CN114228291B - 基于温敏技术的药用复合膜及其加工工艺 - Google Patents
基于温敏技术的药用复合膜及其加工工艺 Download PDFInfo
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- CN114228291B CN114228291B CN202111670869.3A CN202111670869A CN114228291B CN 114228291 B CN114228291 B CN 114228291B CN 202111670869 A CN202111670869 A CN 202111670869A CN 114228291 B CN114228291 B CN 114228291B
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- 239000002131 composite material Substances 0.000 title claims abstract description 49
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- 230000001070 adhesive effect Effects 0.000 claims abstract description 19
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- 239000002202 Polyethylene glycol Substances 0.000 claims abstract description 18
- DMLAVOWQYNRWNQ-UHFFFAOYSA-N azobenzene Chemical compound C1=CC=CC=C1N=NC1=CC=CC=C1 DMLAVOWQYNRWNQ-UHFFFAOYSA-N 0.000 claims abstract description 18
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- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims abstract description 13
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- 239000000243 solution Substances 0.000 claims description 40
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- KSBAEPSJVUENNK-UHFFFAOYSA-L tin(ii) 2-ethylhexanoate Chemical compound [Sn+2].CCCCC(CC)C([O-])=O.CCCCC(CC)C([O-])=O KSBAEPSJVUENNK-UHFFFAOYSA-L 0.000 claims description 8
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- UOCLXMDMGBRAIB-UHFFFAOYSA-N 1,1,1-trichloroethane Chemical compound CC(Cl)(Cl)Cl UOCLXMDMGBRAIB-UHFFFAOYSA-N 0.000 claims description 7
