201024347 六、發明說明： 【發明所屬之技術領域】 本發明有關一種可塑劑組成物，尤其有關一種聚乙烯縮丁醛 之可塑劑組成物。 【先前技術】 典型之聚乙烯縮丁醒·薄膜可藉可塑劑而提供另人滿意之機械 性質、接著性質、封裝性質及_膜加工性。因而聚乙烯縮丁酿 廣泛用於製造膠合玻璃而可應用於汽車工業領域、建築領域以及 太陽能電池領域。 ’、 ❿ 聚乙烯縮丁藤薄膜用之可塑劑除能提供聚乙稀縮丁搭作為膠 ====性及安全性外，尚_與聚乙稀縮丁 因為她佳之可塑劑，以避免加工後 會厭 =移行性對聚乙稀縮丁藤薄膜耐久性影響甚 該特疋範ϋ外’則無法與太多可塑劑 θ ，膜ΐ溫揮發性高故不具耐久性，當可塑劑 衝擊力量及兼顧耐久性能，相將無法消散外來 玻璃時，將對該膠合破璃產生不;:烯、造膠合 及耐，，為 聚乙烯縮猶之心含錯目*性、耐久性考量下，通常 於2wt%左右。 U艮制於某一特定小範圍内例如限定 __觸!_基含量 4 201024347 之聚乙烯縮丁搭之可塑劑，故而對用於聚乙浠縮丁搭之可塑劑進 行廣泛研究，發現藉由特定比例含有特定成份做為可塑劑，可克 服前述問題點，因而完成本發明。 【發明内容】 本發明第一目的係有關一種包括己二酸二(丁基二乙二醇)酯 及二-(2-乙基己酸)三乙二醇酯之可塑劑組成物，其中該己二酸二 (丁基二乙二醇）酯與該二_(2_乙基己酸)三乙二醇酯之重量比為 90 : 10〜1〇 : 90。 該己二酸二(丁基二乙二醇)g旨具有下列化學式：201024347 VI. Description of the Invention: [Technical Field] The present invention relates to a plasticizer composition, and more particularly to a plasticizer composition of polyvinyl butyral. [Prior Art] A typical polyethylene shrink film can provide a satisfactory mechanical property, a bonding property, a packaging property, and a film processability by a plasticizer. Therefore, polyethylene is widely used in the manufacture of glued glass and can be used in the automotive industry, construction, and solar cells. ', ❿ Polyethylene butyl vine film plasticizer in addition to providing polyethylene shrinking butyl as a glue ==== sex and safety, and _ with polyethylene butyl butyl because of its good plasticizer to avoid After processing, the epiglottis=migration effect on the durability of the polystyrene film is very difficult. It can't be too much with the plasticizer θ. The film is highly volatile and therefore not durable, when the plasticizer impacts the force. And when the durability is not enough, the phase will not dissipate the foreign glass, and the glue will not be produced; the olefin, the glue and the resistance, the polyethylene shrinks the heart, and the durability is usually considered. It is about 2wt%. U 艮 于 某一 某一 例如 例如 例如 例如 例如 例如 例如 例如 例如 _ _ _ 2010 2010 2010 2010 2010 2010 2010 2010 2010 2010 2010 2010 2010 2010 2010 2010 2010 2010 2010 2010 2010 2010 2010 2010 2010 2010 2010 2010 2010 2010 2010 2010 2010 2010 2010 The present invention can be accomplished by including a specific component as a plasticizer in a specific ratio to overcome the aforementioned problems. SUMMARY OF THE INVENTION A first object of the present invention relates to a plasticizer composition comprising di(butyl diethylene glycol) adipate and triethylene glycol di-(2-ethylhexanoate), wherein The weight ratio of di(butyl diethylene glycol) adipate to the di-(2-ethylhexanoic acid) triethylene glycol ester is 90: 10 to 1 〇: 90. The di(butyl diglycol) adipate g has the following chemical formula:
C4H9-(〇CH2CH2)2-〇-C(=0)-(CH2)4-C(=〇)-〇-(CH2CH2〇)2-C4H9 ； 及該二-(2-乙基己酸)三乙二醇酯具有下列化學式： C4H9-CH(C2H5)-C(=0)-O-(CH2CH20)3-C(=0)-CH(C2H5)-C4H9 ° 本發明之可塑劑組成物當使用作為聚乙烯縮丁路之可塑劑 時，與聚乙烯縮丁醛樹脂具有良好相容性，藉此可使所形成之聚 乙稀縮丁酸薄膜兼具優異的機械性質及低揮發性。 本發明第二目的係有關一種聚乙烯縮丁醛組成物，其包括100 重量份之聚乙烯縮丁醛及20至50重量份之上述之己二酸二(丁基 一乙二醇)酯及二-(2-乙基己酸)三乙二醇酯之可塑劑組成物；且其 中該己二酸二(丁基二乙二醇)酯與該二_(2_乙基己酸)三乙二 之重量比為90 : 10〜10 : 90。 曰 本發明之可塑劑組成物可適用的聚乙烯縮丁醛可具有15至 30 wt%之羥基含量，較好具有15至25加％之羥基含量且 18至23wt°/。之經基含量。 【實施方式】 本發明提供一種包括己二酸二(丁基二乙二醇)酯及二乙基 己酸)三乙二醇酯之可塑劑組成物，其中該己二酸二(丁基二乙二^ 酯與該二乙基己酸)三乙二醇酯之重量比為90 : 10〜10 : 90，鲂 好為30 : 70至70 : 30。 較 依據本發明’由於本發明之己二酸二(丁基二乙二醇)酯及二 (2乙基己酸)二乙二醇酯之可塑劑組成物與聚乙烯縮丁駿具有良 201024347 =谷性、低揮發性，因此當聚乙烯縮了贿基含量在 仍可獲得例如機顧度等雛優異之聚乙軸丁膜。 _丁酸之絲含量在15至3Gwt%之寬顧_，在使 用士發明之已二酸二(丁基二乙二醇)醋及二(2_乙基已酸)三乙二 物作為可_之下，仍可獲得優異機械強度及 间/ 皿低揮發性之聚乙烯縮丁齡薄膜。 本發明另提供-種聚乙烯縮丁路組成物，其包括1〇〇重量份 =乙1縮Τ献15至55重量份之本個之可_域物；其C4H9-(〇CH2CH2)2-〇-C(=0)-(CH2)4-C(=〇)-〇-(CH2CH2〇)2-C4H9; and the bis-(2-ethylhexanoic acid) III The ethylene glycol ester has the following chemical formula: C4H9-CH(C2H5)-C(=0)-O-(CH2CH20)3-C(=0)-CH(C2H5)-C4H9 ° The plasticizer composition of the present invention is used when When it is a plasticizer for polyethylene shrinkage, it has good compatibility with a polyvinyl butyral resin, whereby the formed polyethylene butyric acid film can have both excellent mechanical properties and low volatility. A second object of the present invention relates to a polyvinyl butyral composition comprising 100 parts by weight of polyvinyl butyral and 20 to 50 parts by weight of the above-mentioned di(butylmonoethylene glycol) adipate and a plasticizer composition of di-(2-ethylhexanoic acid) triethylene glycol ester; and wherein the di(butyl diethylene glycol) adipate and the bis(2-ethylhexanoic acid) tris The weight ratio of the second is 90: 10~10: 90.聚乙烯 The polyvinyl butyral to which the plasticizer composition of the present invention is applicable may have a hydroxyl group content of 15 to 30% by weight, preferably 15 to 25 % by weight of the hydroxyl group and 18 to 23 wt%. Base content. [Embodiment] The present invention provides a plasticizer composition comprising di(butyldiethylene glycol) adipate and triethylene glycol diethylhexanoate, wherein the adipic acid di(butyl) The weight ratio of the ethylenediester to the diethylhexanoic acid) triethylene glycol ester is 90:10 to 10:90, preferably 30:70 to 70:30. Compared with the plasticizer composition of the invention according to the invention of di(butyl diethylene glycol) adipate and di(ethylene dihexanoate) diethylene glycol ester, and the polyethylene shrinking has good 201024347 = gluten, low volatility, so when the polyethylene shrinks the bribe content, it can still obtain the excellent polytriene film such as the machine. _ butyl acid content of 15 to 3 Gwt% of the _, in the use of the invention of adipic acid di(butyl diethylene glycol) vinegar and bis (2-ethylhexanoic acid) triethylene two can be used Under the _, a polyethylene shrinkage film with excellent mechanical strength and low volatility between the dishes and the container is still obtained. The present invention further provides a polyvinyl condensate composition comprising 1 part by weight of a 5% by weight of the 5% of the conjugated material;
