第84113356號專利申請案 中文説明書修正頁(S6年7月） A7 B7 修正 86.7：7?補充束”曰1 五、發明説明（ 經濟·邓中央標準局員工消費合作社印製 本發 備碳加工 性瀝青之 般化之碳 地包括溶 性瀝青之 最後 定化特徵 耗之後， 而不會熔 學不溶作 本發 化之碳加 除及加工 加工物所 另外，出 劑損耗之 成中間物 非髙度延 .明亦提供 物之方法 步驟，另 加工物爲 劑交換步 溶劑以較 ，本發明 之碳加工 接著形成 化。因此 甩之步驟 明提供在 工物，該 物之安定 需時間， 現於本發 後，接著 ，藉由與 伸的。 一種從成溶 。此方法包 外包括形成 碳纖維。製 驟，其中周 適合於製備 提供具有自 物。本發明 之加工物， ，本發明提 之碳加工物 高於成溶劑 碳加工物經 化作用之步 當與先前之 明之碳加工 形成加工物 加工物形成 劑化物 括製備 碳加工 備碳加 於製備 碳加工 身安定 之最佳 該加工 洪在碳 之各向 成溶劑 物之步 工物之 成溶劑 物之溶 化作周 碳加工 物可加 化作闬 同性瀝青丰製 化物之各向同 驟。目前最一 方法可選擇性 化物之各向同 劑取代。 或經改良之安 物爲在溶劑損 熱至碳化溫度 之前，不需化 (請先閱讀背面之注意事項再填寫本頁) 化物之瀝青之流體溫度安定 由加工物之形成，溶劑之移 驟。另外，本發明之安定碳 碳加工物比較時是較低的。 物之任何中間相傾向於在溶 。至於在加工物形成之後形 作用有關之應力，此中間物 圖式簡單說明 圖1係爲傳統瀝青與成溶劑化物之瀝青之氧化安定'化 作用之圖形比較。 本紙張尺度適用中國國家標準（CNS ) A4規格（2丨0X297公釐） 8 五、發明説明（1 ) 背景與摘要 此申請書係關於發明高熔點各向同性之瀝青能夠轉換 成爲成溶劑化物之各向同性之瀝青，藉以降低瀝青之實際 熔點。藉由此發明方法所製備之成溶劑化物之瀝青可紡成. 纖維，而需要些微或不需要安定化處理。 對於紡織傳統之非成溶劑化物之各向同性瀝青之方法 是眾所週知的。目前Ku re ha化學工業公司爲領導先驅，具 有每年9 0 0噸之能力。另外之製造商包括Ashland Oil 公司與KawasakiSteel公司。 各向同性碳纖維通常使用做爲混凝土結構之補强材料 。在此觀點，碳纖維必須比得上鋼及玻璃纖維。因此，.需 要提供碳纖維僅可能之最低成本。在製造碳纖維之方法中 ，最慢及成本最高之步驟爲在纖維碳化之前之做爲紡織之 纖維之安定化（通常由氧化進行）。安定化步驟是需要以 阻止纖維之熔化，在碳化過程期間，其所發生之溫度超過 經濟部中央標準局員工消費合作社印製 (請先閲讀背面之注意事項再填寫本頁) 3 5 0 °C且通常高於1 0 0 〇°C。爲了降低此步驟之時間 與成本，從高熔點瀝青中製造纖維是較佳的。然而，在本 發明之前，在紡織溫度之上熔化之瀝青是不可使用的。 因此，本發明之目的係提供一種製備碳纖維之方法， 該方法不需在安定化之前先氧化。另外，本發明提供一種 成溶劑化物之各向同性之瀝青，該瀝青具有流體溫度至少 4 0 °C，低於在非成溶劑化物之狀態中之相同瀝青之熔點 。另外，本發明提供一種可紡織成爲纖維之成溶劑化物之 瀝青，該瀝青在等於或大於紡織溫度之溫度下脫揮發作用 本紙張尺度適用中國國家標準（CNS ) Α·4規格（210Χ：297公釐） " ~~ — /1 — 經濟部中央標準局員工消費合作社印裂 Α7 Β7 五、發明説明（2 ) 與氧化安定化。 定義 在此申請書與專利範圍中所應用之術語如定義如下： '"瀝青"在此所使用係指由不同工業製備過程，例如 ，天然瀝青，石油瀝青與重油，所產生之副產物具有瀝青 性質之物質，及在石油脂裂解工業所獲得之副產物及從媒 中所獲得高碳成份之瀝青。 $石油瀝青"意指從石油蒸餾物或殘液之催化與熱裂 解中所獲得之殘餘含碳物質。 '"石油煤焦"意指從石油瀝青之高溫熱處理所得之固 態不溶解殘餘物。 "各向同性之瀝青"意指包含在光學上所排列之液態 結晶物中，分子不排爲一線之瀝青。 A非各向同性之瀝青〃或"中間物瀝青'意指包含經 由互相影響而一起組合以形成光學上排列之液態結晶物之 芳香族結構分子之瀝青，該瀝青不是液態就是固態，視溫 度而定。 A中間原"意指當熔解或熔化而形成中間物瀝青之分 子，其包含根據加熱而安排形成液體結晶物之大芳香族分 子之主要混合物。 、假中間原"意指可能之中間物前導之物質，但該物 質經加熱通常不會形成光學經排列之液體結晶物’但經加 熱將直接地形成固態煤焦，因此未見到熔解或熔化。 本紙張尺度適用中國國家標準（CNS ) Μ規格（210X297公釐） (請先閱讀背面之注意事項再填寫本頁) -1丨裝- 訂 A 7 _^_B7_' 五、發明説明（3 ) 對於成溶劑化物之瀝青之$流體溫度'係指成溶劑化 物之瀝青，從超過其熔點之溫度，以每分鐘1 °C之冷卻至 黏度爲6 0 0 0泊（poise)之溫度。若成溶劑化物之瀝 青之熔點易於決定，其總是低於流體溫度。·^成溶劑化物 之瀝青〃意指包含在_青中5至4 0重量％之間之瀝青， 該瀝青具有至少4 0°C之流體溫度，當不與溶劑關連時， 低於該瀝青成份之熔點。 *纖維"意指能夠形成爲有用之物件之纖維長度。 "定向分子結構"意指在所形成之含碳加工物中，中 間物範圍之排列，其排序相對於加工物之軸並提供對加工 物之結構性質。 當提到成溶劑化物之"溶劑含量"時，係指在溶劑之 眞空分離之重量損耗値0在此測定中，無吸入溶劑之樣本 或經分離溶劑之樣本正確地稱重之，在眞空烤箱中，於小 於5mm壓力，1 5 0°C之溫度下，壓碎並加熱1小時。 溶劑含量之百分比係重量損失或差異乘上1 〇 〇，除以原 始樣本之重量。 經濟部中央標準局員工消費合作社印製 (請先閱讀背面之注意事項再填寫本頁) '氧化作用/安定化作用'係藉由加工物與氧或氧化 劑反應，而使得瀝青加工物不可熔化或不可熔解之過程。 "軟化點與熔點"係在惰性氣體之下，在熱階段顯微 鏡上以約5 °C /分鐘加熱樣本所決定之。對於經乾燥之瀝 青之軟化點係指瀝青顆粒之角特徵首度磨圓之溫度。而對 於經乾燥之瀝青之熔點係指經軟化之瀝青可看到首先流動 之溫度。 本紙張尺度適用中國國家標準（CNS ) Μ規格（210X297公釐） η B7 五、發明説明（4 ) 本發明之簡要說明 此發明提供一種成溶劑化物之各向同性之瀝青及一種 製備成溶劑化物之各向同性瀝青之方法。另外，此發明提 供具有唯一安定化性質及高熔化溫度之低成本碳加工物。 另外，本發明提供所出現之任何中間物範圍沿著纖維之軸 不是高度地延伸或延長之碳纖維。 一種典型之製備成溶劑化物之各向同性之瀝青之方法 ，該瀝青包含一起混合成份而形成可溶解之溶劑相及不可 溶之瀝青相。較佳之混合過程是發生於足夠維持所有相在 液體狀態之溫度，之後該系統允許沈澱。在系統沈澱期.間 ，發生相分離。在相分離之後，在不致於破壞成溶劑化物 之各向同性瀝青之條件下，藉由移除液體溶劑相而回收成 溶劑化物之各向同性瀝青。 經濟部中央標準局員工消費合作社印製 (請先閱讀背面之注意事項再填寫本頁) 本發明之成溶劑化物之各向同性瀝青具有小於4 0體 積％之光學各向異性（中間物）。然而，應瞭解乾燥瀝青 而移除溶劑可產生額外之中間物。另外，本發明之成溶劑 化物之各向同性瀝青具有至少4 0 °C之流體溫度，低於未 具有溶劑之相同瀝青之熔點。另外，本發明之成溶劑化物 之各向同性瀝青具有至少5 0重量％甲苯不可溶物。最後 ，視進料瀝青之組成物而定，本發明之成溶劑化物之各向 同性瀝青不是1 )在溶劑移除之後即自動地自身具有安定 作用，就是2 )在相當短之時間週期中，在高於其流體溫 度之溫度下安定化。 本紙張又度適用中國國家標準（CNS ) A4規格（210X297公釐） 第84113356號專利申請案 中文説明書修正頁(S6年7月） A7 B7 修正 86.7：7?補充束”曰1 五、發明説明（ 經濟·邓中央標準局員工消費合作社印製 本發 備碳加工 性瀝青之 般化之碳 地包括溶 性瀝青之 最後 定化特徵 耗之後， 而不會熔 學不溶作 本發 化之碳加 除及加工 加工物所 另外，出 劑損耗之 成中間物 非髙度延 .明亦提供 物之方法 步驟，另 加工物爲 劑交換步 溶劑以較 ，本發明 之碳加工 接著形成 化。因此 甩之步驟 明提供在 工物，該 物之安定 需時間， 現於本發 後，接著 ，藉由與 伸的。 一種從成溶 。此方法包 外包括形成 碳纖維。製 驟，其中周 適合於製備 提供具有自 物。本發明 之加工物， ，本發明提 之碳加工物 高於成溶劑 碳加工物經 化作用之步 當與先前之 明之碳加工 形成加工物 加工物形成 劑化物 括製備 碳加工 備碳加 於製備 碳加工 身安定 之最佳 該加工 洪在碳 之各向 成溶劑 物之步 工物之 成溶劑 物之溶 化作周 碳加工 物可加 化作闬 同性瀝青丰製 化物之各向同 驟。目前最一 方法可選擇性 化物之各向同 劑取代。 或經改良之安 物爲在溶劑損 熱至碳化溫度 之前，不需化 (請先閱讀背面之注意事項再填寫本頁) 化物之瀝青之流體溫度安定 由加工物之形成，溶劑之移 驟。另外，本發明之安定碳 碳加工物比較時是較低的。 物之任何中間相傾向於在溶 。至於在加工物形成之後形 作用有關之應力，此中間物 圖式簡單說明 圖1係爲傳統瀝青與成溶劑化物之瀝青之氧化安定'化 作用之圖形比較。 本紙張尺度適用中國國家標準（CNS ) A4規格（2丨0X297公釐） 8 A7 B7 五、發明説明（6 ) 太發明之詳細發明 .I .成溶劑化物之各向同性瀝青之製備 經濟部中央標準局員工消費合作社印製 (請先閲讀背面之注意事項再填寫本頁) 成溶劑化物之各向同性瀝青之製備一開始選擇適合之 進料瀝青。適合使用於本發明之瀝青將具有約8 8重量％ 至9 6重量％之碳，至多約1 2重量％之氫及不超過6重 量％之硫，氧，氮或其他成份之組成。較佳爲該瀝青分子 之主要部份爲芳香族。另外，該瀝青應具有低濃度之流動 不可溶物。而較佳爲該瀝青具有小於2 0 %之流動不可溶 物。若需要時，在成溶劑化之前或之後過濾該瀝青而達到 適當不可溶物之等級。該瀝青與有機助溶劑，如：甲苯， 氯仿或四氫呋喃，溶化，接著進行溶化之不可溶物質之物 性分離。這些流動之不可溶物典型上包含如灰與無機化合 物之瀝青雜質。在一些例子中，非常高熔化之有機化合物 亦可做爲流動之不可溶物而移除之。通常，具有小於3 0 重量％喹啉不可溶物（Q I )之瀝青將是適當的；然而， 較佳之瀝青應具有介於〇重量％與1 〇重量％之間之Q I 。典型上，這些瀝青具有約從1 0 〇°C至約3 0 0 °C之熔 點範圍。 對於適當瀝青之另一參數爲在溶劑中，例如：甲苯， 之不溶解程度。一般，該瀝青必須包含至少5重量％之甲 苯不可溶物而產生成溶劑化物之各向同性之瀝青產物。較 佳鳥該瀝青將包含至少2 0重量％之甲苯不可溶物。與流 動之不溶解物比較，甲苯不可溶物通常爲需要較濃'溶劑而 變成可溶解化之有機化合物。符合上述要求之瀝青包括合 本紙張尺度適用中國國家標準（CNS ) A4規格（210><297公釐） 經濟部中央標準局員工消費合作社印製 A7 B7 五、發明説明（7 ) 成物質，媒，石油與乙烯焦油瀝青。商業上可購買到之瀝 青包括Ash land A240瀝青，經加熱處理之Ashland A240與 Ashland Aerocarb瀝青。 適當之成溶劑化溶劑之選擇在本發明中晕相當重要的 。典型上適合之溶劑具有溶解度參數範圍爲8. 0至 1 1 . 0。術語*溶解度參數"定義爲 1姻 其中H v : =蒸發熱 R =莫耳氣體常數 Τ =溫度（°κ ) V =莫耳體積 對於溶解度參數之討論請參考非電解質之溶解度 olubilitv of Nnn-Electrolvtes), 1948， J. Hildebra. nd與R . Scott，在此合併做爲參考。在本發明中所發現之 有用溶劑包括：苯，甲苯，二甲苯，四氫某。另外，其他 取代性芳香族溶劑，如，雜芳香族（例如：喹啉與吡陡） 及1至3環芳香族化合物及其部份氫化或烷基化之衍生物 可使用於本發明。取代之芳香族之芳香族調和物與鏈烷烴 溶劑，如：庚烷，在本發明中亦適合。一般，合適之溶劑 將產生四分之一至二倍重瀝青不可溶解物量（由甲苯所製 備之重瀝青不可溶解物量）。對於本發明之目的，溶解度 係由結合一克之瀝青與2 5 m Θ之溶劑在室溫中所量測出 本紙張尺度適用中國國家標準（CNS ) A4規格（210 X 297公釐）_ (請先閱讀背面之注意事項再填寫本頁) :裝. 訂 A7 _ B7 f 丨 五、發明説明（8 ) 〇 本發明之方法，結合如上所述之瀝青與溶劑，提供一 種成溶劑化物之各向同性瀝青。根據本發明之方法，該各 向同性之瀝青在約1小時之週期中，於足夠轉換在混合物 中之所有相轉變爲液態之溫度下及在足夠阻止沸騰之壓力 下與溶劑混合之。在混合之後，沈澱與冷卻該瀝青/溶劑 系統。在此步驟期間，發生相分離，產生液態溶劑相與成 溶劑化物之瀝青相。依設備而定，沈澱之完成時間約5至 3 0分鐘。若需要，可使甩如離心之機械方法而加速相分 離。在相分離之後，所回收之成溶劑化物之瀝青不是液態 就是可冷卻該混合物之液體，而所回收之瀝青係爲沈澱.固 體。在任何一個例子中，較方便之回收方法將是適合的， 例如：輕輕倒出該液態相或過濾而移除固態成溶劑化物之 瀝青。在液體狀態中可連續地回收成溶劑化物之瀝青與溶 劑相。若需要可過濾在液體狀態中之經回收成溶劑化物之 瀝青而移除污染物。 經濟部中央標準局員工消費合作社印製 (請先閱讀背面之注意事項再填寫本頁) 藉由形成各向同性進料瀝青與溶劑之相同結合（在較 低之溫度下，使得溶劑相爲液體而成溶劑化物之瀝青相爲 固體）而獲得成溶劑化物之瀝青。當使用此方法時，該固 體成溶劑化物之瀝青可由傳統之方法，例如過濾，而回收 之。 成溶劑化物之瀝青之非揮發部份之性質可在約1 5 0 °C之溫度下，藉由乾燥該成溶劑化物之瀝青約6 0分鐘而 移除溶劑而量測之。在乾燥瀝青之後，藉由在惰性氣壓之 本紙張尺度適用中國國家標準（CNS ) A4規格（210X297公釐） 經濟部中央標準局員工消費合作社印製 A7 __B7_' ' 五、發明説明（9 ) 下，以約5 °C/分鐘速率之熱階段顯微鏡上加熱而決定軟 化點與熔點。在溶劑移除之後，正常之下，本發明之瀝青 將具有至少2 8 0 °C之軟化點。在大於5 0 0 °C之溫度下 •，較硬之經乾燥之瀝青將軟化；然而，當在惰性氣體中， 以5 °C /分鐘加熱時，這些瀝青將不會熔化。.這些瀝青被 認爲是自身安定化，因此其在連續加熱時，將直接碳化至 碳加工品上。 II .成溶劑化物之各向同性瀝青 ‘ 本發明之成溶劑化物之各向同性瀝青提供幾種超過非 成溶劑化物之各向同性瀝青之重要利益。一般，成溶劑化 物之瀝青將包含從約5重量％至約4 Q重量％之溶劑。另 外，該成溶劑化物之瀝青具有至少5 0重量％之甲苯不可 溶物且可能由至多4 0體積％之光學各向異性所組成。一 旦從該瀝青中移除溶劑，各向異性之成份可增加之。本發 明之成溶劑化物之各向同性之瀝青具有至少4 0 °C，在一 些例子中超過1 0 0°C之流體溫度，低於在非成溶劑化物 之狀態中意即，乾燥瀝青，相同瀝青之熔點。 III .製備碳加工物之方法 本發明另外提供一種從成溶劑化物之各向同性之瀝青 中製造碳加工物之方法。