CN108642866A - 一种用于纺织品的阻燃抑烟溶胶的制备方法及产物 - Google Patents
一种用于纺织品的阻燃抑烟溶胶的制备方法及产物 Download PDFInfo
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Abstract
本发明涉及一种用于纺织品的阻燃抑烟溶胶的制备方法及产物，制备方法如下：1)将铝盐和聚磷酸铵加入到水中混合，调节pH为7‑10，分离后得到絮状沉淀物；将絮状沉淀物分散于水中，加入稀酸溶液待用；2)将蒙脱土加入到聚苯乙烯磺酸钠水溶液中反应，分离后得到改性的蒙脱土；3)将正硅酸乙酯加入到乙醇水溶液中混合，继续加入步骤1)产物和步骤2)产物混合，调节pH为1‑5进行反应，得到阻燃抑烟溶胶。本发明通过合成工艺的改进，将多种阻燃化合物形成结构可控的阻燃溶胶，提高其阻燃抑烟效率及分散性。
Description
技术领域
本发明涉及阻燃抑烟溶胶的制备领域，具体涉及一种用于纺织品的阻燃抑烟溶胶的制备方法及产物。
背景技术
高分子材料在建筑、航空、汽车、电器等方面的应用迅速扩大，但是绝大部分高分子材料的极限氧指数都要低于20％，当遇到高温或者明火时就容易被点燃，增加了火灾发生的概率。因此，加大了对难燃材料的需求。
纺织品主要由天然纤维和合成纤维构成，天然纤维是从植物或动物上直接获取的纤维；合成纤维是用高分子化合物(包括天然的或人工合成的)为原料，经过制备纺丝原液、纺丝和后处理等一系列的工序制得的具有纺织性能的纤维。因为天然纤维和合成纤维都具有易燃性，因此将阻燃剂应用到纺织品中对于预防火灾具有重要意义。
目前，阻燃剂在应用过程中已经暴露出很多问题，如有毒、污染环境等。随着人们环保意识的增强，这些问题日益受到重视。人们不但期望阻燃剂具有高效性，而且希望在其生产过程中尽量减少对环境的污染。当阻燃剂被整理到织物上，与人的皮肤接触时，要求其毒性应降为最低。并在日益严苛的阻燃法规和阻燃剂环保化的发展趋势下，开发出无卤环保阻燃剂具有十分重要的意义。
但是目前阻燃高分子材料制备过程中，是将多种阻燃剂复配协效，但难以同时达到阻燃元素的均匀分布，从而阻燃效率低。
发明内容
本发明的目的在于针对现有技术的不足，提供一种用于纺织品的阻燃抑烟溶胶的制备方法，通过合成工艺的改进，将多种阻燃化合物形成结构可控的阻燃溶胶，提高其阻燃抑烟效率及分散性。
本发明所提供的技术方案为：
一种用于纺织品的阻燃抑烟溶胶的制备方法，包括如下步骤：
1)将铝盐和聚磷酸铵加入到水中混合，调节pH为7-10，分离后得到絮状沉淀物；将絮状沉淀物分散于水中，加入稀酸溶液待用；
2)将蒙脱土加入到聚苯乙烯磺酸钠水溶液中反应，分离后得到改性的蒙脱土；
3)将正硅酸乙酯加入到乙醇水溶液中混合，继续加入步骤1)产物和步骤2)产物混合，调节pH为1-5进行反应，得到阻燃抑烟溶胶。
本发明步骤1)中将聚磷酸铵掺杂于氢氧化铝沉淀物中，防止聚磷酸铵溶解在水中，分散后加入稀酸溶液是为了得到氢氧化铝/聚磷酸铵杂化物溶胶，有利于步骤3)进一步包覆改性。步骤2)中采用聚苯乙烯磺酸钠对蒙脱土进行改性，提高蒙脱土在步骤3)溶液中均匀分散，有利于步骤3)进一步包覆改性。步骤3)中采用正硅酸乙酯水解产生的二氧化硅包覆在聚磷酸铵掺杂的氢氧化铝和改性的蒙脱土表面，得到结构可控的阻燃溶胶，不仅提高了无机阻燃剂的分散性，更是结合了多种阻燃化合物，协同增效提高其阻燃抑烟效率。
作为优选，所述步骤1)铝盐和聚磷酸铵加入到水中混合时温度为20-40℃，时间为1-5h。
作为优选，所述步骤1)调节pH时加入碱液，如常用氨水、碳酸钠、氢氧化钠或氢氧化钾溶液。
作为优选，所述步骤1)铝盐为硝酸铝或硫酸铝。进一步优选为九水硝酸铝、十八水硫酸铝或十六水硫酸铝。
作为优选，所述步骤1)铝盐和聚磷酸铵的质量比为1:1-10。
