TWI281925B - Shaped articles with improved stability - Google Patents
Shaped articles with improved stability Download PDFInfo
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- TWI281925B TWI281925B TW92116124A TW92116124A TWI281925B TW I281925 B TWI281925 B TW I281925B TW 92116124 A TW92116124 A TW 92116124A TW 92116124 A TW92116124 A TW 92116124A TW I281925 B TWI281925 B TW I281925B
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- Prior art keywords
- yarn
- ester
- molded article
- patent application
- poly
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- 150000002148 esters Chemical class 0.000 claims abstract description 38
- 239000000835 fiber Substances 0.000 claims description 85
- KLDXJTOLSGUMSJ-JGWLITMVSA-N Isosorbide Chemical compound O[C@@H]1CO[C@@H]2[C@@H](O)CO[C@@H]21 KLDXJTOLSGUMSJ-JGWLITMVSA-N 0.000 claims description 30
- -1 dicarboxylic acid ester Chemical class 0.000 claims description 29
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- 238000009987 spinning Methods 0.000 claims description 25
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- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 21
- 150000002009 diols Chemical class 0.000 claims description 21
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 claims description 20
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- OFOBLEOULBTSOW-UHFFFAOYSA-N Malonic acid Chemical compound OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 claims description 9
- 239000000178 monomer Substances 0.000 claims description 9
- YPFDHNVEDLHUCE-UHFFFAOYSA-N propane-1,3-diol Chemical compound OCCCO YPFDHNVEDLHUCE-UHFFFAOYSA-N 0.000 claims description 9
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- CYIDZMCFTVVTJO-UHFFFAOYSA-N pyromellitic acid Chemical compound OC(=O)C1=CC(C(O)=O)=C(C(O)=O)C=C1C(O)=O CYIDZMCFTVVTJO-UHFFFAOYSA-N 0.000 description 4
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- 238000004458 analytical method Methods 0.000 description 3
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- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 description 3
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- 239000007858 starting material Substances 0.000 description 3
- 229910052718 tin Inorganic materials 0.000 description 3
- DTQVDTLACAAQTR-DYCDLGHISA-N trifluoroacetic acid-d1 Chemical compound [2H]OC(=O)C(F)(F)F DTQVDTLACAAQTR-DYCDLGHISA-N 0.000 description 3
- 239000011701 zinc Substances 0.000 description 3
- JNYAEWCLZODPBN-JGWLITMVSA-N (2r,3r,4s)-2-[(1r)-1,2-dihydroxyethyl]oxolane-3,4-diol Chemical compound OC[C@@H](O)[C@H]1OC[C@H](O)[C@H]1O JNYAEWCLZODPBN-JGWLITMVSA-N 0.000 description 2
- AZQWKYJCGOJGHM-UHFFFAOYSA-N 1,4-benzoquinone Chemical compound O=C1C=CC(=O)C=C1 AZQWKYJCGOJGHM-UHFFFAOYSA-N 0.000 description 2
- RZVAJINKPMORJF-UHFFFAOYSA-N Acetaminophen Chemical compound CC(=O)NC1=CC=C(O)C=C1 RZVAJINKPMORJF-UHFFFAOYSA-N 0.000 description 2
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- 206010036790 Productive cough Diseases 0.000 description 2
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- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 2
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- QMKYBPDZANOJGF-UHFFFAOYSA-N benzene-1,3,5-tricarboxylic acid Chemical compound OC(=O)C1=CC(C(O)=O)=CC(C(O)=O)=C1 QMKYBPDZANOJGF-UHFFFAOYSA-N 0.000 description 2
