201000699 九、發明說明： 【發明所屬之技術領域】 电成本於入一種以聚對苯二甲酸乙二醇酯為主成分之聚醋樹脂 二ft 對苯二甲酸乙二醇岐/或其之低聚物與不且相 具相溶性的域旨麟'喊物f存在不 【先前技術】 性、H業中6知聚對笨二甲酸乙m纖維具有财久 素材“摩耗性等優異的性f，因此可廣泛地運用在衣服 15 20 由於該等優點’往往會導致編織物單絲產生斷 易脫落，進而嚴重影響高級服飾之外觀。據了解， 裂，小球之械，其乃成因於織物結構之纖維終端不破 切健ΐ小球具有遠高於天然纖維的繞曲抗摩性，所以纖維的 因為塵坡祕織物。普通的聚喊維織物在制過程中往往會 度高，毛輯以切* i 軸毛羽，銳纖維強 用價信ϋ 洛而影響職外觀，轉低織物的使 仏值。針對此賊問題，遂提出許多的改善方法。 酯纖維的文*^、Γ法之一為使用低聚合度的聚酉1訪絲製造低強度之聚 大巾5产地⑫，但此種方法有其缺點，亦即由於聚合物的聚合度 大巾田心也下降，因而導致紡絲及後加丄效率嚴重下降。 理另方法為將聚s旨纖維及其編織物進行加工後之表面處 但此種方法在料幼當地繁紅財-時驗果，更且會 201000699 使織物觸感損失，因而僅適用於特定用途，使用上有其缺點。 5 10 15 再另-種改善方法為在聚合物中導入易斷之酯化物結合，使在 紡絲時有高聚合度補_作業且在形成織物後再進行適當的處 理’使聚合物之?《合度下降*造成強度下降，但當聚合度達某一 程度時’熱水或蒸汽不易崎，因而無法制充分之效果。 曰本特開昭56-34727公報提到利用異苯二曱酸、己二酸、二羧 酸、二魏和多麟、多轉的聚合而得絲合的㈣旨，使聚合 度降低，進而使絲的強度下降，細此種方式對後加卫不易且效 果有限。 曰本特開昭63初18公報提到主成分聚醋加入水分解劑(如* 級之胺鹽）’使纖維含有多孔性的微囊⑽_a_e)，使聚酿具有 低強度的侧。此綠粗大粒子_絲作業不利容易斷絲且易、造 成阻塞。 為能解決上述已知方法產生的缺點及問題，本發明之發明人 極研究’發現當纖_部含有不具相雜的微粒時，經延伸後纖 維表面會產生空洞絲’進而可調整纖維物性赠到產品需求。 【發明内容】 明之目的之-為提供—種以聚對苯二甲酸乙二醇酿為主成 3Γ1樹脂組成物，其包含對苯二甲酸之乙二_旨及/或其之低 t二不具相'合性的無機或有機之微錄顆粒，於進行纺絲延伸 =。’纖維表面形成轉，觀達_絲祕狀纖維強度之目 本發明之聚醋樹脂組成物係以聚對苯二甲酸乙二_旨為主成分 20 201000699 性此組成物適用熔融紡絲法，且可製得具有良好之 對笨、1@乙造雜係她、具有適度之綺及平光效果的聚 對本一甲酸乙二醇酯系聚酯纖維。 相、’麵樹敵祕餘含有錢或械等類的不具 % 下（以下簡稱不具相容性微粒狀顆 成物之聚縮二軸及丨綠之低㈣，錢用該生 聚醋主成分之聚酷樹脂 ⑴由^ 90重1%或以上的聚對苯二曱酸乙二醇醋之聚酿成 所構成； (2) 以反應生成之聚自旨成分的總重量為基準，含有謹至5重量 /〇之平均粒彳[0.05至G.5 μηι之不具相溶性微細狀顆粒分 聚酯中； ⑶ 15 經延伸後，形成纖維，在纖維表面產生如，其空洞平均孔 仁(L)與不具相溶性微粒狀顆粒平均粒徑⑼之比^ 2 至 10 ; ' (4) 依此，製倘纖維強额未添加不具相雜微粒狀顆粒之纖 維強度關係滿足下式： 0.3 $強度下降比值$0.8 其中 含有不相溶性微粒狀顆粒之纖維強度 強度下降比值=----------------------------- 未含有不具相溶性微粒狀顆粒之纖維強度 20 201000699 本發月中’旨纖維合成可使用諸如二酸及二醇之類的化合 如對苯""酸與乙二醇反應製得聚對苯二甲酸乙二醇醋或其 低聚物。 m中了聚對笨二甲酸乙二醇酉旨為主成分之反應生成之聚 八日刀、，里為基準，内含的不具相溶性微粒狀顆粒的含量為 ®社至5重里/°’又以含量介於1至4重量％之纖維強度降低效果 更佳’此含量範圍使纖維強度降低效果佳。而當喊物中含有不 10 具相溶性微粒狀顆粒的含量低於⑽5重量％時，纖維表面形成的 空网不明顯，且纖_度下降比值無法滿足如上所述的條件及效 果，甚至由於微小粉末形成晶核，導致纖維強度會提高，此結果 ，非本發明，_朗效果；另者，當組成物付具相溶性微粒 、顆粒之含里减5%時’則由於不具相雜微粒狀顆粒累積在紡 15 絲過遽it件’造成_性惡化而使其可紡性降低且會有機台磨損 之風險。 ' =㈣之含有吻對苯二情乙二_旨為域分之細旨樹脂組 成物中，内含的不具相溶性微粒狀顆粒之平均粒徑為_至 μιη，以0.1至〇.5μηι為較佳，其中又以平均粒徑在〇 15至叫⑺ 為更，，其使纖維表面空洞_，及纖_度降低效果最佳。當 聚對苯二甲酸乙二_旨之聚_驗成物中含有不具相溶性微^ 狀顆粒的粒徑小於⑼5叩時，纖維表面空洞化效果不明顯，纖維 強度無法滿足如上所述餅及效果；另者，#_不具相溶性微 粒狀顆粒的祕大於Μ μιη ’則磁塞造成簡組件内部壓 升快，紡絲組件週期短，可紡性降低。 20 201000699 根據本發明，存在的不具相溶性微粒狀顆粒之添加 微細粉末，諸如選自包含碳_、二氧化鈦、氧化鋅械 ，化鎂、二氧化矽、硫酸鋇、滑石粉、矽藻土、高嶺土、滑石 等組群’該添加物可以單—或以多種不具相溶性 := 齡方式添加_臟W卜，存她 狀顆粒之添加物亦可為具有不相溶性之有機微細顆粒相:= 相同功效。 /、刃、具有 10 15 維= :(=:種聚酯纖維’其特徵在於她旨纖 ⑴^含9G重量％或以上聚對笨二甲酸乙二醇g旨之㈣成分所 (2) 以反應生成之聚酯成分的總重量為基準，含有〇仍 均粒则至一之不具相溶性微細狀顆粒分散: (3) 經延伸後’纖維表面產生空洞，其空 溶性微粒狀顆粒平均粒徑⑼之比值 於21 〇、不具相 ⑷依^製得的聚酉旨纖維強度與未添加不具相溶二狀 之纖維強度關係式滿足下述： 他狀顆粒 〇·3 ^強度下降比值^0.8 其中 強度下降比值=狀顆粒之纖維強度 未含有不具相溶性微粒狀顆粒之纖維強度·· 20 201000699 根據本發明之一具體實施例，該聚酯纖維為長纖維或短纖維， 較佳為具有極限黏度為0.4至0·7 dl/g之長纖維或短纖維。 根據本發明，聚酯纖維強度下降比介於0.3至0.8之間，以0.4 至0.7為較佳。當聚酯纖維強度下降比值大於0.8時，顯示強度下 降不明顯；而當下降比值小於0.3時，則聚酯纖維之紡絲加工作業 會變得困難。 根據本發明’由該聚酯樹脂組成物形成的聚酯纖維選擇地可含 有其他添加物，諸如安定劑、耐熱劑、著色劑、抗靜電劑、螢光 增白劑等。 本發明之聚酯纖維可形成圓形斷面或異型斷面之纖維，其中一 型斷面纖維意指諸如三角、多邊形、十字、中空等形式的纖維。 本發明之再又一目的係提供一種利用添加物調整聚酯纖維強度 之方法，其特徵在於聚酯樹脂成分存在不具相溶性微粒狀顆粒， 根據本發明之方法，其適用於以聚對苯二曱酸乙二醇酯、聚對苯 二甲酸丙二醇酯、聚對苯二曱酸丁二醇酯、聚丙烯、耐隆6、耐隆 66、壓克力等為主成分之聚酯纖維。 根據本發明之方法，其特徵在於聚酯樹脂成分存在〇 〇5至5重 量0/。之平均粒徑〇.〇5至0,5 μιη之不具相溶性微粒狀顆粒，其中聚 ^樹脂成分由90重量。/〇或以上聚對笨二曱酸乙二醇酯之聚酯所構 成’藉由該不具相溶性微粒狀顆粒之添加物的加入，聚酯樹脂成 分經延伸後，聚酯纖維表面產生空洞，其空洞平均孔徑(L)與不具 相溶性微粒狀顆粒平均粒徑(D)之比值(L/D)介於2至1〇。 、 。、本發明之方法中用以調整聚酯纖維之強伸度的添加物可為無 或有機之不具相溶性微粒狀顆粒，較佳為選自包含碳酸鈣、二氧 -10- 201000699 化鈦、氧化辞、氧化銘、氧化裡、-备& 石夕藻土、高嶺土狀石粉之組群。^切、_鋇、滑石粉、201000699 IX. Description of the invention: [Technical field to which the invention pertains] The cost of electricity is in a polyethylene resin containing polyethylene terephthalate as a main component, or The polymer is not compatible with the domain of the cymbal's singularity, and there is no pre-existing technology. In the H industry, it is known that it has excellent properties such as abrasion resistance. Therefore, it can be widely used in clothes 15 20. Because of these advantages, 'the yarns of the woven fabric are often broken and easily fall off, which seriously affects the appearance of high-grade clothing. It is understood that the crack, the ball of the ball, is