JPS5994620A - Production of carbon fiber by vapor phase method - Google Patents
Production of carbon fiber by vapor phase methodInfo
- Publication number
- JPS5994620A JPS5994620A JP20106582A JP20106582A JPS5994620A JP S5994620 A JPS5994620 A JP S5994620A JP 20106582 A JP20106582 A JP 20106582A JP 20106582 A JP20106582 A JP 20106582A JP S5994620 A JPS5994620 A JP S5994620A
- Authority
- JP
- Japan
- Prior art keywords
- carbon fibers
- substrates
- fiber
- cylinder
- production zone
- 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
- 229920000049 Carbon (fiber) Polymers 0.000 title claims abstract description 20
- 239000004917 carbon fiber Substances 0.000 title claims abstract description 20
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 7
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims description 8
- 238000000034 method Methods 0.000 title abstract description 9
- 239000012808 vapor phase Substances 0.000 title description 4
- 239000000758 substrate Substances 0.000 claims abstract description 26
- 239000000835 fiber Substances 0.000 claims abstract description 14
- 229930195733 hydrocarbon Natural products 0.000 claims abstract description 10
- 150000002430 hydrocarbons Chemical class 0.000 claims abstract description 10
- 239000004215 Carbon black (E152) Substances 0.000 claims abstract description 7
- 230000008021 deposition Effects 0.000 claims description 2
- 238000007380 fibre production Methods 0.000 claims description 2
- 238000005979 thermal decomposition reaction Methods 0.000 claims description 2
- 239000007789 gas Substances 0.000 abstract description 21
- 239000000843 powder Substances 0.000 abstract description 9
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 abstract description 5
- 239000000919 ceramic Substances 0.000 abstract description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 3
- 238000000151 deposition Methods 0.000 abstract description 3
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 abstract description 3
- 229910052863 mullite Inorganic materials 0.000 abstract description 3
- 229910002804 graphite Inorganic materials 0.000 abstract description 2
- 239000010439 graphite Substances 0.000 abstract description 2
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 235000019441 ethanol Nutrition 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- NUMXHEUHHRTBQT-AATRIKPKSA-N 2,4-dimethoxy-1-[(e)-2-nitroethenyl]benzene Chemical compound COC1=CC=C(\C=C\[N+]([O-])=O)C(OC)=C1 NUMXHEUHHRTBQT-AATRIKPKSA-N 0.000 description 1
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 1
- 239000005977 Ethylene Substances 0.000 description 1
- 229910001111 Fine metal Inorganic materials 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 206010037660 Pyrexia Diseases 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 239000000341 volatile oil Substances 0.000 description 1
Landscapes
- Inorganic Fibers (AREA)
Abstract
Description
【発明の詳細な説明】
本発明は炭化水素の熱分解によるいわゆる気相法による
炭素繊維の製造法に関する。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for producing carbon fibers by the so-called gas phase method by thermal decomposition of hydrocarbons.
気相法による炭素繊維は優れた特性、特長をもっている
が、生産性が低いことが工業化の難点とされる。Carbon fiber produced by the vapor phase method has excellent properties and features, but low productivity is said to be a difficulty in industrialization.
従来一般に知られている気相法の炭素繊維は炉内に設置
した横型のセラミック製円筒の内面に基板を設置しＡ、
＋ガス等を流し、次いで円筒内を所定温度に上げ、ベン
ゼン等の炭化水素ガスを１−１２ガス等で希釈して流し
、炭化水素を熱分解し、基板上に炭素繊維を生成、成長
させることにより製造されている。この場合基板上に鉄
粉等の微粒子を存在させることが有効であることも知ら
れている。Conventionally known vapor phase method carbon fiber is produced by placing a substrate on the inner surface of a horizontal ceramic cylinder placed in a furnace.
+ gas etc. is flowed, then the inside of the cylinder is raised to a specified temperature, hydrocarbon gas such as benzene is diluted with 1-12 gas etc. and the hydrocarbon is pyrolyzed and carbon fibers are generated and grown on the substrate. It is manufactured by In this case, it is also known that it is effective to have fine particles such as iron powder on the substrate.
