CN109972388A - 一种快速电加热石墨烯织物的制备方法 - Google Patents
一种快速电加热石墨烯织物的制备方法 Download PDFInfo
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Abstract
本发明提出加热均匀,且柔韧性舒适性更优的快速电加热石墨烯织物的制备方法,采用石墨烯纤维和银纳米线、金纳米线或铜纳米线替代传统的加热电阻丝,其加热更加均匀,电阻小,能耗低,且安全性能更优;并且石墨烯具有更优的柔韧性,使得织物的整合性和舒适性得到提升,整套制备方法简单且经济。
Description
技术领域
本发明涉及电发热织物技术领域,尤其涉及一种快速电加热石墨烯织物的制备方法。
背景技术
尽管在寒冷的季节,人们可以采用添加保暖性衣物来防寒保暖,但是在极寒条件下被动式取暖方式还是存在自身缺陷,无法主动供暖。开发新型主动式取暖衣物成为功能性服装的发展趋势之一。目前市场上使用的发热衣多是内置导电碳纤维,通过电加热的方式产热,缺点是点加热的方式不均匀;电阻丝阻值大,加热慢,能耗大;容易断裂,安全系数低;电阻丝较硬,人体舒适性差。为了寻找一种能够替换加热电阻丝的材料,有人尝试采用石墨烯取代碳纤维制备加热装置。例如:中国专利公开号CN 105188164A公开了一种石墨烯发热体的制备方法。尽管该石墨烯发热体克服了碳纤维发热体的一些缺点,但仍存在整合性不够、柔韧性欠佳、须设置隔热层、舒适性有待进一步提高等问题。中国专利公开号CN106183142A公开了一种基于石墨烯无纺布的自热膜,该发热膜由石墨烯纤维制成,存在制备工艺繁琐、成本高的缺点。
发明内容
本发明的目的在于提出一种加热均匀,且柔韧性舒适性更优的快速电加热石墨烯织物的制备方法。
为达到上述目的,本发明提出一种快速电加热石墨烯织物的制备方法,包括以下步骤:
步骤1:石墨烯纤维分散液的制备:
步骤1.1:制备氧化石墨烯粉末;
步骤1.2:将所述氧化石墨烯粉末加热还原得到石墨烯粉末;
步骤1.3:将所述石墨烯粉末制备成石墨烯纤维;
步骤1.4:取石墨烯纤维和金属米线粉末分散于制备液中;
步骤2:制备石墨烯织物:
步骤2.1:剪取织布贴附于涂布机基板上;
步骤2.2:倒取所述石墨烯纤维分散液于涂布机堆头中;
步骤2.3:调整涂布机的工艺参数;
步骤2.4:将所述石墨烯纤维分散液均匀涂抹于所述织布表面;
步骤2.5:烘干得到所述石墨烯织物;
步骤3:制备得到快速电加热石墨烯织物。
优选的,在步骤1.1中,采用Hummer法制备氧化石墨烯粉末,包括以下步骤:
步骤1.11:将3g膨胀石墨粉分散于360mL浓硫酸和3g硝酸钠中反应48小时,反应温度为25℃,以形成混合溶液;
步骤1.12:将所述混合溶液添加至1.8L包含30%双氧水的去离子水中,已形成去离子水混合液;
步骤1.13:搅拌所述去离子水混合液至溶液颜色由棕色变为亮黄色得到最终产物;
步骤1.14:将所述最终产物用稀盐酸和去离子水洗涤后冷冻干燥得到石墨烯粉末;
优选的,在步骤1.2中,将所述氧化石墨烯粉末在300℃环境下加热还原1小时得到所述石墨烯粉末;
在步骤1.3中,将所述石墨烯粉末经湿法纺丝制备成所述石墨烯纤维。
优选的,在步骤1.4中,称取质量比例为1:1-1:3之间的所述石墨烯纤维和所述金属米线粉末,分散在制备液中制备得到石墨烯纤维分散液;
所述金属米线粉末为银纳米线、金纳米线或铜纳米线;
所述制备液为含有质量分数5-7%CTAB和质量分数为2-3%环氧树脂的去离子水。
