經濟部中央標準局員工消f合作社印製 A7 B7 五、發明説明（/.) 本發明係關於一種低黏度纖維素溶液之製造方法，主 要係有關纖維素溶解於混合溶劑製成溶液之流程製法。 傳統嫘縈纺絲製法，係為粘液濕式訪絲法，如第六圖 所示’將紙漿或纖維素加入氫氧化納（N a Ο Η )而形成 礙化纖維素，再經壓榨、老成後加入二硫化碳（C S ζ ) 黃化成黃酸纖維素，再Κ稀氫氧化納溶解成粘液，然後將 粘液導入纺浴中（含稀硫酸、硫酸納、硫酸鋅等）由坊口 泉出’與纺浴各成份進行中和再生，再經後處理及乾燥而 得成品。所需手續十分繁雜，耗時甚久。因黏液於空氣中 無法凝结再生，僅掂在纺浴内纺絲始能達凝结再生目的， 但是中和再生時會產生硫化氫（Η 2 S )、二硫化碳（ C S 2 )及硫化納（N a 2 S )等之衍生物排放物質*且 廢水含鋅金鼷極易造成環境污染.同時因此種纺絲在纺浴 內進行，流體之砠力造成僅能採低速纺絲，而低速纺絲物 ft較差，因此採用嫘锘粘疲濕式纺絲法之生產方式逐年降 低。近來為克服前述缺點而發展出一套直接溶劑法。 如第七_流程所示，將織維素與溶劑栢互溶解，溶解 之後即成溶液。經纺絲、再生、水洗、乾烽、捲絲而為成 品絲。其中再生過程中配合回收溶劑以能循環利用。 前述直接溶劑法雖較無濕式纺絲法之缺點，有溶劑高 度回收率、溶液可高速纺絲、污染性少、成品物性佳之特 點*但因下列因素迄今尚無法大量推廣生產，在生產利用 價值上無法有效提昇： 本纸張尺度適用中國國家標準（CNS ) A4規格（210X297公釐） ___!________r ^ L__ ,¾ (請先閱讀背面之注意事項再填寫本頁)A7 B7 printed by the Employees ’Cooperative of the Central Bureau of Standards of the Ministry of Economic Affairs V. Description of the invention (/.) The present invention relates to a method for manufacturing a low-viscosity cellulose solution, mainly related to the process of dissolving cellulose in a mixed solvent to prepare a solution . The traditional rayon spinning method is a slime wet silk-visiting method, as shown in the sixth figure, 'pulp or cellulose is added to sodium hydroxide (N a Ο Η) to form hindered cellulose, which is then pressed and aged After adding carbon disulfide (CS ζ) to yellow into cellulose xanthate, then dilute sodium hydroxide to dissolve into a mucus, and then introduce the mucus into the spinning bath (containing dilute sulfuric acid, sodium sulfate, zinc sulfate, etc.) from Fangkouquan 'and The components of the spinning bath are neutralized and regenerated, and then processed and dried to obtain the finished product. The required procedures are very complicated and take a long time. Because the mucus cannot be condensed and regenerated in the air, only spinning in the spinning bath can achieve the purpose of condensate regeneration, but during neutralization, hydrogen sulfide (Η 2 S), carbon disulfide (CS 2) and sodium sulfide (N a 2 S) and other derivatives discharge substances * and the wastewater containing zinc and gold is very likely to cause environmental pollution. At the same time, the spinning is carried out in the spinning bath, and the force of the fluid causes only low-speed spinning, and low-speed spinning The ft is poor, so the production method using the ray-bonded wet spinning method is decreasing year by year. Recently, a set of direct solvent methods have been developed to overcome the aforementioned shortcomings. As shown in the seventh procedure, dissolve oryzanol and solvent cypress to each other, and then dissolve to form a solution. After spinning, regeneration, washing, drying, and winding, it becomes a finished yarn. Among them, the recovery process is combined with the recovery of the solvent to enable recycling. Although the aforementioned direct solvent method is less disadvantageous than the wet spinning method, it has the characteristics of high solvent recovery rate, high-speed spinning of the solution, less pollution, and good physical properties of the finished product. * However, due to the following factors, it has not been possible to promote production in large quantities. The value cannot be effectively improved: This paper scale is applicable to the Chinese National Standard (CNS) A4 specification (210X297mm) ___! ________ r ^ L__, ¾ (Please read the precautions on the back before filling this page)