従来法では円筒内の空間が充分に利用されておらず、丑
たこの炉は炉外のガスの導入部、排出部の長さもかなり
あるので、炉を横に配置すると、建屋の高さ方向の空間
の利用効率が低くなる。In the conventional method, the space inside the cylinder is not fully utilized, and the Ushitako furnace has a considerable length of the gas introduction and exhaust sections outside the furnace, so if the furnace is placed horizontally, space usage efficiency becomes low.
そこで本発明者は先ず円筒を縦型にすることを検討した
。縦型力ら建屋の空間利用率が高凍るばかりでなく、炭
素繊維の析出基板の交換を円筒に接触させずに行なうこ
とができ、操作上も好ましい。Therefore, the inventor first considered making the cylinder vertical. The vertical structure not only improves the space utilization rate of the building, but also allows the carbon fiber deposition substrate to be replaced without contacting the cylinder, which is favorable in terms of operation.
ところが単純に横型を縦型にしただけでは炭素繊維は初
めに生成はするが、その後の成長が阻害されて繊維の収
量が少ない。それは繊維が成長の過程でガスの大きな流
速によって折れたり曲ったすすることが原因であること
がわかった。ガスの流速が大きいのは対流によるためで
あり、供給するガスの量のコントロールではガス流速を
小さくすることはむずかしい。However, if carbon fibers are simply changed from horizontal to vertical, carbon fibers are initially produced, but subsequent growth is inhibited, resulting in a low fiber yield. It was found that this was caused by the fibers being bent or bent due to the large gas flow rate during the growth process. The high gas flow rate is due to convection, and it is difficult to reduce the gas flow rate by controlling the amount of gas supplied.
内径１０ｃＴ１１程度の横型炉の場合、炉内に多少の温
度差が生じても対流によるトラブルは事実上発生しない
。横型でも炉が犬きくなると対流、偏流の問題が生じる
が、縦型に比べると少ない。In the case of a horizontal furnace with an inner diameter of about 10 cT11, troubles due to convection will virtually never occur even if a slight temperature difference occurs within the furnace. Even if the furnace is horizontal, problems with convection and drift will occur if the furnace gets too loud, but these are less common than with vertical furnaces.
本発明の目的は気相法の炭素繊維の生長速度の増大及び
空間利用率の増加により生産性の向上を図ることにある
。An object of the present invention is to improve productivity by increasing the growth rate of carbon fibers using the vapor phase method and increasing the space utilization rate.
このため本発明においては炭化水素が熱分解する空間帯
域に複数の基板をできるだけ等間隔に分散配列させる構
成とした。Therefore, in the present invention, a plurality of substrates are arranged in a distributed manner as evenly spaced as possible in a spatial zone where hydrocarbons are thermally decomposed.
以下図面に例示した装置により本発明を具体的に説明す
る。The present invention will be specifically explained below using the apparatus illustrated in the drawings.
第１図は縦に配置した円筒１内に板状の繊維析出基体２
を配列した状態を示す斜視図である。第２図は基体３と
して棒状のものを配列した状態の斜視図である。Figure 1 shows a plate-shaped fiber precipitation base 2 inside a vertically arranged cylinder 1.
FIG. 3 is a perspective view showing a state in which the FIG. 2 is a perspective view of the base body 3 in which rod-shaped objects are arranged.
円筒】はアルミナ等のセラミック製、基体２はアルミナ
、ムライト、黒鉛質等のセラミック製のものが適する。The cylinder] is preferably made of ceramic such as alumina, and the base 2 is suitably made of ceramic such as alumina, mullite, or graphite.
基体２の数は円筒の太さによって定めるが、その間隔で
、が０５〜２ｃｍに々るようにその数を決めるのがよい
。The number of base bodies 2 is determined by the thickness of the cylinder, and it is preferable to determine the number so that the distance between them is 0.5 to 2 cm.
基体は第２図に示すように棒状体３のものでもよい。こ
の場合は棒状体同志の間隔１２、棒状体と円筒内面との
間隔１３が上記の範囲に入るように選ぶことが好ましい
。４はＦｅ粉等の微粉末である。The base body may be a rod-shaped body 3 as shown in FIG. In this case, it is preferable that the spacing 12 between the rod-like bodies and the spacing 13 between the rod-like bodies and the inner surface of the cylinder fall within the above ranges. 4 is a fine powder such as Fe powder.
