CN113914109B - 多功能粉末填料的制备方法及在织物上制备聚酰胺湿法涂层的应用 - Google Patents
多功能粉末填料的制备方法及在织物上制备聚酰胺湿法涂层的应用 Download PDFInfo
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Abstract
本发明公开了一种兼具阻燃、吸墨等多功能填料的制备及其在聚酰胺湿法中的应用方法,将A组分和B组分按照质量比为1:1~4:1通过接枝反应制得多功能粉末填料,其中A组分包括:二乙二醇二甲醚、反应性阻燃剂、硅烷偶联剂、引发剂,B组分为无机轻质碳酸钙粉末。本发明通过合成的粉末填料代替传统填料,分散于聚酰胺湿法涂层浆料体系,在纺织品上进行应用。多功能填料的环保阻燃吸墨聚酰胺湿法涂层织物具有良好的柔性、阻燃性能和吸墨能力,以及在潮湿环境下pH值稳定,同时可以大幅提高聚酰胺涂层织物的功能性。
Description
技术领域
本发明涉及织物涂层领域,具体涉及一种多功能粉末填料的制备方法及在织物上制备聚酰胺湿法涂层的应用。
背景技术
聚酰胺湿法涂层技术是以甲醇/氯化钙溶剂化作用溶解聚酰胺6废丝成浆,添加填料通过高速搅拌的方式均匀分散制得功能浆料,采用双面刮涂的方式在纺织品上进行应用,聚酰胺湿法涂层技术是20世纪以来将工业上废弃的原材料再次进行回收利用,且进一步发挥其价值的有效途径。
目前,较为常用的填料如高岭土、硅灰石、硅灰石等,填料通过刮涂分布于涂层内部与涂层表面,实现阻燃、吸墨、拒水等功能。因为大部分填料本身亲水性的特点,在水浴交换过程中,填料易向涂层表面析出,发生团聚,造成涂覆不匀从而引起泡点、细孔、起粉等疵病。同时例如以碳酸钙为主的碱性盐填料,在潮湿环境下,涂层表面的填料发生电离,释放酸根离子水解呈碱性,造成pH偏高,人体皮肤不耐受等问题。
现有的填料对浆料粘度影响大,在保证填料功能以及涂层织物服用性能的前提下往往只能添加一种填料,无法兼顾阻燃、吸墨、环保等多功能。
基于现存的问题,往往通过对无机填料粒子改性的方法赋予填料额外的功能,例如雷鹏飞等人通过硬脂酸粉末填料改性(郑今欢,雷鹏飞,王成龙,李红艳,朱清,潘园歌.一种PA湿法涂层的硬脂酸粉末填料的制备方法[P].浙江省:CN109403060B,2021-04-06.)。李红艳等人通过用柠檬酸钠改性高岭土,(李红艳,杨佳盛,郑今欢,叶思佳.填充剂及其改性方法和采用该填充剂的湿法涂层工艺[P].浙江省:CN109161330B,2020-10-13.)。从而获得一定功能的粉末填料,满足生产需要。
发明内容
本发明提出一种兼具阻燃、吸墨等多功能填料的制备方法及其在聚酰胺湿法中的应用方法,以反应型阻燃剂DOPO与碳酸钙以硅烷偶联剂为“桥梁”合成具有阻燃、吸墨、在潮湿环境下不释酸的粉末填料。其疏水亲油性强,在相交换过程中不易在表面析出,减少填料损失以及避免涂覆疵病,从而得到耐干湿摩擦牢度优异且兼具多种功能的聚酰胺涂层织物。
本发明的目的在于提供一种用于聚酰胺湿法涂层的多功能无机粉末填料制备方法。具体是指提供一种在日常多场景使用时,有高结合牢度的纺织品及其生产方法。
本发明的技术方案是:一种多功能粉末填料的制备方法,包括以下步骤:
将A组分和B组分按照质量比为1:1~4:1通过接枝反应制得多功能粉末填料,其中A组分按照以总质量100%计,采用以下质量百分含量的组分:
所述的组分A的制备具体包括:
将反应性阻燃剂溶解于二乙二醇二甲醚中,反应性阻燃剂使反应性阻燃剂完全溶解,形成含反应性阻燃剂的溶液,将硅烷偶联剂与引发剂溶于二乙二醇二甲醚中,再用1~3h(优选为2h)将其逐滴加入含反应性阻燃剂的溶液中,保持60~80℃反应18~30h(优选为24h),体系颜色逐渐由无色变为淡黄色,最后得到浅淡黄色澄清透明的均匀溶液,后经环己烷洗涤、过滤除去溶剂,得到淡黄色溶液的含磷阻燃改性剂,即为组分A。