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Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Textile Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Polymers & Plastics (AREA)
- General Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Mechanical Engineering (AREA)
- Materials Engineering (AREA)
- Artificial Filaments (AREA)
- Polyesters Or Polycarbonates (AREA)
- Yarns And Mechanical Finishing Of Yarns Or Ropes (AREA)
- Nonwoven Fabrics (AREA)
- Woven Fabrics (AREA)
- Carpets (AREA)
- Manufacture Of Macromolecular Shaped Articles (AREA)
- Macromolecular Compounds Obtained By Forming Nitrogen-Containing Linkages In General (AREA)
- Polymers With Sulfur, Phosphorus Or Metals In The Main Chain (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Description
1281925 玖、發明說明： 申請案 本申請案係20〇2年12月19曰提出申請，現在待審之美國 I請案號60/434,599之臨時中請案的非臨時中請案。美國國 豕申請案係於2003年6月1〇日提出，現正待審中。 【發明所屬之技術領域】 本發明針對成型物件，特別指向有增加穩定性含聚 土-共-二脫水糖酯）二羧酸酯或聚（伸烷基-共-二脫水-二 酸酯）之纖維。 夂 【先前技術】 、c—neau等人在美國專利6〇63464號内已揭示混入二 脫Λ糖Λ類諸如1，4_: 3,6_二脫水山梨糖醇（後文以其俗稱 :_s〇rbide)稱之)能大幅提升對酞酸酯聚酯諸 =)亦稱聚_丙二醇醋)，後文稱作抓。 价之相，低的玻璃態化溫度(Tg)(〜45_5(rc )能導致聚合 物於咼溫儲存時些微膠 的炎熱氣候中舍性夕& ”中一例可由有時在熱帶國家 。此外、、° = r維捲線筒内證實。Tg提高降低黏性 此儲存丨起錢環境下料時紡絲纖㈣穩定。類 此姑存丨月況下的部分拉 以致纖維收縮、丹尸心易“曰曰作用，形成稠厚相 不良變化。但，匕刹（担細度）改及儲存後物理性質 二燒醋的醋基轉移作=與對酉太酸之醋化作用或與對酉太酸 醇類諸如乙：=13用第二録之反應，且與初级二 ，丙一®予的反應相比較慢。於是此易導
S603S I281925 致異山梨醇之不充分攙併。用傳統的縮聚作用，此較低活 哇忐導致最後聚酯有較低分子量，由於未反應之異山梨醇 不利於其後聚合作用。 美國案號10/1721丨2内Adelman等曾敘述製備聚（1，3_伸丙 基、共-異山梨醇）對酞酸酯的製程改良，後文簡稱3GIT。但 山木S子之第一羥基與二元酸或其二烷基酯的反應性比 ’3丙一 g予第一經基之相當反應性大為低落。此反應性的差 二有卉夕衫％，其中之一為加長固相聚合步驟所需時間， 取後程序内聚合物的特性黏度上升到良好紡絲性質之約 1·1 dl/g 〇 要求製備攙混二脫水糖醇的聚g旨如3GIT，具低色度及^ 斯之45_5(rcTg較高的Tg，最重要兼具低色度與較高& 此寺改良性質有助於此類聚酯使用於許多商業機會之成受 物件上/包括飲料瓶，膜或片，纖維，單長纖及光學物科 (例如隱形鏡片或數位多用途圖片等）。 ^別要求提高含攙混有二脫水糖醇之聚酯的成型物件之 =，尤其纖維與紗，如部分定向紗、紡絲拉伸紗與散 ^連_不斷長纖紗，及短纖料容許使用高速紡絲過程而 :::屬紗之性質。更要求，此等紗線能用於在較緩 衣之、v線所用相同或類似條件下製備如 物與地毯等產品。 ，又开"y織 本為明提供包含具有此種改良穩定性的經 酸醋聚合物的成型物件。 “文良之-竣 86038 1281925 【發明内容】 曼idj既述 本發明包括一種成型物件，其包含聚（伸烧基-共-二脫水 糠醋)二賴聚(伸炫基-共-二脫水-二讓）。物件伟一 纖維、紗線、膜、非織诰式伊年日此^ ^ k次杈塑物件。纖維為短紗或長 及一均聚物或多長纖。纖唯呈 厲、、隹壬部分疋向紗、紡絲拉伸 纺絲變形紗。 ’ 本發明又包含用此等纖維所製之織物或地毯。 羊細說明— 本發明包含具提局穩定性夕$ 士 k心注之王成型物件型式的經酯改良 的二羧酸酯聚合物。詳t之，甘取人^ ^ 干口之，其聚合物為其中有二脫水糖
醇酯攙併的聚酯。較佳俜枣「, M p # L 平乂 t V'來[(伸烷基-共-二脫水糖酯）對酞 酸醋]或聚（伸烧基-共-二脫水-對肽酸醋）。 1，4: 3,6-二脫水山梨糖醇、一種二醇單體，文内稱作星 山裂醇（―岭聚（1，3_丙二醇對献酸酯）稱作斯。聚 (1,3-伸丙基-共_M:3,6_二脫水七_山梨糖醇對社酸⑺稱作 豁。二-“3-丙二醇稱作〇pG。以丙二醇(1，3—__ glC〇l亦作l，3-pr〇panedi〇l)稱作”3G„。商標以大寫表示。 多種成型物件中結構釋定# * ^"疋性頗為重要，特別在纖維内（部 分定向紗）。獲得增強社福# + ^ ^ 5$、、Q構穩疋性係因提升Tg達成，原係由 聚醋内包含一種脫水糖醇部八 口 P刀之結果。本發明成型物件内 所用經酯改良的二羧酸酯肀入 日來合物係藉將脫水或二脫水糖醇 併入聚合物之兩種方法萝傲。 、備具體例1將脫水糖直接引入聚 (伸烧基-共-二脫水糖二酴获沾 ^竣S曰）。具體例2利用一預先形成 86038 1281925 的酯橋鍵部分幫助將脫水糖併入聚酯。 第一具體例内聚合物係由單體包含伸烷基二醇，較佳1，3-丙二醇；一種糠醇一酐或二酐，較佳異山梨醇；一種二羧 酸，較佳對酞酸或其烷酯；及隨意其他二醇與二酸或二酯 等製備。較佳3GIT聚合物以3GIT為基礎含至少約3，較佳 至少約4 〇1〇卜％(莫耳％)之異山梨醇。最多含約20 mole%， 較佳最多約15 mole%，尤佳最多約丨2 mole%，最好最多約 10 mole%異山梨醇單位，以3git基計。 3GIT聚合物係由對酞酸或其烷酯，丨^-丙二醇與異山梨 醇製備。反應混合物能含少量其他反應劑。二酸或二酯用 嚴以總3GIT為基礎可高達約15 mole%，較佳不超過10 m〇le%，最好不超過2 m〇le%。實例包括異酞酸，丨，仁環己 二幾酸，2,6-萘二羧酸，環己烷二羧酸，琥珀酸，戊二 黾，己二酸，癸二酸，1，12-十二烷二酸，及其等衍生物諸 如此等二羧酸的二甲、二乙、或二丙酯。亦可用少量三官 能酸，如1，3,5-苯三羧酸。 同樣可用最多I5 mole。/。，較佳不超過1〇 m〇]le%，最好不 超過2%之其他3至丨2碳原子酯屬二醇以代替丨，3_丙二醇。實 J L括具貫驗式Η〇-(〇ηΗ2η)_〇Η的二醇，其中11為2_12整數 例如乙二醇，1，4-丁二醇，ι，5_戊二醇，丨，卜己二醇及U0 — 癸二醇。亦包括支鏈二醇如2,2_二曱·丨，3_丙二醇，順-或反 式環己烷二甲醇及順與反式異構物之混合物；2,2〆，心 ^甲13-¾ 丁 一醇；二甘醇；2,2_雙[心（2_羥乙基）苯基]丙 k ’ 1，1-雙[4-(2-羥乙氧）苯基]環己烷；9,9_雙[4_(2_羥乙氧） 86038 1281925 苯基]芴κ土一醇部分係自乙二醇、丁二醇、丙二醇及環 甲酉子衍生。亦可利用少量大於2官能度之醇類，例如三 私甲丙院與季戊四醇。 此外’可按兴山梨醇基礎使用多達15莫耳當量％，較佳 不超過ίο莫耳當量％ ’最好不超過2莫耳當量％的其他脫水 糖醇類。其他脫水糖醇包括1，4: 3,6-二脫水甘露醇；1，4: 3,6-二脫水伊地醇；及丨，4_脫水丁四醇。 、、伯♦反應需要觸媒，隨時添加。所用縮聚觸媒包括Li， Ca ’ Mg ’ Zr ’ Μη，Zn，Pb，Sb，Sn及丁丨之鹽類，諸如醋 酸鹽與氧化物，包括二醇加合物及Ti醇鹽與螯合物。