このように複数の基体を配列することによシ、ガスの対
流は相当防止される。そしてさらに望ましくは円筒の長
さ方向に対する直角断面の最高温度帯域における温度差
が小さいことである。実験によればこの温度差が２０°
Ｃ以下が特によい。これらの条件が満足されると対流に
よるガス流速は１ｃｍ ／ ｓｅａ以下になる。By arranging a plurality of substrates in this manner, gas convection is considerably prevented. More preferably, the temperature difference in the highest temperature zone of the cross section perpendicular to the longitudinal direction of the cylinder is small. According to experiments, this temperature difference is 20°
C or lower is particularly good. When these conditions are satisfied, the gas flow rate due to convection will be 1 cm/sea or less.
基体の表面に公知の方法（特開昭５２−１０３５２８）
に従って金属微粉等を散布する。金属は周期率表の第８
族、ｉｓａ族のもので３００Å以下の超微粉が望ましい
。壕だこれらは化合物であってもよい。A known method (Japanese Unexamined Patent Publication No. 103528/1983) on the surface of the substrate
Spread fine metal powder, etc. according to the following. Metals are number 8 on the periodic table.
Ultrafine powder of 300 Å or less in the isa group is desirable. These may be compounds.
これらの超微粉はアルコール等に分散し、基体にスプレ
ーし、乾燥して使用するが、超微粉であるため、基体が
垂直でも殆んど落下することがない。These ultrafine powders are used by dispersing them in alcohol or the like, spraying them onto a substrate, and drying them, but since they are ultrafine powders, they almost never fall even when the substrate is vertical.
基体を配列した炭素繊維の生成帯域の温度は約１０００
〜１３００°Ｃが適する。炭化水素ガスはＨ２ガス、Ａ
ｒガス等で希釈して用いるが、炭化水素ガスの濃度や混
合ガスの供給速度等は特開昭５２−１０３５２８と同様
である。！、だガスの圧力は常圧附近が取扱い易く望ま
しい。The temperature of the carbon fiber production zone where the substrate is arranged is about 1000℃.
~1300°C is suitable. Hydrocarbon gas is H2 gas, A
Although it is used after being diluted with r gas, etc., the concentration of hydrocarbon gas, the supply rate of mixed gas, etc. are the same as in JP-A-52-103528. ! It is preferable that the pressure of the gas be around normal pressure for ease of handling.
ガスの流す方向は上から下へ又はその逆のどちらでも可
能である。炭化水素としてはベンゼンの外、トルエン、
メタン、エチレン、揮発油等が使用できる。The direction of gas flow can be from top to bottom or vice versa. In addition to benzene, toluene,
Methane, ethylene, volatile oil, etc. can be used.
図示のものは円筒を縦に配置したものであるが、勿論横
型にしても本発明は可能である。Although the cylinder shown in the figure is vertically arranged, the present invention is of course possible even if the cylinder is horizontally arranged.
本発明によれば、繊維の成長速度約０．５ｃｍ１分以」
二で、炭化水素中の炭素の繊維化収率３０％以上と高能
率で炭素繊維を得ることができる。According to the present invention, the fiber growth rate is about 0.5 cm per minute or more.
Second, carbon fibers can be obtained with high efficiency, with a fiberization yield of carbon in hydrocarbons of 30% or more.
実施例
第１図に示すようにアルミナ製円筒（内径１０ｃｍ ）
内にムライト質基板を５枚配置した。基板間の間隔は１
ｃＩｒＬである。また基板の高さは３０ｃｍとした。Example As shown in Figure 1, an alumina cylinder (inner diameter 10 cm)
Five mullite substrates were placed inside. The distance between the boards is 1
cIrL. Further, the height of the substrate was 30 cm.
基板と円筒内面との間隔は約２ｃｍである。The distance between the substrate and the inner surface of the cylinder was approximately 2 cm.
基板にはエチルアルコールに分散したＦｅの超微粉（約
３００人下）をスプレーし、乾燥して使用した。Ultrafine powder of Fe dispersed in ethyl alcohol (approximately 300 ml) was sprayed onto the substrate, dried, and used.
炭化水素ガスとしてはベンゼンを用い、これを２、゛
水素ガ
スで希釈（べ／ゼンの濃度４〜１０容量％）。混合ガス
の送入量は０２〜０５１／分とした２、基板部分の温度
を約１１００°Ｃとし、また基板間の温度差は最も太き
いところで２’Ｃとした。Benzene is used as the hydrocarbon gas, and it is
Dilute with hydrogen gas (concentration of be/zene 4-10% by volume). The feeding rate of the mixed gas was 02 to 051/min2, the temperature of the substrate portion was approximately 1100°C, and the temperature difference between the substrates was 2'C at the widest point.
