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以兩步偶聯法及三步加料法合成苯乙烯丁二烯嵌段共聚物之合成工藝、物性及應用...

國立高雄大學化學工程及材料工程學系碩士班

以兩步偶聯法及三步加料法合成苯乙烯丁二烯嵌段共聚物之合成工藝、物性及應用 = Syntheses, properties, and applications of styrene-butadiene block copolymers prepared by a coupled two-step method and a three-step feeding method

紀錄類型:	書目-語言資料,印刷品 : 單行本
並列題名:	Syntheses, properties, and applications of styrene-butadiene block copolymers prepared by a coupled two-step method and a three-step feeding method
作者:	陳宣旭,
其他團體作者:	國立高雄大學
出版地:	[高雄市]
出版者:	撰者;
出版年:	2014[民103]
面頁冊數:	88面圖，表 : 30公分;
標題:	兩步偶聯法
標題:	coupled two-step method
電子資源:	http://handle.ncl.edu.tw/11296/ndltd/98464301767685522890
附註:	參考書目：面73-74
附註:	103年12月16日公開
摘要註:	本研究以偶合型兩步偶聯法、非偶合型二步加料聚合法及三步加料聚合法，以正丁基鋰引發陰離子聚合反應，合成苯乙烯-丁二烯-苯乙烯嵌段三聚物(SBS, triblock copolymer)/苯乙烯-丁二烯嵌段共聚物(SB, diblock copolymer)。兩步偶聯法第一步先用正丁基鋰引發苯乙烯聚合後，加入丁二烯製成聚苯乙烯-丁二烯基鋰雙嵌段(SBLi)，再加入偶聯劑，製成線型嵌段三聚物。非偶合型二步加料法是在第二步加入丁二烯的同時，把另一部份苯乙烯也加入到反應器中，採用的原理是基於聚苯乙烯基鋰活性鏈端(SLi)，引發丁二烯聚合的能力高於引發苯乙烯聚合的能力，兩者的反應性比與鏈增長速率差異較大，在第二步反應時丁二烯聚合轉化完全之後苯乙烯才開始聚合，非偶合型二步加料法的主要優點是減少了單體加料次數，因而可以減少雜質進入聚合反應體系，減少二嵌段共聚物生成的機會，但當丁二烯和苯乙烯同時存在時，特別是在丁二烯聚合後期，由於苯乙烯相對濃度較大，有時可能會生成少量苯乙烯與丁二烯的無規則鏈段，在一定程度上影響產品的物性。使用三步加料法反應器中加入定量的苯乙烯，接著以正丁基鋰引發陰離子聚合反應，使單體苯乙烯全部轉化為聚合物，接著加入丁二烯，當丁二烯轉化率達90%以上時，將剩下的另一半量的苯乙烯加入，使單體全部轉化。生成的苯乙烯-丁二烯-苯乙烯嵌段共聚物，並利用凝膠滲透層析儀 GPC 分析，找出起始劑用量、起始劑/偶合劑比率、偶合效率和其分子量多寡等相關聯數據的存在。本實驗發現聚合物分子量隨活性的正丁基鋰增加而呈現下降趨勢，偶合型兩步偶聯法在最佳偶合劑效率時，相同配方下的平均分子量會出現最大值；非偶合型二步加料法利用控制起始劑和甲醇莫耳數比，能明顯控制triblock / diblock 分子量；非偶合型三步加料法因增加分子量參考點，在於分子量控制上更能比兩步加料法更準確，對反應控制能力做穩定提升。並依照實驗得知依照相同配方，做非偶合型線性苯乙烯-丁二烯-苯乙烯嵌段共聚物生產，三部加料法可以得到較高的吸油率，在工業製程中可以充更多的擴展油來改變硬度特性，對於降低商業生產成本有較大助益。 In this study, the coupled two-step method, the non-coupled two-step feeding method and three-step feeding method were investigated using n-butyl lithium to initiate anionic polymerizations of styrene-butadiene-styrene triblock copolymer (SBS, triblock copolymer) / styrene-butadiene diblock copolymer (SB, diblock copolymer). With the coupled two-step method, after n-butyl lithium-initiated polymerizations of styrene (SLi), butadiene was added to produce styrene-butadiene block copolymer (SBLi) followed by coupling reactions to make linear block terpolymer. With the non-coupling two-step feeding method, butadiene and styrene were added to the SLi to conduct propagation of the butadiene in the 2nd block, followed by propagation of styrene in the 3rd block on the basis of much higher chain growth rate of butadiene than that of styrene. The main advantage of the non-coupled two-step feeding method is the reduction in the number of monomer additions; this may reduce impurities entering the polymerization reaction system but increase the chance of producing random copolymers in the second step. With the non-coupled three-step method, butadiene was added to the n-butyl lithium-initiated polystyrene (SLi) to produce styrene-butadiene block copolymer (SBLi), followed by adding styrene to produce styrene-butadiene-styrene triblock copolymer. Gel permeation chromatography (GPC) was used to characterize molecular weights and distributions to correlate with the amount of initiator, the initiator / coupled agent ratio, the amount of coupling efficiency, and other relevant data. The molecular weight of the polymer was found to increase with decreasing use of n-butyl lithium. The non-coupled two-step feeding method used the initiator and methanol molar ratio to be able to control triblock / diblock molecular weight. The non-coupled three-step feeding method is more accurate in controlling the molecular weight than the two-step feeding method. Moreover, the non-coupled linear styrene-butadiene-styrene triblock copolymer produced by the three-step feeding method exhibited a higher oil absorption rate than the other methods.

