TW487745B - High speed melt spinning of fluoropolymer fibers - Google Patents

High speed melt spinning of fluoropolymer fibers Download PDF

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Publication number
TW487745B
TW487745B TW89102512A TW89102512A TW487745B TW 487745 B TW487745 B TW 487745B TW 89102512 A TW89102512 A TW 89102512A TW 89102512 A TW89102512 A TW 89102512A TW 487745 B TW487745 B TW 487745B
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Taiwan
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spinneret
spinning
patent application
temperature
scope
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TW89102512A
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Chinese (zh)
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William Cheng Uy
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Du Pont
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Abstract

The processes and apparatus of the present invention concerns melt spinning high viscosity fluoropolymers into single filaments or multi-filament yarns at high spinning speeds. A process for melt spinning a composition comprising a highly fluorinated thermoplastic polymer or a blend of such polymers, comprising the steps of: melting a composition comprising a highly fluorinated thermoplastic polymer or a blend of such polymers to form a molten fluoropolymer composition; conveying said molten fluoropolymer composition under pressure to an extrusion die of an apparatus for melt spinning; and extruding the molten fluoropolymer composition through the extrusion die to form filaments, said die being at a temperature of at least 450 DEG C, at a shear rate of at least 100 sec<SP>-1</SP>, at a spinning speed of at least 500 m/min.

Description

487745487745

五、發明說明(1) 發明背景 置係有關於 絲紗線。 之熱塑性共 的經濟誘因 。面對熔紡 發生破裂, 體破裂出現 降低熔體黏 包括以四氟 聚合物在溶 降解。 以高旋、紡速度冑氟聚合物 聚物之熔紡已為吾人所 驅使這些高價值聚合物須 方法的-個問題是,在高 而在擠壓之纖維上表現成 的臨界剪切、&amp; t &gt; 介^切速率係隨熔體 度的方式都集中在提高熔 乙浠為基底之熱塑性共聚 體黏度可達到任何明顯降V. Description of the invention (1) Background of the invention The device is related to silk yarn. The economic incentives of thermoplastics. In the face of melt-spinning, bulk cracking occurs, and melt viscosity is reduced, including the degradation of tetrafluoropolymer in solution. The problem of melt spinning of fluoropolymer polymers at high spin and spinning speeds has driven me to these high-value polymers. One problem is the critical shear, ; t &gt; the rate of meso-cutting is dependent on the way the melt is focused on increasing the viscosity of the thermoplastic copolymer based on melt ethyl acetate, which can achieve any significant reduction

本發 溶紡成 以四 知。然 以更高 剪切速 表面粗 黏度遞 體的溫 物的許 低之前 明之方 單纖絲 氟乙烯 而,有 速度旋 率下, 糙度。 增而遞 度。然 多聚合 ,便已 法及裝 或多纖 為基底 相當大 紡纖維 熔體會 由於溶減,故而,在 物中, 出現熱 f四氟乙烯(pTFE)均聚物之纖維也是高價值的纖維,尤 =t因其化學及機械性質,如低摩擦係數,熱穩定性及化 學,性。然而,以熔紡加工處理已證明令人困惑。由於聚 四氟^乙烯均聚物纖維習慣上係以包含許多少驟及複雜設備 的为散液旋紡方法來形成,故有很大的經濟誘因來找出一 種熔紡此等纖維之方法。The hair is melt-spun into four knowledge. However, at a higher shear rate, the temperature of the surface coarse viscosity transmitter is lower than that of the single-filament single-filament vinyl fluoride, and there is a roughness under the rate of rotation. Increase and increase. However, if it is polymerized, it will be difficult to melt the melted fibers due to the large size of the fibers. Therefore, the fibers with thermal f-tetrafluoroethylene (pTFE) homopolymer are also high-value fibers. You = t because of its chemical and mechanical properties, such as low coefficient of friction, thermal stability and chemical properties. However, processing with melt spinning has proven confusing. Since PTFE homopolymer fibers are conventionally formed by a spinning spinning method containing many small and complex equipment, there is a large economic incentive to find a method for melt spinning these fibers.

由南黏度聚合物熔體旋紡纖維之問題先前皆係針對於聚 酯。在美國專利3,437,7 25 t,其所描述的喷絲頭總成具 =亡板,加熱板及下板,並在上板與加熱板之間有一提供 空氣空間的隔板。欲旋紡的每一纖絲都有〆中空插入物放 在上板並延伸至下板之底面。熔融聚合物送入插入物之 中’以便通過毛細管旋紡。電加熱器則供應熱量以維持下The problem of spinning fibers from south viscosity polymer melts has previously been directed to polyesters. In US Pat. No. 3,437,7 25 t, the spinneret assembly is described as having a dead plate, a heating plate and a lower plate, and a partition providing an air space between the upper plate and the heating plate. For each filament to be spun, a hollow insert is placed on the upper plate and extends to the bottom of the lower plate. The molten polymer is fed into the insert &apos; for spinning through the capillary. Electric heaters supply heat to maintain

第4頁 487745 五、發明說明(2) 板,加熱板及插入物下部之溫度高於供應之熔融聚合物之 溫度至少60 °C。實例中所列範圍介於29 0與430 C之間的經 加熱毛細管溫度是供旋紡聚酯之用。未提及任何氟聚合物 或以高旋紡速度熔紡氟聚合物所需之溫度。 考务明概述 本發明提供一種熔紡包含高度氟化熱塑性聚合物或此等 聚合物之摻混物之組合物之方法,其包含以下步驟:將包 含高度氟化熱塑性聚合物或此等聚合物之摻混物之組合物 熔解以形成熔融氟聚合物組合物;將該熔融氟聚合物組合 物加壓輸送至熔紡裝置之擠壓模具;及將熔融氟聚合物組 合物擠壓通過擠壓模具以形成熔融纖絲,該模具係在至少 450 °C之溫度下,剪切速度為至少100 sec—1及旋紡速度為 至少500米/分。 本發明也提供一種熔紡包含聚四氟乙烯均聚物之組合物 之方法,其包含以下步驟:將包含聚四氟乙烯均聚物之組 合物熔解以形成熔融聚四氟乙烯組合物;將該熔融聚四氟 乙烯組合物加壓輸送至熔紡裝置之擠壓模具;及將熔融聚 四氟乙烯組合物擠壓通過擠壓模具以形成熔融纖絲。 本發明進一步提供一種包含喷絲頭總成之熔紡纖維之裝 置,其包含過濾裝置;喷絲頭;加長轉移線,該轉移線係 配置於該過濾裝置與該喷絲頭之間;該加長轉移線之加熱 裝置;該噴絲頭之加熱裝置;及配置於該喷絲頭總成以下 之加長退火器。 附圖之簡要說明Page 4 487745 V. Description of the invention (2) The temperature of the lower part of the plate, heating plate and insert is higher than the temperature of the supplied molten polymer by at least 60 ° C. The heated capillary temperatures listed in the examples ranging from 290 to 430 C are for spinning polyester. No mention is made of any fluoropolymer or the temperature required to melt-spin the fluoropolymer at high spin speeds. SUMMARY OF THE INVENTION The present invention provides a method for melt-spinning a composition comprising a highly fluorinated thermoplastic polymer or a blend of such polymers, comprising the steps of: The composition of the blend is melted to form a molten fluoropolymer composition; the molten fluoropolymer composition is conveyed under pressure to an extrusion die of a melt spinning device; and the molten fluoropolymer composition is extruded through extrusion A mold to form molten filaments, the mold is at a temperature of at least 450 ° C, a shear speed of at least 100 sec-1 and a spinning speed of at least 500 m / min. The present invention also provides a method for melt-spinning a composition comprising a polytetrafluoroethylene homopolymer, comprising the steps of: melting the composition comprising a polytetrafluoroethylene homopolymer to form a molten polytetrafluoroethylene composition; The molten polytetrafluoroethylene composition is conveyed under pressure to an extrusion die of a melt spinning device; and the molten polytetrafluoroethylene composition is extruded through the extrusion die to form molten filaments. The present invention further provides a device for melt-spun fibers including a spinneret assembly, which includes a filtering device; a spinneret; and an extended transfer line, the transfer line is arranged between the filtering device and the spinneret; the lengthening The heating device of the transfer line; the heating device of the spinneret; and the extended annealing device arranged below the spinneret assembly. Brief description of the drawings

一部份的剖面圖。 絲頭之熔紡裝置一部份之一具體 圖1為習用熔紡裝置之 圖2為本發明具加長喷 例之剖面圖。 圖3為具縮短加長噴絲 之剖面圖。 頭之熔紡裴置一 部份之一具體例 圖4為本發明具縮短加長 具體例之剖©圖(加敎裝i配置U㉟紡裝置一部份之一 加熱裝置配置在其外表面):置於喷絲頭之中央空腔内及Partial sectional view. A specific part of the melt-spinning device of the silk head is shown in Fig. 1. Fig. 1 is a cross-sectional view of a conventional melt-spinning device. Fig. 3 is a sectional view of a shortened and extended spinneret. Fig. 4 is a sectional view of a specific example of shortening and lengthening according to the present invention (partially equipped with a U-spinning device and a heating device arranged on the outer surface): Placed in the central cavity of the spinneret and

為力圖二為轉本移發線明配熔二裝Λ一具體例之分解剖面®;其特徵 。加長轉移線配置於組合濾器與 圖6為圖5溶纺裝置之經合剖面頭固盤之間。 的ΓΛ本鐘發:月:紡裝置一具體例之分解剖面》;其顯示 的係加長轉移線及噴絲頭之另一具體例。 圖8為圖7熔紡裝置之組合剖面圖。 圖9為本發明熔纺裝置一具體例之概略 圖圖係可用於本發明之徐冷器-具體例之剖面 β 圖10Β為圖10Α —部份之放大圖。An example of the decomposition profile of a specific example of the second embodiment of the transfer line for the transfer of the transfer line is shown; its characteristics. The extension transfer line is arranged between the combined filter and the warp-section head fixing plate of the melt spinning device of FIG. 5. ΓΛ 本 钟 发: Month: An exploded section of a specific example of a spinning device "; another specific example of the extended transfer line and spinneret shown in it. FIG. 8 is a combined sectional view of the melt-spinning device of FIG. 7. Fig. 9 is a schematic view of a specific example of the melt-spinning device of the present invention. The drawing is a cross-section of a specific example of a cooler of the present invention. Fig. 10B is an enlarged view of a portion of Fig. 10A.

圖1 1為Κ例1組合物50 0它時剪切速率(l“ec)對SSF之曲 線圖;其中深色三角形代表最初纖絲斷裂時之紡絲拉伸因 數(SSF )而空心三角形則代表最後纖絲斷裂時之SSF。包括 在内的是旦數/韌度/速度/gpm之一此數據。 圖1 2係一曲線,證明在恒定剪切速率下最先纖絲斷裂時 溫度對SSF所施加之正面影響。圓圈代表在42〇 〇c時之 SSF ;方形代表在4 60 t時之SSF ;及三角形代表在5〇() t時Fig. 11 is a graph of shear rate (l "ec) vs. SSF of the composition of K Example 1 at 50 °; the dark triangle represents the spinning stretch factor (SSF) at the time of initial filament break and the hollow triangle is Represents the SSF at the last filament break. Included is one of denier / toughness / speed / gpm. Figure 1 2 is a curve that proves that the temperature of the first filament breaks at a constant shear rate. The positive influence exerted by SSF. The circle represents SSF at 4200c; the square represents SSF at 4 60 t; and the triangle represents at 50 () t

第6頁 487745 五、發明說明(4) 之SSF(亦請見實例丨)。 圖1 3為流通量對距噴絲頭之固化距離用及不用徐冷器之 曲線圖;使用FEP-5100,30 -密爾/30 -纖絲喷絲頭,3 -吋 直從4 1时長徐冷器及噴絲頭溫度為3 8 〇 °c (三角形),4 3 0 °C (方形)及480 °C (圓圈),其中空心符號代表不用徐冷器, 而深色符號則代表使用徐冷器。 圖1 4為距噴絲頭距離(吋)對紗線溫度用徐冷器(深色符 號)和不用徐冷器(空心符號)之曲線圖;使fflFEp — 51〇〇, 39·4-密爾/30 一纖絲噴絲頭,噴絲頭溫度為48(pc,45·4Page 6 487745 V. SSF of invention description (4) (see also example 丨). Figure 1 3 is the curve of the flux versus the curing distance from the spinneret and without the use of a cooler; using FEP-5100, 30-mil / 30-filament spinneret, 3-inch straight from 4 to 1 hour The temperature of the long cooler and spinneret is 3800 ° C (triangle), 4300 ° C (square) and 480 ° C (circle). The hollow symbol indicates that the cooler is not needed, and the dark symbol indicates Use a Xu cooler. Figure 14 shows the distance (inch) from the spinneret to the temperature of the yarn with a cooler (dark symbol) and without a cooler (open symbol); fflFEp — 51〇〇, 39 · 4- dense / 30 a filament spinneret with a spinneret temperature of 48 (pc, 45 · 4

gpm/~ 0 pph ’其中方形代表旋紡速度4〇〇 mpm時之紗線溫 度’圓圈代表5 0 0 mpm時之紗線溫度,及三角形代表7〇 〇 mpm時之紗線溫度。 圖^為徐冷器長度(吋)對最初纖絲斷裂速度(mpm)之曲 線圖。使用以下:FEP-510()氟聚合物,3〇_密爾/3〇_纖絲喷 絲頭,噴絲頭溫度480它及44 8克/分(gpm)。 圖1 6為實例23之溫度對最初纖絲斷裂速度(mpm)之曲線 =,/、中深色圓圈代表本發明樣本,而方形則代表比較樣 本 。 詳細說曰!gpm / ~ 0 pph 'where the square represents the yarn temperature at a spinning speed of 400 mpm', the circle represents the yarn temperature at 500 mpm, and the triangle represents the yarn temperature at 700 mpm. Figure ^ is a plot of the length of the cooler (inch) versus the initial filament breaking speed (mpm). The following was used: FEP-510 () fluoropolymer, 30-mil / 30-fibre spinneret, spinneret temperature of 480 ° C and 448 g / min (gpm). Figure 16 is the curve of the temperature versus the initial filament breaking speed (mpm) of Example 23 =, /, dark circles represent samples of the present invention, and squares represent comparative samples. Say in detail!

本,明之方法提供高溫旋紡之益處而同時避免其不利 :人物:發明方法中’包含高度氟化熱塑性聚合物或此 〇« -暎,犯物之組合物可曝露於聚合物降解溫度以上 ::明::之時間可長到足以引起熔體黏度降低而不足 引起明顯的聚合物降解發生。在溶纺時,溶融組合物係The method of the present invention provides the benefits of high temperature spin spinning while avoiding its disadvantages: Character: In the method of the invention 'comprising a highly fluorinated thermoplastic polymer or this 〇 «-ying, the composition of the criminal can be exposed above the polymer degradation temperature: : Ming :: The time can be long enough to cause the melt viscosity to decrease and insufficient to cause significant polymer degradation to occur. When melt spinning, melt the composition

/ /HO 五、發明說明(5) 其通過熔體旋紡裝 高的前+ t 衣置之擠壓模具,例如,毛細管時遭遇最 同的剪切速率。在太欢 人舲π丄&amp; ^ 牡+發明之方法中,就是在此點,熔融聚 σ物可加埶至高声翁/L &gt; 糸Α ^… 八氣化聚合物之降解溫度以上之溫度。因 桓且Ϊ南溫之故而可達到高流通量速度,故組合物在擠壓 模f中之駐留時間保持最短。 ^此’本發明提供第一種熔紡包含高度氟化熱塑性聚合 驟2 ^等\聚Θ A之掠&quot;混*物之組合物之方法’其包含下列步 〃·將包含高度氟化熱塑性聚合物或此等聚合物之摻混物 $、及5物溶解以形成溶融氟聚合物組合物;將該溶融氟聚 :物組合物加壓輸送至炫紡裝置之擠壓模具;及將溶融氟 ,合物組合物擠壓通過擠壓模具以形成熔融纖絲,該模具 係在溫度至少4 5 0 °C下,剪切速率為至少1 〇 〇 s e CT1,及旋 紡速度為至少5 0 0米/分。 包括高度氟化熱塑性聚合物或此等聚合物之摻混物之組 合物係在熔解步驟中熔化。用於此一第一種方法之高度氟 化熱塑性聚合物包括聚四氟乙烯(PTFE)以外之均聚物,如 聚亞乙稀基氟(PVDF),及共聚物,如四氟乙烯(tj?E)與包 括全氟烯烴之共聚用單體,如全氟乙烯基烷基化合物,全 氟烷基乙烯基醚或此等聚合物之摻混物製備之共聚物。 1共聚物π —詞,供本發明之用,係意欲涵蓋單一聚合物包 含二或多種共聚用單體之聚合物。代表性全氟乙烯烷基化 合物係六氟丙烯。代表性全氟烷基乙烯基醚係全氣甲基乙 烯基醚(PMVE),全氟乙基乙烯基醚(PEVE)及全氣丙基乙烯 基鱗(PPVE)。較佳之南度氟化聚合物為自四氟乙稀及全氟// HO 5. Description of the invention (5) It uses a melt-spinning high front + t garment to place an extrusion die, for example, the capillary tube encounters the same shear rate. In the method of 欢 π 丄 &amp; ^ + invented by Taihuanren, it is at this point that the molten polyσ can be added to the high temperature / L &gt; 糸 Α ^ ... above the degradation temperature of the eight gasification polymer temperature. Because of the high flow rate that can be achieved due to the low temperature and the low temperature, the residence time of the composition in the extrusion die f is kept to a minimum. ^ This' The present invention provides the first melt-spinning method comprising a highly fluorinated thermoplastic polymerization step 2 ^ The method of the composition of the "sweep" of "PolyA" which includes the following steps: The polymer or blends of these polymers $ and 5 are dissolved to form a melted fluoropolymer composition; the melted fluoropoly: composition is pressurized to the extrusion die of the spinning device; and the melt is melted Fluoride composition is extruded through an extrusion die to form molten filaments, the die is at a temperature of at least 450 ° C, a shear rate of at least 100se CT1, and a spinning speed of at least 50 0 m / min. Compositions comprising highly fluorinated thermoplastic polymers or blends of these polymers are melted during the melting step. The highly fluorinated thermoplastic polymers used in this first method include homopolymers other than polytetrafluoroethylene (PTFE), such as polyvinylidene fluoride (PVDF), and copolymers, such as tetrafluoroethylene (tj E) Copolymers prepared with comonomers including perfluoroolefins, such as perfluorovinyl alkyl compounds, perfluoroalkyl vinyl ethers, or blends of these polymers. 1 Copolymer π, as used in the present invention, is intended to encompass a single polymer containing two or more comonomers. A representative perfluoroethylene alkyl compound is hexafluoropropylene. Typical perfluoroalkyl vinyl ethers are perfluoromethyl vinyl ether (PMVE), perfluoroethyl vinyl ether (PEVE) and perfluoropropyl vinyl scale (PPVE). Preferred Nandu fluorinated polymers are from tetrafluoroethylene and perfluoro