以上の条件で３時間継続し、炭素繊維を生成させた。The above conditions were continued for 3 hours to produce carbon fibers.
比較のため、上記基板の代りに円筒の内面に二つ割の桶
状の基板を合せて円筒内にはめ込み、基板として用い、
その他は上記と同様にして実験した。基板を二つ割とし
たのは繊維の採取を容易にするためである。For comparison, instead of the above substrate, a halved bucket-shaped substrate was placed on the inner surface of a cylinder and fitted into the cylinder, and used as a substrate.
The experiment was otherwise carried out in the same manner as above. The reason why the substrate was divided into two parts was to make it easier to collect the fibers.
結果は次の通り（太さ、長さは平均）
繊維の収量 太 さ 長 さ
本発明 １．９ １−０〜２０μ４〜５ｃ＋ｙ＋
比較例 ０１ｇ ３〜５μ １〜２ＣｍThe results are as follows (thickness and length are average) Fiber yield Thickness Length Invention 1.9 1-0~20μ4~5c+y+
Comparative example 01g 3~5μ 1~2Cm
第１図、第２図は本発明方法に使用される装置の１例を
示す断面図。
１ 円筒、 ２ 基板、 ４ ・・微粉特許出願
人 昭和電工株式会社FIGS. 1 and 2 are cross-sectional views showing one example of an apparatus used in the method of the present invention. 1 cylinder, 2 substrate, 4...Fine powder patent applicant Showa Denko K.K.
Claims (1)
、炭素繊維の生成帯域に複数の繊維析出基体を分散配列
し、ガスの対流を少なくし、繊維の成長を促進させたこ
とを特徴とする炭素繊維の製造法。A method for producing carbon fibers by thermal decomposition of hydrocarbon gas, characterized in that a plurality of fiber deposition substrates are dispersed and arranged in a carbon fiber production zone to reduce gas convection and promote fiber growth. Fiber manufacturing method.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP20106582A JPS5994620A (en) | 1982-11-18 | 1982-11-18 | Production of carbon fiber by vapor phase method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP20106582A JPS5994620A (en) | 1982-11-18 | 1982-11-18 | Production of carbon fiber by vapor phase method |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPS5994620A true JPS5994620A (en) | 1984-05-31 |
Family
ID=16434796
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP20106582A Pending JPS5994620A (en) | 1982-11-18 | 1982-11-18 | Production of carbon fiber by vapor phase method |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS5994620A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS62500943A (en) * | 1984-12-06 | 1987-04-16 | ハイピリオン・カタリシス・インタ−ナシヨナル・インコ−ポレイテツド | carbon fibril |
| JPS63503555A (en) * | 1986-06-06 | 1988-12-22 | ハイピリオン・カタリシス・インターナシヨナル・インコーポレイテツド | Novel carbon fibrils |
| US4855091A (en) * | 1985-04-15 | 1989-08-08 | The Dow Chemical Company | Method for the preparation of carbon filaments |
-
1982
- 1982-11-18 JP JP20106582A patent/JPS5994620A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS62500943A (en) * | 1984-12-06 | 1987-04-16 | ハイピリオン・カタリシス・インタ−ナシヨナル・インコ−ポレイテツド | carbon fibril |
| JPH03174018A (en) * | 1984-12-06 | 1991-07-29 | Hyperion Catalysis Internatl Inc | Carbon fibril, its production and composition containing same |
| US4855091A (en) * | 1985-04-15 | 1989-08-08 | The Dow Chemical Company | Method for the preparation of carbon filaments |
| JPS63503555A (en) * | 1986-06-06 | 1988-12-22 | ハイピリオン・カタリシス・インターナシヨナル・インコーポレイテツド | Novel carbon fibrils |
| JPH01131251A (en) * | 1986-06-06 | 1989-05-24 | Hyperion Catalysis Internatl Inc | Novel carbon fibril, its production and composition containing said fibril |
| JPH0377288B2 (en) * | 1986-06-06 | 1991-12-10 | Haipirion Katarishisu Intern Inc |
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