二(丁基二乙二醇)醋與二_(2_乙基己酸)三乙二醇醋混合 重置比為90:10至1〇:9〇，更好為7〇 : 3〇至7〇 : 3〇。 更好該聚乙烯縮丁醛組成物包括1〇〇重量份之聚乙烯縮丁醛 ^ 20至50重量份之本發明之可塑劑組成物；最好該聚乙稀縮丁 醛、且成物包括100重量份之聚乙稀縮丁搭及3〇至45重 發明之可塑劑組成物。 ^ 本發明中所用之聚乙婦縮丁醛之製備可在觸媒存在下使平均 聚合度約800至3000，較好平均聚合度約1〇〇〇至25〇〇之聚乙烯 醇與丁輯挪合反麟製得者，其為熟知本領域悉知者，因此 並不用以限制本發明之範圍。 上述方法所得之本發明中所用之聚乙烯縮丁醛之羥基含量為 15 至 30 wt%，較好 15 至 25 wt%，最好 18 至 23wt%。 本發明之聚乙烯縮丁醛組成物又可含有其他添加劑，該等添 加劑並無特別限制，只要對由該組成物所製成之薄膜性質無不利The replacement ratio of bis(butyl diethylene glycol) vinegar to bis(2-ethylhexanoic acid) triethylene glycol vinegar is 90:10 to 1〇:9〇, more preferably 7〇: 3〇 7〇: 3〇. More preferably, the polyvinyl butyral composition comprises 1 part by weight of polyvinyl butyral 20 to 50 parts by weight of the plasticizer composition of the present invention; preferably the poly(butyral), and the compound It comprises 100 parts by weight of a polyethylene condensed butadiene and a plastic composition of 3 to 45 weight invention. ^ The preparation of polybutylic aldehyde used in the present invention can be carried out in the presence of a catalyst to give an average degree of polymerization of from about 800 to 3,000, preferably having an average degree of polymerization of from about 1 to 25 Å. It is not known to limit the scope of the invention, which is known to those skilled in the art. The polyvinyl butyral used in the present invention obtained by the above method has a hydroxyl group content of 15 to 30% by weight, preferably 15 to 25 % by weight, preferably 18 to 23 % by weight. The polyvinyl butyral composition of the present invention may further contain other additives, and the additives are not particularly limited as long as they are not detrimental to the properties of the film made of the composition.
影響即可。其非限制具體例包含例如紫外線吸收劑如苯并三唑系 列、由 Ciba-Geigy 所製造銷售之 Tinuvin RTM 326、Tinuvin RTM 320'Tinuvin· RTM. 328;黏著控制劑如鹼金屬或鹼土金屬甲酸鹽、 乙酸鹽，例如甲酸鉀、乙酸鉀、曱酸鎂、乙酸鎂、甲酸鈉、乙酸 鈉等；抗氧化劑如長春石油化學生產之抗氧化劑A〇5〇及抗氧化劑 A060等；以及光安定劑等。 本發明將以下列實施例及比較例更詳細加以説明。惟該等實 施例僅用以說明本發明較佳具體樣態，而非用以限制本發明之範 6 201024347 -二ίϊί本技藝者將可藉由本發明之詳細說明及揭示而作各種 -等修飾及改質在不違離本發明精神及範圍内均屬 p - 下列實補及比較财，使用下列絲測定本發明之 之;Ϊ:Λ基 =乙二醇)醋、二_(2_乙基己酸)三乙二醇酯經混合後 製得ίίΐίί之物化特性及所得可塑劑與聚乙烯縮丁藤摻合後 ❹ 麻丨tbt霧點(相。容性）：使5·6克聚乙烯縮丁搭樹月旨溶於7〇克可塑 酿至150 C使形成澄清溶液後，慢慢冷卻並記錄溶液開始變 溫度’此溫度即為m點愈絲示兩種成分之相容性 田=、ϋ烯縮丁醛之羥基含量：使用ns K6728所述之方法測 置。在有蓋三角瓶中準確稱取0.4克聚乙烯縮丁酿，加入1〇毫 乙酸酐溶液。裝上回流冷凝管充分回流反應2小時，冷卻後 ΪΪΪ管上方加人2G毫升U_二氣乙烧，充分勝後加人5〇毫升 水並使其混合均勻，靜置3〇分鐘。滴加3滴龄酞指示劑以 此aOH、滴定至微紅色出現即為終點。記錄〇 5NNa〇H滴定毫 升數⑻。另進行空白試驗並記錄〇 5NNa〇H滴定毫升數⑼。以下 列計算式計算羥基含量： 經基 wt%=(b-a)，220.25/樣品重 其中 f 為 0.5N NaOH 因數(factor) 製備例1 :聚乙嫌·_丁释夕y備 將1000公斤聚合度17〇〇且皂化值為98.5 mole%之聚乙烯醇 加入9000升水中加熱溶解，使溶液冷卻至煎，加入115公斤 35 wt%舰及590公斤丁酸進行縮合反應，反應維持在耽直至 聚乙烯縮丁酸沉澱析出。然後升溫至6〇。〇。