维生素E护肤纤维素纤维的制备及性能研究
摘要
本文以最为活跃的主客体化学、超分子化学为基础,选择对人体和环境无任何毒副作用,对皮肤无任何刺激的β-环糊精为包覆材料制备出维生素E-β-环糊精包合物,并将这种包合物采用共混法加入纤维素纤维纺丝原液中,通过湿法纺丝制备出维生素E护肤保健纤维,研究了纺丝条件及所得纤维的各项性能。本文研究了氢氧化钠/尿素/硫脲水溶液和离子液体两种溶剂体系对纤维素的溶解情况;通过比较两种溶剂体系的溶解条件、工艺和溶解再生前后的纤维素的各项性能,选择合适的溶剂体系,用以制备性能良好的纺丝原液制备纤维素纤维。
以β-环糊精为壁材,制备了维生素E-β-环糊精的包合物,采用紫外-可见光谱、红外、XRD、TG等方式对包合物进行了鉴定和表征,并对所制备的包合物的缓释性能进行了测试:结果证实维生素E与β-环糊精以1∶1的比例形成包合物,维生素E的色满酚结构进入环糊精空腔之中;所制备的包合物耐热和耐紫外光性能良好;具有良好的缓释性能。研究了NaOH/Urea/Thiourea水溶液和[AMIM]Cl(1-烯丙基-3甲基氯代咪唑)两种溶剂体系对纤维素的溶解情况,综合考虑两种溶剂体系的溶解过程、所需条件和溶解再生后纤维素的各项性能,选择NaOH/Urea/Thiourea水溶液作为纤维素溶剂制备纤维素纤维的纺丝原液,采用共混添加法制备维生素E保健纤维素纤维纺丝原液,用落球法和RT-2000的毛细管流变仪测试了纯纤维素溶液及添加不同量包合物的混合溶液的流变性能,通过试验确定:以聚合度为650,浓度为5%的纤维素溶液为纺丝原液最为合适;在纤维素溶液中添加维生素E-β-环糊精包合物并不改变溶液的流动类型,随着包合物含量的增加,溶液非牛顿指数减小,结构粘度指数增加,可纺性变差。在流变性能测试的基础上进行湿法纺丝,制得纯纤维素纤维和维生素E纤维素纤维,研究了纺丝条件对纤维强力性能的影响,并用单纤强力仪、红外、XRD、热失重等手段测试了所制得的维生素E保健纤维的各项性能;结果显示两步凝固浴法比一步凝固浴法获得的纤维强力性能优异,最佳凝固浴组成分别为:第一凝固浴为10wt%H_2SO_4/10wt%Na_2SO_4水溶液,第二凝固浴为5wt%H_2SO_4水溶液;最佳凝固浴温度为20℃;最佳工艺条件下得到的纯纤维素纤维断裂强力为2.22cN/dtex,随着包合物含量增加,维生素E护肤纤维的断裂强力先是略有增加继而降低,包合物含量为10%时,纤维强力最好,为2.28cN/dtex;扫描电镜照片显示,制得的纤维具有圆型截面,表面和截面均显示光滑和均相的形态;纤维断面的扫描电镜照片显示,在维生素E-β-环糊精包合物含量达15%时出现一定团聚,但团聚颗粒分布均匀;热失重分析结果显示,维生素E纤维素纤维相比纯纤维素纤维热稳定性稍有降低,原因可能是维生素E-β-环糊精包合物的加入导致纤维素大分子之间的分子力降低,经硝酸氧化法鉴定证实采用添加法制备的纤维中确实含有维生素E。
Functional aspects for clothing textiles,which promote the wearing comfort and well-being have become a striking sales argument.Skin-care textile containing vitamin is one of the functional textiles.Cellulose fiber containning vitamin E was prepared in this paper.In order to get cellulose fiber containning vitamin E,preparation of the micro-capsule of vitamin E,the inclusion compound of vitamin E andβ-cyclodextrin, and cellulose solution was investigated,then the fiber was wet-spun by mixing the compound in the cellulose solution.