特別是本發明提供一種從成溶劑 化物之各向同性之瀝青中製造碳纖維之方法。從成溶劑化 物之各向同性之瀝青中製造碳加工物之方法係從成溶劑化 本紙張尺度適用中國國家標隼（CNS ) A4规格（210X2.97公釐） (請先閲讀背面之注意事項再填寫本頁) 袭- 訂 12 I. 經濟部中央標準局員工消費合作社印製 A 7 _____£7_， ， 五、發明説明（10 ) 物之各向同性之瀝青開始。 視所形成之加工物及用以媒合瀝青所使用之溶劑而定 ，該製造方法可要求以適合於本製備方法之溶劑代替媒合 •瀝青。此步驟爲已知之溶劑交換，可由幾種方法達成。一 種方法：要求乾燥成溶劑化物之瀝青而趕走溶劑，接著以 合適之溶劑再媒合該瀝青。而另一種方法提供添加一種具 有高於起始媒合瀝青之沸點之溶劑至成溶劑化物之瀝青中 。然後，加熱此混合物至沸騰而移除較低沸點之溶劑（從 包含較髙沸點溶劑之成溶劑化物之瀝青中離開）。不管何 種方法，典型之製造溶劑將具有約8至約12且可能更高 之溶解度參數。該製造溶劑（非消耗性地）可包括下列溶 劑之一或多種溶劑：甲苯，苯，二甲苯，四氫萘，四氫呋 喃，氯仿，庚烷，吡啶，喹嚀，經鹵化之苯，氯氟苯，及 2至4環芳香族之溶劑，及其部份烷圖化與氫化之衍生物 Ο 一旦該成溶劑化物之瀝青包含一種適合該製造方法之 溶劑，其可藉由在此技藝中已知之方法形成爲碳加工物。 目前，最普通之碳加工物爲碳纖維。 在從成溶劑化物之瀝青中紡織碳纖維之方法中，部份 溶劑將從產品纖維中遺失。在拉絲之後，任何剩餘之溶劑 藉由乾燥纖維而立即移除。溶劑之損失產生具有至少 2 8 0 °C軟化點之碳纖維。另外，所得之纖維將具有高於 纖維之拉絲溫度之熔點。最終，視起始化之進料瀝青而定 ，所得之纖維在碳化之前將不需要額外之處理。 本紙張尺度適用中國國家標準（CNS ) A4規格（210X297公釐） (請先閲讀背面之注意事項再填寫本頁) ...裝. -訂_ 經濟部甲夬標準局員工消費合作社印製 A7 ______B7_ ' 1 五、發明説明（11 ) 具有大於3 5 0 °C開始溫度之軟化溫度之經乾燥纖維 不需在碳化之前先安定化作用。而較佳之纖維爲具有高於 5 0 0 °C之軟化點。在溫度些微低於纖維之軟化點時，加 熱纖維而達成碳化作用。至於纖維發展之碳化作用，纖維 之軟化溫度上昇，允許碳化反應之溫度相對增加。然而， 在碳化反應期間，該纖維從來不會加熱超過其軟化點。對 於具有高於5 0 0 °C軟化點之纖維可在每分鐘2 0 °C之上 昇或更快但不會軟化該纖維之速率下加熱。一般，在 6 0 0 °C加熱，碳化作用完成之。然而，可在甚至較高之 溫度下處理該纖維。 對於具有約2 8 0 °C至5 0 0 °C之間之軟化點之瀝青 ，在碳化之前較佳進行氧化安定化作用。另外，在某些環 境之下，可能需要氧化安定化具有高於5 0 0 °C軟化點之 瀝青。 本發明之一利益爲在相對高溫與低氧濃度中，能夠快 速地氧化安定瀝青且/或由該瀝青所製成之碳加工物。更 明確而言，安定化作用可在高於加工物形成溫度之溫度下 及包含低於5 %氧之大氣中完成之。本發明超過先前氧化 安定化作用之方法之利益由例2與圖1論證之。圖1比較 一種傳統瀝青與成溶劑化物之瀝青之氧化安定化作用。如 圖1之論證，在氧化安定化作用之前，成溶劑化物之瀝青 不需冷卻，且安定化作用發生於較高溫度較短週期時間。 因此，本發明提供一種重要之安全利益，其安全性超過在 氧化安定化作用時藉由排除燃燒危險性之先前技藝。 本紙張尺度適用中國國家標準（CNS ) A4規格（210 X 297公釐） (請先閲讀背面之注意事項再填寫本頁) 1 裝^-------訂------^冒---^---- A7 B7 經濟部中央標準局員工消費合作社印製 五、發明説明（12) IV .從成溶劑化物之瀝青中形成碳纖維 本發明之以瀝青拉絲之纖維總是在成溶劑化物之瀝青 拉絲溫度之上熔化。在溶劑移除之後，本發明之纖維典型 上爲不可熔的。結果，本發明之纖維時常在碳化之前不需 化學安定化。然而在一些情況是需要安定化作用：在僅包 含約2 %至5 %氧之大氣下，在足夠短之週期時間進行時 是需要安定化作用。 一旦經拉絲之纖維碳化，本發明之碳纖維可從連續各 向同性至連續各向異性變化之。然而，出現在這些纖維中 任何各向異性區域之主要部份不具有中間物瀝青碳纖維之 髙度延長範圍特徵。這些纖維具有相當於傳統各向同性瀝 青纖維之張力强度。爲了達成包含各向異性區域之纖維程 度，與完全各向同性之纖維比較，其具有經改良之熱與電 特性。 下列例子用以說明本發明。除非特別指定，否則所有 之份與百分比均爲重量。申請者不希望出現之例子而限制 該理論，本發明之眞實範圍係以所附之申請專利範圍爲原 則。 例1 在經攪拌之壓力鍋^中，以每8 c c溶劑1 g瀝青之比 例，混合A 2 4 0均質瀝青樣本（8重量％甲苯不可溶物 :商業上可從 Ashland Chemical 公司，Columbus, Ohio 購 本紙張尺度適用中國國家標準（CNS )八4規格（210X 297公釐） (請先閱讀背面之注意事項再填寫本頁) -裝· 訂 經濟部中央標準局員工消費合作社印裝 A7 B7 五、發明説明（13) 得）與甲苯。在壓力鍋中灌入氮，短暫地排放並密封。在 8 〇分鐘之期間，加熱該混合物直至達到2 3 3 °C之溫度 。該混合物保持在2 3 3 °C1 0分鐘並攪拌之。該混合物 再保持在2 3 3 °C 1 5分鐘但不需攪拌，然後冷卻之。在 加熱期間，在密閉之壓力鍋中所產生之最大壓力爲1 7 5 ps i g 〇 從壓力鍋之底部回收固體瀝青，經計算該瀝青之產出 率爲6 . 4 %。由光學顯微鏡分析所述之瀝青，發現在小 球體之形式中包含5 %中間物。 在眞空之下，藉由在3 6 0 °C加熱3 0分鐘乾燥固體 瀝青樣本。此步驟從骸瀝青中移除2 8 . 2%之揮發物.。 在顯微鏡熱階段於氮氣之下，以每分鐘增加5 °C之加熱速 率加熱至6 5 0 °C，該經乾燥之瀝青不會軟化或熔化。 例2 以1 g瀝青對8πιθ甲苯之比例，結合Aerocarb 80 (3 0重量％甲苯不可溶物）與甲苯而製備成溶劑化物之 瀝青。在2 3 0 °C攪拌該混合物1小時，允許沈澱1 5分 鐘，然後冷卻之。從容器底部回收濃密固體之成溶劑化物 之瀝青層，產出率爲5 4%。該成溶劑化物之瀝青充分地 均質，僅具有5至1 0||積％非等方向性之細緻球體型式 與部份較大球體。 在眞空之下，在1 5 0°C乾燥成溶劑化物之瀝青樣1 小時以移除溶劑。接著之乾燥，該瀝青損失22 .1重量 本紙張尺度適用中國國家標準（CNS)A4規格（ 210X297公釐）_ (請先閲讀背面之注意事項再填寫本頁) :,-r7~-... >}/ 、 -I-11--1 I —1 I —衣· — I I I I 訂 I I I I --- 經濟部中夬標準局員工消費合作社印製 A7 __B7__' ' 五、發明説明（l4 ) %。在眞空之下，進一步加熱瀝青至3 6 0 °c而移除另外 之4 . 9 %揮發物。此額外損耗似乎是因任何剩餘溶劑之 移除及一些輕油之損耗。分析此樣本顯示總共5 2體積％ 之不等向性。此論証成溶劑化物之各向同性涯青因溶劑之 損失而產生額外之不等向性。 成溶劑化物之均質瀝青之流體溫度在小壓力鍋中藉由 量測攪拌阻抗而決定之。甲苯成溶劑化物之瀝青之部份加 熱至超過其流體溫度之溫度，在此例爲2 3 5 ，然後緩 慢地以約每分鐘1 °C冷卻之。使用此方法，該甲苯成溶劑 化物之瀝青在1 9 1°C達到6 0 0 Opoise之黏度。因此 ，成溶劑化物之瀝青之流體溫度爲4 2 °C，低於Aero car b 進料瀝青之熔點。 後來，經由使用熱階段顯微鏡而決定在移除溶劑之後 ，成溶劑化物之瀝青之溶劑與軟化點。如先前所定義，軟 化發生於瀝青顆粒之尖銳角首先變圓之時機。當看到經軟 化之瀝青之首次可觀察到之流動時，即發生熔化。使用這 些程序與定義，經乾燥之成溶劑化物之瀝青在3 2 3 °C軟 化，在3 2 8 °C熔化。經乾燥之成溶劑化物之瀝青之熔點 爲9 5°C，較高於Aerocarb 8 0進料瀝青。値得注目地 ，在經乾燥之成溶劑化物之瀝青與成溶劑化物之瀝青之流 體溫度之間之熔點差異，在此實驗中至少爲1 3 7°C。 爲了論証經乾燥之非成溶劑化物之瀝青之改善安定化 特徵，氧化經乾燥之成溶劑化物之瀝青樣本與A e r 〇 c a r b 8 0。二種瀝青樣本碾碎成1 0至2 0 〇微米之顆粒，並 本紙張尺度適用中國國家標準（CNS ) A4規格（210 X 297公釐）_ ·! (請先閲讀背面之注意事項再填寫本頁) ----------1---Γ---裝----I"-訂----- A 7 _B7___' 1 五、發明説明（15) 在近乎2 0 °C之溫度（低於其軟化點）氧化3 0分鐘。氧 也氣體爲在氮中2 %氧。因此’.Aer〇carb 8 0進料瀝青 在2 0 5 °C氧化，而經乾燥之成溶劑》化物之瀝青在3 0 0 °C氧化。接著氧化，在氮之下，以每分鐘增高5 °c之方式 加熱而決定每一種瀝青之軟化點與熔點。經安定化之“!·-0 c a r b在2 5 0 °C軟化，在2 5 4 °C熔化，意即在未安定 化之瀝青上有2 2 °C之改善。成對比的是，經安定化之成 溶劑化物之瀝青並未熔化，且僅有2 G %之樣本顯示在加 熱至6 5 0 °C時，軟化之任何證據。很明顯地，在經安定 化之進料瀝青上，經安定化之成溶劑化物之瀝青具有足夠 之改良熱特徵。成溶劑化物之瀝青對未成溶劑化物之瀝青 之特徵比較，由下列提供之。 (請先閱讀背面之注意事項再填寫本頁) 裝· 訂 經濟部中央標隼局員工消費合作社印製 本紙張又度適用中國國家標準（CNS ) A4規格（210 X297公釐） -18 - 五、發明説明（16) 表1 經濟部中央標準局員工消費合作社印製Revised Page of Chinese Specification for Patent Application No. 84113356 (July S6) A7 B7 Amendment 86.7: 7? Supplementary Bundle "1) V. Invention Description (Printed by the Economic and Deng Central Bureau of Standards, Consumer Cooperatives, and issued carbon processing The normalized carbon land of the bitumen includes the finalized characteristics of the soluble bitumen, but it will not melt insoluble as the carbon of the present chemical addition and processing and processing. In addition, the output loss of the intermediate is not delayed. The method and steps of the object are also provided, and the processed object is a solvent exchange step. The carbon processing of the present invention is then formed. Therefore, the step of rejection is provided for the working object, and the stability of the object requires time. After that, by and stretching. A method of dissolving. This method includes the formation of carbon fibers. The manufacturing step is suitable for preparing and providing a self-made product. The processed product of the present invention, and the carbon processed product of the present invention. Steps higher than the chemical conversion of the solvent-forming carbon processed product. When forming the processed product with the previously known carbon, the processed product forming agent includes the preparation of carbon, the preparation of carbon, and the addition of prepared carbon. The stability of the work body is the best. The dissolution of the solubilized material of the stepwise solubilized material in the carbon can be added to the isotropic bitumen isotropic step. One method can be used to replace the isotropic agent of the selected compound. Or the modified compound is not required before the solvent heat loss to the carbonization temperature (please read the precautions on the back before filling this page). Stability is caused by the formation of the processed product and the shift of the solvent. In addition, the stable carbon-carbon processed product of the present invention is relatively low in comparison. Any mesophase of the material tends to dissolve. As for the stress related to the deformation after the processed product is formed This intermediate diagram is a simple illustration. Figure 1 is a graphical comparison