JPS6246645B2 - - Google Patents
Info
- Publication number
- JPS6246645B2 JPS6246645B2 JP58037312A JP3731283A JPS6246645B2 JP S6246645 B2 JPS6246645 B2 JP S6246645B2 JP 58037312 A JP58037312 A JP 58037312A JP 3731283 A JP3731283 A JP 3731283A JP S6246645 B2 JPS6246645 B2 JP S6246645B2
- Authority
- JP
- Japan
- Prior art keywords
- mesophase
- section
- cross
- carbon
- spinning
- 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
- 229920000049 Carbon (fiber) Polymers 0.000 claims description 38
- 239000004917 carbon fiber Substances 0.000 claims description 38
- 238000009987 spinning Methods 0.000 claims description 24
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 20
- 239000000835 fiber Substances 0.000 claims description 15
- 239000011295 pitch Substances 0.000 claims description 14
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 11
- 229910052799 carbon Inorganic materials 0.000 claims description 11
- 239000002994 raw material Substances 0.000 claims description 11
- 238000000034 method Methods 0.000 claims description 7
- 239000011301 petroleum pitch Substances 0.000 claims description 5
- 238000002074 melt spinning Methods 0.000 claims description 4
- 230000001788 irregular Effects 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 description 10
- 239000007789 gas Substances 0.000 description 7
- 239000000463 material Substances 0.000 description 6
- 230000000704 physical effect Effects 0.000 description 6
- 229920005989 resin Polymers 0.000 description 6
- 239000011347 resin Substances 0.000 description 6
- 238000004626 scanning electron microscopy Methods 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 4
- 238000003763 carbonization Methods 0.000 description 3
- 238000004523 catalytic cracking Methods 0.000 description 3
- 238000004821 distillation Methods 0.000 description 3
- 239000002243 precursor Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 239000006227 byproduct Substances 0.000 description 2
- XLJMAIOERFSOGZ-UHFFFAOYSA-N cyanic acid Chemical compound OC#N XLJMAIOERFSOGZ-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 229920002239 polyacrylonitrile Polymers 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000003575 carbonaceous material Substances 0.000 description 1
- 238000010000 carbonizing Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 230000005070 ripening Effects 0.000 description 1
- 239000002341 toxic gas Substances 0.000 description 1
Classifications
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
- D01F9/12—Carbon filaments; Apparatus specially adapted for the manufacture thereof
- D01F9/14—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments
- D01F9/145—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from pitch or distillation residues
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/253—Formation of filaments, threads, or the like with a non-circular cross section; Spinnerette packs therefor
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
- D01F9/12—Carbon filaments; Apparatus specially adapted for the manufacture thereof
- D01F9/14—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments
- D01F9/32—Apparatus therefor
- D01F9/322—Apparatus therefor for manufacturing filaments from pitch
Description
【発明の詳細な説明】
本発明は長繊維の高強度高弾性炭素繊維の製造
工程に於て、その紡糸技術に依つて長繊維の特に
高強度高弾性炭素繊維を製造する方法に関するも
のである。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for producing long fibers, particularly high strength, high modulus carbon fibers, by using spinning technology in the process of producing long fibers, particularly high strength, high modulus carbon fibers. .
本発明方法は減圧軽油の熱接触分解（FCC）
によつて副生される残渣炭素物質の石油系ピツチ
を熱処理してメソフエーズ（偏光顕微鏡によつて
測定し得る）を含有するピツチを製造し、これを
熟成してメソフエーズのみを融着巨大化して、
100％メソフエーズ（偏光顕微鏡によつて容易に
確認することが出来る）を分離精製しこれを円型
とは異なつた断面を有する紡糸ノズル（１例を第
２図に図示するがこれのみに限定するものではな
い）を使用して、紡糸温度300℃乃至330℃で溶融
紡糸し、不融化、炭化して石油系ピツチを原料と
する炭素繊維の断面の走査電子顕微鏡（SEM）
による炭素の配列がランダム状（乱流状）且つ円
形に近い断面を有する長繊維の特に高強度且つ高
弾性炭素繊維を製造する方法である。 The method of the present invention is thermal catalytic cracking (FCC) of vacuum gas oil.
