JPH09124312A - Modification of surface of carbonaceous particle - Google Patents
Modification of surface of carbonaceous particleInfo
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- JPH09124312A JPH09124312A JP7303337A JP30333795A JPH09124312A JP H09124312 A JPH09124312 A JP H09124312A JP 7303337 A JP7303337 A JP 7303337A JP 30333795 A JP30333795 A JP 30333795A JP H09124312 A JPH09124312 A JP H09124312A
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- containing gas
- gas
- steam
- fluorine
- treatment
- Prior art date
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Abstract
Description
【０００１】[0001]
【発明の属する技術分野】本発明は、炭素質粉粒体の表
面改質法に関する。TECHNICAL FIELD The present invention relates to a method for modifying the surface of carbonaceous powder.
【０００２】[0002]
【従来の技術】炭素材料は、多孔性、導電性、電熱性、
耐食性、耐熱衝撃性等種々の点で優れた特性を有する。
通常の標準的な一般炭素材はピッチコークス、カーボン
ブラック、黒鉛等の炭素質粉粒体をピッチ、樹脂等のバ
インダーと混合し、これを所定の形状に成形したのち、
熱処理によって炭素質（黒鉛を含む）製品とされる。こ
れらの製品を得る場合、炭素質粉粒体のバインダーとの
親和性が重要である。また、カーボンブラック等を水、
有機溶剤等の分散媒に分散させて用いるインキ等におい
ても、均一分散させるためにこれらの分散媒との親和性
（濡れ性）が重要となる。そこで、表面の濡れ性が十分
でない炭素質粉粒体の濡れ性向上のために該粉粒体を化
学的に処理して官能基を導入する方法などが検討されて
いる。2. Description of the Related Art Carbon materials are porous, conductive, electrothermal,
It has excellent properties such as corrosion resistance and thermal shock resistance.
Ordinary standard general carbon material is pitch coke, carbon black, carbonaceous powder particles such as graphite are mixed with a binder such as pitch, resin, etc., and this is molded into a predetermined shape,
Heat treatment produces carbonaceous (including graphite) products. When obtaining these products, the affinity of the carbonaceous powder for the binder is important. In addition, carbon black etc.
Even in an ink or the like that is used by dispersing it in a dispersion medium such as an organic solvent, the affinity (wettability) with these dispersion media is important for uniform dispersion. Therefore, in order to improve the wettability of the carbonaceous powders whose surface wettability is not sufficient, a method of chemically treating the powdery granules to introduce a functional group has been studied.
【０００３】たとえば、化学処理としては酸化処理が通
常用いられており、表面に水酸基、カルボニル基、カル
ボキシル基が形成される他に、表面の緻密層が除去され
る、表面積が大きくなる、表面に凹凸が生じるなどの変
化によって濡れ性の向上、接着性の改良に効果を表す。
また、そのほかの化学的手法の１つとしてフッ素ガスを
用いて炭素材とマトリクスとの親和性を増す方法が報告
されている（特開昭６０−１９１０１１号公報参照のこ
と。）For example, an oxidation treatment is usually used as a chemical treatment, and in addition to the formation of hydroxyl groups, carbonyl groups, and carboxyl groups on the surface, the dense layer on the surface is removed, the surface area is increased, and the surface is increased. It is effective in improving wettability and adhesiveness due to changes such as unevenness.
Also, as one of the other chemical methods, a method of increasing the affinity between the carbon material and the matrix by using fluorine gas has been reported (see Japanese Patent Laid-Open No. 60-191011).