caused by the fabric. The fiber terminal of the structure does not break the healthy ball. The ball has much higher bending resistance than the natural fiber, so the fiber is because of the dusty edge. The ordinary poly-wei fabric is often high in the process. Cut * i axis hairiness, sharp fiber strong price letter 洛 Luo and affect the appearance of the job, turn down the fabric to depreciate. For this thief problem, 遂 proposed many improvements. Ester fiber text * ^, one of the methods In order to use the poly-polymerization of the low degree of polymerization The low-strength poly towel 5 is produced in place 12, but this method has its disadvantages, that is, the polymerization degree of the polymer is also decreased due to the polymerization degree of the polymer, thereby causing a serious decrease in the spinning and post-twisting efficiency. The polysyl fiber and its woven fabric are processed on the surface of the fabric, but this method is used to test the fruit in the local red and green, and it will cost the fabric 20101699, so it is only suitable for specific use. 5 10 15 Another improvement is to introduce a breakable ester compound bond into the polymer, so that it has a high degree of polymerization during spinning, and it can be processed after forming the fabric. "The decrease in the degree of concentration* causes a decrease in strength, but when the degree of polymerization reaches a certain level, 'hot water or steam is not easy to be saturated, so it is impossible to produce sufficient effects." The polymerization of citric acid, adipic acid, dicarboxylic acid, diwei and polylin, and multi-rotation to obtain the silky (four) purpose, so that the degree of polymerization is lowered, and the strength of the silk is lowered, and the fine manner is not easy to be added later. And the effect is limited. 曰本特开昭63初18 bulletin It is mentioned that the main component polyacetate is added with a water decomposing agent (such as an amine salt of *) to make the fiber contain a porous microcapsule (10)_a_e), so that the polystyrene has a side with low strength. This green coarse particle is unfavorable for wire breaking operation. In order to solve the shortcomings and problems caused by the above known methods, the inventors of the present invention have been extremely researched to find that when the fiber portion contains particles which are not complicated, the fiber surface will be hollow after the extension. Further, the physical properties of the fiber can be adjusted to the demand of the product. [Summary of the Invention] The purpose of the invention is to provide a resin composition comprising polyethylene terephthalate, which comprises a polyethylene terephthalate. And/or its low-t2 inorganic or organic micro-recorded particles which do not have phase-matching, in the spinning extension = 'the surface of the fiber is formed, and the fiber strength of the invention is the result of the invention. The vinegar resin composition is based on polyethylene terephthalate as the main component. 20 201000699 This composition is suitable for melt spinning, and can be made to have a good pair of stupid, 1@乙造系, her moderate After the convergence of the flat light effect Acid ethylene glycol polyester fibers. The phase, the face of the enemy, contains money or machinery, etc. (hereinafter referred to as the non-compatible particulate matter of the polycondensation of the two axes and the green low (four), the money with the raw vinegar main components Polycarbonate resin (1) consists of a mixture of polyethylene terephthalic acid vinegar of 1% by weight or more; (2) based on the total weight of the components derived from the reaction, 5 weight / 〇 average particle 彳 [0.05 to G. 5 μηι non-compatible micro-fine particles in the polyester; (3) 15 after stretching, the formation of fibers, on the surface of the fiber, such as the void average pores (L) The ratio of the average particle size of the non-compatible particulate particles (9) is 2 to 10; ' (4) According to this, if the fiber strength is not added, the fiber strength relationship without the inclusion of the particulate particles satisfies the following formula: 0.3 Ratio of $0.8, which contains the ratio of fiber strength strength drop of incompatible particulate particles =------------------------------ Fiber strength of soluble particulate particles 20 201000699 This month's 'fiber synthesis can use compounds such as diacids and diols such as benzene "" The reaction of acid with ethylene glycol produces polyethylene terephthalate or its oligomer. m is a poly-day knife formed by the reaction of polyethylene glycol bismuth hydride as the main component. As a benchmark, the content of non-compatible particulate particles contained in the product is from 5% to 5 cc/°', and the fiber strength reduction effect is better at a content of 1 to 4% by weight. When the content of the non-composite particulate particles is less than (10) 5% by weight, the air network formed on the surface of the fiber is not obvious, and the ratio of the decrease in the fiber length cannot satisfy the conditions and effects as described above. Even if the fine powder forms a crystal nucleus, the fiber strength will increase, and as a result, it is not the invention, and the effect is _lang; otherwise, when the composition is provided with the compatible particles and the content of the particles is reduced by 5%, 'because there is no phase The accumulation of micro-particulate particles in the spinning 15 filaments of the 遽 遽 件 ' 造成 造成 造成 造成 造成 _ _ _ _ _ _ _ _ _ _ _ _ _ _ 性 性 性 性 性 性 ' ' ' ' ' ' ' ' ' ' ' ' ' ' ' In the resin composition, the inclusion is not compatible The average particle diameter of the granulated particles is _ to μιη, preferably 0.1 to 5.5μηι, wherein the average particle diameter is 〇15 to (7), which causes the fiber surface void _, and the fiber _ degree to decrease. The best effect is obtained. When the particle size of the non-compatible micro-particles is less than (9) 5 聚, the effect of the hollow surface of the fiber surface is not obvious, and the fiber strength cannot satisfy the above. The cake and the effect; in addition, the #_ non-compatible particulate particles are more than Μ μιη 'the magnetic plug causes the internal pressure rise of the simple assembly, the spinning assembly cycle is short, and the spinnability is reduced. 20 201000699 According to the present invention , the addition of fine powder containing non-compatible particulate particles, such as selected from the group consisting of carbon_, titanium dioxide, zinc oxide, magnesium, cerium oxide, barium sulfate, talc, diatomaceous earth, kaolin, talc, etc. 'The additive may be mono- or in a variety of non-compatible: = age-added _ dirty W Bu, the addition of her-like particles may also be incompatible organic fine particle phase: = same effect. /, blade, with 10 15 dimensions = : (=: a kind of polyester fiber 'characterized by her purpose fiber (1) ^ containing 9G wt% or more of poly(p-diethylammonium dicarboxylate g) (4) component (2) Based on the total weight of the polyester component produced by the reaction, the granules are still homogenous and then the particles are dispersed without uniformity: (3) After the extension, the voids on the surface of the fiber, the average particle size of the air-soluble particulate particles (9) The ratio of the strength of the fiber to 21 〇, which has no phase (4) and the fiber strength of the fiber without the addition of a non-coherent shape, satisfies the following: The shape of the particle 〇·3 ^ intensity decreases ^0.8 Strength reduction ratio = fiber strength of the granules does not contain fiber strength of the non-compatible particulate particles. 