TW213956B - Acrylic fiber and its production method - Google Patents

Acrylic fiber and its production method Download PDF

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TW213956B
TW213956B TW81101454A TW81101454A TW213956B TW 213956 B TW213956 B TW 213956B TW 81101454 A TW81101454 A TW 81101454A TW 81101454 A TW81101454 A TW 81101454A TW 213956 B TW213956 B TW 213956B
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Taiwan
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fiber
item
patent application
polymer
copolymer
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TW81101454A
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Chinese (zh)
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Jin-Shy Tsay
Shiang-Ing Tarng
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Ind Tech Res Inst
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Abstract

This claim is one method which is used to produce the hard to burn, hygroscopic and porosity acrylic fiber. It features that the vinylidene chloride polymer which contains 20 - 35 % chlorine and 940000 - 1000000 weight average molecule acrylonitrile , is resolved in the solution which contains dimethyl acetamide to become dope containing 18 - 30% polymer. After solidifying the dope, it can be extended 6 - 10 times to produce the modacrylic fiber with porosity, 1 - 6 m2/g surface area and 200 - 600% bibulous rate.

Description

經濟部中央標準局印-· A 6 B6 五、發明說明(1 ) 發明背署 難燃亞克力纖維之國際價格平均在傳统亞克力蒙維之 兩倍以上,附加價值極高。一般難燃性纖雒可由以T四種 方式來製成:摻配(Blending),整理(Finishing),添加 劑(Adding)及化學改質(chemical modification):目前 商品级難燃亞克力纖維均屬於共聚合體型,其中主要以氛 乙稀(vinyl chloride)或偏二氯乙嫌(vinylidene chloride)為共單體(comonomer)。丙稀腈(acrylonitrile) 與氣乙烯或偏二氯乙烯共聚合體所製造出來之纖維,稱之 為副丙烯請(modacry lie)纖維。此等纖維除了具有衣箸用 基本良好性質外,由於其氯含量高而且具有難燃性貢,因 此特別適用於製造家倶裝潢業上之毛毯、窗簾、罩布、壁 布;製衣工業上之兒童衣服、操作員衣服、警察、Μ人制 月艮;背包、假髮等産品。 本案所使用之丙烯腈一偏二氛乙烯共聚合體是以本案 發明人先前所發明之製備方法(中華民國專利第80102369 號(1991) ”難燃性丙烯腈-偏二氛乙烯共聚合物之製備方 法”)製造共聚合體。該案提供了一種製備丙烯腈-镉二氛 乙烯共聚合體之改良製備方法,其中該共聚合物含有30〜 70重量%丙烯腈與70〜30重童%之偏二氛乙烯,以及選擇 性地含有1〜6重量%之未飽和乙烯基的第三共聚合單體, 該方法包含使用氧化還原起始劑,在pH值2至4.5之水溶液 中進行懸浮聚合反應(Suspension Polymerisation),該 起始劑糸统包含0.1〜3重量9ίΓ過硫酸鹽及0.1〜3重量% 之亞硫酸鹽或亞硫酸氫鹽(以單體重量為基準),其改良之 t請先閏讀背面之注意事項再填寫本页) .装· .訂. •線· 甲 4 (210X 297 公簷) - 經濟部中央標準局印装 A 6 _ B6 五、發明説明丨—) 含量相同及機械性質相當下,其纖維之難燃性優於商品级 之難燃亞克力纖維,且纖維橫斷面呈現多孔性,具有優異 之吸il性,很適於衣眼或窗簾等之用途。 本發明之聚合a及纖維主要性質測試方法如下·· (一) 難燃聚丙烯腈聚合體之分子量測試:重量平均分子量 (Mw)及分子量分佈(Mw/Mn)是利用Waters Model 440 Gel-Permeation Chromatograph 測得,以含 0.5 % LiBr之二甲基甲證胺做為溶劑,Column是使用 Bondagel E-Linear ,並以單分佈聚苯乙烯做為校正 標準物。 (二) 聚合體中氯含量測試:氛元素分析是將聚合體置於 oxygen flask中燃燒,經吸收液吸收後以汞離子滴定。 (三) 纖維表面積是莉用Micromer丨tics (FlowsorbI 2300) 測得。 (四) 纖維表面及橫新面測試,使用電子頭微鏡(SEM, C a ra b r i d g e S - 3 S 0 )觀察之。 (五) LOI值測試:LCI值(Limiting Oxygen Index)是使用 日本專利JP62579i2 (1987)方法測試。 (六) 單根纖維之機搣性質:以弘逹公司之萬能強力試驗機 (Type 8104)測試,夾頭速度lOmm/m丨η,隔距長 本發明方法所製造難燃亞克力纖維可以藉以下實施例 加以進一步說明,該等實施例僅作為説明之用,而非用於 限制本發明範圍。 (請先閲讀背面之注意事項再填寫本頁) .¾. _訂· •線. 甲 4(210X297 公发) 78. 8. 3,000 經濟部中央標準局印¾ 2139k A6 B6 五、發明説明i 5 以中華民國專利第801023(39號之難燃性丙烯腈一偏二 氛乙烯兵聚合體之製備方法所生産之難燃亞克力聚合, 其聚合3重量平均分子量約1.5X105〜6.4X105,聚合 體中氯含量26-29%:将聚合體在80°C及氮氣下,置於二 甲基乙1胺中攪拌二小時溶解形成紡絲液,聚合體含量20 〜24%間。攪拌均勻後之紡絲液經脱泡、過濾、纺絲(纺 嘴規格L/D = l, D = 0.06nnn)、凝固及水洗後在沸水中牽伸, 再經乾燥定型後所測得之纖維性質。 