【０００４】[0004]
【発明が解決しようとする課題】上記酸化処理において
は、表面処理の程度を強くしても活性点の量は処理の程
度に比例して増加するわけでなく、また表面の粗化は欠
陥の導入に他ならず、より一層の濡れ性の改善が求めら
れている。また、電池活物質として、あるいは固体潤滑
剤として、更に溌水溌油剤としてのフッ化炭素の精製法
として、炭素質物質とフッ素とを反応させて製造された
フッ化炭素を、塩化水素ガス、二酸化イオウガス、二酸
化チッ素ガス、水蒸気またはこれらの混合ガスで接触処
理する方法が提案されている（特開平２−２２１１４号
公報参照のこと。）。しかし、これはあくまで炭素質物
質をフッ素ガスと反応させて得たフッ化炭素中に存在す
る炭素と結合していないフッ素量の調節を目的とするフ
ッ化炭素の精製法に関するものである。In the above oxidation treatment, even if the degree of surface treatment is increased, the amount of active sites does not increase in proportion to the degree of treatment, and surface roughening causes defects. It is nothing but introduction, and further improvement in wettability is required. Further, as a battery active material, or as a solid lubricant, further as a method for purifying fluorocarbon as a water repellent, a fluorocarbon produced by reacting a carbonaceous substance with fluorine, hydrogen chloride gas, A method of contact treatment with sulfur dioxide gas, nitrogen dioxide gas, steam or a mixed gas thereof has been proposed (see Japanese Patent Laid-Open No. 22114/1990). However, this relates only to a method for purifying fluorocarbon for the purpose of adjusting the amount of fluorine that is not bound to carbon existing in fluorocarbon obtained by reacting a carbonaceous substance with fluorine gas.
【０００５】[0005]
【課題を解決するための手段】本発明者らは炭素質粉粒
体の水、有機溶剤等の分散媒への分散性を向上させる目
的で、種々検討を行い、炭素質粉粒体をフッ素含有ガス
で処理した後、水蒸気を含有したガスで処理することに
より、フッ素含有ガスで処理したものに比較して著しく
濡れ性が向上することを見いだし、本発明を完成するに
至った。すなわち、本発明は、炭素質粉粒体の表面をフ
ッ素化処理した後、水蒸気含有ガスで処理することを特
徴とする炭素質粉粒体の表面改質方法を要旨とする。以
下本発明を詳細に説明する。まず、本発明において用い
られる炭素質粉粒体としては特に制限されず、カーボン
ブラック、ピッチコークス、黒鉛等の粉粒体が挙げら
れ、粒径は使用目的に応じ粗粒〜微粒から選定される。Means for Solving the Problems The present inventors have conducted various studies to improve the dispersibility of carbonaceous powders in a dispersion medium such as water or an organic solvent, and have made carbonaceous powders into fluorine. It has been found that the wettability is remarkably improved by treating with a gas containing water and then with a gas containing water vapor, and the present invention has been completed. That is, the gist of the present invention is a method for modifying the surface of a carbonaceous powder which is characterized in that the surface of the carbonaceous powder is fluorinated and then treated with a steam-containing gas. Hereinafter, the present invention will be described in detail. First, the carbonaceous powder used in the present invention is not particularly limited, and examples thereof include powders such as carbon black, pitch coke, and graphite, and the particle size is selected from coarse particles to fine particles according to the purpose of use. .
【０００６】本発明におけるフッ素化処理は、フッ素ガ
ス単独、もしくはフッ素ガスと窒素、アルゴン、ヘリウ
ム等の不活性ガス及び／または酸素、空気等の酸素含有
ガスとの混合ガスを該炭素質粉粒体に、０〜５０℃の温
度、好ましくは０〜３０℃で数秒〜１時間好ましくは数
秒〜３０分程度接触反応させることによって行われる。
それぞれのガスの混合割合は分圧として、フッ素ガス１
〜１００ｍｍＨｇ、好ましくは３〜５０ｍｍＨｇ、酸素
含有ガスを酸素として１〜７５０ｍｍＨｇ、好ましくは
３０〜７１０ｍｍＨｇ、不活性ガス９〜７５９ｍｍＨ
ｇ、好ましくは４５〜４５０ｍｍＨｇの範囲が採用され
る。反応圧力は通常は常圧で行われるが数ｍｍＨｇ〜２
ｋｇ／ｃｍ2 の範囲ならいずれの圧力でもかまわない。
反応装置は特に炭素質粉粒体と反応ガスとの接触が良好
ならいずれの装置でもかまわないが、通常は回転ないし
揺動しながら反応できる装置が好ましい。また、反応系
は密閉系もしくは流通系いずれでも採用できる。次いで
行われる水蒸気含有ガスでの処理は、上記の方法で処理
された炭素質粉粒体に対して行われる。水蒸気含有ガス
の組成は、飽和水蒸気として１〜６０容量％、好ましく
は１０〜４０容量％を含む空気及び／または不活性ガス
である。水蒸気含有ガスの流量は５０〜１０００ｍｌ／
分、好ましくは２００〜８００ｍｌ／分で、温度は１５
０〜３５０℃、好ましくは２００〜３００℃で、処理時
間は数分〜数十時間、好ましくは１〜１０時間で水蒸気
含有ガスによる処理が行われる。処理装置は水蒸気含有
ガスと炭素質粉粒体との接触が良好ならどんなものでも
かまわないが、好ましくはフッ素化処理に用いた装置で
フッ素化処理に引き続いて行われる。一般的に、親水性
はイオン結合性フッ素が多い程、また全酸性基が多い程
高いと云われている。しかるに本発明での水蒸気含有ガ
スで処理することによって、それらはいずれもフッ素処
理品に比べて低くなっているにも拘らず親水性は高くな
っている。この理由は明かでないがフッ素が離脱した活
性点に何らかの含酸素官能基が付加されたものと考えら
れる。全酸性基が相対的に減少しているのは全酸性基と
してカウントされるフッ素の量が顕著に低くなっている
ためと考えられる。本発明により表面改質された炭素質
粉粒体は分散媒、バインダー等のマトリクスとの濡れ性
が向上し、たとえば強度の向上した炭素質成形体、分散