of the oxidation stability of traditional asphalt and solvated asphalt. This paper size applies the Chinese National Standard (CNS) A4 specification (2 丨 0X297 mm) 8 V. Description of the Invention (1) Background and Abstract This application is about the invention of high melting point isotropic asphalt which can be converted into solvate isotropic asphalt to reduce The actual melting point of low bitumen. The solvated bitumen prepared by the method of the present invention can be spun into fibers. It requires little or no stabilization. For the traditional method of spinning non-solvated isotropic bitumen, It is well known. Currently Ku re ha Chemical Industries is a leading pioneer with a capacity of 900 tons per year. Other manufacturers include Ashland Oil and Kawasaki Steel. Isotropic carbon fibers are often used as reinforcing materials for concrete structures. In this view, carbon fiber must be comparable to steel and glass fiber. Therefore, it is necessary to provide the lowest possible cost of carbon fiber. In the method of manufacturing carbon fiber, the slowest and most costly step is to make the textile before the carbonization of the fiber. The stabilization of the fibers (usually by oxidation). The stabilization step is required to prevent the fibers from melting. During the carbonization process, the temperature that has occurred exceeds the printing of the Consumer Cooperatives of the Central Standards Bureau of the Ministry of Economic Affairs (please read the precautions on the back before filling out this page) 3 5 0 ° C And usually higher than 1000 ° C. In order to reduce the time and cost of this step, it is preferred to make fibers from high melting point asphalt. Prior to the present invention, however, asphalt that melted above the textile temperature was not available. Therefore, an object of the present invention is to provide a method for preparing carbon fibers, which method does not require oxidation before stabilization. In addition, the present invention provides a solvated isotropic pitch that has a fluid temperature of at least 40 ° C, which is lower than the melting point of the same pitch in a non-solvated state. In addition, the present invention provides a solvated bitumen that can be woven into fibers. The bitumen is devolatilized at a temperature equal to or greater than the textile temperature. This paper is sized to the Chinese National Standard (CNS) A · 4 (210 ×: 297). (%) &Quot; ~~ — / 1 — Employee Consumer Cooperatives of the Central Bureau of Standards, Ministry of Economic Affairs, printed A7 B7 V. Invention Description (2) and Oxidation Stabilization. Definitions The terms used in this application and the scope of the patent are defined as follows: "" asphalt " as used herein refers to by-products produced by different industrial processes, such as natural asphalt, petroleum asphalt and heavy oil Substances with asphaltic properties, as well as by-products obtained in the petroleum cracking industry and asphalts with high carbon content obtained from media. "Petroleum pitch" means a residual carbonaceous material obtained from the catalytic and thermal cracking of petroleum distillates or raffinates. '" Petroleum coal coke " means a solid insoluble residue obtained from the high temperature heat treatment of petroleum pitch. " Isotropic pitch " means pitch that is not lined up by molecules that are contained in liquid crystals arranged optically. A non-isotropic asphalt or "intermediate asphalt" means an asphalt containing aromatic structure molecules that are combined together to form optically arranged liquid crystals through mutual influence. The asphalt is either liquid or solid, depending on temperature It depends. A Intermediate " means a molecule that, when melted or melted to form an intermediate pitch, contains a major mixture of large aromatic molecules arranged to form liquid crystals upon heating. "False intermediate" means a possible precursor of the intermediate, but the substance usually does not form optically aligned liquid crystals when heated. However, it will directly form solid coal char after heating, so no melting or melt. This paper size applies Chinese National Standard (CNS) M specifications (210X297 mm) (Please read the precautions on the back before filling out this page) -1 丨 Packing-Order A 7 _ ^ _ B7_ 'V. Description of the invention (3) For The "fluid temperature of solvated asphalt" refers to solvated asphalt, which is cooled from a temperature exceeding its melting point at a temperature of 1 ° C per minute to a temperature of 6 00 poise. If the melting point of the solvated bitumen is easily determined, it is always below the temperature of the fluid. ^ Solvent-containing bitumen means bitumen comprised between 5 and 40% by weight of cyanine, the bitumen has a fluid temperature of at least 40 ° C, and when not associated with a solvent, is lower than the bitumen composition Of melting point. * Fiber " means the length of fiber that can be formed into a useful article. " Oriented molecular structure " means an arrangement of intermediate ranges in the formed carbon-containing processed product, the order of which is relative to the axis of the processed product and provides structural properties to the processed product. When referring to " solvent content " as a solvate, it refers to the weight loss of air separation in the solvent. In this measurement, the sample without inhaled solvent or the sample with separated solvent is weighed correctly. In an empty oven, crush and heat for 1 hour at a pressure of less than 5mm and a temperature of 150 ° C. The percentage of solvent content is the weight loss or difference multiplied by 100 and divided by the weight of the original sample. Printed by the Consumer Cooperatives of the Central Standards Bureau of the Ministry of Economic Affairs (please read the precautions on the back before filling this page) 'Oxidation / stabilization' is the reaction of the processed product with oxygen or oxidant, which makes the processed asphalt not meltable or Indissolvable process. " Softening point and melting point " is determined by heating the sample at about 5 ° C / min on a microscope in a hot stage under an inert gas. For the dried bitumen, the softening point refers to the temperature at which the angular characteristics of the asphalt particles are first rounded. The melting point for dried asphalt is the