、1T .-- 經濟部中央標準局員工消費合作杜印製 A7 ------------ B7 五、發明説明（V) (1) _ $素原料之來源仍限於傳統钻液纺絲法之溶解性 m iut # _。而長纖維原料在擴大菫產上取得不易，成本 偏高，原料來源廣度不足。 (2) 胃&粘度：纖維素經溶劑溶解後，溶液粘度高達 8000〜12Q00粕，因高黏度之流體咀力大，高速纺絲時產生 延伸性困難之問題。 維素對溶劑總量之澹度無法有效提高，僅在8〜 1 5 %之間，因濃度太低，以致製造處理成本偏高。 ⑷纖維素聚合度（D P )衰退大：為克服第⑵、⑶項 2 fMl H ’需採高溫、長時間溶解之製程條件，致使纖雄素 之聚合度因長時間高溫而大幅降低衰退，導致強度降低而 有損品質。 ⑸溶劑成本及回收率；使用單一氧化胺系之氧化甲基 IS琳（NMMO)或其它較不穩定之肋溶劑，價格偏高， 且溶解時間長、溫度高*溶劑分解程度高，在高速製绦時 溶劑不易清洗釋出，致溶劑回收率僅94 %左右，溶劑成本 因而偏高。 因此直接溶劑法雖優於傳統粘液濕式纺絲法，但因上 述各項問題，致量產化和普及化程度低，溶劑成本高，織 維強度低等等，是故本發明人不斷悉心改迆、創研，終發 明出一種低黏度纖維素溶液之製造方法•期W高度創新方 法，解決溶劑成本及回收等問題，同時提高纖維物性K提 昇至高速坊絲層次。 -4 - 本紙伕尺度適用中國國家榇準（CNS ) A4規格（210X297公釐) (請先閱讀背面之注意事項再填寫本页) T ·-0 1 A7 B7 五、發明説明（少） 一 本發明之主要目的係、提供一種低黏度纖键素溶液之製 造方法，主要係改變溶劑組成，使製程具有高溶解力、低 钻度、低成本、高回收率之效果；同時纖維素與溶劑彳系使 用m合槠μ低溫捏合押出，再配合薄膜蒸發方式，使溶解 時間有效降低，進而減少纖維素聚合度衰退的問題，強化 纖維產品物性，提昇品質。 因此本發明具體之流程特點如下： ㈠：依成品物性需求，可選用長纖維、短纖維或非溶 解性木漿纖维之混用。 ㈡：使用混合溶劑：其係由三種溶劑相互混合組成， 即係氧化甲基瑪琳（Ν Μ Μ 0 ) 4 5〜7 5 %，正甲基己内隨 胺（N M C ) 22〜38%，及四甲基氛化銨（TMAC) 3〜 1 8%等三種溶劑，混合溶劑中並加入1 〇 〇 〇 ρ ρ μ〜1 %之抗聚 合衰退添加劑： 羥苯基硬脂酸丙酯 [Stearyl-3(3,0,di-tert-4-hydroxy phenyl)Propionate] 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页) ㈢：低溫捏合押出1使用捏合機設備，將纖維素及混 合溶劑在捏合機内K低溫捏合均匀而押出成漿液。 ㈣：利用薄膜蒸發器將漿液之多餘水份迅速蒸發•纖 維素即可溶解於溶劑中。 ㈤：高速纺絲、捲絲之過程，克服再生水渦流及水洗 時強烈飛濺，解決高速纺絲之困難。 ㈥：因低溫低裂解，使回收率得提高到99 . 2% K上。 本紙張尺度適用中國國家標準（CNS ) A4現格（210X297公釐） 經濟部中央標準局員工消費合作社印製 303396五、發明説明（f) 為使 貴審 過程及其他目的 (一） ·[國式部 第一圖係本發明 第二_係本發明 第三圖係本發明 第四圖係本發明 第五圖係本發明 第六圖係傳铳之 第七圖係習知之 (二） *圖號部 (1 ◦)溶液出 (20)薄膜蒸 (22)葉片 (2 4 )熱媒入 (26)水份蒸 (3 0 )溶液中 (3 1 )齒輪泵 (3 3 )再生槽 (3 5 )水洗輪 (37)捲絲 (3 9 )純水 附件一：纖維素 A7 B7 查 杂 員 能 進 —. 步 瞭 解 i ί么 附 較 佳 竄 施 例 及 份 之 流 示 意 圖 〇 之 薄 膜 蒸 發 器 示 意 圖 之 辑 膜 葉 片 斷 面 剖 視 之 纺 絲 流 程 示 意 圖 0 之 回 收 溶 劑 流 程 示 意 嫘 縈 濕 式 纺 絲 法 之 流 直 接 溶 劑 法 之 流 程 示 份 ： P 發 器 ( 2 1 ( 2 3 P ( 2 5 發 出 □ ( 2 7 間 樓 ( 3 2 ( 3 4 ( 3 6 ( 3 8 ( 4 0 種 類 比 較 表 乙 份 0 本發明之特微、製法 圖式詳细說明如后： 圖。 圖。 程示意圖。 意圖。 )馬達 :)入料口 )熱媒出口 )齒輪泵 )噴絲頭 )再生液 )乾燥輪 )泵 )溶劑回收 (讀先閱讀背面之注意事項再填寫本页) 、-° 么'·· 本紙張尺度適用中國國家標準（CNS ) A4規格（210X297公釐） 經濟部中央標準局負工消費合作社印製 Α7 Β7 五、發明説明（j=) 附件二：溶劑種類比較表乙份。 附件三：溶劑種類比較表乙份。 附件四：溶劑成本比較表乙份。 本發明係一種低黏度纖維素溶液之製造方法，請參見 第一圖所示，依流程所示而分項說明； a :首先備妥纖維素及混合溶劑； 本發明所使用之纖維素除了 α -纖維素 (a— Cellulose) 90 上，及長度4«miK上之長纖維 外，低α —纖維素（ot— Cellulose)之短纖維，甚至非 溶解性回收紙漿均可酌量滲用/而得各级強度之成品。 本發明之混合溶劑係由三種溶劑栢互混合組成，並可 再加上抗衰退添加劑。而混合溶劑係具備膨潤性大、溶解 濃度高、溶解速度快、溶解後之聚合度為8 0 0 Μ上，溶劑及 再生液之成份相似等條件，故而於實施上採： ⑴氧化院基胺系（A 1 k y 1 Amine 〇 x i d e)之氧化甲基瑪 ί林（Normal Methyl Morpholine Oxide> NMMO) 45 〜75%， ⑵烷基胺盥系（Alkyl Amine Salt系）之正甲基己内醢胺 (Normal Methyl Caprolactam， NMC) 22〜38 % ， ⑶烷基氨鹽糸（Alkyl Ammonium Salt)之四甲基氯化氨（ Tet r a Methyl Ammo ilium Chloride，TMAC) 3 〜18% 等三種溶劑相互混合； 並在混合溶劑中加入1 0 0 Q P P Μ〜1 %的抗衰退添加劑 本紙張尺度適用中國國家標準（CNS ) Α4規格（210Χ297公釐） ----------^.4 —— (請先閱讀背面之注意事項再填寫本ΪΙ) 訂 五 A7 _B7___ 發明説明（/) :羥苯基硬脂酸丙酯 [St. εβΓγΙ-βΠ,δ,ίϋ-ίεΓΗ-ίιγίίΓΟΧγ p h e n y 1 ) P r ο p i ο n a t e ，M減緩聚合度衰退。 b :低溫捏合押出，使用捏合機設備，做漿液低溫捏 合押出，將紙漿、溶液及添加劑故入捏合機内，以5 G〜（5 〇 C之低溫夾套加熱，當混合約3 0分錡後即成漿液，再配合 捏合機轉動螺桿以將漿液均勻柙出’連缡送往溶解器內溶 解。因本發明之纖維素溶解器為—具有極高溶解效果之薄 膜蒸發器，漿液無需在捏合階段做高溫長時間之預溶，僅 Μ 5 0〜6 0 C做3 0分鐘之混合過程即可*如此可防山纖維素 之聚合度衰退。同時本發明之漿液係以鏍桿速續押出，不 担輸送效果良好，且計道極為正確。 c :利用薄膜蒸發器，使上述漿液之多餘水汾迅速蒸 發，缁維素即可溶解於溶劑中；如第二圖所示，薄_蒸發 器（2 0 )细部结構形態非本發明強調者，基本原理係漿 液由入料口 （23)送入内荷（28)，配合馬達（21 )帶動數組蚰裝的葉片（2 2 )高速旋轉，將漿液在葉片 和内筒（2 8 )壁面間刮成薄膜，冏時將内筒（2 8 )抽 真空成減壓狀態，外茼（29)為熱媒夾套用Μ加熱内茼 (28)，當漿液在薄膜、減壓、加熱狀況下，多餘水份 可在極短時間迅速蒸發，纖維素即可溶解，比如1 5 %纖維 素漿液Μ葉片（2 2 ) 20 0 rpin刮成5咖薄膜，Κ 100〜300、 1T .