所述的反应性阻燃剂为9,10-二氢-9-氧杂-10-磷杂菲-10-氧化物(DOPO)。
所述的引发剂为偶氮二异丁腈(AIBN)。
该方法组分A的制备为DOPO与两种硅烷偶联剂在60~80℃下反应。温度太低,DOPO会从二乙二醇二甲醚中析出,温度太高易导致硅烷偶联剂的自聚合。
所述的硅烷偶联剂为乙烯基三甲氧基硅烷(A171)和甲基乙烯基二甲氧基硅烷(WD23)。该方法所使用的两种硅烷偶联剂A171,WD23摩尔比没有绝对限制,其中优选为摩尔比为A171:WD23=6~8:2~4,最优选为7:3。
无机粉末填料的制备,即通过接枝反应制得多功能粉末填料,具体包括:
将组分A与甲醇共混,后加入B组分(无机轻质碳酸钙粉末),在50~60℃条件下反应18~30h,后经过滤除去溶剂,在80~100℃条件下烘焙1~3h,后经研磨成粉末,即得到多功能粉末填料(即一种兼具阻燃、吸墨等多功能的粉末填料)。
作为优选,在50~60℃条件下反应24h。
所述B组分为无机轻质碳酸钙粉末。所述的无机轻质碳酸钙,其平均粒径为1-5μm,比表面积为5m2/g,吸油值为60~90ml/100g。
将多功能粉末填料用于在织物基底上制备聚酰胺湿法涂层,包括以下步骤:
将织物基底置于聚酰胺湿法涂层浆进行充分浸轧,通过刮刀双面涂覆,在水浴中进行成膜,最后烘干得到聚酰胺涂层织物;
所述的聚酰胺湿法涂层浆按照总质量100%计,采用以下质量百分含量的组分:
所述的聚酰胺湿法涂层浆的制备具体包括:
将甲醇、氯化钙依次加入反应器中,反应30~40min,直至无水氯化钙完全溶解,加入聚酰胺6(具体为聚酰胺6废丝),将反应温度升至60~70℃,使废丝充分浸润60~90min后,加入多功能粉末填料,并开启搅拌30~40min后得到聚酰胺湿法涂层浆。
作为优选,将反应温度升至65℃。
所述的织物基底为70D涤/氨混纺织物基底,浸轧的时间为10~30s,在25~35℃的水浴中进行成膜5~10s,在80~100℃条件下烘干5~10min。
所述涂层浆粘度为1000~1500Pa·s,水浴为质量百分数5%~10%的氯化钠水溶液,水浴温度为25~35℃,浸轧时间为10~30s,水浴交换时间为5~10s,烘干温度为80~100℃,烘干时间为5~10min。
具体地,在织物基底上制备聚酰胺湿法涂层的方法,具体包括:
将70D涤/氨混纺织物基底置于粘度为1000~1500Pa·s的涂层浆中充分浸轧10~30s,通过刮刀双面涂覆,在25~35℃的水浴中进行成膜5~10s,在80~100℃条件下烘干5~10min得到具有阻燃、吸墨等性能的聚酰胺涂层织物,即兼具阻燃、吸墨等多功能的聚酰胺湿法涂层。
多功能填料的环保阻燃吸墨聚酰胺湿法涂层织物具有良好的柔性、阻燃性能和吸墨能力,以及在潮湿环境下pH值稳定,同时可以大幅提高聚酰胺涂层织物的功能性。
该涂层织物所采用的原料纤维没有绝对限制,可以根据使用环境不同选择不同的纤维及不同的纱线进行组织织造。其中优选纺织品为70D涤/氨混纺织物。
该涂层浆的粘度相对较低,最佳涂覆粘度为1000~1500Pa·s,因为粉末填料本身亲水性强,在相转换过程中几乎不发生损失,当粘度过高会造成涂层织物过厚,影响其柔弱度。过低会造成涂覆厚度不够从而引起细孔疵病。
该方法将浆料涂覆在织物表面后,在水浴中发生相转换成膜。本发明所使用的水浴为5%~10%的氯化钠溶液而不能用纯水,在氯化钠溶液中成膜可减少、减缓氯化钙的析出,避免起粉疵病。同时提高涂层织物平整度,减少涂层织物收卷发生起杠问题。