實施例1 纺结步驟如上所述,纺絲及聚合體燦件如下:難燃亞 克力聚合體之重量平均分子量6.4X105,分子量分佈5.5, 聚合體中氯含量27%,纺絲液中聚合體含量24%,凝固液 饶件55% DMAC,溫度40°C,牽伸δ倍,·纺絲後所得纖維強 度為3.68g/d, ί申度13.67%, LOI值44,纖維束中纖雒不 會粘在一起,如圖1所示,纖維表面有直線型凹檜,如圖 2所示,纖雄橫斷面呈現多孔狀,如圖3所示。 實施例2 難燃亞克力聚合體之重量平均分子量5.4Χ105 ,分 子量分佈Mw/Mn值3,聚合體中氛含量28%,纺絲液中聚合 體含量24%,凝固液60%DMAC,溫度30°C,牽伸倍率8, 纺絲後所得纖維強度為3.5 g/d,伸度14,8%, L0I值 44.8。依此筷件製備餓維束中纖維不會粘在一起,如圖4 所示,纖維表面及橫斷面分別如圖5及圖6所示。 (請先閱讀背面之注意事項再填寫本页) •装· -訂· •綠. 甲 4(210X 297公发) 經洚奸中央標準局印¾ A 6 B6 五、_發明説明 2) 處在於該氧化®原起始劑条統,尚含有一約O.lppm至約 5ρριπ (以單體重量為基準)之可提供二價或三價鐵離子之 化合物。 難燃亞克力纖維如美國Union Carbide Chemicals公 司所生産之商品Dyne 1,是將40丙烯腈160氯乙烯共聚合體, 以溶於丙酮形成21%濃度的纺絲液(dope),經乾式纺絲而 製得。Verel 是美國 Eastman Chemical Products公司所 製造的産品,是以40%丙烯腈及60%偏二氣乙烯共聚合體 在丙酮中製成紡絲液,在水中以濕式纺絲製得。Teklan是 英國Courtaulds公司所研製,其共聚合體偽使用等重量 比例的偏二氯乙烯和丙烯腈,再配以少量的其他物質,如 衣康酸(itaconic acid),然後將聚合體溶於丙酮溶劑中 ,製成22%聚合體丙0¾钻液後纺絲。Kanekalon是日本 Kanegafuchi公司之産品,是以60%丙烯腈與40%氛乙烯 共聚合體溶解於乙腈溶劑,然後於乙腈水溶液中濕式纺絲 而製得。 日本專利(公開恃許公報昭62-57911及昭62-57912 (1987))是以40重量%以上丙烯腈,20〜60重量% 偏二氯乙烯及5重量%以下第三共單體共聚合之改質亞 克力(modacrylic),聚合體中加入少量之Sb2 〇s,並且 以二甲基甲醒胺(dimethyl formamide,DMF)為溶劑,製 造高難燃性改質亞克力纖維。 從以上可知除日本專利使用DMF為溶劑製造高難燃性 改質亞克力纖維外,一般商品级難燃亞克力纖維均使用丙 酮或乙腈為溶劑。而本發明之恃色是使用懸浮聚合製造難 甲 4(210X297 {請先閲讀背面之注意事項再填寫本頁) .裝· •訂. 歿洚部中央铭準局印-· A 6 _____ B6 五、發明説明;3 ) 燃亞克力聚合體,其後在so;c氮氣下溶解於二甲基乙證胺 (dimethyl acetam丨de,DMAC)溶剤,在二甲基乙酵胺/水 溶液中抽絲,可製得具高難燃性,高吸濕性及多孔性之亞 克力纖·維,其産品特性是習知技術所製得之難燃亞克力纖 維所不及的。 發明夕譁細説明 本發明所使用之丙烯-偏二氛乙烯共聚合體是利用 中華民國專利第80102369號之方法製備,該方法是使用 水溶液懸浮聚合,其主要待點:(一)使用優良之觸媒,如 過硫酸胺、亞硫酸氫鈉及硫酸、亞鐵,可以提高反應速率 ,使反應時間在2小時以内,單謾轉化率(con vers ion)可 達80%以上。(二)接近常溫及常壓反應,適合於現有傳統 聚丙烯腈之聚合設備,可以提高附加價值及降低成本: 傳統聚丙烯腈纖維(亞克力纖維)使用有機溶劑做溶劑 者佔大多數,包括二甲基甲韹胺、二甲基乙醯胺及二甲亞 ® (dimethyl sul fox丨de, DMS0)等溶劑,若製造難燃亞克 力纖維也使用與一般级亞克力纖雏相同之溶劑,除方便管 理外,也可以使用相同的溶割回收設備,降低生産成本。 目前商品级的難燃亞克力潘維,主要是使用丙ar及乙睹做 為溶劑,且生産扁平横斷面織維,其適用於玩具及地毯等 。雖然日本專利(JP6257911及JP6257912)中是使用二甲基 甲醯胺做為溶劑,但其使用Sb2 0S添加劑來提高其難燃 性,並且無待殊之纖維橫斷面及吸濕性等性質。本發明之 難燃亞克力纖維是使用二甲基乙韹胺做為溶劑纺絲,在氛 {請先閲讀背面之注意事項再填寫本頁) •裝. .訂· •綠· 甲 4(210X297X 沒) A 6 B6 經濟部中央標準局印裂 三、發明釔明(6 J 比較例1 難燃亞克力聚合體之重量平均分子量6.4X105,分 子量分佈5.5,聚合體中氯含量27%,纺絲疲中聚合證含 量24%,凝固液DMAC濃度55%,溫度203C,牽伸倍率8, 纺絲後所得纖維強度為1.69g/d,伸度13.02%, LOI值49 依此條件裝備纖維束中纖維粘在一起,如圖7所示,缓維 橫斷面層孔分佈,如圖8所示,纖維表面有明顯裂痕,如 圖9所示。 比較例2 難燃亞克力聚合體之重量平均分子量6.4X10S,分 子量分佈5.5,聚合體中氯含量27%,纺絲液中聚合體含 量24%,凝固液100%水,溫度30°C,牽伸倍率8,纺絲後 所得纖維強度為1.7g/d,伸度14.6%, L0I值49。依此條 件裝備纖維束中纖維粘在一起,如圖10所示,纖維橫斷面 層孔分佈,如圖11所示,纖維表面有明顯裂痕,如圖12所 不。 本發明所使用之難燃亞克力聚合體,使用二甲基乙醯 胺做溶劑,在常溫下溶解性不佳,在N2氣體下60°c以上 可完全溶解,但以80°C最佳。聚合體含量在24%以下可以 完全溶解,如表1所示,聚合體含量在20〜40%範圍時, 聚合體含量提高,紡絲液粘度隨之提高,但聚合體含量於 26%時,纺絲液粘度反而下降,表示有部份聚合體未完全 溶解。 (請先閱讀背面之注意事項再填寫本页) -装· .訂· -綠· 甲 4(210X 297 公发) A 6 B6 五、诠明( 7 ) 表1 難燃亞克力聚合體含量對纺絲液粘度之影響 聚合體含量(%) 紡絲液粘度(CPS)::: 20 2,600 22 9,600 24 ' 9,800 26 4,700 在80t下測試 (請先閱"背面之注意事項再填寫本頁) 為了顯示本發明之難燃亞克力纖維待性與進步性,與 現有商品做比較,如表2及圖13所示。由結果顯示本發明 之纖維在同樣氛含量下,表面積比商品级産品高,LOI值 也較高,故防火效果較佳,且纖維吸濕率比商品级佳,吸 濕後乾燥性又優於目前商品级産品。亞克力纖維氛含量相 同下,LOI值較高的原因是纖維多孔性,表面積較大,HC1 裂解較快所造成,而HC1是主要的滅火化合物。 裁解I明之難飽段酿趟比較 樣品 Mw 氣含量(%) LOI值(%)表翻(raVg)含水率(%)2含水率(%) KANEKAL0N» 1.5X105 26.1 39.4 0.79 318 247 SNIAi^t 5.4X105 28.1 38.9 0.34 245 221 6.4X105 27.3 43 5.16 510 137 經 濟 部 中 央 標 準 局 印 1. 沸水輔鱗;2.