較佳 觸媒為Sb(III)鹽；Ti(IV)鹽；c〇(II)，Zn⑼或sb(II)的醋酸 鹽，Co(II)或 Sb(III)之烷酸酯鹽；Sb(n)、Sb(ln)或Ge(IV) 的氧化物；Sb(II)' Ge(IV)或Sb(III)之二醇增溶氧化物；原 鈦酸酯（較佳Ti(OR)4其R為有2至12碳原子的烷基，諸如鈦 酸四丁酯或鈦酸四異丙酯）；以溶劑為主的螯合有機鈦酸鹽 (例如 TYZOR AA或 TE觸媒（杜邦公司，Wilmington，DE)); 以水為主螯合之有機鈦酸鹽（例如TYZORLA或TE觸媒，杜 邦公司，Wilmington，DE)或如Putzig在美國專利6,166,170 内說明觸媒在此引用參考；原锆酸酯類（較佳Zr(0R)4)為一 有2至1 2個碳原子的烧基’諸如錯酸四正丙g旨或錯酸四正丁 酯（杜邦公司）；以溶劑為主螯合之有機錯酸酯；與以水為 主螯合的有機鍅酸酯；及其等結合物。以鈦之氧化物為佳 。有效觸媒包括在2002年4月25日所提共同待審的美國專利 申晴案1 0 /1 3 1，9 1 0中說明，本文引用參考。最佳為以溶劑為 86038 -10- 1281925 主聲合之有機鈦酸酯鱼以水 縮聚作用觸媒適宜量—…广5的有機鈦酸醋。 觸媒與輸㈣耳:二：1。至3°〇,或更明碟地 少約1:2,2。。，較佳最心M，。。。至約1:7,30。，宜至 罕乂1土取冋至約1 : 4,400 〇 觸媒亦能用以促進酯化作 ^ m ^ ^ ^ „ 作用或S曰基轉移作用，而縮聚反 應觸媒對酯基轉移作用转 ^, 用特別有效。上述縮聚觸媒亦能用以 催化酯基轉移，且能直掊於略π# 罝接於知化期間存在。技術上所知有 放催化酯化反應的觸婵
At 早…者如錫與鋅觸媒等亦能使用。觸媒 月匕；衣程之任何適當階段加入混合物。 ，（彳’3丙一醇與兴山梨醇）與二羧酸（較佳對S太酸） 或其㈣的莫耳比率係自約11:1至約16:1，較佳至少約 u . 1 ’亚宜最高約u : i。二醇較佳丙三醇，對二脫 水糖醇較佳異山梨醇之莫耳比率係自約2:1至約10"，宜 最少約…及最高約8:1。用其他二醇、脫水糖醇、二酸 或一酉日4應置換當量莫耳數的二醇（H丙二醇與異山梨醇: 或對目太酸或其烧酯以得相同莫耳比。 ♦(伸烷基-共-二脫水糖酯）二羧酸酯之顏色能用著色劑 ，宜染料及/顏料改良。顏色普通以亨特值（HU — )表示，其 相當於試樣的明暗度（”L*”），在紅-綠刻度上之色值（γ")， 在K監刻度上之色值（"b*”），且其係按下文敘述測量。通 ¥要求衣k L至少70之聚合物。同樣，淺色聚合物的，，&*，，與 b且低於約2.G至約_2.G °經發現能用顏色校正添加劑達 成3GIT之此等目標。任何適當著色劑能單獨或混合使用。 為求色淡，亦務要消除或至少降低單體起始材料内所含帶 86038 -11 - 1281925 色雜質。1，3-丙二醇與異山梨醇 外宜低於0.20，較佳低於〇.1〇。 聚合物又包含選自紅外線吸收劑、著色劑、染料、顏料 、褪光劑、難燃劑及uv穩定劑等之添加劑。此等添加劑能 ，任何時間添加，包括在聚合物製造成型物件或其他產品 了 種較適宜4擇為脫除縮合反應中衍生的至少水 後’將紅外線吸收劑、著色劑、染料、顏料、褪光劑、難 =劑、與/或UV穩定劑等加入製程。紅外線吸收劑以石墨或 石反黑為佳。 2造聚合物之聚合程序包含⑴s旨化或§旨基轉移作用與^ 真空縮聚作用。製程能以分批、連續或半連續基礎完成。 酉曰化或酯基轉移作用典型於約180至約2451：範圍内溫度下 在丨“生氛圍及常壓下進行。排出的水或烷醇自反應混合 :中，分餾塔蒸餾送回二醇及二脫水糖醇至反應。大部份 广或浼0子（至少約80%)蒸餾出後減壓至完全除去水與烷 _ π並‘除過多二醇。縮聚作用之辭用以說明製法中齊聚 物、、二鈿合生成聚合物，而除去二醇二脫水糖醇及水。在此 階段必要給取 r- _ 、、I 應觸媒，並於此際隨意添加任何其他需要 的添加齊丨，# i 4 诸如紅外線吸收劑、著色劑、染料、顏料、褪 光劑 、St to ^ u V f患疋劑及其他熱穩定添加劑。反應混合 咸I同時攪拌中加熱直到所求特性黏度（IV)，典型 歷約1至約6 I 士 /、 小蚪。IV上升時熔化黏度亦提高。儘量縮短高 /皿日守間亦右 dl/ ^ 於減少色變。典型地，1V—旦到達至少約0.5 8 較佳至少約0.6 dl/g，則縮聚反應完成。 86038 1281925 如Charbonneau在u_s_ 6,〇63,464中說明，固態聚合作用能 用以升咼縮聚期間所製聚合物的IV，本文引證參考。自隨 意自由酸或酯製程所得的聚合物於縮聚階段結束時移出反 應斋，以幾種傳統方式之任一種分離，如股線、小丸或薄 片。若未充分結晶、分離的聚合物（較佳為3GIT)經加熱至 約8〇°C到12〇°C範圍内溫度能結晶。結晶之聚合物於真空下 或在約19〇°C (典型170。〇至丨95。〇升溫惰性氣流内但$結 晶聚合的熔點溫度以下加熱產生固態聚合產物。固態聚： 反應中繼續在真空下加熱以升高…自〇·8至約^ di:供： 種最後用途。 ,第一具體例内製備聚(伸烷基-共_二脫水糖酯)二缓酸酯 聚合物先使二脫水糖醇與一酸或其二烷_接觸產生一醋 (後文指㈣連部分），㈣將該橋連部分與一 羧酸酯齊聚物縮聚。橋連部分有如下式i的結構：土
X-Ia-(A-I)n-Ab-X 其中： A為一脫水糖醇或二脫水糖醇中g旨殘基 I係一種二酸或其二烷酯中之酯殘基， 由二元酸衍生的I殘基 元酸之二烷酯衍生的I殘 X於連接A殘基時為H，於連接 時為0H，而在連接一由二 基時則為OR， R係一 直或支鏈烷基 a與b為獨立地〇或1，及 86038 -13 - 1281925 η係1至1〇。 醇中的酯殘基為脫除羧基之氫所餘的醇。二酸之酯殘基 係脫除經基的二酸。 有a = 0，b = 0及η=1至1 〇之橋連單體的一例有如下式Η之結 構，係使異山梨醇與異酞酸或一異酞酸二烷酯反應而製備。
式II的橋連部分典型為以上酯類之混合物，其η值為1至 約1 0，酉旨以η = 1佔多。 第二具體例的程序迴避第一具體例内所述異山梨醇與對 馱酸或對酞酸二曱酯直接酯化或酯基轉移作用緩慢反應速 率產生之問題。此點大為改善藉製備一預成型的橋連部分 而攙併二脫水糖醇於聚酯。橋連部分係由一種二酸之酯化
基轉移作用製備。
及在約 〇·4 mm汞（0·05 kPa)以下的壓力加熱 至少約0.8 dl/g，典型歷1至2小時。 前述第一具體例。 以迄特性黏度（IV)達到 可力ϋ觸媒與添加劑如同 86038 14 1281925 未反應之二脫水糖醇於真空加熱期間脫除，且應在縮聚 步驟除至最少。縮聚步驟在熔化試樣上完成，特性黏度與 刀子量增加至最高平衡值。最後，如具體例1說明，具體例 2 +合物的特性黏度藉於氮下之固相聚合作用升高至約1 ·2 dl/g以上。 橋連部分中二酸基包括而不限於自莕二甲酸酯，對酞酸 8曰，異酞酸酯與苯甲酸酯所衍生者。二酸基之特別實例包 括異酞酸，酞酸，2,5-呋喃二羧酸，2,5_p塞吩二羧酸，2·6_ ’丁、文馱，2,7-奈二羧酸，3,4、與4,4，-二苯醚二羧酸，3,4，· 、4,4-一苯化硫二羧酸，3,4，·與4,4，_二苯颯二羧酸，3,4，_ 贫4,4 -一笨甲酮二羧酸，丨，仁萘二羧酸，4,4，_曱又雙（環己） 羧酉夂，反_1，4-裱己二羧酸，順β1，4_環己二羧酸，丨，2_雙（4_ 羧笨氧基）乙烷’ 4,4’-甲撐_雙（苯甲）酸，反_4,4，_芪二羧酸 田馬I 一聚酸，間笨二醋酸與磺基異酞酸，及4,4，-聯笨 ^酉文。一酸不需自對g太酸或對酜酸二甲g旨或自含—酉大驢部 刀之其他化合物何生。亦可用少量的多官能酸或針類，例 =，3,5-苯三賴，苯均四酸，及苯均四酸二野。此外，所 口月芳族”與”脂環”，意謂包括取代的芳族或脂環化合物等 例如經脂基取代之芳族化合物。較佳二酸部分為異献酸。 橋連部分内脫水或二脫水醇基包括但不限於显山梨醇； 以：^-二脫水甘露醇^:^二脫水伊地醇：及^ 脫水丁四醇。較佳二脫水糖醇基為異山梨醇。 橋連單體係由二酸與 得。