4 6 0 5 0 2 A7 _B7 五、發明説明（1 ) 經濟部中央標準局員工消費合作社印衮 ----------#-------II {請先閲讀背面之注意事項异从寫本頁) 一般合成改質聚酯的製程方法，依原料不同可區分為 對苯二甲酸製程(TPA process)和對苯二甲睃二甲酯製程 (DMT process)·^，而所謂對篆二甲酸裝程是以對苯二甲 S^terephthalic acid)、乙二醇[ethylene glycol)和共單趙(如 雙酸、雙酯、雙酸酐、雙醇、聚醚醇、雙酸硫磺酸鹽等等） 經酯化或酯交換反應、聚縮合瓦應合成或由對苯二甲酸和 乙二醇經酯化反應合成中間體對苯二甲酸二乙基醋 (BHET ;bis(hydroxy ethoxyl) terephthalate)後，再加入共單 體經酯化或酯交換反應、聚縮合反應合成改質聚酯。而對 苯二甲酸二甲酯製程指是以對苯二甲酸二甲酯、乙二醇和 共單體經酯交換反應或酯化反應、〉聚縮合反應合成改質聚 酯或以對苯二甲酸二甲酯和乙二醇經酯交換反應合成中間 BHET後，再加入共單體經由g旨化反應或酯交換反應、聚 縮合反應合成改質聚酯。本發明之新穎合成改質聚酯製程 為以聚對苯二曱酸二乙醋(ΡΕΤ ;ρ 〇 lyethylene terephthalate) 和共單鳢為原料，經由熱裂解(thermal degradation)酯化反 應或酯交換反應、聚縮合反應合成改質聚酯。 本發明所合成改質聚酯可以當複合紡絲時之熱驗水溶 液可溶聚酯用，如鞘蕊型複絲之蕊材料，海島型超細 纖維之海材料用，其中複合紡絲的產品中是以仿麂皮、仿 蠢絲、仿桃皮、仿玫瑰瓣等等產品皆用到熱弱鹹水溶液可 溶性聚酯。 從專利文獻整理得一般合成改質聚酯的方法有對苯二 本紙張从i4财關家料（CNS ) Α4· ( 21()：<297公楚） ' 605 02 五、發明説明（2 ) " -- 2製=苯二甲酸二甲瞇程二種糊文獻中以 對苯二甲酸製程合成改質聚轉利說明有⑴特開昭… 33419跡特開昭63-273634齡開說明以對苯二甲酸、 間苯二甲酸（isG_ie add)、3 5.二（甲氧_苯碟翻 (SIPM ； sodium salt of 3,5-di (carbomethoxy) benzene sulfonic acid)和乙二醇為原料合成改質聚酯（熱弱鹹水溶 液可溶性聚醋），(2)棚平9,273G29號公開制以對苯二 甲酸、乙二醇和3,5-二（阱織乙氧基羰勘苯礦酸納 (SIPE ^sodium salt of 3,5-di(beta-hydroxy ethoxycarbonyl) benzene sulfonic acid)為原料合成改質聚輯熱弱蜮水溶液 可溶性聚§§ ’(3)特開平7-258922號公開說明以對苯二甲 酸、間苯二甲酸、間苯二甲酸確酸鈉（SIPA :5 _s〇dium sulfoisophthalic acid)和乙二醇為料合成改質聚醋(熱弱鹹 水溶液可溶液性聚醋），(4)特開平7-316977號公開說明以 對苯二甲酸、間苯二甲酸續酸納、聚乙醇（polyethylene glycol ’分子量為2,000)和乙二醇為原料合成改質聚酯後， 與聚對苯二甲酸二乙酯混練，紡中空絲後，可用鹹性水溶 液水煮溶出改質聚酯，（5)特鄕召6 3-159520號公開說明以 對苯二甲酸、間苯二甲酸續酸納、聚乙醇（分子量400至 6,000)和乙二醇為原料合成改質聚酯（熱弱鹹水溶液可溶 性聚蝎，(6)特開平4- 327209號公開說明以對苯二甲酸、 間苯二甲酸、間苯二甲酸磺酸納、1 ,4-環已烷二酸（1,4-cyclohexane dicarloxylicacid) 和p 二醇為原料合成改 質聚醋 I ----^------.訂 (請先閲讀背面之注意事項/"'寫本頁) 本紙法尺度適用t國國家標準（CNS )以規格（2IOX297公釐） 經濟部中央橾準局員工消費合作社印製 605 02 A7 __ B7 五、發明説明（3 ) (熱弱鹹水溶液可溶性聚酯）。另外，以對苯二甲酸二甲 酯製程合成改質聚酯之專利說明書有(1)特公昭58-39926 號專利說明書指出以對苯二甲酸二甲醋-3,5-二（甲氧羰 基）笨磺酸鈉和乙二醇為原料合成改質聚_(熱弱械水溶 液可溶性聚_，(2)美國專利第4,361,617號專利說明書指 出以對苯二甲酸二甲酯、3,5-二（甲氧羰基）苯磺酸鈉、 磷酸酯和乙二醇為原料合成改質聚酯，其改質聚酯與聚對 苯二甲酸二乙酯混練後，紡中空絲，用鹹性水溶液水煮後， 可溶出改質聚酯’(3)特開昭61-231，221號公開說明以對苯 二甲酸二甲酯、3,5-二（甲氧織）苯確酸納、聚乙醇（分 子量20,000 )和乙二醇為原剩合成改質聚酯，與聚對苯二 甲酸二乙酯混練後，紡中空絲’用鹹性水溶液水煮後，可 溶出改質聚酯，（4)特開平4·361，695號公開說明以對苯二 甲酸一甲醋、間苯一甲酸二甲醋（dimethyl isophthalate)、 3,5-二（甲氧羰基）苯碟酸納和乙二醇為原料合成改質聚 酯（熱弱鹹水溶液可溶性聚酯），（5)特公昭63-256,619號 和特公昭63-152,624號專利說明書指出以對苯二甲酸二甲 酯、聚乙醇、間苯二甲酸、3,5-二（甲氧羰基）苯礦酸納、 3〜20個破之雙酸酯或3〜30碳之雙酐（CVC2{>dialkyal carboxylate or anhydride)勤〜20個後之雙酸和乙二醇合成 改質聚職熱弱鹹水溶液可溶性聚酯 >從^述專利文獻整 理得知沒有人以對聚對苯二甲酸二乙雖和共單禮為原料合 成改質聚酯。 5 a ---------^------:ΐτ------.^ C請先閲讀背面之注意事1^-?.填寫本頁) 本紙張尺度通用中國國家標準（CNS ) A4現格（210X 297公釐） 五、發明説明（4 ) 本發明製程主要是以聚對苯二甲酸二乙酯和共單體（如 雙酸、雙酯、雙酸酐、雙醇、聚醚醇、雙酸磺酸鹽、雙酯 磺酸鹽等等）為原料，經加熱容融，抽真空進行聚缩合反 應i^olycondensation )合成改質聚酯。 本發明製程中加熱熔融後開姆*低真空反應其反應溫 度為200〜290。〇，經過一段時^後，進行抽高真空聚縮合 反應（真空度低於4 torr )。 