该方法将浆料涂覆在织物表面后,在水浴中成膜。本发明的水浴温度为25~35℃,交换时间为5~10s。本发明涂层浆料的在水浴中成膜速率较快,可快速成膜缩短成膜时间,并形成一定丰满度的涂层,当水浴温度过高,分子交换过快会引起涂层起泡疵病,温度过低会造成成膜速度减缓,影响生产效率。
该方法经相交换后的涂层织物烘干温度在80~100℃,本发明粉末填料的结构不适宜采用100℃以上的用高温烘焙,需控制在80~100℃,阻燃成分在120℃左右迅速发挥作用,阻止燃烧,当烘干温度过高会造成粉末填料的阻燃成分流失,影响其阻燃能力以及涂层结构。
该方法最终的聚酰胺湿法涂层织物厚度为0.1~0.13mm,表面的细孔尺寸在0.1~2μm。且在该涂层织物表面覆盖的聚酰胺涂层涂覆均匀,无明显疵病。
根据GB/T 3920-2008《纺织品色牢度试验耐摩擦色牢度》和GB/T 3920-2008《纺织品色牢度试验耐皂洗色牢度》,该涂层织物用于喷墨打印后的摩擦色牢度大于等于4级,耐皂洗牢度大于等于4级。
根据GB/T8424.4-2001《纺织品白度的一期测评方法》,该涂层织物蓝光白度大于等于90。
根据GB/T 7573-2009《纺织品水萃取液pH值的测定》,该涂层织物pH为6.5~7.5,符合环保标准。
与现有技术相比,本发明具有如下优点:
1)、粉末填料是以反应型阻燃剂DOPO与无机轻质碳酸钙以硅烷偶联剂为“桥梁”合成具有阻燃,吸墨以及在潮湿环境下不释酸的多功能填料,其疏水亲油性强,在相交换过程中不易在表面析出,减少填料损失以及避免涂覆疵病。
2)、本发明利用粉末填料结合聚酰胺湿法涂层,在保留湿法涂层透湿,透气以及良好的柔性优点的前提下,粉末填料随着涂覆均匀分散于涂层表面,填料一端接枝的反应型阻燃剂DOPO可发挥阻燃作用,在火灾环境下发挥阻燃作用。
3)、本发明利用粉末填料结合聚酰胺湿法涂层,粉末填料均匀分散与涂层织物,其疏水亲油性强,可实现高效油墨柔版印刷,提高生产印刷效果以及印刷效率。
4)、本发明所得的用于聚酰胺湿法涂层的多功能无机粉末填料与浆料相容性好,涂层浆料具有高稳定性,应用于聚酰胺湿法涂层可获得比现有传统固体粉末填料体系更好的手感、透气性、透湿性、耐磨性、弹性等优良性能,干湿湿摩擦牢度以及耐水洗牢度得到显著提高达到4级以上。
5)、本发明采用的加工方式有效解决在聚酰胺湿法涂层加工过程在中因为涂覆时间过快而导致的起粉、起泡、起杠等问题,有效改善聚酰胺湿法涂层织物表面平整度以及涂层织物手感。大大提高了实际生产质量以及改善涂层织物储存收卷问题。
附图说明
图1为DOPO与中间体DOPO-Si的红外谱图;
图2为碳酸钙与粉末填料的红外谱图;
图3为碳酸钙聚酰胺湿法涂层表面形貌SEM;
图4为粉末填料聚酰胺湿法涂层表面形貌SEM。
具体实施方式
下面结合具体实施例对本发明进行进一步描述,但本发明的技术特征并不局限于此。任何以本发明为基础,为解决基本相同的技术问题,实现基本相同的技术效果,所作出地简单变化、等同替换或者修饰等,皆涵盖于本发明的保护范围之中。
本发明具体实施例中,组分B为无机轻质碳酸钙,平均粒径为1-5μm,比表面积为5m2/g,吸油值为60~90ml/100g。
将DOPO溶解于二乙二醇二甲醚中,使DOPO完全溶解,将摩尔比A171:WD23=7:3的两种硅烷偶联剂与AIBN三者溶于20mL二乙二醇二甲醚中,再用恒压滴液漏斗2h将其逐滴加入DOPO与二乙二醇二甲醚的混合溶液中,保持80℃反应24h。体系颜色逐渐由无色变为淡黄色,最后得到浅淡黄色澄清透明的均匀溶液。后经环己烷洗涤、过滤除去溶剂,得到淡黄色含磷阻燃改性剂。将其与甲醇溶液共混,后加入无机轻质碳酸钙粉末,在60℃条件下反应24h,后经过滤除去溶剂,在100℃条件下烘焙2h,后经研磨成粉末,即得到一种兼具阻燃、吸墨等多功能的粉末填料。
结构如下:
用于聚酰胺湿法涂层的多功能无机粉末填料的应用工艺,具体包括以下步骤:
1)聚酰胺湿法涂层浆的制备:
在室温25℃条件下将甲醇、无水氯化钙依次加入三口烧瓶中,开启搅拌使其充分反应35min,直至无水氯化钙完全溶解,关闭搅拌。加入聚酰胺6废丝,将反应温度升至65℃,使废丝充分浸润80min后,加入兼具阻燃、吸墨等多功能的粉末填料,并开启搅拌30~40min后得到聚酰胺湿法涂层浆。
2)多功能聚酰胺湿法涂层的制备:
将70D涤/氨混纺织物基底置于粘度为1000~1500Pa·s的涂层浆中充分浸轧20s,通过刮刀双面涂覆,在30℃的水浴中进行成膜8s,在90℃条件下烘干10min得到具有阻燃、吸墨等性能的聚酰胺涂层织物,即兼具阻燃、吸墨等多功能的聚酰胺湿法涂层。
实施例1~5和对比例1~3:
以70D涤/氨混纺织物为基底,按照下述表1配方进行组分A的制备,表2配方进行粉末填料的制备,按照表3配方进行聚酰胺湿法涂层浆的调配,然后将湿法涂层浆对织物基底进行双面刮涂,按照表4的浸轧以及水交换时间、烘干温度等条件下得到具有阻燃、吸墨性能的聚酰胺涂层织物。
其中中间产物配方由下列组分组成:
二乙二醇二甲醚 50%~60%
反应性阻燃剂 20%~30%
硅烷偶联剂 10%~20%
引发剂 0.1%~0.2%
表1 中间产物配方(Kg)
实施例1 | 实施例2 | 实施例3 | 实施例4 | 实施例5 | |
二乙二醇二甲醚 | 50 | 52 | 54 | 56 | 60 |
反应性阻燃剂 | 20 | 22 | 25 | 27 | 30 |
硅烷偶联剂 | 30 | 26 | 21 | 17 | 10 |
引发剂 | 0.1 | 0.12 | 0.15 | 0.17 | 0.2 |
粉末填料的制备配方由下列组分组成:
组分A:20%~30%
组分B:5%~15%
无水甲醇余量
表2 粉末填料配方(Kg)
实施例1 | 实施例2 | 实施例3 | 实施例4 | 实施例5 | |
组分A | 20 | 22 | 24 | 26 | 30 |
组分B | 5 | 7 | 9 | 13 | 15 |
备注:其余物质为甲醇,浆料总质量为100kg。
其中聚酰胺湿法涂层浆由下列组分组成:
无水氯化钙 20%~30%
聚酰胺6 10%~15%
粉末填料 10%~30%
无水甲醇余量
表3 聚酰胺湿法涂层浆配方(Kg)
备注:其余物质为甲醇,浆料总质量为100kg。
表4 的浸轧以及水交换时间、烘干温度
表5 检测结果
实施例、对比例中涉及的表征方法说明:
耐摩擦牢度测试是参照GB/T 3920-2008《纺织品色牢度试验耐摩擦色牢度》;耐水洗色牢度测试是参照GB/T3920-2008《纺织品色牢度试验耐皂洗色牢度》对油墨印刷商标涂层织物进行耐水洗色牢度测试。
白度是参照GB/T8424.4-2001《纺织品白度的一期测评方法》进行测试;
涂层厚度由厚度仪测量(上海理涛自动化科技有限公司涂层测厚仪)获得。
硬挺度参照GB/T 7689.4-2013《增强材料机织物测试方法第4部分:弯曲硬挺度的测定》进行测试。
pH参照GB/T 7573-2009《纺织品水萃取液pH值的测定》进行测试。
极限氧指数按照GBT 5454-1997标准测定。
吸墨时间和墨迹长度按照如下方式测试:
裁剪250×25mm的涂层织物样布各三条,在距离样布上方1cm处滴加商品油墨,当油墨完全浸入样布内部并停止扩散视为吸墨完成,记录滴加油墨到最终吸墨完成的时间,重复实验3次,取平均值。
将涂层织物斜向下45°固定好,在距离样布上方1cm处滴加商品油墨并以油墨落下为起点,油墨下滑形成墨迹直至停止滑动,以最终停止的点为终点,记录两点之间的水平距离为墨迹长度,重复实验3次,取平均值。
检测结果如表5示。