temperature at which the softened asphalt can be seen to flow first. This paper size applies Chinese National Standard (CNS) M specifications (210X297 mm) η B7 V. Description of the invention (4) Brief description of the invention This invention provides a solvate-based isotropic pitch and a solvate prepared Method of isotropic asphalt. In addition, this invention provides a low-cost carbon processed product having unique stabilization properties and a high melting temperature. In addition, the present invention provides any intermediate range of carbon fibers that does not extend or extend highly along the fiber axis. A typical method for preparing solvate-containing isotropic asphalt, which comprises mixing components together to form a soluble solvent phase and an insoluble asphalt phase. The preferred mixing process occurs at a temperature sufficient to maintain all phases in a liquid state, after which the system allows precipitation. During the precipitation period of the system, phase separation occurred. After the phase separation, the solvated isotropic pitch is recovered by removing the liquid solvent phase under conditions that do not destroy the solvated isotropic pitch. Printed by the Consumer Cooperative of the Central Bureau of Standards of the Ministry of Economic Affairs (please read the notes on the back before filling this page) The solvated isotropic pitch of the present invention has an optical anisotropy (intermediate) of less than 40% by volume. However, it should be understood that drying the asphalt and removing the solvent can create additional intermediates. In addition, the solvated isotropic pitch of the present invention has a fluid temperature of at least 40 ° C, which is lower than the melting point of the same pitch without the solvent. In addition, the solvated isotropic pitch of the present invention has at least 50% by weight of toluene-insoluble matter. Finally, depending on the composition of the fed bitumen, the solvated isotropic bitumen of the present invention is either 1) after the solvent is removed, it automatically has a stabilizing effect itself, or 2) in a relatively short period of time, Stabilizes at temperatures above its fluid temperature. This paper is again applicable to the Chinese National Standard (CNS) A4 specification (210X297 mm) No. 84113356 Patent Application Chinese Manual Revised Page (S6 Jul) A7 B7 Amended 86.7: 7? Supplementary Bundle "1 Explanation (Economy · Deng Central Bureau of Standards Consumer Consumption Co., Ltd. prints the general carbon of the prepared carbon processable asphalt, including the finalization characteristics of the soluble asphalt, and does not melt and dissolve as the carbon of the local chemical. In addition to the processing and processing of the product, the loss of the output agent into the intermediate is not delayed. Ming also provides the method steps of the product, and the other product is the agent exchange step solvent. The carbon processing of the present invention is then formed. The steps clearly provide the work piece, the stability of the thing takes time, now after the hair, and then with the extension. A solution from the solution. This method includes the formation of carbon fiber. Production steps, which are suitable for preparation and supply It has its own object. The processed product of the present invention, the carbon processed product mentioned in the present invention is higher than the chemical conversion of the solvent-processed carbon processed product. The processed material forming agent includes the preparation of carbon processing, the preparation of carbon, and the stability of the preparation of carbon processing body. The isotropic step of turning into a homogeneous bituminous compound. At present, the most common method is to replace the isotropic agent of the selective compound. Or the modified compound is not required until the solvent heats up to the carbonization temperature (please first Read the notes on the reverse side and fill in this page) The stability of the fluid temperature of the asphalt of the compound is formed by the processed product, and the solvent is shifted. In addition, the stable carbon-carbon processed product of the present invention is relatively low in comparison. Any mesophase Tends to dissolve. As for the stress related to the deformation after the processed product is formed, this intermediate diagram briefly illustrates Figure 1 is a graphical comparison of the oxidation stabilization of traditional asphalt and solvated asphalt. This paper is applicable to this paper. Chinese National Standard (CNS) A4 specification (2 丨 0X297 mm) 8 A7 B7 V. Description of invention (6) Detailed invention of the invention. I. Isotropic isotropy Printed by the Consumer Cooperative of the Central Standards Bureau of the Ministry of Economics and Preparation (please read the precautions on the back before filling this page). The preparation of isotropic asphalt that is solvated initially selects a suitable feed asphalt. Suitable for use in the present invention The pitch will have a composition of about 88% to 96% by weight of carbon, up to about 12% by weight of hydrogen and not more than 6% by weight of sulfur, oxygen, nitrogen, or other components. Preferably, the pitch molecules are The main part is aromatic. In addition, the asphalt should have a low concentration of mobile insolubles. It is preferred that the asphalt has a mobile insoluble of less than 20%. If necessary, it is filtered before or after solvation. The bitumen reaches the level of appropriate insoluble matter. The bitumen is dissolved with an organic co-solvent, such as toluene, chloroform or tetrahydrofuran, followed by physical separation of the dissolved insoluble matter. These flowing insolubles typically contain pitch impurities such as ash and inorganic compounds. In some cases, very high melting organic compounds can also be removed as flowing insolubles. Generally, pitches having less than 30% by weight of quinoline insoluble matter (Q I) will be appropriate; however, preferred pitches should have Q I between 0% and 10% by weight. Typically, these pitches have a melting point range from about 100 ° C to about 300 ° C. Another parameter for a suitable pitch is the degree of insolubility in a solvent, such as toluene. Generally, the bitumen must contain at least 5% by weight of toluene insolubles to produce an