經濟部中央標隼局員工消費合作杜中製 (請先聞讀背面之注意事項及¾本頁) 本發明所提到之(1)雙酸可以為間苯二甲酸、鄰苯二甲 酸、1，4-環己烧二甲酸(1,4-cyclohexane dicarboxylic acid)、 己二酸(adipic acid )、2,6-幾$，6-naphthene dicarboxylic acid )等等’（2)雙酯可以為間苯二甲酸二甲酯、鄰苯二甲 酸二甲酯、1,4-環己烷二甲酸二甲酯、己二酸二甲只酯、1，6_ 環己烷二酸二甲酯等等，（3) 可以為鄰苯二甲酸射等 等’（4)雙醇可以為二乙二醇（diethylene glycol )、3 ,5 -環己 烧二酸續酸納（sodium salt of 3,5-cyclohexane dicarboxylic acid-4-sulfonic acid )、三乙二g|[triethylene glycol)、1，4-環 己二醇（1，4-cyclohexanedimethanol)、丙二酵、2·甲基·1，5-戊二醇、新戊二醇、苯二甲醇Ocylene glycol)等等，（5) 聚鍵醇（polyol )可以為聚乙醇、聚丙醇（polypropylene glycol )、聚丁醇 ^>〇lytetramethylene glycol)，或共聚合物 等等，(6)雙酸續酸鹽可以為間苯二甲酸續酸鈉、間苯二甲 睃績酸鉀、間苯二甲酸磺酸鋰、間苯二甲睃項酸鎮、2,6- 環院己二酸r 4-磧酸納（s〇dium salt of 2,6-dicarboxylic acid- ^_ 6 本紙ft,足度適用中國國家標準（CNS ) A4規格（210X297公釐) 經濟部中央標隼局員工消費合作社印製 10 5 0 2 A7 ____B7 五、發明説明（5) naphlhalenelsummicacid )轉 <7)雙酯磺酸鹽可以為3 5-二（甲氧幾基）苯磺酸鈉、3,5-二（甲氧羰基）苯磺酸鉀、 3.5- 二（甲氧羰基）苯磺酸趣、ϋ二（甲氧羰基）苯績酸 鎂、3,5-二（間· &基乙氧基幾基）苯磺酸納、3,5-二（阱 羥基乙氧基羰基）苯續酸鉀、3,5-二（間羥基乙氧基羰基） 苯續酸裡、3,5-二（間羥基乙氡基羰基）苯磺酸鎂、3,5-二（間經基乙氧基幾基）苯嶙酸四丁基爾tetrabutyl phosphonium 3,5-di (beta-hydroxyethoxycarbonyl) benzene sulfonate]、3,5-二（甲氧羰基）笨磺酸磷酸《四丁基酯 [tetrabutyl phosphonium 3,5-di (carbomethoxy) benzen sulfonate ]、3,5-二（甲氧羰基）環己烷磺酸辦50(1丨腿salt of 3.5- dicarbonmethoxycyclolhexane sulfonic acid)、3，5-二（間 -經基乙氧基幾基）環己烧續酸納[sodium salt of 3,5-di (beta-hydroxyethoxycarbonyl) cyclohexane sulfonic acid]3 ,5-二（甲氧羰基）環己烷磺酸碟酸:四丁基酯[tetrabutyl phosphonium 3,5-bi (carbomethoxy) cyclohexane sulfonate] ' 3,5·二（間《羥基乙氧基羧基）環己烷磺酸磷痊四丁基酯 [tetrabutylphosphonium 3,5-di (beta-hydroxyethoxycarbonyl) cyclohexane sulfonate]等等。 本發明製程所用觸媒可以為銻系化合物(如三氧化二 録、狻録第，系化合樹如二丁基亞錫0 ibudyltin oxide)、 丁基二月桂錫（dibutyl dilauryl tin)等等I，鈦化合物[如四 丁基執 tetrabutyl titanate)、®異稟基鐵 tetraisopropyl 7 I^-------訂------^ (請先閲讀背面之注意事項V填寫本頁) 本紙張尺度適用中國国家標準（CNS ) A4規格（210X297公釐） 經濟部中央揉準局貝工消费合作社印製 五、發明説明（6) titanate )等笱為聚縮合解煤，也可以和醋酸納、醋酸卸、 醏酸鈣、醋酸鎂、醋酸錳、g鈷、醋酸辞、醋酸鉛等等 合用。 本發明製程可以使甩安定劑，如三甲基鱗酸醋(t rimethyl phosphate )，三苯基磷酸酯（triphenyl phosphate)_ 酸、4 6 0 5 0 2 A7 _B7 V. Description of the invention (1) Seal of the Consumer Cooperative of Employees of the Central Standards Bureau of the Ministry of Economic Affairs ------------ # ------- II {Please read the first (Notes are different from this page) The general synthetic polyester method can be divided into terephthalic acid process (TPA process) and terephthalate dimethyl process (DMT process) according to different raw materials. The so-called terephthalic acid loading process is based on terephthalic acid), ethylene glycol, and co-monazine (such as bisacid, diester, dianhydride, bishydric alcohol, polyether alcohol, and diethylene glycol). Acid sulfur sulfonate, etc.) After esterification or transesterification, polycondensation tiles should be synthesized or from terephthalic acid and ethylene glycol through esterification to synthesize the intermediate diethyl phthalate (BHET; bis ( After hydroxy ethoxyl) terephthalate), co-monomers are added to undergo esterification or transesterification, and polycondensation to synthesize modified polyester. The process of dimethyl terephthalate refers to the conversion of modified polyester or terephthalic acid by dimethyl terephthalate, ethylene glycol