图1为实施例5所制得的DOPO与组分A的红外谱图,图2碳酸钙与粉末填料的红外谱图;
在中间产物的FTIR谱图中,DOPO位于2436cm-1处的P-H键特征吸收峰消失,1410cm-1处也出现了P-CH2的特征吸收峰,表明DOPO已经与两种硅烷偶联剂的双键发生加成反应,粉末填料在818cm-1处出现Si-O的特征峰,说明中间产物成功接枝在碳酸钙表面,即得到了预想物。
图3为对比例1所制得的聚酰胺湿法涂层表面形貌,图4为实施例5所制得的聚酰胺湿法涂层表面形貌。
从图3、4对比可以看出,固体填料容易堆积在涂层表面,形成大量的粗糙的颗粒聚集体,而本发明所制聚酰胺涂层织物表面光滑,孔洞结构清晰,吸墨阻燃效果佳。
以上仅是本发明的优选实施方式,应当指出的是,上述优选实施方式不应视为对本发明的限制,本发明的保护范围应当以权利要求所限定的范围为准。对于本技术领域的普通技术人员来说,在不脱离本发明的精神和范围内,还可以做出若干改进和润饰,这些改进和润饰也应视为本发明的保护范围。
Claims (6)
1.采用多功能粉末填料在织物基底上制备聚酰胺湿法涂层的方法,其特征在于,包括以下步骤:
采用多功能粉末填料制备聚酰胺湿法涂层浆,将织物基底置于聚酰胺湿法涂层浆进行充分浸轧,通过刮刀双面涂覆,在水浴中进行成膜,最后烘干得到聚酰胺涂层织物;
所述的聚酰胺湿法涂层浆按照总质量100%计,采用以下质量百分含量的组分:
氯化钙20%~30%;
聚酰胺6废丝10%~15%;
多功能粉末填料10%~30%;
甲醇余量;
其中,所述的聚酰胺湿法涂层浆的制备具体包括:
将甲醇、氯化钙依次加入反应器中,反应30~40min,直至氯化钙完全溶解,加入聚酰胺6废丝,将反应温度升至60~70℃,使聚酰胺6废丝充分浸润60~90min后,加入多功能粉末填料,并开启搅拌30~40min后得到聚酰胺湿法涂层浆;
浸轧的时间为10~30s;在25~35℃的水浴中进行成膜5~10s,在80~100℃条件下烘干5~10min;
其中,多功能粉末填料的制备方法包括以下步骤:
将A组分和B组分按照质量比为1:1~4:1通过接枝反应制得多功能粉末填料,其中A组分按照以总质量100%计,采用以下质量百分含量的组分:
所述B组分为无机轻质碳酸钙粉末。
2.根据权利要求1所述的多功能粉末填料的制备方法,其特征在于,所述的组分A的制备具体包括:将反应性阻燃剂溶解于二乙二醇二甲醚中,使反应性阻燃剂完全溶解,形成含反应性阻燃剂的溶液,将硅烷偶联剂与引发剂溶于二乙二醇二甲醚中,再用1~2h将其逐滴加入含反应性阻燃剂的溶液中,保持60~80℃反应24h,体系颜色逐渐由无色变为淡黄色,最后得到浅淡黄色澄清透明的均匀溶液,后经环己烷洗涤、过滤除去溶剂,得到淡黄色溶液的含磷阻燃改性剂,即为组分A。
3.根据权利要求1或2所述的多功能粉末填料的制备方法,其特征在于,所述的反应性阻燃剂为9,10-二氢-9-氧杂-10-磷杂菲-10-氧化物。
4.根据权利要求1或2所述的多功能粉末填料的制备方法,其特征在于,所述的引发剂为偶氮二异丁腈。
5.根据权利要求1或2所述的多功能粉末填料的制备方法,其特征在于,所述的硅烷偶联剂为乙烯基三甲氧基硅烷和甲基乙烯基二甲氧基硅烷,所述的乙烯基三甲氧基硅烷和甲基乙烯基二甲氧基硅烷的摩尔比为6~8:2~4。
6.根据权利要求1或2所述的多功能粉末填料的制备方法,其特征在于,通过接枝反应制得多功能粉末填料,具体包括:
将组分A与甲醇共混后加入B组分,在50~60℃条件下反应18~30h,后经过滤除去溶剂,在80~100℃条件下焙烘1~3h,后经研磨成粉末,即得到多功能粉末填料。
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