20 201000699 According to a specific embodiment of the present invention, the polyester fiber is a long fiber or a short fiber, preferably having an ultimate viscosity. It is a long fiber or a short fiber of 0.4 to 0.77 dl/g. According to the present invention, the polyester fiber strength reduction ratio is between 0.3 and 0.8, preferably 0.4 to 0.7. When the polyester fiber strength reduction ratio is greater than At 0.8, the display intensity is not significantly reduced; When the reduction ratio is less than 0.3, the spinning operation of the polyester fiber may become difficult. According to the present invention, the polyester fiber formed from the polyester resin composition may optionally contain other additives such as stabilizers, A heat resistant agent, a colorant, an antistatic agent, a fluorescent whitening agent, etc. The polyester fiber of the present invention can form a fiber of a circular cross section or a profiled cross section, wherein the one type of cross section fiber means a triangle, a polygon, a cross. A fiber in the form of a hollow or the like. A further object of the present invention is to provide a method for adjusting the strength of a polyester fiber by using an additive, characterized in that the polyester resin component is present in the form of non-compatible particulate particles, according to the method of the present invention. Suitable for polyethylene terephthalate, polytrimethylene terephthalate, polybutylene terephthalate, polypropylene, Nylon 6, Nylon 66, acrylic, etc. The polyester fiber of the composition. The method according to the present invention is characterized in that the polyester resin component is present in an amount of 〇〇5 to 5 wt%, and the average particle diameter of 〇.5 to 0,5 μηη is not compatible with the particulate particles. Among them The fat component is composed of 90% by weight or more of a polyester of polyethylene terephthalate. By the addition of the additive of the non-compatible particulate particles, the polyester resin component is extended and then aggregated. a void is formed on the surface of the ester fiber, and the ratio (L/D) of the average pore diameter (L) of the void to the average particle diameter (D) of the non-compatible particulate particles is between 2 and 1 〇, which is used in the method of the present invention. The additive for adjusting the elongation of the polyester fiber may be an organic or non-compatible particulate particle, preferably selected from the group consisting of calcium carbonate, dioxo-10-201000699 titanium, oxidation, oxidation, and oxidation. , -Preparation & Shi Shizao soil, kaolin-like stone powder group. ^ cut, _ 钡, talcum powder,
:康本發明之利用添加物調整聚酿纖維 造長纖維或短纖維製程。 心力幻應用於I 【實施方式】 根據本發明之-具體實施例，聚g旨樹脂 嫌Γ右成物形成_纖維在未延 現象，如圖1所示，經延伸後纖維表面 產生0.05至3·0μηι之空洞，如圖2所示。 盆纖目=之微粒狀雜之聚賴縣紡絲後延伸， 其纖維表面並無空洞產生，如圖3所示。根據 =’在以聚對苯二甲酸乙二_為域分之聚自旨組成齡有二 八相洛性微粒狀顆粒佔主成分〇〇5至5重量％，當其中含有不且 才目溶性微粒狀顆粒之含量低於⑽s%時，纖維表时洞不明顯， 圖4所示，且纖維強度下降比值亦無法滿足本發明之效果。.，. 再者’根據本發明之方法製成的聚醋經炫融紡絲後延伸，由於 所含林f她性微粒狀雛，使纖維產生财空洞效果(如 f 2所不）’經延伸後的纖維表面產生空洞，其空 2=粒平均粒徑⑼之比值(L增於2至丨。，藉由纖維表(J 產土玉洞大小，可纖_度伸度，因此，依此製造方法 ^有不具相雜微粒狀難之聚§|纖維強度與未含有不具相溶 十微粒狀顆粒m㈣度比值下降日摘，使纖_物單纖斷 201000699 裂時容易脫落。 、本毛月藉由下述實施例更詳盡地說明，該實施例不意欲 以任何=式限制本發明範圍，雖然設於大範圍的數字範圍 和參數把圍是近似值，但儘可能精碟地紀錄在特定的實施 5 例中的數值。 實施例 本發明的各實施例及比較例中製得的產物之物理性質依 照下列方法進行測定及評估： 10 1.極限黏度(IV) 根據ASTMD2857規範測定方法，將聚酯溶於鄰_氯酚，在恆溫 25 C，以Ubbeiohde黏度§十測定Γν值，單位為(dl/g)。 2. 粒徑分析 15 以HORIBA股份有限公司製造之CAPA-300儀器，測量分布於 聚酉旨中之不具相溶性微粒狀顆粒的分佈狀況。 3. 強伸度之檢測 以自動拉伸試驗儀(STATIMATM)測量纖維之強度與伸度性質。 20 4. 表面空洞 以電子顯微鏡觀察及量測纖維表面之孔洞大小。 5.紡絲性 -12- 201000699 佳： 斷絲次數3次以下/天 可： 斷絲次數4〜5次/天 差： _絲次數6次以上/天 實施例1 擾1均42句 WPAW9·01 “乙二_，先行 50 kg聚酯預‘二吊f :: 〇.35 kg/mm的添加速率’置入内有 頂t物的120公升之不鏽鋼反應罐中， 於245 C下進仃 10 20 於此12〇八林率到達後，將原有之5〇 kg之聚醋預聚物留 =二 不鏽鋼反應罐中，其餘則移入另-1〇〇公升之聚 二添力:lkg(含量2重量%)碳酸細驗細粉末(顆粒平均 … ㈣’而後以25mmHg/min的速度緩慢抽空減壓至 mmHg並同時升溫至意c，俟極限黏度w提高至咖心g後〆 卻切粒製得含林相溶微粒狀無_粒之料苯二甲酸乙二醇酉: 之聚醋產物；該聚g旨經熔融紡絲製程，_製程條件如下：纺^ 溫度為290。〇，孔徑〇.23mm及孔數36孔之口金紡絲，纺絲速度 3000m/min ;之後，再於溫度9(Tc下進行延伸，延伸倍率18 ; ^ 著’經定型溫度140°C定型得到75d/36f之聚g旨纖維。 