and comonomer through transesterification or esterification reaction, polycondensation reaction. After the dimethyl ester and ethylene glycol are transesterified to synthesize intermediate BHET, co-monomers are added to synthesize modified polyesters through g purification reaction, transesterification reaction, and polycondensation reaction. The novel synthetically modified polyester process of the present invention is based on the use of polyethylene terephthalate (PET) and co-monofluorene as raw materials through thermal degradation (esterification or transesterification). 2. Polycondensation reaction synthesizes modified polyester. The modified polyester synthesized by the present invention can be used as an aqueous solution soluble polyester for composite spinning, such as sheath core multifilament core material, sea-island type ultrafine fiber sea material, among which composite spinning products In the case of suede-like, dumb silk, peach-peel, rose-petal and the like, hot and weak saline solution soluble polyester is used. The general method for synthesizing modified polyester from the patent literature is terephthalate paper from i4 Finance House Materials (CNS) A4 · (21 (): < 297 Gongchu) '605 02 V. Description of the invention (2 ) "-2 system = dimethyl phthalate process two kinds of paste in the literature to the terephthalic acid process synthesis of modified modified poly conversion is described in Japanese Patent Application No. 33419, Japanese Patent Application No. 63-273634 Made from terephthalic acid, isophthalic acid (isG_ie add), 3 5. di (methoxy benzene benzoate (SIPM; sodium salt of 3,5-di (carbomethoxy) benzene sulfonic acid) and ethylene glycol as raw materials Synthesis of modified polyester (heat-weak salty water-soluble polyacetate), (2) No. 9,273G29 publicly produced with terephthalic acid, ethylene glycol and 3,5-bis Sodium (SIPE ^ sodium salt of 3,5-di (beta-hydroxy ethoxycarbonyl) benzene sulfonic acid) is used as a raw material to synthesize modified heat-weak rhenium aqueous solution soluble polymer §§ '(3) JP 7-258922 Synthesis of modified terephthalic acid, isophthalic acid, sodium isophthalate (SIPA: 5 _s〇dium sulfoisophthalic acid) and ethylene glycol (Soluble polyacetic acid with hot and weak saline solution), (4) Japanese Unexamined Patent Publication No. 7-316977 discloses terephthalic acid, sodium isophthalate, polyethylene glycol (polyethylene glycol 'molecular weight is 2,000), and ethylene glycol. After the modified polyester is synthesized with alcohol as raw material, it is mixed with polyethylene terephthalate. After spinning the hollow fiber, the modified polyester can be boiled out with a salty aqueous solution. (5) JP 6 3-159520 Publication Description Synthetic modified polyester (heat-weak saline solution-soluble polyscorpion) using terephthalic acid, sodium isophthalate, polyalcohol (molecular weight 400 to 6,000) and ethylene glycol as raw materials ((6) JP-A 4- Publication No. 327209 describes synthesis of modified polymers using terephthalic acid, isophthalic acid, sodium isophthalate sulfonate, 1,4-cyclohexane dicarloxylicacid, and p-diol as raw materials. Vinegar I ---- ^ ------. Order (please read the precautions on the back / " write this page) The paper method scale is applicable to the national standard (CNS) to the specification (2IOX297 mm) Economy Printed by the Central Consumers ’Association of the Ministry of Labor and Consumer Cooperatives 605 02 A7 __ B7 V. Description of the invention (3) (Solubility of hot and weak saline solution) Polyester). In addition, the patent specifications for the synthesis of modified polyesters using the dimethyl terephthalate process include (1) Japanese Patent Publication No. 58-39926, which states that dimethyl terephthalate-3,5-di (Methoxycarbonyl) Sodium benzylsulfonate and ethylene glycol are used as raw materials to synthesize modified poly- (heat-weak mechanical aqueous solution soluble poly-), (2) US Patent No. 4,361,617 patent specification states that dimethyl terephthalate, 3 Modified polyester was synthesized from sodium 5-di (methoxycarbonyl) benzenesulfonate, phosphate and ethylene glycol as raw materials. The modified polyester was mixed with polyethylene terephthalate, and the hollow fiber was spun with After boiling in a salty aqueous solution, soluble modified polyester '(3) JP-A-61-231,221 is published to disclose dimethyl terephthalate and 3,5-bis (methoxytriphenyl) benzoic acid Sodium, polyethanol (molecular weight 20,000) and ethylene glycol are the original synthetic modified polyester. After kneading with polyethylene terephthalate, the hollow fiber is spun with a salty aqueous solution and the modified polymer can be dissolved out. Esters, (4) JP-A-4,361,695 discloses that methyl terephthalate, dimethyl isophthalate, dimethyl isophthalate, 3,5 -Synthesis of modified polyester (sodium hydroxide solution soluble in hot and weak saline) as raw materials of sodium bis (methoxycarbonyl) benzoate and ethylene glycol, (5) Patent Publication No. 63-256,619 and Patent Publication No. 63-152,624 Point out dimethyl terephthalate, polyethanol, isophthalic acid, sodium 3,5-bis (methoxycarbonyl) benzoate, 3 to 20 diacids or 3 to 30 carbon dianhydrides (CVC2 {> dialkyal carboxylate or anhydride) ~ 20 di-acid and ethylene glycol synthesis modified polymer hot and weak saline solution soluble polyester > It is known from the patent document collation that no one Although diethyl phthalate is used as a raw material to synthesize modified polyester. 