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487745 五、發明說明(6) 坑基乙烯基醚製備之共聚物,及自全氟乙烯及六氟丙烯製 備之共聚物。最佳共聚物為具1 — 2 〇莫耳%全氟乙烯基烷基 共聚用單體,較佳3 —1〇莫耳%六氟丙烯或3 —1〇莫耳%六氟丙 烯與0.2-2莫耳% PEVE或PPVE之TFE,及具0.5-10莫耳%全 氟烧基乙烯基醚,包括0.5-3莫耳% ρρνΕ或PEVE之TFE共聚 物。也適合於實行本發明的是高度氟化熱塑性聚合物之摻 混物,包括T F E共聚物之摻混物。 、適合於實行本發明之氟聚合物較佳具有熔體流速(MF R) 為約1至約50克/10分,如根D33 07,D1238 或可供其他高度氟化熱塑性聚合物用之對應試驗於372 下所測得者。 包含高度氟化熱塑性聚合物或此等聚合物之掺混物之組 合物可進一步包含添加劑。此等添加劑可包括,例如顏料 及填料。 在本方法中,以上所討論包含高度氟化聚合物或此等聚 合物之摻混物之組合物係經熔解而形成熔融氟聚合物組合 物、。本技藝所知可提供熔體之任何方法都可使用。代表性 方法可包括將氟聚合物組合物引入擠壓機中,加熱至足以 使組合物熔解之溫度,但至高度氟化熱塑性聚合物或此等 ♦ 5物之摻此物之降解溫度以下。此一溫度係視所用特定 聚合物而定。 一俟組合物成為熔融狀態後,即將其加壓輸送至熔紡裝 置之擠壓模具」如噴絲頭。組合物輸送至擠壓模具之方式 已為本技藝所熟知,且包括具有撞鎚或活塞,單螺旋或雙487745 V. Description of the invention (6) Copolymer prepared from pit-based vinyl ether, and copolymer prepared from perfluoroethylene and hexafluoropropylene. The best copolymer is 1-20 mole% perfluorovinyl alkyl comonomer, preferably 3-10 mole% hexafluoropropylene or 3-10 mole% hexafluoropropylene with 0.2- 2 mole% PEVE or PPVE TFE, and 0.5-10 mole% perfluoroalkyl vinyl ether, including 0.5-3 mole% ρρνΕ or TFE copolymer of PEVE. Also suitable for practicing the present invention are blends of highly fluorinated thermoplastic polymers, including blends of TF E copolymers. Fluoropolymers suitable for the practice of the present invention preferably have a melt flow rate (MF R) of about 1 to about 50 grams / 10 minutes, such as D33 07, D1238, or other counterparts that can be used for other highly fluorinated thermoplastic polymers. Tested at 372. Compositions comprising highly fluorinated thermoplastic polymers or blends of these polymers may further include additives. These additives may include, for example, pigments and fillers. In this method, the composition discussed above comprising a highly fluorinated polymer or a blend of these polymers is melted to form a molten fluoropolymer composition. Any method known in the art to provide a melt can be used. A representative method may include introducing the fluoropolymer composition into an extruder and heating it to a temperature sufficient to melt the composition, but below the degradation temperature of a highly fluorinated thermoplastic polymer or a blend of these materials. This temperature depends on the particular polymer used. Once the composition has become molten, it is conveyed under pressure to an extrusion die of a melt spinning device, such as a spinneret. The manner in which the composition is delivered to the extrusion die is well known in the art and includes having a ram or piston, single spiral or double

第9頁 487745 五、發明說明(7) 螺旋之裝置。在本發明方法之較佳具 以熔解及輸送適合實行本發明之熔融%^中’擠屋機係用 ^具以分別形成單纖絲或多纖絲纖維產物。擠:: 管及螺旋’以及模具較佳係自耐腐钱材料,包括高鎳$ f 耐腐蝕鋼合金,如Hastelloy C〜276 (Cab〇t公司,K〇k〇m〇里 ΙΝ·)所製成。許多適當擠壓機,包括螺旋式及活塞式,已 為本技藝所知且在市面上可購得。也可包括計量裝置,如 齒輪泵以利計量螺旋及喷絲頭之間的熔體。 *在本發明之方法中,熔融氟聚合物組合物在輸送至擠壓 模具後’即經由擠壓模具之孔洞擠壓,該模具係在溫度至 少450。(:下,剪切速率為至少1〇〇 se(rl及旋紡速度為至少 5 〇 0米/分。 擠壓模具之孔洞可為任何所要剖面形狀,而以圓形剖面 开i狀為較佳。經發現適用於本發明方法之圓形剖面孔洞之 ^ ·5主4·0^米之範圍内,但本發明之實行並不 限於違犯圍。可用於本發明之擠壓模具孔洞之長度與直徑 =it佳係在約^1至約8 ··1之範圍内。雖然孔型並不重要, 但右孔係以一或二同心圓配置則為較佳,而以單圓配置為 更佳。 洎圖1顯不熱_塑性聚合物習用熔紡裝置之一部份,噴絲頭 =成10 °所不為銜接器1,其可藉插入衡接器1點線之間的 二間9内的昆式加熱器加熱且附著於用以輸送及熔解氟聚 ^物組合物之裝置(未示出);含熔體過濾裝置3,一般為 碑網之過濾、纪合件2 ;及具有面板5之習用喷絲頭4,面板5 487745 五、發明說明(8) =配置在/喷、,、糸頭4之一端,與喷絲頭4之另一端距離為h。 朱、’、t頭4係鄰接過濾組合件2之底面8配置,並與過濾組合 起藉由扣螺帽6固定於銜接器1。喷絲頭總成10係藉 ;己置於螺帽6周圍之帶式加熱器7加熱。圖1中,喷 絲Τ -般係藉其與扣螺帽6之導電接觸加熱。 僅加熱噴絲頭成設’並無便利的方法用以 中。任 面板5,因為噴絲頭4整個套在扣環之 區域之相ί ϊ ϋ面板5之嘗試都會將噴絲頭總成10其他 面板5以外區域1 77加熱至類似或略低溫度。噴絲頭總成1 〇 溫度或以上备佶,此—不當加熱至氟聚合物組合物之降解 下,且在草此_氟聚合物組合物非所欲地長期曝露於高溫 在本下會導致聚合物過度降解。 以此處某些氟雙人擠壓模具係加熱至溫度至少45 0 °C。 高於約50〇一。(: //物組合物而言,擠壓模具可加熱至溫度 解,可藉由將樁厭、\至這些溫度而不使氟聚合物組合物降 之其他區域作熱陪模具與含有氟聚合物組合物之熔紡裝置 通過擠壓模具時^離,達成。當熔融氟聚合物組合物開始 快速降低,而=丄^兩之模具溫度會引起聚合物熔體黏度 降低熔體在高溫;之:::=模具、。為避免熱降解,必須 時間的函數,若,、w : 一 、4。因為降解不僅是溫度也是 因此,本發明在,較佳為停留時間應降至最短。 絲頭面板中之喷,的區域,亦即擠壓模具,例如在喷 擠壓模具可與;提供最高溫度。因此,、 _ 一虱承合物組合物接觸之熔紡裝置之其 第11頁 487745Page 9 487745 V. Description of the invention (7) Spiral device. In the method of the present invention, it is preferred to use melting and conveying melt% suitable for carrying out the present invention. The house extrusion machine is used to form monofilament or multifilament fiber products, respectively. Extrusion :: The tube and the spiral 'and the mold are preferably made of corrosion-resistant materials, including high nickel $ f corrosion-resistant steel alloys, such as Hastelloy C ~ 276 (Cab〇t Corporation, Kokomori ΙΝ ·). production. Many suitable extruders, including screw and piston, are known in the art and are commercially available. It can also include metering devices such as gear pumps to meter the melt between the spiral and the spinneret. * In the method of the present invention, the molten fluoropolymer composition is extruded through the holes of the extrusion die after being conveyed to the extrusion die, and the die is at a temperature of at least 450. (: Below, the shear rate is at least 100se (rl and the spinning speed is at least 5000m / min. The hole of the extrusion die can be any desired cross-sectional shape, and a circular cross-sectional opening i-shaped is more suitable It is found to be suitable for the circular cross section of the method of the present invention within the range of ^ · 5 main 4 · 0 ^ meters, but the practice of the present invention is not limited to violation of the fence. The length of the hole of the extrusion die of the present invention And diameter = it is better in the range of about ^ 1 to about 8 ·· 1. Although the hole type is not important, the right hole system is better configured with one or two concentric circles, and the single circle configuration is more suitable.洎 Figure 1 shows a part of the conventional melt-spinning device for plastic polymers. The spinneret = 10 ° is not the connector 1. It can be inserted into the two between the point line of the connector 1. The Kun heater in 9 is heated and attached to a device (not shown) for conveying and melting the fluoropolyurethane composition; it includes a melt filtering device 3, which is generally a filter and a piece 2 of the monument network; and Conventional spinneret 4 with panel 5 and panel 5 487745 V. Description of the invention (8) = arranged at one end of / sprayer 4 and the other of the spinneret 4 and the other of the spinneret 4 The distance is h. Zhu, ', and t heads 4 are arranged adjacent to the bottom surface 8 of the filter assembly 2 and are fixed to the connector 1 by the button nut 6 with the filter assembly. The spinneret assembly 10 is borrowed; The belt heater 7 around the nut 6 is used for heating. In Fig. 1, the spinneret T is generally heated by its conductive contact with the button nut 6. Only heating the spinneret is provided. There is no convenient method for Medium. Any panel 5, because the spinneret 4 is completely covered in the area of the buckle. Attempts of panel 5 will heat the spinneret assembly 10 and other regions 5 outside the panel 5 to a similar or slightly lower temperature. The spinneret assembly is prepared at a temperature of 10 ° C or more. This—improper heating to the degradation of the fluoropolymer composition, and in this case the undesired long-term exposure of the fluoropolymer composition to high temperatures will cause the The polymer is excessively degraded. Here, some fluorine double extrusion dies are heated to a temperature of at least 45 0 ° C. Above about 501. (: // For the composition composition, the extrusion dies can be heated to a temperature solution. It is possible to accompany the mold and other areas by reducing the temperature of the pile to these temperatures without lowering the fluoropolymer composition. The melt spinning device of the fluoropolymer composition is achieved by extruding the mold when it is extruded. When the molten fluoropolymer composition begins to decrease rapidly, the mold temperature of the two will cause the polymer melt viscosity to decrease. ; :: == mould, in order to avoid thermal degradation, a function of time is necessary, if, w: a, 4. Because degradation is not only temperature but also, the present invention, preferably, the residence time should be minimized. The area of the nozzle in the silk panel, that is, the extrusion die, for example, in the extrusion die, can be provided with; the highest temperature. Therefore, _ a lice bearing composition of the melt spinning device of its page 11 487745

他區域保持熱隔離。 八2絲頭或其包括面板之部份可與噴絲頭總成之其他區域 ::加熱。提供高局部化加熱至溫度至少45〇。〇之任/ 3可用於實行本發明。此等裝置包括線圈加熱器 ^ 力a無線電頻率’傳導,感應或對; r二之裝置,如感應加熱器。可使用絕緣,如陶瓷絕緣, =ί供隔離而因此面板與可能與氟聚合物組合物接觸之熔 頭^置其他區域間之熱隔離。也可在擠壓模具以外之噴絲Other areas remain thermally isolated. The 8 2 silk head or the part including the panel can be connected to other areas of the spinneret assembly :: heating. Provide high localized heating to a temperature of at least 45 °. Renzhi / 3 can be used to practice the present invention. These devices include coil heaters ^ a radio frequency 'conduction, induction or pairing; r two devices, such as induction heaters. Insulation, such as ceramic insulation, may be used to provide thermal insulation between the panel and other areas where the panel may be in contact with a fused polymer that may come into contact with the fluoropolymer composition. Spinning outside the extrusion die

,或噴絲頭總成區域使用一或多個冷却夹套以提壓模 具之熱隔離。 佾查梹 —為便利擠壓模具之熱隔離,在本發明之一具體例中,僅 =增加圖1所示習用喷絲頭兩端間之距離h,使噴絲頭面 反/、喷絲頭本體隔離,已發現很理想。以此方式增加距 ^ ’圖2中以h’所示,能使喷絲頭面板與喷絲頭總成其餘 4份整體分開加熱。因此,本發明之噴絲頭面板,在、一具 $例中是以距離h,與過濾組合件之底面隔開,該距離足^ §噴絲頭面板分開加熱。Or, one or more cooling jackets are used in the spinneret assembly area to improve the thermal isolation of the mold.佾 Check 梹 —In order to facilitate the thermal isolation of the extrusion die, in a specific example of the present invention, only the distance h between the two ends of the conventional spinneret shown in FIG. 1 is increased to make the spinner face reverse / spinning The head body is isolated and has been found to be ideal. Increasing the distance in this way ^ 'shown by h' in FIG. 2 enables the spinneret panel and the remaining 4 parts of the spinneret assembly to be separately heated as a whole. Therefore, the spinneret panel of the present invention is separated from the bottom surface of the filter assembly by a distance h in one example, which is sufficient to separately heat the spinneret panel.

&gt;圖2所示為喷絲頭總成2 〇,其具有附著於溶解及/或輸送 氣聚合物組合物之裝置(未示出)之銜接器21 ;含篩網23及 底面2 8之過濾組合件;具面板2 5之加長噴絲頭2 4,面板2 5 係配置在噴絲頭24之一端,與噴絲頭24在過濾組合件22底 面28之另一端相距h,;其中h,&gt;h而圖!及2中之其他尺寸保 持相同,致能使面板25伸出至扣螺帽26之外。由於面板25 如此自扣螺帽2 6突出’故可使用加熱裝置2 9來單獨加熱面&gt; Figure 2 shows a spinneret assembly 20, which has an adapter 21 attached to a device (not shown) that dissolves and / or conveys the gaseous polymer composition; includes a screen 23 and a bottom surface 2 of 8 Filter assembly; extended spinneret 24 with panel 25, panel 25 is disposed at one end of spinneret 24, and h from spinneret 24 at the other end of bottom 28 of filter assembly 22, where h , &Gt; h and map! The other dimensions remain the same as in 2, enabling the panel 25 to protrude beyond the button nut 26. Since the panel 25 protrudes from the snap nut 2 6 in this way, the heating device 2 9 can be used to individually heat the surface

第12頁 487745 五、發明說明(ίο) 板2 5,而因此面板2 5即與喷絲頭總成之其餘部份熱隔開。 加熱裝置2 7,如帶式或線圈加熱器,係配置在扣螺帽2 6周 圍。 可用於本發明之喷絲頭總成之另一替代具體例係在圖3 以噴絲頭總成3 0顯示。在此具體例中,圖2之扣螺帽2 6之 下部在尺寸上縮小,例如,扣螺帽較薄,請閱圖3中之扣 螺帽3 6。在此,加長喷絲頭3 4之本體相對於圖2喷絲頭2 4 之長度係縮短,但喷絲頭3 4仍係加長(相對於圖1之喷絲頭 4 ),以便延伸超出扣螺帽4 6之外,而能使面板3 5藉由裝置 3 9與所示供喷絲頭總成另一區域加熱之裝置3 7分開加,熱。 也顯示者為銜接器3 1,其係附著於熔解及/或輸送氟聚合 物組合物之裝置(未示出);過遽組合件3 2及過Ι置3 3、’ 及導槽38。 · · • 、 〆 在本發明之上述具體例中,輸送至噴絲頭之熔融組合物 可藉配置於喷絲頭外壁周圍之裝置加熱,而因此鄰近/]、孔 之壁之熔體之溫度高於熔體中心之溫度。此一溫度1不均勻 • · &gt; 性-外面最高並向熔體中心冷却-之影響會弓1起纖絲向喷絲 頭中央彎曲,。已發現,在高喷射速度下,^些氟聚合物組 合物之彎曲角度高於4 5。。此一現象之衝擊计為可達到之 高速纖絲連續性之減低,為降低聚合物熔體最外及最内部 份間的任何溫度梯度,可在小孔48内提供一加熱裝、置,如 可在加長喷絲頭4 4之中央放進匣式加熱器,如圖4之喷絲 頭總成4 0所示。也顯示於圖4者為銜接器4 1,其係固著於 熔解及/或輸送氟聚合物組合物之裝置(未示出);過濾組Page 12 487745 V. Description of the Invention The plate 25 is thus thermally separated from the rest of the spinneret assembly. The heating device 27, such as a belt or coil heater, is arranged around the nut 26. Another alternative specific example of the spinneret assembly that can be used in the present invention is shown in FIG. 3 as the spinneret assembly 30. In this specific example, the lower portion of the buckle nut 26 in FIG. 2 is reduced in size. For example, the buckle nut is thinner. Please refer to the buckle nut 36 in FIG. 3. Here, the length of the body of the lengthened spinneret 34 is shorter than that of the spinneret 2 4 in FIG. 2, but the spinneret 34 is still longer (compared to the spinneret 4 in FIG. 1) so as to extend beyond the button. Outside the nut 4 6, the panel 3 5 can be heated by means of the device 3 9 separately from the device 3 7 shown in the other region of the spinneret assembly for heating. Also shown are adapters 31, which are attached to a device (not shown) that melts and / or transports the fluoropolymer composition; the pass-through assembly 32, and the pass-through assembly 3 3 'and the guide groove 38. · · · 〆 In the above specific examples of the present invention, the molten composition delivered to the spinneret can be heated by a device arranged around the outer wall of the spinneret, and thus the temperature of the melt adjacent to /] and the wall of the hole Above the melt center. This temperature 1 is non-uniform. • &gt; The effect-the highest outside and cooling towards the melt center-the effect of bowing the filaments towards the center of the spinneret. It has been found that the bending angle of some fluoropolymer compositions is higher than 45 at high jet speeds. . The impact of this phenomenon is to reduce the continuity of the high-speed filament that can be achieved. In order to reduce any temperature gradient between the outermost and innermost parts of the polymer melt, a heating device can be provided in the small hole 48. For example, the cassette heater can be placed in the center of the elongated spinneret 44, as shown in the spinneret assembly 40 of Fig. 4. Also shown in Fig. 4 is an adapter 41, which is fixed to a device (not shown) for melting and / or transporting the fluoropolymer composition; a filter set