A petroleum-based pitch containing residual carbon substances produced as a by-product is heat-treated to produce a pitch containing mesophases (which can be measured using a polarizing microscope), and this is aged to fuse only the mesophases to a large size. ,
Separate and purify 100% mesophase (which can be easily confirmed with a polarizing microscope) and use a spinning nozzle with a cross section different from a circular one (an example is shown in Figure 2, but this is limited to only this). Scanning electron microscopy (SEM) of a cross-section of carbon fiber made from petroleum pitch, which is melt-spun at a spinning temperature of 300°C to 330°C, infusible, and carbonized using
This is a method for producing particularly high-strength and high-elasticity long fiber carbon fibers having a random (turbulent) carbon arrangement and a nearly circular cross section.
近年航空機、自動車、その他輸送機製作工業の
急速な成長の結果、それに必要な材料として特別
な物質との組合わせによつて製作され、それのい
くつかの物理的性質が極めて勝れており而も特異
性を発揮しうる材料を望む声が大きくなつている
が、特に強い強度及び弾性を具備し、同時に軽量
で安価な材料の出現が強く要求されている。 As a result of the rapid growth of the aircraft, automobile, and other transportation manufacturing industries in recent years, the necessary materials have been manufactured by combining special substances, and some of them have extremely superior physical properties. There is a growing demand for materials that can exhibit specificity, and there is a strong demand for materials that have particularly high strength and elasticity, and at the same time are lightweight and inexpensive.
しかるに現在の技術でかゝる材料を多量に安定
して供給することが出来ないので、これに答える
ため複合材料（強化樹脂）の製造に関する研究が
盛んに行なわれている。 However, it is not possible to stably supply such materials in large quantities with current technology, and in order to solve this problem, research is being actively conducted on the production of composite materials (reinforced resins).
強化樹脂に使用される最も有望な材料の一つと
して長繊維の高強度高弾性炭素繊維がある。この
材料は前述の産業の急速な成長が始まりかけた際
に現われたもので、この長繊維の高強度高弾性炭
素繊維と樹脂とを組合せると他に全く類例を見な
いような特性を発揮する強化樹脂を得ることが出
来る。しかし残念なことであるが、強化樹脂用の
長繊維の高強度高弾性炭素繊維は現在極めて高価
なため、これを使用する強化樹脂が極めて顕著な
特性を発揮するにもかゝわらず、その需要があま
りのびていない。 One of the most promising materials for use in reinforced resins is long-fiber, high-strength, high-modulus carbon fiber. This material emerged at the beginning of the rapid growth of the aforementioned industry, and the combination of this long-fiber, high-strength, high-modulus carbon fiber and resin exhibited properties that were completely unparalleled. It is possible to obtain a reinforced resin that Unfortunately, long-fiber, high-strength, high-modulus carbon fibers for reinforced resins are currently extremely expensive, so even though reinforced resins using them exhibit extremely remarkable properties, Demand is not growing very much.
現在入手出来る長繊維の高強度高弾性炭素繊維
はその原料が特殊な製造法によつて製糸されたポ
リアクリロニトリル繊維が主であることは公知の
事実である。このポリアクリロニトリル繊維は炭
素繊維の前駆体として高価であるばかりでなく、
この前駆体からの炭素繊維の収率が約45％で極め
て悪い。この事実が優れた物性を有する高強度高
弾性炭素繊維を製造する製造装置を巨大化し、更
に炭化処理時に副生する有毒ガス（青酸ガス）の
処理費等に依つて最終製品の高強度高弾性炭素繊
維の製造コストを益々高めることになつている。 It is a well-known fact that the raw material of currently available long-fiber, high-strength, high-elasticity carbon fibers is mainly polyacrylonitrile fibers spun by a special manufacturing method. This polyacrylonitrile fiber is not only expensive as a carbon fiber precursor, but also
The yield of carbon fiber from this precursor is approximately 45%, which is extremely poor. This fact has made the manufacturing equipment for manufacturing high-strength, high-modulus carbon fibers with excellent physical properties huge, and the cost of processing toxic gas (cyanic acid gas) produced as a by-product during the carbonization process has made it difficult to produce high-strength, high-modulus carbon fibers in the final product. The cost of producing carbon fiber is becoming increasingly high.