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- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 7
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- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims description 7
- 235000010267 sodium hydrogen sulphite Nutrition 0.000 claims description 7
- 239000004289 sodium hydrogen sulphite Substances 0.000 claims description 7
- 230000001376 precipitating effect Effects 0.000 claims description 6
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 4
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Abstract
本发明公开了基于温敏技术的药用复合膜及其加工工艺;包括以下步骤:S1:将聚乙二醇与乙交酯、丙交酯混合均匀,即为聚酯;将聚酯、氧化石墨烯和偶氮苯聚N‑异丙基丙烯酰胺熔融共混,挤出,定型,即为聚酯膜层;S2:将十二烷基硫酸钠溶于去离子水中,加入填料,与聚偏二氯乙烯乳液,搅拌均匀,成膜,干燥,即为聚偏二氟乙烯膜层;S3:在聚酯膜层单面涂覆胶黏剂,形成第一胶黏剂层后,与聚偏二氯乙烯膜层复合,熟化,在聚偏二氯乙烯膜层另一面涂覆胶黏剂,形成第二胶黏剂层后,与聚乙烯膜层复合,熟化,即为药用复合膜,本发明制备的药用复合膜为三层复合结构,具有气体、水分阻隔性、优异的机械强度。
Description
技术领域
本发明涉及药品包装技术领域,具体为基于温敏技术的药用复合膜及其加工工艺。
背景技术
随着时代快节奏的发展,人们生活压力越来越大,因此,对于药品的需求越来越高,而药品是一类特殊用品,对于其包装,具有较高的要求,比如,包装本身不能影响药品本身药效,同时阻隔外界环境对药品的影响。
常用的药品包装膜常用PE为基材,PE稳定性强,耐腐蚀以及无毒,但是其阻隔性较差,因此,限制其在药品包装膜方面的应用。
而聚酯是一种无色透明的聚合物薄膜,在生物医学方面具有广泛的应用,但是聚酯薄膜不具备温敏性,为了扩展聚酯薄膜的应用,因此常在聚酯表面接枝其他基团提升薄膜性能。
发明内容
本发明的目的在于提供基于温敏技术的药用复合膜及其加工工艺,以解决上述背景技术中提出的问题。
为了解决上述技术问题,本发明提供如下技术方案:
基于温敏技术的药用复合膜的加工工艺,包括以下步骤:
S1:通入氩气,升温至70-80℃,将除水的聚乙二醇与乙交酯、丙交酯混合均匀,除水反应0.5-1h后,加入辛酸亚锡,升温至120-130℃,油浴反应12-13h,用热水洗涤,沉淀物冷冻干燥,即为聚酯;将聚酯、氧化石墨烯和偶氮苯聚N-异丙基丙烯酰胺熔融共混,抽提24-28h后,干燥后,用挤出机挤出,定型,即为聚酯膜层;