繼腿濕讎续溫VJ艰粒含轉,Printed by the Central Bureau of Standards of the Ministry of Economic Affairs-· A 6 B6 V. Description of Invention (1) Backing of Invention The international price of flame retardant acrylic fiber is more than twice that of traditional acrylic Mengwei, and the added value is extremely high. The general flame retardant fiber can be made in four ways: blending, finishing, additives and chemical modification: at present, commercial grade flame retardant acrylic fibers are all common Polymer type, which mainly uses vinyl chloride or vinylidene chloride as the comonomer. The fibers made from the copolymer of acrylonitrile and gaseous ethylene or vinylidene chloride are called modacry lie fibers. In addition to the basic good properties of these clothes, these fibers are particularly suitable for the manufacture of blankets, curtains, drapes and wall coverings in the home decoration industry because of their high chlorine content and flame retardant properties; Children's clothing, operator's clothing, police, M-made Yue Gen; backpacks, wigs and other products. The acrylonitrile-vinylidene chloride copolymer used in this case is based on the preparation method previously invented by the inventor of this case (Republic of China Patent No. 80102369 (1991) "Preparation of flame-retardant acrylonitrile-vinylidene chloride copolymer Method ") manufacture of interpolymers. This case provides an improved preparation method for the preparation of acrylonitrile-cadmium dihydrogen ethylene copolymer, wherein the copolymer contains 30 to 70% by weight of acrylonitrile and 70 to 30% by weight of vinylidene dichloride, and selectively A third comonomer containing 1 to 6% by weight of unsaturated vinyl groups. The method includes the use of a redox initiator to perform suspension polymerization (Suspension Polymerisation) in an aqueous solution with a pH of 2 to 4.5. The agent system consists of 0.1 ~ 3 weight of 9μΓ persulfate and 0.1 ~ 3% by weight of sulfite or bisulfite (based on the weight of the monomer). For its improvement, please read the notes on the back before filling in This page) .Installed. .Ordered. • Line · A 4 (210X 297 common eaves)-Printed by the Central Bureau of Standards of the Ministry of Economic Affairs A 6 _ B6 V. Description of invention 丨 —) The content is the same and the mechanical properties are equivalent. The flame retardancy is better than commercial grade flame retardant acrylic fiber, and the fiber cross section is porous, with excellent il absorption, and is very suitable for the purpose of clothing eyes or curtains. The test methods for the main properties of the polymerization a and the fiber of the present invention are as follows: (1) The molecular weight test of the flame-retardant polyacrylonitrile polymer: the weight average molecular weight (Mw) and molecular weight distribution (Mw / Mn) are based on Waters Model 440 Gel-Permeation Chromatograph measured using 0.5% LiBr in dimethyl methyl amine as the solvent, Column used Bondagel E-Linear, and single-distribution polystyrene as the calibration standard. (2) Chlorine content test in polymer: Atmospheric element analysis is to put the polymer in an oxygen flask and burn it. After being absorbed