長繊維の高強度高弾性炭素繊維を安価に製造す
る一つの方法として、メソフエーズを含有するピ
ツチから製造する極めて安価な方法が特公昭54−
1810に記載されており、メソフエーズを含有する
ピツチが長繊維の高強度高弾性炭素繊維の原料と
して極めて優れた原料であることは公知の事実で
ある。然るに高強度高弾性炭素繊維の原料のピツ
チはメソフエーズの含有量且つメソフエーズその
もの物性が炭素繊維の物性に大きな影響を与える
ことは当然で、メソフエーズの含有量の高い程、
且つ品質の良いメソフエーズ程炭素繊維の物性が
向上される。しかしながら100％メソフエーズを
原料として断面の円形の紡糸ノズルで溶融紡糸
し、不融化、炭化して製造される炭素繊維はその
断面の炭素の配列がラジアル状（放射状）とな
り、第３図に示す如く炭素繊維に亀裂を生じて、
製造される炭素繊維は全く商品価値がない。 As a method for inexpensively producing long-fiber, high-strength, high-elastic carbon fibers, an extremely inexpensive method for producing from pitch containing mesophase was proposed in the Japanese Patent Publication Publication No. 1973-1.
1810, and it is a well-known fact that pitch containing mesophase is an extremely excellent raw material for long-fiber, high-strength, high-modulus carbon fibers. However, it is natural that the pitch of the raw material for high-strength, high-elasticity carbon fibers has a large effect on the mesophase content and the physical properties of the mesophase itself, and the higher the mesophase content, the higher the mesophase content.
In addition, the better the quality of mesophase, the better the physical properties of the carbon fiber. However, carbon fibers produced by melt-spinning 100% mesophase using a spinning nozzle with a circular cross-section, infusibility, and carbonization have a radial arrangement of carbon in the cross-section, as shown in Figure 3. Cracks occur in the carbon fiber,
The carbon fiber produced has no commercial value at all.
本発明の目的は断面の亀裂が全く生じない円形
に近い断面を有する長繊維の高強度高弾性炭素繊
維を製造する方法を提供することであり、この目
的は次に示す本発明によつて達成される。 The purpose of the present invention is to provide a method for producing long-fiber, high-strength, high-modulus carbon fibers having a nearly circular cross-section in which no cracks occur in the cross-section, and this purpose is achieved by the present invention described below. be done.
本発明の発明者は種々研究した結果、100％メ
ソフエーズ（偏光顕微鏡によつて容易に確認する
ことが出来る）を原料として製造される炭素繊磯
維の断面のSEMによる炭素の配列をランダム状
（乱流状）にすることによつて亀裂を全く無くす
ること、及び高品質の100％メソフエーズを原料
として炭素繊維を製造すると、炭素繊維の物性特
に強度が顕著に向上する傾向があることを見い出
した。炭素繊維の断面の走査顕微鏡（SEM）に
よる炭素の配列をランダム状にする方法として、
100％メソフエーズを円型とは異なつた断面を有
する紡糸ノズル（第２図にその１例を図示するが
これ丈に限定されない）で、紡糸温度250℃乃至
350℃で溶融紡糸し、不融化、炭化して製造する
炭素繊維の断面の炭素配列がランダム状の全く亀
裂が無く且つ円形に近い断面を有する長繊維の特
に高強度（強度270Kg／mm2以上）高弾性炭素繊維
を製造することが出来る。 As a result of various studies, the inventors of the present invention found that the carbon arrangement was found to be random ( It was discovered that the physical properties of carbon fibers, particularly their strength, tend to improve significantly when carbon fibers are produced using high-quality 100% mesophase as a raw material. Ta. As a method to make the carbon arrangement random by scanning the cross section of carbon fiber using a scanning microscope (SEM),
100% mesophase is spun at a spinning temperature of 250°C to
The carbon fibers produced by melt spinning at 350℃, infusibility, and carbonization have a random carbon arrangement in the cross section, no cracks at all, and a nearly circular cross section with particularly high strength (strength of 270 kg/mm 2 or more). ) It is possible to produce high modulus carbon fiber.