O:\62\62592.PTD 第13頁 487745 五、發明說明(11) 合件4 2 ;過濾裝 板4 5 〇 本發明提供之 5 0,係為快速加 槽6 2 (相當於圖3 頭面板55之體積 一具體例也提供 内,藉由加熱裝 此,本發明方法 氟聚合物組合物 溫度以下之中間 5 2之部份可藉配 移線58導槽62内 加熱裝置6 0預加 合物組合物之熔 面板5 5在此一具 之加熱裝置61分 及過濾裝置5 3下 喷絲頭5 4可拆除 5 2。也顯示者為 聚合物組合物之 圖7及8顯示本 走轉移線7 8且可 圖5及6所示具體 置4 3 ;扣螺帽4 6 ;加熱裝置4 7及4 9 ;及面 進一步具體例,在圖5及6中顯示為噴絲頭 熱熔體並通過轉移線58内所提供之狹窄導 之導槽3 8 ),及為減少上游直接送到噴絲 。藉由減少體積,停留時間即可縮短。此 一機會,讓組合物還在轉移線5 8之導槽6 2 置6 0之使用,而有一中間溫度區域。因 可進一步包括使氣聚合物組合物曝露於自 之熔體溫度至擠壓模具,例如喷絲頭面板 溫度。如所示,轉移線5 8鄰近過濾組合件 置於扣螺帽5 6周圍之加熱裝置5 7加熱。轉 之氟聚合物組合物可藉加熱裝置57及/或 熱至至少一中間溫度,此一溫度可在氟聚 解溫度至低於面板5 5溫度之溫度範圍内。 體例中係顯示為藉固定於喷絲頭套管5 9上 開加熱,轉移線5 8係配置於過濾組合件5 2 游,接著為喷絲頭5 4,顯示為圓盤形狀。 以供清潔及更換而不用移開過濾組合件 銜接器5 1,其係固著於熔解及/或輸送氟 裝置(未示出)。 發明之喷絲頭總成7 0,此一具體例容許移 容納較大直徑之圓盤喷絲頭,此係相對於 例,如喷絲頭7 4而言。喷絲頭螺帽7 9將具O: \ 62 \ 62592.PTD Page 13 487745 V. Description of the invention (11) Combination 4 2; Filter mounting plate 4 5 0 50 provided by the present invention is a fast groove 6 2 (equivalent to the head of Figure 3) A specific example of the volume of the panel 55 is also provided. By heating to install this, the middle 5 2 part below the temperature of the fluoropolymer composition of the method of the present invention can be equipped with a transfer line 58 in a guide groove 62 and a heating device 6 0 pre-added. The melting panel 5 of the composition composition is divided into a heating device 61 points and a filtering device 5 3 under the spinneret 5 4 can be removed 5 2. Also shown in Figures 7 and 8 of the polymer composition Transfer line 7 8 and can be placed as shown in Figures 5 and 6 4 3; nut 4 6; heating device 4 7 and 4 9; and further specific examples, shown in Figures 5 and 6 as hot melt of the spinneret The body passes through the narrow guide grooves 3 8) provided in the transfer line 58 and is directly sent to the spinneret in order to reduce the upstream. By reducing the volume, the residence time can be shortened. At this opportunity, the composition is still used in the guide groove 6 2 of the transfer line 5 8 and 60, and there is an intermediate temperature region. This may further include exposing the aeropolymer composition to a temperature from the melt to an extrusion die, such as a spinneret panel temperature. As shown, the transfer line 5 8 is heated adjacent to the filter assembly by a heating device 5 7 placed around the nut 5 6. The converted fluoropolymer composition can be heated to at least an intermediate temperature by the heating device 57 and / or, and this temperature can be in a temperature range from the fluoropolymerization temperature to a temperature lower than the temperature of the panel 55. In the system, it is shown that it is heated by being fixed on the spinneret sleeve 5 9, and the transfer line 5 8 is arranged on the filter assembly 5 2, and then the spinneret 5 4 is shown in the shape of a disk. For cleaning and replacement without removing the filter assembly adapter 51, which is fixed to a melting and / or transporting fluorine device (not shown). The invention of the spinneret assembly 70, this specific example allows to accommodate a larger diameter disc spinneret, which is relative to the example, such as the spinneret 74. Spinneret nut 7 9 will have

O:\62\62592.PTD 第14頁 487745O: \ 62 \ 62592.PTD Page 14 487745

五、發明說明(12) 有面板75之圓盤喷絲頭74固定於轉移線78之面82之底部。 轉移線78内之窄内流槽83使氟聚合物組合物之體積減小並 縮短其在高溫下之停留時間以進一步降低降解之機會。轉 移線78也藉由其分開之加熱裝置80提供一種逐漸上升至過 濾裝置73與噴絲頭74間之中間溫度。同時,所示轉移線具 體例提供更均勻及更快速之熱傳輸。此一具體例之額外優 點為圓盤噴絲頭7 4在無須移走過濾組合件下即可更換,且 圓盤可更容易製造。也顯示者為銜接器71,其係固著於溶 解及/或輸送氟聚合物組合物之裝置(未示出);具有多個 分佈槽提供過濾裝置73支撐之板72 ;由加熱裝置77圍繞之 扣螺帽76 ;配置於過濾裝置73與轉移線78中間之室84 ;及 面板7 5。 咸信本發明方法提供”自身熔體潤滑擠壓、se丨f id七 lubricated extrusion)。所謂”自身熔體潤滑擠壓”,係 意指唯有擠出物之皮,即熔體直接與小孔之壁鄰接之部” 份,被極熱之模具孔表面加熱至極高之溫度,造成熔體此 一部份之黏度降至極低,而同時由於短接觸或停留時間之 故,擠出物之本體保持於較低溫度。外層皮大幅降低之黏 度像是一層薄的潤滑膜,因此容許擠壓變成柱塞流,其中 擠出物之本體經歷的是均勻速度。 ^ 如此處所用,”剪切速率”係指表觀壁剪切速率 (apparent wall shear rate),計算為4Q/;rR3(Q=體積流 速,R=毛細管半徑)。在本發明之方法中,剪切速率係、至 少1 0 0 / sec。在既定組態及一定溫度下可達到理想纖維熔V. Description of the invention (12) The disc spinneret 74 with the panel 75 is fixed to the bottom of the surface 82 of the transfer line 78. The narrow internal flow grooves 83 in the transfer line 78 reduce the volume of the fluoropolymer composition and shorten its residence time at high temperatures to further reduce the chance of degradation. The transfer line 78 also provides a gradual rise to an intermediate temperature between the filter device 73 and the spinneret 74 by means of a separate heating device 80. At the same time, the transfer line shown provides more uniform and faster heat transfer. An additional advantage of this specific example is that the disc spinneret 7 4 can be replaced without removing the filter assembly, and the disc can be manufactured more easily. Also shown is an adapter 71, which is fixed to a device (not shown) that dissolves and / or transports the fluoropolymer composition; a plate 72 with a plurality of distribution slots to provide support for the filtering device 73; surrounded by a heating device 77 A button nut 76; a chamber 84 disposed between the filtering device 73 and the transfer line 78; and a panel 75. Xianxin The method of the present invention provides "self-melt lubricating extrusion, lubricated extrusion". The so-called "self-melt lubricating extrusion" means only the skin of the extrudate, that is, the melt directly and small The part of the wall adjacent to the hole is heated to a very high temperature by the extremely hot mold hole surface, which causes the viscosity of this part of the melt to be extremely low, and at the same time due to short contact or residence time, the extrudate The body is kept at a lower temperature. The greatly reduced viscosity of the outer skin is like a thin lubricating film, so the extrusion is allowed to turn into a plunger flow, in which the body of the extrudate experiences a uniform velocity. ^ As used herein, "shear rate" refers to the apparent wall shear rate, calculated as 4Q /; rR3 (Q = volume flow rate, R = capillary radius). In the method of the present invention, the shear rate is at least 100 / sec. Ideal fiber melting can be achieved at a given configuration and temperature

第15頁 487745 五、發明說明(13) 紡之剪切速率範圍係隨聚合物熔體黏度遞增而漸次變窄。 操作窗可藉提升溫度來代替熔體因高速致出現破裂之臨界 剪切速率而擴大,但要避免聚合物降解。熔體破裂之臨界 溫度/剪切速率在此係藉提高一定溫度及模具尺寸之流通 率直至可看出表面粗Μ度而測定,如炫融擠出物由透明變 至稍微不透明,即顯示熔體已發生破裂。流通率之進一步 提高會產生非所欲較粗表面粗糙度及較差旋紡性能及性 質。 本發明方法之旋紡速度為至少5 0 0米/分,且在此處係以 最後一支輥之旋紡速度測定,該最後一支輥視熔紡裝置之 組態而定,可為捲取輥或可為捲繞輥。 在實行本發明時發現,剪切速率及SSF兩者皆對旋紡纖 絲之強度有相當大的影響。剪切速率提高而SSF降低即可 維持相同強度,反之亦然,此由實例1可資證明且如圖11 曲線所示。 本發明之方法可進一步包括遮護纖絲。遮護纖絲時,圍 繞纖絲之空氣即可保持於較纖絲若曝露於未節制周圍空氣 時更暖和之溫度,而因此可防止纖絲快速冷却。未節制周 圍空氣,尤其是湍流空氣,會造成纖絲快速冷却,此非所 宜,因其可對纖絲可能有之拉伸量有害。因此遮護纖絲可 容許更高之旋紡拉伸拉細。已發現,若熔融紡絲流水線在 擠壓模具(毛細管直徑)之直徑5 0倍以上之距離發生固化 時,即可得高旋紡之高SSF (也請參閱圖1 3 )。固化距離較 佳大於毛細管直徑之直徑5 0 0倍以上。遮護可藉熔融纖絲Page 15 487745 V. Description of the invention (13) The shear rate range of spinning is gradually narrowed as the polymer melt viscosity increases. The operating window can be enlarged by increasing the temperature instead of the critical shear rate of the melt due to high-speed fracture, but to avoid polymer degradation. The critical temperature / shear rate of melt fracture is determined here by increasing the flow rate of a certain temperature and mold size until the surface roughness can be seen. If the melt extrudate changes from transparent to slightly opaque, it shows melting The body has ruptured. Further increase in the flow rate will result in undesired coarser surface roughness and poorer spinning performance and properties. The spinning speed of the method of the present invention is at least 500 m / min, and it is determined here by the spinning speed of the last roll, which depends on the configuration of the melt spinning device, and can be a roll The take-up roll may be a take-up roll. In the practice of the present invention, it was found that both the shear rate and SSF have a considerable effect on the strength of the spin-spun fiber. Increasing the shear rate and decreasing the SSF can maintain the same strength, and vice versa, which can be proved by Example 1 and shown in the curve of Figure 11. The method of the present invention may further include shielding the filaments. When covering the filaments, the air surrounding the filaments can be maintained at a warmer temperature than the filaments if exposed to uncontrolled ambient air, thus preventing the filaments from cooling rapidly. Uncontrolled ambient air, especially turbulent air, can cause rapid cooling of the filaments, which is not desirable because it can be harmful to the amount of stretching that the filaments may have. Therefore, the shielding filaments allow higher spin-spinning. It has been found that if the melt-spinning line solidifies at a distance of more than 50 times the diameter of the extrusion die (capillary diameter), a high SSF with high spin spinning can be obtained (see also Figure 1 3). The curing distance is preferably more than 500 times the diameter of the capillary. Fused filament

O:\62\62592.PTD 第16頁 487745 五、發明說明(14) 前進通過徐冷器而完成。徐冷器容許高速 旋紡拉伸至高程度,而因此提高旋紡速度。之熔融纖絲 移動通過徐冷器底部會使空氣溫度被吸入,2❼線快速 提供可將極熱之熔融纖絲部份冷却而不快速=徐冷器仍然 圍空氣產生湍流的相當安靜環境,使得纖維J却且防止周 點以上至遠較不使用徐冷器者距喷絲頭更遠保持於其熔 曲線顯示於圖13。徐冷器之使用也較不使用=離。此以 固化紗線於較高溫度下,如圖14所示。H余:^以維持 用可容許較高之旋紡速度,如圖15所示(註===之使 冷器)。 亇代表無徐 可用於本發明之徐冷器之一具體例顯示於圖1 及 所不,徐冷器20 0包括内管2〇2,其為同心配 2』4中的長管;外管直徑稍*,長度則可與内管實質卜相吕 :此ΪΓΓ可固定於外管2°4内而伸出至外管2〇4以下, 供熔融纖絲之出口,且進一步在外管2〇4頂端造成 0柱口,。開口2〇5容許空氣被吸入内管2。2之内 1 ’内&amp; 202可在内管202與外管204間之環形空間 &amp;吐#預熱雖然不提供外部加熱,但環形空間2 0 8可在旋 田Ϊ ί由擠壓之熱熔融纖絲之熱輻射而加熱。可具有圓形 二、。之頂^緣2 1 〇坐落在外管2 〇4之頂端。較佳由細目篩 郝梂如^目鋒網構成之網狀管2 1 2可固著於頂凸緣2 1 0,並 9(1 β #内官2〇2之内壁配置。網狀管212軸向延伸通過内室 206超出開口 2ίΚ j 網狀管212,可進牛不Λ在内管之整個長度提供網狀管。 運—步包括固著於或緊臨第一篩網之第二O: \ 62 \ 62592.PTD Page 16 487745 V. Description of the invention (14) The advance is completed by the Xu cooler. The spin cooler allows high-speed spin-spinning to a high degree, thus increasing spin-spinning speed. The molten filament moving through the bottom of the Xu cooler will cause the temperature of the air to be sucked in. The 2❼ line quickly provides the extremely hot molten filaments to be cooled and not fast. The fiber J prevents the melting point from being more than the perimeter to farther from the spinneret than the person who does not use the Xu cooler, and its melting curve is shown in FIG. 13. The use of Xu cooler is also less used = off. This cures the yarn at higher temperatures, as shown in Figure 14. H surplus: ^ to maintain the allowable higher spinning speed, as shown in Figure 15 (Note === to make the cooler).亇 represents a specific example of a Xu cooler that can be used in the present invention. Fig. 1 and the other examples, Xu cooler 200 includes an inner tube 202, which is a long tube in the concentric distribution 2 "4; The diameter is slightly *, and the length can be similar to the inner tube: this ΪΓΓ can be fixed in the outer tube 2 ° 4 and extended below the outer tube 204, for the outlet of the molten filaments, and further in the outer tube 20. 4 tops cause 0 posts. The opening 205 allows air to be drawn into the inner tube 2. Within 2 'inner &amp; 202 can be an annular space between the inner tube 202 and the outer tube 204 &amp; spit #preheating Although not providing external heating, the annular space 2 0 8 can be heated in Xuantianyu by the thermal radiation of the extruded hot-melt filaments. May have a round shape. The top edge 2 1 0 is located on the top of the outer tube 2 04. The mesh tube 2 1 2 which is preferably composed of a fine mesh sieve Hao Ruru ^ mesh front mesh can be fixed to the top flange 2 10, and 9 (1 β # 内 官 2002 inner wall configuration. The mesh tube 212 axial Extending through the inner chamber 206 beyond the opening 2 Κj mesh tube 212, the mesh tube can be provided throughout the entire length of the inner tube. Transport-step includes a second fixed to or immediately adjacent to the first screen

//45 五、發明說明(15) 更細目篩網,如1 〇 〇目篩網,係用以降低進入空氣之湍 流’同時便利空氣實質均勻分佈,俾空氣經向前行進入内 室2 0 6通過開口 2 0 5。也顯示出多孔環形板隔離物2 1 4,其 係配置在内管20 2與外管204之間並連接至内管2 02之外表 面或外管204之内表面,且可用以防止内管202自外管204 掉落。細網目之篩網2 1 6可放置於板2 1 4之頂端,以擴散及 分佈空氣向上前行進入開口 205。此等隔離物214及216係 視需要採用。視需要選用之玻璃環220可供目視觀察熔融 紡絲流水線及喷絲頭正面。// 45 V. Description of the invention (15) More fine-mesh screens, such as 100-mesh screens, are used to reduce the turbulence of the incoming air, and at the same time, facilitate the substantially uniform distribution of air. 6 through the opening 2 0 5. Also shown is a porous annular plate spacer 2 1 4 which is arranged between the inner tube 202 and the outer tube 204 and is connected to the outer surface of the inner tube 202 or the inner surface of the outer tube 204 and can be used to prevent the inner tube 202 dropped from the outer tube 204. A fine mesh screen 2 1 6 can be placed on the top of the plate 2 1 4 to diffuse and distribute air upwards into the opening 205. These spacers 214 and 216 are used as necessary. The optional glass ring 220 can be used to visually observe the melt spinning line and the front of the spinneret.

徐冷器之内及外管可由包括金屬如銘或塑膠如Lucite® 之材料製成。徐冷器可為自立或以適當安裝機構固定,而 該安裝機構可固著於熔紡裝置之其他元件或固定於其他材 料以保持其固定。 本發明之方法可進一步包含使擠出物以一或多股之形式 通過驟冷區至收集紡纖之裝置。驟冷區可在周圍溫度下, 或視所用特定製程組態之需要而定,予以加熱或冷却。The inner and outer tubes of the Xu cooler can be made of materials including metal such as Ming or plastic such as Lucite®. The Xu cooler can be self-supporting or fixed with a suitable mounting mechanism that can be fixed to other components of the melt spinning device or to other materials to keep it fixed. The method of the present invention may further comprise passing the extrudate through the quench zone in one or more strands to a device for collecting the spun fibers. The quench zone can be heated or cooled at ambient temperature, or as required by the specific process configuration used.

任何收集纖維之裝置都適合於實行本發明。此等裝置包 括轉動筒,旋轉器(pi dd ler),或捲繞機,較佳具橫動 程,這些全部皆為本技藝所知。其他方式包括為製造短纖 束或纖維體用之一種切碎或切斷連續紡抽纖維之製程。還 有其他方式包括線上直接將紡抽纖維併入織物结構或複合 結構中。在以下所述具體例中發現適合之一種i置為市面 上可自Leesona公司(Burlington,NC)購得之高1紡織型 捲繞機。Any device for collecting fibers is suitable for practicing the present invention. Such devices include a rotating drum, a piddler, or a winder, preferably with a traverse, all of which are known in the art. Other methods include a process of chopping or cutting continuous spinning and drawing fibers for the manufacture of short tows or fibrous bodies. Still other methods include directly spinning the drawn fibers into a fabric or composite structure on the wire. A suitable type found in the specific examples described below is a high 1 textile type winder commercially available from Leesona (Burlington, NC).