S2:将对苯二酚和三氯乙烷溶于氢氧化钠溶液中,通入氮气,在60-70℃反应0.5-1h,蒸馏,收集偏氯乙烯单体,在去离子水中,加入亚硫酸氢钠、十二烷基苯磺酸钠、过硫酸钾和辛基酚聚氧乙烯基醚,搅拌均匀,调节溶液pH,真空条件下,加入丙烯酸甲酯和偏氯乙烯单体,反应10-15min,升温至40-50℃,继续反应10-15h,即为聚偏二氯乙烯乳液;
S3:将十二烷基硫酸钠溶于去离子水中,加入填料,混合均匀,超声反应后,干燥溶于去离子水中,加入聚偏二氯乙烯乳液,搅拌均匀,在聚四氟乙烯平板中成膜,干燥,即为聚偏二氟乙烯膜层;
S4:在聚酯膜层单面涂覆胶黏剂,形成第一胶黏剂层后,将聚偏二氯乙烯膜层与第一胶黏剂层复合,在20-30℃下熟化15-30h后,在30-45℃下继续熟化10-20h,接着在聚偏二氯乙烯膜层另一面涂覆胶黏剂,形成第二胶黏剂层后,将第二胶黏剂层与聚乙烯膜层复合,在20-50℃下熟化20-40h,即为药用复合膜。
作为优化,所述聚偏二氯乙烯膜层厚度为20-30μm;聚酯膜层厚度为20-30μm;聚乙烯膜层厚度为20-60μm。
作为优化,步骤S2中,溶液pH值为6-7。
作为优化,所述聚乙二醇的分子量为1500;所述乙交酯和丙交酯的摩尔比为12.5:1。
作为优化,所述第一胶黏剂层和第二胶粘剂层为聚氨酯胶黏剂。
作为优化,所述偶氮苯聚N-异丙基丙烯酰胺的加工工艺为:将α-溴代异丁酰胺溶于四氢呋喃溶液中,加入混合溶液,在0-15℃反应8-15h,析出、过滤、重结晶后,即为引发剂,将引发剂与N-异丙基丙烯酰胺、氯化铜、N-N’亚甲基双丙烯酰胺、三-(N-N-二甲基氨基乙基)混合均匀,通入氩气,升温至20-25℃,加入异丙醇和水,水浴反应1-2h,加入四氢呋喃,沉淀,干燥。
作为优化,混合溶液为4-(4’-甲氧基苯基偶氮苯酚)和三乙胺、四氢呋喃的混合溶液。
作为优化,引发剂、N-异丙基丙烯酰胺、氯化铜、N-N’亚甲基双丙烯酰胺、三-(N-N-二甲基氨基乙基)、异丙醇、水的质量比为1:30:1:3:0.9:60:30。
作为优化,所述填料为二氧化硅和二氧化钛中的一种或多种。
作为优化,根据以上任意一项所述的基于温敏技术的药用复合膜的加工工艺制备的药用复合膜。
1、本申请在聚酯膜层引入偶氮苯聚N-异丙基丙烯酰胺和氧化石墨烯,提高了膜层之间的紧密性和阻隔性,可以阻隔外界氧气以及水份,加入疏水性强的偶氮苯基团,使药用复合膜整体呈现疏水性,从而提高药用复合膜的阻隔性,保证药品质量,利用开环反应,将聚乙二醇两端的羟基接枝聚丙交酯乙交酯制成聚酯,再与偶氮苯聚N-异丙基丙烯酰胺共混,提高了聚合物的分散性,同时使聚酯膜层具有较强的阻隔性。同时,氧化石墨烯分子之间的相互作用使得聚合物中的大分子发生重排,提高了聚酯膜层的机械强度。并且,本申请制备的聚酯膜层具有温敏和光敏双重敏感性,使药用复合膜不论保存在什么样的环境中,整体的阻隔性都较强。
2、利用十二烷基硫酸钠对填料进行改性,使填料与聚合物具有较好的相容性,再与聚偏二氯乙烯进行混合,可以提高复合膜的阻隔性以及机械性能,填料可以填补聚偏二氯乙烯表面的空隙,提高成膜性能,从而提高聚偏二氯乙烯膜层的阻隔性,同时,填料的加入增强了聚偏二氯乙烯膜层的拉伸强度以及断裂伸长率。同时聚偏二氯乙烯膜层和聚酯层会填补复合膜表面的空隙,使结构变得紧密,提高药用复合膜整体的阻隔性。
与现有技术相比,本发明所达到的有益效果是:本发明制备的药用复合膜为三层复合结构,三层结构均采用阻隔性能强的物质作为基材,可以阻隔气体以及水份,保证药品质量,同时,制备过程中,不需要高温复合,也不会产生有机溶剂,安全环保。因此,本申请制备的药用复合膜具有气体、水分阻隔性、优异的机械强度。
具体实施方式
