CN115074883A - 一种光热防伪纱线及其制备方法和应用 - Google Patents
一种光热防伪纱线及其制备方法和应用 Download PDFInfo
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Abstract
本发明涉及一种光热防伪纱线及其制备方法和应用,将纤维素形成的纺丝液提供给喷丝板,挤出的溶液通过高速热空气进行拉伸,并在水雾凝固室中凝固,进行牵伸,得到的长丝束浸渍到铯盐溶液中,同时棉短纤纱浸渍到钨酸盐溶液中,长丝束与棉短纤维纱进行赛络菲尔纺,纺出的纱浸渍在还原剂中进行原位反应,最后通过洗涤和干燥得到光热防伪纱线。本发明采用铯、钨离子对纱线进行防伪加密,可通过对金属铯、钨离子进行检测追踪识别光热纱线真伪。
Description
技术领域
本发明涉及纺丝技术与防伪检测技术领域,尤其涉及一种光热防伪纱线及其制备方法和应用。
背景技术
近年来,光热衣物深受人们青睐,冬天人们需要穿较多的衣服进行保温,为了使衣物具有较好的保暖性能,往往在其中会填充一些蓬松质材料以增添其中的静止空气含量,进而防止热量散失,达到恒温保暖的目的。目前来看,光热纱线的应用研究较少,中国专利CN201410157524.1提供一种太阳能相变储热纱线制造方法,将相变材料的制造、纤维材料混合、开棉、梳棉、并条、制粗纱、制细纱、络筒、染色等工序,所述相变材料制造为将相变材料进行微珠包覆。太阳能相变储热纱线制造方法具有可靠性高、光热能力好、温度适应性好、在常温下工作、材料寿命长,制造简便、使用范围广等优点,但这种相变储热纱线的制备具有较差的力学性能,毛羽数量较多。中国专利CN202110750958.2提供一种浆纱涂覆光热相变复合纱线及其制备方法,首先配置聚乙烯醇缩丁醛/碳化锆/氧化铝悬浮液和聚乙烯醇缩丁醛溶液;然后制备熔融态石蜡材料;最后以聚乙烯醇缩丁醛/碳化锆/氧化铝涂层为表层,以石蜡为中间层,以涤纶/聚乙烯醇缩丁醛/碳化锆/氧化铝复合纱线或纯涤纶纱线为芯纱,通过涂覆法制备涤纶/聚乙烯醇缩丁醛/碳化锆/氧化铝/石蜡复合纱线。此发明具有光热转换功能,光热转换效率较高;具有相变功能,可实现储热调温;制备方法简单、经济、快速;使用寿命长,形稳性较好。但存在光热相变材料脱落的问题,多次洗涤之后效率存在下降的趋势。中国专利CN202110750956.3提供一种光热转换多功能织物及其制备方法,将碳化锆加入到聚合物溶液中,搅拌均匀,然后进行超声震荡,制成聚合物-ZrC悬浊液;将纱线顺次通过聚合物-ZrC悬浊液浆槽和浆纱机的烘筒,制得纱线/聚合物/ZrC复合纱线;将纱线/聚合物/ZrC复合纱线进行织造得到具有光热转换功能的多功能织物。此发明的织物具有以下优点:具有优异的光热转换功能和抗紫外功能,吸光能力强,光热转换效率高且可调节;制备过程简单,纱线采用传统上浆工艺即可;加工过程不损害纱线,且增强了纱线的物理化学性能;可多次循环使用,耐洗涤,循环稳定性好。但由于通过上浆方式将光热物质涂覆在织物表面难免会发生脱落现象,并不能保证使用寿命长。
