CN113215817A - 一种具有阻燃功能的华达呢面料的制备方法 - Google Patents
一种具有阻燃功能的华达呢面料的制备方法 Download PDFInfo
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Abstract
本发明提供了一种具有阻燃功能的华达呢面料的制备方法,包括以下步骤:S1.硅溶胶的制备;S2.溶胶涂覆的华达呢面料的制备S3.含碳酸钙的华达呢面料的制备;S4.壳聚糖‑石墨烯‑碳酸钙复合阻燃华达呢面料的制备,得到阻燃型华达呢面料。本发明提供一种高聚物/无机纳米复合材料阻燃剂,对织物进行复合整理,得到一种具备阻燃效果并对环境友好的复合阻燃面料。
Description
技术领域
本发明涉及绿色阻燃面料领域,具体涉及一种具有阻燃功能的华达呢面料的制备方法。
背景技术
生态环境问题是当今世界人类面临的中心问题之一,目前地球生态环境的恶化已明显威胁人类的生存。据不完全统计,世界上现有生产或使用的化学品多达10万余种。仅美国化学工业每年就要排放30多亿吨的化学废弃物进入环境。绿色化学是将原料分子中的原子百分之百地转变成产物,不生成或很少生成副产品或废物,实现废物“零排放”的一种化学生产工艺。该工艺具有原料无毒无害、转化率高、环境友好等特性。绿色阻燃剂因其从设计思想、原料选择、配色设计、工艺流程到产品的保存、应用及废品处理等各个环节都遵从绿色化学理念,也就是说最大限度地减少或取消那些对人类健康、生态环境、社会安全有害的原料和生产工艺的使用,不以人的安全和环境污染为代价来提高材料的阻燃效果,所以它真正实现了从源头上阻止阻燃材料的污染。
绿色阻燃剂如无卤阻燃剂,因其高效、低烟、低毒等特性,最终可以取代含卤阻燃剂。磷系阻燃剂和无机氢氧化物也应进一步加强研究,特别是在阻燃剂的微胶囊化技术、超细化技术、表面改性处理技术等方面。而高聚物/无机纳米复合材料阻燃剂因其具有优良的阻燃性能和物理性能以及无毒、无污染等优点,必将成为下一步研究开发的重点。随着人们对聚合物阻燃体系环境友好性要求的不断提高,纳米高聚物/无机复合材料应当是今后阻燃剂改性研究的主要方向。
发明内容
要解决的技术问题:本发明的目的是提供一种高聚物/无机纳米复合材料阻燃剂,对织物进行复合整理,得到一种具备阻燃效果并对环境友好的复合阻燃面料。
技术方案:一种具有阻燃功能的华达呢面料的制备方法,包括以下步骤:
S1.硅溶胶的制备:将正硅酸四乙酯和无水乙醇混合均匀,边搅拌边加入含有CaCl2的NH3·H2O溶液,然后加入PEG混合搅拌均匀,最后得到均一的无色透明的硅溶胶;
S2.溶胶涂覆的华达呢面料的制备:将华达呢面料加入至硅溶胶中浸泡,浸轧,先在常温下进行老化,然后升温进行老化,得到溶胶涂覆的华达呢面料;
S3.含碳酸钙的华达呢面料的制备:将步骤S2中制备的溶胶涂覆的华达呢面料浸渍于含有Na2CO3的溶液中,充分接触反应,得到含有含碳酸钙的华达呢面料;
S4.壳聚糖-石墨烯-碳酸钙复合阻燃华达呢面料的制备:将步骤S3制备的华达呢面料浸渍于壳聚糖-石墨烯溶液中,在壳聚糖-石墨烯溶液中浸泡,然后浸轧,在一定温度烘干,得到阻燃型华达呢面料。