これに使用する円型とは異つた断面の紡糸ノズ
ルの型状の例として第２図に図示したが、これに
限定するものでない。ノズル孔の断面が円形に近
いが完全な円周から円の中心に向つて滑かな曲線
を画いて一様にノズル壁が凸出し孔用き部の断面
積ｓが完全な円であつた場合の断面積s′の約50〜
約80％を占める様にすべきである。第２図のもの
は約54％位になつている。この断面積の比が上記
範囲より小さくなると糸切れが起り易くなる。炭
素繊維製造用の原料のピツチとして100％メソフ
エーズを使用するためピツチそのものの炭素の配
向性が良好なため断面の円型の紡糸ノズルを使用
して溶融紡糸すると炭素繊維の炭素の配列がラジ
アル状となる。しかるに100％メソフエーズを溶
融紡糸する場合に異型の断面の紡糸ノズル内で
100％メソフエーズの流れに乱流の作用を与える
ことのできる型の断面を有する紡糸ノズルを使用
することに依つて炭素の配列をランダム状にする
ことが出来る。 Although FIG. 2 shows an example of the shape of the spinning nozzle having a cross section different from the circular shape used for this purpose, the present invention is not limited thereto. When the cross-section of the nozzle hole is close to a circle, but the nozzle wall is uniformly protruding from the perfect circumference with a smooth curve toward the center of the circle, and the cross-sectional area s of the hole-use part is a perfect circle. The cross-sectional area of s′ is about 50~
It should account for approximately 80%. The figure in Figure 2 is about 54%. If this cross-sectional area ratio is smaller than the above range, thread breakage is likely to occur. Since 100% mesophase is used as the raw material pitch for producing carbon fibers, the pitch itself has good carbon orientation, so when melt-spun using a spinning nozzle with a circular cross section, the carbon fibers have a radial arrangement. becomes. However, when melt-spinning 100% mesophase, inside a spinning nozzle with an irregular cross-section,
By using a spinning nozzle with a cross-section of a type capable of imparting a turbulent effect to the flow of 100% mesophase, the carbon arrangement can be made random.
炭素繊維製造用の原料の100％メソフエーズは
減圧軽油の熱接触分解（FCC）で副生される残
渣炭素物質の石油系ピツチ（初留404℃乃至409℃
以上）の留分を非酸化性ガスに依つて加熱温度
360℃乃至420℃で加熱処理して、メソフエーズを
含有するピツチを製造し、後メソフエーズを生成
する条件より全く別の熟成条件メソフエーズを含
有するピツチを処理してメソフエーズのみを融着
巨大化して熟成温度にて物性の差を利用して100
メソフエーズを分離精製して製造される。 100% mesophase, the raw material for carbon fiber manufacturing, is petroleum-based pitch (initial distillation 404°C to 409°C), a residual carbon material by-produced in the thermal catalytic cracking (FCC) of vacuum gas oil.
heating the fraction (above) using non-oxidizing gas
Pitches containing mesophases are produced by heat treatment at 360℃ to 420℃, and then ripened under completely different conditions than those for producing mesophases.The pitches containing mesophases are treated to fuse only the mesophases, making them large and ripening. 100 using the difference in physical properties at temperature
Manufactured by separating and purifying mesophase.
実施例 １
減圧軽油の熱接触分解（FCC）で副生される
残渣炭素物質の石油系ピツチ（初留404℃乃至終
留560℃以下）の留分にメタンガスを送入しなが
ら加熱温度400℃で２時間加熱処理して前駆体
（Ｒ＆Ｂ相当軟化点67℃）をつくり、之を更に常
圧にてメタンガスを送入しながら加熱温度400℃
で６時間加熱処理してメソフエーズを45.2％含有
するピツチをつくり、後このメソフエーズを含有
するピツチをそのまゝピツチを生成する条件と全
く別の条件で熟成してメソフエーズのみを融着巨
大化させてこの温度で比重の差を利用して100％
メソフエーズを分離し、之を原料として第２図に
示す紡糸ノズルを使用し、紡糸温度310℃、紡糸
速度130ｍ／分で紡糸し、このフイラメント原糸
を300℃で不融化し、2400℃で炭化して、炭素繊
維の断面の炭素の配列がランダム状の長繊維の強
度282Kg／mm2、弾性率48〓／mm2、伸度0.58％の全
く亀裂の無い高強度高弾性炭素繊維を製造するこ
とが出来た。製品のSEMによる断面を第１図に
示す。がこの実験を何回でも繰返したら亀裂の全
く入つていないものが恒に得られた。Example 1 The heating temperature was 400°C while feeding methane gas into the petroleum-based distillate (initial distillation 404°C to final distillation 560°C or lower) of residual carbon substances produced by thermal catalytic cracking (FCC) of vacuum gas oil. A precursor (R&B equivalent softening point of 67°C) was prepared by heating for 2 hours, and then heated to a temperature of 400°C while feeding methane gas at normal pressure.
Heat-treated for 6 hours to produce pitches containing 45.2% mesophases, and then the pitches containing mesophases were aged under conditions completely different from those for producing pitches as they were, to fuse only the mesophases and make them gigantic. 100% using the difference in specific gravity at the lever temperature
Separate mesophase, use this as a raw material, and use the spinning nozzle shown in Figure 2 to spin at a spinning temperature of 310°C and a spinning speed of 130 m/min. This filament yarn is infusible at 300°C and carbonized at 2400°C. By doing so, we produce high-strength, high-modulus carbon fibers with a long fiber strength of 282 kg/mm 2 , an elastic modulus of 48〓/mm 2 , and an elongation of 0.58%, with no cracks at all. I was able to do it. Figure 1 shows a cross section of the product taken by SEM. However, if this experiment was repeated many times, a product without any cracks was always obtained.