-- A7 of consumer cooperation of the Central Bureau of Standards of the Ministry of Economic Affairs. Printed A7 ------------ B7 V. Description of the invention (V) (1) _ The source of raw materials is still limited to traditional diamonds Solubility of liquid spinning method miut # _. However, long-fiber raw materials are not easy to obtain in expanding shizuku production, the cost is relatively high, and the breadth of raw materials is insufficient. (2) Stomach & Viscosity: After the cellulose is dissolved by the solvent, the solution viscosity is as high as 8000 ~ 12Q00 meal. Due to the high viscosity of the fluid nozzle, the problem of extensibility is difficult during high-speed spinning. The degree of vitamins to the total amount of solvents cannot be effectively increased, only between 8 and 15%, because the concentration is too low, so that the manufacturing and processing costs are too high. ⑷The degree of cellulose polymerization (DP) declines greatly: In order to overcome the process conditions of 2 fMl H 'in item ⑵ and ⑶, which requires high temperature and long-term dissolution, the degree of polymerization of cellotropin is greatly reduced due to long-term high temperature. Decreased strength detracts from quality. ⑸ Solvent cost and recovery rate; using a single amine oxide-based oxidized methyl IS Lin (NMMO) or other less stable rib solvents, the price is relatively high, and the dissolution time is long, the temperature is high * The degree of solvent decomposition is high, at a high speed The solvent is not easy to clean and release during satin, and the solvent recovery rate is only about 94%, so the cost of the solvent is high. Therefore, although the direct solvent method is superior to the traditional slime wet spinning method, due to the above problems, the mass production and popularization are low, the cost of the solvent is high, and the strength of the weave dimension is low. After reforming and researching, a method of manufacturing a low-viscosity cellulose solution was finally invented. The period W was a highly innovative method to solve the problems of solvent cost and recovery, and at the same time improve the fiber properties K to the high-speed square silk level. -4-This paper is applicable to China National Standard (CNS) A4 (210X297mm) (please read the precautions on the back before filling this page) T · -0 1 A7 B7 Fifth, invention description (less) 1 copy The main purpose of the invention is to provide a method for manufacturing a low-viscosity fibronectin solution, mainly to change the solvent composition, so that the process has the effects of high solubility, low drilling, low cost and high recovery; at the same time, cellulose and solvent The system uses m-mixed-mu to knead and extrude, and then cooperates with the film evaporation method to effectively reduce the dissolution time, thereby reducing the problem of degradation of cellulose polymerization degree, strengthening the physical properties of fiber products, and improving quality. Therefore, the specific process characteristics of the present invention are as follows: (1): According to the physical properties of the finished product, a mixture of long fiber, short fiber or non-soluble wood pulp fiber can be selected. (Ii) Use mixed solvent: it is composed of three solvents mixed with each other, namely, methyl methoxide (Ν Μ Μ 0) 4 5 ~ 75%, n-methyl caprolactone (NMC) 22 ~ 38%, And tetramethyl