487745 五、發明說明(16) 如:ϊ Ϊ紡技藝已知可幫助輪送纖維之此等其他裝置皆可 器及類似物之使用。 虱棒,分離 知可在纖維上施加抗靜電處理。此等處理已為本業所熟 本發明之方法可進一步包含拉伸纖維、鬆弛 纖維y在捲取親與—組拉伸輥之間拉伸。此等拉;木487745 V. Description of the invention (16) For example: 其他 Ϊ spinning technology is known to help the rotation of fibers, these other devices can be used and the like. Lice stick, separation It is known that antistatic treatment can be applied to the fiber. Such treatments are well known in the art. The method of the present invention may further include drawing the fibers, and relaxing the fibers y between the take-up rollers and the set of drawing rollers. These pull; wood

業Γ ΐ知ϋ提高纖維物度及降低線密度。捲取親;予 以加熱以賦予纖維更高程度之拉伸,溫度及拉伸产I ίϊ=隹性質而定。同樣地,“略諳本技藝;所知之 額外乂驟也可加至本方法以鬆弛纖維。 本發明也提供第二種熔紡包含聚四氟乙烯均聚物之組合 物之方法,其包含下列步驟:將包含聚四氟乙烯均聚物之 ,合物熔解以形成熔融聚四氟乙烯組合物;將該熔融聚四 ,乙稀加壓輸送至熔紡裝置之擠壓模具中;及將熔融聚四 氣乙烯組合物擠壓通過擠壓模具以形成熔融纖維。 在熔紡均聚物之方法中,聚四氟乙烯(PTFE),較佳pTFE 均聚物係在溫度48 0 °C以下會產生熔融流者。較佳均聚物 包括Zonyl®氟添加物,pTFE粒狀成形粉級,如Tefl〇n® PTFE TE-6472,及PTFE潤滑之膏擠壓樹脂,如Teflon® PTFE 62,全部皆可自杜邦公司(Wi lmingt〇n,^Ε)購得。 由於呈現熔融流特徵所需之極度溫度瀕臨熱降解邊緣,故 本方法在PTFE均聚物之成功熔體處理及紡纖上特別重要。 以上有關第一種熔紡高度氟化熱塑性組合物之方法及其It is known that the fiber content is increased and the linear density is reduced. Take up the parent; give heat to give the fiber a higher degree of stretching, the temperature and the tensile properties depend on the properties. Similarly, "a little bit of the skill; additional steps known can be added to the process to relax the fibers. The present invention also provides a second method of melt spinning a composition comprising a polytetrafluoroethylene homopolymer, comprising The following steps: melting the polytetrafluoroethylene homopolymer to form a molten polytetrafluoroethylene composition; conveying the molten polytetrafluoroethylene to an extrusion die of a melt spinning device; and The molten polytetraethylene composition is extruded through an extrusion die to form molten fibers. In the method of melt-spinning homopolymer, polytetrafluoroethylene (PTFE), preferably pTFE homopolymer, is at a temperature below 48 ° C. Those that will produce melt flow. Preferred homopolymers include Zonyl® fluorine additives, pTFE granular shaped powder grades, such as Teflon® PTFE TE-6472, and PTFE lubricating paste extrusion resins, such as Teflon® PTFE 62, All are available from DuPont (Wilmington, ^ Ε). Because the extreme temperature required to exhibit the characteristics of the melt flow is near the edge of thermal degradation, this method is used on the successful melt treatment of PTFE homopolymers and on spinning fibers This is especially important. The method and composition of

画 第19頁 487745 五、發明說明(ΙΌ 可用之裝置之說 法。然而,第一 紡速度之限制可 較佳為至少4 5 0 t 至少200 mpm ; ^ 本發明進一步 裝置之噴絲頭總 置於該過濾裝置 置;該噴絲頭之 長徐冷器。 熔纺技藝習用 明裝置。噴絲頭 細管壁之喷絲頭 該正面可包含分 絲頭内毛細管之 頭之毛細管孔較 孔較佳係以二同 線單獨移走以便 自過濾、組合件及 之加熱裝置可包 者所知之傳導, 以上及實例中 空間隔開之内管 吋。加長徐冷器 之任何過濾熔紡纖維 係作成可讓喷絲頭之 之部份與熔喷裝置之 開之板或為喷絲頭本 長度與直徑比較佳為 佳配置成全部的孔都 心圓或一圓配置。噴 容易請洗或更換。同 喷絲頭移走。轉移線 括帶式加熱器,線圈 對流或感應加熱器。 更詳細說明之加長徐 &amp;外詧。内管之内徑 —步包含鄰近内 明都適合於溶紡聚四氣乙烯組合物之方 種方法所發現對模具溫度或剪切速率或旋 能不適用於本PTFE方法。擠壓模具之溫度 :。旋纺速度較佳為至少5 0 m p m ;更佳為 3最佳為至少500 mpm。 提供一種熔紡纖維之裝置,其包含有過濾 成;喷絲頭;加長轉移線,該轉移線係配 與該喷絲頭之間;該加長轉移線之加熱裝 加熱裝置及配置於該噴絲頭總成以下之加 之裝置皆可用於本發 正面,例如,包括毛 其他部份分開加熱; 體之一整體部份。噴 約1 ·· 1至約8 ·· 1。噴絲 可均句加熱。毛細管 、、糸頭較佳係可自轉移 樣地’轉移線較佳可 之加熱裝置及噴絲頭 加熱器或熟諳本技藝 冷器較佳包含以環形 f佳自約3吋至約8 管内壁配置之網狀Draw on page 19 487745 V. Description of the invention (1Ό Applicable device. However, the first spinning speed limit may preferably be at least 450 mt at least 200 mpm; ^ The spinneret of the further device of the present invention is always placed The filter device is provided; the long cooler of the spinneret is used. The melt spinning technique is used. The spinneret of the thin tube wall of the spinneret. It is separately removed by two lines so that the self-filtering, assembly, and heating device can cover the conduction known to the person. The above and the inner space of the example are separated by inches. Any filter melt-spun fiber with an extended cooler is made. The part of the spinneret and the opening plate of the meltblowing device or the length and diameter of the spinneret are better. It can be configured so that all the holes are centered or round. The spray is easy to wash or replace. The same spray The wire head is removed. The transfer line includes a belt heater, a coil convection or an induction heater. More detailed description of the extension Xu &amp; outer tube. The inner diameter of the inner tube-steps including the adjacent inner Ming are suitable for melt spinning polygas Recipe of ethylene composition The method found that the mold temperature or shear rate or spin energy is not applicable to the PTFE method. The temperature of the extrusion mold: The spin speed is preferably at least 50 mpm; more preferably 3, most preferably at least 500 mpm. A device for melt-spinning fibers, comprising a filter element; a spinneret; an extension transfer line, the transfer line is arranged between the spinneret; a heating device for heating the extension transfer line and a spinneret; The following devices can be used for the front of the hair, for example, the other parts of the hair are separately heated; the whole part of the body. Spray about 1 ·· 1 to about 8 · · 1. The spinner can be heated evenly. Capillary tube and hoe are preferably self-transferable. The transfer line is preferably a heating device and a spinneret heater or cooked. The cooler of this technology preferably includes an inner wall of the tube in a circular shape, preferably from about 3 inches to about 8 Configuration mesh

487745 五、發明說明(18) 管’至少延伸至内管長度之一部份。加長徐冷器可進—步 包含至少一配置於環形空間内之多孔板,徑向延伸於該外 管之周圍,並附著於該内管之外璧,該外管之内壁或兩者 上。 篩網可放置於這些多孔板上或其鄰近。空氣可由開〇或 孔口進入徐冷器之環形空間。徐冷器可進一步包含测量或 控制空氣流速之裝置,如針閥或流量計。 本發明裝置可進一步包含收集、纺纖絲之裝置。本技藝習 知之任何裝置皆可使用,包括,但不限於,捲取輥,杈伸 輥及捲繞輥。487745 V. Description of the invention (18) The tube 'extends to at least a part of the length of the inner tube. The elongated cooler can be further advanced. It includes at least one perforated plate arranged in the annular space, extending radially around the outer tube, and attached to the outer tube of the inner tube, the inner wall of the outer tube, or both. Screens can be placed on or near these multiwell plates. The air can enter the annular space of the Xu cooler through the opening or the orifice. The Xu cooler may further include a device for measuring or controlling the air flow rate, such as a needle valve or a flow meter. The device of the present invention may further include a device for collecting and spinning filaments. Any device known in the art can be used, including, but not limited to, a take-up roll, a branch roll, and a take-up roll.

本發明用於溶紡之裝置之一具體例,你_ y T網不马炫 紡裝置1 0 0。所示為加料料斗丨〇 2,聚合物組合物,較佳為 丸粒形式’即加至其中。這些丸粒經加熱並輸送通過螺衣 擠壓機1 0 3。在聚合物或摻混物熔化後,即予加壓輸送至 泵座104,通過過濾組合件1〇5,轉移線106至具有正面1〇 之噴絲頭1 0 7。玻璃套管1 〇 9可供觀察熔融纖絲。溶融氧? 合物係經由噴絲頭1 0 7面板1 〇 8之一或多個小孔擠壓,、4 成連續股線’其導入通過加長徐冷器1 1 〇中,在此股 到遮護以防快速冷却。離開徐冷器時,紡纖即前 xA specific example of the apparatus for solvent spinning according to the present invention is the Ni_Y net spinning horse apparatus 100. Shown is a feed hopper 02, to which the polymer composition, preferably in the form of pellets, is added. These pellets are heated and transported through a screw-top extruder 103. After the polymer or blend is melted, it is pre-pressurized and conveyed to the pump base 104, passes through the filter assembly 105, and transfers the line 106 to a spinneret 107 with a front surface 10. The glass sleeve 109 can be used to observe the molten filaments. Dissolved oxygen? The composition is extruded through one or more small holes of the spinneret 1 07 panel 1 08, and is formed into a continuous strand. The strand is introduced through an elongated cooler 1 1 0, where the strand is shielded to Prevents rapid cooling. When leaving the cooler, the spinning fiber is the front x

尾形導絲器m,經導向導絲器116改變方向而接 以進行視需要之表面處理,再至一對捲取輥113,一· 伸輥1 1 4及捲繞機1 1 5。可添加額外拉伸,也可’ 一對拉 本發明方法及裝置製成之纖維可用於妨端口加鬆他親 、W 巧 πσ。Π Λ V. ^ 品可用於高級運動服裝,如短襪。此等爐維 凡寻纺袭 隹可和其他纖乡The tail wire guide m is changed in direction by the guide wire guide 116 for surface treatment as required, and then to a pair of take-up rollers 113, a stretcher 1 1 4 and a winder 1 15. Additional stretching may be added, or a pair of stretching. The fibers made by the method and device of the present invention can be used to add ports to loosen, πσ. Π Λ V. ^ goods can be used in advanced sportswear, such as socks. These furnaces are where Fan Xun seeks to attack, and Keke and other fiber towns

487745 發明說明(19) 混合織布。PTFE纖維可用於濕過濾用之工業級紗線。ptfe 纖維也可切碎供乾潤滑劑軸承之用。 實例 在實例中係使用以下聚合物(全部可自杜邦公司,487745 Description of the invention (19) Hybrid fabric. PTFE fibers can be used for industrial grade yarns for wet filtration. Ptfe fibers can also be shredded for dry lubricant bearings. Examples The following polymers are used in the examples (all available from DuPont,

Wilmington,DE)購得:Wilmington, DE) purchased:

Teflon® PFA 340,TFE與全氟丙基乙烯基醚之丘聚物Teflon® PFA 340, a polymer of TFE and perfluoropropyl vinyl ether

Teflon㊣FEP 5100, TFE,六氟丙烯及全氟乙基乙烯基醚 之共聚物Teflon㊣FEP 5100, copolymer of TFE, hexafluoropropylene and perfluoroethyl vinyl ether

Zony1® MP-1300 PTFE Teflon® TE-6462 PTFE Teflon® PTFE TE—6472 ,粒狀成形粉 Tefl0n® PTFE 62,潤滑之膏擠壓樹脂Zony1® MP-1300 PTFE Teflon® TE-6462 PTFE Teflon® PTFE TE—6472, granular shaped powder Tefl0n® PTFE 62, lubricating paste extrusion resin

Zony1® MP-1600N, PTFE 除非另有註明,所用聚合物為丁以1〇n® PFA 34〇。 tm 測忒喷絲頭溫度,剪切速率及紡絲拉伸因數(SSF )對旋 紡速度之影響。 旋紡係使用1 · 0-吋直徑鋼製單螺旋擠壓機,該擠壓機 接至紡絲泵座,其再依次連接至具以下特點之喷絲頭銜 器··使用旁通板代替紡絲泵。使用如圖2所示之加長噴絲 2,其中nh’ π為2· 0吋。使用3〇_密爾39一孔噴絲頭,其中 全部孔全在一圓内,來涵蓋自低至中等剪切速率,例如 6 〇 /秒至約1 8 〇 /秒之剪切速率,而使用丨5 —密爾2 5 —孔噴絲、 頭來涵蓋中至高剪切速率,例如約35〇 /秒至約丨,15〇 /秒’、。 五、發明說^(20^ &quot; — ' 寸向’ 1 · 25对内徑線圈加熱器(工業加熱器公司)包纏 絲/長噴絲頭之下1吋部份周圍,並用其將包括面板之噴 、j邵份分開加熱。使用習知之捲取輥和捲繞機。 、、絲頭前的溫度分佈為螺旋擠壓機3 5 〇 t,泵座至佔於 壓機與喷絲頭間之組合濾器38〇它。使用Tef l〇n@ pFA 40進行三次旋坊作業。噴絲頭溫度設定於42〇艽,46〇它 或 5〇〇 °。。 在42〇C時’溶體破裂(M.F·)係在約180/sec勢切速率發 生。全部纖絲完整而無熔體破裂之最高可能旋紡速度為在 剪切速率約90/秒時稍微低於219 mpm。在此速度及剪切時 之纖維韌度為1 · 02 gpd。最後纖絲斷裂之最高旋紡速度為 在剪切速率約60/秒時49 0 mpm,且纖維韌度為1.68 gpd, 纖絲旦數則為4. 0。 在4 6 0 °C時,可旋紡之剪切速率提高到稍低於7 2 0 /秒才 出現熔體破裂。最初纖維斷裂時之最高測得旋紡速度為在 剪切速率160/秒時435 mpm,且纖維擁有韌度為1. 13 gpd。最後纖維斷裂之最高旋紡速度為在剪切速率約160/ 秒時8 5 0 mpm。旋紡至最後纖絲斷裂之纖維之最高纖維韌 度係1· 61 gpd。旋紡速度為580 mpm而纖絲旦數為2· 〇。 5 0 0 °C噴絲頭樣本之剪切速率對旋紡拉伸因數之曲線顯 示於圖11。深色三角形代表最初纖維斷裂之數據,而空心 三角形則代表最後纖絲斷裂之數據。在5 0 0 °C時,可旋紡 剪切速率,在熔體破裂出現之前’推進到稍低於1,150/ 秒。最初纖維斷裂之最高旋紡速度為在剪切速率約1 8 0 /秒Zony1® MP-1600N, PTFE Unless otherwise stated, the polymer used is 10n® PFA 34. tm measures the effects of spinneret temperature, shear rate, and spinning stretch factor (SSF) on spinning speed. Rotary spinning uses a 1.0-inch-diameter steel single-screw extruder connected to a spinning pump base, which in turn is connected to a spinneret with the following characteristics: · Bypass plates are used instead of spinning Wire pump. An elongated spinneret 2 as shown in Fig. 2 was used, where nh 'π was 2.0 inches. A 30_Mill 39-hole spinneret is used, in which all holes are all in a circle to cover a low to medium shear rate, such as a shear rate of 60 / sec to about 180 / sec. 5—Mill 2 5—hole spinneret, head to cover medium to high shear rates, for example, about 350 / second to about 1,500, / second '. V. Invention ^ (20 ^ &quot; — 'inch to' 1 · 25 pairs of inner diameter coil heater (Industrial heater company) wrapped around the 1 inch portion of the filament / long spinneret, and will use it to include Panel spraying and heating are separately heated. The conventional coiling roller and winding machine are used. The temperature distribution in front of the silk head is a screw extruder of 3 〇t, and the pump seat is occupied by the press and the spinneret. The combination filter was 38 ° it. Three swirling operations were performed using Tef lon @ pFA 40. The spinneret temperature was set at 42.0 ° C, 4600 ° or 500 ° ... 'Solution at 42 ° C Fracture (MF ·) occurs at a potential shear rate of about 180 / sec. The highest possible spinning speed of all filaments without melt fracture is slightly below 219 mpm at a shear rate of about 90 / sec. At this speed And the fiber tenacity at the time of shearing is 1.02 gpd. The maximum spinning speed of the final fiber break is 49 0 mpm at a shear rate of about 60 / s, and the fiber tenacity is 1.68 gpd, and the fiber denier is It is 4.0. At 4 60 ° C, the spin-spinning shear rate is increased to slightly below 7 2 0 / second before melt fracture occurs. The highest measured at the time of initial fiber break The spinning speed was 435 mpm at a shear rate of 160 / second, and the fiber possessed a tenacity of 1.13 gpd. The highest spinning speed of the final fiber break was 850 mpm at a shear rate of about 160 / second. Spinning The highest fiber tenacity of the fiber to the last filament break was 1. 61 gpd. The spinning speed was 580 mpm and the fiber denier was 2.0. The shear rate of the spinneret sample at 50 0 ° C was measured for spinning The curve of the stretching factor is shown in Figure 11. The dark triangles represent the data of the initial fiber break, and the hollow triangles represent the data of the last filament break. At 500 ° C, the spin-spinning shear rate is in the melt Prior to the occurrence of cracking, it was advanced to slightly below 1,150 / sec. The highest spinning speed of the initial fiber break was at a shear rate of about 180 / sec.

487745 五、發明說明(21) 時9 3 3 mpm,且纖維擁有韌度為丨.〇4 gpd。最後纖維斷裂 之最高旋紡速度為在約180/秒時930 m pm,且在此速度下 動度為1.15 gpd。 因此,可看出,隨著喷絲頭溫度由4 2 〇。〇增至5 〇 〇。〇,可 達到的旋紡速度即增加4. 3倍。 溫度,在恒定剪切速率之最初纖維斷裂下,對SSF產生 正面影響,如圖12所示。深色圓形顯示42〇它時之SSF ;深 色方形顯示4 60 °C時之SSF及深色三角形顯示5〇〇 °c之SSF。 車乂向之SSF係意指在相同流通速率及一定喷絲孔大小下, 捲取輥速度較旋紡速度為高。 ^在其餘實例中,除非另有註明,旋紡係使用上述設備進 仃’但係使用1 · 5吋直徑耐腐蝕單螺旋擠壓機(κ丨丨1丨〇n擠 $機公司,Cedar Grove,N.J·製造)。此種擠壓機有三個 =開之加熱區,在以下溫度分佈中以”螺旋區1、2及3 &quot;表 不°使用夾環將擠壓機和螺旋銜接器結合固定在一起,而 螺旋銜接器再固著於喷絲頭銜接器。夾環係使用圓柱棒匣 式加熱器加熱,而螺旋銜接器及喷絲頭銜接器則使用匣式 加熱器加熱。帶式加熱器係用於加熱過濾組合件。除非另 有言主明’任何存在的轉移線及噴絲頭正面皆使用帶式或線 圈加熱器加熱。使用習用捲取及捲繞裝置,包括Lees〇na 捲繞機。 旋紡係使用30 -密爾3〇 ~孔加長噴絲頭。喷射速度為1 · 9 ’以流通速率丨· 3克/分/孔進行。裝置之旋紡溫度() 487745487745 V. Description of the invention (21): 9 3 3 mpm, and the fiber has a tenacity of .04 gpd. The maximum spinning speed of the final fiber break was 930 m pm at about 180 / s, and the mobility was 1.15 gpd at this speed. Therefore, it can be seen that as the spinneret temperature increases from 4 2 0. 〇 increased to 500. 〇, the achievable spinning speed increased by 4.3 times. Temperature, at the initial fiber break at a constant shear rate, has a positive effect on SSF, as shown in Figure 12. Dark circles show SSF at 42 °; dark squares show SSF at 4 60 ° C and dark triangles show SSF at 500 ° c. The SSF in the turning direction means that at the same flow rate and a certain spinning hole size, the take-up roller speed is higher than the spinning speed. ^ In the remaining examples, unless otherwise noted, the spinning system uses the above-mentioned equipment, but uses a 1.5-inch diameter corrosion-resistant single-screw extruder (κ 丨 丨 1 丨 〇n extruder company, Cedar Grove , Made by NJ ·). This type of extruder has three heating zones that are open. In the following temperature distribution, "screw zones 1, 2 and 3" are used to express the use of clamp rings to fix the extruder and the screw adapter together, and the screw The adapter is then fixed to the spinner adapter. The clamp ring is heated by a cylindrical cartridge heater, while the spiral adapter and the spinner adapter are heated by a cassette heater. The belt heater is used for heating Filter assembly. Unless otherwise stated, 'Any existing transfer line and spinneret front is heated with a tape or coil heater. Use conventional winding and winding devices, including Leeson winders. Spinning Use 30-mil 30 ~ hole extension spinneret. Spray speed is 1 · 9 'at flow rate 丨 · 3g / min / hole. Spinning temperature of the device () 487745