下面将对本发明实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例仅仅是本发明一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例,都属于本发明保护的范围。
实施例1:基于温敏技术的药用复合膜的加工工艺,包括以下步骤:
S1:将7份4-(4’-甲氧基苯基偶氮苯酚)、9份三乙胺溶于100份四氢呋喃溶液中,制成混合溶液,将9份α-溴代异丁酰胺溶于100份四氢呋喃溶液中,缓慢加入混合溶液,在0℃反应8h,过滤、减压浓缩,在碳酸氢钠的水溶液中析出、过滤、重结晶后,即为引发剂,将引发剂与N-异丙基丙烯酰胺、氯化铜、N-N’亚甲基双丙烯酰胺、三-(N-N-二甲基氨基乙基)混合均匀,通入氩气,升温至20℃,加入异丙醇和水,水浴反应1h后,加入90份四氢呋喃溶液,同时去除铜盐,在石油醚中沉淀,干燥即为偶氮苯聚N-异丙基丙烯酰胺;
S2:通入氩气,升温至70℃,将25份除水的聚乙二醇与乙交酯、丙交酯混合均匀,除水反应0.5h后,加入0.1份辛酸亚锡,升温至120℃,油浴反应12h,用热水洗涤,沉淀物冷冻干燥,即为聚酯;将3份聚酯、1份氧化石墨烯和1份偶氮苯聚N-异丙基丙烯酰胺熔融共混,无水乙醇抽提24h后,干燥后,用挤出机挤出,定型,即为聚酯膜层;
S3:将0.5份对苯二酚和120份三氯乙烷溶于氢氧化钠溶液中,通入氮气,在60℃反应0.5h,蒸馏,收集31℃的偏氯乙烯单体后,在150份去离子水中,加入0.2份亚硫酸氢钠、2份十二烷基苯磺酸钠、0.5份过硫酸钾和1份辛基酚聚氧乙烯基醚,搅拌均匀,调节溶液pH为6,真空条件下,加入10份丙烯酸甲酯和90份偏氯乙烯单体,反应10min,升温至40℃,继续反应10h,即为聚偏二氯乙烯乳液;
S4:将0.01份十二烷基硫酸钠溶于100份去离子水中,加入0.5份二氧化硅,搅拌反应0.5h后,调节溶液pH为3,超声反应20min后,干燥后,取0.2份溶于100份去离子水中,缓慢滴加40份聚偏二氯乙烯乳液,搅拌均匀,反应0.5h,在聚四氟乙烯平板中成膜,干燥,即为聚偏二氟乙烯膜层;
S5:在聚酯膜层单面涂覆聚氨酯胶黏剂,形成第一胶黏剂层后,将聚偏二氯乙烯膜层与第一胶黏剂层复合,在25℃下熟化25h后,在40℃下继续熟化15h,接着在聚偏二氯乙烯膜层另一面涂覆聚氨酯胶黏剂,形成第二胶黏剂层后,将第二胶黏剂层与聚乙烯膜层复合,在35℃下熟化35h,即为药用复合膜。
本实施例中,聚偏二氯乙烯膜层厚度为20μm;聚酯膜层厚度为20μm;聚乙烯膜层厚度为40μm。
引发剂、N-异丙基丙烯酰胺、氯化铜、N-N’亚甲基双丙烯酰胺、三-(N-N-二甲基氨基乙基)、异丙醇、水的质量比为1:30:1:3:0.9:60:30。
聚乙二醇分子量为1500,乙交酯和丙交酯的摩尔比为12.5:1。
实施例2:基于温敏技术的药用复合膜的加工工艺,包括以下步骤:
S1:将8份4-(4’-甲氧基苯基偶氮苯酚)、10份三乙胺溶于105份四氢呋喃溶液中,制成混合溶液,将10份α-溴代异丁酰胺溶于105份四氢呋喃溶液中,缓慢加入混合溶液,在5℃反应10h,过滤、减压浓缩,在碳酸氢钠的水溶液中析出、过滤、重结晶后,即为引发剂,将引发剂与N-异丙基丙烯酰胺、氯化铜、N-N’亚甲基双丙烯酰胺、三-(N-N-二甲基氨基乙基)混合均匀,通入氩气,升温至21℃,加入异丙醇和水,水浴反应1-2h后,加入95份四氢呋喃溶液,同时去除铜盐,在石油醚中沉淀,干燥即为偶氮苯聚N-异丙基丙烯酰胺;
S2:通入氩气,升温至75℃,将26份除水的聚乙二醇与乙交酯、丙交酯混合均匀,除水反应0.8h后,加入0.2份辛酸亚锡,升温至125℃,油浴反应12.5h,用热水洗涤,沉淀物冷冻干燥,即为聚酯;将4份聚酯、2份氧化石墨烯和2份偶氮苯聚N-异丙基丙烯酰胺熔融共混,无水乙醇抽提26h后,干燥后,用挤出机挤出,定型,即为聚酯膜层;