优选的,所述华达呢面料为含棉华达呢面料。
优选的,所述正硅酸四乙酯和乙醇的摩尔比为1:30-35。
优选的,所述含有CaCl2的NH3·H2O溶液加入量为按照溶液体系中SiO2:NH3:CaCl2的摩尔比为2:1:0.2-0.5。
优选的,所述华达呢在硅溶胶中的浸泡时间为10-30min,轧余率为60-90%,常温老化时间为20-48h,升温老化的温度为40-60℃,时间为8-12h。
优选的,所述华达呢面料浸渍于壳聚糖-石墨烯溶液中浸泡时间为10-30min,轧余率为60-90%,烘干温度为50-60℃。
优选的,所述壳聚糖-石墨烯溶液的制备方法为:将壳聚糖溶解于体积浓度为2-5%的冰醋酸溶液中,制备浓度为1-2wt.%的壳聚糖溶液,然后按照壳聚糖和石墨烯的比例为30:1-5的比例将石墨烯加入至壳聚糖溶液中,得到壳聚糖-石墨烯溶液。
有益效果:本发明的阻燃面料具有以下优点:
本发明的阻燃通过溶胶-凝胶形成的无机膜起到的隔绝空气以及隔热作用,在纤维表面形成了致密的膨胀隔热炭层和CNT的网络结构,构筑了完善的绝热防护层,从而使得棉织物在燃烧后保持了完整的纤维结构。
具体实施方式
实施例1
一种具有阻燃功能的华达呢面料的制备方法,包括以下步骤:
S1.硅溶胶的制备:将正硅酸四乙酯和无水乙醇混合均匀,正硅酸四乙酯和乙醇的摩尔比为1:30,边搅拌边加入含有CaCl2的NH3·H2O溶液,溶液体系中SiO2:NH3:CaCl2的摩尔比为2:1:0.2,然后加入PEG混合搅拌均匀,最后得到均一的无色透明的硅溶胶;
S2.溶胶涂覆的华达呢面料的制备:将华达呢面料加入至硅溶胶中浸泡10min,浸轧,轧余率为60%,先在常温下进行老化20h,然后在40℃升温进行老化12h,得到溶胶涂覆的华达呢面料;
S3.含碳酸钙的华达呢面料的制备:将步骤S2中制备的溶胶涂覆的华达呢面料浸渍于含有Na2CO3的溶液中,充分接触反应,得到含有含碳酸钙的华达呢面料;
S4.壳聚糖-石墨烯-碳酸钙复合阻燃华达呢面料的制备:将步骤S3制备的华达呢面料浸渍于壳聚糖-石墨烯溶液中,在壳聚糖-石墨烯溶液中浸泡10min,然后浸轧,轧余率为60%,在50℃温度烘干,得到阻燃型华达呢面料;
其中,将壳聚糖溶解于体积浓度为2%的冰醋酸溶液中,制备浓度为1wt.%的壳聚糖溶液,然后按照壳聚糖和石墨烯的比例为30:1的比例将石墨烯加入至壳聚糖溶液中,得到壳聚糖-石墨烯溶液。
实施例2
一种具有阻燃功能的华达呢面料的制备方法,包括以下步骤:
S1.硅溶胶的制备:将正硅酸四乙酯和无水乙醇混合均匀,正硅酸四乙酯和乙醇的摩尔比为1:35,边搅拌边加入含有CaCl2的NH3·H2O溶液,溶液体系中SiO2:NH3:CaCl2的摩尔比为2:1:0.5,然后加入PEG混合搅拌均匀,最后得到均一的无色透明的硅溶胶;
S2.溶胶涂覆的华达呢面料的制备:将华达呢面料加入至硅溶胶中浸泡30min,浸轧,轧余率为90%,先在常温下进行老化48h,然后在60℃升温进行老化8h,得到溶胶涂覆的华达呢面料;
S3.含碳酸钙的华达呢面料的制备:将步骤S2中制备的溶胶涂覆的华达呢面料浸渍于含有Na2CO3的溶液中,充分接触反应,得到含有含碳酸钙的华达呢面料;