分佈為: 螺旋區 1 ’, 2— 350 350 螺旋銜接噴絲頭銜 ^-——-—器噴絲頭 350 380 353 480 480 500 剪切迷率為3 2 8/秒,達到的最大旋紡逮度 mpe ’以最初纖絲斷裂(FFB)之旋纺拉伸因$ 8 所得纖維之旦數,勤度,伸長率及模數分K5:。 gpd/61%/5·6 gpd 。 ⑺马·11 d/Ο·了6 實例3 此實例之旋紡係類似於實例2進行,但下 5吋问成錐形之鋁製徐冷器, 噴絲頭冒出時遮嗜他楚么么吳目七 以在熔鍅纖絲自 ^ ^ 、護彼等。徐冷器具方形剖面,頂端為丨2吋 π二乂 &gt;开^芏底部為1 · 〇吋四方。使用實例2所用相同 ‘度/刀仰,但有以下改變:38〇。〇螺旋銜接器,47〇它噴絲 頭銜接器,4 70。(:組合濾器。剪切速率為32 8/秒。在相同 流通速率1,3克/分/孔下及使用實例2所用相同3〇一密爾3〇一 孔加長喷絲頭,最高旋紡速度提高了 35%,或385 mpm至 1,485 mpm ’以在FFB時之SSF為782而言。所得織維之旦 數’勃度’伸長率及模數分別為:9.4 d/Ό. 了 2 gpd /了 6%/ 5.1 g p d 〇 : 實例4 此旋紡係類似於實例2及3進行,但使兩不同的徐冷器' 為此旋紡,使用的是具有12吋xl2吋方形剖面之6呎3吋高The distribution is: Spiral zone 1 ', 2—350 350 Spiral joint spinneret ^ -——--- Applicator spinneret 350 380 353 480 480 500 Shearing rate is 3 2 8 / s The degree mpe 'is based on the spinning draw of the initial filament break (FFB). The fiber denier, duty, elongation and modulus of the fiber obtained by $ 8 are K5 :. gpd / 61% / 5 · 6 gpd. ⑺ 马 · 11 d / Ο · 了 6 Example 3 The spin spinning system of this example is performed similarly to Example 2, but the next 5 inches are asked to form a cone-shaped aluminum cooler. Does the spinneret appear to obscure others? What Wu Muqi took in melting the filaments to protect them. The cross section of the Xu cold appliance is square, the top is 2 inches, and the bottom is 1.0 square. The same ‘degree / blade elevation’ used in Example 2 was used, but with the following change: 38 °. 〇 Spiral adapter, 47 ° It spinneret adapter, 4 70. (: Combined filter. Shear rate is 32 8 / sec. At the same flow rate of 1.3 g / min / hole and the same 30-mil 30-hole extension spinneret used in the same example 2, the highest spin spinning Increased speed by 35%, or 385 mpm to 1,485 mpm, based on the SSF at FFB of 782. The obtained weaving and weaving denier 'Broth' elongation and modulus are: 9.4 d / Ό. 2 gpd /% 6% / 5.1 gpd 〇: Example 4 This spin spinning system was performed similarly to Examples 2 and 3, but two different spin coolers were used for this spin spinning, using 6 feet with a 12-inch x 12-inch square cross-section. 3 inches tall

第25頁 487745 五、發明說明(2Γ)) 自立Luc it e®徐冷器。使用實例3所用相同溫度。剪切速率 為328 /秒。最高旋紡速度提高至丨,756 mpm,以在FFB時之 SSF為9 24 ’而言。此與實例2比較旋紡速度增加了 60%,或與 實例3比較旋紡速度增加了 1 8%。所得纖維之旦數,韌度, 伸長率及模數分別為:6.0 d/1.16 gpd/28%/l〇 gPd。 實例5 本實例使用如圖3所示具有縮短加長噴絲頭之喷絲頭總 成。過慮組合件底面與嗔絲頭面板間之距離為1 · 2 5忖。使 用實例4所用之相同溫度分佈及相同6吋3呎Luc it e®徐冷 器。剪切速率為32 8 /秒。達到的最高旋紡速度為1, 860 !1^111’以在??8時之33?為979而言。此一高速樣本未測試:纖 維性質,但在相同條件下以剪切速率342/秒及旋紡速度 1,7 0 1 mpm旋紡之另一樣本則具纖維性質(旦數,韌度,伸 κ 率及模數分別)為:了,6 d/1.01 gpd/68%/6.2 gpd。 實例6 旋纺係如實例5進行,但縮短之加長喷絲頭使用感應加 熱線圈加熱’並使用以下溫度分佈上之改變:44 0乞組合濾 器’ 5 2 2 - 5 3 1 °C喷絲頭。所得纖維之旦數,韌度,伸長率 及模數分別為:9. 6 d/1. 06 gpd/49%/8. 7 gpd。 實例7 . *7~ ' 二: 旋紡係如I倒6進行,但所用徐冷器為實例3所用相同:二錐 形錯製徐冷器。、、為了觀察紡絲流水線,在徐冷器頂部增如 一 12 -叶立方透明Lucite®箱。剪切速率為342/秒。FFB時 之最高旋紡速度為I860 mpin。所得纖維之旦數,韌度,Page 25 487745 V. Description of the invention (2Γ)) Self-supporting Luc it e® cooler. The same temperature used in Example 3 was used. The shear rate is 328 / sec. The maximum spinning speed is increased to 丨, 756 mpm, with an SSF of 9 24 ′ at FFB. This is a 60% increase in spin speed compared to Example 2, or an 18% increase in spin speed compared to Example 3. The denier, tenacity, elongation and modulus of the obtained fibers were 6.0 d / 1.16 gpd / 28% / 10 gPd, respectively. Example 5 This example uses a spinneret assembly having a shortened and extended spinneret as shown in FIG. The distance between the bottom surface of the filter assembly and the reed head panel is 1 · 2 5 忖. The same temperature distribution and the same 6 inch 3 foot Luc it e® cooler used in Example 4 were used. The shear rate is 32 8 / sec. The maximum spinning speed reached is 1,860! 1 ^ 111 ’ ? 33 o'clock at 8 o'clock is 979. This high-speed sample is not tested: fiber properties, but under the same conditions, the other samples spun at a shear rate of 342 / s and a spinning speed of 7.1 0 1 mpm have fiber properties (denier, toughness, elongation κ The ratio and modulus are respectively): Yes, 6 d / 1.01 gpd / 68% / 6.2 gpd. Example 6 The spinning system was performed as in Example 5, but the shortened lengthened spinneret was heated using an induction heating coil and used the following temperature distribution change: 44 0 combined filter 5 2 2-5 3 1 ° C spinneret . The denier, tenacity, elongation and modulus of the obtained fibers were: 9.6 d / 1. 06 gpd / 49% / 8. 7 gpd. Example 7. * 7 ~ 'Second: The spinning system is performed as I down 6 but the Xu cooler used is the same as that used in Example 3: the two cone-shaped mismatched Xu cooler. In order to observe the spinning assembly line, a 12-leaf cubic transparent Lucite® box is added on the top of the Xu cooler. The shear rate is 342 / second. The maximum spinning speed at FFB is I860 mpin. Denier, tenacity of the obtained fiber,

第26頁 487745 五、發明說明(24) d/Ι. 02 gpd/54%/7. 7 gpd 伸長率及模數分別為: 實例8 旋紡係使用如圖4所示&gt; _ ^ 式加熱器(可自工業加妖絲頭f行’噴絲頭中央有g 嗔絲頭外面有標準帶式加\\司,s\ratford, CT購得)而 面板之噴絲頭長度為125…、益。過濾組合件底面至噴絲頭 • &lt; 5〜饤。所用溫度分佈為: 螺旋區 1 2 350 350 350 ^ 螺旋銜噴絲頭組合濾噴絲頭 $3^8雙銜接器 器 中央噴絲頭 380 380 411 410 496 500 所用喷絲頭有2 6孔;铁而 ^ 樣保持不變。因此,;=、乡母孔之流通量與實例2至6者一 纺速度為丨,9 7 6 mpm,以ϋ率約相同,即3 4 2/秒。最高旋 度增加6%係歸因於溶體t 2為1,040而言。與實例5比較速 纖維性質-…勃度在Λν絲頭中有更均Λ之加熱。 gPd/55%/L〇 gpd。 伸長率及模數分別為:5.6 d/1.09 以潰絲頭銜接器及組合濾器4〇〇艽及噴絲頭相同5〇〇 t旋 纺之另、一樣+所得最高速度在SS F為丨,〇丨〇時為丨,92〇 mpm°纖維勃度較高,而旦數,韌度,伸長率及模數之纖 难 U 貝 /則得戈口下:5 . 6 d / 1, 2 5 g p d / 5 4 % / 7 g P d。 實例9 使用如圖6 ^斤示噴絲頭總成測試本具體例達到高旋紡連 度之效力。$毫菊1 5孔1 · 0吋直徑具3 0 -密爾直徑孔之圓:爹噴 絲頭。所用徐冷器為實例4所用之6呎3吋匕^丨七^徐冷—Page 26 487745 V. Description of the invention (24) d / Ι. 02 gpd / 54% / 7. 7 gpd Elongation and modulus are as follows: Example 8 The spinning system is used as shown in Figure 4 &gt; _ ^ heating (Can be obtained from the industrial processing demon silk head f line 'the spinner has g in the center of the spinneret and a standard belt type is added outside the spar, s \ ratford, CT), and the spinneret length of the panel is 125 ..., beneficial. Filter assembly bottom to spinneret • &lt; 5 ~ 5. The temperature distribution used is: Spiral zone 1 2 350 350 350 ^ Spiral spinneret combined filter spinneret $ 3 ^ 8 Dual adapter central spinneret 380 380 411 410 496 500 Spinneret used has 2 6 holes; iron But ^ remains the same. Therefore, the flow rate of; =, the mother hole is the same as that of Examples 2 to 6. The spinning speed is 丨, 9 7 6 mpm, and the rate is about the same, that is, 3 4 2 / sec. The 6% increase in the maximum rotation is attributable to a solution t 2 of 1,040. Compared with Example 5, the fiber properties -... the degree of brilliance has a more uniform heating in the Δν silk head. gPd / 55% / L gpd. The elongation and modulus are respectively: 5.6 d / 1.09. Spinning the same with the spinneret adapter and combination filter 4004 and the spinneret are the same and the same. + The maximum speed obtained is SS F, 〇 丨 〇 at 丨, 9200mpm ° fiber stiffness is high, while the denier, toughness, elongation and modulus of the fiber are difficult to reach: 5.6 d / 1, 2 5 gpd / 5 4% / 7 g P d. Example 9 Using the spinneret assembly shown in Figure 6 to test the effectiveness of this specific example to achieve high spin spinning continuity. $ 零 菊 1 5 hole 1 · 0 inch diameter with 30-mil diameter hole round: daddy silk head. The Xu cooler used was the 6-foot-3 inch dagger used in Example 4 ^ 丨 七 ^ 徐 冷 —

0:\62\62592.PTD 第27頁 487745 五、發明說明(25) 器。組合濾杰使用帶式加熱器。自過濾組合件底面至喷絲 頭圓盤測得之轉移線為3 · 1 2 5忖。 在螺旋rpm 4. 0下,總流通速率為2〇 · 3克/分(2· 7磅/時) 或1 · 3 5克/分/孔。此與先前實例之每孔流通速率大致相 同。在以下條件下旋紡速度達到丨,8丨6 m p m時全部纖絲都 完整:螺旋擠壓機全部三區溫度都設定於3 5 0 °C ;夾環及螺 旋銜接器設定於3 8 0 t ,則定之熔體溫度為3 8 9 °C ;噴絲頭 銜接器及組合濾器設定於4 3 0 °C ;轉移線設定於4 7 0 °C ;及 噴絲頭設定於5 0 0 °C。 噴絲頭銜接器及組合濾器溫度降低與轉移線溫度提高進 一步改良了旋紡速度: 噴絲頭銜接器 性質 ; 及組合濾器 轉移線 噴絲頭 最高速度 旦數/韌度/伸長率/觀 430〇C 474〇C 500°C 1,816 mpm 6.5/1.20/45%/10 420〇C 471〇C 500°C 1,969 mpm 5.5/1.24/24%/12 410°C 471〇C 500°C 1,965 mpm 5.6/1.38/35%/! 3 400°C 470〇C 500°C 1,950 mpm 5.8/1.27/32%/12 400°C 480〇C 500°C 1,994 mpm 5.3/1.48/48%/! 2 旋紡速度達到1,9 9 4 mpm係較實例4之旋紡速度1 , 756 mpm改良了 14%。剪切速率為34 7 /秒。纖維韌度自1 · 16 gpd 至1 · 4 8 gpd毛良了 2 8 °/。。此一強度上之改良,除了較高承 度外,歸功H么合物較少或無降解。 二:子 在1,0 0 0 mpm、、時,收集若干紗線樣本以測試旋紡過程冬0: \ 62 \ 62592.PTD Page 27 487745 V. Description of the invention (25). The combination filter uses a belt heater. The transfer line measured from the bottom of the filter assembly to the spinneret disc was 3 · 1 2 5 忖. At a screw rpm of 4.0, the total flow rate was 2.0 3 g / min (2.7 lb / hr) or 1.3 g / min / well. This is approximately the same as the flow rate per well in the previous example. Under the following conditions, the spinning speed reached 丨, all filaments were complete at 8 丨 6 mpm: the temperature of all three zones of the screw extruder was set to 3 50 ° C; the clamp ring and the screw adapter were set to 3 8 0 t , The set melt temperature is 3 89 ° C; the spinner head adapter and combination filter are set at 4 30 ° C; the transfer line is set at 4 7 0 ° C; and the spinneret is set at 5 0 ° C . Spinneret adapter and combined filter temperature reduction and transfer line temperature increase further improved spinning speed: Spinneret adapter properties; and combined filter transfer line spinneret maximum speed denier / toughness / elongation / view 〇C 474〇C 500 ° C 1,816 mpm 6.5 / 1.20 / 45% / 10 420〇C 471〇C 500 ° C 1,969 mpm 5.5 / 1.24 / 24% / 12 410 ° C 471〇C 500 ° C 1,965 mpm 5.6 / 1.38 / 35% /! 3 400 ° C 470 ° C 500 ° C 1,950 mpm 5.8 / 1.27 / 32% / 12 400 ° C 480 ° C 500 ° C 1,994 mpm 5.3 / 1.48 / 48% /! 2 Spinning speed reached 1,9 9 4 mpm is a 14% improvement over the spinning speed of 1,756 mpm of Example 4. The shear rate was 34 7 / sec. The fiber tenacity ranged from 1 · 16 gpd to 1 · 4 8 gpd. . This improvement in strength, in addition to higher load, is due to less or no degradation of the H-mer compound. Two: Sub At 1, 00 mpm, hour, collect several yarn samples to test the spinning process in winter

O:\62\62592.PTO 第2«頁 487745O: \ 62 \ 62592.PTO Page 2 «page 487745

長期穩疋性。纖絲旋纺連續性極佳,可捲繞β Q分及丨〇 5 分,兩者皆係隨意落捲。纖維性質〜旦數/韌度/伸長率/模 數分別為:,11 d/0.94-1.01 gpd/68-80%/7·5 gpd。 在1,5 Ο G in p m疑纺並持續4分之一樣本,其纖絲之旦數/ 勃度/伸長率/模數分別為:7.2 d/1.20 gpd/39%/11 gpd。 在1,OOO mpm旋紡並在28 0 t下線内拉伸丨· 4倍之另一樣 本,其纖維之旦數/韌度/伸長率/模數分別為:7 · 6 d / 1 . 4工 g p d / 2 5 % / 1 4 g p d 〇Long-term stability. Filament spinning has excellent continuity, and can be wound with β Q points and 丨 05 points, both of which are randomly dropped. The fiber properties ~ denier / toughness / elongation / modulus are: 11 d / 0.94-1.01 gpd / 68-80% / 7.5 gpd. At 1,50 G in p m of suspected spinning and lasting a quarter of a sample, the denier of the filaments / brightness / elongation / modulus were: 7.2 d / 1.20 gpd / 39% / 11 gpd. Spin-spun at 1,000 mpm and stretched in the lower line at 2800 t. In another sample, the denier / toughness / elongation / modulus of the fiber was 7 · 6 d / 1.4. Gpd / 2 5% / 1 4 gpd 〇

對在你冷器出口’沿加熱之捲取輥之上及捲繞機之上的 紗線路徑所收集到的空氣樣本所作之測量並未測出有任何 釋出氣體。聚合物熱降解會產生氣體。由於釋出的氣體也 可犯會入或溶於纖維内,故在管瓶及其頭部空間枚集-到 的纖維,在不同時間使用紅外線分光法,氣體層析法/質 語法及離子層析法檢測,也不含有任何釋出氣體。此外, 將纖維樣本加熱至2 0 〇。(:以期釋出任何溶解的氣體,但均 未檢出。這些結果證實,儘管在本方法中使用高達5 〇〇乞 之溫度以促進高剪切速率,高旋紡速度及高SSF,但並無 聚合物降解。PFA聚合物在承受低至425 °C之溫度超過1分 鐘即會輕易降解。Measurements of air samples collected at the exit of your cooler along the yarn path above the heated take-up roll and above the winder did not detect any outgassing. Thermal degradation of polymers generates gases. Since the released gas can also enter or dissolve in the fiber, the fibers collected in the vial and its head space are used at different times using infrared spectrometry, gas chromatography / mass grammar, and ion layer. Analytical method does not contain any released gas. In addition, the fiber sample was heated to 200. (: In order to release any dissolved gas, but none were detected. These results confirm that although temperatures as high as 500 ° C are used in this method to promote high shear rates, high spin speeds, and high SSF, but No polymer degradation. PFA polymers will easily degrade when subjected to temperatures as low as 425 ° C for more than 1 minute.

