【発明の詳細な説明】本発明は組成がＨ１成分、Ｂ、成分、その他からなる石
油系ピッチを加熱処理及び熟成処理する過程に於けるＨ
０成分及びＢ、成分の変化を究明追兇して。DETAILED DESCRIPTION OF THE INVENTION The present invention aims to reduce H in the process of heat treatment and aging treatment of petroleum pitch whose composition consists of H1 component, B component, and others.
Investigate the changes in the 0 and B components.
特定範囲のＨ０成分、Ｂ、成分、Ｑ、 Ｓ、成分及びＱ
．ｉ．成分から成る１００９６メソフエーズピツチをａ
造する方法に関する。Specific range of H0 component, B, component, Q, S, component and Q
．． i. 10,096 mesophasic pitches consisting of a
Concerning how to build.
近年航空機、自動車、その他権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
せに依シ、そ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っ
ているが、特に高い強度及び弾性を具備し、同時に動量
で安価な材料の出現が強く安来されている。しかるに現
在の技術でか＼る材料を多菫に安定供給することが出来
なりので、これに答えるための複合材（強化樹脂）の製
造に関する研兇が盛んに行われている。In recent years, as a result of the rapid growth of the aircraft, automobile, and other power transport manufacturing industries, the necessary materials have become dependent on the combination of special substances, and some of their physical properties are extremely superior and unique. There is a growing demand for materials that can exhibit high properties, and there is a strong demand for materials that have particularly high strength and elasticity, and at the same time are flexible and inexpensive. However, with the current technology, it is not possible to stably supply such materials to a wide range of materials, so research is being actively conducted on the production of composite materials (reinforced resins) in order to meet this demand.
複合材に使用される最も有望な材料の一つとして一＆稙
維の高強度高弾性炭素繊維がある。この材料は前述の種
々の輸送機製作工業の急速な成長が始まりかけ念際に舘
く挽れたもので、この炭素稙維を樹脂と組合せると、全
く類例を見ないような特性を発揮する複合材を得ること
が出来る。One of the most promising materials used in composites is high-strength, high-modulus carbon fiber. This material was created at the last minute just as the aforementioned rapid growth of the transportation equipment manufacturing industry began, and when this carbon fiber was combined with resin, it exhibited completely unprecedented properties. It is possible to obtain a composite material that
現在入手出来る高強度−弾性に紫稙維はポリアクリロニ
トリル繊維を特殊な方法で耐炎化し、後炭化して製造さ
れることは公知の事実であるが、このポリアクリロニト
リル繊維は前駆体として高価であるはかりでなく、この
前駆体からの炭素繊維の収率も約４５％の如く低いため
、アクリロニトリル糸（ＰＡＮ系）からの炭素繊維は高
価である。It is a well-known fact that the currently available high-strength and elastic purple fibers are manufactured by making polyacrylonitrile fibers flame-resistant using a special method and then carbonizing them, but this polyacrylonitrile fiber is expensive as a precursor. Carbon fibers from acrylonitrile yarns (PAN-based) are expensive, as the yield of carbon fibers from this precursor is also low, such as about 45%.
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
てメソフェーズを官有するピッチを原料として高強度高
弾性炭素繊維を製造する方法が持分１ｉ８５４−１，８
１０に記載されており、メソフェーズを含有するピッチ
が高強度高弾性炭素繊維の原料であることは公知のφ実
である。然るにこのメソフェーズ金含有するピッチは多
くの非メソピッチを含有し、高強度高弾性炭素繊維の原
料として最適と考えられない。As a method for manufacturing high-strength, high-modulus carbon fibers at low cost, there is a method for manufacturing high-strength, high-modulus carbon fibers using mesophase-bearing pitch as a raw material.
10, and it is a well-known fact that pitch containing mesophase is a raw material for high-strength, high-elasticity carbon fibers. However, this mesophase gold-containing pitch contains a large amount of non-mesopitch and is not considered optimal as a raw material for high-strength, high-modulus carbon fibers.
又特公昭５７−８８，０１６に依れば、Ｈ００チ約２．
０％乃至約２０．０％、Ｂ、成分約１５．０％乃至４５
．０％を含有し、残余はＱ、Ｓ、成分で約９０ｅｓ以上
メソフェーズを含有するピッチを原料とする炭素繊維の
製造性が記載され、しかもそれの特性が特公昭５７−８
８．０１６に記載されている。それに依るとその炭化温
度は１．５００℃であるが、その物性の１１は高強度高
弾性炭素＠維とは全く菖えぬ。According to Special Publication No. 57-88, 016, H00chi approx. 2.
