JPS5812202B2 - Futsukakokuenno Seizouhou - Google Patents
Futsukakokuenno SeizouhouInfo
- Publication number
- JPS5812202B2 JPS5812202B2 JP49112253A JP11225374A JPS5812202B2 JP S5812202 B2 JPS5812202 B2 JP S5812202B2 JP 49112253 A JP49112253 A JP 49112253A JP 11225374 A JP11225374 A JP 11225374A JP S5812202 B2 JPS5812202 B2 JP S5812202B2
- Authority
- JP
- Japan
- Prior art keywords
- carbon
- reaction
- activation
- fluorine
- activated carbon
- 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.)
- Expired
Links
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- Carbon And Carbon Compounds (AREA)
Description
【発明の詳細な説明】 本発明はフツ化黒鉛の製造法に関する。[Detailed description of the invention] The present invention relates to a method for producing graphite fluoride.
従来、フツ化黒鉛の製造に用いられるカニボン原料とし
て、天然黒鉛、コークス、木炭、熱硬化性樹脂炭、カー
ボンプラックおよび活性炭等が知られている。Conventionally, natural graphite, coke, charcoal, thermosetting resin charcoal, carbon plaque, activated carbon, and the like are known as raw materials for producing graphite fluoride.
天然黒鉛を用いた場合、フッ素との反応温度は３００〜
５００℃と高《、フツ化黒鉛の収率も低い。When using natural graphite, the reaction temperature with fluorine is 300~
The temperature is as high as 500°C, and the yield of graphite fluoride is also low.
コークス、木炭等の易黒鉛化性カーボンとの反応は、原
料カーボンの特性、すなわち熱履歴、真比重、結晶子の
大きさなどに影響を受ける。The reaction with graphitizable carbon such as coke and charcoal is affected by the characteristics of the raw carbon, such as thermal history, true specific gravity, and crystallite size.
８００〜１６００℃で熱処理されたもの、或は真比重が
１９５〜２２０でしかも結晶子の大きさが１０〜７５Ｘ
のカーボン原料を用いた場合にはＣ：Ｆ＝１：１の組成
をもつフツ化黒鉛を高収率で生成するが、２８０〜４０
０℃の反応温度を必要とし、又それ以外の特性値のもの
はフッ素と十分に反応させず、不均一化反応の進行によ
ってＣ：Ｆ＝１：１のフツ化黒鉛を生成し難い。Heat treated at 800-1600℃, or true specific gravity 195-220 and crystallite size 10-75X
When using a carbon raw material of 280 to 40
A reaction temperature of 0° C. is required, and those having other characteristic values do not react sufficiently with fluorine, making it difficult to produce graphite fluoride with C:F=1:1 due to the progress of the heterogeneous reaction.
カーボンブラックや活性炭とフイ素の反応は、反応速度
が非常に速く反応抑制が困難である。The reaction between carbon black or activated carbon and fluorine is extremely fast and difficult to suppress.
活性炭に反応抑制剤を用いてフツ化カーボン（ＣＦ文）
ｎ製造の円滑化を計る方法も提案されているが、この方
法では約１５重量係のフッ素以外のハロゲンが含まれて
高純度のフツ化カーボンが得られない。Carbon fluoride using activated carbon with a reaction inhibitor (CF text)
A method has also been proposed to facilitate the production of n, but this method contains about 15% by weight of halogens other than fluorine, making it impossible to obtain high purity carbon fluoride.
熱硬化性樹脂を炭化して得られる難黒鉛化性カーバンの
場合、その水素含有量が約３．５重量係以下のものを用
いると異常反応あるいは不均一化反応等の異常現象もな
＜Ｃ：Ｆ＝１：１のフツ化黒鉛を得ることが出来るが、
これでも２５０〜４００℃の反応温度で数時間を要する
等多《の問題点がある。In the case of a non-graphitizable carbane obtained by carbonizing a thermosetting resin, if the hydrogen content is less than about 3.5% by weight, abnormal phenomena such as abnormal reactions or heterogeneous reactions will not occur <C :F=1:1 graphite fluoride can be obtained, but
Even with this, there are many problems, such as the need for several hours at a reaction temperature of 250 to 400°C.