實例1 0 此旋紡係傘於實例9,但約1 / 8对之感應加熱器線齋、包 在噴絲頭正面二次。螺旋擠壓機至螵旋銜接器之溫度分伟 保持於與實例9相同。剪切速率為34 7/秒。SSF在FFB時為 1,087時,最高旋紡速度(甴實例9之1,994 mpm)至2, 06 5Example 10 This spin-spun umbrella was used in Example 9, but about 1/8 of the induction heater was fastened and wrapped on the front of the spinneret twice. The temperature of the screw extruder to the screw adapter was kept the same as in Example 9. The shear rate was 34 7 / sec. SSF at 1,087 at FFB, maximum spinning speed (1,994 mpm in Example 9) to 2, 06 5

第29頁 487745 五、發明說明(27) m p m有3 . 6 %之改良。所得最高速度及性質顯示於下 噴絲頭銜接器 及組合濾器 轉移線 噴絲頭 性質 最高速度旦數/韌度/伸長_模數Page 29 487745 V. Description of the invention (27) m p m has an improvement of 3.6%. The highest speed and properties obtained are shown in the lower spinneret adapter and combined filter transfer line spinneret properties. Maximum speed denier / toughness / elongation_modulus

430〇C430〇C

400°C 470〇C400 ° C 470〇C

480〇C 520°C480〇C 520 ° C

525〇C 1,910 mpm 2,065 mpm 6.9/1.04/59%/6.5 5.6/1.2i/32%/ll 旋紡連續性證明極佳,當樣本在9 9 7 m p m旋紡9 0分且隨 意落捲時。纖維性質-旦數/韌度/伸長率/模數分別為: 1 0· 3 d/0. 97 gpd/68%/3. 6 gpd。 實例1 1 使用如圖8所示之喷絲頭總成,喷絲頭正面直徑為 1 . 7 5&quot;。有3 0 -密爾直徑之孔6 0個3以總流通量8 1 g p in或 1 0. 了碎/ a寺(pph)言,每孔流通速率為1 . 35 gpm。使用實例 7頂端有1 2吋Luc i te®箱之錐形鋁製徐冷器《所用溫度 (°C )分佈為: 螺旋區 1 3 螺旋銜噴絲頭組合濾 夾環 接器銜接器 器 轉移線噴絲頭 350 350 350 380 380 400 400 477 500 最高旋紡速度為1 , 3 5 9 m p m。剪切速率為3 4 7 /秒。纖維 性質-旦數/韌度/伸長率/模數分別為:8.0 d/1.04 gp&lt;!/ 6 7 0/〇/7· 1 gpd。 旋紡速^與如實例7之3 0孔噴絲頭比較降低之理由,-被 認為是總流通、、量大2倍致徐冷器保留太多熱量之故。:擦冷525 ° C 1,910 mpm 2,065 mpm 6.9 / 1.04 / 59% / 6.5 5.6 / 1.2i / 32% / ll Spinning continuity proved to be excellent, when the sample was spun at 9 97 m p m for 90 minutes and unwinded at will. The fiber properties-denier / toughness / elongation / modulus were: 1 0 · 3 d / 0. 97 gpd / 68% / 3. 6 gpd. Example 11 1 A spinneret assembly as shown in FIG. 8 was used, and the front diameter of the spinneret was 1.7 5 &quot;. There are 60 holes with a diameter of 30-mil, and the total flow rate is 8 1 g p in or 10. The flow rate per hole is 1. 35 gpm. Example 7 Conical aluminum cooler with 12 inch Lucite® box at the top "The temperature (° C) distribution is: Spiral zone 1 3 Spiral spinneret combined filter clamp ring adapter adapter connector transfer Spinneret 350 350 350 380 380 400 400 477 500 The maximum spinning speed is 1, 3 5 9 mpm. The shear rate is 3 4 7 / sec. The fiber properties-denier / toughness / elongation / modulus were: 8.0 d / 1.04 gp &lt;! / 6 7 0 / 〇 / 7.1 gpd. The reason why the spinning speed is lower than that of the 30-hole spinneret of Example 7 is considered to be that the total amount of circulation and the volume is twice as large, which causes the Xu cooler to retain too much heat. : Wipe cold

O:\62\62592.PTD 第30頁 487745 五、發明說明(28) 器係以較大容量之6吸3对L u c i t e ®箱徐冷器代替 ^ 旋紡速度增高至1,500 mpm。所用溫度分(。厂、 最南 匕)佈為: 螺旋區 1 螺旋銜噴絲頭組合^ 夾環 接器銜接器 350 !50 350 380 380 420 噴絲頭 420 500 520 纖維性質-旦數/韌度/伸長率/模數分別為:7.2 d/1 2Q gpd/48%/9.4 gpd 〇 為減低徐冷器内之過度熱保留,將沿徐冷器長度而設且 幾乎涵蓋其一側之徐冷器門完全打開並以多孔筛網覆蓋以 提供安靜的空氣移動而不產生湍流。使用3 / 3 2时直徑孔, 孔中心至中心隔開3/ 1 6吋之多孔金屬板,與使用門關閉之 徐冷器比較,最高旋紡速度至1,623 mpm改良了 8%,使用 以下稍微不同之溫度(°C )分佈: 螺旋區 ^旋銜噴絲頭組合濾 __1^__證^銜接器 器 轉移線噴絲萌 350 350 350 380 380 400 400 500 520 纖維性質-旦數/韌度/伸長率/模數分別為:7. 5 d/i. 18 gpd/5 0 %/8. 9 gpd 〇 在上述以^^金屬板覆蓋之前徐冷器觀察到一些非均心句 之空氣移動’因:為有擴散的空氣在前面進出移動而其他三 面則無。放置於噴絲頭正面附近的熱電偶顯示溫度由3 6 8 °C變動至3 9 0 °C,或變化2 2 °C。O: \ 62 \ 62592.PTD Page 30 487745 V. Description of the invention (28) The device is replaced by a large-capacity 6 suction 3 pair Lucite® box cooler. ^ The spinning speed is increased to 1,500 mpm. The temperature used (.factory, southernmost) cloth is: Spiral zone 1 Spiral spinneret combination ^ Clip ring connector adapter 350! 50 350 380 380 420 Spinneret 420 500 520 Fiber properties-denier / toughness Degrees / elongation / modulus are: 7.2 d / 1 2Q gpd / 48% / 9.4 gpd 〇 To reduce excessive heat retention in the cooler, it will be set along the length of the cooler and almost covers one side of the cooler. The cooler door is fully open and covered with a perforated screen to provide quiet air movement without turbulence. The use of 3/3 2 hole diameter holes, 3/16 inches of porous metal plates separated from the center of the hole, compared with the use of the closed door cooler, the maximum spinning speed to 1,623 mpm improved by 8%, using the following slightly Different temperature (° C) distribution: Spiral zone ^ Spindle spinneret combination filter __1 ^ __ Certificate ^ Connector transfer line spinneret 350 350 350 380 380 400 400 500 520 Fiber properties-denier / toughness Degrees / elongation / modulus are: 7. 5 d / i. 18 gpd / 5 0% / 8. 9 gpd 〇 Before the above ^^ metal plate was covered, some cool air was observed by the cooler. The 'moving' cause: there is diffused air moving in and out in the front and none on the other three sides. The thermocouple placed near the front of the spinneret showed a temperature change from 3 6 8 ° C to 3 9 0 ° C, or 2 2 ° C.

第31頁 487745 五、發明說明(29) 使用較大的Lu cite®徐冷器;剖面20吋x24吋,高度71. 5 吋,頂部有噴絲頭開口而底部有可接近紡絲流水線之開 口。旋紡時,有太多的上下空氣運動,而致旋紡速度降 低。 將插入物放至徐冷器底部以使20吋x24吋開口縮小至20 吋四方。這些插入物向下成錐形,俾紗線會掉入。所測量 溫度波動仍高至2 5 °C,但實際溫度明顯較冷,2 4 0 °C至2 6 5 °C (註:雖然測得之溫度較小型徐冷器為低,但兩徐冷器間 絕對溫度之比較不應太正確視之,因為熱電偶之位置可能 無法精確定位)。空氣穩定性明顯較安靜。以相同溫度分 佈而言,最高旋紡速度改良了 ,且比小型徐冷器所記錄到 的稍高:1,68 0 mpm。纖維性質-旦數/韌度/伸長率/模數分 別為:8,2 d/0.84 gpd/59%/5.9 gpd 。 實例1 2 以前述設計之徐冷器而言,欲在徐冷器底部接觸紗線以 便將其送至吸管搶以使紗線在全部紗線加工路程至捲繞機 中生頭(s t r i ng i ng up ),有些困難。此外,溶融紡絲流水 線之徐冷端視自然空氣對流不加以控制而定。這二個問題 係以如圖1 0 A及1 0 B所示徐冷器設計解決。此一徐冷器輕易 地容許紗線在其底部圓錐形出口集束捲繞(p i c k i n g - u p )。 從壓縮空氣f而來的進入空氣經内及外管間的環.形空間s, 並向上通過若+干、細網目篩網以消除渦流,進入頂部並徑向 朝向熔融纖絲。空氣容許經由徐冷器之下孔α進入,而空 氣流速則以針闊控制並以流量計測量。内管上部6吋的溫Page 31 487745 V. Description of the invention (29) Use a larger Lu cite® cooler; 20 ”x 24” in cross section, 71.5 ”in height, with a spinneret opening at the top and an opening accessible to the spinning line at the bottom . During spinning, there is too much up-and-down air movement, which reduces the spinning speed. Place the insert on the bottom of the cooler to reduce the 20 "x 24" opening to a 20 "square. These inserts are tapered downwards and the reeling yarn will fall in. The measured temperature fluctuation is still as high as 25 ° C, but the actual temperature is significantly colder, 240 ° C to 265 ° C (Note: Although the measured temperature of the smaller type cooler is low, but the two The comparison of absolute temperature between devices should not be viewed too correctly, because the position of the thermocouple may not be accurately positioned). The air stability is significantly quieter. For the same temperature distribution, the maximum spinning speed is improved and slightly higher than that recorded by the small spin cooler: 1,680 mpm. Fiber properties-denier / toughness / elongation / modulus are: 8.2 d / 0.84 gpd / 59% / 5.9 gpd. Example 1 2 In the case of the Xu cooler of the aforementioned design, it is necessary to contact the yarn at the bottom of the Xu cooler in order to send it to the suction pipe to make the yarn reach the end of the winding machine during the entire yarn processing distance (stri ng i ng up), some difficulties. In addition, the cold end of the melt spinning line depends on the natural air convection being left uncontrolled. These two problems are solved by the design of the cooler as shown in Figures 10 A and 10 B. This cooler easily allows the yarn to be bundled around its bottom conical outlet (p i c k i n g-u p). The incoming air from the compressed air f passes through the ring-shaped space s between the inner and outer tubes, and passes upward through the dry + fine mesh screen to eliminate vortices, enters the top and radially faces the molten filaments. Air is allowed to enter through the hole α below the cooler, while the air velocity is controlled by the needle width and measured by a flow meter. 6 inches above the inner tube

487745 五、發明說明(30) 度可藉隔開1吋之熱電偶偵測。内及外管間之空間入口孔 之高度可調整於1 · 0吋至4. 0吋之間。1,0吋高的玻璃環可 供目視觀’察熔融紡絲流水線及噴絲頭正面。 旋紡係使用如圖8構型之噴絲頭總成進行,該總成為3 0 孔3 9· 4 -密爾直徑,具長度/直徑比為3. 0之喷絲頭。旋紡 係以流通量為1 · 3 gpm,在以下溫度分佈下進行:3 5 0。(:, 螺旋擠壓機至組合濾器;45 0 °C,轉移線;及5 0 0 °C,噴絲 頭。徐冷器内部之溫度為:2 6 8 °C,距噴絲頭正面1吋處; 2 5 2 °C ’距喷絲頭正面2吋處;及2 2 2 °C,距喷絲頭正面6吋 處。溫度波動可予忽視,因變化僅2 °C,而先前實例徐冷 器所觀察到的變化則高達2 5 °C。剪切速率為1 5 1 /秒。達到 的最高旋紡速度為1,737 mpm,纖維性質-旦數/韌度/伸長 率 / 模數分別為:4. 2 d/1 · 17 gpd/57%/7. 8 gpd。 當極佳的旋紡連續性,由1,0 0 5 mpm之3. 5小時紗線捲裝 及在240 °C 702 mpm之捲取親速度線内拉伸1,4倍表現時, 此一旋紡系統之堅實性即獲得證實。紗線捲裝之淨重超過 2 0磅,且在6 · 0吋筒管上之絲餅為2. 0吋厚。溫度(。(:)分佈 螺旋區 1 2-3 350 350 ^-350487745 5. Description of the invention (30) degrees can be detected by thermocouples separated by 1 inch. The height of the space entrance hole between the inner and outer tubes can be adjusted between 1.0 inches and 4.0 inches. The 1.0-inch-high glass ring allows visual inspection of the melt spinning line and the front of the spinneret. The spin-spinning system is performed using a spinneret assembly configured as shown in FIG. 8, which has a 30-hole 3 9 · 4-mil diameter and a spinneret having a length / diameter ratio of 3.0. Spinning is performed at a flow rate of 1.3 gpm with the following temperature distribution: 3 50. (:, Screw extruder to combined filter; 45 ° C, transfer line; and 500 ° C, spinneret. The temperature inside the Xu cooler is: 2 6 8 ° C, 1 from the front of the spinneret Inches; 2 5 2 ° C '2 inches from the front of the spinneret; and 2 2 ° C, 6 inches from the front of the spinneret. Temperature fluctuations can be ignored because the change is only 2 ° C, compared with the previous example The change observed by the Xu cooler is as high as 25 ° C. The shear rate is 15 1 / s. The maximum spinning speed reached is 1,737 mpm, fiber properties-denier / tenacity / elongation / die The numbers are: 4.2 d / 1 · 17 gpd / 57% / 7. 8 gpd. When the spinning continuity is excellent, it consists of 1, 5 0 5 mpm, 3.5 hours of yarn package and 240 The solidity of this spinning system has been proven when the coiling speed of 702 mpm is 1,4 times the in-line stretching performance. The net weight of the yarn package exceeds 20 pounds, and it is in a 6.0 inch tube. The silk cake on the tube is 2.0 inches thick. Temperature (. :) Spiral zone 1 2-3 350 350 ^ -350

螺旋銜噴絲頭組合減 夾環 接器銜接器 器 轉移線噴絲頭 . 350 350 350 350 448 500 一:: 纖維性質-旦數/韌度/伸長率/模數分別為:12. 6 d/0. 80 gpd/92%/3,8 gpd 。Spiral spinneret combined reduction clamp ring adapter adapter transfer line spinneret. 350 350 350 350 448 500 1: Fiber properties-denier / toughness / elongation / modulus are: 12. 6 d / 0. 80 gpd / 92% / 3,8 gpd.

第33頁 487745 五、發明說明(31) 實例1 3 旋紡係如實例12進行,但使用Teflon® FEP 5100氟聚合 物替代PFA· 3 40。溫度(。&lt;:)分佈為: 螺旋區 螺旋銜噴絲頭組合濾 1 2 3 夾環接器銜接器 器 轉移線噴絲頭 315 319 325 325 325 325 325 401 480 本實例所用溫度較PFA聚合物者為低,因為FEP較PFA不穩 定。剪切速率為161/sec。達成的最高旋紡速度為1,290 mpm。纖維性質-旦數/韌度/伸長率/模數分別為:7· 3 d /1· 04 gpd/36%/10 gpd 。 實例1 4 此旋紡係為測試實例13為Teflon® FEP 5100聚合物所發 展之製程之堅實性而進行。使用實例1 2及1 3相同設計之極 佳旋紡連續性係以如實例1 2之PF A聚合物之相同捲取速度 70 0 mpm獲得之3. 5 -小時筒管顯示。紗線在線外以相同之 拉伸比1· 4倍拉伸,但在較低溫度20 0 °C下為之,因為FEP 之熔點( 260 °C )較PFA之熔點( 3 0 5 °C )為低。紗線捲裝與實 例1 2之PF A 3 4 0聚合物旋紡類似。所用溫度(°C )分佈較實. 例1 3所用者抵,亦即: · -二 - 一 螺旋區 螺旋銜噴絲頭組合濾 — —7^--~~^ 銜接器 器 轉移線噴絲頭 J〇5 j1° 315 315 315 315 315 393 480Page 33 487745 V. Description of the invention (31) Example 1 3 The spinning system was performed as in Example 12, but Teflon® FEP 5100 fluoropolymer was used instead of PFA · 40. The temperature (. &Lt; :) distribution is: Spiral zone spiral armature spinneret combined filter 1 2 3 clamp ring adapter adapter adapter transfer line spinneret 315 319 325 325 325 325 325 401 480 The temperature used in this example is higher than PFA polymerization It is low because FEP is less stable than PFA. The shear rate is 161 / sec. The highest spinning speed reached was 1,290 mpm. Fiber properties-denier / toughness / elongation / modulus were: 7 · 3 d / 1 · 04 gpd / 36% / 10 gpd. Example 1 4 This spinning system was used to test the robustness of the process developed in Example 13 for the Teflon® FEP 5100 polymer. The excellent spin-spinning continuity of the same design using Examples 1 2 and 13 was obtained at a 3.5-hour bobbin display obtained at the same take-up speed of 7 0 mpm as the PFA polymer of Example 12. The yarn is stretched at the same draw ratio of 1.4 times outside the line, but at a lower temperature of 20 ° C, because the melting point of FEP (260 ° C) is higher than the melting point of PFA (3 0 5 ° C). As low. The yarn package was similar to the PF A 3 40 polymer spin spinning of Example 12. The used temperature (° C) has a more solid distribution. Example 1 3 is used, that is: · -2-a spiral area spinneret spinneret combined filter — 7 ^-~~ ^ adapter transfer line spinneret Head J〇5 j1 ° 315 315 315 315 315 315 393 480

第34頁 487745 五、發明說明(32) 剪切速率為1 63/秒。拉伸纖維性質-旦數/韌度/伸長率/模 數分別為:,12· 2 d/0. 97 gPd/45%/5. 8 gpd。 實例1 5 使用造粒子Zony 1® MP- 1 3 0 0 PTFE進行PTFE均聚物之旋 紡。均聚物之造粒型係由細ΡΤρE粉使用包含1,〇 1 3個 0.257 -叶直徑嵌入棒之陽模與2·〇吋厚之陰模之造粒機壓 實。具密度約0.36克/毫升之粉末係在壓機中於噸以上 壓力下壓實而製成具0.28吋直徑,0.50吋長度及密度1.58 克/毫升之丸粒。使用與實例相同之設備及3〇—孔喷絲頭。 所用溫度(°C )分佈為: 螺旋區 螺旋銜噴絲頭組合濾 _!_2,- 3 夾環 接器銜接器 器 轉移線噴絲頭 400 400 400 400 400 410 410 450 520 自喷絲頭正面冒出之熔融纖絲顯現半透明及閃光,顯示有 些降解。然而,纖絲卻不以連續形式自徐冷器出來,而是 成小塊及小片出來。流通速率由〇· 1 7克/分/孔改為1. 33克 /分/孔並不會產生連續纖絲。 在MP - 1 3 00丸粒自加料斗流光後,即在料斗中加入約2 Q0. 克之粉狀均聚物ΤΕ- 646 2並擠壓而成長又連續之纖二 絲。自由落下之:連續纖絲很有韌性,且可搬運或用指頭輕 拉而不斷裂。測得纖絲之旦數為349。 實例1 6Page 34 487745 V. Description of the invention (32) The shear rate is 1 63 / sec. Tensile fiber properties-denier / toughness / elongation / modulus are: 12 · 2 d / 0. 97 gPd / 45% / 5. 8 gpd. Example 1 5 Spinning of a PTFE homopolymer was performed using granulated Zony 1® MP-1 3 0 0 PTFE. The homopolymer granulation type was compacted from a fine PTPH powder using a granulator containing 1,013 0.257-leaf diameter embedded rods and a 2.0-inch thick female mold. The powder with a density of about 0.36 g / ml is compacted in a press at a pressure of more than a ton to make pellets with a diameter of 0.28 inches, a length of 0.50 inches, and a density of 1.58 g / ml. The same equipment and 30-hole spinneret were used as in the example. The temperature (° C) used is: Spiral zone spiral spinneret combined filter _! _ 2,-3 clamp ring adapter adapter transfer line spinneret 400 400 400 400 400 410 410 450 520 from the front of the spinneret The emerging molten filaments appeared translucent and shimmering, showing some degradation. However, the filaments do not come out of the Xu cooler in a continuous form, but come out in small pieces and pieces. The flow rate was changed from 0.17 g / min / hole to 1.33 g / min / hole without generating continuous filaments. After the MP-1 3 00 pellets flowed from the hopper, about 2 Q0. G of powdered homopolymer TE- 646 2 was added to the hopper and extruded to grow a continuous fiber filament. Free fall: continuous filaments are tough and can be handled or lightly pulled with your fingers without breaking. The filament count was 349. Example 1 6

第35頁 487745 五、發明說明(33) 為旋紡Teflon® PTFE ΤΓΕ - 6 472,將實例15所用擠壓機及 旋紡裝置提高至以下高溫度(°C)分佈,並先使用PEA 340 以避免PTF.E均聚物接著因在持續2. 5小時的加熱過程令停 滞而發生降解: 螺旋區 螺旋銜噴絲頭組合濾 __丄― 2 3 夾環 接器銜接器 器 轉移線噴絲頭 470 470 470 470 470 470 470 450 510 將分類為粒狀成型粉之Teflon® PTFE TE-6472壓縮粉粒, 在PFA丸粒加料出清後加入,且螺旋以14.0 rpm轉動。在 Teflon® PTFE TE-6472丸粒加入後6分鐘,發現濾器組舍 件壓力快速自204 psi上升至1,〇〇〇 psi以上,顯示 Teflon® PTFE TE-64 72已到達紐合件。將螺旋速度隨時調 整,並將噴絲頭溫度升高至55〇它以維持組合件壓力於 1,0 0 0 psi 。擠壓出的是連續透明熔融纖絲,但含有氣 泡,顯示有熱降解,並固化成白色纖絲。在2· 〇 rpm時, 測得之流通量為7, 6 gpm,而預期的為1〇· 5 gpm。即使螺 旋rpm保持於2. 0 rpm,仍發現流通量會不斷地降至〇. 4 gpm ’且連續纖絲開始斷裂成連接在長(長至48吋)與極細 纖絲之間的注頭(drips)。這些極細的纖絲視覺上與輕岭 蛛網相似到可漂浮在空氣中。測得之纖絲旦·數為 〇 · 6以下與1 8之間。此清楚證明P T F E可熔紡至極細纖絲曰 數。 、’、— 流通量降低之原因係擠壓機筒管入口之環堵塞,而有效Page 35 487745 V. Description of the invention (33) Spin spinning Teflon® PTFE ΤΓΕ-6 472, increase the extruder and spinning device used in Example 15 to the following high temperature (° C) distribution, and first use PEA 340 to Avoid degradation of the PTF.E homopolymer due to stagnation in the heating process lasting 2.5 hours: Spiral zone spiral spinneret combination filter __ 丄 ― 2 3 clamp ring adapter adapter transfer line spinneret Head 470 470 470 470 470 470 470 470 450 510 Teflon® PTFE TE-6472, which is classified as granular molding powder, is compressed, added after the PFA pellets are cleared, and the screw is rotated at 14.0 rpm. Six minutes after the addition of Teflon® PTFE TE-6472 pellets, it was found that the pressure of the filter assembly rose rapidly from 204 psi to more than 1,000 psi, indicating that Teflon® PTFE TE-64 72 had reached the joint. Adjust the spiral speed at any time and raise the spinneret temperature to 55 ° to maintain the assembly pressure at 1,000 psi. Extruded was continuous transparent molten filaments, but contained air bubbles, showed thermal degradation, and solidified into white filaments. At 2.0 rpm, the measured throughput was 7.6 gpm, while the expected flow rate was 10.5 gpm. Even though the spiral rpm was maintained at 2.0 rpm, it was found that the throughput would continue to drop to 0.4 gpm 'and the continuous filaments began to break into a tip (between 48 inches) and a very fine filament ( drips). These extremely thin filaments are visually similar to light ridge cobwebs and float in the air. The measured fibril denier number was between 0.6 and 18 and below. This clearly proves that P T F E can be melt-spun to extremely fine filaments. , ’, — The reason for the decrease in the flow is that the ring of the tube inlet of the extruder is blocked, which is effective.

