酸に黒鉛粉を加え、混合してスラリーとし九もの
に、過酸化水素水を加えることによってなされるが、８
−ヒドロキシキノリンの添加は黒鉛粉−濃硫酸スラリー
又は過酸化水素水いずれＫｍ加しても効果は大差ない。The graphite intercalation compound, which is ineffective at less than 0.01 weight, can be made by adding graphite powder to sulfuric acid, mixing to form a slurry, and adding hydrogen peroxide to the mixture.
-When adding hydroxyquinoline, there is no significant difference in the effect whether Km is added to graphite powder-concentrated sulfuric acid slurry or hydrogen peroxide solution.
またさらに反応の安定化を図るため過酸化水素水は０〜
５℃の一定温度に保持することが好ましい。In addition, in order to further stabilize the reaction, the hydrogen peroxide solution was
Preferably, the temperature is maintained at a constant temperature of 5°C.
こうして得られた反応物を適当な脱液装置、たとえばフ
ィルタープレス、遠心脱水装置などにより処理黒鉛と残
存処理液とを分離し、脱液した反応物を大量の水中に投
じて反応を停止させた後。The reaction product thus obtained was separated from the treated graphite and the remaining treatment liquid using a suitable dewatering device such as a filter press or centrifugal dewatering device, and the deliquid reactant was poured into a large amount of water to stop the reaction. rear.
水洗、脱水をく抄返して目的とする黒鉛層間化合物を得
る。The desired graphite intercalation compound is obtained by repeating the water washing and dehydration.
黒鉛層間化合物の性能を示す目安としては層間挿入量（
慢）が用いられる。The intercalation amount (
arrogance) is used.
層間挿入量の測定は水洗、脱水した後、得られた黒鉛層
間化合物に付着し念水分を１１０℃以下の温度で除去し
た重量： ｗ、 ＄ Ｗｌ測定後の試料を３５０℃で１
時間加熱し、黒鉛層間の反応物質を揮発させたあとの重
量；Ｗ鵞とから下式によ抄求められる。The amount of intercalation was measured by washing and dehydrating the graphite intercalation compound, and then removing the moisture attached to the obtained graphite intercalation compound at a temperature of 110°C or lower: w, $ Wl After measuring the sample, the sample was heated to 350°C.
The weight after heating for a period of time to volatilize the reactants between the graphite layers is calculated from the following formula.
（作用）
上記の様に濃硫酸および過酸化水素水を用いた黒鉛層間
化合物の製造法にシいて、８−ヒドロキシキノリンを添
加することＫより、過酸化水素水の分解が抑制され、黒
鉛層間化合物の形成反応が安定化するのは下記理由によ
ると考えられる。(Function) According to the method for producing a graphite intercalation compound using concentrated sulfuric acid and hydrogen peroxide solution as described above, by adding 8-hydroxyquinoline, the decomposition of hydrogen peroxide solution is suppressed and the graphite interlayer compound is produced by adding 8-hydroxyquinoline. It is thought that the reason why the compound formation reaction is stabilized is as follows.
過酸化水素水は（１）弐に示す様に水と酸素に分解され
るが、この分解は原料である黒鉛や硫酸中に含まれてい
る金属分（特に鉄分）Ｋよって促進される。しかし８−
ヒドロキシキノリンを添加することによシ金属分は８−
ヒドロキシキノリンとの錯体を形成し、不導体化される
ため過酸化水素水の分解が抑制されるのである。Hydrogen peroxide is decomposed into water and oxygen as shown in (1) 2, but this decomposition is promoted by the metal content (especially iron content) K contained in the raw materials graphite and sulfuric acid. But 8-
By adding hydroxyquinoline, the metal content is reduced to 8-
Since it forms a complex with hydroxyquinoline and becomes a passivator, the decomposition of hydrogen peroxide is suppressed.
２Ｈ＊０＊ −一づ−２ＨｓＯ＋０冨
（１）（実施例）
次に本発明の詳細な説明する。2H*0* -Izu-2HsO+0Tomi
(1) (Example) Next, the present invention will be explained in detail.
実施例１
固定炭素分９９重量％、灰分α６重量％、平均粒径４２
メツシユのマダカルカス産鱗状黒鉛粉ｌｏｏｇを濃度９
８重量−の濃硫酸８００ｇ中に浸漬混合し九硫酸−黒鉛
粉スラＩ）−に８−ヒドロキシキノリン（試薬特級）０
．３ｇを添加し１分間攪拌した。これに５℃に保持した
濃度１５重量−の過酸化水素水５０９を加え、２分間攪
拌した。Example 1 Fixed carbon content 99% by weight, ash content α6% by weight, average particle size 42
Melted scaly graphite powder from Madakalcas in Metsuyu with a concentration of 9
8-Hydroxyquinoline (special grade reagent) was mixed by immersion in 800 g of concentrated sulfuric acid, and 8-hydroxyquinoline (reagent special grade) was mixed with 9-sulfuric acid-graphite powder slurry I).
．． 3 g was added and stirred for 1 minute. To this was added hydrogen peroxide solution 509 with a concentration of 15% by weight kept at 5°C, and the mixture was stirred for 2 minutes.