The complex of vitamin E andβ-cyclodextrin was prepared,and the prepared inclusion compound was analysed by using UV,FTIR,XRD,TG etc.It is found that the inclusion ratio of vitamin E andβ-cyclodextrin is 1:1.The stability of the complex to the UV light and heat is excellent.And the complex of vitamin E andβ-cyclodextrin possesses desirable slow release property,which is best in 35-40℃.
To get desirable cellulose spinning solution,dissolution of cellulose in NaOH/Urea/Thiourea aqueous solution and ionic liquids(AMIMC1 and BMIMC1) was researched in this paper.7wt%NaOH/9wt%Urea/9wt%Thiourea aqueous solution and AMIMC1 were found have the greatest power to dissolve cellulose.Throgh investigating the dissolution condition and properties of the regenerated cellulose, 7wt%NaOH/9wt%Urea/9wt%Thiourea aqueous solution,the preferable solvent,is chose for preparing the spinning solution.
Cellulose spinning solution containing the vitamin E/β-cyclodextrin complex was prepared by mixing the complex in the cellulose solution.Rheological property of cellulose solution and that containing the vitamin E/β-cyclodextrin complex was tested by the falling sphere vis-cometer and capillary rheometer.Cellulose with(?)=650 was found be best for preparing the spinning solution,and 5%was the optimal concentration of spinning solution.The flow behavior of the spinning solution was not changed by blending of the complex in cellulose solution,whose non-newtonian index decreased as the content of the added complex increased.
Based on the study of rheological property of the cellulose solution,the cellulose fiber and the skin-care fiber containing vitamin E was made by wetting spinning method.The coagulant composition and condition was researched.It was found that fiber spun from two-step coagulation was better than one step coagulant,and the composition of the two coagulant was 10wt%H_2SO_4/10wt%Na_2SO_4 aqueous solutioin and 5wt%H_2SO_4 aqueous solution respectively,and the best coagulating temperature was 20℃.And the most appropriate content of the comlex is 10%.The stength of cellulose fiber and that containning vitamin E spun with the best spinning technique was 2.22cN/dtex and 2.28 cN/dtex.Round cross-section,smooth surface and even distribution was observed in the SEM photograph of the prepared fiber.
以β-环糊精为壁材,制备了维生素E-β-环糊精的包合物,采用紫外-可见光谱、红外、XRD、TG等方式对包合物进行了鉴定和表征,并对所制备的包合物的缓释性能进行了测试:结果证实维生素E与β-环糊精以1∶1的比例形成包合物,维生素E的色满酚结构进入环糊精空腔之中;所制备的包合物耐热和耐紫外光性能良好;具有良好的缓释性能。研究了NaOH/Urea/Thiourea水溶液和[AMIM]Cl(1-烯丙基-3甲基氯代咪唑)两种溶剂体系对纤维素的溶解情况,综合考虑两种溶剂体系的溶解过程、所需条件和溶解再生后纤维素的各项性能,选择NaOH/Urea/Thiourea水溶液作为纤维素溶剂制备纤维素纤维的纺丝原液,采用共混添加法制备维生素E保健纤维素纤维纺丝原液,用落球法和RT-2000的毛细管流变仪测试了纯纤维素溶液及添加不同量包合物的混合溶液的流变性能,通过试验确定:以聚合度为650,浓度为5%的纤维素溶液为纺丝原液最为合适;在纤维素溶液中添加维生素E-β-环糊精包合物并不改变溶液的流动类型,随着包合物含量的增加,溶液非牛顿指数减小,结构粘度指数增加,可纺性变差。在流变性能测试的基础上进行湿法纺丝,制得纯纤维素纤维和维生素E纤维素纤维,研究了纺丝条件对纤维强力性能的影响,并用单纤强力仪、红外、XRD、热失重等手段测试了所制得的维生素E保健纤维的各项性能;结果显示两步凝固浴法比一步凝固浴法获得的纤维强力性能优异,最佳凝固浴组成分别为:第一凝固浴为10wt%H_2SO_4/10wt%Na_2SO_4水溶液,第二凝固浴为5wt%H_2SO_4水溶液;最佳凝固浴温度为20℃;最佳工艺条件下得到的纯纤维素纤维断裂强力为2.22cN/dtex,随着包合物含量增加,维生素E护肤纤维的断裂强力先是略有增加继而降低,包合物含量为10%时,纤维强力最好,为2.28cN/dtex;扫描电镜照片显示,制得的纤维具有圆型截面,表面和截面均显示光滑和均相的形态;纤维断面的扫描电镜照片显示,在维生素E-β-环糊精包合物含量达15%时出现一定团聚,但团聚颗粒分布均匀;热失重分析结果显示,维生素E纤维素纤维相比纯纤维素纤维热稳定性稍有降低,原因可能是维生素E-β-环糊精包合物的加入导致纤维素大分子之间的分子力降低,经硝酸氧化法鉴定证实采用添加法制备的纤维中确实含有维生素E。