isotropic pitch product that becomes a solvate. Preferably, the asphalt will contain at least 20% by weight of toluene-insoluble matter. Compared with flowing insolubles, toluene insolubles usually require more concentrated solvents to become soluble organic compounds. Asphalts that meet the above requirements include the Chinese paper standard (CNS) A4 specification (210 > < 297 mm) for the paper size. A7 B7 printed by the Consumer Cooperatives of the Central Standards Bureau of the Ministry of Economic Affairs. Medium, petroleum and ethylene tar pitch. Commercially available bitumen includes Ash land A240 asphalt, heat treated Ashland A240 and Ashland Aerocarb asphalt. The selection of a suitable solvating solvent is very important in the present invention. Typically, suitable solvents have a solubility parameter ranging from 8.0 to 1 1.0. The term * solubility parameter is defined as 1 where H v: = heat of evaporation R = Mohr gas constant T = temperature (° κ) V = Mohr volume For a discussion of solubility parameters, please refer to the non-electrolyte solubility olubilitv of Nnn- Electrolvtes), 1948, J. Hildebra. Nd and R. Scott, incorporated herein by reference. Useful solvents found in the present invention include: benzene, toluene, xylene, tetrahydrogen. In addition, other substituted aromatic solvents such as heteroaromatics (e.g., quinoline and pyridoxine) and 1 to 3 ring aromatic compounds and their partially hydrogenated or alkylated derivatives can be used in the present invention. Substituted aromatic aromatic blends and paraffin solvents such as heptane are also suitable in the present invention. In general, a suitable solvent will produce a quarter to twice the amount of heavy asphalt insoluble matter (the amount of heavy asphalt insoluble matter prepared from toluene). For the purpose of the present invention, the solubility is measured at room temperature by combining one gram of asphalt and a solvent of 25 m Θ at room temperature. This paper is sized to the Chinese National Standard (CNS) A4 (210 X 297 mm) _ (Please Read the notes on the back before filling this page): Pack. Order A7 _ B7 f 丨 V. Description of the invention (8) 〇 The method of the present invention combines the asphalt and the solvent as described above to provide a solvate-oriented solution Homosexual asphalt. According to the method of the present invention, the isotropic pitch is mixed with a solvent at a temperature sufficient to convert all phases in the mixture to a liquid state and at a pressure sufficient to prevent boiling in a period of about one hour. After mixing, the asphalt / solvent system is precipitated and cooled. During this step, phase separation occurs, producing a liquid solvent phase and a solvated asphalt phase. Depending on the equipment, the completion time of precipitation is about 5 to 30 minutes. If necessary, a mechanical method such as centrifugation can be used to accelerate the phase separation. After phase separation, the recovered solvated asphalt is either liquid or a liquid that can cool the mixture, and the recovered asphalt is a precipitated solid. In any case, a more convenient recovery method will be suitable, for example: gently decanting the liquid phase or filtering to remove solid solvated asphalt. The bitumen and solvent phases can be continuously recovered as a solvate in the liquid state. If necessary, the asphalt recovered in the liquid state, which has been recovered as a solvate, can be filtered to remove contaminants. Printed by the Consumer Cooperatives of the Central Standards Bureau of the Ministry of Economic Affairs (please read the precautions on the back before filling this page) by forming the same combination of isotropically fed asphalt and solvent (at lower temperatures, the solvent phase is liquid The solvated asphalt phase is solid) to obtain a solvated asphalt. When using this method, the solid solvated pitch can be recovered by conventional methods such as filtration. The properties of the non-volatile portion of the solvated asphalt can be measured at a temperature of about 150 ° C by removing the solvent by drying the solvated asphalt for about 60 minutes. After drying the asphalt, apply the Chinese National Standard (CNS) A4 specification (210X297 mm) at the paper size of the inert gas pressure. Printed by A7 __B7_ 'in the Consumer Cooperatives of the Central Standards Bureau of the Ministry of Economic Affairs. The softening point and melting point are determined by heating on a thermal stage microscope at a rate of about 5 ° C / minute. After the solvent is removed, the bitumen of the present invention will normally have a softening point of at least 280 ° C. At temperatures greater than 500 ° C • Harder dried asphalt will soften; however, these asphalts will not melt when heated at 5 ° C / min in an inert gas. These asphalts are considered to be self-stabilizing, so they will be carbonized directly to carbon processed products when continuously heated. II. Solvated Isotropic Asphalt ‘The solvated isotropic pitch of the present invention provides several important benefits over unsolvated isotropic pitch. Generally, the solvated asphalt will contain from about 5 weight percent to about 4 weight percent solvent. In addition, the solvated pitch has at least 50% by weight of toluene-insoluble matter and may consist of up to 40% by volume of optical anisotropy. Once the solvent is removed from the pitch, the anisotropic content can be increased. The isosolved bitumen of the present invention has a fluid temperature of at least 40 ° C, in some cases exceeding 100 ° C, which is lower than in the unsolvated state, meaning dry asphalt, the same asphalt Of melting point. III. Method for preparing carbon processed product The present invention also provides a method for manufacturing a carbon processed product from a solvated isotropic pitch. In particular, the present invention provides a method for producing carbon fibers from a solvated isotropic pitch. The method of manufacturing carbon processed products from solvated isotropic pitch is to apply the Chinese National Standard (CNS) A4 specification (210X2.97 mm) from the solvated paper size (please read the precautions on the back first) (Fill in this page again) Strike-Book 12 I. Printing of A 7 _____ £ 7_ by the Consumer Cooperatives of the Central Bureau of Standards of the Ministry of Economic Affairs, V. Description of