CN107190510B - 基于碳纳米管的高导热柔性发热丝的制备方法 - Google Patents
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Abstract
本发明公开的基于碳纳米管的高导热柔性发热丝的制备方法，通过对涤纶纱线进行碱减法预处理，随后与碳纳米管导热悬浮液进行混合浸染，最后依次经过初期固化‑柔性处理‑最终固化得到高导热的柔性发热丝。本发明的制备方法采用碳纳米管作为导热主要材料，同时将碳纳米管优异的热学性能与涤纶复合纤维良好的机械性能有机结合，使其耗能低、通电后具有高效率的发热效能；相比于传统金属发热丝不仅有较好的柔性、强度、弹性，同时具有较好的穿戴安全性，便于制成织物；相比于复合发热材料，填充材料得到很好的分散，热转换率高，同时提高了复合发热材料的综合性能，有很好的实用价值。
Description
技术领域
本发明属于柔性发热丝技术领域，具体涉及一种基于碳纳米管的高导热柔性发热丝的制备方法。
背景技术
随着科学技术的发展和生活水平的提高，人们对生活服装及日用、专业纺织品的要求也越来越高，纺织品向智能化、交互式、功能高度集成化方向发展，使得纺织品具有了许多特定功能，其中柔性发热纺织品是其重要分支之一。
要使得智能纺织品达到优异的导热性能，就要求发热织物具有良好的导热性、耐腐蚀性、质量轻、柔性好、能耗低等优点。目前常见发热织物有两种组成形式：一种是传统发热织物，即通过在织物内部添加发热的金属丝制成加热层实现；另一种是通过复合加热材料与原丝编织形成。传统的发热织物采用导热性好的金属丝材质——银，其成本高昂，且发热织物质感硬、弯折度低、不可洗涤，在穿戴过程中易随着弯折强度加大而发生断裂，很难同时满足安全舒适、高电热转换效率的特点；而复合加热材料编制形成的导热层多采用非金属材料，例如碳纤维及聚合物混合涂抹而成，对原丝及溶剂的制备要求高，成型后存在导热填料涂抹厚度不均匀、易分层脱落、导热性不佳，复合材料的综合性能差等缺陷。
发明内容
本发明的目的是提供一种基于碳纳米管的高导热柔性发热丝的制备方法，解决了现有发热丝使用成本昂贵、导热性不佳、制备的发热织物综合性能较差的问题。
本发明所采用的技术方案是，基于碳纳米管的高导热柔性发热丝的制备方法，具体包括以下步骤：
步骤1，采用碱减法处理选取的涤纶纱线，得到复合牢度强的涤纶纱线基材；
步骤2，制备碳纳米管导热悬浮液并将其倒入印染装置中，同时将步骤1的涤纶纱线基材浸入碳纳米管导热悬浮液中浸染，得到碳纳米管沉积的涤纶纱线；
步骤3，将步骤2的碳纳米管沉积的涤纶纱线置入干燥炉中2-4min，取出后浸入柔性化处理溶液，得到表面覆膜的涤纶纱线；
步骤4，将步骤3的表面覆膜的涤纶纱线置入固化炉中进行固化成型处理，即得到高导热柔性发热丝。
本发明的特征还在于，
步骤1中的碱减法具体为：将涤纶纱线浸入质量分数为1-3％的NaOH溶液中进行界面处理，其处理条件为：NaOH溶液温度90-110℃、浸入时间2-5min，涤纶纱线随后取出洗涤4-6次后晾干。
步骤2中的碳纳米管导热悬浮液的制备方法：将质量比为9-11:0.3-0.5:1的碳纳米管、3-磺丙基十四烷基二甲甜菜碱和聚氧乙烯十二烷基磺酸醚依次加入定量的去离子水中，随后倒入超声波清洗器中振荡，得到分散均匀的碳纳米管导热悬浮液。
超声波清洗器中超声时间35-45min，超声温度30-50℃，频率40-60HZ。
步骤2中的浸染时间3-7min，浸染温度30-50℃，频率40-60HZ。
步骤3的干燥炉的温度为110-130℃。