优选的,在步骤2.1中,剪取尺寸25×25cm的厚度1~3mm的所述织布贴附在所述涂布机基板上;
所述织布为机织布或者针织布。
优选的,在步骤2.2中,倒取100-300mL所述石墨烯纤维分散液于所述涂布机堆头中。
优选的,在步骤2.3中,所述涂布机的工艺参数为所述涂布机的涂抹速度为5-8cm/s。
优选的,在步骤2.5中,在温度为50-70℃的环境下烘干2-4小时得到所述石墨烯织物。
优选的,在所述步骤3,包括以下步骤:
步骤3.1:通过涂布机在所述石墨烯织物表面构建纳米导电层;
步骤3.2:在所述石墨烯织物表面涂覆防水层;
步骤3.3:采用铜胶带贴附于所述石墨烯织物两端引出导线;
步骤3.4:将所述导线外接调压器和电源。
优选的,在步骤3.3中,采用聚氨酯或聚二甲基硅氧烷在所述石墨烯织物表面涂覆防水层;
在步骤3.4中,所述电源的电压为5V。
与现有技术相比,本发明的优势之处在于:本发明采用石墨烯纤维和银纳米线、金纳米线或铜纳米线替代传统的加热电阻丝,其加热更加均匀,电阻小,能耗低,且安全性能更优;并且石墨烯具有更优的柔韧性,使得织物的整合性和舒适性得到提升;整套制备方法简单且经济。
附图说明
图1为本发明一实施例中一种快速电加热石墨烯织物的制备方法的工艺流程图。
图2为本发明中一种快速电加热石墨烯织物的发热红外成像图。
具体实施方式
为使本发明的目的、技术方案和优点更加清楚,下面将对本发明的技术方案作进一步地说明。
如图1和图2所示,本发明提出一种快速电加热石墨烯织物的制备方法,包括以下步骤:
步骤1:石墨烯纤维分散液的制备:
步骤1.1:制备氧化石墨烯粉末;
步骤1.2:将氧化石墨烯粉末加热还原得到石墨烯粉末;
步骤1.3:将石墨烯粉末制备成石墨烯纤维;
步骤1.4:取石墨烯纤维和金属米线粉末分散于制备液中;
步骤2:制备石墨烯织物:
步骤2.1:剪取织布贴附于涂布机基板上;
步骤2.2:倒取石墨烯纤维分散液于涂布机堆头中;
步骤2.3:调整涂布机的工艺参数;
步骤2.4:将石墨烯纤维分散液均匀涂抹于织布表面;
步骤2.5:烘干得到石墨烯织物;
步骤3:制备得到快速电加热石墨烯织物。
在本实施例中,在步骤1.1中,采用Hummer法制备氧化石墨烯粉末,包括以下步骤:
步骤1.11:将3g膨胀石墨粉分散于360mL浓硫酸和3g硝酸钠中反应48小时,反应温度为25℃,以形成混合溶液;
步骤1.12:将混合溶液添加至1.8L包含30%双氧水的去离子水中,已形成去离子水混合液;
步骤1.13:搅拌去离子水混合液至溶液颜色由棕色变为亮黄色得到最终产物;
步骤1.14:将最终产物用稀盐酸和去离子水洗涤后冷冻干燥得到石墨烯粉末;
在本实施例中,在步骤1.2中,将氧化石墨烯粉末在300℃环境下加热还原1小时得到石墨烯粉末;
在步骤1.3中,将石墨烯粉末经湿法纺丝制备成石墨烯纤维。
在本实施例中,在步骤1.4中,称取质量比例为1:1-1:3之间的石墨烯纤维和金属米线粉末,分散在制备液中制备得到石墨烯纤维分散液;
金属米线粉末为银纳米线、金纳米线或铜纳米线;
制备液为含有质量分数5-7%CTAB(溴化十六烷基三甲胺)和质量分数为2-3%环氧树脂的去离子水。
在本实施例中,在步骤2.1中,剪取尺寸25×25cm的厚度1~3mm的织布贴附在涂布机基板上;
织布为机织布或者针织布。
在本实施例中,在步骤2.2中,倒取100-300mL石墨烯纤维分散液于涂布机堆头中。
在本实施例中,在步骤2.3中,涂布机的工艺参数为涂布机的涂抹速度为5-8cm/s。