此處敘述異自太酸與 二脫水糖醇於一觸媒存在下加熱製 齐山梨醇的程序包含在惰性氣體氛 86038 ' 15- 1281925 圍下於約9(M40微克/g呈適宜觸媒形式之錫存在下（例如正 丁基錫酸）加熱0至100111〇1^/()過量之異山梨醇，較佳2〇至4〇 mole%過量的異山梨醇與異酞酸。溫度約21〇至，較 乜240至2 60 C。放出水約30分鐘後得透明溶液，繼續加熱 至不再排水，典型經約丨至2小時，指示酯化反應終了。 二脫水糖醇：二烷酯之莫耳比宜約丨·4 : 1。在氮氣清洗 下加熱攪拌混合物至約250它，其時開始放出醇（用異酞酸 二甲酯之指定情況中為甲醇）。在25〇t：繼續加熱攪拌至不 再放醇（典型經約2小時以上），指示酯基轉移反應完全。 在二酸與二烷酯二種途徑中需要時能於真空下加熱立即 脫除未反應的二脫水糖醇，但典型較佳於後來縮聚期間脫 除。 / 以上形成之橋連部份隨後，以聚（伸烷基酯）預聚物重量 計，藉由混合一聚（伸烷基酯）預聚物或齊聚物與〇·5至 ，較佳2至20%，最好4至10%的橋連單體接受縮聚作用。預 聚物較佳為聚（伸烷基對酞酸酯）。聚（伸烷基對酞酸酯）預聚 物有自約0.02至約〇.〇6 dl/g之特性黏度，較佳為聚（I，、伸丙 基對酞酸酯）齊聚物。重要在經1^^4{1測量聚酯預聚物含 以下重量比的未反應二醇，因為縮聚期間此等未反應之二 醇出現干擾酯基轉移作用製程。未反應的二醇能藉真空汽 提脫除，或將預聚物碾細，以水萃取二醇後乾燥。9觸二^ 鈦酸烷式，根據所加預聚物/橋連單體混合物重量計用量為 10至200微克/g之鈦。混合物在惰性氣體氛圍下於約至 290 C，較佳240至260°C及壓力低於約〇4 mm汞（〇〇5 kpa) 86038 1281925 加熱溶化，直到特性黏度（IV)達到至少〇8 ， 至2小時。真空加熱期間脫除未反應的二脫水搪，：[丨 驟4日門+ 一 & u ， 尤K搪酉子。縮聚步 ， 式樣上完成，特性黏度（與分子量）辦力$ n 大平衡值。 卞里）i日加至最 广具體例1說明任何在產物内之黃色調能用著色，r 染料與/或顏料修正。作低色度製品亦務必消除或至:、： 二”體起：：料内存有的發色雜質。起始材料之UV吸：率 ⑽賊時宜低於〇·20,較佳於22〇nm時在〇.1〇以下。 聚合物另含選自紅外線吸收劑、著色劑、染料 褪錢、難燃劑及UV穩定劑等的添加劑。此等添加劑能於 ::間加入’包括聚合物製成成型物件或其他產物時： U驟後在所得聚合物上與 6 1士 W 一脫水橋酿沾 、寸照試樣比較測量證明其攙併 ， 叩及較高冷結晶溫度（T 玻m溫度 又（「㈦，k供頌者價值予纖維、薄膜、 表面與工程熱塑組份方面幾種最後用途適 度（Tg)與冷結晶溫度（Tee)二者 〜、化皿 單位而俱增。 以冋聚合物内二脫水糖醇 縮聚的聚合物產品之特性黏度約q.8心對有些最後制 品諸如纺絲纖維的最適加工性嫌低。因此縮二 緩慢氮流下在約300 mm Hg (39 k 逍傻於 。 Μ之減壓烘箱内於熔點 下約20C的溫度(在約l90t)接受固相聚合作用。特定溫度 以縮聚產物之熔點為依據。在最後IV約〇_85或以下時聚人 :勿顯不纖維性質不良。最後IV約丨·2以上產生加工與纺絲問 題° 86038 -17- 1281925 本發明其他具體例中橋遠 ^ #分能接受與各種聚酯齊聚物 縮聚’包括而不限於聚（對酞 V 丁狀@久乙二醇），聚（三甲撐對献酸 酯），聚（四甲撐對酞酸酯），盥耳 ；"♦(伸烷基1，4-環己二羧酸酯） 及類似齊聚物。 由本毛明橋連部分與聚（伸烷基酯）預聚物縮聚作用所產 的最後縮聚聚合物，名稱聚[(伸烷基_共_二脫水糖酯）二羧 酸酯]，用作起始材料以製造成型物件。 本發明另一具體例中式1構造之聚[(伸烷基-共-二脫水糖 酯）二緩酸醋]亦包括含至少30 mole%聚[(伸烷基-共·二脫 水糠醋）一緩酸酯]單位的共聚物。較佳聚合物含至少8 5 mole%，更佳至少90 m〇le%，甚至尤佳至少95或至少98 mole%，最好約100 m〇ie%之聚[(伸烷基-共-二脫水糖酯）二 叛酸酯]重複單位。 本發明的聚[(伸烷基-共-二脫水糖酯）二羧酸酯]組合物 含三種單體，即伸烷基二醇、脫水糖醇酯、與二羧酸。另 /具體例内共聚物可包括用4種或更多反應劑各有二成酉旨 基製作之共聚酯。例如，能用一共聚[(伸烷基-共-二脫水糠 酯）二羧酸酯]，其中製作共聚酯所用的共聚單體係選自有 4-12碳原子之線型環狀與支鏈的酯屬二羧酸（例如丁二酸 、戊二酸、己二酸、十二炼二酸，及丨，4-環己二羧酸）；對 g太酸以外有8-12碳原子之芳屬二羧酸（例如異酞酸與2,6、| 二象酸）；有2-8碳原子的線蜇，環狀與支鏈脂屬二醇（1 兩二醇以外例如乙二醇，1，2 -丙二醇，1，4 - 丁一酉手，3 -甲、；[，5、 戊二醇，2,2-二甲-1,3-丙二酵，2_甲-1，3-丙二醇，與1，4、環 86038 1281925 ro 及有4_10碳原子之脂屬與芳屬醚二醇（例如_ (2,羥乙^ 上、 于如虱g昆雙 )岵，或分子量低於約46〇的聚（乙撐_ 二7掩 )—办，包i去 牙醚二醇）。共聚用單體典型存在共聚酯中含量 T s里軏圍約 冬 mole%，含量能多達3〇 m〇le%。 當有另一具體例内聚[(伸烷基_共_二脫水糖 與最客1 π , 曰^ —羧酸酯 mole%之其他聚合物摻混。實例為由其他二醇制 的聚酯如上說明者。*宜聚[(伸烷基_共_二脫水糖： :酸酯]含至少85mole%，較佳至少9〇m〇le%，甚至更佳: 95或至少98 mole。/。，最好約1〇〇 m〇le%聚[(伸烷基-共一 月兄水糖酯）二羧酸酯]聚合物。 、一 、、二S曰改良之一羧酸酯聚合物用或配合習用製法作成多種 成型物件包括纖維、紗線、薄膜、非織物或模塑物件。特 別有利者為使用聚合物提供纖維與紗線於高溫儲存時有加 kI疋性。纖維為單長纖或多組份長纖。加強穩定性許可 在製造作業中利用較高紡絲速度。 本發明的成型物件有Tg至少55，較佳至少60，尤佳至少 70 §在暖和溫度儲存時高T g對物件的穩定性有貢獻。成 型物件有IV自約1.5至約2.5。 所謂”多組份長纖”意指一種由二種聚合物作成之長纖， 其中之一形成連繽相，另一係分散遍及纖維的一或多不連 續相，其中至少二聚合物自同一擠壓機中成攙混物擠出。 本發明使製造長纖能在較低速度製備紗線所用相似條件 下後來加工作業中使用。本發明用聚合物在製備多長纖紗 程序内包括紡絲速度至少2500 m/m時有效。 86038 1281925 本發明成型物件含部分定向之紗線。部分定向的聚（丙二 _對献酸酯）紗敘述於美國專利第6,287,688與6,333，1〇6號 及美國專利公開第2(m/3()378號内說明，均在此引證參考 。製造部分定向紗的基本步驟包括紡絲、交織及其中所述 捲繞長纖。本發明能用#統製作部分定向聚i紗使用之諸 步驟或其他步驟作業；但提供進行具有穩定包裝與紗線性 質之方法的優點。 來口物紡絲之岫宜加熱至高於其熔點的溫度，並於約a]$ 至約295t之溫度擠壓通過紡絲嘴。溫度較高有利於縮短逗 留時間。 二部分定向紗線為多長纖紗。紗線（亦稱”束”）宜含至少約1〇 較佳至少約25根長纖，典型能含多達約⑼根以上，較佳多 至約1〇0根，更好最多約80根長纖。普通紗線常含34, 48 ’ 68或72根長纖。紗線典型有總丹尼爾（心^叫至少約^， 較佳至少約20,宜至少約5〇,且高達約1，5〇〇或以上 至約2 5 0為宜。 以南 長纖宜至少約〇.5 dpf，較佳至少約1 dpf，最高至約1〇以 上dpf，較佳最高約7dpf。典型長纖約3至7扑[，細長纖約 〇·5 至約 2.5 dpf。 紡絲速度能運轉自約U00至約8,〇〇〇以上公尺/分鐘 (m/m ) ’宜至少約2，_ m/m，較佳至少約2,500 m/m。 #刀疋向紗線通常捲繞成包，用以製作織造或非織造織 :勿或再處理成其他型紗如變形紗。亦能儲在罐内然後製備 織物或再加工，或能直接使用而不作包裝或其他儲存。 86038 -20- I28l925 本务明的成型物件亦包含纺絲拉伸紗。 佳製造步驟包括紡絲、拉伸 i 4伸紗之較 1甲 ^思與較佳韌化、（I、左立 、及捲繞長纖供文内用酯改 丨現思交織 似裝備聚（對酞酸乙二醇酯）紗所用者。 之長纖類 較佳在紡絲前加熱聚合物