by the absorption liquid, it is titrated with mercury ions. (3) The fiber surface area is measured by Micromerstics (FlowsorbI 2300). (4) Testing of the fiber surface and the transverse new surface, using an electronic head micro-mirror (SEM, Carra b r i d g e S-3 S 0) to observe it. (5) LOI value test: The LCI value (Limiting Oxygen Index) is tested using the method of Japanese Patent JP62579i2 (1987). (6) Mechanical properties of single fiber: tested by HongYu Universal Strength Testing Machine (Type 8104), chuck speed lOmm / m 丨 η, long separation distance The flame retardant acrylic fiber produced by the method of the present invention can be borrowed as follows The embodiments are further described. The embodiments are only for illustrative purposes, and are not intended to limit the scope of the present invention. (Please read the precautions on the back before filling in this page). ¾. _ Order · line. A 4 (210X297 public issue) 78. 8. 3,000 Printed by the Central Bureau of Standards of the Ministry of Economic Affairs ② 2139k A6 B6 V. Description of invention i 5 The flame retardant acrylic polymerization produced by the preparation method of the flame retardant acrylonitrile-vinylidene polymer of No. 801023 (No. 39 of the Republic of China), which has a polymerization weight average molecular weight of about 1.5X105 ~ 6.4X105, in the polymer Chlorine content 26-29%: The polymer is placed in dimethyl ethyl amine at 80 ° C and nitrogen and stirred for two hours to dissolve to form a spinning solution. The polymer content is between 20 and 24%. Fibre properties measured after defoaming, filtering, spinning (spinning nozzle specifications L / D = l, D = 0.06nnn), coagulation and water washing, drawing in boiling water, drying and shaping. 1 The spinning process is as described above. The spinning and polymer parts are as follows: the weight average molecular weight of the flame retardant acrylic polymer is 6.4X105, the molecular weight distribution is 5.5, the chlorine content in the polymer is 27%, and the spinning polymer content is 24% , 55% DMAC for coagulation liquid, temperature 40 ° C, drawing δ times, the fiber strength after spinning is 3.68 g / d, ί Shen 13.67%, LOI value 44, fiber lobe in the fiber bundle will not stick together, as shown in Figure 1, the surface of the fiber has a linear concave cypress, as shown in Figure 2, the cross section of the male fiber It is porous, as shown in Figure 3. Example 2 The weight average molecular weight of the flame retardant acrylic polymer is 5.4X105, the molecular weight distribution Mw / Mn value is 3, the atmosphere content in the polymer is 28%, and the spinning liquid content is 24% , Coagulation liquid 60% DMAC, temperature 30 ° C, draft ratio 8, fiber strength after spinning is 3.5 g / d, elongation 14,8%, L0I value 44.8. According to the chopsticks, the fibers in the hungry dimensional bundle are prepared It will not stick together, as shown in Figure 4, the fiber surface and cross section are shown in Figure 5 and Figure 6. (Please read the precautions on the back before filling this page) • Install ·-Order · • Green. A 4 (210X 