CN107604678A - 一种丁烯酸酯‑接枝淀粉及其制备方法与应用 - Google Patents
一种丁烯酸酯‑接枝淀粉及其制备方法与应用 Download PDFInfo
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Abstract
本发明公开了一种丁烯酸酯‑接枝淀粉及其制备方法与应用,涉及材料领域。本发明的一种丁烯酸酯‑接枝淀粉浆纱性能高,挂浆率高,能够用于织物提高织物与人体接触面的舒适程度,具有良好的亲肤透气性,同时,本发明的一种丁烯酸酯‑接枝淀粉对棉纤维具有良好的黏附性,增强纤维之间的抱合。
Description
本申请是发明名称为“一种防紫外线织物”的分案申请
原申请的申请日为:2015-12-07
原申请的申请号为:2015108834059。
技术领域
本发明涉及一种材料,尤其是一种丁烯酸酯-接枝淀粉及其制备方法与应用。
背景技术
随着技术发展和社会的不断进步,人们在生活水平大大提高的同时,对生活质量的要求也越来越高,全球环境遭到破坏的今天,返璞归真,回归大自然已经成为人们衡量生活质量的重要标准,穿着节能环保的纤维制品,是当今人们的时尚追求。高新技术的发展,使纺织纤维新原料开发也得到了快速发展,各种新型绿色环保纤维不断被研发面世。
然而现有技术中的纤维织物功能性较为单一,无法在满足人体穿着舒适度的同时,具有良好防紫外线功能。
发明内容
本发明的发明目的在于:针对上述存在的问题,提供一种在满足人体穿着舒适度的同时,具有良好防紫外线功能的防紫外线织物。
本发明采用的技术方案如下:
本发明的一种防紫外线织物,包括混纺层,所述混纺层由16.3%壳聚糖纤维,19.7%石墨烯粘胶复合纤维和64%棉纤维组成。
由于采用了上述技术方案,独立棉纤维的舒适度高,但是纤维的断裂强度较低,衣物很容易失去光泽;壳聚糖纤维是由海洋生物提取的纯天然绿色纤维,具有良好的通透性、吸湿性和保湿性、生物相容性、无免疫原性和可生物降解性,但壳聚糖纤维转曲少,强度低,抱合力差,吸放湿速度快,回潮率低于15%时静电现象严重,壳聚糖纤维开松较难,有较多硬并丝,纯纺生条难度较大;石墨烯粘胶复合纤维的断裂强度大,且具有良好的阻燃性,和防紫外线性能,将三者进行混纺可以综合各自的优点,避开缺陷,得到的复合纤维不仅断裂强度得到提高,在具有良好亲肤舒适性的同时具有防紫外线的功能。
本发明的一种防紫外线织物,所述混纺层的上表面覆有碳纤维-聚醚型聚氨酯层,所述混纺层的下表面覆有丁烯酸酯-接枝淀粉层,所述碳纤维-聚醚型聚氨酯层的厚度为400μm,所述混纺层的厚度为0.2cm,所述丁烯酸酯-接枝淀粉层的厚度为600μm。
由于采用了上述技术方案,混纺层上表面的碳纤维-聚醚型聚氨酯层具有良好的耐热性,同时具有高弹性、高韧性和优良的耐磨性,在织物的表面覆有该层,可以增加衣物的使用寿命,同时在衣物表面出现污渍时,方便清洁;在火灾等突发危险状况时,该层的耐热特性可以保证衣物不会着火,增加逃生的几率。
丁烯酸酯-接枝淀粉层对棉纤维具有良好的黏附性,增强纤维之间的抱合,同时该层的浆纱性能高,挂浆率高,能够提高织物与人体接触面的舒适程度,具有良好的亲肤透气性。
本发明的一种防紫外线织物,所述棉纤维经过预处理,所述预处理的步骤为,
步骤一:取0.1mol/L的柠檬酸2.0mL与0.1mol/L的柠檬酸钠18.0mL配制成为pH为6.4的柠檬酸-柠檬酸钠缓冲溶液;