性の良好なインキ類等を得ることができる。In the fluorination treatment in the present invention, the carbonaceous powder particles are prepared by using fluorine gas alone or a mixed gas of fluorine gas and an inert gas such as nitrogen, argon and helium and / or an oxygen-containing gas such as oxygen and air. It is carried out by subjecting the body to a catalytic reaction at a temperature of 0 to 50 ° C., preferably 0 to 30 ° C. for a few seconds to 1 hour, preferably a few seconds to 30 minutes.
The mixing ratio of each gas is a partial pressure of fluorine gas 1
-100 mmHg, preferably 3-50 mmHg, oxygen-containing gas as oxygen, 1-750 mmHg, preferably 30-710 mmHg, inert gas 9-759 mmHg
g, preferably in the range of 45 to 450 mmHg. The reaction pressure is usually atmospheric pressure, but several mmHg to 2
Any pressure may be used within the range of kg / cm 2 .
Any reaction device may be used as long as the contact between the carbonaceous powder and the reaction gas is good, but a device that can react while rotating or rocking is usually preferable. The reaction system may be either a closed system or a distribution system. The subsequent treatment with the steam-containing gas is performed on the carbonaceous powder and granules treated by the above method. The composition of the steam-containing gas is air and / or an inert gas containing 1 to 60% by volume, preferably 10 to 40% by volume as saturated steam. Flow rate of water vapor containing gas is 50 ~ 1000ml /
Min, preferably 200-800 ml / min, temperature 15
The treatment with the steam-containing gas is carried out at 0 to 350 ° C., preferably 200 to 300 ° C., and the treatment time is several minutes to several tens hours, preferably 1 to 10 hours. The treatment apparatus may be any apparatus as long as the contact between the steam-containing gas and the carbonaceous powder is good, but the apparatus used for the fluorination treatment is preferably used subsequent to the fluorination treatment. In general, it is said that the hydrophilicity is higher as the amount of ion-bonding fluorine is larger and the total amount of acidic groups is larger. However, by treating with the steam-containing gas according to the present invention, the hydrophilicity of each of them is higher, although they are lower than those of the fluorine-treated product. The reason for this is not clear, but it is considered that some kind of oxygen-containing functional group is added to the active site from which fluorine is released. It is considered that the relative decrease in the total acidic groups is due to the significantly low amount of fluorine counted as total acidic groups. The surface-modified carbonaceous powder according to the present invention has improved wettability with a dispersion medium, a matrix such as a binder, and for example, a carbonaceous compact having improved strength, and inks having good dispersibility can be obtained. You can
【０００７】[0007]
【発明の実施の形態】本発明は、炭素質粉粒体の表面
に、先ずフッ素化処理、次いで水蒸気含有ガス処理を施
すものであるが、本発明の目的が、分散媒、バインダー
等のマトリクスとの濡れ性が向上し、たとえば強度の向
上した炭素質成形体、分散性の良好なインキの製造に適
した表面改質された炭素質粉粒体を得ることにあるの
で、この目的達成に有効な範囲内の様々な実施の形態が
採用される。BEST MODE FOR CARRYING OUT THE INVENTION In the present invention, the surface of a carbonaceous powder is first subjected to a fluorination treatment and then a steam-containing gas treatment. The purpose of the present invention is to provide a matrix such as a dispersion medium and a binder. In order to achieve this object, it is to obtain a carbonaceous molding having improved wettability with, for example, a carbonaceous molding having improved strength and a surface-modified carbonaceous powder suitable for producing an ink having good dispersibility. Various embodiments within the effective range are adopted.