S4.壳聚糖-石墨烯-碳酸钙复合阻燃华达呢面料的制备:将步骤S3制备的华达呢面料浸渍于壳聚糖-石墨烯溶液中,在壳聚糖-石墨烯溶液中浸泡30min,然后浸轧,轧余率为90%,在60℃温度烘干,得到阻燃型华达呢面料;
其中,将壳聚糖溶解于体积浓度为5%的冰醋酸溶液中,制备浓度为2wt.%的壳聚糖溶液,然后按照壳聚糖和石墨烯的比例为30:5的比例将石墨烯加入至壳聚糖溶液中,得到壳聚糖-石墨烯溶液。
实施例3
一种具有阻燃功能的华达呢面料的制备方法,包括以下步骤:
S1.硅溶胶的制备:将正硅酸四乙酯和无水乙醇混合均匀,正硅酸四乙酯和乙醇的摩尔比为1:31,边搅拌边加入含有CaCl2的NH3·H2O溶液,溶液体系中SiO2:NH3:CaCl2的摩尔比为2:1:0.3,然后加入PEG混合搅拌均匀,最后得到均一的无色透明的硅溶胶;
S2.溶胶涂覆的华达呢面料的制备:将华达呢面料加入至硅溶胶中浸泡15-25min,浸轧,轧余率为70%,先在常温下进行老化30h,然后在45℃升温进行老化10h,得到溶胶涂覆的华达呢面料;
S3.含碳酸钙的华达呢面料的制备:将步骤S2中制备的溶胶涂覆的华达呢面料浸渍于含有Na2CO3的溶液中,充分接触反应,得到含有含碳酸钙的华达呢面料;
S4.壳聚糖-石墨烯-碳酸钙复合阻燃华达呢面料的制备:将步骤S3制备的华达呢面料浸渍于壳聚糖-石墨烯溶液中,在壳聚糖-石墨烯溶液中浸泡15min,然后浸轧,轧余率为80%,在50℃温度烘干,得到阻燃型华达呢面料;
其中,将壳聚糖溶解于体积浓度为3%的冰醋酸溶液中,制备浓度为1.2wt.%的壳聚糖溶液,然后按照壳聚糖和石墨烯的比例为30:2的比例将石墨烯加入至壳聚糖溶液中,得到壳聚糖-石墨烯溶液。
实施例4
一种具有阻燃功能的华达呢面料的制备方法,包括以下步骤:
S1.硅溶胶的制备:将正硅酸四乙酯和无水乙醇混合均匀,正硅酸四乙酯和乙醇的摩尔比为1:34,边搅拌边加入含有CaCl2的NH3·H2O溶液,溶液体系中SiO2:NH3:CaCl2的摩尔比为2:1:0.4,然后加入PEG混合搅拌均匀,最后得到均一的无色透明的硅溶胶;
S2.溶胶涂覆的华达呢面料的制备:将华达呢面料加入至硅溶胶中浸泡15-25min,浸轧,轧余率为80%,先在常温下进行老化40h,然后在55℃升温进行老化9h,得到溶胶涂覆的华达呢面料;
S3.含碳酸钙的华达呢面料的制备:将步骤S2中制备的溶胶涂覆的华达呢面料浸渍于含有Na2CO3的溶液中,充分接触反应,得到含有含碳酸钙的华达呢面料;
S4.壳聚糖-石墨烯-碳酸钙复合阻燃华达呢面料的制备:将步骤S3制备的华达呢面料浸渍于壳聚糖-石墨烯溶液中,在壳聚糖-石墨烯溶液中浸15-25min,然后浸轧,轧余率为70%,在60℃温度烘干,得到阻燃型华达呢面料;
其中,将壳聚糖溶解于体积浓度为4%的冰醋酸溶液中,制备浓度为1.6wt.%的壳聚糖溶液,然后按照壳聚糖和石墨烯的比例为30:4的比例将石墨烯加入至壳聚糖溶液中,得到壳聚糖-石墨烯溶液。
实施例5
一种具有阻燃功能的华达呢面料的制备方法,包括以下步骤:
S1.硅溶胶的制备:将正硅酸四乙酯和无水乙醇混合均匀,正硅酸四乙酯和乙醇的摩尔比为1:32,边搅拌边加入含有CaCl2的NH3·H2O溶液,溶液体系中SiO2:NH3:CaCl2的摩尔比为2:1:0.35,然后加入PEG混合搅拌均匀,最后得到均一的无色透明的硅溶胶;
S2.溶胶涂覆的华达呢面料的制备:将华达呢面料加入至硅溶胶中浸泡20min,浸轧,轧余率为75%,先在常温下进行老化35h,然后在50℃升温进行老化10h,得到溶胶涂覆的华达呢面料;
S3.含碳酸钙的华达呢面料的制备:将步骤S2中制备的溶胶涂覆的华达呢面料浸渍于含有Na2CO3的溶液中,充分接触反应,得到含有含碳酸钙的华达呢面料;
S4.壳聚糖-石墨烯-碳酸钙复合阻燃华达呢面料的制备:将步骤S3制备的华达呢面料浸渍于壳聚糖-石墨烯溶液中,在壳聚糖-石墨烯溶液中浸泡20min,然后浸轧,轧余率为75%,在55℃温度烘干,得到阻燃型华达呢面料;
其中,将壳聚糖溶解于体积浓度为3.6%的冰醋酸溶液中,制备浓度为1.4wt.%的壳聚糖溶液,然后按照壳聚糖和石墨烯的比例为30:3的比例将石墨烯加入至壳聚糖溶液中,得到壳聚糖-石墨烯溶液。
对比例1
一种具有阻燃功能的华达呢面料的制备方法,包括以下步骤:
S1.硅溶胶的制备:将正硅酸四乙酯和无水乙醇混合均匀,正硅酸四乙酯和乙醇的摩尔比为1:34,边搅拌边加入NH3·H2O溶液,溶液体系中SiO2:NH3的摩尔比为2:1,然后加入PEG混合搅拌均匀,最后得到均一的无色透明的硅溶胶;
S2.溶胶涂覆的华达呢面料的制备:将华达呢面料加入至硅溶胶中浸泡15-25min,浸轧,轧余率为80%,先在常温下进行老化40h,然后在55℃升温进行老化9h,得到溶胶涂覆的华达呢面料;
S3.壳聚糖-石墨烯复合阻燃华达呢面料的制备:将步骤S3制备的华达呢面料浸渍于壳聚糖-石墨烯溶液中,在壳聚糖-石墨烯溶液中浸15-25min,然后浸轧,轧余率为70%,在60℃温度烘干,得到阻燃型华达呢面料;
其中,将壳聚糖溶解于体积浓度为4%的冰醋酸溶液中,制备浓度为1.6wt.%的壳聚糖溶液,然后按照壳聚糖和石墨烯的比例为30:4的比例将石墨烯加入至壳聚糖溶液中,得到壳聚糖-石墨烯溶液。
对比例2
一种具有阻燃功能的华达呢面料的制备方法,包括以下步骤:
S1.硅溶胶的制备:将正硅酸四乙酯和无水乙醇混合均匀,正硅酸四乙酯和乙醇的摩尔比为1:34,边搅拌边加入含有CaCl2的NH3·H2O溶液,溶液体系中SiO2:NH3:CaCl2的摩尔比为2:1:0.4,然后加入PEG混合搅拌均匀,最后得到均一的无色透明的硅溶胶;
S2.溶胶涂覆的华达呢面料的制备:将华达呢面料加入至硅溶胶中浸泡15-25min,浸轧,轧余率为80%,先在常温下进行老化40h,然后在55℃升温进行老化9h,得到溶胶涂覆的华达呢面料;
S3.含碳酸钙的华达呢面料的制备:将步骤S2中制备的溶胶涂覆的华达呢面料浸渍于含有Na2CO3的溶液中,充分接触反应,得到含有含碳酸钙的华达呢面料;
S4.壳聚糖-碳酸钙复合阻燃华达呢面料的制备:将步骤S3制备的华达呢面料浸渍于壳聚糖溶液中,在壳聚糖溶液中浸15-25min,然后浸轧,轧余率为70%,在60℃温度烘干,得到阻燃型华达呢面料;