本发明旨在提供一种采用铯钨青铜材料制备的纱线,铯钨青铜材料具有价格低廉、无毒、环保、光热能力强等特点,具有很大潜力应用前景。目前,关于铯钨材料的纺织应用屡见不鲜。如专利CN202111542562.5公开了一种具有紫外及近红外屏蔽性能的蚕丝纤维,该蚕丝纤维中包含纳米钨青铜(如纳米铯钨青铜),钨青铜是一种具有混合价态钨离子化合物,具有近红外屏蔽性能,从而使蚕丝纤维具有出色的紫外及近红外遮蔽性能,可以控制人体散热,为提高人体热舒适度和降低建筑能耗提供了有效途径。其制备时将钨青铜作为家蚕饲料喂养家蚕,随后将得到的蚕茧进行处理,得到所述蚕丝纤维。专利CN201922080925.2公开了一种保暖面料,其在印刷底层中添加钨酸铯蓄热保温材料。CN201610621351.3公开了一种光能纤维,其通过将铯钨复合材料和纤维原材料切片混合熔融后,经过纺丝得到。肖沭等(基于光蓄热温敏变色织物的制备与性能,2022)采用纳米铯钨粉作为光蓄热材料,温敏变色微胶囊作为显色材料,将纳米铯钨粉和显色材料混色染料通过丝网印花印制在涤纶双层织物上,以实现蓄热和温敏变色。伊利强(静电纺丝法制备智能纳米调温纤维及其性能研究,2021)以PVB为皮,以正十八烷为芯,制备了皮芯型相变调温材料,并通过在皮层中添加铯钨青铜使复合纤维具有吸收近红外光并转换成热能的功能。综上,现有技术将铯钨青铜材料用于纺织品时,均是直接将铯钨青铜涂覆或混合在纺丝液中,直接涂覆会导致铯钨青铜材料易脱落,从而影响光热性能以及防伪效果,混在纺丝液中将会导致铯钨青铜材料只在纤维素里而不存在于棉纤维中,影响光热性能,因此仍需进一步改进。
发明内容
为解决上述技术问题,本发明提供了一种基于铯钨青铜材料的光热防伪纱线,通过原位反应实现负载而非直接涂覆或复合,使本发明制备的光热防伪纱线稳定性更高,选择合适的载体纤维提高纱线的机械性能和负载效率,在防伪检测时,铯钨青铜材料与丝和棉纺织而成的纱线结合更紧密,保证了检测准确度,即使洗涤多次之后仍然保持较好的光热性能和防伪性能,应用性强。
本发明的第一个目的是提供一种光热防伪纱线的制备方法,包括以下步骤:
S1、将纤维素形成的纺丝液通过湿式溶液吹纺得到长束丝,将长丝束浸渍到第一溶液中;将棉纤维浸渍到第二溶液中;
当第一溶液为铯盐溶液时,第二溶液为钨酸盐溶液;当第一溶液为钨酸盐溶液时,第二溶液为铯盐溶液;
S2、以步骤S1得到的长束丝和棉纤维进行赛络菲尔纺;
S3、将步骤S2得到的纱线浸渍在还原剂中反应,经洗涤、干燥后得到所述光热防伪纱线。
进一步地,在步骤S1中,所述纺丝液是将纤维素溶于1-乙基-3-甲基咪唑磷酸二乙酯盐离子液体(EMIMDEP)形成的溶液,优选在90-110℃下进行微波溶解。在纺丝时,溶剂应可溶解聚合物以形成具有一定含量和黏度的溶液,并且对其挥发性、电荷、含量等都有一定限定,以调节纤维尺寸、形貌等特征,因此,本发明中选择离子液体EMIMDEP溶解纤维素,并通过优化工艺参数(温度、溶解手段等)以便于后续纺丝及离子负载。
进一步地,在步骤S1中,纺丝液的浓度为5-10wt%。
进一步地,在步骤S1中,所述的湿式溶液吹纺,挤出的纺丝液通过高速热空气在气隙上拉伸,并在水雾凝固室中凝固,其中,高速热空气的温度保持在140-180℃。
进一步地,在步骤S1中,铯盐包括但不限于碳酸铯、硫酸铯、氯化铯等,其浓度为0.1-0.5mol/L。
进一步地,在步骤S1中,钨酸盐包括但不限于钨酸钠、钨酸钾等,其浓度为0.1-0.5mol/L。