Invention (10) Isotropic asphalt. Depending on the formed processed product and the solvent used to mediate the asphalt, the manufacturing method may require that a solvent suitable for this preparation method be used in place of the mediated asphalt. This step is known as solvent exchange and can be achieved by several methods. One method: require the asphalt to be dried to a solvate to drive off the solvent, and then re-mediate the asphalt with a suitable solvent. Yet another method provides the addition of a solvent having a boiling point higher than the starting mediated pitch to the solvated pitch. The mixture is then heated to boiling to remove lower boiling solvents (leaving from solvated asphalt containing higher boiling solvents). Regardless of the method, a typical manufacturing solvent will have a solubility parameter of about 8 to about 12 and possibly higher. The manufacturing solvent (non-expendable) may include one or more of the following solvents: toluene, benzene, xylene, tetrahydronaphthalene, tetrahydrofuran, chloroform, heptane, pyridine, quinone, halogenated benzene, chlorofluorobenzene And 2- to 4-ring aromatic solvents, and their partially alkylated and hydrogenated derivatives. Once the solvated bitumen contains a solvent suitable for the manufacturing method, it can be obtained by using a solvent known in the art. The method is formed into a carbon processed product. At present, the most common carbon processed product is carbon fiber. In the method of weaving carbon fibers from solvated pitch, some of the solvent will be lost from the product fibers. After drawing, any remaining solvent is removed immediately by drying the fibers. The loss of solvent produces carbon fibers with a softening point of at least 280 ° C. In addition, the resulting fiber will have a melting point that is higher than the fiber drawing temperature. Finally, depending on the starting feed pitch, the resulting fibers will not require additional treatment before carbonization. This paper size applies to China National Standard (CNS) A4 (210X297 mm) (Please read the precautions on the back before filling out this page) ... Packing.-Order _ Printed by A7, Employees' Cooperatives, Ministry of Economic Affairs ______B7_ '1 V. Description of the invention (11) The dried fibers with a softening temperature greater than 350 ° C starting temperature need not be stabilized before carbonization. The preferred fibers are those with a softening point above 500 ° C. When the temperature is slightly lower than the softening point of the fiber, the fiber is heated to achieve carbonization. As for the carbonization of fiber development, the softening temperature of the fiber rises, allowing the temperature of the carbonization reaction to increase relatively. During the carbonization reaction, however, the fiber never heats past its softening point. For fibers with a softening point above 500 ° C, heating can be performed at a rate above 20 ° C per minute or faster but without softening the fiber. Generally, carbonization is completed by heating at 600 ° C. However, the fibers can be treated at even higher temperatures. For bitumen with a softening point between about 280 ° C and 500 ° C, oxidative stabilization is preferably performed before carbonization. In addition, under certain circumstances, it may be necessary to oxidize and stabilize asphalt with a softening point above 500 ° C. An advantage of the present invention is that it can rapidly oxidize stable asphalt and / or a carbon processed product made of the asphalt at relatively high temperature and low oxygen concentration. More specifically, stabilization can be performed at temperatures above the temperature at which the workpiece is formed and in an atmosphere containing less than 5% oxygen. The benefits of the present invention over previous methods of oxidative stabilization are demonstrated by Example 2 and Figure 1. Figure 1 compares the oxidative stabilization of a conventional pitch with a solvated pitch. As demonstrated in Figure 1, prior to oxidative stabilization, the solvated asphalt does not need to be cooled, and stabilization occurs at higher temperatures and shorter cycle times. Thus, the present invention provides an important safety benefit that exceeds the prior art by eliminating the danger of combustion during oxidative stabilization. This paper size applies to Chinese National Standard (CNS) A4 (210 X 297 mm) (Please read the precautions on the back before filling this page) 1 Pack ^ ------- Order ------ ^ Risk --- ^ ---- A7 B7 Printed by the Consumer Cooperatives of the Central Standards Bureau of the Ministry of Economic Affairs. 5. Description of the invention (12) IV. Carbon fiber formation from solvated asphalt. The solvated asphalt melts above the wire drawing temperature. After the solvent is removed, the fibers of the present invention are typically infusible. As a result, the fibers of the present invention often do not require chemical stabilization before carbonization. However, in some cases stabilization is required: in an atmosphere containing only about 2 to 5% oxygen, stabilization is required when performed in a sufficiently short cycle time. Once the drawn fiber is carbonized, the carbon fiber of the present invention can be changed from continuous isotropic to continuous anisotropic. However, the major part of any anisotropic region appearing in these fibers does not have the characteristics of the extended range of the pitch pitch carbon fiber. These fibers have a tensile strength equivalent to that of conventional isotropic asphalt fibers. In order to achieve a degree of fiber containing anisotropic regions, it has improved thermal and electrical characteristics compared to fully isotropic fibers. The following examples illustrate the invention. Unless otherwise specified, all parts and percentages are by weight. Applicants do not want examples to limit this theory. The true scope of the invention is based on the scope of the attached patent application. Example 1 In a stirred pressure cooker, A 2 40 homogeneous asphalt sample (8% by weight toluene-insoluble matter) was mixed at a ratio of 1 g of asphalt per 8 cc of solvent: commercially available from Ashland Chemical Company, Columbus, Ohio This paper size applies to China National Standards (CNS) 8-4 specifications (210X 297 mm) (Please read the notes on the back before filling out this