$ 9 Ο ς ^ 、谷點/皿度’並於約？ U 至約295 C之溫度擠壓通過噴 、、々235 時間。 …“。溫度較高有效縮短逗留 此等紗亦係多長纖紗。 根，甚至較佳至少…5」以亦私作束”)宜含至少約1〇 . 勺根長、纖，典型能多至約150# m 車父佳最多約1〇〇根，尤 、.勺150根以上’ 、68、或以 取夕約8〇根長纖。通常為含34、48 或72根長纖的紗線。此 約5，护/土 寻、v線典型有總丹尼爾至少 、勺5,較佳至少約2〇，更佳至 旧玍乂 最多約25〇。 取夕約1，500以上，適宜 長纖宜至少約0」dpf，較佳 0.8 dpf, - ^ ^ {至乂为〇·5 dpf ’更佳至少約 ，取多約1〇以上d f， 拉伸P i 仏、、、勺5 dpf，最好高至約3 dpf。
拉伸比至少i.(H，宜至少約12 P 宜最高約5 ,較佳高π 至夕約1.3。拉伸比 早乂仏阿至約3，最適高至約2 5。 上!二度(在拉伸步驟末端棍處測量)能運轉自約秦 上，:以=高到約8__。紡絲拉伸紗常捲繞於包裝 變形紗。織造或非織造織物或再加工成其他紗型諸如 紗成型物件亦包含變形紗。變形紗能由部分定向 伸紗製備。主要差異在部分定向紗常需拉伸而 、、万糸拉伸紗則已經拉伸。 86038 1281925 美國專利第6,287,688與6,333，1〇6號及美國專利公開第 2 00 1/30378號皆在此引用參考，說明自部分定向紗製造變 形紗之基本步驟。本發明能用其等步驟或製作部分定向聚 酯紗的其他習用步驟實行。基本步驟包括放鬆包裝中紗線 、拉伸、加撚、加熱固定、解燃並捲繞於包裝上。織紋藉 捻撚、熱固授予皺褶，並靠通稱假撚之方法解捻。假撚織 紋經謹慎控制避免紗纖過度毀損。 美國專利第6,287,688與6,333，1〇6號及美國專利公開第 2001/30378號中說明摩擦假撚的適宜程序，包含加敎部分 定向紗至14代與22代間之溫度，用_加
使在加撚插入裝置與加熱器入口 /置捻V 至-的扭角而捲紗於一繞線器上。自=*紗線有約46。 程相同，惟降低拉伸至極低度（例如^申紗製備時製 此等變形紗咖”束”）含有降至 纺絲拉伸紗的相同長纖數所用部分^向紗與 甚至更佳至少約25根長纖，典型能含二 佳最多約100根’尤佳最多約8〇 : 根以上’較 爾至少約！，宜至少2〇。較、。々線典型有總丹尼 或更多，宜高約250。 至》約50’最多至約1，則， 長纖宜至少約(M dpf’較佳至少 〇-8dPf，最多約1〇以上dpf，較 古· Pf’更佳至少約 3 dpf。 土攻巧約5 dPf，最好至多約
由部分定向的紗製備時拉伸比至I ’更佳至少約1.3。拉伸比宜最古二、丨，01，較佳至少約以 取阿到約5,較佳最高約3,最 86038 -22 - 1281925 好最高至約2.5。拉伸速度（拉伸步驟終端輥處測量）運轉能 自50至約U200 m/m以上’宜至少約3〇〇 —，較佳最高到 約 1，0 0 0 m / m。 用纺絲拉伸紗製備時，速度（於纖維接觸第一導輥處測量） 能運轉自約50至約U00 m/m以上。較佳至少約3〇〇 m/m, 隶好袁南約800 m/m。 變形紗係用以製作織造或非織物或其他纺織物。 本發明的成型物件亦含鬆散之連續長纖。鬆散連續長纖 (bulked C0nunu0us filament，BCF)紗及其製造說明見 Howell等人之美國專利第5,645,782號，&⑽汁等人之第 6，1〇9,015號與Chuah的第6，1 1 3,825號；美國專利申請案第 09/895,906 ^ 09/708,209 ^ 〇9/93 8,760 ^ 1 〇/〇9953 73 f ^ 別為代理人案號CH2783，RD7850，CH2800與CH2848號） ，及W〇99/19557，全在文内引用參考。BCF紗係用以製備 各型地毯及紡織品，包括織造物與非織物。 涉及製備有關鬆散連續長纖之較佳步驟包括紡絲（例如 柘I冷却與塗覆（紡絲處理）長纖），單一或多段拉伸（宜用 加熱輥、加熱栓或熱流體援助（例如蒸汽或空氣））於約⑽至 約20(TC及約3至約5,宜至少約3·4，較佳最高至約4 5，在 約120至約200 C之溫度韌化，膨化，捲纏（能於一步驟内與 恥化或在之後以分由步驟進行），視情況膨化，及捲繞長纖 於包裝上供後來使用。 鬆散連續長纖紗用熟知技術製成地毯。許多紗線典型一 起&成k索’在諸如功熱器的裝置suESSEN或SUPERBA内 86038 23 1281925 熱固定’然後成簇加邊為初步襯底，再塗敷膠乳黏合劑作 第二襯底。 本發明之成型物件含短纖維。短纖維與產物用美國專利 申請案第09/934,904與09/934,905號所述方法製備，二者皆 於 2001/8/22提出，與 w〇 0 1 /68962，WO 01/76923，W〇 02/22925及WO 02/22927等均在本文引證參考。短纖維係由 ♦ 口物於約245至約285 QC溫度熔化紡絲製成長纖，驟冷長 纖、拉伸驟冷長纖、捲皺拉伸長纖，切割長纖成短纖維， 較佳長度約0.2至約6吋（約〇·5至約15 cm)。 一種較佳製程包含：（a)提供一聚合物，（b)於約至約 285 C溫度熔紡已炼聚合物成長纖，⑷驟冷長纖，⑷拉伸 驟冷的長纖，⑷缝㈣長纖用賴鍾機使切有約g 至約30摺之皺度（約3至約12摺續/⑽），⑴在約μ至約1贼 溫度放鬆摺_長纖，及（g)切割放鬆之長纖短纖維，較佳 長度約0 · 2至約6 口寸（約〇 $ 5 ί c ( 至約15 cm)。本製法的一較佳呈體 例内拉伸長纖於約8 5至約 輕在張力下實行。另一:減後捲鈹，化宜用加熱 不經拿刃化。 n、體例中拉伸之長纖在捲摺前 短纖維適用於製備織物紗 台匕田舰处从β I 入、々、’物幾造或非織品， 此用仏、滅、、隹填充使用與製作地毯。 本發明成型物件亦含單具徐 單具_ 早長缄。草長纖宜係1〇至200dpf 早長..減、早長纖紗及其用途在美國
1 167 594及 wo 2001/75200 中日 ，·^0,909號’ I 明雖主要敘述有關多長纖紗線：二=用參考… 緊角午文内所述優先與戶 86038 -24 ~ 1281925 途能實用於單長纖。 長纖能係圓形或有其他形狀 射狀（亦稱作sol)、扇形橢圖、 亦作 quatra-channel)、扇形帶、 或多孔。 ，諸如八瓣狀、三角形、曰 二葉片、四槽（tetra-channel τ星爆等。可係實體、空心 除製作更安定纖維外，聚（伸烷基-共-二脫水糖酿）二羧酸 酯聚合物適用於製造熱塑性成型物件，其係藉由注模，吹 塑、擠壓與壓縮模，及製造塗料、疊層與黏合劑、製造包 裝與工業用薄膜、製造其他能熔化處理之產品諸如聚胺基 曱酸酯、聚醚醯胺及聚脲烷脲纖維以及製造泡沫與澆鑄^ 體之活性擠壓製造。 本發明在以下實例内示範，非欲限制。其中除非另行指 出’全部百分比、份數等均係重量計。 【實施方式】 實例 以下刀析技術與材料在貫例内使用。 玫璃態化黑度（Tg) 用差示掃描量熱術（DSC)測定Tg值。一聚合物的1〇11^試 樣磨碎至通過2〇目篩（7.9 cm·1)，以帶有冰凍冷卻附件（其以 加熱速率1〇 C /分自室溫至280 °C控制冷卻之丁a儀器2920 DSC進行分析。試樣遂於28〇t保持2分鐘，在液態氮中驟 冷後自室溫再加熱至2801：。聯合的軟體計算出Tg，Tc(結 曰曰/里度）與Tm(炼點）。測量Tg與溶點之手續係按292〇 之ΤΑ儀裔手冊說明使用。 86038 •25 · 1281925 聚合物成分 異山梨醇與二-1，3-丙二醇（DPG)含量之莫耳百分比用 3GIT的質子NMR光譜分析測定。溶解約2〇 mg 3GIT於1 mL· 三氟醋酸-d(CF3COOD，99.5原子。/。，見以下材料節）。試樣 在室溫用一 Varian (Palo Alto, CA) 5〇〇 MHz分光光度計分 析。 IL_色與 用一帶漫反射附件之Varian (Pal〇 Alt〇 CA)Cary 5 UWVis/NlR分光光度計測定3GIT試樣的顏色與亮度。以有2 度觀察角與CIE A光源之Grams/32軟體内顏色分析應用處 理反射數據。計算亨特L*，a*及b*。L*座標指示亮度，其 中〇為黑而100係白。a*值能係正或負，其正值標示紅色， 負值指示綠色。b*值相仿，正值指示黃色，負值表示藍色。 