步骤二:将棉纤维完全浸泡入缓冲溶液中,按照棉纤维:羟基羧酸质量比1:0.04向缓冲溶液中加入羟基羧酸,按照棉纤维:羧酸基甜菜碱质量比1:0.08向缓冲溶液中加入羧酸基甜菜碱,浸泡30min;
步骤四:按照棉纤维:果胶酶:纤维素酶质量比1:0.05:0.02向缓冲液中加入果胶酶和纤维素酶,水浴加热至27℃,恒温搅拌5min后,按照棉纤维:脂肪酶质量比1:0.01向缓冲液中加入脂肪酶,水浴升温至32℃,恒温搅拌8min;
步骤五:将棉纤维取出放置在鼓风干燥箱中,在温度为105℃的条件下将棉纤维彻底烘干,将棉纤维放入液氮中超低温处理30min;
步骤六:将经过超低温处理的棉纤维放入温度为52℃的pH为6.4的柠檬酸-柠檬酸钠缓冲溶液中,加热恢复至室温后放置在鼓风干燥箱中,在温度为105℃的条件下将棉纤维彻底烘干,得到经过预处理的棉纤维。
本发明的一种防紫外线织物,所述石墨烯粘胶复合纤维通过以下步骤制备而成,
步骤一:按浓硫酸:石墨粉:硝酸钠质量比65:1:0.6在冰浴的条件下向浓硫酸中加入石墨粉和硝酸钠,搅拌溶解30min后,按照石墨粉:高锰酸钾质量比1:5,向混合溶液中加入高锰酸钾,搅拌10h后,按照浓硫酸:去离子水体积比1:1向混合溶液中加入去离子水,将混合物置于真空度为0.93的条件下,按照1.2℃/h的速率缓慢升温至52℃,保持52℃恒温继续搅拌22h后,按照浓硫酸比双氧水体积比1:0.1向混合溶液中加入双氧水,在52℃温度下搅拌2.5h后离心,将固液分离取固体,固体分别用5%的稀盐酸和去离子水冲洗,干燥后得到氧化石墨烯;
步骤二:将氧化石墨烯以1000 mL/h的挤出速度在一字形模口的制备装置中挤出,于10℃的凝固液中停留凝固成氧化石墨烯水凝胶膜;
步骤三:称取一份氧化石墨烯水凝胶膜,按照氧化石墨烯水凝胶膜:粘胶纺丝原液摩尔比1:20将氧化石墨烯水凝胶膜与粘胶纺丝原液均匀混合,通过环境温度为27℃,环境湿度为43.6%,电压为11.4kV,接收距离为12cm的直流电场,进行静电纺丝,得到石墨烯粘胶复合纤维。
本发明的一种防紫外线织物,所述碳纤维-聚醚型聚氨酯层通过将碳纤维-聚醚型聚氨酯高温喷涂至混纺层上表面,所述丁烯酸酯-接枝淀粉层通过将丁烯酸酯-接枝淀粉高温喷涂至混纺层下表面。
由于采用了上述技术方案,高温喷涂至混纺层表面的碳纤维-聚醚型聚氨酯和丁烯酸酯-接枝淀粉能够在一定程度上渗入混纺层的分子间隙中,增加三种材料的结合度。
本发明的一种防紫外线织物,所述碳纤维-聚醚型聚氨酯通过以下步骤制备而成,
步骤一:取一份甲氧基硅烷用适量甲醇稀释,取一份乙氧基硅烷用适量乙醇稀释,将稀释的甲氧基硅烷和稀释的乙氧基硅烷等比例混合,按照甲氧基硅烷:水摩尔比1:5向混合溶液中加入去离子水,加入乙酸调节溶液pH为5.1,常温搅拌至完全溶解;
步骤二:按照甲氧基硅烷:碳纤维摩尔比1:2向溶液中加入碳纤维,常温搅拌30min,放入鼓风干燥箱中,在温度为120℃的条件下烘干2h,制得碳纤维处理液;
步骤三:称取一份四氢呋喃均聚醚,加入适量甲醇作为溶液,按照四氢呋喃均聚醚:碳纤维摩尔比1:0.6向溶液中加入碳纤维处理液,加热至65℃,搅拌反应15min,按照四氢呋喃均聚醚:二苯基甲烷二异氰酸酯摩尔比1:0.1向溶液中加入二苯基甲烷二异氰酸酯,加热回流反应5h,完全反应后,旋转蒸发仪蒸去溶剂,制得预聚体;
步骤三:取一份预聚体加热至85℃,按照预聚体:1,4-丁二醇摩尔比1:1向预聚体中加入1,4-丁二醇搅拌混合5min,在70kPa的压力条件下冷却至常温,得到碳纤维-聚醚型聚氨酯。
