CN106750411A - 有机两性共聚高分子互穿网络凝胶的制备方法 - Google Patents
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Abstract
本发明涉及一种有机两性共聚高分子互穿网络凝胶的制备方法。该方法是用甲基丙烯酰氧乙基三甲基氯化铵、乙烯基吡咯烷酮、咖啡酸作共聚单体,二甲基丙烯酸聚乙二醇酯作交联剂,过硫酸钾‑亚硫酸氢钠作引发剂在去离子水中进行共聚合反应得到有机两性共聚高分子第一网络凝胶;该第一网络凝胶在富马酸、D‑甘露糖、甲基丙烯酸羟乙酯、二甲基丙烯酸乙二醇酯和去离子水配制的水溶液中溶胀,该水溶液中的单体、交联剂经过硫酸钾、吡哆醇盐酸盐的作用发生共聚合、酯化反应,最后得到有机两性共聚高分子互穿网络凝胶。
Description
技术领域
本发明涉及一种有机两性共聚高分子互穿网络凝胶的制备方法。
背景技术
凝胶是一种特别的分散体系,高聚物分子或胶体颗粒相互联结形成三维空间网状结构,能吸收大量的水溶胀又不溶于水,在水中可保持一定形状,兼具固体和液体双重性质。宏观上看,高分子凝胶具有一定的形状,施加一定外力会变形,去除外力后会恢复原来形状,具有固体的粘弹性;微观上看,高分子凝胶具有三维网络结构不溶于水,三维网络分子可在水中伸展,具有液体性质。具有柔软、含水量高又有橡胶粘弹性的凝胶在环保、纺织、建材、石化、食品、农林园艺、日用化妆品等诸多方面有了广泛的应用。
包括人类在内的生物体都是高分子凝胶组成,大多带有电性,如蛋白质、氨基酸。共聚两性高分子互穿网络凝胶随共聚组分的改变可得到千变万化的特异性能,特别是高含水量和分子中的电性与人体结构的相似性,良好的生物相容性,环境刺激响应性,在生物医药领域的药物控释、生物传感、组织工程等领域得到了一些应用。
目前有机两性共聚高分子互穿网络凝胶的制备方法主要存在的问题是单体丙烯酰胺属“致癌、致畸变、致突变”的剧毒品,交联剂N,N亚甲基二丙烯酰胺毒性较大,对凝胶存在不利的毒性影响;单一的交联剂形成的互穿网络凝胶稳定性较低。开发采用无毒或低毒的单体、交联剂进行共聚合以降低凝胶毒性,使用复配交联剂形成多重互穿网络提高凝胶稳定性的有机两性共聚高分子互穿网络凝胶的制备方法具有较大实用价值。
发明内容
针对目前有机两性共聚高分子互穿网络凝胶的制备方法存在的问题,本发明的目的是提供一种采用无毒或低毒单体、交联剂进行共聚合以降低凝胶毒性,使用复配交联剂形成多重互穿网络提高凝胶稳定性的有机两性共聚高分子互穿网络凝胶的制备方法,其特征是在可密闭反应器中加入A组分和去离子水搅拌制备水溶液,控制A组分的重量浓度为28%~62%;溶液制备完成后,抽真空至相对真空度为-0.02MPa~-0.08MPa,通入氮气恢复反应器至常压后,在搅拌下加入由B组分和去离子水配制的水溶液,B组分的重量浓度为20%~40%;B组分的水溶液加料结束后,升温至35℃~50℃,在搅拌下加入由C组分和去离子水配制的水溶液,C组分的重量浓度为5%~15%;控制pH值为4~10,在35℃~50℃恒温,继续搅拌反应2h~3.5h,得到有机两性共聚高分子第一网络凝胶;然后进行冷却,在通入氮气下,将该第一网络凝胶放入装有D组分和去离子水配制的水溶液的可密闭反应器中溶胀,D组分的重量浓度为1.8%~11%,按重量计,第一网络凝胶:D组分去离子水溶液的重量比=1:(95~155),溶胀2h~6h;再加入由E组分和去离子水配制的水溶液继续溶胀,E组分的重量浓度为10%~20%,溶胀16 h~24 h;溶胀完成后,升温至75℃~95℃,控制pH值为3~7,在75℃~95℃恒温,反应4h~6h,得到有机两性共聚高分子互穿网络凝胶。所述A组分由甲基丙烯酰氧乙基三甲基氯化铵、乙烯基吡咯烷酮、咖啡酸组成,按物质的量计,甲基丙烯酰氧乙基三甲基氯化铵:乙烯基吡咯烷酮:咖啡酸的物质的量之比=(0.5~1.2):(0.3~1.6):(0.4~1.1);B组分是二甲基丙烯酸聚乙二醇酯,数均分子量为2000~20000,其投料重量是A组分总重量的2.5%~11%;C组分由过硫酸钾-亚硫酸氢钠组成,其投料总重量是A组分总重量的0.3%~1.8%,按重量计,过硫酸钾:亚硫酸氢钠的重量之比=1:(0.2~1.1);D组分由富马酸、D-甘露糖、甲基丙烯酸羟乙酯和二甲基丙烯酸乙二醇酯组成,按物质的量计,富马酸:D-甘露糖:甲基丙烯酸羟乙酯的物质的量之比=(0.4~1.6):(0.08~0.32):(0.4~1.1),按重量计,二甲基丙烯酸乙二醇酯投料重量是富马酸、D-甘露糖、甲基丙烯酸羟乙酯三种单体总重量的1.8%~5.5%;E组分由过硫酸钾、吡哆醇盐酸盐组成,过硫酸钾投料重量是D组分总重量的0.1%~1.2%,吡哆醇盐酸盐投料总重量是D组分总重量的0.8%~5.6%。