进一步地,在步骤S2中,进行赛络菲尔纺时,棉纤维刚进入纺纱工艺时是粗纱,随后纺成细纱,粗纱捻系数65-74,锭速490-500r/min,细纱牵伸倍数31-34,锭速为1250-1300r/min。由于赛络菲尔纺工艺,通过棉纤维与纤维素的复合,使制备得到光热防伪纱线具有生物降解性、良好的热稳定性和优异的机械性能。
进一步地,在步骤S3中,还原剂优选为柠檬酸溶液。
进一步地,在步骤S3中,柠檬酸溶液的浓度为0.5-1.5mol/L,溶液温度为180-200℃。
进一步地,在步骤S3中,采用醇溶液进行洗涤,除去表面杂质,优选为乙醇。
进一步地,所述的光热防伪纱线,光照下纱线升温速率8-12℃/min。
本发明的第二个目的是提供一种由上述制备方法得到的光热防伪纱线。
本发明创造性地将铯钨青铜的反应原料分别与不同纱线复合,后经原位反应制备得到具有蓄热性能的铯钨青铜材料,搭配赛络菲尔纺工艺实现纤维素和棉纤维的复合,使制备得到光热防伪纱线具有生物降解性、良好的热稳定性和优异的机械性能,且原位反应使得纱线之间结合更为紧密,其中的蓄热材料不易脱落,从而大大提高本发明制备的光热防伪纱线的稳定性。
本发明的第三个目的是提供上述光热防伪纱线在防伪检测中的应用。
进一步地,防伪检测具体操作为:对铯、钨离子的定量进行检测,鉴别光热纱线的真伪。
借由上述方案,本发明至少具有以下优点:
(1)本发明使用铯、钨离子可以使纱线具有光热性能,铯、钨具有无毒环保性能,而且铯、钨离子可以使用电感耦合等离子光谱法测试含量来辨别光热纱线的真伪。
(2)本发明使用湿式溶液吹纺和赛络非尔纺相结合,两种工艺发挥其优势相辅相成,使得纱线的力学性能优异,毛羽数量减少,纤维直径较小。
(3)本发明将铯、钨离子分别浸渍在长丝束和棉短纤纱上,通过原位反应使铯钨粉融入纱线中,可以提高使用寿命、光热材料的稳定性好。
上述说明仅是本发明技术方案的概述,为了能够更清楚了解本发明的技术手段,并可依照说明书的内容予以实施,以下以本发明的较佳实施例并配合详细附图说明如后。
附图说明
为了使本发明的内容更容易被清楚的理解,下面根据本发明的具体实施例并结合附图,对本发明作进一步详细的说明。
图1为本发明的光热防伪纱线制备的工艺流程示意图。
附图标记说明:101纺丝液;102齿轮泵;103热空气;104水雾凝固室;105浸渍槽;106赛络菲尔纺;107棉筒;108反应槽;109烘箱;110收集筒。
具体实施方式
下面结合附图和具体实施例对本发明作进一步说明,以使本领域的技术人员可以更好地理解本发明并能予以实施,但所举实施例不作为对本发明的限定。
实施例1
本实施例提供了一种光热防伪纱线制备及方法,具体步骤如下:
(1)首先将纤维素(购自广州市润宏化工有限公司)和1-乙基-3-甲基咪唑磷酸二乙酯(EMIMDEP)(购自林州市科能材料科技有限公司)离子液体混合形成纺丝液,溶解时在80℃下进行微波溶解,微波功率为600W,纺丝液浓度为5wt%。
得到的纺丝液101,通过湿式溶液吹纺获得长丝束,纺丝溶液通过齿轮泵102提供给喷丝板。挤出的溶液通过高速热空气103在气隙上拉伸,并在水雾凝固室104中凝固,通过牵伸形成丝。其中喷丝板孔-孔间距为1.6毫米,喷嘴直径喷嘴长度分别为0.20mm、2.0mm,模唇间隙设定为0.2毫米。齿轮泵以每26孔0.3至0.9mL min-1的吞吐率提供给喷丝板。高速热空气为160℃。水雾凝固室中,蒸馏水和压缩干燥空气的供应量分别为每个喷嘴14g min-1和16L min-1。