【０００８】本発明の方法が適用される炭素質粉粒体と
しては、使用目的に応じ、種類としてはカーボンブラッ
ク、ピッチコークス、黒鉛等種々のものが挙げられ、粒
径も粗粒から微粒まで様々なものが挙げられる。フッ素
化処理は、フッ素ガス単独、もしくはフッ素ガスと不活
性ガス及び／または酸素含有ガスとの混合ガスを炭素質
粉粒体表面に接触反応させることにより施されるが、接
触反応の条件は０〜５０℃の温度、数秒〜１時間の範囲
で任意選定される。それぞれのガスの混合割合は分圧と
して、フッ素ガス１〜１００ｍｍＨｇ、酸素含有ガスを
酸素として１〜７５０ｍｍＨｇ、不活性ガス９〜７５９
ｍｍＨｇの範囲から採用される。反応圧力は通常は常圧
で行われるが、数ｍｍＨｇ〜２ｋｇ／ｃｍ2 の範囲内な
らばいずれの圧力でも差し支えない。反応装置は回転な
いし揺動形式が好ましく、反応系は、密閉系もしくは流
動系いずれも採用できる。水蒸気含有ガスでの処理は、
飽和水蒸気として１〜６０容量％を含む空気及び／また
は不活性ガスを、水蒸気含有ガスの流量５０〜１０００
ｍｌ／分で、温度１５０〜３５０℃で、数分〜数十時間
接触反応させることにより行われる。処理装置は、炭素
質粉粒体と水蒸気含有ガスとの接触が良好に行われるの
であればいずれの装置も採用されるが、フッ素化処理に
用いた装置でフッ素化処理に引き続いて行うのが好まし
い。The carbonaceous powder to which the method of the present invention is applied includes various types such as carbon black, pitch coke, and graphite according to the purpose of use, and the particle size ranges from coarse particles to fine particles. There are various things. The fluorination treatment is carried out by reacting fluorine gas alone or a mixed gas of fluorine gas and an inert gas and / or an oxygen-containing gas with the surface of the carbonaceous powder particles, but the contact reaction condition is 0. It is arbitrarily selected at a temperature of -50 ° C and a range of several seconds to one hour. The mixing ratio of each gas is 1 to 100 mmHg of fluorine gas, 1 to 750 mmHg of oxygen containing gas as oxygen, and 9 to 759 of inert gas.
It is adopted from the range of mmHg. The reaction pressure is usually atmospheric pressure, but any pressure may be used as long as it is within a range of several mmHg to 2 kg / cm 2 . The reactor is preferably a rotating or rocking type, and the reaction system may be either a closed system or a fluid system. Treatment with water vapor containing gas,
Air and / or an inert gas containing 1 to 60% by volume as saturated steam is used, and the flow rate of the steam-containing gas is 50 to 1000.
The reaction is carried out at a temperature of 150 to 350 ° C. for several minutes to several tens of hours at ml / min. As the treatment device, any device can be adopted as long as good contact between the carbonaceous powder and the water vapor-containing gas is performed, but it is possible to use the device used for the fluorination treatment after the fluorination treatment. preferable.