對上述製得的聚酯纖維進行各項物理性質之測盆姓 果列於表1。 實施例2 重複與實施例1的製程及條件進行反應，但調整碳酸舞 無機微細粉末之顆粒平均粒徑為0.105 μπι，最後製得極限黏度為 -13- 201000699 乙一醇酯聚g旨產物。重複與實施例1相同 ’得到75d/36f之聚酯纖維。: Kang Ben's invention utilizes additives to adjust the process of growing fiber or staple fiber. In order to solve the problem, according to the embodiment of the present invention, the polyg is intended to form a resin, and the fiber is not elongated. As shown in FIG. 1, the surface of the fiber is 0.05 to 3 after stretching. · 0μηι hollow, as shown in Figure 2. After the spinning of the granules of the granules of the granules, the granules of the granules of the granules have no voids, as shown in Fig. 3. According to the =' concentration in the polyethylene terephthalate group, the octagonal granular particles occupy 5 to 5 wt% of the main component, and when it contains When the content of the particulate particles is less than (10) s%, the time at which the fibers are formed is not conspicuous, as shown in Fig. 4, and the ratio of the decrease in the strength of the fibers does not satisfy the effect of the present invention. Furthermore, 'the vinegar made according to the method of the present invention is stretched after being spun and spun, and because of the inclusion of her granules, the fiber has a void effect (such as f 2). The surface of the fiber after the extension has a void, and the ratio of the empty 2 = average particle diameter (9) (L is increased from 2 to 丨., by the fiber table (J is the size of the jade hole, the fiber can be stretched, therefore, The manufacturing method has the advantage that the fiber strength is not mixed with the particles, and the fiber strength does not contain the undissolved ten-particle particles, and the m (four) degree ratio decreases, so that the fiber is easily peeled off when the fiber is broken. The present invention is explained in more detail by the following examples, which are not intended to limit the scope of the invention in any form, although numerical ranges and parameter ranges are approximated in a wide range, but are recorded as specific as possible. The numerical values in the 5 examples were carried out.EXAMPLES The physical properties of the products obtained in the respective examples and comparative examples of the present invention were measured and evaluated according to the following methods: 10 1. Ultimate viscosity (IV) According to the ASTM D2857 specification, The polyester is soluble in o-chlorophenol at a constant temperature of 25 C. Ubbeiohde viscosity § Measured Γν value in units of (dl/g) 2. Particle size analysis 15 Measure the distribution of non-compatible particulate particles distributed in the group by the CAPA-300 instrument manufactured by HORIBA Co., Ltd. Condition 3. Detection of tensile strength The strength and elongation properties of the fiber were measured by an automatic tensile tester (STATIMATM). 20 4. Surface voids The size of the pores on the surface of the fiber was observed and measured by electron microscopy. -12- 201000699 Good: The number of broken wires is less than 3 times/day: The number of broken wires is 4~5 times/day difference: _The number of wire times is more than 6 times/day Example 1 Disturbing 1 is 42 sentences WPAW9·01 “乙二_ , first 50 kg polyester pre-two suspension f :: 添加.35 kg / mm addition rate 'put into the 120 liter stainless steel reaction tank with top t, enter 仃 10 20 at 245 C After the arrival of the 〇八林 rate, the original 5 〇kg of the poly acetal prepolymer is left in the second stainless steel reaction tank, and the rest is transferred to another 1-1 liter of the second additive: lkg (content 2% by weight) Carbonic acid fine powder (particle average... (4)' and then slowly evacuated to mmHg at a rate of 25mmHg/min and simultaneously heated to Meaning c, 俟 ultimate viscosity w is increased to the core of the coffee g, but the granules are obtained by the granules of the phthalocyanine: the polyacetate product; the polyg is melt-spun Process, _ process conditions are as follows: spinning ^ temperature is 290. 