得到的长束丝通过浸渍槽105,其中溶液为碳酸铯(购自国药集团化学试剂有限公司)溶液中,碳酸铯溶液浓度为0.5mol/L。
(2)将棉筒107中19.7tex棉短纤纱通过浸渍槽105,其中溶液为钨酸钠(购自国药集团化学试剂有限公司)溶液,钨酸钠溶液浓度为0.5mol/L。
(3)将浸渍过的丝与棉在赛络菲尔纺106工艺中混纺,形成纱线,其中赛络菲尔纺工艺参数粗纱捻系数为70,锭速495r/min。细纱牵伸倍数31,锭速为1250r/min。
(4)将纱线浸渍到反应槽108,其中溶液为柠檬酸(购自国药集团化学试剂有限公司)溶液,柠檬酸溶液浓度为1mol/L,溶液温度为190℃。
最后通过烘箱109使其充分反应,烘箱的温度为190℃。反应完成之后,使用乙醇进行洗涤三次,在60℃烘箱中使其烘干,最终收集到收集筒110里。
(5)将纱线a放在距离R95e(100W)的飞利浦灯40cm处,照射120s。
实施例2
(1)首先将纤维素和1-乙基-3-甲基咪唑磷酸二乙酯(EMIMDEP)离子液体混合形成纺丝液,纺丝液浓度为10wt%。
得到的纺丝液101,通过湿式溶液吹纺获得长丝束,纺丝溶液通过齿轮泵102提供给喷丝板。挤出的溶液通过高速热空气103在气隙上拉伸,并在水雾凝固室104中凝固,通过牵伸形成丝。其中喷丝板孔-孔间距为1.6毫米,喷嘴直径喷嘴长度分别为0.20mm、2.0mm,模唇间隙设定为0.2毫米。齿轮泵以每26孔0.3至0.9mL min-1的吞吐率提供给喷丝板。高速热空气为160℃。水雾凝固室中,蒸馏水和压缩干燥空气的供应量分别为每个喷嘴14g min-1和16L min-1。
得到的长束丝通过浸渍槽105,其中溶液为氯化铯溶液中,氯化铯溶液浓度为0.1mol/L。
(2)将棉筒107中19.7tex棉短纤纱通过浸渍槽105,其中溶液为钨酸钠溶液中,钨酸钠溶液浓度为0.1mol/L。
(3)将浸渍过的丝与棉在赛络菲尔纺106工艺中混纺,形成纱线,其中赛络菲尔纺工艺参数粗纱捻系数为62,锭速500r/min。细纱牵伸倍数34,锭速为1300r/min。
(4)将纱线浸渍到反应槽108,其中溶液为柠檬酸溶液,柠檬酸溶液浓度为0.5mol/L,溶液温度为200℃。
最后通过烘箱109使其充分反应,烘箱的温度为200℃。反应完成之后,使用乙醇进行洗涤三次,在60℃烘箱中使其烘干,最终收集到收集筒110里。
将纱线b放在距离R95e(100W)的飞利浦灯40cm处,照射120s。
对比例1
纺丝液制备方法同实施例1。
将得到的纺丝液通过湿式溶液吹纺获得长丝束,纺丝溶液通过齿轮泵提供给喷丝板。挤出的溶液通过高速热空气在气隙上拉伸,并在水雾凝固室中凝固,通过牵伸形成丝。其中喷丝板孔-孔间距为1.6毫米,喷嘴直径喷嘴长度分别为0.20mm、2.0mm,模唇间隙设定为0.2毫米。齿轮泵以每26孔0.3至0.9mL min-1的吞吐率提供给喷丝板。高速热空气为160℃。水雾凝固室中,蒸馏水和压缩干燥空气的供应量分别为每个喷嘴14g min-1和16L min-1。
得到的长束丝与棉筒中19.7tex棉短纤纱在赛络菲尔纺工艺中混纺,形成纱线,其中赛络菲尔纺工艺参数粗纱捻系数为70,锭速495r/min。细纱牵伸倍数31,锭速为1250r/min。