【０００９】[0009]
【実施例】以下、実施例により本発明を詳細に説明する
が、本発明の要旨を越えない限りこれら実施例に限定さ
れるものではない。 実施例１ 表−１に示すカーボンブラック（三菱化学社製 ＭＡ１
００、粒子径２２ｎｍ）を、フッ素化処理用反応器内に
入れ、容器内を真空に保った後フッ素ガスを導入し、室
温でフッ素圧５ｍｍＨｇ、酸素圧５０ｍｍＨｇ、窒素圧
７０５ｍｍＨｇ、５分間の条件でフッ素化処理した。こ
のものを温度２５０℃で、飽和水蒸気２５容量％を含ん
だ空気６００ｍｌ／分を流しながら２時間処理した。得
られた改質カーボンブラックの水に対する濡れ性の尺度
として簡易親水性および浸漬熱を測定した。EXAMPLES The present invention will be described in detail below with reference to examples, but the present invention is not limited to these examples as long as the gist of the present invention is not exceeded. Example 1 Carbon black shown in Table 1 (MA1 manufactured by Mitsubishi Chemical Corporation)
00, particle diameter 22 nm) was placed in a reactor for fluorination treatment, fluorine gas was introduced after keeping the inside of the container under vacuum, and fluorine pressure was 5 mmHg, oxygen pressure was 50 mmHg, and nitrogen pressure was 705 mmHg at room temperature for 5 minutes. Was fluorinated. This was treated at a temperature of 250 ° C. for 2 hours while flowing 600 ml / min of air containing 25% by volume of saturated steam. Simple hydrophilicity and immersion heat were measured as a measure of the wettability of the obtained modified carbon black with water.
【００１０】〔簡易親水性の測定法〕室温でビーカーに
水３０ｍｌを入れ、その上に約３０ｍｇのサンプルを落
として水に沈む時間の違いによって親水性のランクづけ
を行った。ランクづけは次の通りであり、水に沈む時間
が速い方が親水性が高いことを示す。 Ｓ；１５秒以内、Ａ；１５〜３０秒、Ａ′；３０〜４５
秒、Ｂ；４５〜６０秒、Ｂ′；６０〜７５秒、Ｃ；７５
〜９０秒、Ｃ′；９０秒以上（落ちない） 〔浸漬熱の測定法〕浸漬熱は、東京理工（株）社製、双
子型カロリメーターを用い、水に対する浸漬熱を文献
（セラミックス第１１巻（１９７６）Ｎｏ．５，ＰＰ．
４３３−４４０）に従って測定した。[Simple hydrophilicity measuring method] 30 ml of water was placed in a beaker at room temperature, about 30 mg of a sample was dropped on the beaker, and the hydrophilicity was ranked according to the difference in the time of immersion in water. The ranking is as follows, and the faster the time to sink in water is, the higher the hydrophilicity is. S: Within 15 seconds, A: 15 to 30 seconds, A ': 30 to 45
Seconds, B; 45-60 seconds, B '; 60-75 seconds, C; 75
~ 90 seconds, C '; 90 seconds or more (does not fall) [Measuring method of immersion heat] For immersion heat, use a twin calorimeter manufactured by Tokyo Riko Co., Ltd. Volume (1976) No. 5, PP.
433-440).
【００１１】〔サンプルの前処理〕カーボンブラックを
０．３ｇ精秤し、これをガラスアンプルに取り、１０-5
ｔｏｒｒの真空下１５０℃で３時間加熱脱気処理後その
まま封管した。 〔測定〕上記アンプルを２０ｃｃの水が入った容器に入
れ、これを双子型カロリメーター内にセットする。恒温
槽内の温度が一定（２５℃）になってから、ガラスアン
プルを破壊して、水とカーボンブラックを接触させ、こ
の時発生する熱量を検出した。ガラスアンプルの破壊熱
は参照側の空アンプルの破壊熱を差し引くことによって
校正した。測定された値は１１８ｅｒｇ／ｃｍ2 であ
り、原料カーボンブラックの値８２ｅｒｇ／ｃｍ2 と比
較して大きな値を示した。結果を表−２に示した。ま
た、簡易親水性を測定したところランクＳであった。以
上の結果を表−２に示した。[Pretreatment of sample] 0.3 g of carbon black was precisely weighed and placed in a glass ampoule to obtain 10 -5.