第36頁 487745 五、發明說明(34) 防止氟聚合物丸粒之加入。為清除堵塞,將全部聚合物抽 出直至可看到螺旋。將p F A丸粒加入,並使用固定於0 · 5吋 棒之特製長方形板(尺寸與筒管開口相合)推入。將螺旋轉 動便會使PFA小粒自螺旋表面刮除黏著的PTFE壓縮粉末。 在堵塞清除並恢復加料後,再將PTFE壓縮粉粒加入。在 螺旋速度5· 〇 rpm及測得流通量為9· 3 gpm下,連續纖絲都 可甴全部30孔旋紡並以捲取輥在30 mpm下捲取。極佳之旋 纺連續性持續了約1 5分鐘,才再發生環堵塞,此由組合件 壓力降低可看出。此一試驗清楚證明均聚物PTFE可熔紡。 溫度(它)分佈為: 螺旋區 螺旋銜噴絲頭組合爐 1 2 3 夾環 銜接器 器 轉移線噴絲頭 420 440 480 485 485 485 485 495 500 PTFE纖維樣本 具勃性可搬運而 不脆斷且可依抗張試驗。 樣本識別 纖絲旦數 強度(克) 韌度(gpd) 自由落下 686 36.0 0.05 自由落下 1,042 71.8 0.07 30 mpm 332 14.0 0.04 實例1 7 ^5* ,二 * * 以分 類為經潤;滑 之膏擠壓樹脂之了 e f 1 on® PTFE 62 進行- 旋纺。 將粉末在50 噸壓力下類似壓縮成圓柱粒,直徑0 · 2 8 吋及長度0. 5 2 一吋及密度約1 · 6 g/cc 〇Page 36 487745 V. Description of the invention (34) Prevent the addition of fluoropolymer pellets. To clear the blockage, remove all polymer until the helix is visible. Add the p F A pellets and push in using a special rectangular plate (dimensions to the tube opening) fixed to a 0.5 inch rod. Turning the screw will cause the small particles of PFA to scrape out the sticky PTFE compressed powder from the surface of the screw. After the blockage is cleared and the feed is resumed, the PTFE compressed powder is added again. At a spiral speed of 5.0 rpm and a measured throughput of 9.3 gpm, continuous filaments can be spun in all 30 holes and taken up by a take-up roll at 30 mpm. Excellent spinning continuity lasted about 15 minutes before ring clogging occurred, which can be seen from the reduced pressure in the assembly. This test clearly demonstrates that the homopolymer PTFE can be melt-spun. The temperature (it) distribution is: Spiral zone spiral armature spinneret combined furnace 1 2 3 clamp ring adapter transfer line spinneret 420 440 480 485 485 485 485 495 500 500 PTFE fiber samples can be transported without brittleness And according to the tensile test. Sample identification fibril denier strength (g) Toughness (gpd) Free fall 686 36.0 0.05 Free fall 1,042 71.8 0.07 30 mpm 332 14.0 0.04 Example 1 7 ^ 5 *, two * * Classified as a moisturizer; smooth paste Pressed resin ef 1 on® PTFE 62-spin spinning. The powder is similarly compressed into cylindrical particles under a pressure of 50 tons, with a diameter of 0.28 inches and a length of 0.52 inches and a density of about 1.6 g / cc.

第37頁 487745 五、發明說明(35) 使用如實例1 6之相同設備及起始程序。在3. 8 rpm螺旋 速度下將Tef Ion® PTFE 62丸粒加入。開始時加入情況良 好,且測得之流通量為9 · 9 gpm,而預期者為20 gpm。將 螺旋速度提升至7.7 rpm。發現組合件壓力不停地上升, 並藉由降低螺旋速度保持於1,2 0 0 p s i,顯示加入情況良 好。環堵塞又發生致組合件壓力降低。將螺旋再提升至3 〇 rpm,堵塞即告鬆散且組合件壓力上升。在1〇 rpm時,組 合件壓力攀升至高達2,150 psi,當連續纖絲以55 mpm旋 紡時。旋紡連續性持續約5分之久,才又發生環堵塞。 實例1 8 將實例1 6及1 7紡得之纖維置於加熱之鹽浴中熱拉伸。將 纖絲切成長約1吋,並固定於兩尖端鑷子中間,並在短暫 浸入鹽浴時一邊拉伸。拉伸溫度係自3 3 0 °C至4 0 0 °C。織維 不能在320 °C下拉伸。PTFE均聚物之熔點係自325 °C至342 C ,因此纖維係在熔融狀態下拉伸。纖絲輕易地拉伸了 5 · 0倍至8 · 0倍拉伸比。纖絲由交又偏光下無較佳定向之光 亮變至在一方向之強藍色及在9 〇。方向之粉紅色,顯示沿 纖維軸有較佳分子定向。34 0 °C拉伸溫度使定向達到最高 程度。經拉伸具有測定旦數為7· 7之纖絲,其所產生的韌 度達0. 2 gpd。 實例 19 - 一: 一 使用實例9所述及圖6所示之喷絲頭旋紡Tef ι〇η® — P F A - 3 4 0 ’並比較啥絲頭不能分開加熱之習知喷絲頭總成 設計(見圖1 )之旋紡條件與噴絲頭與組合濾器熱隔開之喷Page 37 487745 V. Description of the invention (35) Use the same equipment and starting procedure as in Example 16. Tef Ion® PTFE 62 pellets were added at a spiral speed of 3.8 rpm. The addition was good at the beginning and the measured flux was 9.9 gpm, compared to the expected 20 gpm. Increase the screw speed to 7.7 rpm. It was found that the pressure of the assembly kept rising and kept at 1,200 p s i by decreasing the spiral speed, indicating that the joining condition was good. Ring clogging again causes the assembly pressure to decrease. Raise the screw to 30 rpm again, the blockage will loosen and the assembly pressure will increase. At 10 rpm, the assembly pressure climbed up to 2,150 psi when the continuous filament was spun at 55 mpm. Spinning continuity lasted about 5 minutes before ring blockage occurred again. Example 18 The fibers spun from Examples 16 and 17 were heat drawn in a heated salt bath. The filament was cut into about 1 inch, fixed in the middle of the two-point tweezers, and stretched while immersed briefly in the salt bath. The stretching temperature is from 330 ° C to 400 ° C. Weaving fabrics cannot be stretched at 320 ° C. The melting point of PTFE homopolymer is from 325 ° C to 342 C, so the fiber is drawn in the molten state. The filaments are easily stretched by a draw ratio of 5 · 0 to 8 · 0. The fibrils change from light with no better orientation under cross and polarized light to strong blue in one direction and at 90. The pink color of the direction indicates a better molecular orientation along the fiber axis. 34 0 ° C stretching temperature maximizes orientation. 2 gpd。 Tensile fiber with a measured denier of 7.7, the resulting toughness of 0.2 gpd. Example 19-One: A spinneret spinning using the spinneret described in Example 9 and shown in Fig. 6-PFA-3 4 0 'and compare the conventional spinneret assembly that cannot be heated separately. The spinning conditions of the design (see Figure 1) and the thermal separation of the spinneret and the combined filter

第38頁 487745 〜、發明說明(36) — 絲頭之旋紡條件。熱隔開在本具體例中部份係藉在組合渡 器底面與喷絲頭正面間加入轉移線而獲得。 使用相同喷絲頭系統但保持喷絲頭於相同恒定溫度下, 進行二對照組試驗。使用1 〇孔3 〇 -密爾噴絲頭。Page 38 487745 ~, Description of the Invention (36) — Spinning conditions of silk ends. The thermal separation in this example was obtained in part by adding a transfer line between the bottom of the combination ferry and the front of the spinneret. Two control groups were run using the same spinneret system but keeping the spinnerets at the same constant temperature. A 10-hole 30-mil spinneret was used.

第—對照組旋紡係藉溫度(t:)分佈保持於以下所示之 3 5 ϋ °c進行: 螺旋區 螺旋銜噴絲頭組合濾 一 1 2 3 夾環 接器銜接器 器 轉移線噴絲頭 350 350 350 350 350 350 350 350 350 將流通量提高,直至在0.178 gpm/孔發現些微熔體破 裂。在最高流通量下之剪切速率為45.7 /秒,且達到的最 高旋紡速度為58 mpm,而喷射速度為〇·26 mpm及SSF為 2 23。 第二對照組旋紡係在以下所示較高溫度分佈4 0 0 °C下進 行: 螺旋區 螺旋銜噴絲頭組合德 i 2 3 夾環 接器銜接器 器 轉移線噴絲頭 35〇 350 350 350 350 350 400 400 400 較高溫度40¾^¾:容許流通量達到〇. 37 0 gpm/孔後才發主多 體破裂。在炫Γ體破裂前之較低流通量〇· 238 gpm/孔下,最 高旋紡速度即達2 0 6 mpm。在最高流通量下及在溶體破裂 之邊緣,達到的最高旋紡速度為3 8 1 mpm,此時剪切速率The first-control group spin spinning was performed by keeping the temperature (t :) distribution at 3 5 ϋ ° c as shown below: Spiral zone spiral spinneret combination filter 1 1 2 3 clamp ring adapter adapter transfer line spray The wire head 350 350 350 350 350 350 350 350 350 increased the throughput until some micromelt rupture was found at 0.178 gpm / well. The shear rate at the highest throughput was 45.7 / sec, and the highest spinning speed reached was 58 mpm, while the jet speed was 0.26 mpm and the SSF was 223. The second control group spin spinning system was performed at a higher temperature distribution of 400 ° C as shown below: Helix area spiral armature spinneret combination De i 2 3 clamp ring adapter adapter transfer line spinneret 35〇350 350 350 350 350 400 400 400 Higher temperature 40¾ ^ ¾: Allow the flow rate to reach 0.37 gpm / well before the main multibody rupture occurs. At a lower flow rate of 0.238 gpm / hole before the rupture of the body, the maximum spinning speed is 206 mpm. At the highest throughput and at the edge of the solution rupture, the maximum spinning speed reached 3 8 1 mpm, at which time the shear rate

第%頁 487745 五、發明說明(37) 為95/秒,喷射速度為0.54 mpm及SSF為704 使用以下溫度(°C )分佈: 螺旋區 1 螺旋銜噴絲頭組合濾 夾環 接器銜接器 器 轉移線噴絲頭 325 330 335 335 335 335 335 450 500 以此溫度分饰,流通量可推進到高達1 , 1 2 5 g p m /孔,3倍 於均一 4 0 0 °C之對照組,且熔體仍未破裂。達到的最高旋 紡速度,在剪切速率2 8 9 /秒,喷射速度1,6 4 511^111及33? 1,189下,為1,956 mpm,5倍於均一 4 0 0 °C之對照組。 對照組試驗未在5 0 0 °C模擬,因為在習知喷絲頭系統中 組合濾器必須加熱到相同的5 0 0 °C溫度。組合濾器在5 0 Q °C 下時,聚合物會因在組合濾器中的長停留時間,1 0 . 1分, 而嚴重降解。在4 2 5 °C下,聚合物會在不到1 . 3分鐘内開始 降解。 實例2 0 進行以下試驗以測定熔融纖絲固化時離開喷絲頭正面之 距離。固化確定已在目視觀察到透明纖絲變不透明時發 生。此一觀察係以高強度燈光直接按照射纖絲束而更清楚 看出。透明過渡到不透明可由自由落下(藉重力)至速度高 達2 0 0 m p m時觀察到。熔融纖絲之擠壓係以有及無徐冷管 進行。在使U余冷管之情形時,係使用特殊透明玻璃徐-冷 管以便可目1:¾察;該徐冷管直徑3 . 0吋,長4 1叶。所:¾ 噴絲頭有30個36-密爾直徑孔。使用Teflon® FEP- 51 00聚Page% 487745 V. Description of the invention (37) is 95 / s, spraying speed is 0.54 mpm and SSF is 704. Use the following temperature (° C) distribution: Spiral zone 1 Spiral spinneret combined filter clamp ring adapter adapter 325 330 335 335 335 335 335 335 450 500 at this temperature, the flow rate can be advanced up to 1, 12 5 gpm / well, 3 times the control group with a uniform temperature of 400 ° C, and The melt has not yet broken. The highest spinning speed reached is 1,956 mpm at a shear rate of 2 8 9 / s, and a jet speed of 1,6 4 511 ^ 111 and 33? 1,189, which is 5 times the uniform 4 0 0 ° C. Control group. The control group test was not simulated at 500 ° C, because in conventional spinneret systems, the combined filter must be heated to the same temperature of 500 ° C. When the combined filter is at 50 Q ° C, the polymer will be severely degraded due to the long residence time in the combined filter, 10.1 minutes. At 4 2 ° C, the polymer will begin to degrade in less than 1.3 minutes. Example 20 The following test was performed to determine the distance from the front of the spinneret when the molten filament was solidified. Curing confirmed that it occurred when the transparent filaments became opaque. This observation is more clearly seen with the high-intensity light directly following the tow. The transition from transparent to opaque can be observed from free fall (by gravity) to speeds up to 200 m p m. The extrusion of the melted filaments was performed with or without a chilled tube. In the case of U waste cooling pipe, a special transparent glass Xu-cooling pipe is used so that it can be inspected with an eye 1: ¾; the Xu cooling pipe is 3.0 inches in diameter and 41 leaves long. So: ¾ The spinneret has 30 36-mil diameter holes. Using Teflon® FEP- 51 00 Poly

0:\62\62592.PTD 第40頁 487745 五、發明說明(38) 合物。 繪製於圖1 3之結果顯示空心符號的無徐冷器數據,而使 用徐冷器者則為實心符號。曲線顯示在三個固定噴絲頭溫 度:38 0 °C (三角形符號),43 0 °C (方形符號)及48 0 °C (圓形 符號)下,自由落下距離係總流通量之逐增函數。該曲線 顯示在固定溫度下,固化距離隨總流通量增加而增加。該 曲線也顯示在相同流通量下,固化距離隨噴絲頭溫度增高 而增加。再者,曲線顯示使用徐冷管時,固化距離約為不 使用徐冷管者之二倍遠。 在另一個不使用徐冷管在捲取速度200 mpm下使固化距 離由約6对增加至約1 5叶之試驗中,顯示纖絲生頭之影 響。是故,圖1 3所示固化距離代表最短固化距離。 使用以下溫度(°C )分佈: 螺旋區 螺旋銜噴# __13 夾環接器 接器 器 轉移線噴絲頭 275 285 295 315 315 315 315 380 380,430,480 實例2 1 將PTFE均聚物級,Zony 1® MP- 1 6 0 0 N,熔體加工處理並 使用圖8所示噴絲頭總成旋紡成纖維。將聚合物粉末放、_ 具0. 25吋直i轧之0. 5吋高陰模中,使用小於0. 2·5吋直-疰 棒,壓縮成約0.:1吋厚之薄圓盤。製造約2磅之這些薄圓盤 丸粒。將丸粒用手加至螺旋擠壓機中至剛好填滿螺旋之螺 紋部份以預防被壓碎及在螺旋_引起沾黏及環堵塞。使用0: \ 62 \ 62592.PTD Page 40 487745 V. Description of the invention (38) Compound. The results plotted in Fig. 13 show the data of the hollow cooler without the cooler, while those using the cooler are the solid ones. The curve shows the temperature of three fixed spinnerets: 38 0 ° C (triangular symbol), 43 0 ° C (square symbol) and 48 0 ° C (circular symbol). function. The curve shows that at a fixed temperature, the curing distance increases with the increase in total throughput. This curve also shows that at the same throughput, the curing distance increases as the spinneret temperature increases. In addition, the curve shows that the curing distance is about twice as long as when using a cold tube. In another test in which the solidification distance was increased from about 6 pairs to about 15 leaves at a take-up speed of 200 mpm without using a cold tube, the effect of fibrillation was shown. Therefore, the curing distance shown in FIG. 13 represents the shortest curing distance. Use the following temperature (° C) distribution: Spiral zone spiral nozzle # __13 Clip ring connector adapter transfer line spinneret 275 285 295 315 315 315 315 315 380 380,430,480 Example 2 1 PTFE homopolymer grade, Zony 1® MP-1600 N, melt processed and spun into fibers using a spinneret assembly as shown in FIG. Put the polymer powder in a 0.5-inch high female mold with a 0.25-inch straight roll, and use a 0.2-inch straight- 疰 rod to compress it into a thin disk with a thickness of about 0: 1 inch. . About 2 pounds of these thin disc pellets were made. Add the pellets by hand to the screw extruder until it just fills the spiral part of the spiral to prevent crushing and causing sticking and ring blockage in the spiral. use

第41頁 487745 五、發明說明(39) 以下溫度分佈。 螺旋區 , 1 2 3 夾環 螺旋銜 接器 噴絲頭 銜接器 組合濾 器 轉移線噴絲頭 380 385 390 390 390 390 390 450 500。。 在螺旋速度1 . 9 4 r pm時,使用1 0孔3 0 -密爾直徑噴絲頭之 流通量為9. 4克/分,而組合件壓力為2 38 -246 psi。使用 實例1 2所用及圖1 Ο A與1 Ο B所示之徐冷器。未遭遇環堵塞問 題。旋紡在丸粒用完即告停止。 1 0根纖絲起用手集束並送至捲取輥上,並在繞一次後, 使用吸管搶將紗線一路生頭至L e e s ο n a捲繞機。最初旋紡 速度為30 mpm,且速度次第升高到最高2 02 mpm。3纖絲之 纖絲旦數測量為:3 3,3 6及4 1。4 1旦數纖絲測得之初紡纖 維性質(旦數/韌度/斷裂伸長率/模數)為41旦/0.05 gpd / 1 · 3%/ 3· 7 gpd。Page 41 487745 V. Description of the invention (39) The following temperature distribution. Spiral area, 1 2 3 clamp ring Spiral adapter Spinneret adapter Combined filter Transfer line spinneret 380 385 390 390 390 390 390 390 450 500. . At a spiral speed of 1.94 r pm, a 10-hole 30-mil diameter spinneret was used with a throughput of 9.4 g / min and the assembly pressure was 2 38 -246 psi. The cooler used in Example 12 and shown in Figs. 10A and 10B. No ring blockage was encountered. Spinning stopped when the pellets were used up. 10 filaments are bundled by hand and sent to the take-up roller, and after winding once, the yarn is swept all the way to the Lee s n a winder using a straw. The initial spinning speed was 30 mpm, and the speed rose for the second time to a maximum of 202 mpm. The fiber denier of 3 filaments is measured as: 3 3, 3 6 and 4 1. 4 The properties of the first-spun fiber (denier / toughness / elongation at break / modulus) measured from 1 1 denier filaments are 41 deniers /0.05 gpd / 1 · 3% / 3 · 7 gpd.