将纱线c浸渍到铯钨青铜浆料里,其中浆料制备条件为碳酸铯溶液浓度为0.5mol/L、钨酸钠溶液浓度为0.5mol/L、柠檬酸溶液浓度为1mol/L、聚碳酸树脂,反应温度为190℃。最后通过烘箱烘干,烘箱的温度为60℃,收集到收集筒里。
对比例2
(1)将纤维素使用湿法纺丝制备成长束丝,其中,纺丝液制备同实施例1,凝固浴为20%浓度的二甲基亚砜(DMSO)溶液,具体湿法纺丝参数如下,将所述纺丝液缓慢注入纺丝机料釜中,在0.3MPa压力下将纺丝液挤出纺丝,纺丝温度80℃;喷丝板孔数50孔,孔径80μm;泵供量0.71m L/min;凝固牵伸比为0.90;水洗牵伸比为1.10;水洗温度为60℃。
得到的长束丝通过浸渍槽105,其中溶液为碳酸铯溶液,碳酸铯溶液浓度为0.5mol/L。
(2)将棉筒107中19.7tex棉短纤纱通过浸渍槽105,其中溶液为钨酸钠(购自国药集团化学试剂有限公司)溶液,钨酸钠溶液浓度为0.5mol/L。
(3)将浸渍过的丝与棉在赛络菲尔纺106工艺中混纺,形成纱线,其中赛络菲尔纺工艺参数粗纱捻系数为70,锭速495r/min。细纱牵伸倍数31,锭速为1250r/min。
(4)将纱线浸渍到反应槽108,其中溶液为柠檬酸(购自国药集团化学试剂有限公司)溶液,柠檬酸溶液浓度为1mol/L,溶液温度为190℃。
最后通过烘箱109使其充分反应,烘箱的温度为190℃。反应完成之后,使用乙醇进行洗涤三次,在60℃烘箱中使其烘干,最终收集到收集筒110里,得到纱线d。
对比例3
(1)将碳酸铯溶液浓度为0.5mol/L、钨酸钠溶液浓度为0.5mol/L、柠檬酸溶液浓度为1mol/L制备出来的铯钨青铜粉混入纺丝液里,纺丝液制备方法同实施例1。
将混有铯钨青铜粉的纺丝液通过湿式溶液吹纺获得长丝束,纺丝溶液通过齿轮泵102提供给喷丝板。挤出的溶液通过高速热空气103在气隙上拉伸,并在水雾凝固室104中凝固,通过牵伸形成丝。其中喷丝板孔-孔间距为1.6毫米,喷嘴直径喷嘴长度分别为0.20mm、2.0mm,模唇间隙设定为0.2毫米。齿轮泵以每26孔0.3至0.9mL min-1的吞吐率提供给喷丝板。高速热空气为160℃。水雾凝固室中,蒸馏水和压缩干燥空气的供应量分别为每个喷嘴14g min-1和16L min-1。
(2)将(1)得到的丝与棉筒107中19.7tex棉短纤纱在赛络菲尔纺工艺中混纺,形成纱线,其中赛络菲尔纺工艺参数粗纱捻系数为70,锭速495r/min。细纱牵伸倍数31,锭速为1250r/min。得到纱线e。
对比例4
碳酸铯溶液浓度为0.8mol/L,钨酸钠溶液浓度为0.8mol/L,其余同实施例1,得到纱线f。
测试例
(1)将光热防伪纱线进行溶解,采用35g/L氢氧化钠溶解处理十五个小时,浴比1:5采用电感耦合等离子光谱法对光热防伪纱线溶液进行检测,测试金属元素的含量辨别真伪。
纱线通过美的MFC100型滚筒洗衣机(无锡小天鹅股份有限公司制造)进行洗涤,洗涤程序由一次主洗、两次漂洗和3次脱水组成,其中洗涤和漂洗后各进行一次脱水,在洗涤过程中,控制洗衣机的进水量为20L,主洗时间27min,脱水转速800r/min,洗涤温度30℃。洗涤结束后,将纱线取出,自然条件下悬挂晾干,重复洗涤五十次。
表1检测及光热性能测试结果