本发明的一种防紫外线织物,所述丁烯酸酯-接枝淀粉通过以下步骤制备而成,
步骤一:称取一份淀粉,取适量水作为溶剂,调节溶液pH为4.7,加入适量异丙醇配制成为淀粉质量分数为37%的悬浮液,搅拌30min;
步骤二:按照淀粉:NaOH质量比1:0.05向溶液中加入NaOH,加热升温至30℃,恒温搅拌30min,按照NaOH:烯丙基氯摩尔比1:1.2向溶液中缓慢滴加烯丙基氯,升温至50℃,恒温搅拌24h;
步骤三:过滤,取固体重新分散于体积比为18:82的蒸馏水-乙醇溶液中,用醋酸调节pH至7,抽滤后用适量蒸馏水洗涤,干燥得到烯丙基醚化淀粉;
步骤四:取一份烯丙基醚化淀粉,取适量水作为溶剂,配置成为质量分数为37%的悬浮液,用醋酸调节pH为4.2,通入氮气作为保护气;
步骤五:在保护气存在下按照烯丙基醚化淀粉:丁烯酸酯:丁烯酸:过氧化二叔丁基醚摩尔比1:1:1.5:1.2向溶液中同时缓慢滴加丁烯酸酯,丁烯酸和过氧化二叔丁基醚,常温搅拌3h,调节pH为7,过滤,取固体干燥制得丁烯酸酯-接枝淀粉。
本发明的一种防紫外线织物,所述混纺层由棉纤维梭织后,壳聚糖纤维与石墨烯粘胶复合纤维穿绕而成;所述棉纤维梭织的经纱为50支,纬纱为45支,经纬密度为108*58;所述壳聚糖纤维沿棉纤维梭织的经向穿绕,所述石墨烯粘胶沿棉纤维梭织的维向穿绕。
由于采用了上述技术方案,得到的混纺层在节约成本的前提下最大限度的提高断裂强度,UV透过率为3.7%。
综上所述,由于采用了上述技术方案,本发明的有益效果是:
1.可以增加织物的使用寿命,同时在织物表面出现污渍时,方便清洁。
2.在保证亲肤舒适度的同时,具有良好的耐热阻燃特性及防紫外线特性,提高了纤维的断裂强度,延长了织物的寿命。
具体实施方式
下面对本发明作详细的说明。
为了使发明的目的、技术方案及优点更加清楚明白,以下结合实施例,对本发明进行进一步详细说明。应当理解,此处所描述的具体实施例仅仅用以解释本发明,并不用于限定本发明。
实施例1
一种防紫外线织物,包括混纺层,混纺层由16.3%壳聚糖纤维,19.7%石墨烯粘胶复合纤维和64%棉纤维组成。
混纺层的上表面覆有碳纤维-聚醚型聚氨酯层,所述混纺层的下表面覆有丁烯酸酯-接枝淀粉层,所述碳纤维-聚醚型聚氨酯层的厚度为400μm,所述混纺层的厚度为0.2cm,所述丁烯酸酯-接枝淀粉层的厚度为600μm。
碳纤维-聚醚型聚氨酯层通过将碳纤维-聚醚型聚氨酯经过高温熔融后喷涂至混纺层上表面,丁烯酸酯-接枝淀粉层通过将丁烯酸酯-接枝淀粉高温熔融后喷涂至混纺层下表面。
混纺层由棉纤维梭织后,壳聚糖纤维与石墨烯粘胶复合纤维穿绕而成;棉纤维梭织的经纱为50支,纬纱为45支,经纬密度为108*58;壳聚糖纤维沿棉纤维梭织的经向穿绕,石墨烯粘胶沿棉纤维梭织的维向穿绕。
实施例2
本发明的一种防紫外线织物,其中棉纤维经过预处理,预处理的步骤为,
步骤一:取0.1mol/L的柠檬酸2.0mL与0.1mol/L的柠檬酸钠18.0mL配制成为pH为6.4的柠檬酸-柠檬酸钠缓冲溶液;
步骤二:将棉纤维完全浸泡入缓冲溶液中,按照棉纤维:羟基羧酸质量比1:0.04向缓冲溶液中加入羟基羧酸,按照棉纤维:羧酸基甜菜碱质量比1:0.08向缓冲溶液中加入羧酸基甜菜碱,浸泡30min;
步骤四:按照棉纤维:果胶酶:纤维素酶质量比1:0.05:0.02向缓冲液中加入果胶酶和纤维素酶,水浴加热至27℃,恒温搅拌5min后,按照棉纤维:脂肪酶质量比1:0.01向缓冲液中加入脂肪酶,水浴升温至32℃,恒温搅拌8min;