297 public issue) Printed by the Central Bureau of Standards and Abilities ¾ A 6 B6 V. _Invention Description 2) The original initiator system of Oxidation® still contains about 0.1 ppm to about 5 ρριπ (with The weight of the monomer is based on a compound that can provide bivalent or trivalent iron ions. Flame-retardant acrylic fiber, such as Dyne 1, produced by Union Carbide Chemicals of the United States, is made by dry spinning of 40 acrylonitrile 160 vinyl chloride copolymer, dissolved in acetone, to form a 21% concentration dope. Get. Verel is a product manufactured by Eastman Chemical Products in the United States. It is made from 40% acrylonitrile and 60% vinylidene fluoride copolymer in acetone and wet spinning in water. Teklan was developed by Courtaulds in the UK. Its copolymers pseudo-equalize vinylidene chloride and acrylonitrile with a small amount of other substances, such as itaconic acid, and then dissolve the polymer in acetone. In the process, 22% polymer acrylic fluid was prepared and spun. Kanekalon is a product of Kanegafuchi Corporation of Japan. It is prepared by dissolving 60% acrylonitrile and 40% vinyl chloride copolymer in acetonitrile solvent, and then wet spinning in acetonitrile aqueous solution. Japanese patents (Public Publications No. Sho 62-57911 and Sho 62-57912 (1987)) are copolymerization of 40% by weight or more of acrylonitrile, 20 ~ 60% by weight of vinylidene chloride and 5% by weight or less of a third comonomer Modified acrylic (modacrylic), a small amount of Sb2 〇s is added to the polymer, and dimethyl formamide (DMF) is used as a solvent to produce highly flame-retardant modified acrylic fibers. As can be seen from the above, except that Japanese patents use DMF as a solvent to produce highly flame-retardant modified acrylic fibers, general commercial grade flame-retardant acrylic fibers use acetone or acetonitrile as solvents. The color of the present invention is the use of suspension polymerization to manufacture refractory 4 (210X297 (please read the precautions on the back before filling in this page). Installed • • Ordered. The Central Bureau of the Ministry of the Ministry of the Ministry of Central Affairs--A 6 _____ B6 5 3. Description of the invention; 3) Acrylic polymer burning, then dissolved in dimethyl acetamidine (DMAC) under nitrogen gas; so as to draw silk in dimethylacetamide / water solution, Acrylic fiber with high flame retardancy, high hygroscopicity and porosity can be prepared. Its product characteristics are beyond the flame retardant acrylic fiber made by the conventional technology. Detailed description of the invention The propylene-vinylidene ethylene copolymer used in the present invention is prepared by the method of Republic of China Patent No. 80102369. This method uses suspension polymerization of aqueous solution, and its main points are: (1) Use excellent The medium, such as ammonium persulfate, sodium bisulfite, sulfuric acid and ferrous iron, can increase the reaction rate, make the reaction time within 2 hours, and the single conversion rate (con vers ion) can reach more than 80%. (2) Close to normal temperature