5 a --------- ^ ------: ΐτ ------. ^ C Please read the notes on the back 1 ^-?. Fill in this page) This paper size is common in China National Standard (CNS) A4 is now available (210X 297 mm) 5. Description of the invention (4) The process of the present invention is mainly based on polyethylene terephthalate and comonomers (such as bisacid, diester, dianhydride, Diol, polyether alcohol, diacid sulfonate, diester sulfonate, etc.) are used as raw materials, and the polycondensation reaction (i ^ olycondensation) is carried out after heating and melting, and the modified polyester is synthesized. In the process of the present invention, the reaction temperature of the kelvin * low-vacuum reaction after heating and melting is 200-290. 〇 After a certain period of time, a high vacuum polycondensation reaction (vacuum degree is less than 4 torr) is performed. The consumption cooperation of employees of the Central Bureau of Standards, Ministry of Economic Affairs, Du Zhong system (please read the precautions on the back and this page first) The (1) bisacid mentioned in the present invention can be isophthalic acid, phthalic acid, 1 1,4-cyclohexane dicarboxylic acid, adipic acid, 2,6-naphthene dicarboxylic acid, etc. '(2) diesters can be Dimethyl phthalate, dimethyl phthalate, dimethyl 1,4-cyclohexanedicarboxylate, dimethyl adipate, dimethyl 1,6-cyclohexanedicarboxylate, etc., (3) It can be phthalic acid, etc. '(4) The bisol can be diethylene glycol, 3,5-cyclohexanane diacid sodium salt (sodium salt of 3,5-cyclohexane dicarboxylic acid-4-sulfonic acid), triethylene g | [triethylene glycol), 1,4-cyclohexanedimethanol, malonase, 2 · methyl · 1,5-pentane Alcohol, neopentyl glycol, xylene glycol), etc. (5) The polyol can be polyethanol, polypropylene glycol, polybutanol ^ > 〇lytetramethylene glycol), Copolymers, etc. (6) The diacid salts can be sodium isophthalate, potassium isophthalate, lithium isophthalate sulfonate, isophthalate, Sodium salt of 2,6-dicarboxylic acid- ^ _ 6 paper ft, 2-6-dicarboxylic acid a 4-dicarboxylic acid, sufficient to the Chinese National Standard (CNS) A4 specification (210X297 mm) Printed by the Consumers' Cooperative of the Central Bureau of Standards of the Ministry of Economic Affairs 10 5 0 2 A7 ____B7 V. Description of the invention (5) naphlhalenelsummicacid) Transform < 7) The diester sulfonate can be 3 5-bis (methoxyisopropyl) benzenesulfonate Sodium, 3,5-Di (methoxycarbonyl) benzenesulfonate, 3.5-Di (methoxycarbonyl) benzenesulfonate, Magnesium bis (methoxycarbonyl) benzoate, 3,5-Di (methane) · &Amp; Isoethoxyquinyl) benzene sulfonate, 3,5-bis (trap hydroxyethoxycarbonyl) benzoic acid potassium, 3,5-bis (m-hydroxyethoxycarbonyl) benzoic acid , 3,5-Di (m-hydroxyethylfluorenylcarbonyl) benzene sulfonate, 3,5-Di (m-Crysthoxyethoxy) yl tetrabutyl phosphonium tetrabutyl phosphonium 3,5-di (beta -hydroxyethoxycarbonyl) benzene sulfonate], 3,5-bis (methoxy Tetrabenzyl sulfonate [tetrabutyl phosphonium 3,5-di (carbomethoxy) benzen sulfonate], 3,5-di (methoxycarbonyl) cyclohexanesulfonic acid office 50 (1 丨 salt