本发明的技术方法是这样实现的:在可密闭反应器中制备甲基丙烯酰氧乙基三甲基氯化铵CH2=C(CH3)COO(CH2)2N(CH3)3Cl、乙烯基吡咯烷酮CH2=CH-(C4H6NO)、咖啡酸(HO)2C6H3CH=CHCOOH共聚单体和去离子水在搅拌下制备成混合均匀的水溶液;抽真空去氧后,通入氮气保护,加入交联剂二甲基丙烯酸聚乙二醇酯的水溶液;升温后,再加入氧化还原引发剂过硫酸钾-亚硫酸氢钠K2S2O8-NaHSO3的水溶液,经引发、共聚合链增长反应,交联剂二甲基丙烯酸聚乙二醇酯参与共聚反应和线型共聚大分子发生交联反应形成交联网络结构,经链终止反应,得到有机两性共聚高分子第一网络凝胶。通入氮气保护,有机两性共聚高分子第一网络凝胶在富马酸HOOCCH=CHCOOH、D-甘露糖HOCH2(CHOH)4CHO、甲基丙烯酸羟乙酯CH2=C(CH3)COOCH2CH2OH、二甲基丙烯酸乙二醇酯CH2=C(CH3)COO(CH2)2OOC(CH3)C=CH2的水溶液作用下溶胀,再加入引发剂过硫酸钾K2S2O8、催化剂吡哆醇盐酸盐(CH3)(HOCH2)2(HO)C5HN·HCl水溶液的作用下继续溶胀,溶胀过程中,水溶液中的单体、交联剂、引发剂、催化剂进入到有机两性共聚高分子第一网络凝胶内部并均匀分布;升温后,经引发、共聚合链增长反应形成线型共聚大分子,交联剂二甲基丙烯酸乙二醇酯参与共聚反应和线型共聚大分子发生交联反应,形成交联网络结构,吡哆醇盐酸盐催化带羧基基团的分子和带羟基基团的分子发生酯化反应,由于D-甘露糖带有五个OH基团与带羧基基团的分子反应形成交联网络结构;进一步反应,最后由于自由基共聚合大分子的链终止和酯化反应的完成,形成有机两性共聚高分子互穿网络凝胶。
相对于现有技术方法,本发明突出优点是制备技术中所用的单体甲基丙烯酰氧乙基三甲基氯化铵、甲基丙烯酸羟乙酯低毒,单体咖啡酸、富马酸、乙烯基吡咯烷酮和交联剂二甲基丙烯酸聚乙二醇酯、二甲基丙烯酸乙二醇酯、D-甘露糖无毒,降低了凝胶毒性;制备的互穿网络凝胶具有自由基交联和酯化交联网络结构,提高了互穿网络凝胶的稳定性;制备方法简单、反应条件温和、宜于生产,具有良好的环境效益和经济效益。
具体实施方式
实施例1:将124.5g甲基丙烯酰氧乙基三甲基氯化铵,44.5g乙烯基吡咯烷酮,90g咖啡酸和604ml的去离子水加入到容积为2L的可密闭反应器中搅拌混合均匀,该水溶液的重量浓度为30%,抽真空至相对真空度-0.025MPa,然后通入氮气恢复反应器至常压,加入7.77g数均分子量为3000的二甲基丙烯酸聚乙二醇酯和29.3ml去离子水配制的水溶液,该水溶液的重量浓度为21%;然后升温至38℃,加入1g过硫酸钾、0.3g亚硫酸氢钠和22.25ml去离子水配制的水溶液,该水溶液的重量浓度为5.5%;在38℃恒温,控制pH值为4.5,继续搅拌反应2.3h,得到有机两性共聚高分子第一网络凝胶;然后进行冷却,在通入氮气下,有机两性共聚高分子第一网络凝胶71.97g投入容积为15L的密闭反应器中溶胀,该反应器中装有58g富马酸、18g D-甘露糖、65g甲基丙烯酸羟乙酯、2.82g二甲基丙烯酸乙二醇酯和7053.23ml去离子水配制的水溶液,该水溶液的重量浓度为2%,第一网络凝胶的重量(71.97g):该水溶液的重量(7197.17g)=1:100,溶胀2.3h;再加入0.29g过硫酸钾、1.44g吡哆醇盐酸盐和14.72ml去离子水配制的水溶液继续溶胀,该水溶液的重量浓度为10.5%,溶胀17 h;溶胀完成后升温至78℃,控制pH值为5,在78℃恒温反应4.3h,得到有机两性共聚高分子互穿网络凝胶。该凝胶不溶于水,能在水中溶胀,凝胶溶胀率(ESR)=6720%(去离子水),凝胶溶胀率(ESR)=6690%(重量浓度1%的NaCl水溶液)。