and normal pressure reaction, suitable for the existing traditional polyacrylonitrile polymerization equipment, which can increase the added value and reduce costs: Traditional polyacrylonitrile fiber (acrylic fiber) uses organic solvents as the solvent, including the second Solvents such as methyl methylamine, dimethylacetamide and dimethyl sulfoxide (dimethyl sul fox 丨 de, DMS0), if the flame retardant acrylic fiber is manufactured, the same solvent as the general-grade acrylic fiber is used, except for convenient management In addition, the same solution cutting recovery equipment can also be used to reduce production costs. At present, commercial grade flame-retardant acrylic panwei mainly uses propylene and ethene as solvents, and produces flat cross-sectional weaves, which are suitable for toys and carpets. Although Japanese patents (JP6257911 and JP6257912) use dimethylformamide as a solvent, it uses Sb2 0S additives to improve its flame retardancy, and it does not need special properties such as fiber cross section and hygroscopicity. The flame-retardant acrylic fiber of the present invention uses dimethyl ethyl amine as the solvent spinning, in the atmosphere {please read the precautions on the back and then fill out this page) • Installed. Ordered • • Green · A 4 (210X297X no ) A 6 B6 Printed by the Central Bureau of Standards of the Ministry of Economy III. Invented Yttrium Ming (6 J Comparative Example 1 The weight average molecular weight of the flame retardant acrylic polymer is 6.4X105, the molecular weight distribution is 5.5, the chlorine content in the polymer is 27%, and the spinning is fatigued The content of the polymerization certificate is 24%, the concentration of DMAC in the coagulating liquid is 55%, the temperature is 203C, the draw ratio is 8. The fiber strength after spinning is 1.69g / d, the elongation is 13.02%, and the LOI value is 49. Together, as shown in Figure 7, the pore distribution of the slow-dimensional cross-sectional layer, as shown in Figure 8, has obvious cracks on the fiber surface, as shown in Figure 9. Comparative Example 2 The weight average molecular weight of the flame retardant acrylic polymer is 6.4X10S , Molecular weight distribution 5.5, chlorine content in the polymer is 27%, polymer content in the spinning solution is 24%, coagulation liquid is 100% water, temperature is 30 ° C, draft ratio is 8, the fiber strength after spinning is 1.7g / d , Elongation 14.6%, L0I value 49. According to this condition, the fibers in the fiber bundle stick together, as shown in Figure 10, the fiber The distribution of pores in the cross-section is shown in Figure 11, and there are obvious cracks on the surface of the fiber, as shown in Figure 12. The flame-retardant acrylic polymer used in the present invention uses dimethylacetamide as a solvent and dissolves at room temperature Poor performance, it can be completely dissolved under N2 gas above 60 ° C, but it is best at 80 ° C. The polymer content can be completely dissolved below 24%, as shown in Table 1, the polymer content is in the range of 20 ~ 40% When the polymer content increases, the