反應混合物在6〇。〇維 持3小時，攪拌使反應完全。聚乙烯縮丁醛沉澱物以去離子水洗 蘇後於乾聽巾乾燥，麟17 4wt%祕含量之聚乙烯縮丁路。 製備例2:聚乙締袍j酸之贺色 循實施例1之相同方法，但以550公斤之丁醛替代實例1之 7 201024347 丁醛量，獲得經得羥基含量為218加％之聚乙烯縮丁醛。 實施例1-12 使得自製備例1-2之聚乙烯丁縮醛5.6克分別與70克之可塑 劑摻合獲f掺合物，可塑劑為已二酸二(丁基二乙二醇)酯及二_(2_ 乙基己酸)二乙二醇酯以表1所示比例之混合物，接著進行摻合 之霧點測試’結果如表1所示。. 表1 成份的重量 聚乙烯縮丁醛 羥基含ί： Cwt%) 霧點°C 己二酸二(丁 基二乙二醇) 酯 二·0乙基己 酸)三乙二醇 酯 實施例1 100 0 17.4 47 實施例2 80 20 17.4 52 實施例3 60 40 17.4 60 實施例4 40 60 17.4 66 實施例5 20 80 17.4 78 實施例6 0 100 17.4 102 實施例7 100 0 21.8 85 實施例8 80 20 21.8 95 實施例9 60 40 21.8 102 貪施例10 40 60 21.8 108 實施例11 20 80 21.8 116 — 實施例12 0 100 21.8 135 比鮫例1-2 ❹ 使得自製備例1-2之聚乙烯丁縮醛5.6克分別與70克乙二酸 二己酯(DHA)可塑劑進行如上述之霧點測試，結果如表2所示。 表2 聚乙烯縮丁醛羥基含詈fwt%、 霧點°C 比較例1 17.4 128 比較例2 21.8 142 由表1及表2之結果顯示，本發明之己二酸二(丁基二乙二醇) 醋及二-2-乙基己酸三乙二醇酯可塑劑組成物與聚乙烯縮丁酿樹脂 之相容性優於DHA。相容性愈佳表示加工成薄膜後較不易產生相 分離而造成性質不良。 宜兹^13-17及東考例1 201024347 實施例13-17及參考例〗係使用製備例2所製得之聚乙烯縮丁 盤樹脂100重量份依序與實施例7_12所示重量百分比之可塑劑組 ‘ 成物(如表3) 38重量份於高強度混合機中混合。此已塑化之非均 ，聚乙烯縮丁醛混合物在押出機中熔化，並迫使熔融物通過形成 薄膜之模頭。熔融溫度約195t：，擠磨成約0.76毫米之聚乙烯縮 丁醛薄片。 *使所製得之聚乙烯縮丁醛薄片置入兩片平板玻璃間(3〇公分 長*30公分寬*3毫米寬）。使膠合玻璃置入橡膠袋中抽真空，真空 度20托耳維持10分鐘以去除空氣’維持真空度以5。(：/分鐘升溫 速率升溫至100。(：，冷卻後取出膠合玻璃。將膠合玻璃置高遷 中。高壓蚤溫度升溫至130ΐ，塵力升至13公斤/平 分鐘。高壓釜溫度冷卻至5(rc以下後罐而製成膠合玻璃成品。 口以下列方法測定聚乙烯縮丁醛薄膜之拉力強度、相容性、熱 重損失率。並町财法歌製紅膠合_之邊 ^ 及耐貫穿性職。結果如表4所示。The impact can be. Non-limiting examples thereof include, for example, ultraviolet absorbers such as benzotriazole series, Tinuvin RTM 326 manufactured by Ciba-Geigy, Tinuvin RTM 320'Tinuvin·RTM. 328; adhesion control agents such as alkali metal or alkaline earth metal formic acid Salt, acetate, such as potassium formate, potassium acetate, magnesium citrate, magnesium acetate, sodium formate, sodium acetate, etc.; antioxidants such as anti-oxidant A〇5〇 and antioxidant A060 produced by Changchun Petrochemical; and light stabilizers, etc. . The invention will be described in more detail in the following examples and comparative examples. The present invention is only intended to illustrate the preferred embodiment of the present invention, and is not intended to limit the scope of the present invention. The present invention can be modified by the detailed description and disclosure of the present invention. And the modification is in the spirit and scope of the present invention, and is the following p- the following practical and comparative wealth, and the following yarn is used to determine the present invention; Ϊ: thiol = ethylene glycol) vinegar, two _ (2_B After the mixture, the physicochemical properties of the triethylene glycol ester are obtained, and the obtained plasticizer is blended with the polyethylene butyl sulphate. The tbt fog point (phase. Capacitive): 5·6 g Ethylene condensate is dissolved in 7 gram of plastic and can be brewed to 150 C. After forming a clear solution, slowly cool and record the solution to start to change temperature. 