在本实施例中,在步骤2.5中,在温度为50-70℃的环境下烘干2-4小时得到石墨烯织物。
在本实施例中,在步骤3,包括以下步骤:
步骤3.1:通过涂布机在石墨烯织物表面构建纳米导电层;
步骤3.2:在石墨烯织物表面涂覆防水层;
步骤3.3:采用铜胶带贴附于石墨烯织物两端引出导线;
步骤3.4:将导线外接调压器和电源。
在本实施例中,在步骤3.3中,采用聚氨酯或聚二甲基硅氧烷在石墨烯织物表面涂覆防水层;
在步骤3.4中,电源的电压为5V。
与在本实施例中,本发明采用石墨烯纤维和银纳米线、金纳米线或铜纳米线替代传统的加热电阻丝,其加热更加均匀,电阻小,能耗低,且安全性能更优;并且石墨烯具有更优的柔韧性,使得织物的整合性和舒适性得到提升;整套制备方法简单且经济。
以下将通过五个具体实施例对本发明做出进一步的解释说明:
实施例1
称取1g石墨烯纤维粉末和1g银纳米线粉末重新分散在含有10mg/mL CTAB和2mg/mL环氧树脂的500mL去离子水中制备石墨烯分散液备用。剪取尺寸25×25cm的厚度1mm的机织或针织布贴附在涂布机的基板上,倒取100mL上述分散液于涂布机推头中,调整涂布机速度为5cm/s。完成石墨烯纤维、银纳米线混合液的均匀涂布,60℃烘燥2小时,后即得石墨烯纤维织物。表面涂覆厚度10μm的PU和PDMS防水涂层后,外接导线、调压器、电源后制成快速电加热石墨烯纤维织物。
实施例2
称取2g石墨烯纤维粉末和1g铜纳米线粉末重新分散在含有20mg/mL CTAB和3mg/mL环氧树脂的500mL去离子水中制备石墨烯纤维分散液备用。剪取尺寸25×25cm的厚度2mm的机织或针织布贴附在涂布机的基板上,倒取200mL上述分散液于涂布机推头中,调整涂布机速度为6cm/s。完成石墨烯纤维、铜纳米线混合液的均匀涂布,50℃烘燥3小时,后即得石墨烯纤维织物。表面涂覆厚度10μm的PU和PDMS防水涂层后,外接导线、调压器、电源后制成快速电加热石墨烯纤维织物。
实施例3
称取3g石墨烯纤维粉末和2g银纳米线粉末重新分散在含有15mg/mL CTAB和2mg/mL环氧树脂的500mL去离子水中制备石墨烯纤维分散液备用。剪取尺寸25×25cm的厚度3mm的机织或针织布贴附在涂布机的基板上,倒取220mL上述分散液于涂布机推头中,调整涂布机速度为8cm/s。完成石墨烯纤维、银纳米线混合液的均匀涂布,70℃烘燥2小时,后即得石墨烯纤维织物。表面涂覆厚度12μm的PU和PDMS防水涂层后,外接导线、调压器、电源后制成快速电加热石墨烯纤维织物。
实施例4
称取2.8g石墨烯纤维粉末和1.2g金纳米线粉末重新分散在含有13mg/mL CTAB和3mg/mL环氧树脂的500mL去离子水中制备石墨烯纤维分散液备用。剪取尺寸25×25cm的厚度2mm的机织或针织布贴附在涂布机的基板上,倒取300mL上述分散液于涂布机推头中,调整涂布机速度为8cm/s。完成石墨烯纤维、银纳米线混合液的均匀涂布,65℃烘燥2小时,后即得石墨烯纤维织物。表面涂覆厚度10μm的PU和PDMS防水涂层后,外接导线、调压器、电源后制成快速电加热石墨烯纤维织物。
本发明具有制备方法简单、重复性高等特点,为研究开发发热均匀、整合度高、舒适性好的快速电加热石墨烯织物提供了技术支持,在智能服装领域具有很好的应用前景。
上述仅为本发明的优选实施例而已,并不对本发明起到任何限制作用。任何所属技术领域的技术人员,在不脱离本发明的技术方案的范围内,对本发明揭露的技术方案和技术内容做任何形式的等同替换或修改等变动,均属未脱离本发明的技术方案的内容,仍属于本发明的保护范围之内。