特性黏庶 特性黏度用一 Viscotek Υ-900型強制流動黏度計測量。聚 合物溶解於50/50 w/w三氟醋酸/甲基氯成〇4% (wt/v〇1)濃 度’於19。(：試驗。所用方法在ASTM D2857.95内說明。 收縮-張力分折器 收、纟佰-張力分析态係杜邦公司（Kinst〇n，NC)製作以分析 紗線張力與溫度的關聯。分析器裝設有溫度控制器（〇_6〇〇 C，Valley只(^6儀器公司在ph〇enixvnie，pA製）控制加熱 至度，一 Statham負載電池（UL4-0.5型）與Statham通用換 能CEU UC3型（金電池）作張力偵察器以測量張力，與 Hewlett Packard 7035B Χ-γ記錄哭。 86038 -26- 1281925 紗線試樣以固定長度1 〇〇 mm安裝作線圈。對線圈施加預 張力於0.01公克/丹尼爾。紗線張力以30°C/分鐘之加熱速率 在2 5至2 2 5 C範圍内測量。最南溫度為張力達到最大時的溫 度。 材料 異山梨醇係得自法國Lestrem之Roquette Freres。 1，3 - 丁二醇係得自W i 1 m i n g t ο η，D E的杜邦公司。 TA-33-LP 對酞酸係得自 Naperville，Illinois 之 Amoco。 99.5原子％的三氟醋酸_d (CF3c〇〇d)係得自Milwaukee， Wisconsin之 Aldrich 〇 HS-325 SANDOPLAST Red BB，HS-510 SANDOPLAST Blue 2B，POLYS YNTHREN Blue R，及 CLARIANT RSB violet 係付自 Coventry，Rhode Island Clariant的 Corporation。 對酉太酸一甲酯係得自W i 1 m i n g t ο η N C之K o s a。 TYZOR LA(—種含水二羥雙銨乳酸鈦）係得自 Wilmington DE的杜邦公司。 觸媒A係一觸媒溶液，由537克醋酸鋅與12〇〇克水混合製 備’溶液於室溫（約25°C)以人工攪拌加入244克TYZORLA (見上文），然後加4 3克乳酸於溶液。 觸媒B係一觸媒溶液，由15〇克磷酸鈉與丨5〇克水混合製得 溶液’於室溫（約25。(：）將溶液以人工攪拌加入1，000克 TYZOR LA(見上）。 實例1 本實例示範製備本發明的聚合物呈丸狀，小丸之固態聚 86038 -27- 1281925 一作用’與聚S旨的、紡絲。 在一 公升不銹鋼容器中加747.45克對酞酸，367.08克 1 3 又
’ ·丙二醇’ 149.94克異山梨醇，1.08 mL觸媒B，0.27 mL S水氯氧化四甲基銨（25重量％)，0·0079克SANDOPLAST R1
Ue 2Β ’與〇·⑽19克SANDOPLAS Red。提升整批溫度至 古 取南240 ◦ ’同時經塔脫水。脫除69克冷凝物時將反應器 各物降至2.0 mm Hg (0.27 kPa)，以利於250°c時縮聚。 測 ~ 1¥為 〇.54，Tg為 60.4°C。亨特色值為 L* = 69.2，a* = -l .89 b 1 ·64。異山梨醇含量為5.56 mole%，聚合物含〇·3 m〇le% dpg 〇 此聚合物於氮氣加壓下擠壓通過模具形成股束，拉經冷 水槽進入切斷機作成1/8吋（3·2 mm)丸粒。結晶丸粒在19〇 °C真空烘箱中於約300 mm Hg (39 kPa)減壓及緩和氮氣流 下接受固態聚合作用歷5曰。二天後所得IVg〇92 dl/g，五 曰後最後IV為1.071 dl/g。所產聚合物適用以製成型物件， 如上文敘述者。 於固相聚合作用步驟後，聚合物在1 2 0 °C真空烘箱内乾燥 至少1 6小時。已乾的聚合物迅即轉移入維持室溫之氮氣籠 罩之供料漏斗，以3 5克/min送料至一雙螺桿再溶器。桶脸 加熱部分設定第i區於250°C，第2至8區於26〇t，泵塞處260 °C，及包裝加熱器處265t。欲每分鐘紡絲95丹尼爾25〇〇 m ，設定計量泵於29.0克/分鐘，一穩定泵則設定於6克/分鐘 以保持物料通過總量3 5克/分鐘。紡絲計量栗擠壓聚合物通 過一砂濾器紡絲包與一有〇 · 〇 1 〇，’（ 0 · 2 5 m m)直徑及〇 〇 4 〇，，（ 1 86038 -28 - 1281925 _)毛細深度孔的34個圓孔噴絲嘴，其係保持於靴。離 開喷絲嘴之長纖流經21t:的空氣驟冷，集合成束並施纺絲 整理。：表面下速度2500 m/min之前進幸昆移送紗束至交織 喷射後送至以2550 m/min轉動的捲繞作業。 紡絲條件與性質概述於下表i。 實例2 重複實例1製程。纺絲條件與性質摘要說明於表卜
交例A 本比較例顯示自DMT製備— 3GT聚合物（即不同異山梨醇）。 在一 公升授動玻璃容器内加胤4〇克對酉太酸二甲酉旨， 197.86 克 1，3 -丙二醇，及〇 I' •3 3 mL觸媒A，沉浸容器於加埶油 =。提升整體溫度至最高2贼，同時經塔柱移去甲醇。 °、’'、、/飞'皿度超過6 7 c ’關閉凝縮物閥以避免自塔頂損 失1，3-丙二醇。當5小時内可能已脫除ία g甲醇内之⑹ 社時，降低反應器内容物至 260C時縮聚作用。測得IV 〇64」丨/§及47外。亨特色 值為L*’」’ a* = 0.97及b*=2.54。聚合物不含異山梨醇， 含 DPG量 0.19 mole%。 此聚合物接受固態聚合作用並如實勝聚合物般纺成 纖維。 、 重複比較例A製程。紡 絲條件及 性質摘述於表 86038 '29 - 1281925 表1 實例 聚合物 成分 纺絲捲繞 速度 (m/min) 丹尼爾 強度 (g/d) 延伸率 (%) Tg/Tm (°〇** 實例 1 3GT異山梨 醇5.6 mole% 2500/2550 93.6 2.84 64.53 63.58/211.07 2 同實例1 2500/2550 95.4 2.76 65.2 59.47/213.78 比較例 A 100% 3GT 2500/2550 97.2 2.63 90.24 45.95/227.29 B 同A 2500/2550 95.4 2,68 88.80 43.87/227.54 表1顯示相對於比較例，本案實例有較低熔點，較高Tg 與較高強度。其變化改善了 POY的老化安定性。 **Tg與Tm用DSC測量。 實例3 POY纖維結構穩定度試驗 比較例A doff 7與實例1 doff 10之POY係用以在熱環境下 比較P0Y纖維結構穩定度。為模擬熱環境，P0Y包裝經暴 露於41 °C烘箱中加熱〇，0.5，2.5，17，48，及73小時。用 前述分析器以每分鐘3(TC加熱速率於0.01公克/丹尼爾的起 始張力測量收縮-張力。如表2顯示張力在25-225 °C溫度範 圍内表現特徵。相對於無異山梨醇之3GT於41 °C加熱73小 時後的尖峯張力降落47%，有異山梨醇的3GT之最高張力有 9%降落，此指示有異山梨醇之3GT具明顯穩定結構。 86038 -30- 1281925 當有突然收縮-張力增加時由玻璃態化溫度（Tg)指出。如 下表現無異山梨醇之3GT有—重大Tg移動自52 4至6〇2。〇 而有異山术醇的3GT於加熱17小時後僅輕微移動自59·4至 61.1°C。Tg移動量在加熱48與73小時後有異山梨醇之3〇τ比 無山梨醇的3 GT亦相對平穩。i ^ μ 心加熱後T g較穩定提示纖維在 熱環境下熟化後結構更穩定。如表2顯示，收縮.張力 示有異山㈣的3GT比無異山梨醇的抓之結構更為穩定。 12纖維穩定度數t
加熱(小時 實例識別丄
實例1