'This temperature is m point. The silk shows the compatibility of the two components. =, hydroxyl content of terpene butyral: measured by the method described in ns K6728. Accurately weigh 0.4 g of polyethylene in a capped triangular flask and add 1 〇 milliacetic anhydride solution. The reflux condenser was installed and refluxed for 2 hours. After cooling, 2 g of U_2 gas was added to the top of the tube, and 5 liters of water was added to the mixture, and the mixture was uniformly mixed and allowed to stand for 3 minutes. The addition of 3 drops of the cockroach indicator to the end of the aOH, titration to reddish color is the end point. Record 〇 5NNa〇H titration in milliliters (8). A blank test was also performed and the number of milliliters (9) titrated by 〇 5NNa〇H was recorded. Calculate the hydroxyl content by the following formula: Base weight % = (ba), 220.25 / sample weight where f is 0.5 N NaOH factor (factor) Preparation Example 1: Polyethylene _ _ 释 释 y y y 17 〇〇 and the saponification value of 98.5 mole% of polyvinyl alcohol was added to 9000 liters of water to dissolve, so that the solution was cooled to fry, 115 kg of 35 wt% ship and 590 kg of butyric acid were added for condensation reaction, and the reaction was maintained until 聚乙烯The butyric acid precipitated and precipitated. Then warm up to 6 〇. Hey. The reaction mixture was at 6 Torr. The mixture was held for 3 hours and stirred to complete the reaction. The polyvinyl butyral precipitate was washed with deionized water and then dried in a dry towel. The lining of 14 wt% of the polyurethane was reduced. Preparation Example 2: The same method as in Example 1, except that 550 kg of butyraldehyde was used instead of the example 1 of 7 201024347 butyraldehyde amount, and a polyethylene having a hydroxyl group content of 218% by weight was obtained. Butyral. Examples 1-12 A blend of 5.6 g of polyvinyl butyral from Preparation Examples 1-2 and 70 g of a plasticizer was respectively obtained to obtain a f blend, and the plasticizer was di(butyl diethylene glycol) adipic acid. And the mixture of di-(2-ethylhexanoic acid) diethylene glycol ester in the ratio shown in Table 1 followed by the blending fog point test is shown in Table 1. Table 1 Weight of the component Polyvinyl butyral hydroxyl group ί: Cwt%) Fog point °C Di(butyl diethylene glycol adipate) ester Di·0 ethylhexanoic acid) Triethylene glycol ester Example 1 100 0 17.4 47 Example 2 80 20 17.4 52 Example 3 60 40 17.4 60 Example 4 40 60 17.4 66 Example 5 20 80 17.4 78 Example 6 0 100 17.4 102 Example 7 100 0 21.8 85 Example 8 80 20 21.8 95 Example 9 60 40 21.8 102 Greedy Example 10 40 60 21.8 108 Example 11 20 80 21.8 116 - Example 12 0 100 21.8 135 Comparative Example 1-2 使得 Makes the polymerization from Preparation Example 1-2 5.6 g of ethylene butyral was separately subjected to the