以兩步偶聯法及三步加料法合成苯乙烯丁二烯嵌段共聚物之合成工藝、物性及應用 = Syntheses, properties, and applications of styrene-butadiene block copolymers prepared by a coupled two-step method and a three-step feeding method
陳, 宣旭

以兩步偶聯法及三步加料法合成苯乙烯丁二烯嵌段共聚物之合成工藝、物性及應用 = Syntheses, properties, and applications of styrene-butadiene block copolymers prepared by a coupled two-step method and a three-step feeding method / 陳宣旭撰 - [高雄市] : 撰者, 2014[民103]. - 88面 ; 圖，表 ; 30公分.
參考書目：面73-74103年12月16日公開.
兩步偶聯法coupled two-step method

以兩步偶聯法及三步加料法合成苯乙烯丁二烯嵌段共聚物之合成工藝、物性及應用 = Syntheses, properties, and applications of styrene-butadiene block copolymers prepared by a coupled two-step method and a three-step feeding method
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330 $a 本研究以偶合型兩步偶聯法、非偶合型二步加料聚合法及三步加料聚合法，以正丁基鋰引發陰離子聚合反應，合成苯乙烯-丁二烯-苯乙烯嵌段三聚物(SBS, triblock copolymer)/苯乙烯-丁二烯嵌段共聚物(SB, diblock copolymer)。兩步偶聯法第一步先用正丁基鋰引發苯乙烯聚合後，加入丁二烯製成聚苯乙烯-丁二烯基鋰雙嵌段(SBLi)，再加入偶聯劑，製成線型嵌段三聚物。非偶合型二步加料法是在第二步加入丁二烯的同時，把另一部份苯乙烯也加入到反應器中，採用的原理是基於聚苯乙烯基鋰活性鏈端(SLi)，引發丁二烯聚合的能力高於引發苯乙烯聚合的能力，兩者的反應性比與鏈增長速率差異較大，在第二步反應時丁二烯聚合轉化完全之後苯乙烯才開始聚合，非偶合型二步加料法的主要優點是減少了單體加料次數，因而可以減少雜質進入聚合反應體系，減少二嵌段共聚物生成的機會，但當丁二烯和苯乙烯同時存在時，特別是在丁二烯聚合後期，由於苯乙烯相對濃度較大，有時可能會生成少量苯乙烯與丁二烯的無規則鏈段，在一定程度上影響產品的物性。使用三步加料法反應器中加入定量的苯乙烯，接著以正丁基鋰引發陰離子聚合反應，使單體苯乙烯全部轉化為聚合物，接著加入丁二烯，當丁二烯轉化率達90%以上時，將剩下的另一半量的苯乙烯加入，使單體全部轉化。生成的苯乙烯-丁二烯-苯乙烯嵌段共聚物，並利用凝膠滲透層析儀 GPC 分析，找出起始劑用量、起始劑/偶合劑比率、偶合效率和其分子量多寡等相關聯數據的存在。本實驗發現聚合物分子量隨活性的正丁基鋰增加而呈現下降趨勢，偶合型兩步偶聯法在最佳偶合劑效率時，相同配方下的平均分子量會出現最大值；非偶合型二步加料法利用控制起始劑和甲醇莫耳數比，能明顯控制triblock / diblock 分子量；非偶合型三步加料法因增加分子量參考點，在於分子量控制上更能比兩步加料法更準確，對反應控制能力做穩定提升。並依照實驗得知依照相同配方，做非偶合型線性苯乙烯-丁二烯-苯乙烯嵌段共聚物生產，三部加料法可以得到較高的吸油率，在工業製程中可以充更多的擴展油來改變硬度特性，對於降低商業生產成本有較大助益。 In this study, the coupled two-step method, the non-coupled two-step feeding method and three-step feeding method were investigated using n-butyl lithium to initiate anionic polymerizations of styrene-butadiene-styrene triblock copolymer (SBS, triblock copolymer) / styrene-butadiene diblock copolymer (SB, diblock copolymer). With the coupled two-step method, after n-butyl lithium-initiated polymerizations of styrene (SLi), butadiene was added to produce styrene-butadiene block copolymer (SBLi) followed by coupling reactions to make linear block terpolymer. With the non-coupling two-step feeding method, butadiene and styrene were added to the SLi to conduct propagation of the butadiene in the 2nd block, followed by propagation of styrene in the 3rd block on the basis of much higher chain growth rate of butadiene than that of styrene. The main advantage of the non-coupled two-step feeding method is the reduction in the number of monomer additions; this may reduce impurities entering the polymerization reaction system but increase the chance of producing random copolymers in the second step. With the non-coupled three-step method, butadiene was added to the n-butyl lithium-initiated polystyrene (SLi) to produce styrene-butadiene block copolymer (SBLi), followed by adding styrene to produce styrene-butadiene-styrene triblock copolymer. Gel permeation chromatography (GPC) was used to characterize molecular weights and distributions to correlate with the amount of initiator, the initiator / coupled agent ratio, the amount of coupling efficiency, and other relevant data. The molecular weight of the polymer was found to increase with decreasing use of n-butyl lithium. The non-coupled two-step feeding method used the initiator and methanol molar ratio to be able to control triblock / diblock molecular weight. The non-coupled three-step feeding method is more accurate in controlling the molecular weight than the two-step feeding method. Moreover, the non-coupled linear styrene-butadiene-styrene triblock copolymer produced by the three-step feeding method exhibited a higher oil absorption rate than the other methods.
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