Teflon® PTFE 62係使用切碎片及薄圓盤丸粒旋紡以避 免環堵塞。所用溫度(°C )分佈為:Teflon® PTFE 62 is spun with cut pieces and thin disc pellets to avoid ring clogging. The used temperature (° C) distribution is:

螺旋區 1 2 3 夾環 螺旋銜 接器 噴絲頭 銜接器 組合濾 器 轉移線噴絲頭 440 445 _ 450 450 450 450 450 450 500°C 切碎丸粒加入良:好不會堵塞。然而,丸粒圓盤終究產生環 堵塞問題。堵塞發生之前,在剪切速率自1 δ 3 /秒至6 1 4 /秒 之下,旋纺達到6 0 m ρ m。Spiral area 1 2 3 Clamp ring Spiral adapter Spinneret adapter Combined filter Transfer line spinneret 440 445 _ 450 450 450 450 450 450 500 ° C Add finely chopped pellets: it will not block. However, the pellet disc eventually caused ring clogging problems. Before clogging, the spinning rate reached 60 m ρ m at shear rates from 1 δ 3 / s to 6 1 4 / s.

487745 五、發明說明(40) 實例22 如實例21使用相同噴絲頭總成類似製備z〇nyl@ MP - 1 6 0 0 N. PTFE均聚物粉末之丸粒。在以丁溫度分佈下’ 藉由使用及不使用徐冷器旋紡,研究徐冷器之效果。通過 3 0 -密爾直徑3 0 -孔噴絲頭,在剪切速率7 2 /秒下之流通量 為8. 4克/分。 螺旋區 螺旋銜噴絲頭組合濾 1 2 3 __ 夾環接器銜接器 器 轉移線噴絲487745 V. Description of the invention (40) Example 22 The same spinneret assembly as in Example 21 was used to similarly prepare ZOnyl @ MP-16 0 0 N. PTFE homopolymer powder pellets. Under the temperature distribution, the effect of the spin cooler was studied with and without spin cooler spinning. 4 克 / 分。 Through a 30-mil diameter 30-hole spinneret, the flow rate at a shear rate of 7 2 / sec is 8.4 grams / minute. Spiral area Spiral armature spinneret combination filter 1 2 3 __ Clamp ring adapter adapter A transfer line spinneret

315 330 340 340 340 340 340 400 4〇〇 G m.徐冷器。約15 %的這些擠出纖絲在垂直自由落下踩 離5吸8对無法支撑本身重量。存續下來的纖絲,在斷裂之 前能以最高速度僅1 5 mpm旋紡。 使用4 8吋長徐冷器••全部纖絲皆係不斷自由落至地板。最 初纖絲斷裂(FFB)之旋紡速度為50 mpm,而達到的最高旋 紡速度(MSS)為480 mpm。將轉移線及噴絲頭溫度提升至 450 °C 及 5 0 0 °C,FFB 即改進至 85 mpm,而 MSS 則為 250 mpm。紗線清楚可看出厚及薄。據發現,紗線均勻度隨室 溫空氣經過徐冷器夾套引入徐冷器頂端而改良。在250 cfh(立方呎/時)時,紗線變均勻。在此旋紡條件下,MSS . 改進至404碎nF。纖維性質-旦數/韌度/斷裂伸長率/模·泰: 為 5· 8/0· 16 gpdt/l 2%/8 gpd。 一 實例2 3 本試驗使用Teflon® FEP-5100作為氟聚合物組合物,益315 330 340 340 340 340 340 340 400 4 00 G m. Xu cooler. About 15% of these extruded filaments fall freely in a vertical step, and 5 suction 8 pairs cannot support their weight. The surviving filaments can be spun at a maximum speed of only 15 mpm before breaking. Using a 48-inch long Xu cooler •• All filaments are constantly free to fall to the floor. The initial spinning speed of the filament break (FFB) was 50 mpm, and the maximum spinning speed (MSS) reached was 480 mpm. Increasing the transfer line and spinneret temperature to 450 ° C and 500 ° C, the FFB is improved to 85 mpm and the MSS is 250 mpm. The yarn is clearly visible as thick and thin. It was found that the uniformity of the yarn was improved as room temperature air was introduced into the top of the cooler through the cooler jacket. At 250 cfh (cubic feet per hour), the yarn becomes uniform. Under this spinning condition, the MSS. Improved to 404 nF. Fiber properties-denier / toughness / elongation at break / die · Thai: 5 · 8/0 · 16 gpdt / l 2% / 8 gpd. Example 2 3 This test uses Teflon® FEP-5100 as the fluoropolymer composition.

第43頁 487745 五、發明說明(4i) ' --_^ 證明熱隔離喷絲頭之優點。使用如圖8所示之噴絲-成。對照組也在相同總成進行,但各組件的溫度^ #為 同。對照k之溫度(t:)分佈為: &amp; ’、持相 螺旋區 1 2 3 夾環 螺旋銜 接器 噴絲頭 銜接器 組合爐 器 驗線 噴糸么eg 275 300 350 350 350 350 350 ----—- 350 一貝 丨、 350 275 350 400 400 400 400 400 400 400 275 350 400 400 450 450 450 450 450 螺旋區1及2之溫度分佈保持低且直至螺旋區3或夹環才、 試驗溫度。若螺旋區1及2在試驗溫度下,降解將更嚴重^ 本發明樣本之溫度分佈為:Page 43 487745 V. Description of the invention (4i) '--_ ^ Prove the advantages of the thermally isolated spinneret. A spinner as shown in FIG. 8 was used. The control group was also performed in the same assembly, but the temperature of each component was the same. The temperature (t :) distribution of the control k is: &amp; ', Phase holding spiral zone 1 2 3 Spiral ring spiral adapter Spinneret adapter Combined furnace inspection line spray nozzle eg 275 300 350 350 350 350 350- ----- 350 a bee 丨, 350 275 350 400 400 400 400 400 400 400 275 350 400 400 450 450 450 450 450 450 The temperature distribution of spiral zone 1 and 2 is kept low and until the spiral zone 3 or the clamp ring, the test temperature . If the spiral regions 1 and 2 are at the test temperature, the degradation will be more serious ^ The temperature distribution of the sample of the present invention is:

螺旋銜噴絲頭組合濾 ~垂器銜接器器 300 300 300 300 3〇〇 ^ ~Spiral spinneret combination filter ~ Vertical adapter 300 300 300 300 300 ^ ~

剪切速率為:10 gpm時86 /秒,27.2 gpm時232 /秒,42 gpm 時3 5 9 /秒,及4 5 g pm時3 8 5 /秒。如圖1 6可看出,在喷絲頭 溫度約48 0 °C時達到旋紡速度1,9〇〇 mpm ’而無任何明顯的 降解。然而,對照組卻在嗔絲頭溫度4 達到在該溫摩 下之旋纺速_名肩6〇 〇 mPm時’遭遇輕微熱降解’而在約no °c,旋紡速度時’遭遇嚴重熱降解。 ~Shear rates were: 86 / sec at 10 gpm, 232 / sec at 27.2 gpm, 3 5 9 / sec at 42 gpm, and 3 8 5 / sec at 45 gpm. As can be seen in Fig. 16, the spinning speed of 1,900 mpm 'was reached without any significant degradation at a spinneret temperature of approximately 48 ° C. However, the control group was 'sufficiently thermally degraded' when the reel head temperature 4 reached the spin spinning speed at this temperature_name shoulder 600 mPm and at about no ° c, the spinning was 'severely heated' degradation. ~

Claims (1)

487745 六、申請專利範圍 1. 一種熔紡包含高度氟化熱塑性聚合物或此等聚合物摻 混物之組合物之方法,包含下列步驟: 將包含高度氟化熱塑性聚合物或此等聚合物摻混物之 組合物熔解以形成熔融氟聚合物組合物; 將該熔融氟聚合物組合物加壓輸送至熔紡裝置之擠壓 模具;及 將該熔融氟聚合物組合物擠壓通過擠壓模具以形成纖 絲,該模具係在溫度至少4 5 0 °C ,剪切速率至少100秒M, 旋紡速度至少5 0 0米/分下。 2 .如申請專利範圍第1項之方法,進一步包含遮護纖 絲。 3 .如申請專利範圍第1項之方法,進一步含使熔融氟_聚 合物組合物在該組合物播壓通過撥壓模具之前,曝露於介 於該組合物熔解溫度與低於擠壓模具溫度之溫度間的中間 溫度。 4.如申請專利範圍第1項之方法,其中高度氟化聚合物 之熔體流指數在3 7 2 °C時為1至5 0克/ 1 0分。 5 .如申請專利範圍第1項之方法,其中氟化聚合物係四 氟乙烯與全氟烴之共聚物。 6 .如申請專利範圍第5項之方法,其中氟化聚合物係四 氟乙烯與六氟乙烯之共聚物。 7.如申請利範圍第5項之方法,其中氟化聚合物係四_ 氫乙烯與全f .k基乙烯基醚之共聚物。 —’ 8 .如申請專利範圍第7項之方法,其中全氟烷基乙烯基487745 VI. Application for Patent Scope 1. A method for melt-spinning a composition containing a highly fluorinated thermoplastic polymer or a blend of such polymers, comprising the following steps: Blending a polymer containing a highly fluorinated thermoplastic polymer or these polymers The mixed composition is melted to form a molten fluoropolymer composition; the molten fluoropolymer composition is conveyed under pressure to an extrusion die of a melt spinning device; and the molten fluoropolymer composition is extruded through an extrusion die To form filaments, the mold is at a temperature of at least 450 ° C, a shear rate of at least 100 seconds M, and a spinning speed of at least 500 m / min. 2. The method according to item 1 of the patent application scope, further comprising shielding the filaments. 3. The method according to item 1 of the patent application scope, further comprising exposing the molten fluoropolymer composition to a temperature between the melting temperature of the composition and the temperature of the extrusion die before the composition is propelled through the pressure die. Intermediate temperature. 4. The method according to item 1 of the patent application range, wherein the melt flow index of the highly fluorinated polymer is 1 to 50 g / 10 minutes at 37 2 ° C. 5. The method of claim 1 in which the fluorinated polymer is a copolymer of tetrafluoroethylene and a perfluorocarbon. 6. The method of claim 5 in which the fluorinated polymer is a copolymer of tetrafluoroethylene and hexafluoroethylene. 7. The method according to claim 5, wherein the fluorinated polymer is a copolymer of tetrahydroethylene and a full f.k-based vinyl ether. — '8. The method according to item 7 of the scope of patent application, wherein the perfluoroalkyl vinyl group 0:\62\62592.PTD 第45頁 487745 六、申請專利範圍 醚係全氟甲基乙烯基醚、全氟乙基乙烯基醚,及全氟丙基 乙烯基醚。 9.如申請專利範圍第1項之方法,其中模具之溫度為至 少 5 0 0 °C 。 1 〇.如申請專利範圍第1項之方法,其中擠壓模具係與可 含有氟聚合物組合物之裝置之其他部份熱隔離。 1 1 .如申請專利範圍第1項之方法,其中旋紡速度為至少 1 0 0 0米/分。 1 2.如申請專利範圍第1項之方法,其中剪切速率為至少 5 0 0 秒-l。 1 3.如申請專利範圍第1項之方法,進一步包含將纖維拉 伸。 1 4.如申請專利範圍第1項之方法,進一步包含鬆弛階 段。 1 5. —種熔紡包含聚四氟乙烯均聚物之組合物之方法, 包含下列步驟:將包含聚四氟乙烯均聚物之組合物熔解以 形成熔融聚四氟乙烯組合物;將該熔融聚四氟乙烯組合物 加壓輸送至熔紡裝置之擠壓模具;及將該熔融聚四氟乙烯 組合物擠壓通過擠壓模具以形成熔融纖絲。 1 6.如申請專利範圍第1 5項之方法,其中擠壓模具之溫 度為至少4 5 0 °C 。 1 7.如申利範圍第1 5項之方法,其中旋紡速度為,-少 5 0 m p m。’. 一 1 8.如申請專利範圍第1 7項之方法,其中旋紡速度為至0: \ 62 \ 62592.PTD Page 45 487745 6. Scope of patent application Ether is perfluoromethyl vinyl ether, perfluoroethyl vinyl ether, and perfluoropropyl vinyl ether. 9. The method according to item 1 of the patent application scope, wherein the temperature of the mold is at least 500 ° C. 10. The method according to item 1 of the scope of patent application, wherein the extrusion die is thermally isolated from other parts of the device which may contain the fluoropolymer composition. 1 1. The method according to item 1 of the scope of patent application, wherein the spinning speed is at least 1000 m / min. 1 2. The method according to item 1 of the patent application range, wherein the shear rate is at least 500 seconds-l. 1 3. The method of claim 1 further comprising stretching the fiber. 1 4. The method according to item 1 of the patent application scope further comprises a relaxation stage. 15. A method of melt spinning a composition comprising a polytetrafluoroethylene homopolymer, comprising the steps of: melting the composition comprising a polytetrafluoroethylene homopolymer to form a molten polytetrafluoroethylene composition; The molten polytetrafluoroethylene composition is conveyed under pressure to an extrusion die of a melt spinning device; and the molten polytetrafluoroethylene composition is extruded through an extrusion die to form molten filaments. 16. The method according to item 15 of the scope of patent application, wherein the temperature of the extrusion die is at least 450 ° C. 1 7. The method according to item 15 of the claim range, wherein the spinning speed is-less than 50 m p m. ′. 1 1 8. The method according to item 17 of the scope of patent application, wherein the spinning speed is to 0:\62\62592.PTD 第46頁 487745 t、申請專利範圍 少 2 0 0 mpm 〇 其中旋紡速度為至 進一步包含遮護纖 1 9.如申請專利範圍第1 8項之方法 少 5 0 0 m ρ πί。 2 〇 .如申請專利範圍第1 5項之方法 絲。 2 1 . —種熔紡纖維之裝置,包含: 喷絲頭總成,其包含: 過濾裝置; 噴絲頭; 加長轉移線,該轉移線係配置於該過遽裝置與該喷 絲頭之間; 該加長轉移線之加熱裝置;及 加熱該噴絲頭之加熱裝置;及 配置於該噴絲頭總成下面之加長徐冷器。 22. 如申請專利範圍第21項之裝置,其中加長徐冷器包 含配置於外管内之内管,該内管與該外管以環形空間相互 隔開。 23. 如申請專利範圍第22項之裝置,進一步包含配置在 該内管之内壁附近且在該内管長度至少部份向下延伸之網 狀管。 24. 如申請專利範圍第22項之裝置,進一步包含至少一 個配置於該_環形空間,向該外管周圍徑向延伸且附著於,該 * 内管外壁或外管内壁或兩者上之多孔板。 -- 25. 如申請專利範圍第24項之裝置,進一步包括放置於0: \ 62 \ 62592.PTD Page 46 487745 t. The scope of patent application is less than 2 0 0 mpm 〇The spin speed is up to further including shielding fiber 1 9. If the method of item 18 of the patent scope is less than 5 0 0 m ρ πί. 20. The method as described in the 15th patent application. 2 1. A device for melt-spinning fibers, including: a spinneret assembly including: a filtering device; a spinneret; an extended transfer line, the transfer line being arranged between the passing device and the spinneret A heating device for the extension transfer line; a heating device for heating the spinneret; and an elongated cooler arranged below the spinneret assembly. 22. The device according to item 21 of the patent application, wherein the elongated cooler includes an inner tube arranged in an outer tube, and the inner tube and the outer tube are separated from each other by an annular space. 23. The device according to item 22 of the scope of patent application, further comprising a mesh tube arranged near the inner wall of the inner tube and extending at least part of the length of the inner tube downward. 24. The device according to item 22 of the scope of patent application, further comprising at least one porous arranged on the annular space, extending radially around the outer tube and attached to the outer wall of the inner tube or the outer wall of the outer tube or both board. -25. If the device in the scope of patent application No. 24, further includes placing O:\62\62591 PTD 第47頁 487745 t、申請專利範圍 其中加長徐冷器進 ) 其中喷絲頭係可移 其中轉移線係可移 其中該噴絲頭之加 該至少一個多孔板上或其附近之篩網 2 6.如申請專利範圍第2 1項之裝置 一步包含測量或控制空氣流速之裝置 2 7.如申請專利範圍第2 1項之裝置 動。 2 8.如申請專利範圍第2 1項之裝置 動。 2 9.如申請專利範圍第2 1項之裝置 熱裝置係傳導加熱器,對流加熱器或感應加熱器。 3 0 ·如申請專利範圍第2 1項之裝置,其中喷絲頭具有眾 多擠壓孔,其全部配置成一圓形。 31.如申請專利範圍第21項之裝置,進一步包含收集旋 紡纖絲之裝置。O: \ 62 \ 62591 PTD Page 47 487745 t. The scope of the patent application includes the extension of the Xu cooler.) The spinneret can be moved. The transfer line can be moved. The spinneret can be added to the at least one perforated plate or The nearby screen 2 6. If the device in the scope of patent application No. 21 includes a device for measuring or controlling the air flow rate in one step 2 7. The device in the scope of patent application No. 21 operates. 2 8. If the device in scope 21 of the patent application is activated. 2 9. The device according to item 21 of the patent application. The thermal device is a conduction heater, a convection heater or an induction heater. 30. The device according to item 21 of the patent application range, wherein the spinneret has a plurality of extrusion holes, all of which are arranged in a circle. 31. The device of claim 21, further comprising a device for collecting spinning filaments. 0:\62\62592.PTD 第48頁0: \ 62 \ 62592.PTD Page 48
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