0% to about 20.0%, B, component about 15.0% to 45
．． The paper describes the manufacturability of carbon fibers made from pitch containing mesophase of approximately 90 es or more, with the remainder being Q, S, and the remaining components, and its characteristics are described in Japanese Patent Publication No. 57-8.
8.016. According to this, its carbonization temperature is 1.500°C, but its physical properties 11 are completely different from those of high-strength, high-elastic carbon fiber.
本発明の目的は溶融紡糸用の１００暢メンフエーズピツ
チの組成がＨ０成分、Ｂ、成分、Ｑ、 Ｓ、成分及びＱ
．ｉ．成分よりなり、それの生成機構の解明を基にし原
料の石油系ピッチの組成のＨ０成分及びＢ、成分の加熱
、熟成処理の過程を制御して高強度高弾性炭素繊維用１
００％メソフェーズピッチとし最適の組成の１００％メ
ソフェーズピッチを製造する方法を提供することである
。The object of the present invention is that the composition of a 100-strand memphaze pitch for melt spinning is H0 component, B component, Q, S component, and Q.
．． i. Based on the elucidation of the formation mechanism of these components, the H0 component and B of the composition of petroleum-based pitch as a raw material, and the heating and aging process of the components are controlled to produce high-strength, high-elastic carbon fiber 1.
An object of the present invention is to provide a method for producing 100% mesophase pitch having an optimal composition.
高強だ高弾性炭素繊維用の安価な且つ物性の安定した１
００％メソフェーズピッチを製造する方法として、極め
て安価な石油系ピッチ（Ｈ，成分、Ｂ。1. Inexpensive and stable physical properties for high strength and high elasticity carbon fiber.
As a method for producing 00% mesophase pitch, extremely cheap petroleum-based pitch (H, component, B.
成分、その他）を原料とし、Ｈ８成分及びＢ、成分が加
熱処理及び熟成処理中に軸通する天々の成分の動向及び
変化を追求して、１００９６メソフエーズビツチを合理
的に製造することにある。To rationally manufacture 10096 mesophase bits by using H8 component, B component, and other components as raw materials and pursuing trends and changes in the natural components that pass through heat treatment and aging treatment. It is in.
その目的とするところは、脱硫減圧軽油の熱接触分解（
ＦＣＣ）に依って一生する石油系ピッチ（初ｗ２４０℃
乃至終留５６０℃）を減圧蒸留して関囁カットした留分
（初留４６０℃乃至終留５６０℃、Ｈ０成分２０．０％
乃至８４．Ｏｓ、 Ｂ、成分１６．０９６乃至８０．０
％、Ｑ．ｉ．成分０．２％、無機質物０．１悌）に非酸
化性ガスを吹き込み撹拌しつゝ温度３８０℃乃至４２０
℃で２時間乃至１０時間常圧或は加圧下で加熱処理し、
メソフェーズ（偏光ｗ４倣鋭で確認する）を５．０％乃
至１５．（ｌ含有するピッチを造り、この生成ピッチを
温度３００℃乃至３５０℃で８時間乃至３０１１間非酸
化性ガス気流下熟成させ、生成ピッチ中のメソフェーズ
のみを１層巨大化させ、その熟成温度で比重の差に依っ
て上層に全くメソフェーズを含有せぬ非メソピッチ（偏
光顕微鏡で確認。The purpose of this is to thermally catalytic cracking of desulfurized vacuum gas oil (
Petroleum-based pitch (first w240℃) that lasts a lifetime depending on FCC)
Distilled under reduced pressure from 560°C to final distillate and cut the fraction (from 460°C to final distillate 560°C, H0 component 20.0%)
to 84. Os, B, component 16.096 to 80.0
%, Q. i. Non-oxidizing gas was blown into the mixture (0.2% of ingredients, 0.1% of inorganic matter) and the mixture was heated to a temperature of 380°C to 420°C while stirring.