Claims (10)
1.一种快速电加热石墨烯织物的制备方法,其特征在于,包括以下步骤:
步骤1:石墨烯纤维分散液的制备:
步骤1.1:制备氧化石墨烯粉末;
步骤1.2:将所述氧化石墨烯粉末加热还原得到石墨烯粉末;
步骤1.3:将所述石墨烯粉末制备成石墨烯纤维;
步骤1.4:取石墨烯纤维和金属米线粉末分散于制备液中;
步骤2:制备石墨烯织物:
步骤2.1:剪取织布贴附于涂布机基板上;
步骤2.2:倒取所述石墨烯纤维分散液于涂布机堆头中;
步骤2.3:调整涂布机的工艺参数;
步骤2.4:将所述石墨烯纤维分散液均匀涂抹于所述织布表面;
步骤2.5:烘干得到所述石墨烯织物;
步骤3:制备得到快速电加热石墨烯织物。
2.根据权利要求1所述的快速电加热石墨烯织物的制备方法,其特征在于,在步骤1.1中,采用Hummer法制备氧化石墨烯粉末,包括以下步骤:
步骤1.11:将3g膨胀石墨粉分散于360mL浓硫酸和3g硝酸钠中反应48小时,反应温度为25℃,以形成混合溶液;
步骤1.12:将所述混合溶液添加至1.8L包含30%双氧水的去离子水中,已形成去离子水混合液;
步骤1.13:搅拌所述去离子水混合液至溶液颜色由棕色变为亮黄色得到最终产物:
步骤1.14:将所述最终产物用稀盐酸和去离子水洗涤后冷冻干燥得到石墨烯粉末。
3.根据权利要求1所述的快速电加热石墨烯织物的制备方法,其特征在于,在步骤1.2中,将所述氧化石墨烯粉末在300℃环境下加热还原1小时得到所述石墨烯粉末;
在步骤1.3中,将所述石墨烯粉末经湿法纺丝制备成所述石墨烯纤维。
4.根据权利要求1所述的快速电加热石墨烯织物的制备方法,其特征在于,在步骤1.4中,称取质量比例为1:1-1:3之间的所述石墨烯纤维和所述金属米线粉末,分散在制备液中制备得到石墨烯纤维分散液;
所述金属米线粉末为银纳米线、金纳米线或铜纳米线;
所述制备液为含有质量分数5-7%CTAB和质量分数为2-3%环氧树脂的去离子水。
5.根据权利要求1所述的快速电加热石墨烯织物的制备方法,其特征在于,在步骤2.1中,剪取尺寸25×25cm的厚度1~3mm的所述织布贴附在所述涂布机基板上;
所述织布为机织布或者针织布。
6.根据权利要求1所述的快速电加热石墨烯织物的制备方法,其特征在于,在步骤2.2中,倒取100-300mL所述石墨烯纤维分散液于所述涂布机堆头中。
7.根据权利要求1所述的快速电加热石墨烯织物的制备方法,其特征在于,在步骤2.3中,所述涂布机的工艺参数为所述涂布机的涂抹速度为5-8cm/s。
8.根据权利要求1所述的快速电加热石墨烯织物的制备方法,其特征在于,在步骤2.5中,在温度为50-70℃的环境下烘干2-4小时得到所述石墨烯织物。
9.根据权利要求1所述的快速电加热石墨烯织物的制备方法,其特征在于,在所述步骤3,包括以下步骤:
步骤3.1:通过涂布机在所述石墨烯织物表面构建纳米导电层;
步骤3.2:在所述石墨烯织物表面涂覆防水层;
步骤3.3:采用铜胶带贴附于所述石墨烯织物两端引出导线;
步骤3.4:将所述导线外接调压器和电源。
10.根据权利要求9所述的快速电加热石墨烯织物的制备方法,其特征在于,在步骤3.3中,采用聚氨酯或聚二甲基硅氧烷在所述石墨烯织物表面涂覆防水层;
在步骤3.4中,所述电源的电压为5V。
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