page)-Binding and ordering printed by the Consumer Standards Cooperative of the Central Standards Bureau of the Ministry of Economic Affairs A7 B7 5. Description of the invention (13)) and toluene. Fill the pressure cooker with nitrogen, drain briefly and seal. During 80 minutes, the mixture was heated until a temperature of 2 3 ° C was reached. The mixture was kept at 230 ° C for 10 minutes and stirred. The mixture was kept at 2 3 3 ° C for 15 minutes without stirring, and then cooled. During heating, the maximum pressure generated in a closed pressure cooker was 175 ps i g 〇 solid asphalt was recovered from the bottom of the pressure cooker, and the yield of the asphalt was calculated to be 6.4%. The pitch was analyzed by an optical microscope and found to contain 5% of intermediates in the form of small spheres. Dry the solid bitumen sample by heating at 360 ° C for 30 minutes under air. This step removes 28.2% of volatiles from the bitumen. Under the microscope thermal stage, under nitrogen, the heating rate is increased by 5 ° C per minute to 650 ° C. The dried asphalt will not soften or melt. Example 2 A solvate pitch was prepared by combining Aerocarb 80 (30% by weight of toluene-insoluble matter) with toluene at a ratio of 1 g pitch to 8 πθ toluene. The mixture was stirred at 230 ° C for 1 hour, allowed to settle for 15 minutes, and then cooled. A dense solid solvated asphalt layer was recovered from the bottom of the container with a yield of 54%. The solvated asphalt is sufficiently homogeneous, with only a fine sphere type with a non-isotropic direction of 5 to 10 ||%, and some larger spheres. Dry the solvated asphalt sample at 150 ° C for 1 hour under air to remove the solvent. After drying, the asphalt loses 22.1 weight. The paper size is in accordance with China National Standard (CNS) A4 (210X297 mm) _ (Please read the precautions on the back before filling this page):,-r7 ~-.. >} /, -I-11--1 I —1 I —Clothing — — IIII Order IIII --- Printed by A7 __B7__ 'in the Consumer Consumption Cooperative of the China Standards Bureau of the Ministry of Economy . Under emptying, the asphalt was further heated to 360 ° C to remove another 4.9% of volatiles. This additional loss appears to be due to the removal of any remaining solvents and the loss of some light oil. Analysis of this sample revealed a total of 52% by volume anisotropy. This argument demonstrates that the isotropic cyanocyanate that is a solvate produces additional anisotropy due to the loss of solvent. The temperature of the solvated homogeneous pitch is determined in a small pressure cooker by measuring the stirring resistance. The toluene-solvated bitumen is heated to a temperature above its fluid temperature, in this case 2 3 5 and then slowly cooled at about 1 ° C per minute. Using this method, the toluene-solvated asphalt reaches a viscosity of 600 Opoise at 191 ° C. Therefore, the fluid temperature of the solvated asphalt is 4 2 ° C, which is lower than the melting point of the Aero car b feed asphalt. Later, by using a thermal stage microscope, the solvent and softening point of the solvated asphalt after the removal of the solvent were determined. As previously defined, softening occurs when the sharp angle of the asphalt particles first becomes round. Melting occurs when the first observable flow of the softened asphalt is seen. Using these procedures and definitions, the dried solvated asphalt softens at 3 2 3 ° C and melts at 3 2 8 ° C. The melting point of the dried solvated asphalt is 95 ° C, which is higher than the Aerocarb 80 feed asphalt. Notably, the difference in melting point between the fluid temperature of the dried solvated bitumen and the solvated bitumen was at least 137 ° C in this experiment. In order to demonstrate the improved stabilization characteristics of the dried unsolvated asphalt, the dried solvated asphalt sample and A e r oc a r b 80 were oxidized. Two kinds of asphalt samples are crushed into particles of 10 to 200 microns, and the paper size applies the Chinese National Standard (CNS) A4 specification (210 X 297 mm) _ ·! (Please read the precautions on the back before filling (This page) ---------- 1 --- Γ --- install ---- I " -order ----- A 7 _B7___ '1 V. Description of the invention (15) In the near 2 Oxidation at a temperature of 0 ° C (below its softening point) for 30 minutes. Oxygen is also 2% oxygen in nitrogen. Therefore, the '.Aerobacarb 80 feed pitch is oxidized at 250 ° C, and the dried solvate pitch is oxidized at 300 ° C. It is then oxidized and heated under nitrogen at an increase of 5 ° C per minute to determine the softening point and melting point of each asphalt. The stabilized "! · -0 carb softens at 250 ° C and melts at 25 4 ° C, which means an improvement of 2 2 ° C on unstabilized asphalt. In contrast, after stabilization The solvated bitumen did not melt, and only 2 G% of the sample showed any evidence of softening when heated to 650 ° C. Obviously, on stabilized feed bitumen, the The stabilized solvated asphalt has sufficient improved thermal characteristics. The characteristics comparison of solvated asphalt to unsolvated asphalt is provided by the following. (Please read the precautions on the back before filling this page) The paper printed by the Central Consumers ’Agency Consumer Cooperatives of the Ministry of Economic Affairs is again applicable to the Chinese National Standard (CNS) A4 specification (210 X297 mm) -18-V. Description of the invention (16) Table 1 Printed by a cooperative