spinning solution viscosity increases, but when the polymer content is 26%, the spinning solution viscosity decreases instead, indicating that some of the polymer has not completely dissolved. (Please read the precautions on the back side first (Fill in this page) -Package · Order ·-Green · A 4 (210X 297 public) A 6 B6 V. Interpretation (7) Table 1 Effect of flame retardant acrylic polymer content on the viscosity of spinning solution %) Spinning fluid viscosity (CPS) ::: 20 2,600 22 9,600 24 '9,800 26 4,700 Tested at 80t (please read the "Notes on the back before filling in this page") In order to show the flame retardant acrylic fiber of the present invention Sex and progress, compared with existing products, as shown in Table 2 and Figure 13 The results show that the fiber of the present invention has a higher surface area than commercial products at the same atmosphere content and a higher LOI value, so the fireproof effect is better, and the fiber moisture absorption rate is better than commercial grade, and the drying after moisture absorption is superior At present, commercial grade products. Under the same acrylic fiber atmosphere content, the higher LOI value is due to the porosity of the fiber, the larger surface area, and the faster cracking of HC1, which is the main fire extinguishing compound. Dissecting the comparison of the samples from the difficult-to-saturated section of the Ming Dynasty Mw gas content (%) LOI value (%) table turn (raVg) moisture content (%) 2 moisture content (%) KANEKAL0N »1.5X105 26.1 39.4 0.79 318 247 SNIAi ^ t 5.4X105 28.1 38.9 0.34 245 221 6.4X105 27.3 43 5.16 510 137 Printed by the Central Standards Bureau of the Ministry of Economic Affairs 1. Boiling water auxiliary scale; 2. After the leg wet claw continued temperature VJ hard grain contains the transfer,

A 8 BS 經濟部中央標準局印裝 圖式 圖1難燃亞克力纖維照片(X20) 圖2難燃亞克力纖維之表面SEM照片(X 1000) 圖3 難燃亞克力纖維之橫斷面SEM照Η (X 1000) 圖4 難燃亞克力纖維束之照片(Χ20) 圖5 難燃亞克力纖維之表面SEM照片(Χ 1000) 圖6難燃亞克力纖雒之橫斷面SEM照片(X 1000) 圖7 難燃亞克力纖維束之照片(xk〇) 圖8難燃亞克力纖維之橫斷面SEM照片(X 1000) 圖9難燃亞克力纖維之表面SEM照片(X 1000) 圖10 難燃亞克力纖雏束之照Η (X20) 圖11難燃亞克力纖雒之橫斷面SEM照片(X 1000) 圖12 難燃亞克力纖維之表面SEM照片(X 1000) (A) SNIA(XSOO) (B) KANEKALON ( x 500) (C)本發明之纖維(x 1000) 圖13 難燃亞克力纖維橫斷面比較 ί請先聞讀背函之注意事頊再行缚製) • JiT. 甲 Ί(210Χ 297 公尨)A 8 BS Printed pattern of the Central Bureau of Standards of the Ministry of Economy Figure 1 Photograph of flame retardant acrylic fiber (X20) Figure 2 SEM photograph of the surface of flame retardant acrylic fiber (X 1000) Figure 3 SEM photo of the cross section of flame retardant acrylic fiber ( X 1000) Figure 4 Photograph of flame retardant acrylic fiber bundle (Χ20) Figure 5 SEM photograph of surface of flame retardant acrylic fiber (Χ1000) Figure 6 Cross-sectional SEM photo of flame retardant acrylic fiber lo (X 1000) Figure 7 Flame retardant Photograph of acrylic fiber bundle (xk〇) Figure 8 SEM photo of the cross section of flame retardant acrylic fiber (X 1000) Figure 9 SEM photo of the surface of flame retardant acrylic fiber (X 1000) Figure 10 Photograph of flame retardant acrylic fiber embryonic beam (X20) Figure 11 SEM photograph of the cross section of flame retardant acrylic fiber (X 1000) Figure 12 SEM photograph of the surface of flame retardant acrylic fiber (X 1000) (A) SNIA (XSOO) (B) KANEKALON (x 500) ( C) The fiber of the present invention (x 1000) Fig. 13 Comparison of the cross-section of flame-retardant acrylic fiber. Please read the notes on the back letter before binding) • JiT. 甲 Ί (210Χ 297 公 尨)