Heat treatment at ℃ for 2 hours to 10 hours under normal pressure or pressure,
Mesophase (confirmed with polarized light w4 scanning sharp) 5.0% to 15. (Pitch containing l is produced, and this produced pitch is aged at a temperature of 300°C to 350°C for 8 hours to 3011 hours under a stream of non-oxidizing gas, only the mesophase in the produced pitch becomes one layer larger, and at that aging temperature Due to the difference in specific gravity, the upper layer does not contain any mesophase (confirmed with a polarizing microscope).
Ｈ００チ１０．０％乃至１７．０％、Ｂ、成分２２．０
％乃至４６．０％、Ｑ、 Ｓ、成分４２．０％乃至６０
．０％、Ｑ．ｉ．成分０．５％以下、このｑ、ｚ、成分
は水路することに依９可溶）と下層にメソフェーズと画
然と分離精製し、これを前躯体として使用する。同この
際石油系ピッチを製造するための熱接触分解（ＦＣＣ）
で使用される触媒の無機質の倣粉末及び分解温度約５１
０℃で副生ずるキノリンネ溶分の有機物等を前述のメソ
フェーズピッチ中に包含させることが出来る、従って分
離精製する非メソピッチを溶融紡糸用の１００％メン７
エーズビツチ製造用の前駆体として使用する事に依シ、
原料の石油系ピッチ中に混入する無機質の雇媒及び中ノ
リン不浴の有機質物を全く無くすることが可能となシ、
従って前駆体にこれ等の混入物が全く無くなシ溶Ｍ幼糸
用の１００％メソフェーズピッチ中にも混入することも
無くなるので、これ等の混入物に依る浴融紡糸の際の糸
切を無くすると云う他めて優れた効果を発揮することが
出来る。H00chi 10.0% to 17.0%, B, component 22.0
% to 46.0%, Q, S, component 42.0% to 60
．． 0%, Q. i. The components 0.5% or less (q, z, 9) are clearly separated and purified from the mesophase in the lower layer and used as a precursor. At this time, thermal catalytic cracking (FCC) was used to produce petroleum-based pitch.
The inorganic imitation powder of the catalyst used in and the decomposition temperature of about 51
It is possible to incorporate the organic matter of the quinoline solution which is produced as a by-product at 0°C into the above-mentioned mesophase pitch.
Depending on its use as a precursor for the production of
It is possible to completely eliminate inorganic solvents and non-bathable organic substances mixed in the raw petroleum pitch,
Therefore, these contaminants are completely absent from the precursor, and they will not be mixed in the 100% mesophase pitch for molten M young yarn, so thread breakage during bath-melt spinning due to these contaminants will be avoided. In addition to eliminating it, excellent effects can be achieved.
前述の非メソピッチ（Ｈ，成分１０．０％乃至１７．０
％。The aforementioned non-mesopitch (H, component 10.0% to 17.0%
%.
Ｂ、成分２２．０ ％乃至４６．０ ｓ、 Ｑ、８．成
分４２．０ ％乃至６０．０％、Ｑ．ｉ．成分０．５％
以下）１００部に対して後述の非メソピッチ（Ｈ，成分
２．０４乃至６．０％、Ｂ。B, component 22.0% to 46.0s, Q, 8. Ingredients: 42.0% to 60.0%, Q. i. Ingredients 0.5%
Below) 100 parts of non-mesopitch (H, component 2.04 to 6.0%, B) as described below.
成分２２．０％乃至３３．０％、Ｑ、 ８．成分６０．
０チ乃至８２、Ｏｓ、 Ｑ、 ｉ、成分０．４％乃至４
．０％）を６０部乃至１４０部混合し、これ勢の混合物
に常圧或は加圧下で非酸化性ガスを吹き込み撹拌しつゝ
温度３８０℃乃至４３０℃で１時間乃至６時間加熱処理
してメソフェーズを１５％乃至６０％含有するピッチを
造り、この生成ピッチを温度３００℃乃至３５０℃で時
間５時間乃至Ｉ時間非酸化性ガス下で熟成させピッチ中
のメソフェーズのみを融着巨大化させその熟成温度で物
性（比重或は粘度）の差に依９上層に全くメソフェーズ
を含有せぬ非メソピッチ（Ｈ，成分２．０％乃至６．Ｏ
ｌ、Ｂ、成分２２．０ ％乃至３３．０９６゜ｑ、 ｓ
、成分６０．０％乃至８２．０％、Ｑ．ｉ．成分０．４
％乃至４．０傷このＱ．ｉ．成分は水添に依り可溶）を
下層に１００％メソフェーズピッチ（Ｈ，成分０．４％
乃至４．０％、Ｂ、成分８．０％乃至２１．０％、Ｑ、
Ｓ、成分４２．Ｏ優乃至５６．０％、Ｑ、 ｔ、 ２
８．０％乃至４４．０％このＱ、１゜成分は水痘に依り
可溶）を画然と区分する。この分離精製した１００俤メ
ソ７エーズピツチは前述の如（Ｈ，成分、Ｂ、成分、Ｑ
、Ｓ、成分及びｑ、ｉ、成分の４成分が夫々互に融合し
てメソフェーズピッチを形成しているが、この成分中Ｈ
１１成はその分子量も小さく４成分中最も挿発し易い、
従って１００％メソフェーズピッチを溶融紡糸する際紡
糸孔からより多くＨ００成が飛散して糸切れの原因とな
るので。Ingredients 22.0% to 33.0%, Q, 8. Ingredient 60.