Functional aspects for clothing textiles,which promote the wearing comfort and well-being have become a striking sales argument.Skin-care textile containing vitamin is one of the functional textiles.Cellulose fiber containning vitamin E was prepared in this paper.In order to get cellulose fiber containning vitamin E,preparation of the micro-capsule of vitamin E,the inclusion compound of vitamin E andβ-cyclodextrin, and cellulose solution was investigated,then the fiber was wet-spun by mixing the compound in the cellulose solution.
The complex of vitamin E andβ-cyclodextrin was prepared,and the prepared inclusion compound was analysed by using UV,FTIR,XRD,TG etc.It is found that the inclusion ratio of vitamin E andβ-cyclodextrin is 1:1.The stability of the complex to the UV light and heat is excellent.And the complex of vitamin E andβ-cyclodextrin possesses desirable slow release property,which is best in 35-40℃.
To get desirable cellulose spinning solution,dissolution of cellulose in NaOH/Urea/Thiourea aqueous solution and ionic liquids(AMIMC1 and BMIMC1) was researched in this paper.7wt%NaOH/9wt%Urea/9wt%Thiourea aqueous solution and AMIMC1 were found have the greatest power to dissolve cellulose.Throgh investigating the dissolution condition and properties of the regenerated cellulose, 7wt%NaOH/9wt%Urea/9wt%Thiourea aqueous solution,the preferable solvent,is chose for preparing the spinning solution.
Cellulose spinning solution containing the vitamin E/β-cyclodextrin complex was prepared by mixing the complex in the cellulose solution.Rheological property of cellulose solution and that containing the vitamin E/β-cyclodextrin complex was tested by the falling sphere vis-cometer and capillary rheometer.Cellulose with(?)=650 was found be best for preparing the spinning solution,and 5%was the optimal concentration of spinning solution.The flow behavior of the spinning solution was not changed by blending of the complex in cellulose solution,whose non-newtonian index decreased as the content of the added complex increased.
Based on the study of rheological property of the cellulose solution,the cellulose fiber and the skin-care fiber containing vitamin E was made by wetting spinning method.The coagulant composition and condition was researched.It was found that fiber spun from two-step coagulation was better than one step coagulant,and the composition of the two coagulant was 10wt%H_2SO_4/10wt%Na_2SO_4 aqueous solutioin and 5wt%H_2SO_4 aqueous solution respectively,and the best coagulating temperature was 20℃.And the most appropriate content of the comlex is 10%.The stength of cellulose fiber and that containning vitamin E spun with the best spinning technique was 2.22cN/dtex and 2.28 cN/dtex.Round cross-section,smooth surface and even distribution was observed in the SEM photograph of the prepared fiber.
引文
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