本発明は前記のような問題点を解決するため、フツ化黒
鉛製造用カーボン原料について研究を行なった結果、各
種権化材をアンモニアガスにより活性化して得られた活
性炭を用いることにより、安全にかつ容易に非常に低温
でフッ素と反応し、大きな反応速度で高収率でＣ：Ｆ＝
１：１の組成を有し化学式（ＣＦ）ｎで表わされる純度
の高い無機高分子化合物、フツ化黒鉛を製造できること
を見いだして完成したものである。In order to solve the above-mentioned problems, the present invention was developed as a result of research on carbon raw materials for producing graphite fluoride, and by using activated carbon obtained by activating various activated materials with ammonia gas, it is possible to safely and easily reacts with fluorine at very low temperatures to form C:F= in high yields with large reaction rates.
This process was completed after discovering that it was possible to produce graphite fluoride, a highly pure inorganic polymer compound having a 1:1 composition and represented by the chemical formula (CF)n.
本発明に用いられる活性炭は木、樹脂等を炭化したもの
、或は黒鉛、石炭、コークス等をアンモニアガスにより
活硅化したものである。The activated carbon used in the present invention is carbonized wood, resin, etc., or activated silicification of graphite, coal, coke, etc. with ammonia gas.
活性炭の粒子内部に存在するミクロ孔、遷移孔、マクロ
孔といらた細孔部の構造は原料カーボンの種類、活性化
条件によって非常に影響を受ける。The structure of pores such as micropores, transition pores, and macropores that exist inside activated carbon particles is greatly influenced by the type of raw carbon and activation conditions.
本発明においては、原料カーボンとして木炭、塩化ビニ
ル樹脂炭、塩化ビニリデン樹脂炭、また活性化条件とし
てアンモニアガスで８５０〜１０００℃で１０〜５０分
間処理する方法がとくに好ましい。In the present invention, it is particularly preferable to use charcoal, vinyl chloride resin charcoal, or vinylidene chloride resin charcoal as the raw material carbon, and to use ammonia gas as the activation condition for 10 to 50 minutes at 850 to 1000°C.
また、活性化による活性化度が３０〜７５係のものが好
ましい。Moreover, those having an activation degree of 30 to 75 are preferable.
（こｋで活性化度は活性化による原料カーボンの減量率
で示される。(Here, the degree of activation is indicated by the rate of weight loss of raw material carbon due to activation.
）アンモニアガスによる活性化により得られた活性炭の
表面積は１０００〜１５００ｍ２／ｇと大きく、フッ素
との接触有効面積が大きく、しかもフッ素は活性炭の細
孔部あるいは粒子間に容易に拡散する。) The activated carbon obtained by activation with ammonia gas has a large surface area of 1000 to 1500 m2/g, and has a large effective area of contact with fluorine, and fluorine easily diffuses into the pores or between particles of the activated carbon.
さらに表面積が大きいにもか〜わらず従来の活性炭やカ
ーボンブラックにくらべ異常反応あるいは不均一化反応
もなく、また１５０〜３００℃の比較的低い温度で反応
し、Ｃ：Ｆ＝１：１のフツ化黒鉛を容易Ｋかつ安全に造
ることができる。Furthermore, despite having a large surface area, there is no abnormal reaction or non-uniform reaction compared to conventional activated carbon or carbon black, and it reacts at a relatively low temperature of 150 to 300°C, with a C:F ratio of 1:1. Graphite fluoride can be produced easily and safely.
以下に本発明の実施例について述べる。Examples of the present invention will be described below.
実施例 １
市販のナラ木炭をアンモニアガスで９５０℃ＩＯ〜５０
分間賦活して、活性化度が１７係、３６係、７１係の活
性炭を得た。Example 1 Commercially available oak charcoal was heated to 950°C IO to 50°C with ammonia gas.
After activation for minutes, activated carbons with activation degrees of 17, 36, and 71 were obtained.
このようにして得た活性炭を粉砕し、１５０メッシュ（
ＪＩＳ）下に篩別してフッ素化試験用試料とした。The activated carbon thus obtained was crushed to 150 mesh (
JIS) was sieved to prepare a sample for fluorination test.