above-mentioned haze test with 70 g of dihexyl oxalate (DHA) plasticizer, and the results are shown in Table 2. Table 2 Polyvinyl butyral hydroxyl group 詈fwt%, haze point °C Comparative Example 1 17.4 128 Comparative Example 2 21.8 142 The results of Table 1 and Table 2 show that the adipic acid di(butyldiethylene) of the present invention Alcohol) The compatibility of the vinegar and the di-2-ethylhexanoic acid triethylene glycol plasticizer composition with the polyethylene shortening resin is superior to DHA. The better compatibility means that the phase separation is less likely to occur after processing into a film, resulting in poor properties.宜兹^13-17 and East Test Example 1 201024347 Examples 13-17 and Reference Examples 100 parts by weight of the polyvinyl butyl disk resin prepared in Preparation Example 2 and the weight percentages shown in Example 7-12 Plasticizer Group's (as shown in Table 3) 38 parts by weight were mixed in a high intensity mixer. This plasticized heterogeneous, polyvinyl butyral mixture melts in the extruder and forces the melt through a die that forms a film. The melting temperature was about 195 t: and it was extruded into a polyvinyl butyral sheet of about 0.76 mm. * Place the prepared polyvinyl butyral sheet between two sheets of flat glass (3 cm long * 30 cm wide * 3 mm wide). The glued glass was placed in a rubber bag and evacuated, and the vacuum was maintained at 20 Torr for 10 minutes to remove air to maintain a vacuum of 5. (: / minute heating rate is raised to 100. (:, after cooling, the glued glass is taken out. The glued glass is placed at a high level. The temperature of the high pressure 蚤 is raised to 130 ΐ, the dust force is raised to 13 kg / ft., and the autoclave temperature is cooled to 5 (The rc is made into a finished glass after the can. The mouth measures the tensile strength, compatibility, and thermogravimetric loss rate of the polyvinyl butyral film by the following method. Throughout the job, the results are shown in Table 4.
么、拉气強度：依據ASTMD4】2之方法製成試片，試驗前聚乙 縮丁_雜持在20.6。(：及相躲度23.5%環境下則、時U 以拉伸速度毫米7分鐘進行試驗。記錄試片斷裂 ❹ Β、相容性：將聚乙烯縮丁搭薄膜夾在兩片吸油中， ，度職及屹中72小時，觀察吸油紙有無；渗 出則代表與可塑劑不相容，反之則代表相容。 若滲 c、熱重損失率：聚乙烯縮丁醛薄膜置於16〇。 小時，量_膜·損失率。喊1小時及2 D、邊緣尺寸安定性：將所製得之膠合玻璃置 95%環境下持續2星期，觀察膠合玻璃邊緣白化之距目子溼度 ^平均落絲度:試驗前將30*3—膠合_ 1() ° 4小時。朗電磁性落球試驗機使2.27公 =J保持 撞擊按CNS10986，R3117規定支撐臺上之撞擊膠 ^^落下 球是否穿透膠合玻璃，測試程序如下 δ ，檢查鋼 201024347 1)將鋼球設定在5米高度，落下鋼球撞擊第一組膠合玻璃； i)假如鋼球貫穿膠合玻璃，則測試結果記錄為不合格； 11}假如鋼球未貫穿膠合玻璃而支撐在膠合玻璃上，則測 試結果記錄為合格； 2) 將膠合玻璃從支撐臺上移去並清理破碎片後，將次一組 玻璃置於支撐臺上； 、口 3) f鋼球升至規定高度，假如前一組測試合格，則落球高度較 月|J 一組尚度升高0.25米，若前一組測試不合格，則落球高 度較前一組高度降低0.25米’並記錄結果是合格或不合格； 4) 重覆2)〜3)的步驟至1〇組膠合玻璃全部測試完畢； 5) 計算平均落球高度。 比較例3 如實施例13-17之相同方式，使100重量份之製備例2聚 稀縮丁_⑽份可麵齡啊_改紅 ^ 一-(2-乙基己酸)三乙二醇酯。並如上述所述般薄膜及 璃之性質。結果如表4所示。 