其中,将壳聚糖溶解于体积浓度为4%的冰醋酸溶液中,制备浓度为1.6wt.%的壳聚糖溶液。根据GB/T 5455-1997,采用AG5100A垂直燃烧测试仪进行织物样品的燃烧性能测试
点火时间(s) | 续燃时间(s) | 余灼时间(s) | 残余质量(%) | |
普通华达呢 | 0 | 90 | 256 | 0.5 |
实施例1 | 5 | 60 | 0 | 85.7 |
实施例2 | 8 | 35 | 0 | 87.5 |
实施例3 | 10 | 0 | 0 | 98.2 |
实施例4 | 11 | 0 | 0 | 96.5 |
实施例5 | 10 | 0 | 0 | 97.6 |
对比例1 | 10 | 55 | 23 | 76.8 |
对比例2 | 4 | 55 | 104 | 22.1 |
Claims (7)
1.一种具有阻燃功能的华达呢面料的制备方法,其特征在于,包括以下步骤:
S1.硅溶胶的制备:将正硅酸四乙酯和无水乙醇混合均匀,边搅拌边加入含有CaCl2的NH3·H2O溶液,然后加入PEG混合搅拌均匀,最后得到均一的无色透明的硅溶胶;
S2.溶胶涂覆的华达呢面料的制备:将华达呢面料加入至硅溶胶中浸泡,浸轧,先在常温下进行老化,然后升温进行老化,得到溶胶涂覆的华达呢面料;
S3.含碳酸钙的华达呢面料的制备:将步骤S2中制备的溶胶涂覆的华达呢面料浸渍于含有Na2CO3的溶液中,充分接触反应,得到含有含碳酸钙的华达呢面料;
S4.壳聚糖-石墨烯-碳酸钙复合阻燃华达呢面料的制备:将步骤S3制备的华达呢面料浸渍于壳聚糖-石墨烯溶液中,在壳聚糖-石墨烯溶液中浸泡,然后浸轧,在一定温度烘干,得到阻燃型华达呢面料。
2.根据权利要求1所述具有阻燃功能的华达呢面料的制备方法,其特征在于:所述华达呢面料为含棉华达呢面料。
3.根据权利要求1所述具有阻燃功能的华达呢面料的制备方法,其特征在于:所述正硅酸四乙酯和乙醇的摩尔比为1:30-35。
4.根据权利要求1所述具有阻燃功能的华达呢面料的制备方法,其特征在于:所述含有CaCl2的NH3·H2O溶液加入量为按照溶液体系中SiO2:NH3:CaCl2的摩尔比为2:1:0.2-0.5。
5.根据权利要求1所述具有阻燃功能的华达呢面料的制备方法,其特征在于:所述华达呢在硅溶胶中的浸泡时间为10-30min,轧余率为60-90%,常温老化时间为20-48h,升温老化的温度为40-60℃,时间为8-12h。
6.根据权利要求1所述具有阻燃功能的华达呢面料的制备方法,其特征在于:所述华达呢面料浸渍于壳聚糖-石墨烯溶液中浸泡时间为10-30min,轧余率为60-90%,烘干温度为50-60℃。
7.根据权利要求1所述具有阻燃功能的华达呢面料的制备方法,其特征在于,所述壳聚糖-石墨烯溶液的制备方法为:将壳聚糖溶解于体积浓度为2-5%的冰醋酸溶液中,制备浓度为1-2wt.%的壳聚糖溶液,然后按照壳聚糖和石墨烯的比例为30:1-5的比例将石墨烯加入至壳聚糖溶液中,得到壳聚糖-石墨烯溶液。
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