步骤五:将棉纤维取出放置在鼓风干燥箱中,在温度为105℃的条件下将棉纤维彻底烘干,将棉纤维放入液氮中超低温处理30min;
步骤六:将经过超低温处理的棉纤维放入温度为52℃的pH为6.4的柠檬酸-柠檬酸钠缓冲溶液中,加热恢复至室温后放置在鼓风干燥箱中,在温度为105℃的条件下将棉纤维彻底烘干,得到经过预处理的棉纤维。
实施例3
本发明的一种防紫外线织物,石墨烯粘胶复合纤维通过以下步骤制备而成,
步骤一:按浓硫酸:石墨粉:硝酸钠质量比65:1:0.6在冰浴的条件下向浓硫酸中加入石墨粉和硝酸钠,搅拌溶解30min后,按照石墨粉:高锰酸钾质量比1:5,向混合溶液中加入高锰酸钾,搅拌10h后,按照浓硫酸:去离子水体积比1:1向混合溶液中加入去离子水,将混合物置于真空度为0.93的条件下,按照1.2℃/h的速率缓慢升温至52℃,保持52℃恒温继续搅拌22h后,按照浓硫酸比双氧水体积比1:0.1向混合溶液中加入双氧水,在52℃温度下搅拌2.5h后离心,将固液分离取固体,固体分别用5%的稀盐酸和去离子水冲洗,干燥后得到氧化石墨烯;
步骤二:将氧化石墨烯以1000 mL/h的挤出速度在一字形模口的制备装置中挤出,于10℃的凝固液中停留凝固成氧化石墨烯水凝胶膜;
步骤三:称取一份氧化石墨烯水凝胶膜,按照氧化石墨烯水凝胶膜:粘胶纺丝原液摩尔比1:20将氧化石墨烯水凝胶膜与粘胶纺丝原液均匀混合,通过环境温度为27℃,环境湿度为43.6%,电压为11.4kV,接收距离为12cm的直流电场,进行静电纺丝,得到石墨烯粘胶复合纤维。
实施例4
本发明的一种防紫外线织物,碳纤维-聚醚型聚氨酯通过以下步骤制备而成,
步骤一:取一份甲氧基硅烷用适量甲醇稀释,取一份乙氧基硅烷用适量乙醇稀释,将稀释的甲氧基硅烷和稀释的乙氧基硅烷等比例混合,按照甲氧基硅烷:水摩尔比1:5向混合溶液中加入去离子水,加入乙酸调节溶液pH为5.1,常温搅拌至完全溶解;
步骤二:按照甲氧基硅烷:碳纤维摩尔比1:2向溶液中加入碳纤维,常温搅拌30min,放入鼓风干燥箱中,在温度为120℃的条件下烘干2h,制得碳纤维处理液;
步骤三:称取一份四氢呋喃均聚醚,加入适量甲醇作为溶液,按照四氢呋喃均聚醚:碳纤维摩尔比1:0.6向溶液中加入碳纤维处理液,加热至65℃,搅拌反应15min,按照四氢呋喃均聚醚:二苯基甲烷二异氰酸酯摩尔比1:0.1向溶液中加入二苯基甲烷二异氰酸酯,加热回流反应5h,完全反应后,旋转蒸发仪蒸去溶剂,制得预聚体;
步骤四:取一份预聚体加热至85℃,按照预聚体:1,4-丁二醇摩尔比1:1向预聚体中加入1,4-丁二醇搅拌混合5min,在70kPa的压力条件下冷却至常温,得到碳纤维-聚醚型聚氨酯。
实施例5
本发明的一种防紫外线织物,丁烯酸酯-接枝淀粉通过以下步骤制备而成,
步骤一:称取一份淀粉,取适量水作为溶剂,调节溶液pH为4.7,加入适量异丙醇配制成为淀粉质量分数为37%的悬浮液,搅拌30min;
步骤二:按照淀粉:NaOH质量比1:0.05向溶液中加入NaOH,加热升温至30℃,恒温搅拌30min,按照NaOH:烯丙基氯摩尔比1:1.2向溶液中缓慢滴加烯丙基氯,升温至50℃,恒温搅拌24h;
步骤三:过滤,取固体重新分散于体积比为18:82的蒸馏水-乙醇溶液中,用醋酸调节pH至7,抽滤后用适量蒸馏水洗涤,干燥得到烯丙基醚化淀粉;
步骤四:取一份烯丙基醚化淀粉,取适量水作为溶剂,配置成为质量分数为37%的悬浮液,用醋酸调节pH为4.2,通入氮气作为保护气;