ammonium oxychloride (TMAC) 3 ~ 18% and other three solvents. Mix the solvent and add 100,000 ρ ρ μ ~ 1% of the anti-polymerization degradation additive: hydroxyphenyl stearate [Stearyl -3 (3,0, di-tert-4-hydroxy phenyl) Propionate] Printed by the Employee Consumer Cooperative of the Central Standards Bureau of the Ministry of Economic Affairs (please read the precautions on the back before filling in this page) ㈢: low temperature kneading extrusion 1 use a kneading machine Equipment, knead cellulose and mixed solvent in a kneader at a low temperature and knead evenly to extrude into a slurry. (Iv): Use a thin-film evaporator to quickly evaporate excess water from the slurry. Cellulose can be dissolved in the solvent. ㈤: The process of high-speed spinning and yarn winding overcomes the vortex of reclaimed water and the strong splash during washing, and solves the difficulty of high-speed spinning. ㈥: Due to the low temperature and low cracking, the recovery rate can be increased to 99.2% K. This paper scale is applicable to the Chinese National Standard (CNS) A4 format (210X297 mm) Printed by the Ministry of Economic Affairs Central Standards Bureau employee consumer cooperative 303396 V. Description of invention (f) For the purpose of making your review process and other purposes (1) The first picture of the formula is the second picture of the present invention_the third picture of the present invention is the fourth picture of the present invention The fifth picture of the present invention is the sixth picture of the present invention The seventh picture of the book is the seventh picture of the conventional (2) * picture Number part (1 ◦) solution out (20) film steaming (22) blade (2 4) heat medium into (26) moisture steaming (3 0) solution (3 1) gear pump (3 3) regeneration tank (3 5) Washing wheel (37) Coiled wire (3 9) Pure water Annex I: Cellulose A7 B7 Checkers can enter-. Learn more about the thin film evaporator with better channeling examples and partial flow diagram. Schematic diagram of the membrane blade cross-section of the spinning process. Schematic diagram of the recovery solvent 0. Schematic diagram of the flow of the wet wet spinning method. Direct flow of the solvent method: P hair (2 1 (2 3 P (2 5 Issue □ ( 2 7 buildings (3 2 (3 4 (3 6 (3 8 (4 0 Type comparison table 0 0 Motor :) Feed port) Heat medium outlet) Gear pump) Spinneret) Regeneration liquid) Drying wheel) Pump) Solvent recovery (Read the precautions on the back before filling in this page),-° What's this paper The standard is applicable to the Chinese National Standard (CNS) A4 specification (210X297mm). The A7 Β7 is printed by the Consumer Labor Cooperative of the Central Standards Bureau of the Ministry of Economy. V. Description of the invention (j =) Appendix 2: A comparison table of solvent types. Appendix 3: A comparison table of solvent types. Appendix 4: A copy of the solvent cost comparison table. The present invention is a method for manufacturing a low-viscosity cellulose solution, please refer to the first figure, and explain it according to the flow chart; a: first prepare cellulose and mixed solvent; the cellulose used in the present invention -In addition to cellulose (a- Cellulose) 90, and long fibers with a length of 4 «miK, short fibers with low alpha-cellulose (ot- Cellulose), and even non-soluble recycled pulp can be infiltrated / derived Finished products at all levels of strength. The mixed solvent of the present invention is composed of three solvents mixed with each other, and anti-decay additives can be added. The mixed solvent has the conditions of large swelling, high dissolution concentration, fast dissolution rate, degree of polymerization after dissolution of 800 Μ, similar composition of solvent and regenerated liquid, so the implementation of the above: (A 1 ky 1 Amine 〇xide) Oxygen methyl malin (Normal Methyl Morpholine Oxide> NMMO) 45 ~ 75%, ⑵ alkylamine (Alkyl Amine Salt system) n-methyl caprolactam (Normal Methyl Caprolactam, NMC) 22 ~ 38%, ⑶ Alkyl Ammonium Salt (Tet ra Methyl Ammo ilium Chloride, TMAC) 3 ~ 18% and other three solvents are mixed with each other; And add 100 QPP Μ ~ 1% anti-decay additive to the mixed solvent. The paper standard is applicable to China National Standard (CNS) Α4 specification (210Χ297mm) ---------- ^. 4 ---- (Please read the precautions on the back before filling in this ΪΙ) Order 5 A7 _B7___ Description of invention (/): Propyl hydroxystearate [St. εβΓγΙ-βΠ, δ, ίϋ-ίεΓΗ-ίιγίίΓΟΧγ pheny 1) P r ο pi ο nate, M slows down the degree of polymerization decline. b: Low temperature kneading and extruding, use the kneader equipment to do low temperature kneading and extruding, put the pulp, solution and additives into the kneader, and heat it with a low temperature jacket of 5 G ~ (5 〇C, after mixing for about 30 minutes. It becomes a slurry, and then cooperate with the kneader to rotate the screw to evenly remove the slurry and send it to the dissolver. Because the cellulose dissolver of the present invention is a thin film evaporator with extremely high dissolution effect, the slurry does not need to be kneaded. In the stage, pre-dissolve at high temperature for a long time, only M 5 0 ~ 6 0 C can be mixed for 30 minutes. This can prevent the polymerization degree of mountain cellulose from declining. At the same time, the slurry of the present invention is continuously extruded at the speed of the screw , It does not have a good transport effect, and the counting path is very correct. C: Using a thin-film evaporator, the excess water of the above slurry is quickly evaporated, and the vitamin can be dissolved in the solvent; as shown in the second figure, thin_evaporation The detailed structure of the device (2 0) is not emphasized by the present invention. The basic principle is that the slurry is fed into the internal load (28) from the feed port (23), and the motor (21) drives the blades (2 2) rotating at high speed. , Put the slurry in the blade and (2 8) Scraping a thin film between the walls, vacuuming the inner cylinder (2 8) to a decompressed state at the moment, the outer chrysanthemum (29) is a heat medium jacket, and heating the inner choke (28) with Μ. Under pressure and heating, excess water can evaporate quickly in a very short time, and the cellulose can be dissolved. For example, 15% cellulose slurry M blade (2 2) 20 0 rpin scraped into 5 coffee film, K 100 ~ 300