Aerocarb 80 成溶劑化物 之瀝青 經乾燥之瀝青特徵1， 軟化點，°c 228 323 熔點，°c 233 328 成溶劑化物之瀝青之流體溫 度 2，。c — 191 瀝青安定化（2%〇2在N2中） 溫度，°C 205 300 時間，分鐘 30 30 經安定化之瀝青特徵1， 軟化點，°C 250 <20%至 650 熔點，°C 254 無至6_5 0 在N 2之下，以5 °C /分鐘熱階段觀察。 在冷卻時，其黏度近乎6 0 0 poise之溫度。 (請先閲讀背面之注意事項再填寫本頁) VH..- ^^!5;1"1·*民 · ^:v_ ---.—訂--- A7 ___._ B7_1 五、蚕明説明（I7 ) 例3 此例論証從例3之成溶劑化物之各向同性之瀝青紡織 成碳纖維之利益在從Aer Dear b進料瀝青紡織成纖維之利益 之上。在從例3之成溶劑化物之瀝青紡織成纖維之前，成 溶劑化物之瀝青以四氫某再溶解之。再溶解之步驟包含乾 燥該成溶劑化物之瀝青以移除甲苯，接著結合該瀝青與四 氫某（以7 : 2 =瀝青：溶劑之比例）。四氫某成溶劑化 物之瀝青在2 3 0°C平衡3 0分鐘。該經再溶解之瀝青具 有1 6 1 °C之流體溫度。 經濟部中央標隼局員工消費合作社印製 (請先閲讀背面之注意事項再填寫本頁) 成溶劑化物之瀝青與Aerocarb進料瀝青熔化並紡織成 爲纖維。在1 8 7°C，成溶劑化物之瀝青形成5 0至65 微米之纖維。從成溶劑化物之瀝青中做爲紡織而成之纖維 包含剩餘之溶劑。這些纖維在氮之下，在二分鐘內加熱至 2 9 0 °C，然後更進一步以5 °C /分鐘之速率加熱而決定 做成紡織而成之纖維之軟化點與熔點。軟化，藉由尖銳邊 緣之磨圓與一些纖維之彎曲所指示，在3 0 2 °C被觀測出 。而熔化，藉由纖維之邊緣之變圓及膨脹及纖維接合點之 熔化所指示，於3 5 3 °C被觀測出。必須注意的是做爲紡 織而成之纖維通常較易軟化且較小心地乾燥之纖維較慢熔 化° 與本發明成對照，在紡織成爲4 0至6 G微米纖維之 前需要將AerDcarb進料瀝青加熱至2 9 8 °C°這些做爲紡 織而成之纖維在二分鐘加熱至2 0 0 °C，然後更進一步以 每分鐘5 °C之速率加熱之.。這些纖維在2 2 7 °C軟化且在 本紙張尺度適用中國國家標準（CNS ) A4規格（210X297公釐）_ 2〇 - B7 五、發明説明（is) 2 3 4 °C熔化。 此外，二組纖維皆安定化。成溶劑化物之瀝青纖維在 2 7 〇°C，藉由曝露於氮中2%氧，6 0分鐘而安定化（ 8 3 °C較高於紡織溫度）。然後將該纖維在氮之下，以每 分鐘2 Ο X加熱而昇至6 5 0 °C。該纖維並不會軟化或熔 化。而Aero car b進料瀝青纖維在1 9 5 °C曝露於相同含有 氧氣之氣體中6 0分鐘。注意：因這些纖維之熔點，需較 低溫之溫度。在氮之下，以每分鐘2 0°C之上昇溫度，這 些纖維在2 4 8 °C軟化並在2 5 8 °C熔化。如表2所示， 這些結果很明顯地論證出以成溶劑化物之瀝青易於改善安 定化及達成降低紡織之溫度。 (請先閲讀背面之注意事項再填寫本頁) 經濟部中央標率局員工消費合作社印製 21 本紙張尺度逋用中國國家標準（CNS ) A#規格（2丨〇><297公釐） A7 B7 五、發明説明（l9) 表2 經濟部中央標準局員工消費合作社印製Aerocarb 80 solvated asphalt Features 1 of dried asphalt, softening point, ° c 228 323 melting point, ° c 233 328 fluid temperature of solvated asphalt2. c — 191 Stabilization of asphalt (2% 〇2 in N2) Temperature, ° C 205 300 Time, minutes 30 30 Stabilized asphalt characteristics 1, softening point, ° C 250 < 20% to 650 melting point, ° C 254 None to 6_5 0 Under N 2, observe at 5 ° C / min thermal stage. When cooled, its viscosity is close to 6 0 0 poise temperature. (Please read the precautions on the back before filling this page) VH ..- ^^! 5; 1 " 1 · * 民 · ^: v_ ---.— order --- A7 ___._ B7_1 V. Silkworm Explanation (I7) Example 3 This example demonstrates that the benefits of spinning the carbon fiber from the solvated isotropic pitch of the solvate of Example 3 outweigh the benefits of feeding asphalt spinning fibers from Aer Dear b. Before spinning from the solvated pitch of Example 3 into fibers, the solvated pitch was redissolved with tetrahydrogen. The re-dissolving step includes drying the solvated asphalt to remove toluene, and then combining the asphalt with tetrahydrogen (in a ratio of 7: 2 = asphalt: solvent). Tetrahydrous solvated asphalt was equilibrated at 230 ° C for 30 minutes. The redissolved asphalt has a fluid temperature of 161 ° C. Printed by the Consumers' Cooperative of the Central Bureau of Standards, Ministry of Economic Affairs (please read the precautions on the back before filling this page) The solvated asphalt and Aerocarb feed asphalt are melted and woven into fibers. At 18 ° C, the solvated pitch forms fibers of 50 to 65 microns. Textiles made from solvated pitch contain the remaining solvent. Under nitrogen, these fibers are heated to 290 ° C in two minutes, and then heated at a rate of 5 ° C / minute to determine the softening point and melting point of the woven fiber. Softening, as indicated by the rounded edges of sharp edges and the bending of some fibers, was observed at 30.2 ° C. Melting, as indicated by the rounding and swelling of the edges of the fibers and the melting of the fiber joints, was observed at 3 5 3 ° C. It must be noted that fibers made as weaving are usually easier to soften and fibers that dry less carefully melt slowly. In contrast to the present invention, AerDcarb feed bitumen needs to be heated before spinning into 40 to 6 G micron fibers To 298 ° C ° These woven fibers are heated to 200 ° C in two minutes, and then heated at a rate of 5 ° C per minute. These fibers are softened at 2 7 ° C and the Chinese national standard (CNS) A4 specification (210X297 mm) _ 20-B7 is applied at the paper size. V. Description of the invention (is) 2 3 4 ° C melting. In addition, both groups of fibers are stabilized. The solvated pitch fiber was stabilized at 270 ° C by exposure to 2% oxygen in nitrogen for 60 minutes (83 ° C higher than the textile temperature). The fiber was then heated to 650 ° C under nitrogen at 20 ° C per minute. The fiber does not soften or melt. Aero car b feed pitch fibers were exposed to the same oxygen-containing gas at 19 5 ° C for 60 minutes. Note: Due to the melting point of these fibers, lower temperatures are required. Under nitrogen, at a rising temperature of 20 ° C per minute, these fibers softened at 248 ° C and melted at 258 ° C. As shown in Table 2, these results clearly demonstrate that solvated asphalt is easy to improve stability and achieve lower textile temperatures. (Please read the precautions on the back before filling out this page) Printed by the Central Consumer Bureau of the Ministry of Economic Affairs 21 Consumer Cooperatives Printed on this paper adopts China National Standard (CNS) A # Specifications (2 丨 〇 > < 297 mm) A7 B7 V. Description of Invention (l9) Table 2 Printed by the Consumer Cooperative of the Central Standards Bureau of the Ministry of Economic Affairs
Aerocarb 80 成溶劑化物 之瀝青 熔化紡織溫度，°c 298 187 關於經紡織而成之熔化行 爲1 -軟化，°c 227 302 熔化，°c 234 353 纖維安定化（在N 2中2 % 0 2 ) 溫度，°C 195 270 時間，分鐘 60 60 經安定化之纖維特徵2， 軟化點，°c 248 無至650 熔點，°c 258 無至650 在N 2之下，以5 π /分鐘之熱階段觀察 在Ν2之下，以2 〇〇c/分鐘之熱階段觀察 本紙張尺度適用中國國家檩準（CNS ) A4規格（21〇x29?公釐） -22 - (請先閲讀背面之注意事項再填寫本頁) ___\PL_____^_ Γ___[ _ ____一_^_________ 0 am t·——^· ^^^^1 flflu n^i nn Ϊ·^^1· m^i —B^^— ·-: ^ —^ϋ mu ^i^i— vm a^tmt tn^i ^^^^1 ffm me ^-F 澤 - i J#% , A7 B7 1 1 五、發明説明（2〇) 另外，從此申請書之考慮或在此所發明.之練習，這些 發明之體系對於熟知此領域之人士是顯而易見的。本申請 書與例子僅做爲模範，而非藉由此限制本發明之眞實領域 與精神，而下列申請專利範圍方爲本發明之眞實領域與精 神0 (請先閱讀背面之注意事項再填寫本頁) 裝· 訂 經濟部中央標準局員工消費合作社印製 本紙張尺度適用中國國家標準（CNS ) A4規格（210X297公釐）-23 -Aerocarb 80 Solvent-based pitch melting textile temperature, ° c 298 187 About the melting behavior of warp 1-softening, ° c 227 302 melting, ° c 234 353 fiber stabilization (in N 2 2% 0 2) Temperature, ° C 195 270 time, minutes 60 60 Stabilized fiber characteristics 2, softening point, ° c 248 to 650 melting point, ° c 258 to 650 under N 2 at 5 π / minute thermal stage Observe under N2, observe at the thermal stage of 2000c / min. The paper size is applicable to China National Standard (CNS) A4 (21 × 29? Mm) -22-(Please read the precautions on the back before (Fill in this page) ___ \ PL _____ ^ _ Γ ___ [_ ____ 一 _ ^ _________ 0 am t · —— ^ · ^^^^ 1 flflu n ^ i nn Ϊ · ^^ 1 · m ^ i —B ^^ — ·-: ^ — ^ Ϋ mu ^ i ^ i— vm a ^ tmt tn ^ i ^^^^ 1 ffm me ^ -F Ze-i J #%, A7 B7 1 1 V. Description of the invention (2〇) In addition, The system of these inventions will be apparent to those skilled in the art from the consideration of this application or the practice of this invention. This application and examples are only examples, not to limit the actual field and spirit of the present invention, and the following patent application scope is the actual field and spirit of the present invention. 0 (Please read the notes on the back before filling this Pages) Binding and binding. Printed on paper printed by employees' cooperatives of the Central Standards Bureau of the Ministry of Economic Affairs. Applicable to China National Standard (CNS) A4 (210X297 mm)-23-