S3:将0.6份对苯二酚和125份三氯乙烷溶于氢氧化钠溶液中,通入氮气,在65℃反应0.7h,蒸馏,收集31℃的偏氯乙烯单体后,在155份去离子水中,加入0.3份亚硫酸氢钠、3份十二烷基苯磺酸钠、0.6份过硫酸钾和1.1份辛基酚聚氧乙烯基醚,搅拌均匀,调节溶液pH为6.5,真空条件下,加入11份丙烯酸甲酯和91份偏氯乙烯单体,反应12min,升温至45℃,继续反应11h,即为聚偏二氯乙烯乳液;
S4:将0.02份十二烷基硫酸钠溶于105份去离子水中,加入0.6份二氧化硅,搅拌反应0.7h后,调节溶液pH为3.5,超声反应30min后,干燥后,取0.3份溶于105份去离子水中,缓慢滴加41份聚偏二氯乙烯乳液,搅拌均匀,反应0.8h,在聚四氟乙烯平板中成膜,干燥,即为聚偏二氟乙烯膜层;
S5:在聚酯膜层单面涂覆聚氨酯胶黏剂,形成第一胶黏剂层后,将聚偏二氯乙烯膜层与第一胶黏剂层复合,在25℃下熟化20h后,在35℃下继续熟化15h,接着在聚偏二氯乙烯膜层另一面涂覆聚氨酯胶黏剂,形成第二胶黏剂层后,将第二胶黏剂层与聚乙烯膜层复合,在40℃下熟化35h,即为药用复合膜。
本实施例中,聚偏二氯乙烯膜层厚度为25μm;聚酯膜层厚度为25μm;聚乙烯膜层厚度为45μm。
引发剂、N-异丙基丙烯酰胺、氯化铜、N-N’亚甲基双丙烯酰胺、三-(N-N-二甲基氨基乙基)、异丙醇、水的质量比为1:30:1:3:0.9:60:30。
聚乙二醇分子量为1500,乙交酯和丙交酯的摩尔比为12.5:1。
实施例3:基于温敏技术的药用复合膜的加工工艺,包括以下步骤:
S1:将9份4-(4’-甲氧基苯基偶氮苯酚)、11份三乙胺溶于110份四氢呋喃溶液中,制成混合溶液,将11份α-溴代异丁酰胺溶于四氢呋喃溶液中,缓慢加入混合溶液,在10℃反应12h,过滤、减压浓缩,在碳酸氢钠的水溶液中析出、过滤、重结晶后,即为引发剂,将引发剂与N-异丙基丙烯酰胺、氯化铜、N-N’亚甲基双丙烯酰胺、三-(N-N-二甲基氨基乙基)混合均匀,通入氩气,升温至23℃,加入异丙醇和水,水浴反应1.9h后,加入90份四氢呋喃溶液,同时去除铜盐,在石油醚中沉淀,干燥即为偶氮苯聚N-异丙基丙烯酰胺;
S2:通入氩气,升温至78℃,将27份除水的聚乙二醇与乙交酯、丙交酯混合均匀,除水反应0.9h后,加入0.3份辛酸亚锡,升温至1280℃,油浴反应12.9h,用热水洗涤,沉淀物冷冻干燥,即为聚酯;将5份聚酯、2份氧化石墨烯和2份偶氮苯聚N-异丙基丙烯酰胺熔融共混,无水乙醇抽提27h后,干燥后,用挤出机挤出,定型,即为聚酯膜层;
S3:将0.7份对苯二酚和130份三氯乙烷溶于氢氧化钠溶液中,通入氮气,在68℃反应0.9h,蒸馏,收集32℃的偏氯乙烯单体后,在160份去离子水中,加入0.4份亚硫酸氢钠、4份十二烷基苯磺酸钠、0.7份过硫酸钾和1.2份辛基酚聚氧乙烯基醚,搅拌均匀,调节溶液pH为6.8,真空条件下,加入12份丙烯酸甲酯和100份偏氯乙烯单体,反应14min,升温至40-50℃,继续反应14h,即为聚偏二氯乙烯乳液;
S4:将0.03份十二烷基硫酸钠溶于110份去离子水中,加入0.7份二氧化硅,搅拌反应0.9h后,调节溶液pH为3.8,超声反应35min后,干燥后,取0.4份溶于110份去离子水中,缓慢滴加42份聚偏二氯乙烯乳液,搅拌均匀,反应0.9h,在聚四氟乙烯平板中成膜,干燥,即为聚偏二氟乙烯膜层;