〇, aperture 〇.23mm and the number of holes 36 holes of gold spinning, spinning speed 3000m / min; then, at temperature 9 (Tc extension, extension ratio 18 ; ^ 'Fixed at a temperature of 140 ° C to obtain a 75d / 36f poly-g fiber. The physical properties of the polyester fibers obtained above were measured in Table 1. Example 2 The reaction was repeated with the process and conditions of Example 1, except that the average particle diameter of the inorganic fine powder of the carbonated dance was adjusted to 0.105 μm, and finally the final viscosity was -13-201000699. The same procedure as in Example 1 was repeated to obtain a 75d/36f polyester fiber.
酿纖維進行各項物理性質之測試，其結 貫施例J 機條件進行反應，但調整碳酸妈無 10 0.64之聚阿，最後製得極限黏度為 ΛΑ ^ ^ ^ _甲夂乙一知酯聚酯產物。重複與實施例1相同 、、、、、ν、製程及條件，得到75d/36f之聚酯纖維。 里對上述製得的聚_維進行各項物理性質之測試，其 果列於表1。 〃 比較例 15 二二 甲酸(TPA)，19.购之乙二醇_，先行 ^成均勻的漿液，於常壓下以a35 kg/min的添加速率，置入内有 kg «預聚物的⑽公升之不鑛鋼反應罐中 20 ο.64之聚對苯二曱酸 的紡絲製程及條件 對上述製得的聚 果列於表1。 ^ ^ ^ ^ - kg ； ' 。升之不鏽鋼反應罐中’其餘則移入另-100公升之聚 合=罐，聚財不添加不具相溶性微粒狀顆粒，而後以Μ 緩慢抽空減駐1 mmHg紳_至赋， 1的^*至__後冷卻切粒製得聚®旨；重複實施例 •14· 201000699 比較例 重複與實施例！的製程，但調整碳酸舞 均粒控為讀哗，製得《產物，經_製^聚之顆粒平 項物理性質之測試，其結果列於表丨。孓目曰纖維及進行各 比較例 糾重複一础1的製程’但調整碳酸_無機微纟吟龙之 均粒控為G.7 μιη ’製得聚g旨產物，經紡絲製得聚^之顆粒平 項物理性質之測試，其結果列於表丨。 s、、裁、、隹及進行各 實施例 平均粒徑 比值 — (μιη) (L/D)max 施例1 0.315 —_?_ 實施例2 1 — 0.105 實施例3 0.490 10 比較例1 ___ 一一·« _^較例2 0.04 1.5 例3 0.7 紡絲性The brewed fiber was tested for various physical properties, and the reaction was carried out under the condition of J, but the adjustment of the carbonated mother did not have 10 0.64 of polyaluminum, and finally the ultimate viscosity was ΛΑ ^ ^ ^ _ 夂 一 一 知 ester polyester product. The same,,,,, ν, process and conditions as in Example 1 were repeated to obtain a 75d/36f polyester fiber. The physical properties of the above-prepared poly-dimensional were tested, and the results are shown in Table 1. 〃 Comparative Example 15 Dicarboxylic acid (TPA), 19. Ethylene glycol purchased _, first into a uniform slurry, at a rate of a35 kg / min at atmospheric pressure, placed with kg «prepolymer (10) Spinning process and conditions of 20 ο. 64 polyterephthalic acid in a liter of non-mineral steel reaction tank The above-obtained fruit is listed in Table 1. ^ ^ ^ ^ - kg ; ' . In the stainless steel reaction tank, the rest is transferred to another 100 liters of polymerization = tank, and the accumulation of non-compatible particulate particles is not added, and then slowly evacuated by 1 HHg 绅 _ to Fu, 1 ^* to _ _ post-cooling pellets to obtain a polymer®; repeated examples • 14· 201000699 Comparative examples are repeated with examples! The process, but the adjustment of the carbonic acid dance is controlled by the granules, and the "products, the physical properties of the granules of the granules are measured. The results are shown in Table 丨.孓 曰 曰 及 及 及 及 及 及 及 及 及 及 及 及 及 及 及 及 及 及 ' ' ' ' ' ' ' ' ' ' ' ' ' ' ' ' ' ' ' ' ' ' ' ' ' ' ' ' ' ' ' ' The test of the physical properties of the particle flat terms is shown in Table 丨. s, 裁, 隹, and carry out the average particle size ratio of each example - (μιη) (L / D) max Example 1 0.315 - _?_ Example 2 1 - 0.105 Example 3 0.490 10 Comparative Example 1 ___一·« _^ Comparative Example 2 0.04 1.5 Case 3 0.7 Spinning
纖維強度 (g/d) 強度下降比Fiber strength (g/d) strength reduction ratio