步骤3中的柔性化处理溶液：将质量比为1:1的水性聚氨酯和丁腈橡胶在温度70-90℃下混合置入去离子水中，形成柔性化处理溶液。
步骤4中固化炉中的烘干温度50-70℃，烘干时间2-4min。
本发明的制备方法有益效果是：
a)本发明的制备方法采用碱减法对涤纶纱线进行界面处理，提高了涤纶纱线纤维的复合牢度，更易印染；
b)本发明的制备方法采用添加增塑剂-水性聚氨酯和丁腈橡胶的后处理工艺，增加发热丝的柔性和可洗涤性，使涂覆的碳纳米管更易弯曲、洗涤，不易结块、脱落；
c)本发明制备的非金属发热丝，电热转换率高、环保节能、携带使用便捷，为制备发热织物和医疗发热器件提供了良好的基础，有很好的实用价值。
具体实施方式
下面通过具体实施方式对本发明的制备方法进行详细说明。
本发明基于碳纳米管的高导热柔性发热丝的制备方法，包括以下步骤：
步骤1，采用碱减法对选取的涤纶纱线进行界面处理，得到复合牢度强的涤纶纱线基材，碱减法具体为：将涤纶纱线浸入质量分数为1-3％的NaOH溶液中，其处理条件为，NaOH溶液温度90-110℃、浸入时间2-5min，涤纶纱线随后取出洗涤4-6次后晾干；
步骤2，制备碳纳米管导热悬浮液并将其倒入印染装置中，同时将步骤1的涤纶纱线基材浸入碳纳米管导热悬浮液中浸染，浸染时间3-7min、浸染温度30-50℃、频率40-60HZ，得到碳纳米管沉积的涤纶纱线，此时通过保证浸染时间和振动频率，使碳纳米管材料可充分渗入基材内部，并在纱线表面均匀涂覆；
其中，碳纳米管导热悬浮液的制备方法：将质量比为9-11:0.3-0.5:1的碳纳米管、3-磺丙基十四烷基二甲甜菜碱和聚氧乙烯十二烷基磺酸醚依次加入定量的去离子水中，随后倒入超声波清洗器中振荡，得到分散均匀的碳纳米管导热悬浮液，超声波清洗器中超声时间35-45min、超声温度30-50℃、频率40-60HZ，碳纳米管应做润湿处理后再加入到去离子水中；
步骤3，将步骤2的碳纳米管沉积的涤纶纱线置入温度为110-130℃的干燥炉中2-4min，保证其固化成型，取出后浸入柔性化处理溶液，得到表面覆膜的涤纶纱线，其中，将质量比为1:1的水性聚氨酯和丁腈橡胶在温度70-90℃下混合置入去离子水中，形成柔性化处理溶液；
步骤4，将步骤3的表面覆膜的涤纶纱线置入固化炉中进行最终的固化成型处理，即得到高导热柔性发热丝，其中，固化炉中的烘干温度50-70℃，烘干时间2-4min。
实施例1
(1)涤纶纱线的预处理
对选取的涤纶纱线采用碱减法进行界面处理，即将涤纶纱线浸入质量分数为1％的NaOH溶液中，随后取出洗涤4次后晾干，得到复合牢度强的涤纶纱线基材；具体参数为NaOH溶液温度90℃、浸入时间2min。
(2)碳纳米管的沉积
将质量比为9:0.3:1的碳纳米管、3-磺丙基十四烷基二甲甜菜碱和聚氧乙烯十二烷基磺酸醚依次加入定量的去离子水中，随后倒入超声波清洗器中振荡，得到碳纳米管导热悬浮液，超声时间35min、超声温度30℃、频率40HZ；将碳纳米管导热悬浮液倒入印染装置中，同时将涤纶纱线基材浸入其中浸染，浸染时间3min、浸染温度30℃、频率40HZ，得到碳纳米管沉积的涤纶纱线。
(3)涤纶纱线的柔性处理和固化成型
将碳纳米管沉积的涤纶纱线置入温度为110℃的干燥炉中2min，保证其固化成型，取出后浸入柔性化处理溶液，得到表面覆膜的涤纶纱线，随后将其置入温度为50℃的固化炉中2min，进行最终的固化成型处理，得到高导热柔性发热丝，其中，柔性化处理溶液通过将质量比为1:1的水性聚氨酯和丁腈橡胶在温度70℃下混合置入去离子水中形成。
实施例2
(1)涤纶纱线的预处理