対照例 １
実施例１のピツチを使用し紡糸ノズル（0.3）
を使用しその他同じ紡糸不融化・炭化条件で炭素
繊維を製造した。この実験も何回も繰返したが第
２図に示す様に恒に炭素の配列が放射状で亀裂が
入つたものしか得られなかつた。Control example 1 Spinning nozzle (0.3) using the pitch of Example 1
Carbon fibers were produced using the same spinning, infusible and carbonizing conditions. This experiment was repeated many times, but as shown in Figure 2, the only result was one in which the carbon was arranged in a radial pattern with cracks.
参照例 ２
最適紡糸温度を決定するため250℃以下の温度
で紡糸を試みたが紡糸用原料の100％メソフエー
ズの粘度が小さくなり紡糸性が悪く紡糸困難であ
つた。350℃以上の温度では紡糸用原料の100％メ
ソフエーズの粘度が大きくなり過ぎ紡糸フイラメ
ントの糸切れが頻繁に生じて連続して紡糸できな
くなつた。Reference Example 2 In order to determine the optimum spinning temperature, spinning was attempted at a temperature of 250° C. or lower, but the viscosity of 100% mesophase, the raw material for spinning, was low, resulting in poor spinnability and difficulty in spinning. At temperatures above 350°C, the viscosity of the 100% mesophase raw material for spinning became too high, causing frequent breakage of the spinning filament, making continuous spinning impossible.
第１図は本願発明で得られた炭素繊維のSEM
による断面図を示す。第２図は異型断面のノズル
最狭部の断面図を示す。第３図は参照例１で得ら
れた炭素繊素のSEMによる断面図を示す。
Figure 1 is an SEM of carbon fiber obtained by the present invention.
A cross-sectional view is shown. FIG. 2 shows a sectional view of the narrowest part of the nozzle with an irregular cross section. FIG. 3 shows a SEM cross-sectional view of the carbon fiber obtained in Reference Example 1.
Claims (1)
有するピツチをつくり、これを熟成してメソフエ
ーズのみを融着巨大化して、100％メソフエーズ
を分離精製し、これを異型の断面を有する紡糸ノ
ズルで溶融紡糸し、不融化、炭化して製造する炭
素繊維の断面の炭素の配列がランダム状（乱流
状）且つ円形に近い断面を有する長繊維の高強度
高弾性炭素繊維を製造する方法。 ２ 石油系ピツチを原料としてメソフエーズを含
有するピツチをつくり、これを熟成してメソフエ
ーズのみを融着巨大化して、100％メソフエーズ
を分離精製し、これを円型とは異なつた断面の紡
糸ノズルを使用し、紡糸温度250℃乃至350℃で溶
融紡糸し、不融化、炭化して製造する炭素繊維の
断面の炭素の配列がランダム状（乱流状）且つ円
形に近い断面を有する長繊維の高強度高弾性炭素
繊維を製造する特許請求の範囲第１項の方法。[Scope of Claims] 1. Pitch containing mesophase is made using petroleum pitch as a raw material, and this is matured to fuse only the mesophase into a large size, and 100% mesophase is separated and purified, and this is made to have an irregular cross section. The carbon fiber is melt-spun with a spinning nozzle, infusible, and carbonized to produce long-fiber, high-strength, high-elastic carbon fibers in which the cross-section of the carbon fibers is random (turbulent) and has a nearly circular cross-section. Method. 2. Make pitch containing mesophase using petroleum pitch as a raw material, mature it to fuse only the mesophase into a large size, separate and refine 100% mesophase, and spin this into a spinning nozzle with a cross section different from the circular one. The carbon fibers produced by melt-spinning at a spinning temperature of 250°C to 350°C, infusible, and carbonized have long fibers with a random (turbulent) carbon arrangement and a nearly circular cross-section. A method according to claim 1 for producing a high strength and high modulus carbon fiber.