不可纺 由表1所列之結果顯示，本發明之含有平均粒徑在01至〇5 _ 的不具相溶性微粒狀顆粒之聚顆(實施例！至3)纖維強度與不含有 不具相溶性微粒狀顆粒之聚酯纖維之強度相較下，本發明之纖維 15. 15 201000699 強度降低比值效果明顯。 而含有平均粒徑小於0.1 μιη(比較例2)或大於〇 5 μπι(比較例3) 的不具相溶性微粒狀顆粒之聚酯纖維強度與不含有不具相溶性微 粒狀顆粒之聚g旨纖維之強度她下纖維強麟低比值效果不明 顯0 實施例4 fit_ 1㈣程’但調整碳祕無機微細粉末之重量比為 5重量％，其結果列於表2。 10 實施例5 f複貫施例1的製程’但調整碳賴無機微細粉末之重量比為 0.05重量％ ’其結果列於表2。 15 比鮫例4 $複實施例1的製程’但調整碳祕無機微細粉末之重量比為 6重量％，其結果列於表2。 比鉸例5 20 1 程’但調整碳祕無機微細粉末之重量比為 0.01重量％，其結果列於表2。 __^ 2 實施例 重量比(％) 纺絲桃 〜丨.一 維強度(g/d) 伸度(％) 強度下降比 * 16 - 201000699 實施例1 2 佳 ------- 2.5 ~~—' — 18 1~---- 50% 實施例4 5 可 —.丨"— 1.98 14 39 6% 實施例5 0.05 佳 - 4.0 28 8〇〇/λ 比較例4 6 差 1.4 10 97% 比較例5 0.01 佳 5.1 32 -----—一 二 / /0 102% 由表2所列之結果顯示，本發明之含有〇 〇5至5重量〇/〇的不具 才曰目溶性微粒狀顆粒之聚酿(實施例卜4、5)對照於與含有大於/重 量％(比較例4)或者低於〇.05重量％(比較例5)的不具相溶性微 顆粒之聚_維強度她下，本發明之纖軸度降低效果較明顯。 實施例6 M 42.38kg2_:m(TPA)，19〇lkg^KEG)，^ 10 擾成均勻的漿液，於常壓下以G.35 kg/min的添加速率，置入内有 5〇 kg聚酯預聚物的no公升之不鏽鋼反應罐中，於245它下進行 醋化反應，當轉化率到達98%後，將原有之5〇 kg之聚§|預聚物留 於此120公升之不鏽鋼反應罐中，其餘則移入另一 1〇〇公升之聚 合，應罐，添加lkg(含量2重量％)碳酸約無機微細粉末(顆粒平均 粒徑0.315 μπι)，而後以25 mmHg/min的速度緩慢抽空減壓至j mmHg並同時升溫至28(rc，俟極限黏度w提高至〇 64_後冷 卻切粒製得含林相賴粒狀無機雌之料苯二情乙二醇^ 之聚醋產物；再進行以熔融紡絲，條件為：_溫度29叱，孔^ 〇.23mm及孔數36孔之口金紡絲，紡絲速度45〇〇 m/min，並於^ 伸溫度9(TC下進行延伸，延伸倍率3 ();經定型溫度14叱定型得 -17- 201000699 ^ 75·之全延伸性纖維，進行物理性質檢測，其 表3。 實施例7 : 將42.3叫之對苯二甲酸⑽），19 〇1岭之乙二醇㈣，先行 均勻的漿液’於常壓下以0.35 kg/min的添加速率，置入内有 50 kg聚醋預聚物的12〇公升之不鏽鋼反應罐中，於2衫 ，化率到達98%後，將原有之5Q kg之聚醋預聚物留 於此20 A升之不鏽鋼反應罐中，其餘則移入另—刚公升之 15 口反應罐’添加lkg(含量2重量％)碳酸妈無機微細粉末(顆粒平均 粒么0.3,15 μηι)，而後以25随~_的速度緩慢抽空減麗至1 mmHg並同時升溫至28〇。〇 ’俟極限黏度w提高至ο·%卿後* 卻切粒製得含有不相溶微粒狀無機顆粒之聚對苯二甲酸乙二醇gI 之聚醋產物，·再進行熔融紡絲，經延伸溫度、定型、切棉製程，曰 得到1.6D*38rnm之短纖維。進行物理性質之檢測，其結果列於表 -- 表3 實施例 農量比(0/〇) 紡絲性 纖維強度(g/d) 伸度(％) — 強度下降!；(· 實施例6 2 佳一 2.4 ~------ 18 '----- 48% 實施例7 ----- 2 ------- 佳 2.0 18 40% 維之有不具相溶性微粒一 -18- 20 201000699 本發明之效杲 依^明方法製狀雜，具有良好之_性、延伸 ，、_融_魏伸，由㈣軸含林具她性之益機' 或有機粒子微粒狀顆粒，使纖維表面產生具有空洞效果，且右^ 度，使纖維織物單纖斷裂時容易脫落。應用;： 具有良好表觀及深染效果。 '切 10 ^上具體實_翻峨日脉發狀技納容補點，使 ^技術領域之通常知識者能瞭解本案之目的及内容並據以實施 非用以揭限本發明’故在未偏縣伽之内容 或修掷的發明’仍應涵蓋在本發鴨如。/ &成的改良 15 洞 【圖式簡單說明】 圖1為含不相溶微粒狀顆粒之未延伸前絲條表面，表面無空 微粒狀顆粒之延伸後纖維表面孔洞分佈 纖維 20 經延伸後產生空洞 圖3為不含有不相溶微粒狀顆粒之延伸絲表面， 僅有極^3空=1%不具相容性微粒狀顆粒之纖維 延伸絲表面， 表面無空洞 【主要元件符號說明】 •19-Non-spun, as shown by the results in Table 1, shows that the particles of the present invention having a non-compatible particulate particle having an average particle diameter of from 01 to 〇5 _ (Example! to 3) have a fiber strength and do not contain non-compatible particles. The strength of the polyester fiber of the granules is relatively lower than that of the fiber of the present invention. 15.15 201000699 The effect of the strength reduction ratio is remarkable. And the strength of the polyester fiber containing the non-compatible particulate particles having an average particle diameter of less than 0.1 μm (Comparative Example 2) or greater than 〇5 μm (Comparative Example 3) and the polyg-containing fiber not containing the non-compatible particulate particles The strength of her lower fiber strength and low ratio effect is not obvious. 0 Example 4 fit_1 (four) course 'but the weight ratio of the carbon secret inorganic fine powder is adjusted to 5% by weight, and the results are shown in Table 2. 10 Example 5 f The process of the first embodiment was repeated, but the weight ratio of the carbon-base inorganic fine powder was adjusted to 0.05% by weight. The results are shown in Table 2. 15 Comparative Example 4 The process of the above Example 1 was carried out, but the weight ratio of the carbonaceous inorganic fine powder was adjusted to 6% by weight, and the results are shown in Table 2. The weight ratio of the carbonaceous inorganic fine powder was adjusted to 0.01% by weight in the case of the hinge example 5, and the results are shown in Table 2. __^ 2 Example weight ratio (%) Spinning peach ~ 一. One-dimensional strength (g / d) Elongation (%) Strength reduction ratio * 16 - 201000699 Example 1 2 Good ------- 2.5 ~ ~—' — 18 1~---- 50% Example 4 5 can be..