实施例2:将228.25g甲基丙烯酰氧乙基三甲基氯化铵,166.71g乙烯基吡咯烷酮,180.15g咖啡酸和383.41ml的去离子水加入到容积为1L可密闭反应器中搅拌混合均匀,该水溶液的重量浓度为60%,抽真空至相对真空度-0.075MPa,然后通入氮气恢复反应器至常压,加入57.51g数均分子量为19000的二甲基丙烯酸聚乙二醇酯和90ml去离子水配制的水溶液,该水溶液的重量浓度为39%;然后升温至48℃,加入4.31g过硫酸钾、4.31g亚硫酸氢钠和50.87ml去离子水配制的水溶液,该水溶液的重量浓度为14.5%,;在48℃恒温,控制pH值为8.3,继续搅拌反应3.3h,得到有机两性共聚高分子第一网络凝胶;然后进行冷却,在通入氮气下,有机两性共聚高分子第一网络凝胶25.08g投入容积为5L的可密闭反应器中溶胀,该反应器中装有174.1g富马酸、54g D-甘露糖、130.14g甲基丙烯酸羟乙酯、17.9g二甲基丙烯酸乙二醇酯和3385.87ml去离子水配制的水溶液,该水溶液的重量浓度为10%,第一网络凝胶的重量(25.08g):该水溶液的重量(3762.08g)=1:150,溶胀5.7h,再加入0.75g过硫酸钾、3.76g吡哆醇盐酸盐和18.64ml去离子水配制的水溶液继续溶胀,该水溶液的重量浓度为19.5%,溶胀23 h;溶胀完成后升温至93℃,控制pH值为6,在93℃恒温反应5.6h,得到有机两性共聚高分子互穿网络凝胶。该凝胶不溶于水,能在水中溶胀,凝胶溶胀率(ESR)=5217%(去离子水),凝胶溶胀率(ESR)=5163%(重量浓度1%的NaCl水溶液)。
Claims (1)
1.一种有机两性共聚高分子互穿网络凝胶的制备方法,其特征是在可密闭反应器中加入A组分和去离子水搅拌制备水溶液,控制A组分的重量浓度为28%~62%,溶液制备完成后,抽真空至相对真空度为-0.02MPa~-0.08MPa,通入氮气恢复反应器至常压后,在搅拌下加入由B组分和去离子水配制的水溶液,B组分的重量浓度为20%~40%,B组分的水溶液加料结束后,升温至35℃~50℃,在搅拌下加入由C组分和去离子水配制的水溶液,C组分的重量浓度为5%~15%,控制pH值为4~10,在35℃~50℃恒温,继续搅拌反应2h~3.5h,得到有机两性共聚高分子第一网络凝胶,然后进行冷却,在通入氮气下,将该第一网络凝胶投入装有D组分和去离子水配制的水溶液的可密闭反应器中溶胀,D组分的重量浓度为1.8%~11%,按重量计,第一网络凝胶:D组分去离子水溶液的重量比=1:(95~155),溶胀时间为2h~6h,再加入由E组分和去离子水配制的水溶液继续溶胀,E组分的重量浓度为10%~20%,溶胀时间为16 h~24 h,溶胀完成后,升温至75℃~95℃,控制pH值为3~7,在75℃~95℃恒温,反应4h~6h,得到有机两性共聚高分子互穿网络凝胶;所述A组分由甲基丙烯酰氧乙基三甲基氯化铵、乙烯基吡咯烷酮、咖啡酸组成,按物质的量计,甲基丙烯酰氧乙基三甲基氯化铵:乙烯基吡咯烷酮:咖啡酸的物质的量之比=(0.5~1.2):(0.3~1.6):(0.4~1.1),B组分是二甲基丙烯酸聚乙二醇酯,数均分子量为2000~20000,其投料重量是A组分总重量的2.5%~11%,C组分由过硫酸钾-亚硫酸氢钠组成,其投料总重量是A组分总重量的0.3%~1.8%,按重量计,过硫酸钾:亚硫酸氢钠的重量之比=1:(0.2~1.1),D组分由富马酸、D-甘露糖、甲基丙烯酸羟乙酯和二甲基丙烯酸乙二醇酯组成,按物质的量计,富马酸:D-甘露糖:甲基丙烯酸羟乙酯的物质的量之比=(0.4~1.6):(0.08~0.32):(0.4~1.1),按重量计,二甲基丙烯酸乙二醇酯投料重量是富马酸、D-甘露糖、甲基丙烯酸羟乙酯三种单体总重量的1.8%~5.5%,E组分由过硫酸钾、吡哆醇盐酸盐组成,过硫酸钾投料重量是D组分总重量的0.1%~1.2%,吡哆醇盐酸盐投料重量是D组分总重量的0.8%~5.6%。
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