0chi to 82, Os, Q, i, component 0.4% to 4
．． 0%) were mixed, and the mixture was heated at a temperature of 380°C to 430°C for 1 to 6 hours while blowing a non-oxidizing gas under normal pressure or pressurization and stirring. A pitch containing 15% to 60% of mesophase is produced, and the resulting pitch is aged at a temperature of 300°C to 350°C for 5 to 1 hours under a non-oxidizing gas to fuse only the mesophase in the pitch and make it large. It depends on the difference in physical properties (specific gravity or viscosity) depending on the aging temperature. 9 Non-mesopitch (H, component 2.0% to 6.0
l, B, component 22.0% to 33.096゜q, s
, components 60.0% to 82.0%, Q. i. Ingredients 0.4
% to 4.0 scratches on this Q. i. 100% mesophase pitch (H, component 0.4%
4.0% to 4.0%, B, component 8.0% to 21.0%, Q,
S, component 42. O good to 56.0%, Q, t, 2
8.0% to 44.0% (this Q, 1° component is soluble depending on chickenpox) is clearly classified. This separated and purified 100 yen meso 7Aze pitch was prepared as described above (H, component, B, component, Q).
, S, component and q, i, component fuse together to form mesophase pitch, but in this component, H
11 has a small molecular weight and is the most easily detected among the four components.
Therefore, when melt-spinning 100% mesophase pitch, more H00 particles are scattered from the spinning holes, causing yarn breakage.
このＨ１１成は紡糸される炭素繊維の物性にも良い影響
を与えるとは考えられぬ。This H11 formation is not considered to have a positive effect on the physical properties of the spun carbon fiber.
コ（７）１００１メソフエーズピツチの紡糸性を改善し
、更にこのピッチから炭素繊維の物性の向上のりａｅ）
１００％メソフェーズピッチ中のＨ１１成を炭素数６乃
至８の脂肪族縦比水素に依る溶剤抽出法で除去して得ら
れるラフネート（Ｈ，成分０．１％以下、Ｂ、成分８．
０％乃至２２．０％、Ｑ、Ｓ、成分４２．０％乃至５８
．０％、Ｑ．ｉ．成分２９．０％乃至４６．０畳）の１
００係メソフエーズピツチをｍ融紡糸用に使用する。こ
の組成の１００％メソフェーズピッチは、平均分子量の
分布がより平均化され、紡糸性も改善され、紡糸孔が多
穴（数百個以上）の場合にも糸切れも殆ど無く長時間紡
糸を可能とする。このラフィネートの１００％メソフェ
ーズピッチの軟化点２４０℃乃至２７０’Ｃ１粘度３２
０℃で１００．１！イズ乃至１６０ポイズであるが、ラ
フィネートの１００％メソフェーズピッチの各成分即ち
Ｈ１１成、Ｂ、成分、Ｑ、 ８．成分及びＱ．ｉ．成分
の割合史に夫々の構造に依り、ラフィネートの１００％
メソフェーズピッチの物性即ち軟化点、粘度、平均分子
量及び＃融紡糸性等が直接定まるもので、従って夫々の
構造及び割合とラフィネートの物性との関係を切り離す
ことは全く出来ない。(7) Improving the spinnability of 1001 mesophase pitch and further improving the physical properties of carbon fiber from this pitch (ae)
Roughnate (H, component 0.1% or less, B, component 8.