从表1中可知,铯钨青铜的浓度对光热性能产生影响,随着浓度的增加光热性能变强,达到极点之后将会下降;将铯钨青铜浆料直接浸渍在其表面,力学性能并没有影响,然而在洗涤过程中,随着洗涤次数增加铯钨青铜的含量将会大大降低;湿法纺丝的方法制备,纺出来的长丝束结晶度较低,得到的丝较粗,力学性能较差,且在洗涤过程会使铯钨青铜发生流失。
(2)按GB/T3293—1997测定毛羽数量,按GB/T5324—2009测定条干均匀率,按GB/T3916—1997测定断裂伸长率,结果见表2。
表2纤维参数测定结果
测试项目 | a | b | c | d | e | f |
毛羽数量(10m)<sup>-1</sup> | 80 | 82 | 90 | 87 | 94 | 97 |
条干均匀率% | 88.88 | 86.88 | 82.72 | 82.16 | 83.82 | 82.57 |
断裂伸长率% | 13 | 12.56 | 11.43 | 10.29 | 12.09 | 10.36 |
断裂强度(c N/dtex) | 3.16 | 2.98 | 2.46 | 2.11 | 2.89 | 2.22 |
显然,上述实施例仅仅是为清楚地说明所作的举例,并非对实施方式的限定。对于所属领域的普通技术人员来说,在上述说明的基础上还可以做出其它不同形式变化或变动。这里无需也无法对所有的实施方式予以穷举。而由此所引申出的显而易见的变化或变动仍处于本发明创造的保护范围之中。
Claims (10)
1.一种光热防伪纱线的制备方法,其特征在于,包括以下步骤:
S1、将纤维素形成的纺丝液通过湿式溶液吹纺得到长束丝,将长丝束浸渍到第一溶液中;
将棉纤维浸渍到第二溶液中;
其中,当第一溶液为铯盐溶液时,第二溶液为钨酸盐溶液;当第一溶液为钨酸盐溶液时,第二溶液为铯盐溶液;
S2、以步骤S1得到的长束丝和棉纤维进行赛络菲尔纺;
S3、将步骤S2得到的纱线浸渍在还原剂中反应,经洗涤、干燥后得到所述光热防伪纱线。
2.根据权利要求1所述的制备方法,其特征在于:在步骤S1中,所述纺丝液是将纤维素溶于1-乙基-3-甲基咪唑磷酸二乙酯盐离子液体形成的溶液。
3.根据权利要求2所述的制备方法,其特征在于:将所述纤维素在90-110℃下进行微波溶解。
4.根据权利要求1所述的制备方法,其特征在于:在步骤S1中,所述纺丝液的浓度为5-10wt%。
5.根据权利要求1所述的制备方法,其特征在于:在步骤S1中,所述的湿式溶液吹纺,挤出的纺丝液通过高速热空气在气隙上拉伸,并在水雾凝固室中凝固,其中,高速热空气的温度保持在140-180℃。
6.根据权利要求1所述的制备方法,其特征在于:所述铯盐溶液的浓度为0.1-0.5mol/L,所述钨酸盐溶液的浓度为0.1-0.5mol/L。
7.根据权利要求1所述的制备方法,其特征在于:在步骤S2中,所述的赛络菲尔纺,粗纱捻系数65-74,锭速490-500r/min,细纱牵伸倍数31-34,锭速为1250-1300r/min。
8.根据权利要求1所述的制备方法,其特征在于:在180-200℃下进行反应。
9.权利要求1-8任一项所述的制备方法制备得到的光热防伪纱线。
10.权利要求9所述的光热防伪纱线在防伪检测中的应用。
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