of 3.5 -dicarbonmethoxycyclolhexane sulfonic acid), 3,5-di Di (methoxycarbonyl) cyclohexanesulfonic acid: tetrabutyl phosphonium 3,5-bi (carbomethoxy) cyclohexane sulfonate] '3,5 · bis (m-hydroxyethoxycarboxy) cyclohexane Tetrabutylphosphonium 3,5-di (beta-hydroxyethoxycarbonyl) cyclohexane sulfonate and so on. The catalyst used in the process of the present invention may be an antimony-based compound (such as dioxo trioxide, dioxin, a compound tree such as dibutyltin oxide), dibutyl dilauryl tin, etc. Titanium compounds (such as tetrabutyl titanate), ® isofluorenyl iron tetraisopropyl 7 I ^ ------- Order ------ ^ (Please read the precautions on the back first and fill out this page) This Paper size applies Chinese National Standard (CNS) A4 specification (210X297 mm) Printed by the Central Government Bureau of the Ministry of Economic Affairs, Printed by Shellfish Consumer Cooperative, V. Description of Invention (6) titanate, etc. It can be used for polycondensation to dissolve coal, and can also be used with sodium acetate , Acetic acid unloading, calcium acetate, magnesium acetate, manganese acetate, g cobalt, acetate, lead acetate, etc. In the process of the present invention, stabilizers such as trimethyl phosphate, triphenyl phosphate, acid,
Irganoxl〇l〇 等等。 兹舉數個實施例說明如下，所舉實施例僅係對本發明 方法作概括性例示，並無限制衣發明範圍之意，就此先作 聲明。 實施例 將反應物（組成用量見表1 )放入反應槽内，開始昇溫 及擾拌’當反應槽内溫昇至230。〇附近，便開始抽真，其 真空度每隔6分鐘往下調i〇cmjjg直到真空度達76cmHg (76 cmHg為高真空度，〇 cmHg 大氣壓y時，開始 使用馬力較大之馬達抽高真空，此時反應槽内溫度約26〇 C附近，維持正常合成聚對苯二甲酸二乙酯之反應溫度至 攪拌阻力上昇至某一定值後（見表丨之數據)，使用氮氣 破真空，加壓下料，所得樣品分杆如下表(表丨）。本合成 使用觸煤為二氧化二鐵醋酸敏醋酸幹醋酸鈉（3 〇〇ppm /200PPm /200pPm /200pPm )，若有外加雙酸時，需加入2 莫耳數之乙二醇用量。 (1)Ι·ν·減測試方法 本紙張尺度逍用中國困家標準（CNS ) Α4規格（2r〇X29Ti^"y---- .—-I ^^1 - - I....... - - I HI - I 1*衣 I — II - :- I n (請先閲讀背面之注意事項再填寫本頁) ^0502 A7 五、發明説明（7) 以四氣乙烷/苯紛重量比40/60為溶劑唭中配製樣品 濃度為0.5g/dl、0.33g/dl O.213g/dlii〇.215g/dl， 於3 0 °C下，使甩Cannon-150型黏度管測樣品溶液流過 黏度管時間，經過計算及作圖求得I.V.質。 (2)熱弱蜮水性溶液測試水溶性 測試條件為100 t，水煮1 4畴氧化鈉水溶液 濃度20 g /!)，稱原來樣品重（w。），在氫氧化鈉水溶 液水煮一個小時後之重量(Ws球得CWVWdW/100 %值’為在氫氧化納水溶液水煮後重量減輕之百分比 (可溶解量百分比），測量氫氧化納水煮後重量減輕之 樣品為粉碎後之樣品。 ----------士衣------，訂 (請先聞讀背面之注意事項再¥寫本頁) 經濟部中央標準局員工消費合作社印製 本紙張尺度適用中吨家梯準（CNS) A4規格（2丨Gx 297公楚） ^ 60502 A7 B7 五、發明説明（8) 表1_合成改質聚酯之組成，扭力上昇格數，I.V·及氫 _氧化納水溶液水煮後重量減少百分比 趙濟部中央櫺準局負工消费合作社印製 編號 組成（莫耳比） 反應 内溫 扭力 上昇 格數 I.V -—--- 氫氧化 鈉 減量百 分比 01 BHET/SIPE(100/10) 278°C 7 0.30 63% 02 PET/SIPE(100/10) 279〇C 7 0.40 80% 03 PET/SIPE/IPA(100/10/7) 287〇C 6 0.37 全溶 04 PET/SIPA/IPA(100/10/7) 287〇C 6 0.36 全溶 05 PET/SIPM/IPA(100/10/7) 287〇C 6 0.38 全溶 06 PET/SIPE/PEG- 1,000(100/10/1) 277°C l_ 7 0.41 85% 07 PET/SIPE/AA(100/10/7) 277°C 7 0.43 82% 08 PET/SIPE/IPA/DEG(100/10/7 /1) 283°C 7 0.42 全溶 09 PET/SIPE/DEG(100/10/1) 278°C 7 0.39 83% 10 PET/BSIPE/DEG(100/10/7) 283°C 7 0.47 全溶 11 PET/BSIPE(100/10) 278°C 7 — 0.45 78% 12 PET/SIPE/CHDA(100/10/7) 278°C 6 0.42 全溶 13 BHET/SIPE/IPA(100/10/7) 287°C 6 0.33 全溶 10 ----------裝------訂一------,Α * (請先閲讀背面之注意事項-ίε'填寫本頁) . 