Priority Applications (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP3731283A JPS59163424A (en) | 1983-03-09 | 1983-03-09 | Spinning of petroleum mesophase |
| DE19833346256 DE3346256C2 (en) | 1983-03-09 | 1983-12-21 | Process for the production of continuous yarns from carbon fibers |
| FR8400184A FR2542329B1 (en) | 1983-03-09 | 1984-01-06 | METHOD OF SPINNING A MESOPHASE OF OIL ORIGIN |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP3731283A JPS59163424A (en) | 1983-03-09 | 1983-03-09 | Spinning of petroleum mesophase |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS59163424A JPS59163424A (en) | 1984-09-14 |
| JPS6246645B2 true JPS6246645B2 (en) | 1987-10-03 |
Family
ID=12494167
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP3731283A Granted JPS59163424A (en) | 1983-03-09 | 1983-03-09 | Spinning of petroleum mesophase |
Country Status (3)
| Country | Link |
|---|---|
| JP (1) | JPS59163424A (en) |
| DE (1) | DE3346256C2 (en) |
| FR (1) | FR2542329B1 (en) |
Families Citing this family (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0781211B2 (en) * | 1983-11-10 | 1995-08-30 | 株式会社ペトカ | Carbon fiber manufacturing method |
| JPS61113827A (en) * | 1984-11-06 | 1986-05-31 | Teijin Ltd | Production of high-performance pitch-based carbon fiber |
| DE3441727A1 (en) * | 1984-11-15 | 1986-05-15 | Bergwerksverband Gmbh, 4300 Essen | METHOD FOR PRODUCING ANISOTROPIC CARBON FIBERS |
| US5154908A (en) * | 1985-09-12 | 1992-10-13 | Clemson University | Carbon fibers and method for producing same |
| JPS62160970A (en) * | 1986-01-09 | 1987-07-16 | Honda Motor Co Ltd | Assembly device for car body |
| US5156831A (en) * | 1986-01-21 | 1992-10-20 | Clemson University | Method for producing high strength, melt spun carbon fibers |
| US5149517A (en) * | 1986-01-21 | 1992-09-22 | Clemson University | High strength, melt spun carbon fibers and method for producing same |
| JPS62170526A (en) * | 1986-01-22 | 1987-07-27 | Osaka Gas Co Ltd | Production of carbon fiber having elliptic cross-section |
| US4915926A (en) * | 1988-02-22 | 1990-04-10 | E. I. Dupont De Nemours And Company | Balanced ultra-high modulus and high tensile strength carbon fibers |
| US5145616A (en) * | 1988-06-10 | 1992-09-08 | Teijin Limited | Process for the preparation of pitch-based carbon fiber |
| US5037589A (en) * | 1988-11-18 | 1991-08-06 | Nippon Steel Corporation | Method of producing mesophase pitch type carbon fibers and nozzle for spinning same |
| US7165963B2 (en) * | 2003-10-31 | 2007-01-23 | Invista North America S.A.R.L. | Spinneret for producing circular cross section yarn and process for making the same |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5742927A (en) * | 1980-08-28 | 1982-03-10 | Secr Defence Brit | Production of high strength and high elastic ratio reinforcing fiber and composite material containing same |
| JPS57119984A (en) * | 1980-07-21 | 1982-07-26 | Toa Nenryo Kogyo Kk | Preparation of meso-phase pitch |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB991224A (en) * | 1962-05-29 | 1965-05-05 | Snia Viscosa | Improvements in or relating to spinnerets |
| US4209500A (en) * | 1977-10-03 | 1980-06-24 | Union Carbide Corporation | Low molecular weight mesophase pitch |
| US4303631A (en) * | 1980-06-26 | 1981-12-01 | Union Carbide Corporation | Process for producing carbon fibers |
-
1983
- 1983-03-09 JP JP3731283A patent/JPS59163424A/en active Granted
- 1983-12-21 DE DE19833346256 patent/DE3346256C2/en not_active Expired
-
1984
- 1984-01-06 FR FR8400184A patent/FR2542329B1/en not_active Expired
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS57119984A (en) * | 1980-07-21 | 1982-07-26 | Toa Nenryo Kogyo Kk | Preparation of meso-phase pitch |
| JPS5742927A (en) * | 1980-08-28 | 1982-03-10 | Secr Defence Brit | Production of high strength and high elastic ratio reinforcing fiber and composite material containing same |
Also Published As
| Publication number | Publication date |
|---|---|
| JPS59163424A (en) | 1984-09-14 |
| FR2542329A1 (en) | 1984-09-14 |
| DE3346256C2 (en) | 1992-01-16 |
| FR2542329B1 (en) | 1986-05-16 |
| DE3346256A1 (en) | 1984-09-13 |
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