敬 表3 聚乙烯縮丁醛羥基 含量 可塑劑 ~ 己二酸二(丁基二 乙-醇)酯 二-(2_乙基己酸)三 乙二醇酷 —y苑例is —實施你丨14 實施你M S —實施例1fi 實施你丨17 參老你Μ 21.8wt% 21.8wt% 2L8m% 21.8wt%~ 21.8wt% _10Q_ -80_ -60_ _4〇_ 20 20-- 40 ~ 60~ 80 ---多，iy·」丄 Zl.owt% 0 Γόο 201024347 表4 實施 例13 實施 例14 實施 例15 實施 例16 實施 例17 參考 例1 比較 例3 熱重損失率(％)， 160°C*lhr 0.88 1.24 1.64 1.71 2.25 3.35 5.10 熱重損失率(％)， 160°C*?.hr 1.22 1.68 2.57 2.72 3.59 6.28 8.95 斷裂拉力強膚OVTpa〉 32.4 33.5 33.1 32.5 32.9 34.7 31.7 斷裂伸長率⑼Λ 332 320 302 300 311 280 254 100%伸長竿拉力強度 fMtDa) 2.03 3.85 4.94 5.15 5.64 6.39 7.21 __土控落球高唐fm、 4.60 5.15 5.40 5.75 5.75 5.75 5.50 逯緣尺寸安定性^辜#、 1.5 r 2 2 2 2 5 10 相容性 相容 相容 相容 相容 相容 相容 不相 容 " -— 只βοια 丄/ 个贫一敗一、j签一 乙二醇)+S旨及二-2-乙基己酸三乙二醇酯混合可塑劑製成之聚乙烯 縮丁醛薄膜其熱重損失率低於比較例3之僅使用DHA作為可塑劑 及，考例1之僅使用二_(2乙基己酸)三乙二醇酯作為可塑劑，有助 於薄膜加工及玻璃膠合程序之安全性及耐久性能提昇，製成之膠 合玻璃能兼顧優異之耐貫穿性及邊緣尺寸安定性。 且由表1及表4之數據可知，於實施例i中僅使用己二酸二(丁 基二乙二醇)酯作為可塑劑時，雖顯示霧點較低，亦即雖盥聚乙烯 縮丁搭之姆性健，但所製得之賴之平均落球高度^相對較 低，顯示其耐衝擊性相較較不足。故充分證明藉由本發明之可塑 劑組成物作為聚乙烯縮丁醛之可塑劑，其與聚乙烯縮丁醛之相容 性良好，且由此所製得之聚乙烯縮丁醛薄膜之耐衝擊性以及 尺寸安定性均良好。 【圖式簡單說明】 【主要元件符號說明】 11What is the strength of the gas: The test piece is made according to the method of ASTM D4, 2, and the polybutylene is held at 20.6 before the test. (: and the degree of hiding in 23.5% environment, then U is tested at a tensile speed of 7 minutes. Record the test piece break ❹ 相容, compatibility: the polyethylene shrink film is sandwiched between two pieces of oil absorption, 72 hours in the duty and sputum, observe the presence or absence of oil-absorbing paper; exudation represents incompatibility with plasticizer, and vice versa. If the permeability, thermal weight loss rate: polyvinyl butyral film placed at 16 〇. Hour, amount _ membrane · loss rate. Shout 1 hour and 2 D, edge size stability: the prepared glued glass is placed in a 95% environment for 2 weeks, observe the whitening of the edge of the glued glass, the humidity of the eyes ^ average drop Silkness: 30*3—glue _ 1() ° 4 hours before the test. Long electromagnetic drop ball test machine makes 2.27 gong = J keep impact. According to CNS10986, R3117, the impact glue on the support table ^^ Glued glass, the test procedure is as follows δ, check steel 201024347 1) set the steel ball to a height of 5 meters, drop the steel ball to hit the first set of glued glass; i) If the steel ball penetrates the glued glass, the test result is recorded as unqualified; } If the steel ball does not penetrate the glued glass and is supported on the glued glass , the test results are recorded as qualified; 2) After removing the glued glass from the support table and cleaning the broken piece, place the next set of glass on the support table; and 3) f steel ball rises to the specified height, if before If a group of tests is qualified, the height of the ball is increased by 0.25 meters compared with the month of the month. If the previous group fails the test, the height of the ball is reduced by 0.25 m from the height of the previous group and the result is