S5:在聚酯膜层单面涂覆聚氨酯胶黏剂,形成第一胶黏剂层后,将聚偏二氯乙烯膜层与第一胶黏剂层复合,在20℃下熟化15h后,在30℃下继续熟化10h,接着在聚偏二氯乙烯膜层另一面涂覆聚氨酯胶黏剂,形成第二胶黏剂层后,将第二胶黏剂层与聚乙烯膜层复合,在20℃下熟化20h,即为药用复合膜。
本实施例中,聚偏二氯乙烯膜层厚度为25μm;聚酯膜层厚度为25μm;聚乙烯膜层厚度为50μm。
引发剂、N-异丙基丙烯酰胺、氯化铜、N-N’亚甲基双丙烯酰胺、三-(N-N-二甲基氨基乙基)、异丙醇、水的质量比为1:30:1:3:0.9:60:30。
聚乙二醇分子量为1500,乙交酯和丙交酯的摩尔比为12.5:1。
实施例4:基于温敏技术的药用复合膜的加工工艺,包括以下步骤:
S1:将10份4-(4’-甲氧基苯基偶氮苯酚)、12份三乙胺溶于115份四氢呋喃溶液中,制成混合溶液,将12份α-溴代异丁酰胺溶于四氢呋喃溶液中,缓慢加入混合溶液,在15℃反应15h,过滤、减压浓缩,在碳酸氢钠的水溶液中析出、过滤、重结晶后,即为引发剂,将引发剂与N-异丙基丙烯酰胺、氯化铜、N-N’亚甲基双丙烯酰胺、三-(N-N-二甲基氨基乙基)混合均匀,通入氩气,升温至25℃,加入异丙醇和水,水浴反应1-2h后,加入110份四氢呋喃溶液,同时去除铜盐,在石油醚中沉淀,干燥即为偶氮苯聚N-异丙基丙烯酰胺;
S2:通入氩气,升温至80℃,将28份除水的聚乙二醇与乙交酯、丙交酯混合均匀,除水反应1h后,加入0.4份辛酸亚锡,升温至130℃,油浴反应13h,用热水洗涤,沉淀物冷冻干燥,即为聚酯;将8份聚酯、3份氧化石墨烯和3份偶氮苯聚N-异丙基丙烯酰胺熔融共混,无水乙醇抽提24-28h后,干燥后,用挤出机挤出,定型,即为聚酯膜层;
S3:将0.8份对苯二酚和135份三氯乙烷溶于氢氧化钠溶液中,通入氮气,在60-70℃反应1h,蒸馏,收集33℃的偏氯乙烯单体后,在165份去离子水中,加入0.5份亚硫酸氢钠、5份十二烷基苯磺酸钠、0.9份过硫酸钾和1.3份辛基酚聚氧乙烯基醚,搅拌均匀,调节溶液pH为7,真空条件下,加入13份丙烯酸甲酯和110份偏氯乙烯单体,反应15min,升温至-50℃,继续反应15h,即为聚偏二氯乙烯乳液;
S4:将0.04份十二烷基硫酸钠溶于120份去离子水中,加入0.8份二氧化硅,搅拌反应1h后,调节溶液pH为4,超声反应40min后,干燥后,取0.5份溶于115份去离子水中,缓慢滴加43份聚偏二氯乙烯乳液,搅拌均匀,反应1h,在聚四氟乙烯平板中成膜,干燥,即为聚偏二氟乙烯膜层;
S5:在聚酯膜层单面涂覆聚氨酯胶黏剂,形成第一胶黏剂层后,将聚偏二氯乙烯膜层与第一胶黏剂层复合,在30℃下熟化30h后,在45℃下继续熟化20h,接着在聚偏二氯乙烯膜层另一面涂覆聚氨酯胶黏剂,形成第二胶黏剂层后,将第二胶黏剂层与聚乙烯膜层复合,在50℃下熟化40h,即为药用复合膜。
本实施例中,聚偏二氯乙烯膜层厚度为30μm;聚酯膜层厚度为30μm;聚乙烯膜层厚度为60μm。
引发剂、N-异丙基丙烯酰胺、氯化铜、N-N’亚甲基双丙烯酰胺、三-(N-N-二甲基氨基乙基)、异丙醇、水的质量比为1:30:1:3:0.9:60:30。
聚乙二醇分子量为1500,乙交酯和丙交酯的摩尔比为12.5:1。
对比例
对比例1:基于温敏技术的药用复合膜的加工工艺,包括以下步骤:
S1:将7份4-(4’-甲氧基苯基偶氮苯酚)、9份三乙胺溶于100份四氢呋喃溶液中,制成混合溶液,将9份α-溴代异丁酰胺溶于100份四氢呋喃溶液中,缓慢加入混合溶液,在0℃反应8h,过滤、减压浓缩,在碳酸氢钠的水溶液中析出、过滤、重结晶后,即为引发剂,将引发剂与N-异丙基丙烯酰胺、氯化铜、N-N’亚甲基双丙烯酰胺、三-(N-N-二甲基氨基乙基)混合均匀,通入氩气,升温至20℃,加入异丙醇和水,水浴反应1h后,加入90份四氢呋喃溶液,同时去除铜盐,在石油醚中沉淀,干燥即为偶氮苯聚N-异丙基丙烯酰胺;
S2:通入氩气,升温至70℃,将25份除水的聚乙二醇与乙交酯、丙交酯混合均匀,除水反应0.5h后,加入0.1份辛酸亚锡,升温至120℃,油浴反应12h,用热水洗涤,沉淀物冷冻干燥,即为聚酯;将3份聚酯、1份氧化石墨烯和1份偶氮苯聚N-异丙基丙烯酰胺熔融共混,无水乙醇抽提24h后,干燥后,用挤出机挤出,定型,即为聚酯膜层;
S3:在聚酯膜层一面涂覆聚氨酯胶黏剂,形成胶黏剂层后,与聚乙烯膜层复合,在20℃下熟化20h,即为药用复合膜。
本实施例中,聚酯膜层厚度为20μm;聚乙烯膜层厚度为40μm。
引发剂、N-异丙基丙烯酰胺、氯化铜、N-N’亚甲基双丙烯酰胺、三-(N-N-二甲基氨基乙基)、异丙醇、水的质量比为1:30:1:3:0.9:60:30。
聚乙二醇分子量为1500,乙交酯和丙交酯的摩尔比为12.5:1。
对比例2:基于温敏技术的药用复合膜的加工工艺,包括以下步骤:
S1:通入氩气,升温至70℃,将25份除水的聚乙二醇与乙交酯、丙交酯混合均匀,除水反应0.5h后,加入0.1份辛酸亚锡,升温至120℃,油浴反应12h,用热水洗涤,沉淀物冷冻干燥后,挤出,定型,即为聚酯膜层;
S2:将0.01份十二烷基硫酸钠溶于100份去离子水中,加入0.5份二氧化硅,搅拌反应0.5h后,调节溶液pH为3,超声反应20min后,干燥后,取0.2份溶于100份去离子水中,缓慢滴加40份聚偏二氯乙烯乳液,搅拌均匀,反应0.5h,在聚四氟乙烯平板中成膜,干燥,即为聚偏二氟乙烯膜层;
S3:将0.5份对苯二酚和120份三氯乙烷溶于氢氧化钠溶液中,通入氮气,在60℃反应0.5h,蒸馏,收集31℃的偏氯乙烯单体后,在150份去离子水中,加入0.2份亚硫酸氢钠、2份十二烷基苯磺酸钠、0.5份过硫酸钾和1份辛基酚聚氧乙烯基醚,搅拌均匀,调节溶液pH为6,真空条件下,加入10份丙烯酸甲酯和90份偏氯乙烯单体,反应10min,升温至40℃,继续反应10h,即为聚偏二氯乙烯乳液;
S4:在聚酯膜层单面涂覆聚氨酯胶黏剂,形成第一胶黏剂层后,将聚偏二氯乙烯膜层与第一胶黏剂层复合,在25℃下熟化25h后,在40℃下继续熟化15h,接着在聚偏二氯乙烯膜层另一面涂覆聚氨酯胶黏剂,形成第二胶黏剂层后,将第二胶黏剂层与聚乙烯膜层复合,在35℃下熟化35h,即为药用复合膜。
本实施例中,聚偏二氯乙烯膜层厚度为20μm;聚酯膜层厚度为20μm;聚乙烯膜层厚度为40μm。
聚乙二醇分子量为1500,乙交酯和丙交酯的摩尔比为12.5:1。
实验数据
水蒸气透过量:根据YBB00092003-2015《水蒸气透过量测定法》进行检测。
氧气透过量:根据YBB00082003-2015《气体透过量测定法》进行检测。
表1实施例1-5、对比例1-2各项检测结果
结论:
1.实施例1-4与对比例1对比,对比例1没有加入聚偏二氯乙烯膜层,导致药用复合膜的性能均有所下降,表明利用填料填补聚偏二氯乙烯膜层表面的孔隙,可以提高药用复合膜机械强度,与聚酯膜层复合可以进一步提高药用复合膜的阻隔性。
2.实施例1-4与对比例2对比,对比例2没有将聚N-异丙基丙烯酰胺与聚酯复合,导致药用复合膜阻隔性下降。