0% to 22.0%, Q, S, component 42.0% to 58
．． 0%, Q. i. component 29.0% to 46.0 tatami)
00 mesophase pitch is used for m-melt spinning. 100% mesophase pitch with this composition has a more even average molecular weight distribution, improved spinnability, and allows long-time spinning with almost no yarn breakage even when there are many spinning holes (several hundred or more). shall be. Softening point of 100% mesophase pitch of this raffinate: 240°C to 270'C1 Viscosity: 32
100.1 at 0℃! 160 poise, each component of 100% mesophase pitch of raffinate, namely H11 component, B component, Q, 8. Ingredients and Q. i. 100% of raffinate, depending on the composition of each component
The physical properties of mesophase pitch, such as softening point, viscosity, average molecular weight, #melt spinnability, etc., are directly determined, and therefore the relationship between each structure and proportion and the physical properties of raffinate cannot be separated at all.
１００％メソフェーズぎツチを製造する際上層に分離さ
れる全くメソフェーズを含有せぬ非メソピッチ（Ｈ，成
分２．０囁乃至６．０％、Ｂ、成分２２．０％乃至３３
．０％、Ｑ、 Ｓ、成分６０．０％乃至８２．０％、Ｑ
．ｉ．成分０．４％乃至４．０ ％ ）は前述の前駆体
と混合し、１００ ％メソフェーズぎツチを製造するた
めの原料とすることが出来る。100% Mesophase Non-mesopitch containing no mesophase (H, component 2.0% to 6.0%, B, component 22.0% to 33%) separated into the upper layer when producing 100% mesophase.
．． 0%, Q, S, component 60.0% to 82.0%, Q
．． i. The components (0.4% to 4.0%) can be mixed with the aforementioned precursors and used as raw materials for producing 100% mesophase joints.
同１００％メソ７エーズピツチ製造用の原料の前駆体の
非メソピッチ（Ｈ１１成１０．０％乃至１７．０ ｓ。Non-mesopitch (H11 formation 10.0% to 17.0 s) as a precursor of the raw material for producing 100% meso-7Aze pitch.
Ｂ、成分２２．０％乃至４６．０％、Ｑ、 Ｓ、成分４
２．０％乃至６２．０％、Ｑ、ｉ、成分０．５％以下）
を製造する好ましい加熱処理条件は温度３９０℃乃至４
１０℃、時間４時間乃至８時間、好ましい熟成Ｍ７Ｎ条
件は温良３１０℃乃至３３０℃、時間１０時間乃至（９
）時間で、更に１ｔＪＯ％メソフェーズピッチをｓ造す
る好ましい加熱処理条件は温度３９０℃乃至４１０℃１
時間１時間乃主４時間で、それの熟成ＭＮ条件は前駆体
を製造する熟成Ｍ８１着条件と殆ど同じである。B, component 22.0% to 46.0%, Q, S, component 4
2.0% to 62.0%, Q, i, component 0.5% or less)
The preferred heat treatment conditions for manufacturing are a temperature of 390°C to 4.
10℃, time 4 hours to 8 hours, preferable aging M7N conditions are temperature 310℃ to 330℃, time 10 hours to (9
) time, and the preferable heat treatment conditions for further forming 1 tJO% mesophase pitch are at a temperature of 390°C to 410°C.
The aging time was 1 hour to 4 hours, and the aging MN conditions were almost the same as the aging M81 conditions for producing the precursor.
これ等の加熱処理及び熟成融着処理に使用する非酸化性
ガスはエタン、プロ、ｅン、ブタン、沸点の低い１負化
しない留分及び最も優れているガスは石油ピッチから減
圧蒸留し造る留分を加熱処理する際細生するドライガス
（例えは水素６．０％、メタン７４．６％、エタン１３
．３暢、プロ／９７３．６％、ブタン１．３％、ペンタ
ン０．９％、オレフィン約０．３％）を挙げることが出
来る。The non-oxidizing gases used in these heat treatments and aging fusion treatments are ethane, pro, ene, butane, fractions with low boiling points that do not turn negative, and the best gases are distilled under reduced pressure from petroleum pitch. Dry gas (e.g. 6.0% hydrogen, 74.6% methane, 13% ethane) that forms when heat-treating the fraction.
