CN116876116A - 一种改性聚丙烯腈纤维的制备方法 - Google Patents

一种改性聚丙烯腈纤维的制备方法 Download PDF

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CN116876116A
CN116876116A CN202310898373.4A CN202310898373A CN116876116A CN 116876116 A CN116876116 A CN 116876116A CN 202310898373 A CN202310898373 A CN 202310898373A CN 116876116 A CN116876116 A CN 116876116A
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CN116876116B (zh
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杨世玉
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Zhejiang Zhili New Material Co ltd
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Abstract

本申请提供一种改性聚丙烯腈纤维的制备方法，属于聚丙烯腈纤维制造技术领域。分别制备聚丙烯腈纤维原丝、改性剂和改性液后，先将聚丙烯腈纤维原丝浸渍在氯酸乙醇溶液中改性后，再充分烘干、预氧化处理后，置于改性液中浸渍、充分烘干、预氧化氮气介质中炭化，得到成品改性聚丙烯腈纤维。上述方法获得的改性聚丙烯腈纤维不仅具有优异的阻燃性，还可以提高纤维的断裂强度、卷曲度和抱合力。

Description

一种改性聚丙烯腈纤维的制备方法
技术领域
本申请涉及一种改性聚丙烯腈纤维的制备方法，属于聚丙烯腈纤维制造技术领域。
背景技术
聚丙烯腈基纤维是20世纪中期发展起来的一种新型材料，具有质轻、价廉、耐高温、耐腐蚀、导电、阻燃等优异性能，应用领域涉及人民生活、医药交通、航海航天及国防科技等。聚丙烯腈基纤维具有适宜的纺织加工性能，可用于织造纯纺或混纺纺织面料。但聚丙烯腈纤维本身内部存在一定的结构缺陷，在碳化过程由于高温处理还会继续出现一些新的缺陷，造成碳化后纤维的卷曲度较低、抱合力较弱、强力下降，对后道纺纱工序造成一定的难度。
发明内容
有鉴于此，本申请提供一种改性聚丙烯腈纤维的制备方法，在获得优异阻燃性的同时，还可以改善聚丙烯腈纤维的纺纱性能，提高纤维的断裂强力。
具体地，本申请是通过以下方案实现的：
一种改性聚丙烯腈纤维的制备方法，包括以下步骤：
1)原丝制备：将聚丙烯腈粉末中加入N,N-二甲基甲酰胺，加热搅拌处理后，得到纺丝原液，采用高压静电纺丝工艺，得到聚丙烯腈纤维原丝，所述高压静电纺丝参数：溶液挤出速度0.5～0.8mL/h，电压15～25kV；
2)改性纳米Si/Cu颗粒的制备：称取0.05mol/L聚氧乙烯山梨醇酐单油酸酯100mL于四颈烧瓶中，加入适量连二亚硫酸钠充分搅拌，搅拌速度500转/分钟，并升温至80℃，量取0.5mol/L五水硫酸铜100～200mL于分液漏斗中，80℃下每分钟60～80滴的速度全部滴加完毕后继续搅拌反应2～3小时，降温后再加入纳米二氧化硅、十二烷基苯磺酸钠，室温继续搅拌60～120min，结束后在混合物中加入乙醇搅拌至浆糊状，球磨2～5h，烘干，得到改性纳米Si/Cu颗粒；
3)浸渍处理：将聚丙烯腈纤维原丝浸渍在氯酸乙醇溶液中，浸渍30～60min后，充分烘干，再于210～270℃预氧化处理10～60min；
4)改性整理：称取改性纳米Si/Cu颗粒、木质素磺酸钠、瓜尔胶加入去离子水溶解后，充分搅拌后在高速均质机上处理3～5min得改性整理液，然后将步骤3)处理得到的纤维浸渍于改性整理液中30～60min，再充分烘干后，于250～290℃预氧化处理30～60min，最后于氮气介质中、800～1000℃炭化2～3h，得到成品改性聚丙烯腈纤维。
上述方案采用聚丙烯腈粉末作为原料，采用凝胶纺丝工艺制备聚丙烯腈原丝，先用氯酸对原丝进行浸渍整理和预氧化处理，再用改性纳米Si/Cu颗粒对浸渍、预氧化处理后原丝进行改性整理，最后进行高温延伸和碳化处理，提高聚丙烯腈纤维的取向度，提高其断裂强力，改善其抱合力，该纤维同时还具有优异的阻燃性能。
进一步的，作为优选：
步骤1)中，
所述聚丙烯腈粉末的添加量为5～8％。
所述加热搅拌处理中，温度为80～150℃，时长40～50h。
步骤3)中，
所述氯酸乙醇溶液是由氯酸溶解于无水乙醇中得到，溶液浓度为1.0～2.0mol/L。
所述充分烘干的烘干温度为80～100℃，烘干时长25～40min。