Claims (1)

修補充 A7 B7 C7 D7 ='申請專利範面 經濟部中央標準局员工消費合作社印製 1. 一種製備高難燃、高吸濕及多孔性之亞克力纖維的方法, 其特擻係氣含量20〜35%,重量平均分子量9.〇Χ1〇4 〜1.ΟΧΙΟ6之含丙烯腈一偏二氯乙烯共聚合體,溶解於 二甲基乙醯胺溶劑或含有二甲基乙醯胺之溶劑中,做成 聚合體含量18〜30%之紡絲液,經凝固液濕式紡絲後, 牽伸6〜10倍製得多孔性改質亞克力纖維,其纖維表面 積為1〜6^4,纖維吸水率為200〜600%。 2. 如申請專利範圍第1項所述之方法,其中含丙烯腈一偏 二氣乙烯共聚合體之重量平均分子量為1.0Χ105〜7.0 x 10s ,氛含量25〜29%。 3. 如申請專利範圍第1項或第2項所述之方法,其中共聚 合體溶解在含有二甲基乙醯胺溶劑下,聚合體含量20〜 26% 0 4. 如申請專利範圍第1項或第2項所述之方法,其中共聚 合體溶解的溫度為60〜90¾。 5. 如申請專利範圍第1項所述之方法,其中濕式紡絲的凝 固液二甲基乙醯胺濃度為20〜65%,溫度20〜40 °C。 (請先閲讀背面之注意事項再填寫本頁) 丨裝 订. .'*6^. 本紙张又度適用中國园家橒準(CNS)甲4規恪(210 X 297公兑〉 81.9.10,000Repair supplement A7 B7 C7 D7 = 'Patent application for printing Printed by Employee Consumer Cooperative of the Central Bureau of Standards of the Ministry of Economy 1. A method for preparing highly flame-retardant, highly hygroscopic and porous acrylic fibers with a special gas content of 20 ~ 35%, weight average molecular weight 9.〇Χ10〇4 ~ 1.ΟΧΙΟ6 acrylonitrile-containing vinylidene chloride copolymer, dissolved in dimethylacetamide solvent or a solvent containing dimethylacetamide, do A spinning solution with a polymer content of 18 to 30%, after wet spinning of the coagulating solution, a porous modified acrylic fiber is prepared by drawing 6 to 10 times, and its fiber surface area is 1 to 6 ^ 4, fiber water absorption rate 200 ~ 600%. 2. The method as described in item 1 of the patent application, in which the weight average molecular weight of the vinylidene-vinylidene copolymer containing acrylonitrile is 1.0 × 105 ~ 7.0 x 10s, and the atmosphere content is 25 ~ 29%. 3. The method as described in item 1 or item 2 of the patent application scope, in which the copolymer is dissolved in a solvent containing dimethylacetamide, the polymer content is 20 ~ 26% 0 4. If the patent application item 1 Or the method according to item 2, wherein the temperature at which the copolymer is dissolved is 60 to 90¾. 5. The method as described in item 1 of the patent application scope, in which the concentration of dimethylacetamide in the wet spinning solid solution is 20 to 65% and the temperature is 20 to 40 ° C. (Please read the precautions on the back before filling in this page) 丨 Binder ... '* 6 ^. This paper is again applicable to China Yuanjia Luzhun (CNS) A4 (210 X 297 public exchange rate) 81.9.10,000
TW81101454A 1992-02-25 1992-02-25 Acrylic fiber and its production method TW213956B (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
TWI381075B (en) * 2005-08-09 2013-01-01 Teijin Ltd Double layer fabric and the use of its heat-resistant protective clothing

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
TWI381075B (en) * 2005-08-09 2013-01-01 Teijin Ltd Double layer fabric and the use of its heat-resistant protective clothing

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