Torr真空度，及8QT：溫度加熱控剌，而在五分鑌内排除水 -8- 表紙張尺度適用中國國家揉準（CNS ) A4規格（210X297公釐） I . .1' —装 訂----*~一 ·_線 (請先閱讀背面之注意事項再填寫本頁) 經濟部中央梂準局貝工消費合作社印製 83.5 5,000 0.88 經濟部中央標準局男工消費合作杜印製 A 7 B7 五、發明説明（/) 份到9〜1 1 %溶解條件，即可將纖維素溶解。 d :溶解後，g卩進行纺絲、再生、水洗、乾燥、捲絲 之過程，如第四_所示，谣將纖维素溶液經齒輪泵（3 Γ )，送經嗅絲頭（3 2 )、再生槽（3 3 )、水洗輪（3 5 )、乾燥輪（3 6 )而經捲絲機（3 7 )而捲取成成品 絲’此為公知過程，不再螯述。但有一點不同，當纺絲經 水洗輪（3 Γ> )之纯水（3 3 )沖洗後會產生含4%溶劑、 9 6 %水之稀釋液，再將此稀釋液利兩泵（3 8 )抽至再生 槽（3 3 ) ’當做再生液循環使用，其濃度控制於6%溶劑 及 9 4 %之水。再生液之溢流液則送往溶劑回收（4 0 ) 部門，回收成溶劑以便重覆使用。 e :溶劑回收 本流程乃配合進行，如第五圖即是回收溶劑流程；當 再生液—經U F限外過濾（u 11 r a - F i 11 e r) 4 R 0逆滲透 濃縮（R e v e r s e - 0 s m 〇 s i s )蒸汽濃縮—樹脂交換等步驟， SP得到回收溶劑。本發明因在溶解階段採用低溫低裂解， 在纺絲階段做充份溶劑循環使用，故捩耗低，回收效率可 達 99 · 2% K 上。 由K上說明製程後，K下述明本發明所產生之創新效 果；Torr vacuum degree, and 8QT: temperature heating control, and water is eliminated within five minutes -8- table paper scale is applicable to China National Standardization (CNS) A4 specification (210X297 mm) I .1 '-binding- --- * ~ 一 · _Line (please read the precautions on the back before filling in this page) Printed by the Ministry of Economic Affairs Bureau of the Central Bureau of Economic Affairs, Beigong Consumer Cooperative 83.5 5,000 0.88 Printed by the Ministry of Economic Affairs, Central Bureau of Standards, Male Workers ’Consumer Cooperation Du A 7 B7 V. Description of the invention (/) When the dissolution conditions are 9 ~ 11%, the cellulose can be dissolved. d: After dissolution, the process of spinning, regeneration, water washing, drying and winding is performed. As shown in the fourth step, the cellulose solution is passed through the gear pump (3 Γ) and sent through the olfactory filament head (3 2). The regeneration tank (3 3), the water washing wheel (3 5), and the drying wheel (3 6) are wound into the finished yarn by the winder (3 7). This is a well-known process and will not be described anymore. However, there is a difference. When the spinning is washed with pure water (3 3) of the washing wheel (3 Γ), a dilution solution containing 4% solvent and 96% water will be produced. This dilution solution is then used by two pumps (3 8) Pumped to the regeneration tank (3 3) 'Used as the regeneration liquid for recycling, its concentration is controlled at 6% solvent and 94% water. The overflow liquid of the regenerated liquid is sent to the solvent recovery (40) department where it is recovered as a solvent for repeated use. e: Solvent recovery This process is carried out in coordination, as shown in the fifth figure is the solvent recovery process; when the regeneration liquid is filtered outside the UF limit (u 11 ra-F i 11 er) 4 R 0 reverse osmosis concentration (R everse-0 sm 〇sis) steam concentration-resin exchange and other steps, SP get recovered solvent. Because the invention adopts low temperature and low cracking in the dissolving stage and recycles the sufficient solvent in the spinning stage, the consumption is low, and the recovery efficiency can reach 99.2% K. After explaining the process from K, the following describes the innovative effects of the present invention;
㈠·擴大纖維素原料來源，因本發明所使用之溶劑具 有極好之溶解能力，故本發明適甩之纖維素除了 〇： —纖雄素（a - Cellulose) 9 0 % K上，及長度4咖K -----,11 裝------訂-----^ .線 (請先閲讀背面之注意事項再填寫本頁) 本紙伕尺度適用中國國家標準（CMS ) Α4規格（210X297公釐} 83.5 5,000 0.88 3〇3396 A7 B7___ ι、發明説明（》） 上之長纖維外，低α —纖維素（α — C e 1 1 u 1 〇 s e)之短纖 維，甚至非溶解性紙槳均可的量摻周，適用纖維原料廣泛 而沒有選擇困難性。尤其本發明之溶劑對各種長、短纖維 均具有良好膨潤效果，其比較如附件一表列所示： 因此長、短纖維素均能因本發明之混合溶劑而具有良 好膨潤性、助溶及溶解效果。 ㈡·提昇溶解能力，本發明之溶劑均符合膨潤性大、 溶解濃度高、溶解速度快、溶解後之聚合度為8QQ以上，溶 劑及再生液之成份相似等條件，下表即為本發明之溶劑與 其它溶劑溶解試驗之比較，如附件二所示。 Θ ·降低溶液黏度，影響溶液粘度之變數含⑴纖維素 聚合度⑵纖維素濃度⑶溫度⑷溶劑姐成等，若將⑴、⑵、 (3)條阵固定，溶劑之组成與溶液粘度關係如附件三所示。 本發明在相同條件下，粘度較m —氧化甲基瑪琳為低 12 %，故可降低纺絲溫度5至1 〇 ，減少溶劑裂解，幫助 回收率之提昇，可提高3至8%之回收率。 ---------{—裝------訂-----{.線 (請先閲讀背面之注意事項再填寫本頁) 經濟部中央棣準局貝工消費合作社印製 退退 衰衰 度易 合極 聚下 素之 維溫 纖高 少間 減時.