．． 3%, pro/973.6%, butane 1.3%, pentane 0.9%, olefin approximately 0.3%).
実施例１脱硫減圧軽油の熱接触分解（ＦＣＣ）に依って副生する
石油系ピッチ（Ｈ，成分７６．１８％、Ｂ、成分２３．
８２俤、Ｑ．ｉ．成分０．１％、無機質物０．１暢以下
）を減圧蒸留して８５優カツトし念留分（初留４６０℃
乃至終留５６０℃、Ｈ１１成４３．８％、Ｂ、成分５５
．２％、Ｑ．ｉ．成分Ｏ，Ｓ Ｓ、無機質物０．１％）
にプロパンガスを吹き込み攪拌しながら加熱温度４００
℃で６時間加熱処理し、後生成ピッチをプロ／Ｑンガス
下温度３２０℃で田時間熟成させ、生成ピッチ中のメソ
フェーズのみを融着巨大化させ、その熟成温度で比重の
差に依り上層に全くメソフェーズを含有せぬ非メソピッ
チ（Ｈ，成分１１．３４％、Ｂ．成分４２．４２俤、Ｑ
、Ｓ、成分４５．８６％、Ｑ．ｉ．成分０．３８％）を
下層にメソフェーズピッチをと画然と分＊ｔ、ｔａする
。Example 1 Petroleum pitch (H, component 76.18%, B, component 23.1%) produced by thermal catalytic cracking (FCC) of desulfurized vacuum gas oil.
82 yen, Q. i. 0.1% of components, less than 0.1% of inorganic substances) are distilled under reduced pressure to cut 85% of the total fraction (initial distillation at 460°C).
to final distillation 560°C, H11 composition 43.8%, B, component 55
．． 2%, Q. i. Ingredients O, SS, inorganic substances 0.1%)
Blow in propane gas and heat to 400 ml while stirring.
After heat treatment at ℃ for 6 hours, the resulting pitch is aged for an hour at 320℃ under Pro/Q gas, and only the mesophase in the generated pitch is fused and becomes gigantic. Non-mesopitch containing no mesophase (H, component 11.34%, B. component 42.42 yen, Q
, S, component 45.86%, Q. i. 0.38%) and mesophase pitch as the lower layer.
この分離精製した高強度高弾性炭素繊維製造用の非メソ
ピッチを製造すると共に下層に分離する融着巨大化し九
メソ７エーズビツチ中に石油系ピッチ中に既存するキノ
リンネ溶分及び触媒の微小無機質物を包含させ、これ等
の夾雑物を全く含有せぬ前述の非メソピッチ１００部に
対して後述の非メソピッチ（Ｈ，成分３．７３優、Ｂ、
成分３１．８２％、Ｑ、Ｓ。This separated and refined non-mesopitch for producing high-strength, high-elastic carbon fibers is produced, and the quinolinated content and catalyst minute inorganic substances existing in the petroleum-based pitch are removed during the fusion process, which is separated into the lower layer and becomes gigantic. To 100 parts of the above-mentioned non-mesopitch containing no impurities, the below-mentioned non-mesopitch (H, component 3.73%, B,
Ingredients 31.82%, Q, S.
成分６３．９５％、Ｑ．ｉ．成分０．５０９６） １０
０部を混合しプロパンガスを吹き込み攪拌しながら加熱
温度４００℃で２時間加熱処理しメソフェーズを４４．
５％含有するピッチを造り、この生成ピッチをプロパン
ガス下温度３２０℃で加時間熟成させ、ピッチ中のメソ
フェーズのみを融着巨大化させ、温度３２０℃で上層に
全くメソフェーズを含有せぬ非メソピッチ（Ｈ，成分３
．７３％、Ｂ、成分３１．８２％、Ｑ、 ８．成分６３
．９５％、Ｑ．ｉ．成分０．５０％）を下層に１００％
メソフェーズピッチ（Ｈ，成分２．６０％、Ｂ、成分１
８．８２％、Ｑ、 Ｓ、成分４８．６０％、Ｑ．ｉ．成
分２９．９８ ｅｓ ）とに比重の差に依シ画然と分ｊ
ＩＩｈＩ製し、この１００ ％メソフェーズピッチをヘ
プタンの溶剤で抽出して得られるラフィネートの１００
％メソフェーズピッチ（Ｈ０成分０．１６％、Ｂ、成分
１８．８５％、Ｑ、Ｂ、成分４８．６７俤、Ｑ．ｉ．成
分３２．３２％）を得ることができる。この高強度高弾
性炭素繊維製造用の原料のラフィネートの１００％メソ
フェーズピッチの軟化点は２５２℃、粘度は３２０℃で
１２４ポイズである。Ingredients: 63.95%, Q. i. Component 0.5096) 10
0 parts were mixed and heated at a heating temperature of 400°C for 2 hours while blowing propane gas and stirring to form a mesophase of 44.0 parts.