步骤4)中，
所述改性纳米Si/Cu颗粒、木质素磺酸钠、瓜尔胶的质量百分比分别为2～15％、1～10％、1～6％。
所述充分烘干的烘干温度为80～100℃，烘干时长25～40min。
上述方案获得的改性聚丙烯腈纤维面料阻燃性能满足国家标准，续燃时间和阴燃时间均不超过0s，抗热传递性能好，水洗前后的断裂强力均超过600N。
附图说明
图1为实施例1中改性前后纤维的扫描电镜图，
放大倍数均为1000倍，a-未改性纤维，b-改性后纤维；
图2为实施例1中改性纳米Si/Cu整理前后聚丙烯腈纤维的FTIR图；
图3为改性纳米Si/Cu颗粒的TEM图。
具体实施方式
实施例1
本实施例一种改性聚丙烯腈纤维的制备方法，包括以下步骤：
(1)聚丙烯腈原丝制备：
将聚丙烯腈粉末置于烧瓶中，向其中加入N，N－二甲基甲酰胺后，加热至90℃搅拌48h，形成纺丝原液，纺丝原液中聚丙烯腈质量浓度为5％，采用高压静电纺丝机制备聚丙烯腈纤维。静电纺丝工艺参数为：溶液挤出速度0.6mL/h，接收距离20cm，电压21kV。
(2)改性纳米Si/Cu颗粒制备：
称取0.05mol/L聚氧乙烯山梨醇酐单油酸酯100mL于四颈烧瓶中，加入适量连二亚硫酸钠充分搅拌，搅拌速度500转/分钟，并升温至80℃，量取0.5mol/L五水硫酸铜100mL于分液漏斗中，80℃下每分钟60滴的速度全部滴加完毕后继续搅拌反应2小时，降温后再加入纳米二氧化硅、十二烷基苯磺酸钠，室温继续搅拌80min，结束后在混合物中加入乙醇搅拌至浆糊状，450r/min球磨3h，然后将球磨罐放置在鼓风式烘箱内100℃干燥12h，得到改性纳米Si/Cu颗粒。
对所得产物进行TEM检测，结果如图3所示：改性纳米Si/Cu颗粒的粒径大概保持在50-60nm范围之间，呈近似球状，具有明显微胶囊形态，在水溶液中呈“石榴状”聚集。
(3)聚丙烯腈原丝氯酸改性处理：
在分析天平上称取氯酸放入500mL烧杯中，加入无水乙醇溶解，配制1.0mol/L氯酸乙醇溶液100mL。再称取20.00g的聚丙烯腈纤维原丝，放入氯酸溶液中浸渍30min，浸渍温度40℃，再放入100℃烘箱内下烘干30min，待充分干燥后取出，放入预氧化炉中在200℃下预氧化10min。
(4)改性聚丙烯腈高性能纤维的制备：
称取10.00g的改性纳米Si/Cu颗粒、5.00g的木质素磺酸钠、3.00g的瓜尔胶溶解于去离子水中配制成100mL溶液，充分搅拌后加入在高速均质机上处理5min得到改性液，然后将预氧化处理后的纤维浸渍于改性液中30min，再放入80℃烘箱内下烘干30min，待充分干燥后取出。放入预氧化炉中在270℃下预氧化10～30min，最后将预氧化处理后的纤维转入氮气介质中，于800℃炭化处理3h，得到改性聚丙烯腈纤维。
对步骤(1)、(3)、(4)得到的纤维分别进行测试，结果如图1～3所示。
从图1可以看出：未改性纤维表面较光滑，而改性后纤维间附着较多颗粒状物质，纤维表面可见有膜状物质包裹。
经步骤(4)的改性整理后的纤维如图2所示，与未改性纤维相比，改性后纤维在1720cm-1处羧基中C＝O的伸缩振动峰以及1250cm-1处C-O的对称、不对称伸缩振动峰的吸收强度明显增强，在1020cm-1附近可能出现的-OH振动峰，说明整理后纤维活性基团增加，该现象有利于改善纤维内部缺陷。
将上述方法所得改性聚丙烯腈纤维通过紧密赛络纺纺纱后织造。
对上述方法得到的改性聚丙烯腈织物进行性能测试，结果如表1所示。
表1：改性聚丙烯腈纤维所得面料的性能对照表
从上表可以看出：上述方法织造的改性聚丙烯腈面料具有优异的阻燃性能、耐高温和耐酸碱腐蚀性能，还具有优异的断裂强力，环保舒适。
本案还对其他影响纱线、面料性能的因素进行了实验，具体如实施例2～3所示。
实施例2
本实施例与实施例1的设置相同，区别在于：改性液中，改性纳米Si/Cu铜颗粒的添加量(质量百分比)不同。结果如表2所示。
表2：不同改性纳米Si/Cu颗粒添加量对纤维性能的影响
从表2可以看出：随着改性纳米Si/Cu颗粒质量百分数的增加，改性聚丙烯腈纱线的断裂强度、屈服强力和初始模量逐渐增加，断裂伸长率略有增加；与未改性聚丙烯腈纤维相比，改性聚丙烯腈纱线的断裂强度、初始模量和屈服强力提高。
实施例3
本实施例与实施例1的设置相同，但步骤(3)中的浸渍温度与时间参数不同，结果如表3所示。
表3：不同浸渍参数对纱线性能的影响
对比表3可以看出：随着浸渍温度的提高，浸渍时间的延长，改性聚丙烯腈纱线的断裂强度、屈服强力和初始模量略有提高，当浸渍温度40℃、浸渍时间为30min时(即实施例1)，纱线综合性能相对最佳。
纱线断裂强度、屈服强力和初始模量的测试：根据标准GB/T3916-1997《单根纱线断裂强力及断裂伸长的测定》测定纱线断裂强度及伸长率。测试条件：温度20℃，相对湿度65％。