After heating and degassing at 150 ° C. for 3 hours under a vacuum of torr, the tube was sealed as it was. [Measurement] The above ampoule is placed in a container containing 20 cc of water and set in a twin calorimeter. After the temperature in the constant temperature bath became constant (25 ° C.), the glass ampoule was broken to bring water into contact with carbon black, and the amount of heat generated at this time was detected. The heat of destruction of the glass ampoule was calibrated by subtracting the heat of destruction of the empty ampoule on the reference side. The measured value was 118 erg / cm 2 , which was a large value as compared with the value of the raw carbon black of 82 erg / cm 2 . The results are shown in Table-2. Further, the simple hydrophilicity was measured and found to be rank S. The above results are shown in Table 2.
【００１２】実施例２ 実施例１と同様にしてフッ素化処理したものを、温度２
００℃で、飽和水蒸気２５容量％を含んだ空気６００ｍ
ｌ／分を流しながら８時間処理した。得られた改質カー
ボンブラックの水に対する濡れ性の尺度として簡易親水
性を測定した。簡易親水性の結果はランクＳであった。
結果を表−２に示した。 比較例１ 実施例１で用いたのと同じカーボンブラックを、実施例
１と同様の条件でフッ素化したものの簡易親水性を測定
したところランクはＡであった。結果を表−２に示し
た。Example 2 The same fluorination treatment as in Example 1 was conducted at a temperature of 2
600 m of air containing 25% by volume of saturated steam at 00 ° C
It was treated for 8 hours while flowing 1 / min. Simple hydrophilicity was measured as a measure of the wettability of the obtained modified carbon black with water. The result of the simple hydrophilicity was rank S.
The results are shown in Table-2. Comparative Example 1 The same carbon black used in Example 1 was fluorinated under the same conditions as in Example 1, and the simple hydrophilicity was measured and the rank was A. The results are shown in Table-2.
【００１３】比較例２ 実施例１と同様にしてフッ素化処理したものを、温度２
５０℃で、空気雰囲気で２時間処理した。このものの簡
易親水性を測定したところ、ランクはＢであった。結果
を表−２に示した。 比較例３ 実施例１と同様にしてフッ素化処理したものを、温度２
５０℃で空気６００ｍｌ／分流しながら２時間処理し
た。このものの簡易親水性を測定したところ、ランクは
Ａ′であった。結果を表−２に示した。Comparative Example 2 The same fluorination treatment as in Example 1 was conducted at a temperature of 2
It was treated at 50 ° C. in an air atmosphere for 2 hours. When the simple hydrophilicity of this product was measured, the rank was B. The results are shown in Table-2. Comparative Example 3 The same fluorination treatment as in Example 1 was conducted at a temperature of 2
It was treated at 50 ° C. for 2 hours while flowing 600 ml / minute of air. When the simple hydrophilicity of this product was measured, the rank was A '. The results are shown in Table-2.
【００１４】[0014]
【表１】 [Table 1]
【００１５】[0015]
【表２】 [Table 2]
【００１６】[0016]
【発明の効果】本発明方法によれば、表面の濡れ性が向
上した炭素粉粒体を得ることができる。そしてこの炭素
粉粒体を原料として強度の向上した炭素質成形体、分散
性の良好なインキ類等を得ることができる。According to the method of the present invention, it is possible to obtain carbon powder particles having improved surface wettability. Then, a carbonaceous compact having improved strength, inks having good dispersibility, and the like can be obtained by using this carbon powder as a raw material.
Claims (6)
処理を施したあと、水蒸気含有ガスで処理することを特
徴とする炭素質粉粒体の表面改質法。1. A method for modifying the surface of a carbonaceous powder, which comprises subjecting the surface of the carbonaceous powder to a fluorine-containing gas treatment and then a steam-containing gas treatment.
を０〜５０℃の温度で、数秒〜１時間接触させることか
ら成るフッ素含有ガス処理を施す請求項１記載の表面改
質法。2. The surface modification method according to claim 1, wherein the surface of the carbonaceous powder is treated with a fluorine-containing gas at a temperature of 0 to 50 ° C. for several seconds to 1 hour. .
くはフッ素ガスと不活性ガス及び／または酸素含有ガス
との混合ガスである請求項１または２記載の表面改質
法。3. The surface modification method according to claim 1, wherein the fluorine-containing gas is a fluorine gas alone or a mixed gas of a fluorine gas and an inert gas and / or an oxygen-containing gas.