，作 解用速 . 長象操溶使快 ㈣在琨 3 可⑵下 度該 仍 壓 合低 下 減 下 KV ο ο 11 至 降 度 溫 聚降 因而 法式 劑方 溶種 接三 直採 之明 知發 習本 度 溫 此 在 強 力 能 解 溶 因 在%0 薄 成 刮 而 器 發 蒸 。 膜 素薄 維合 纖配 之，到 上合份 K 捏水 %溫除 20低油 至 解 溶 8 迅 能 即 % 本紙張尺度適用中國國家橾準（CNS ) A4規格（210X297公釐） 83.5 5,〇〇〇 〇-88 五、 發明説明（今） A7 B7 (3) ·如前所述加入之抗聚合度衰退劑。 ㈤.降低溶劑成本； (1)本發明之混合溶劑各單價之加權平均值得較單一氧 化申基瑪琳為低，如附件四所示。 ⑵因本發明之溶液钻度較低，聚合度高，溶解時間由 二小時降至五分鐘，故纺絲溫度可降低至5〜1 Ο Ό，溶劑裂 解程度降低，回收率可提高至99.2%K上。 ㈥‘提高產品物性；使闬本發明所製成之缴維素溶液 抽絲後所得成品絲之物性與習用製法比較，確有明顯之提 升： 經濟部中央揉隼局貝工消費合作社印製 纺絲速度 丹 尼 乾強度 溼強度 伸 率 熱水收縮率 聚合度 本發明 習甩 1000〜1500 m/fflin 100〜150 i/m i η (公尺/分） 120丹尼 5 . 2 g / d K 上 (克/丹尼 7 〜4 . 5 g / d 9 〜12% 1% K下 500〜800 120丹尼 2 . 0〜2 . 7g/d 1.6〜2.2g/d 18〜24% 10 〜12% 320〜360 綜上所述，高濃度、低黏度、低聚合衰退之優點，適 於1 0 0 0 m / m i η (公尺/分）Μ上之高速纺絲，產製出高性能之 纖維產品。又，纖維素原料來源範圍大，溶劑取得成本及 -11- 本紙張尺度適用中國國家標準（CNS ) Α4規格（210Χ297公釐〉 83.5 5,000 0.88 --------.一丨裝------訂-----；.線 (請先閲讀背面之注意事項再填寫本頁) A7 B7 五、發明説明（（Ό) 消耗蠆均低，成本競爭力強，且溶劑回收率高，污染性低 ，公害問題大幅改善。係一極為新式、高度創作之新發明 ，應符專利申請要件，爰依法提出申請。 I---------裝------訂----L 線 (請先閱讀背面之注意事項再填寫本頁) 經濟部中央標準局貝工消費合作社印製 -1.2- 本紙張尺度適用中國國家梯準（CNS ) Α4規格（210X297公釐） 83_5 5,000 0.88(1) Expanding the source of cellulose raw materials, because the solvent used in the present invention has excellent dissolving power, so the suitable cellulose to be thrown away in the present invention is 0:-Cellulose (a-Cellulose) 90% K, and length 4 Coffee K -----, 11 Pack ------ Order ----- ^. Line (please read the precautions on the back before filling this page) This paper is applicable to the Chinese National Standard (CMS) Α4 Specifications (210X297 mm) 83.5 5,000 0.88 3〇3396 A7 B7___ ι, invention description ("), in addition to the long fiber, low α-cellulose (α-C e 1 1 u 1 〇se) short fiber, even non- The dissolving paper paddle can be mixed in various amounts, suitable for a wide range of fiber materials without difficulty in selection. Especially, the solvent of the present invention has a good swelling effect on various long and short fibers, and the comparison is shown in the table in Appendix 1: 、 Short cellulose can have good swelling, solubilizing and dissolving effect due to the mixed solvent of the present invention. (2) Improve the dissolving power, the solvents of the present invention are consistent with large swelling, high dissolving concentration, fast dissolving speed, after dissolving The polymerization degree is above 8QQ, and the component phases of the solvent and the regeneration liquid The following table shows the comparison of the dissolution test of the solvent of the present invention with other solvents, as shown in Annex 2. Θ · Variables that reduce the viscosity of the solution and affect the solution viscosity include (1) cellulose polymerization degree (2) cellulose concentration (3) temperature (4) solvent Jiecheng et al., If the ⑴, ⑵, (3) bar arrays are fixed, the relationship between the composition of the solvent and the viscosity of the solution is shown in Annex 3. Under the same conditions, the viscosity of the present invention is 12% lower than that of m-methyl methoxide Therefore, the spinning temperature can be reduced by 5 to 10, solvent cracking can be reduced, the recovery rate can be improved, and the recovery rate can be increased by 3 to 8%. --------- {— 装 ------ Order ----- {. Line (please read the precautions on the back before filling in this page) Printed by the Ministry of Economic Affairs, Central Bureau