对选取的涤纶纱线采用碱减法进行界面处理，即将涤纶纱线浸入质量分数为3％的NaOH溶液中，随后取出洗涤6次后晾干，得到复合牢度强的涤纶纱线基材；具体参数为NaOH溶液温度110℃、浸入时间5min。
(2)碳纳米管的沉积
将质量比为11:0.5:1的碳纳米管、3-磺丙基十四烷基二甲甜菜碱和聚氧乙烯十二烷基磺酸醚依次加入定量的去离子水中，随后倒入超声波清洗器中振荡，得到碳纳米管导热悬浮液，超声时间45min、超声温度50℃、频率60HZ；将碳纳米管导热悬浮液倒入印染装置中，同时将涤纶纱线基材浸入其中浸染，浸染时间7min、浸染温度50℃、频率60HZ，得到碳纳米管沉积的涤纶纱线。
(3)涤纶纱线的柔性处理和固化成型
将碳纳米管沉积的涤纶纱线置入温度为130℃的干燥炉中4min，保证其固化成型，取出后浸入柔性化处理溶液，得到表面覆膜的涤纶纱线，随后将其置入温度为70℃的固化炉中4min，进行最终的固化成型处理，得到高导热柔性发热丝，其中，柔性化处理溶液通过将质量比为1:1的水性聚氨酯和丁腈橡胶在温度90℃下混合置入去离子水中形成。
实施例3
(1)涤纶纱线的预处理
对选取的涤纶纱线采用碱减法进行界面处理，即将涤纶纱线浸入质量分数为2％的NaOH溶液中，随后取出洗涤5次后晾干，得到复合牢度强的涤纶纱线基材；具体参数为NaOH溶液温度100℃、浸入时间3min。
(2)碳纳米管的沉积
将质量比为10:0.4:1的碳纳米管、3-磺丙基十四烷基二甲甜菜碱和聚氧乙烯十二烷基磺酸醚依次加入定量的去离子水中，随后倒入超声波清洗器中振荡，得到碳纳米管导热悬浮液，超声时间40min、超声温度40℃、频率50HZ；将碳纳米管导热悬浮液倒入印染装置中，同时将涤纶纱线基材浸入其中浸染，浸染时间5min、浸染温度40℃、频率50HZ，得到碳纳米管沉积的涤纶纱线。
(3)涤纶纱线的柔性处理和固化成型
将碳纳米管沉积的涤纶纱线置入温度为120℃的干燥炉中3min，保证其固化成型，取出后浸入柔性化处理溶液，得到表面覆膜的涤纶纱线，随后将其置入温度为60℃的固化炉中3min，进行最终的固化成型处理，得到高导热柔性发热丝，其中，柔性化处理溶液通过将质量比为1:1的水性聚氨酯和丁腈橡胶在温度80℃下混合置入去离子水中形成。
实施例4
(1)涤纶纱线的预处理
对选取的涤纶纱线采用碱减法进行界面处理，即将涤纶纱线浸入质量分数为1.5％的NaOH溶液中，随后取出洗涤5次后晾干，得到复合牢度强的涤纶纱线基材；具体参数为NaOH溶液温度95℃、浸入时间4min。
(2)碳纳米管的沉积
将质量比为9.5:0.35:1的碳纳米管、3-磺丙基十四烷基二甲甜菜碱和聚氧乙烯十二烷基磺酸醚依次加入定量的去离子水中，随后倒入超声波清洗器中振荡，得到碳纳米管导热悬浮液，超声时间38min、超声温度35℃、频率45HZ；将碳纳米管导热悬浮液倒入印染装置中，同时将涤纶纱线基材浸入其中浸染，浸染时间4min、浸染温度35℃、频率45HZ，得到碳纳米管沉积的涤纶纱线。
(3)涤纶纱线的柔性处理和固化成型
将碳纳米管沉积的涤纶纱线置入温度为115℃的干燥炉中2.5min，保证其固化成型，取出后浸入柔性化处理溶液，得到表面覆膜的涤纶纱线，随后将其置入温度为55℃的固化炉中2.5min，进行最终的固化成型处理，得到高导热柔性发热丝，其中，柔性化处理溶液通过将质量比为1:1的水性聚氨酯和丁腈橡胶在温度75℃下混合置入去离子水中形成。
实施例5
(1)涤纶纱线的预处理
对选取的涤纶纱线采用碱减法进行界面处理，即将涤纶纱线浸入质量分数为2.5％的NaOH溶液中，随后取出洗涤4次后晾干，得到复合牢度强的涤纶纱线基材；具体参数为NaOH溶液温度115℃、浸入时间3.5min。