Pitch containing 5% is produced, and the resulting pitch is aged under propane gas at a temperature of 320°C for a time to fuse only the mesophase in the pitch to a large size. (H, component 3
．． 73%, B, component 31.82%, Q, 8. Ingredient 63
．． 95%, Q. i. component 0.50%) in the lower layer 100%
Mesophase pitch (H, component 2.60%, B, component 1
8.82%, Q, S, component 48.60%, Q. i. It clearly depends on the difference in specific gravity between component 29.98 es) and
100% of the raffinate obtained by extracting this 100% mesophase pitch with a solvent of heptane.
% mesophase pitch (H0 component 0.16%, B component 18.85%, Q, B component 48.67, Qi component 32.32%). The softening point of 100% mesophase pitch of raffinate, which is a raw material for producing this high-strength, high-modulus carbon fiber, is 252°C, and the viscosity is 124 poise at 320°C.
紡糸用のラフィネートの原料の１００％メン７エーズピ
′ツチを製造する際に使用する非メンピッチ（Ｈ，成分
３．７３％、Ｂ、成分３１．８２％、Ｑ、Ｓ、成分６３
．９５％、Ｑ．ｉ．成分０．５０優）には１００係メソ
フエーズピツチを製造するｌｉｍ！＆ｉｊ生する上層の
全くメソフェーズを含有せぬ非メンピッチを分離して之
に当てることが出来る。Non-men pitch (H, component 3.73%, B, component 31.82%, Q, S, component 63
．． 95%, Q. i. Ingredients 0.50%) is lim to produce 100 mesophase pitches! &ij The upper layer of non-mempic which does not contain any mesophase can be separated and applied thereto.
扁強度高弾性炭素繊維の原料の１００優メンフエーズピ
ツチの組成がＨ０成分、Ｂ、成分、Ｑ、 Ｓ、成分及び
Ｑ．ｉ．成分よシ桝成されていること依シ、原料の石油
系ピッチの組成のＨ６成分及びＢ、成分の加熱処理及び
熟成処理の工程の変化にともなう変遷を退％解明するこ
とに依シ常に物性の安定した１００ ％メソフェーズピ
ッチを造り、更にこれからＨ０成分のみを除去すること
に依夛、浴融紡糸性も極めて優れたものとなシ、これを
原料とする長繊維の炭素繊維は高強度超高弾性で全く画
期的物性を発揮することが出来る。The composition of 100-yellow phase pitch, which is a raw material for flat strength and high modulus carbon fiber, is H0 component, B component, Q, S component, and Q. i. The physical properties of the H6 and B components of the petroleum-based pitch used as a raw material depend on the composition of the raw material, and it is important to elucidate the changes caused by changes in the heat treatment and aging process of the components. By creating a stable 100% mesophase pitch and removing only the H0 component from it, it has extremely excellent bath melt spinnability, and the long fiber carbon fiber made from this as a raw material has high strength and ultra-high strength. It can exhibit completely innovative physical properties due to its elasticity.
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2460087AJPS63196721A (en) | 1987-02-06 | 1987-02-06 | Production of 100% mesophase for carbon yarn having high strength and high modulus of elasticity |
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2460087AJPS63196721A (en) | 1987-02-06 | 1987-02-06 | Production of 100% mesophase for carbon yarn having high strength and high modulus of elasticity |
| Publication Number | Publication Date |
|---|---|
| JPS63196721Atrue JPS63196721A (en) | 1988-08-15 |
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2460087APendingJPS63196721A (en) | 1987-02-06 | 1987-02-06 | Production of 100% mesophase for carbon yarn having high strength and high modulus of elasticity |
| Country | Link |
|---|---|
| JP (1) | JPS63196721A (en) |
| Publication | Publication Date | Title |
|---|---|---|
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