として１〜６０容量％含有する空気及び／又は不活性ガ
スである請求項１〜３のいずれかに記載の表面改質法。4. The surface modification method according to claim 1, wherein the steam-containing gas is air and / or an inert gas containing 1 to 60% by volume of steam as saturated steam.
〜１０００ｍｌ／分の水蒸気含有ガスと、温度１５０〜
３５０℃で、数分〜数十時間接触させることにより行う
請求項１〜４のいずれかに記載の表面改質法。5. The treatment with a steam-containing gas is performed at a flow rate of 50.
~ 1000 ml / min steam-containing gas, temperature 150 ~
The surface modification method according to any one of claims 1 to 4, which is performed by contacting at 350 ° C for several minutes to several tens of hours.
を０〜３０℃の温度で、数秒〜３０分間接触させてフッ
素含有ガス処理を施したあと、水蒸気を飽和水蒸気とし
て１０〜４０容量％含有し、流量が２００〜８００ｍｌ
／分の水蒸気含有ガスと、温度２００〜３００℃で、１
時間〜１０時間接触させることを特徴とする炭素質粉粒
体の表面改質法。6. The surface of the carbonaceous powder is brought into contact with a fluorine-containing gas at a temperature of 0 to 30 ° C. for several seconds to 30 minutes to carry out a fluorine-containing gas treatment, and then steam is changed to saturated steam of 10 to 40. Volume% content, flow rate 200-800ml
/ Min with steam-containing gas at a temperature of 200 to 300 ° C.
A method for modifying the surface of a carbonaceous powder, which comprises contacting for 10 to 10 hours.
Priority Applications (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP7303337A JPH09124312A (en) | 1995-10-30 | 1995-10-30 | Modification of surface of carbonaceous particle |
| US08/739,295 US5871864A (en) | 1995-10-30 | 1996-10-29 | Lithium secondary cells and methods for preparing active materials for negative electrodes |
| US09/124,186 US6106977A (en) | 1995-10-30 | 1998-07-28 | Lithium secondary cells and methods for preparing active materials for negative electrodes |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP7303337A JPH09124312A (en) | 1995-10-30 | 1995-10-30 | Modification of surface of carbonaceous particle |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH09124312A true JPH09124312A (en) | 1997-05-13 |
Family
ID=17919765
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP7303337A Pending JPH09124312A (en) | 1995-10-30 | 1995-10-30 | Modification of surface of carbonaceous particle |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH09124312A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2009125602A (en) * | 2007-11-19 | 2009-06-11 | Daikin Ind Ltd | Granular material treatment apparatus and granular material treatment system |
| DE102007060307A1 (en) | 2007-12-12 | 2009-06-18 | Evonik Degussa Gmbh | Process for the aftertreatment of carbon black |
| US8157899B2 (en) | 2007-11-19 | 2012-04-17 | Daikin Industries, Ltd. | Particulate material processing apparatus and particulate material processing system |
| US8852739B2 (en) | 2010-02-23 | 2014-10-07 | Evonik Carbon Black Gmbh | Carbon black, method for the production thereof, and use thereof |
| US8915998B2 (en) | 2008-11-27 | 2014-12-23 | Evonik Carbon Black Gmbh | Pigment granulate, method for producing the same and use thereof |
-
1995
- 1995-10-30 JP JP7303337A patent/JPH09124312A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2009125602A (en) * | 2007-11-19 | 2009-06-11 | Daikin Ind Ltd | Granular material treatment apparatus and granular material treatment system |
| US8157899B2 (en) | 2007-11-19 | 2012-04-17 | Daikin Industries, Ltd. | Particulate material processing apparatus and particulate material processing system |
| DE102007060307A1 (en) | 2007-12-12 | 2009-06-18 | Evonik Degussa Gmbh | Process for the aftertreatment of carbon black |
| US8915998B2 (en) | 2008-11-27 | 2014-12-23 | Evonik Carbon Black Gmbh | Pigment granulate, method for producing the same and use thereof |
| US8852739B2 (en) | 2010-02-23 | 2014-10-07 | Evonik Carbon Black Gmbh | Carbon black, method for the production thereof, and use thereof |
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