Claims (8)

1.一种改性聚丙烯腈纤维的制备方法，其特征在于，包括以下步骤：
1）原丝制备：将聚丙烯腈粉末中加入N,N-二甲基甲酰胺，加热搅拌处理后，得到纺丝原液，采用高压静电纺丝工艺，得到聚丙烯腈纤维原丝，所述高压静电纺丝参数：溶液挤出速度0.5～0.8mL/h，电压15～25kV；
2）改性纳米Si/Cu颗粒的制备：向聚氧乙烯山梨醇酐单油酸酯中加入连二亚硫酸钠充分混合，搅拌，升温至80℃，以每分钟60～80滴的速度滴入五水硫酸铜后，继续搅拌反应2～3小时，降至室温，加入纳米二氧化硅、十二烷基苯磺酸钠，继续搅拌60～120min后，加入乙醇搅拌至浆糊状，球磨2～5h，烘干，得到改性纳米Si/Cu颗粒；
3）浸渍处理：将聚丙烯腈纤维原丝浸渍在氯酸乙醇溶液中，浸渍30～60min后，充分烘干，再于180～250℃预氧化处理10～60min；
4）改性处理：称取改性纳米Si/Cu颗粒、木质素磺酸钠、瓜尔胶溶解后，均质处理得改性液，然后将步骤3）处理得到的纤维浸渍于改性液中30～60min，再充分烘干后，于250～290℃预氧化处理30～60min，最后于氮气介质中、800～1000℃炭化2～3h，得到成品改性聚丙烯腈纤维。
2.根据权利要求1所述的一种改性聚丙烯腈纤维的制备方法，其特征在于：步骤1）中，所述聚丙烯腈粉末的添加量为5～8%。
3.根据权利要求1所述的一种改性聚丙烯腈纤维的制备方法，其特征在于：步骤1）中，所述加热搅拌处理中，温度为80～150℃，时长40～50h。
4.根据权利要求1所述的一种改性聚丙烯腈纤维的制备方法，其特征在于：步骤3）中，所述氯酸乙醇溶液是由氯酸溶解于无水乙醇中得到，溶液浓度为1.0～2.0mol/L。
5.根据权利要求1所述的一种改性聚丙烯腈纤维的制备方法，其特征在于：步骤3）中，浸渍温度30～40℃，浸渍时长30～60min。
6.根据权利要求1所述的一种改性聚丙烯腈纤维的制备方法，其特征在于：步骤3）中，所述充分烘干的烘干温度为80～100℃，烘干时长25～40min。
7.根据权利要求1所述的一种改性聚丙烯腈纤维的制备方法，其特征在于：步骤4）中，所述改性纳米Si/Cu颗粒、木质素磺酸钠、瓜尔胶的添加质量百分数为2～15%、1～10%、1～6%。
8.根据权利要求1所述的一种改性聚丙烯腈纤维的制备方法，其特征在于：步骤4）中，所述充分烘干的烘干温度为80～100℃，烘干时长25～40min。
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