Tg，。C 59.0 60.7 59.4 61.1 63.5 65.8 收縮·•張力(％) 〜--- 58.6 """ ------ 46.3 ~~———___ 41.8 42.2 42.1 49.7 比較例A —*—— Tg，°c -------- 52.9 52.2 52.4 60.2 65.1 *—— 67.9 收縮-張力(％) ....... 1 - 48.6 ------- 37.3 ~~-----__ 11.4 ~—------ 7.8 6.4 5.5 —~~~~^ 表2内貝例1相對比較例A表現延長加熱時Tg較少變化而 $為減低收、、伯-張力。此：性質均指示含異山梨醇的纖維^ 疋度增進。Tg變化與較高收縮，力指示發生纖維結晶，此 變化乃與纖維儲存接π、& ι „ ^ 子後不適當之不穩定性相聯。收纟但·張力數 據描述於圖1，复Φ Δ托— — '、甲Α指示比較例，Α與Β指示貫例1。 f 例4 在2 L授動不錄鋼容器中加873 9〇克對酞酸二甲醋， 86038 •31 - 1281925 367.08克1，3-丙二醇，149.84克異山梨醇，0.75 11^觸媒八與 1.8 mL氫氧化四曱基銨水溶液（25重量％)。整批升溫至最高 24〇°C，同時經塔柱脫除甲醇。凝縮物脫除288克時降低反 應器内容物至2.6 mm Hg (〇.35 kPa)於25〇t：溫度供縮聚作 用。測得IV 0.50 dl/g ’ Tg為63.代。亨特色值為5 ’ a*=0.02及b* = 7_7。異山梨醇含量為5〇7 _u%，聚合物 含 0.07 mole % 二-1，3-丙二醇。 本發明雖已以有關明確具體例敘述，廊、 其可作許多變異與修訂而不月兒本發明領域/欲限制 【圖式簡單說明】 ^ 3 ° 圖1描繪本發明實例丨之組合物於41。匚日± 熱時間（以小時計）的纖維收缩率百八 τ 〃原來長度對加 之含異山梨醇之實例1以B表 b之曲線圖，本發明 一 认π ,相對之A田 貫例A之對照組合物以A表示。 热兴山梨醇之比較 86038 - 32-
Claims (1)
128 >9SS6i24號專利申請案 申請專利範圍替換本(96年2月)为 秦、 拾、申請專利範圍： 1· 一種成型物件，其包含聚[(三伸甲基-共-二脫水糖酯） 二羧酸酯]或聚（三伸甲基-共-二脫水二羧酸酯）。 2·根據申請專利範圍第1項之成型物件，其包含聚[(三伸 甲基-共-二脫水糖酯）對酞酸酯]或聚（三伸甲基-共-二脫 水對酞酸酯）。 3·根據申請專利範圍第1項之成型物件，其具有I V.自〇.5至 2·5 〇 4.根據申請專利範圍第丨項之成型物件’其為纖維、紗線鲁 、薄膜、非織造物或一模塑物件。 ，其係短纖維或長 其係一具有Tg至 ，其係—具有Tg至 5 ·根據申請專利範圍第4項之成型物件 纖0 6·根據申請專利範圍第4項之成型物件 少5 5之纖維。 根據申請專利範圍第4項之成型物件 少60之纖維。 其係—具有TgS _ 根據申請專利範圍第4項之成型物件， 少70之纖維。
紗線之形式之短纖維。 之成型物件，其係呈部分定向
紗線之形式之短纖維。 之成型物件，其係呈紡絲拉伸
的紗線形式之短纖維。 之成型物件，其係呈紡絲變形 86038-960202.doc 1281925 12.根射請專利範圍第5項之成型物件，其係另含著色劑、 染料、顏料、褪光劑、難燃劑、紅外線吸收劑或 劑之短纖維。 & 13· —種多長纖紗，宜包含聚（ …b 3水（一伸甲基-共-二脫水糖酯） 酉太酸酉旨或聚（三#甲其j£ _ 、 甲T暴/、- 一脫水糖對酉太酸酯）的多組份 14. 根據申請專利範圍第13項之紗，其中紗係部份定向紗。 15. 根據中請專利範圍第13項之紗，其中紗係纺絲拉伸紗， 其係於2500至8_ m/min的拉伸速度下拉伸長纖製僙 ’速度在拉伸步驟終端輥輪處測定。 、 16. 根據申請專利範圍第13項之紗，其係經⑷製備一卷呷 份定向紗，（b)解開卷裝中紗線，⑷拉伸多組份長纖^ 形成抽紗，（d)假撚變形拉伸紗作成變形紗，及 紗線於包裝上。 % i 7 .根據申請專利範圍第i 3項之紗’其係經⑷以拉伸步驟觀 輪末端處所量2500至_ m/m的拉伸速度拉伸長纖^ 備一卷紡絲拉伸紗線，（b)解開卷裝中紗線，（c)假撚變籲 形拉伸紗形成變形紗，及（e)捲繞紗線於包裝上。 18.根據中請專利範圍第13項之紗，其係呈散農連續長纖式 19. 根據中請專利範圍第13項之紗，其另含著色劑、紅外線 吸收劑或UV安定劑。 ' 20. 根據申請專利範圍第1項之成型物件， ”乃各多達約30 mole%的共聚物。 86038-960202.doc 1281925 21 22, 23, 24, 25, .一種織物，其係由申請專利範圍第9、1〇或^項之成型 物件構成。 .一種織物，其係由申請專利範圍第14、15、16或17項之 紗構成。 ，一種地毯，其係由申請專利範圍第18項之紗構成。 .根據申請專利範圍第1項之成型物件，其中該聚[(三伸甲 基-共-二脫水糖酯）二羧酸酯]或聚（三伸甲基_共_二脫水 二羧酸酯）係由包含以下之單體形成：（a) 一含丨，％丙二醇 之伸烷基一醇單體；（b)—種糖醇一酐或二酐；及（c)一種· 二羧酸或其烷酯，其中（a)+(b):(c)之莫耳比例係由約11:1 至約1.6:1，且該（a):(b)之莫耳比例係由約2:1至約1〇:1。 根據申請專利範圍第2項之成型物件，其中該成型物件包 含由以下所形成之多[(三伸甲基·共_二脫水糖酯）對酞酸 酉曰]· (a)1，3·丙二醇；（b)對酞酸或其烷酯；（c)以聚[(三 伸甲基-共-二脫水糖酯）對酞酸酯]為基礎之約3至約2〇 莫耳％之異山梨醇；（d)視情況以聚[(三伸甲基-共-二脫 水糖酯）對酞酸酯]為基礎高達15莫耳％之其他3至12碳原籲 子之脂族二醇；（e)視情況以聚[(三伸曱基_共_二脫水糖 酉曰）對酞酸酯]為基礎高達約丨5莫耳％之其他二酸或二酯 ，及⑴視h況可使用以異山梨醇為基礎高達丨5莫耳當量 之其他脫水糖醇；及其中i，％丙二醇及其他二醇：對酞酸 及其烷酯及二羧酸或其烷酯之莫耳比例係由約丨.丨··丨至約 1.6:1 ’且1，3丙二醇及其他二醇：異山梨醇及脫水糖醇之比 例係由約2:1至約1 〇: 1。 86038-960202.doc
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| US20100044928A1 (en) * | 2008-08-22 | 2010-02-25 | E. I. Du Pont De Nemours And Company | Process for Shaped Articles from Polyester Blends |
| US20100044266A1 (en) * | 2008-08-22 | 2010-02-25 | E. I. Du Pont De Nemours And Company | Polyester Blends |
| US8604105B2 (en) | 2010-09-03 | 2013-12-10 | Eastman Chemical Company | Flame retardant copolyester compositions |
| US8846960B2 (en) | 2011-05-24 | 2014-09-30 | Eastman Chemical Company | Oxidation process to produce a crude and/or purified carboxylic acid product |
| US9199958B2 (en) | 2011-05-24 | 2015-12-01 | Eastman Chemical Company | Oxidation process to produce a crude and/or purified carboxylic acid product |
| US8791277B2 (en) | 2011-05-24 | 2014-07-29 | Eastman Chemical Company | Oxidation process to produce a crude and/or purified carboxylic acid product |
| US20120302768A1 (en) | 2011-05-24 | 2012-11-29 | Eastman Chemical Company | Oxidation process to produce a crude and/or purified carboxylic acid product |