of Industry and Commerce, Beigong Consumer Cooperatives, the regression temperature and decay rate are easy to gather, and the temperature is high. Reduce time in a short time, for solution speed. Long elephants dissolve to make it fast (3) ⑵ lower degree should still be pressed down to reduce KV ο ο 11 to drop in temperature and temperature to reduce the concentration of the French side Straight-minded knowing that the present temperature is strong and can dissolve because it is thin at% 0 and becomes steamed. It is prepared with plain thin-dimensional synthetic fiber, up to the upper part K, kneading water,% temperature, removing 20, low oil, and dissolving 8, and it can be dissolved quickly. This paper size is applicable to the Chinese National Standard (CNS) A4 specification (210X297 mm) 83.5 5, 〇〇 〇〇-88 V. Description of the invention (present) A7 B7 (3) The anti-polymerization degree decay agent added as mentioned above. (V) Reduce the solvent cost; (1) The weighted average of the unit prices of the mixed solvents of the present invention is worth comparing The single oxide Shenji Marin is low, as shown in Annex IV. ⑵ Due to the low drilling degree and high polymerization degree of the solution of the present invention, the dissolution time is reduced from two hours to five minutes, so the spinning temperature can be reduced to 5 ~ 1 Ο Ό, the degree of solvent cracking is reduced, and the recovery rate can be increased to 99.2% K up. ㈥ 'Improve the physical properties of the product; compare the physical properties of the finished silk obtained after spinning the carbendazim solution made by the present invention with the conventional production method, and there is indeed a clear improvement: The Ministry of Economic Affairs Central Knead Falconry Bureau Bei Gong Consumer Cooperative Printed Textile Silk speed Danny dry strength wet strength elongation hot water shrinkage polymerization degree of the present invention throw 1000 ~ 1500 m / fflin 100 ~ 150 i / mi η (meter / min) 120 Denny 5.2 g / d K on (G / danny 7 ~ 4.5 g / d 9 ~ 12% 1% K under 500 ~ 800 120 danny 2. 0 ~ 2.7 g / d 1.6 ~ 2.2g / d 18 ~ 24% 10 ~ 12% 320 ~ 360 In summary, the advantages of high concentration, low viscosity, and low polymerization decline are suitable for high-speed spinning at 1000 m / mi η (meter / min) Μ to produce high-performance fibers Products. In addition, the source of cellulose raw materials is large, the cost of solvent acquisition and -11- This paper scale is applicable to the Chinese National Standard (CNS) Α4 specification (210Χ297 mm> 83.5 5,000 0.88 --------. ------ Subscribe -----; line (please read the precautions on the back before filling in this page) A7 B7 5. Description of the invention ((Ό) Low consumption, low cost competitiveness, strong The recovery rate of the agent is high, the pollution is low, and the pollution problem is greatly improved. It is an extremely new and highly creative new invention, which should meet the requirements of the patent application and file the application according to the law. I --------- 装 --- --- order ---- L line (please read the notes on the back before filling in this page) Printed by Beigong Consumer Cooperative of Central Bureau of Standards, Ministry of Economic Affairs-1.2- This paper size is applicable to China National Standards (CNS) Α4 specifications (210X297mm) 83_5 5,000 0.88