步骤五:在保护气存在下按照烯丙基醚化淀粉:丁烯酸酯:丁烯酸:过氧化二叔丁基醚摩尔比1:1:1.5:1.2向溶液中同时缓慢滴加丁烯酸酯,丁烯酸和过氧化二叔丁基醚,常温搅拌3h,调节pH为7,过滤,取固体干燥制得丁烯酸酯-接枝淀粉。
以上所述仅为本发明的较佳实施例而已,并不用以限制本发明,凡在本发明的精神和原则之内所作的任何修改、等同替换和改进等,均应包含在本发明的保护范围之内。
Claims (7)
1.一种丁烯酸酯-接枝淀粉的制备方法,其特征在于,其包括:
步骤一:称取一份淀粉,取适量水作为溶剂,调节溶液pH为4.7,加入适量异丙醇配制成为淀粉质量分数为37%的悬浮液,搅拌30min;
步骤二:按照淀粉:NaOH质量比1:0.05向溶液中加入NaOH,加热升温至30℃,恒温搅拌30min,按照NaOH:烯丙基氯摩尔比1:1.2向溶液中缓慢滴加烯丙基氯,升温至50℃,恒温搅拌24h;
步骤三:过滤,取固体重新分散于体积比为18:82的蒸馏水-乙醇溶液中,用醋酸调节pH至7,抽滤后用适量蒸馏水洗涤,干燥得到烯丙基醚化淀粉;
步骤四:取一份烯丙基醚化淀粉,取适量水作为溶剂,配置成为质量分数为37%的悬浮液,用醋酸调节pH为4.2,通入氮气作为保护气;
步骤五:在保护气存在下按照烯丙基醚化淀粉:丁烯酸酯:丁烯酸:过氧化二叔丁基醚摩尔比1:1:1.5:1.2向溶液中同时缓慢滴加丁烯酸酯,丁烯酸和过氧化二叔丁基醚,常温搅拌3h,调节pH为7,过滤,取固体干燥制得丁烯酸酯-接枝淀粉。
2.一种丁烯酸酯-接枝淀粉,其特征在于,其由权利要求1所述的制备方法制备而成。
3.权利要求2所述的丁烯酸酯-接枝淀粉在制备防紫外线织物中的应用。
4.根据权利要求3的应用,其特征在于,所述防紫外线织物包括混纺层,所述混纺层上表面覆有碳纤维-聚醚型聚氨酯层,所述混纺层的下表面覆有丁烯酸酯-接枝淀粉层。
5.根据权利要求4所述的应用,其特征在于,所述碳纤维-聚醚型聚氨酯层的厚度为400μm,所述混纺层的厚度为0.2cm,所述丁烯酸酯-接枝淀粉层的厚度为600μm。
6.根据权利要求5所述的应用,其特征在于,所述混纺层由16.3%壳聚糖纤维,19.7%石墨烯粘胶复合纤维和64%棉纤维组成。
7.根据权利要求6所述的应用,其特征在于,所述棉纤维经过预处理,所述预处理的步骤为,
步骤一:取0.1mol/L的柠檬酸2.0mL与0.1mol/L的柠檬酸钠18.0mL配制成为pH为6.4的柠檬酸-柠檬酸钠缓冲溶液;
步骤二:将棉纤维完全浸泡入缓冲溶液中,按照棉纤维:羟基羧酸质量比1:0.04向缓冲溶液中加入羟基羧酸,按照棉纤维:羧酸基甜菜碱质量比1:0.08向缓冲溶液中加入羧酸基甜菜碱,浸泡30min;
步骤三:按照棉纤维:果胶酶:纤维素酶质量比1:0.05:0.02向缓冲液中加入果胶酶和纤维素酶,水浴加热至27℃,恒温搅拌5min后,按照棉纤维:脂肪酶质量比1:0.01向缓冲液中加入脂肪酶,水浴升温至32℃,恒温搅拌8min;
步骤四:将棉纤维取出放置在鼓风干燥箱中,在温度为105℃的条件下将棉纤维彻底烘干,将棉纤维放入液氮中超低温处理30min;
步骤五:将经过超低温处理的棉纤维放入温度为52℃的pH为6.4的柠檬酸-柠檬酸钠缓冲溶液中,加热恢复至室温后放置在鼓风干燥箱中,在温度为105℃的条件下将棉纤维彻底烘干,得到经过预处理的棉纤维。
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