攪拌＆６０分間放置した後１反応処理液を濾過して得た
固形物を水洗、脱水し黒鉛層間化合物を作成した。After stirring and leaving for 60 minutes, the solid substance obtained by filtering the first reaction treatment liquid was washed with water and dehydrated to prepare a graphite intercalation compound.
実施例２
固定炭素分９２重量％、灰分７．５重量％、平均粒径４
８メツシユのマダガスカル産鱗状黒鉛粉を用いた以外は
前記実施例１と同一手法により黒鉛層間化合物を作成し
た。Example 2 Fixed carbon content 92% by weight, ash content 7.5% by weight, average particle size 4
A graphite intercalation compound was prepared by the same method as in Example 1 except that 8 meshes of scaly graphite powder from Madagascar was used.
実施例３
実施例１の黒鉛粉を濃度９３重量％の濃硫酸８００ｇ中
に浸漬混合してスラリーとし、以下実施例１と同一手法
によシ黒鉛層間化合物を作成した。Example 3 The graphite powder of Example 1 was immersed and mixed in 800 g of concentrated sulfuric acid with a concentration of 93% by weight to form a slurry, and a graphite intercalation compound was prepared in the same manner as in Example 1.
比較例１
実施例１と同一の黒鉛粉、＊硫酸を用いて実施例１と同
様にして作成した硫酸−黒鉛粉スラリーに、５℃に保持
した濃度１５重量％の過酸化水素水５０９を加え２分間
攪拌した。以後実施例１と同一手法により黒鉛層間化合
物を作成した。Comparative Example 1 To a sulfuric acid-graphite powder slurry prepared in the same manner as in Example 1 using the same graphite powder and *sulfuric acid as in Example 1, hydrogen peroxide solution 509 with a concentration of 15% by weight kept at 5°C was added. Stir for 2 minutes. Thereafter, a graphite intercalation compound was created using the same method as in Example 1.
比較例２
８−ヒドロキシキノリンを添加しないほかは実施例２と
同一手法により黒鉛層間化合物を作成した。Comparative Example 2 A graphite intercalation compound was produced by the same method as in Example 2 except that 8-hydroxyquinoline was not added.
比較例３
８−ヒドロキシキノリンを添加しないほかは実施例３と
同一の手法により黒鉛層間化合物を作成した。Comparative Example 3 A graphite intercalation compound was produced by the same method as in Example 3 except that 8-hydroxyquinoline was not added.
実施例１，２，３．比較例１，２．３で得た黒鉛層間化
合物について層間挿入量（Ｓ）を測定した。Examples 1, 2, 3. The intercalation amount (S) of the graphite intercalation compounds obtained in Comparative Examples 1 and 2.3 was measured.
その結果を第１表に示す。The results are shown in Table 1.
以下余白
第１表
第１表から９層間挿入量は８−ヒドロキシキノリンを加
えることにより増大することが明瞭である。又実施例２
のように黒鉛の純度が多少低く。It is clear from Table 1 in Table 1 below that the amount of interlayer intercalation increases by adding 8-hydroxyquinoline. Also, Example 2
As in, the purity of graphite is somewhat low.
実施例３のよう＆ｌｌ硫酸の濃度が幾分小さいものであ
っても眉間挿入量を大きくすることができる。Even if the concentration of &ll sulfuric acid is somewhat small as in Example 3, the amount inserted between the eyebrows can be increased.
（発明の効果）
本発明によれば９反応の安定化剤として８−ヒドロキシ
キノリンを添加するので、安定剤を添加しない従来法に
比べて反応物質の残存率（層間挿入量）が高い安定した
黒鉛層間化合物が得られる。また多少純度の低い黒鉛、
濃度の小さい濃硫酸の使用も可能となる。(Effect of the invention) According to the present invention, since 8-hydroxyquinoline is added as a stabilizer for the 9 reactions, the residual rate (intercalation amount) of the reactant is higher than in the conventional method in which no stabilizer is added. A graphite intercalation compound is obtained. Also, graphite with a slightly lower purity,
It also becomes possible to use concentrated sulfuric acid with a low concentration.
Claims (1)
水とを反応させて黒鉛層間化合物を製造する方法におい
て、あらかじめ前記スラリー又は過酸化水素水に、過酸
化水素に対して０．０１重量％以上の８−ヒドロキシキ
ノリンを添加することを特徴とする黒鉛層間化合物の製
造法。1. In a method of producing a graphite intercalation compound by reacting a slurry in which graphite powder is dispersed in concentrated sulfuric acid and a hydrogen peroxide solution, a 0.01 1. A method for producing a graphite intercalation compound, which comprises adding 8-hydroxyquinoline in an amount of at least % by weight.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP61307545A JPS63159212A (en) | 1986-12-23 | 1986-12-23 | Production of interlaminar compound of graphite |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP61307545A JPS63159212A (en) | 1986-12-23 | 1986-12-23 | Production of interlaminar compound of graphite |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPS63159212A true JPS63159212A (en) | 1988-07-02 |
Family
ID=17970381
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP61307545A Pending JPS63159212A (en) | 1986-12-23 | 1986-12-23 | Production of interlaminar compound of graphite |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS63159212A (en) |
-
1986
- 1986-12-23 JP JP61307545A patent/JPS63159212A/en active Pending
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