(2)碳纳米管的沉积
将质量比为10.5:0.45:1的碳纳米管、3-磺丙基十四烷基二甲甜菜碱和聚氧乙烯十二烷基磺酸醚依次加入定量的去离子水中，随后倒入超声波清洗器中振荡，得到碳纳米管导热悬浮液，超声时间42min、超声温度45℃、频率55HZ；将碳纳米管导热悬浮液倒入印染装置中，同时将涤纶纱线基材浸入其中浸染，浸染时间6min、浸染温度45℃、频率55HZ，得到碳纳米管沉积的涤纶纱线。
(3)涤纶纱线的柔性处理和固化成型
将碳纳米管沉积的涤纶纱线置入温度为125℃的干燥炉中3.5min，保证其固化成型，取出后浸入柔性化处理溶液，得到表面覆膜的涤纶纱线，随后将其置入温度为65℃的固化炉中3.5min，进行最终的固化成型处理，得到高导热柔性发热丝，其中，柔性化处理溶液通过将质量比为1:1的水性聚氨酯和丁腈橡胶在温度85℃下混合置入去离子水中形成。
通过上述实施例1-5可知，采用碳纳米管涂覆涤纶纱线纤维直接制备高导热、柔性发热丝，降低了柔性发热丝的制备难度，缩短了制备周期；碳纳米管/涤纶复合发热丝与金属导电发热丝相比，手感轻薄、透气性强、耐折性好；与非金属复合加热材料，如碳纤维及聚合物混合的制备方法相比，工艺简单，过程可控，且制备的复合织物既具有碳纳米管的导电性能，又能保持基体织物的机械性能，为制备非金属发热织物提供了一种新思路。
Claims (7)
1.基于碳纳米管的高导热柔性发热丝的制备方法，其特征在于，包括以下步骤：
步骤1，采用碱减法处理选取的涤纶纱线，得到的涤纶纱线基材；
其中，所述碱减法具体为：将涤纶纱线浸入质量分数为1-3％的NaOH溶液中进行界面处理，其处理条件为：NaOH溶液温度90-110℃、浸入时间2-5min，涤纶纱线随后取出洗涤4-6次后晾干；
步骤2，制备碳纳米管导热悬浮液并将其倒入印染装置中，同时将步骤1的涤纶纱线基材浸入碳纳米管导热悬浮液中浸染，得到碳纳米管沉积的涤纶纱线；
步骤3，将步骤2的碳纳米管沉积的涤纶纱线置入干燥炉中2-4min，取出后浸入柔性化处理溶液，得到表面覆膜的涤纶纱线；
步骤4，将步骤3的表面覆膜的涤纶纱线置入固化炉中进行固化成型处理，即得到高导热柔性发热丝。
2.根据权利要求1所述的基于碳纳米管的高导热柔性发热丝的制备方法，其特征在于，所述的步骤2中的碳纳米管导热悬浮液的制备方法：将质量比为9-11:0.3-0.5:1的碳纳米管、3-磺丙基十四烷基二甲甜菜碱和聚氧乙烯十二烷基磺酸醚依次加入定量的去离子水中，随后倒入超声波清洗器中振荡，得到分散均匀的碳纳米管导热悬浮液。
3.根据权利要求2所述的基于碳纳米管的高导热柔性发热丝的制备方法，其特征在于，所述超声波清洗器中超声时间35-45min，超声温度30-50℃，频率40-60HZ。
4.根据权利要求1所述的基于碳纳米管的高导热柔性发热丝的制备方法，其特征在于，所述步骤2中的浸染时间3-7min、浸染温度30-50℃、频率40-60HZ。
5.根据权利要求1所述的基于碳纳米管的高导热柔性发热丝的制备方法，其特征在于，所述步骤3的干燥炉的温度为110-130℃。
6.根据权利要求1所述的基于碳纳米管的高导热柔性发热丝的制备方法，其特征在于，所述步骤3中的柔性化处理溶液：将质量比为1:1的水性聚氨酯和丁腈橡胶在温度70-90℃下混合置入去离子水中，形成柔性化处理溶液。
7.根据权利要求1所述的基于碳纳米管的高导热柔性发热丝的制备方法，其特征在于，所述步骤4中固化炉中的烘干温度50-70℃，烘干时间2-4min。
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