本紙張尺度適用中國國家標準（CMS ) Α4规格（2IOX29?公釐） A7 460502 五'發明説明（9) 備註： (1) BHET是用對苯二甲酸/乙二醇(莫耳比為1/1·3)經由 酯化反應合成，反應溫度為250 °C，酯化反應程度為 95%以上。 (2) SIPE為3,5-二(間羥基乙氧基羰基)苯續酸鈉之二乙 二醇溶液(40%)。 (3) PET為聚對苯二曱酸二乙酯，以苯紛/四氣乙烧(重量 比為3/2)為溶劑，30°C測得其I.V.為0.64，其莫耳數 為樣品重量除以聚對苯二甲酸二乙酯重覆單位之重量 為莫耳數。 (4) IPA為間苯二甲酸。 (5) SIPA為間苯二甲酸磺酸鈉。 ⑹SIPM為3,5_二(甲氧羰基)苯礦酸鈉。 ⑺PEG-1，000為聚乙醇，分子量為1，000。 (8) DEG為二乙二醇。 (9) BSIPE為3,5(-二(間-羥基乙氧基羰基)苯磺酸磷酸-四 丁酯。 (10) CHDA為1,4-環已烷二甲酸。 I I —二· I —ft I : _ n I— - -1— ·- - -1 Ji - II Τ» > J J 、T (請先閲讀背面之注意事項再禎寫本頁) 經濟部中央標準局員工消f合作社印製 本紙張尺度適用t國囷家標準（CNS ) A4規格（210X297公釐）Irganox10l0 and so on. Several examples are described below. The examples are merely general illustrations of the method of the present invention, and are not intended to limit the scope of the invention. Example The reactants (see Table 1 for the composition and dosage) were placed in a reaction tank, and the temperature was raised and stirred. When the temperature in the reaction tank rose to 230. Near 〇, it began to pump, and its vacuum degree was adjusted down every 6 minutes until the vacuum reached 76 cmHg (76 cmHg is high vacuum, 〇cmHg atmospheric pressure y, began to use a higher horsepower motor to pump high vacuum, At this time, the temperature in the reaction tank is about 26 ° C. After maintaining the normal reaction temperature for the synthesis of polyethylene terephthalate until the stirring resistance rises to a certain value (see the data in Table 丨), use nitrogen to break the vacuum and pressurize. The sample is divided as shown in the following table (Table 丨). This synthesis uses ferrous dioxide, ferric oxide, acetic acid, and dry sodium acetate (300 ppm / 200PPm / 200pPm / 200pPm). If bisacid is added, Need to add 2 moles of ethylene glycol. (1) Ι · ν · minus test method The paper size is in accordance with China Standards (CNS) Α4 specification (2r〇X29Ti ^ " y ----.— -I ^^ 1--I .......--I HI-I 1 * 衣 I — II-:-I n (Please read the precautions on the back before filling this page) ^ 0502 A7 V. Description of the invention (7) A sample concentration of 0.5 g / dl, 0.33 g / dl, O.213 g / dlii, and 215 g / dl was prepared in a solvent having a weight ratio of 40/60 of tetragas ethane / benzene as a solvent. Cannon-150 viscosity tube test sample solution flowing through the viscosity tube time at 30 ° C, calculated and graphed to obtain the quality of IV. (2) heat and weak water solution test for water solubility test conditions of 100 t, The concentration of boiled 1 4 domain sodium hydroxide aqueous solution is 20 g /!), The original sample weight (w.) Is weighed, and the weight of the sodium hydroxide aqueous solution after boiling for one hour (Ws ball gets CWVWdW / 100% value 'is in the hydroxide Percentage of weight loss of sodium hydroxide solution after boiling (% of soluble amount), the weight loss of sodium hydroxide solution after boiling