| US9573120B2 (en) | 2014-05-08 | 2017-02-21 | Eastman Chemical Company | Furan-2,5-dicarboxylic acid purge process |
| US8791278B2 (en) | 2011-05-24 | 2014-07-29 | Eastman Chemical Company | Oxidation process to produce a crude and/or purified carboxylic acid product |
| US20130095269A1 (en) | 2011-10-14 | 2013-04-18 | Eastman Chemical Company | Polyester compositions containing furandicarboxylic acid or an ester thereof and ethylene glycol |
| US8748479B2 (en) | 2012-06-22 | 2014-06-10 | Eastman Chemical Company | Process for purifying crude furan 2,5-dicarboxylic acid using hydrogenation |
| US8859788B2 (en) | 2012-06-22 | 2014-10-14 | Eastman Chemical Company | Esterification of furan-2,5-dicarboxylic acid to a dialkyl-furan-2,5-dicarboxylate vapor with rectification |
| US8969404B2 (en) | 2012-06-22 | 2015-03-03 | Eastman Chemical Company | Purifying crude furan 2,5-dicarboxylic acid by hydrogenation |
| US8912349B2 (en) | 2012-06-22 | 2014-12-16 | Eastman Chemical Company | Method for producing purified dialkyl-furan-2,5-dicarboxylate separation and solid liquid separation |
| US8658810B2 (en) | 2012-06-22 | 2014-02-25 | Eastman Chemical Company | Method for producing purified dialkyl-furan-2,5-dicarboxylate vapor |
| US9029580B2 (en) | 2012-07-20 | 2015-05-12 | Eastman Chemical Company | Oxidation process to produce a purified carboxylic acid product via solvent displacement and post oxidation |
| US8809556B2 (en) | 2012-07-20 | 2014-08-19 | Eastman Chemical Company | Oxidation process to produce a purified carboxylic acid product via solvent displacement and post oxidation |
| US8772513B2 (en) | 2012-08-30 | 2014-07-08 | Eastman Chemical Company | Oxidation process to produce a crude dry carboxylic acid product |
| US8916720B2 (en) | 2012-11-20 | 2014-12-23 | Eastman Chemical Company | Process for producing dry purified furan-2,5-dicarboxylic acid with oxidation off-gas treatment |
| US9156805B2 (en) | 2012-11-20 | 2015-10-13 | Eastman Chemical Company | Oxidative purification method for producing purified dry furan-2,5-dicarboxylic acid |
| US8916719B2 (en) | 2012-11-20 | 2014-12-23 | Eastman Chemical Company | Process for producing dry purified furan-2,5-dicarboxylic acid with oxidation off-gas treatment |
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| US9943834B2 (en) | 2014-05-08 | 2018-04-17 | Eastman Chemical Company | Furan-2,5-dicarboxylic acid purge process |
| US10696645B2 (en) | 2017-07-20 | 2020-06-30 | Eastman Chemical Company | Method for producing purified dialkyl-furan-2,5-dicarboxylate |
| FR3072094B1 (fr) * | 2017-10-11 | 2020-09-04 | Roquette Freres | Polyester thermoplastique hautement incorpore en motif 1,4 : 3,6-dianhydro-l-iditol |
| EP3784647B1 (en) * | 2018-04-25 | 2022-05-11 | DSM IP Assets B.V. | Novel dicarboxylic acid diesters |
| CN109677067B (zh) * | 2018-12-27 | 2021-03-12 | 合肥乐凯科技产业有限公司 | 一种高挺度聚酯薄膜 |
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| US6914120B2 (en) * | 2002-11-13 | 2005-07-05 | Eastman Chemical Company | Method for making isosorbide containing polyesters |
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| US20040121116A1 (en) | 2004-06-24 |
| JP2006511736A (ja) | 2006-04-06 |
| KR20050083574A (ko) | 2005-08-26 |
| US7052764B2 (en) | 2006-05-30 |
| MXPA04012509A (es) | 2005-02-17 |
| EP1573099B1 (en) | 2012-01-04 |
| WO2004061174A1 (en) | 2004-07-22 |
| KR101042436B1 (ko) | 2011-06-16 |
| CN1675418A (zh) | 2005-09-28 |
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