最后应说明的是:以上所述仅为本发明的优选实施例而已,并不用于限制本发明,尽管参照前述实施例对本发明进行了详细的说明,对于本领域的技术人员来说,其依然可以对前述各实施例所记载的技术方案进行修改,或者对其中部分技术特征进行等同替换。凡在本发明的精神和原则之内,所作的任何修改、等同替换、改进等,均应包含在本发明的保护范围之内。
Claims (10)
1.基于温敏技术的药用复合膜的加工工艺,其特征在于:包括以下步骤:
S1:通入氩气,升温至70-80℃,将除水的聚乙二醇与乙交酯、丙交酯混合均匀,除水反应0.5-1h后,加入辛酸亚锡,升温至120-130℃,油浴反应12-13h,用热水洗涤,沉淀物冷冻干燥,即为聚酯;将聚酯、氧化石墨烯和偶氮苯聚N-异丙基丙烯酰胺熔融共混,抽提24-28h后,干燥后,用挤出机挤出,定型,即为聚酯膜层;
S2:将对苯二酚和三氯乙烷溶于氢氧化钠溶液中,通入氮气,在60-70℃反应0.5-1h,蒸馏,收集偏氯乙烯单体,在去离子水中,加入亚硫酸氢钠、十二烷基苯磺酸钠、过硫酸钾和辛基酚聚氧乙烯基醚,搅拌均匀,调节溶液pH,真空条件下,加入丙烯酸甲酯和偏氯乙烯单体,反应10-15min,升温至40-50℃,继续反应10-15h,即为聚偏二氯乙烯乳液;
S3:将十二烷基硫酸钠溶于去离子水中,加入填料,混合均匀,超声反应后,干燥溶于去离子水中,加入聚偏二氯乙烯乳液,搅拌均匀,在聚四氟乙烯平板中成膜,干燥,即为聚偏二氟乙烯膜层;
S4:在聚酯膜层单面涂覆胶黏剂,形成第一胶黏剂层后,将聚偏二氯乙烯膜层与第一胶黏剂层复合,在20-30℃下熟化15-30h后,在30-45℃下继续熟化10-20h,接着在聚偏二氯乙烯膜层另一面涂覆胶黏剂,形成第二胶黏剂层后,将第二胶黏剂层与聚乙烯膜层复合,在20-50℃下熟化20-40h,即为药用复合膜。
2.根据权利要求1所述的基于温敏技术的药用复合膜的加工工艺,其特征在于:所述聚偏二氯乙烯膜层厚度为20-30μm;聚酯膜层厚度为20-30μm;聚乙烯膜层厚度为20-60μm。
3.根据权利要求1所述的基于温敏技术的药用复合膜的加工工艺,其特征在于:步骤S2中,溶液pH值为6-7。
4.根据权利要求1所述的基于温敏技术的药用复合膜的加工工艺,其特征在于:所述聚乙二醇的分子量为1500;所述乙交酯和丙交酯的摩尔比为12.5:1。
5.根据权利要求1所述的基于温敏技术的药用复合膜的加工工艺,其特征在于:所述第一胶黏剂层和第二胶粘剂层为聚氨酯胶黏剂。
6.根据权利要求1所述的基于温敏技术的药用复合膜的加工工艺,其特征在于:所述偶氮苯聚N-异丙基丙烯酰胺的加工工艺为:将α-溴代异丁酰胺溶于四氢呋喃溶液中,加入混合溶液,在0-15℃反应8-15h,析出、过滤、重结晶后,即为引发剂,将引发剂与N-异丙基丙烯酰胺、氯化铜、N-N’亚甲基双丙烯酰胺、三-(N-N-二甲基氨基乙基)混合均匀,通入氩气,升温至20-25℃,加入异丙醇和水,水浴反应1-2h,加入四氢呋喃,沉淀,干燥。
7.根据权利要求6所述的基于温敏技术的药用复合膜的加工工艺,其特征在于:混合溶液为4-(4’-甲氧基苯基偶氮苯酚)和三乙胺、四氢呋喃的混合溶液。
8.根据权利要求6所述的基于温敏技术的药用复合膜的加工工艺,其特征在于:引发剂、N-异丙基丙烯酰胺、氯化铜、N-N’亚甲基双丙烯酰胺、三-(N-N-二甲基氨基乙基)、异丙醇、水的质量比为1:30:1:3:0.9:60:30。
9.根据权利要求1所述的基于温敏技术的药用复合膜的加工工艺,其特征在于:所述填料为二氧化硅和二氧化钛中的一种或多种。
10.根据权利要求1-9任意一项所述的基于温敏技术的药用复合膜的加工工艺制备的药用复合膜。
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