is measured as crushed sample. ---------- Shiyi ----- -, Order (please read the precautions on the back before writing this page) The paper size printed by the Employees' Cooperatives of the Central Bureau of Standards of the Ministry of Economic Affairs applies to the paper size of CNS A4 (2 丨 Gx 297) ^ 60502 A7 B7 V. Description of the invention (8) Table 1_ Composition of synthetic modified polyester, torque increase number, IV · and hydrogen_sodium oxide aqueous solution weight reduction percentage after boiled Printed number composition (Morr ratio) Response to internal temperature torque rise grid number IV ------ Percent reduction of sodium oxide 01 BHET / SIPE (100/10) 278 ° C 7 0.30 63% 02 PET / SIPE (100/10) 279〇C 7 0.40 80% 03 PET / SIPE / IPA (100/10/7) 287 〇C 6 0.37 fully soluble 04 PET / SIPA / IPA (100/10/7) 287〇C 6 0.36 fully soluble 05 PET / SIPM / IPA (100/10/7) 287〇C 6 0.38 fully soluble 06 PET / SIPE / PEG- 1,000 (100/10/1) 277 ° C l_ 7 0.41 85% 07 PET / SIPE / AA (100/10/7) 277 ° C 7 0.43 82% 08 PET / SIPE / IPA / DEG (100 / 10/7 / 1) 283 ° C 7 0.42 fully soluble 09 PET / SIPE / DEG (100/10/1) 278 ° C 7 0.39 83% 10 PET / BSIPE / DEG (100/10/7) 283 ° C 7 0.47 Fully soluble 11 PET / BSIPE (100/10) 278 ° C 7 — 0.45 78% 12 PET / SIPE / CHDA (100/10/7) 278 ° C 6 0.42 Fully soluble 13 BHET / SIPE / IPA (100/10 / 7) 287 ° C 6 0.33 Total solution 10 ---------- installation ------ order one ------, Α * (Please read the precautions on the back-ίε ' (Fill in this page). This paper size applies Chinese National Standard (CMS) A4 specification (2IOX29? Mm) A7 460502 Five 'invention description (9) Remarks: (1) BHET is using terephthalic acid / ethylene glycol (Mo Ear ratio is 1/1 · 3) synthesized by esterification reaction, the reaction temperature is 250 ° C, and the degree of esterification reaction is 95% On. (2) SIPE is a diethylene glycol solution (40%) of sodium 3,5-bis (m-hydroxyethoxycarbonyl) benzoate. (3) PET is diethyl terephthalate, benzene / tetrakis (3/2 weight ratio) is used as the solvent, the IV measured at 30 ° C is 0.64, and the mole number is the sample The weight divided by the weight of the polyethylene terephthalate repeating unit is the number of moles. (4) IPA is isophthalic acid. (5) SIPA is sodium isophthalate. ⑹SIPM is 3,5_bis (methoxycarbonyl) sodium benzoate. ⑺PEG-1,000 is polyethanol and has a molecular weight of 1,000. (8) DEG is diethylene glycol. (9) BSIPE is 3,5 (-bis (m-hydroxyethoxycarbonyl) benzenesulfonic acid phosphate-tetrabutyl ester. (10) CHDA is 1,4-cyclohexanedicarboxylic acid. II —Di · I — ft I: _ n I—--1— ·---1 Ji-II Τ »> JJ 、 T (Please read the notes on the back before writing this page) Staff of the Central Standards Bureau of the Ministry of Economic Affairs and the cooperative seal The paper size of the paper is applicable to the National Standard (CNS) A4 (210X297 mm)