試料、０．２ｇをニッケル製反応器に入れ、外部より加
熱しつつ反応器内をアルゴンで置換し、各所定温度でフ
ッ素分圧１／３ａｔｍ（全反１ａｔｍ）のフッ素一窒素
混合ガスを送入（１５０ｍｌ／ｍｉｎ）Ｌて、１０分間
反応を行なわせて反応後の重量変化を求めた。0.2 g of the sample was placed in a nickel reactor, the inside of the reactor was replaced with argon while being heated from the outside, and a fluorine-nitrogen mixed gas with a fluorine partial pressure of 1/3 atm (1 atm total) was sent at each predetermined temperature. (150 ml/min), the reaction was carried out for 10 minutes, and the weight change after the reaction was determined.
その結果は第１図に示すとおりで、活性化度が３６係以
上の試料は１５０〜２５０℃の範囲で容易にＣ：Ｆ＝１
：１のフツ化黒鉛を得た。The results are shown in Figure 1. Samples with an activation degree of 36 coefficients or higher can be easily converted to C:F=1 in the range of 150 to 250°C.
:1 fluorinated graphite was obtained.
実施例 ２
ポリ塩化ビニル粉末を熱硫酸で１５０〜１６０℃５０時
間処理後、次いで窒素ガス雰囲気中で９００℃、２時間
加熱して得た樹脂炭をアンモニアガスで９５０℃、１０
〜５０分間賦活して、活性化度が１２係、３２係、７２
係の活性炭を得て、これをフッ素化試験用試料とした。Example 2 Polyvinyl chloride powder was treated with hot sulfuric acid at 150 to 160°C for 50 hours, and then resin charcoal obtained by heating at 900°C for 2 hours in a nitrogen gas atmosphere was treated with ammonia gas at 950°C for 10 hours.
Activation for ~50 minutes, activation level is 12, 32, 72
Activated carbon was obtained and used as a sample for fluorination test.
以下実施例１と同様にしてフッ素化反応を行なった。Thereafter, a fluorination reaction was carried out in the same manner as in Example 1.
結果は第２図に示すとおりで、活性化度が３２係以上の
試料は１５０〜３００℃の範囲で容易にＣ：Ｆ＝１：１
のフツ化黒鉛を得た。The results are shown in Figure 2. Samples with an activation degree of 32 or higher can easily have a C:F ratio of 1:1 in the range of 150 to 300°C.
fluorinated graphite was obtained.
上記実施例においては不均一化反応も起らず容易にフツ
化黒鉛を生成させることができた。In the above examples, fluorinated graphite could be easily produced without causing a heterogeneous reaction.
第１図は実施例１、また第２図は実施例２による反応結
果（フッ素化温度一試料の重量増加率）を示すグラフで
ある。FIG. 1 is a graph showing reaction results (fluorination temperature vs. weight increase rate of sample) in Example 1 and FIG. 2 in Example 2.
Claims (1)
製造法において、前記カーボン原料として、アンモニア
ガス雰囲気下８５０〜１０００℃で１０〜５０分間活性
化して得られた活性化度３０〜７５係の活性炭を１５０
〜３００℃でフッ素と反応させることを特徴とする前記
製造法。1. In a method for producing graphite fluoride in which a carbon raw material and fluorine are reacted, the carbon raw material is activated carbon with an activation degree of 30 to 75 obtained by activation at 850 to 1000°C for 10 to 50 minutes in an ammonia gas atmosphere. 150
The above production method, characterized in that the reaction is carried out with fluorine at ~300°C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP49112253A JPS5812202B2 (en) | 1974-10-01 | 1974-10-01 | Futsukakokuenno Seizouhou |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP49112253A JPS5812202B2 (en) | 1974-10-01 | 1974-10-01 | Futsukakokuenno Seizouhou |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS5139597A JPS5139597A (en) | 1976-04-02 |
| JPS5812202B2 true JPS5812202B2 (en) | 1983-03-07 |
Family
ID=14582066
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP49112253A Expired JPS5812202B2 (en) | 1974-10-01 | 1974-10-01 | Futsukakokuenno Seizouhou |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS5812202B2 (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS58176110A (en) * | 1982-04-12 | 1983-10-15 | Central Glass Co Ltd | Production of graphite fluoride |
| CN111204735B (en) * | 2020-01-16 | 2021-07-27 | 厦门稀土材料研究所 | Preparation method and application of carbon fluoride material |
-
1974
- 1974-10-01 JP JP49112253A patent/JPS5812202B2/en not_active Expired
Also Published As
| Publication number | Publication date |
|---|---|
| JPS5139597A (en) | 1976-04-02 |
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