丨"- 1.98 14 39 6% Example 5 0.05 Good - 4.0 28 8〇〇/λ Comparative Example 4 6 Difference 1.4 10 97 % Comparative Example 5 0.01 Good 5.1 32 ------1-2/ /0 102% The results listed in Table 2 show that the present invention contains 〇〇5 to 5 weight 〇/〇 of non-markable soluble particles. The granules of the granules (Examples 4 and 5) were compared to the poly-dimensional strength of the non-compatible microparticles containing more than /% by weight (Comparative Example 4) or less than 5% by weight (Comparative Example 5). Under her, the effect of reducing the fiber axis of the present invention is more obvious. Example 6 M 42.38kg2_:m(TPA), 19〇lkg^KEG), ^ 10 Disturbed into a uniform slurry, at a rate of G.35 kg/min at normal pressure, 5 公斤 kg was placed inside. In the no-liter stainless steel reaction tank of the ester prepolymer, the vinegarization reaction is carried out under 245. When the conversion rate reaches 98%, the original 5 〇kg of the §|prepolymer is left at 120 liters. In the stainless steel reaction tank, the rest is transferred to another 1 liter liter of polymerization, and the tank should be added with lkg (content 2% by weight) carbonic acid about inorganic fine powder (particle average particle diameter 0.315 μπι), and then at a speed of 25 mmHg/min. Slowly evacuate and depressurize to j mmHg and simultaneously heat up to 28 (rc, 俟 ultimate viscosity w is increased to 〇64_, and then the granules are obtained by cooling the granules to obtain the polylactic acid product of the granule-like inorganic female material benzene diethylene glycol And further melt-spinning, the conditions are: _ temperature 29 叱, hole ^ 〇. 23 mm and the number of holes 36 holes of gold spinning, spinning speed 45 〇〇 m / min, and at the temperature of 9 (TC) The extension was carried out, the stretching ratio was 3 (); the fully extended fiber of -17-201000699 ^ 75· was set at a setting temperature of 14 ,, and the physical property was examined, and Table 3 was performed. : 42.3 is called terephthalic acid (10)), 19 〇1 linger of ethylene glycol (four), the first uniform slurry 'at a normal pressure at a rate of 0.35 kg / min, placed in a 50 kg poly lactic acid prepolymerization In the 12-liter liter stainless steel reaction tank of the material, after the rate of 98% was reached in the 2 shirts, the original 5Q kg of the polyester prepolymer was left in the 20 A-liter stainless steel reaction tank, and the rest was transferred to another - 15 liters of reaction tank just added lkg (content 2% by weight) of carbonated inorganic fine powder (particle average particle 0.3, 15 μηι), and then slowly evacuated to 1 mmHg at a rate of 25 with ~_ and simultaneously The temperature is raised to 28 〇. 〇 '俟 ultimate viscosity w is increased to ο·% * 却 却 却 却 却 制 制 制 制 制 制 制 制 制 制 含有 含有 含有 含有 含有 含有 含有 含有 含有 含有 含有 含有 含有 含有 含有 含有 含有 含有 含有 含有Melt spinning, elongation temperature, shaping, and cotton cutting process, 曰 曰 曰 曰 曰 曰 曰 1.6 1.6 1.6 1.6 1.6 1.6 1.6 1.6 1.6 1.6 1.6 1.6 1.6 1.6 1.6 1.6 1.6 1.6 1.6 1.6 1.6 1.6 1.6 1.6 1.6 1.6 1.6 1.6 1.6 1.6 1.6 1.6 1.6 1.6 1.6 1.6 1.6 1.6 1.6 1.6 1.6 1.6 1.6 Silk fiber strength (g/d) Elongation (%) - Strength drop!; (· Example 6 2 Jiayi 2.4 ~------ 18 '----- 48% Example 7 ----- 2 ------- Good 2.0 18 40% Dimensional with non-compatible particles -18- 20 201000699 The effect of the invention is based on the method of the Ming method, with good _ sex, Extension, _ _ _ Wei extension, by (four) axis containing forest with her sexual machine ' or organic particle particles, so that the surface of the fiber has a hollow effect, and right ^, so that the fiber fabric single fiber breaks easily fall off . Application;: Good appearance and deep dyeing effect. 'Cut 10 ^ on the actual _ 峨 峨 发 发 发 发 发 发 , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , The invention of the partial gamma or the invention of the throwing 'should still be covered in this hair duck. / & improved 15 holes [schematic description] Figure 1 is the surface of the unstretched front strip containing immiscible particulate particles. After the surface is free of particulate particles, the fiber surface pore distribution fiber 20 is extended. Cavity is generated. Figure 3 shows the surface of the extended filament which does not contain immiscible particulate particles. There is only a fiber surface of the fiber that is not compatible with the particulate particles, and there is no void on the surface. [Main component symbol description] 19-