qualified or unqualified; 4) Repeat steps 2) to 3) until the 1〇 group of bonded glass is completely tested; 5) Calculate the average falling ball height. Comparative Example 3 In the same manner as in Examples 13-17, 100 parts by weight of Preparation Example 2 polycondensed _(10) parts can be aged _ _ red ^ 1-(2-ethylhexanoic acid) triethylene glycol ester. And the properties of the film and the glass as described above. The results are shown in Table 4.敬表3 Polyvinyl butyral hydroxyl content plasticizer ~ Di(butyl butyl alcohol) adipic acid di-(2-ethylhexanoic acid) triethylene glycol cool - y court example is - implement you 丨14 Implementing Your MS - Example 1fi Implementing Your 丨17 参老你Μ 21.8wt% 21.8wt% 2L8m% 21.8wt%~ 21.8wt% _10Q_ -80_ -60_ _4〇_ 20 20-- 40 ~ 60~ 80 -- -multi, iy·"丄Zl.owt% 0 Γόο 201024347 Table 4 Example 13 Example 14 Example 15 Example 16 Example 17 Reference Example 1 Comparative Example 3 Thermogravimetric loss rate (%), 160 ° C * lhr 0.88 1.24 1.64 1.71 2.25 3.35 5.10 Thermogravimetric loss rate (%), 160°C*?.hr 1.22 1.68 2.57 2.72 3.59 6.28 8.95 Breaking tensile strength OVTa> 32.4 33.5 33.1 32.5 32.9 34.7 31.7 Elongation at break (9)Λ 332 320 302 300 311 280 254 100% elongation 竿 tensile strength fMtDa) 2.03 3.85 4.94 5.15 5.64 6.39 7.21 __ soil control falling ball Gaotang fm, 4.60 5.15 5.40 5.75 5.75 5.75 5.50 逯 edge size stability ^ 辜 #, 1.5 r 2 2 2 2 5 10 Compatibility Compatible Compatible Compatible Compatible Compatible Compatible " -- Only βοια 丄/ One Poor One, One Signed One The polyethylene butyral film made of ethylene glycol)+S and di-2-ethylhexanoate triethylene glycol ester mixed plasticizer has a lower heat weight loss rate than that of Comparative Example 3 using only DHA as a plasticizer. And, the use of di-(2-ethylhexanoic acid) triethylene glycol ester as the plasticizer in the test case 1 contributes to the improvement of the safety and durability of the film processing and the glass bonding process, and the manufactured glued glass can be balanced. Excellent penetration resistance and edge dimensional stability. It can be seen from the data of Tables 1 and 4 that when only di(butyl diethylene glycol) adipate is used as the plasticizer in Example i, although the fog point is low, that is, the polyethylene shrinkage is obtained. Ding is the best, but the average height of the ball is relatively low, indicating that its impact resistance is relatively insufficient. Therefore, the plasticizer composition of the present invention is sufficiently proved to be a plasticizer of polyvinyl butyral, which has good compatibility with polyvinyl butyral, and the impact of the polyvinyl butyral film thus obtained is impact resistant. Both sex and dimensional stability are good. [Simple description of the diagram] [Explanation of main component symbols] 11