作为优选，所述步骤1)铝盐与水的质量比为1:5-50。
作为优选，所述步骤1)稀酸溶液的质量分数为5-15％，所述稀酸溶液为冰醋酸、硫酸、硝酸或盐酸溶液；所述稀酸溶液与铝盐的质量比为1:50-100。
作为优选，所述步骤2)反应时温度为15-40℃，时间为0.5-4h。
作为优选，所述步骤2)聚苯乙烯磺酸钠水溶液中聚苯乙烯磺酸钠与水的质量比为1:50-100。
作为优选，所述步骤2)聚苯乙烯磺酸钠与蒙脱土的质量比为1:50-100。
作为优选，所述步骤3)进行反应的温度为20-40℃，时间为1-6h。
作为优选，所述步骤3)乙醇水溶液中水与乙醇的质量比为1:1-10，乙醇与正硅酸乙酯的质量比为1:1-10。
作为优选，所述步骤3)中步骤1)产物与步骤2)产物的质量比为1:1-10。
作为优选，所述步骤3)中正硅酸乙酯与步骤1)产物和步骤2)产物的总质量之比为1:1-10。
本发明还涉及一种如上述的制备方法制备得到的用于纺织品的阻燃抑烟溶胶。该阻燃抑烟溶胶可适合用作聚酯、聚丙烯、聚乙烯纺织品等的高效阻燃抑烟剂，具有优异的阻燃性、抑烟性、抗熔滴和自熄性。
同现有技术相比，本发明的有益效果体现在：
(1)本发明中阻燃抑烟溶胶的工艺可操作性高，成本可控，较容易实现产业化生产，具有巨大的经济和社会效益。
(2)本发明中制备的阻燃抑烟溶胶其阻燃抑烟效率高，具有耐高温，分散性优异，有效防析出，无毒，环保等优点。
(3)本发明中制备的阻燃抑烟溶胶的粒径分布均匀，溶胶为白色溶液，与颜料色配型优异，应用领域广泛，有很好的应用开发前景。
附图说明
图1为实施例1中制备的阻燃抑烟溶胶的光学显微镜照片；
图2为实施例2中制备的阻燃抑烟溶胶的光学显微镜照片；
图3为实施例3中制备的阻燃抑烟溶胶的光学显微镜照片；
图4为对比例1中制备的溶胶的光学显微镜照片；
图5为对比例2中制备的溶胶的光学显微镜照片。
具体实施方式
下面通过实施例对本发明作进一步具体的描述，有必要在此指出的是以下实施例只用于对本发明进行进一步说明，不能理解为对本发明保护范围的限制，该领域的技术熟练的人可根据上述本发明的内容做出的一些非本质的改进和调整，仍属于本发明的保护范围。
实施例1
1)将1kg九水硝酸铝和1kg聚磷酸铵加入到10kg去离子水中，25℃条件下混合1h，然后加入氨水使溶液pH调节为8，冷却、过滤后；将产物分散于10kg水中，然后加入质量分数10％硝酸水溶液0.02kg，待用。
2)将1kg聚苯乙烯磺酸钠和50kg去离子水搅拌均匀，然后加入50kg蒙脱土，25℃条件下反应1h后，再经冷却、过滤、待用。
3)将2kg正硅酸乙酯和1kg无水乙醇加入到1kg去离子水中，然后加入步骤1)产物1kg、步骤2)产物1kg，再用质量分数10％盐酸水溶液使溶液pH调节为3.5，25℃条件下反应3h后，获得阻燃抑烟溶胶。
所得的阻燃抑烟溶胶的光学显微镜照片如图1所示，此阻燃抑烟溶胶粒径分布均匀，无团聚体出现，说明分散性优异。
实施例2
1)将1kg九水硝酸铝和5kg聚磷酸铵加入到30kg去离子水中，25℃条件下混合1h，然后加入氨水使溶液pH调节为8，冷却、过滤后；将产物分散于10kg水中，然后加入质量分数10％硝酸水溶液0.013kg，待用。
2)将1kg聚苯乙烯磺酸钠和75kg去离子水搅拌均匀，然后加入75kg蒙脱土，25℃条件下反应1h后，再经冷却、过滤、待用。
3)将2kg正硅酸乙酯和2kg无水乙醇加入到0.5kg去离子水中，然后加入步骤1)产物1kg、步骤2)产物5kg，再用质量分数10％盐酸水溶液使溶液pH调节为3.5，35℃条件下反应5h后，获得阻燃抑烟溶胶。
所得的阻燃抑烟溶胶的光学显微镜照片如图2所示，此阻燃抑烟溶胶粒径分布均匀，无团聚体出现，说明分散性优异。
实施例3
1)将1kg九水硝酸铝和10kg聚磷酸铵加入到50kg去离子水中，30℃条件下混合1h，然后加入氨水使溶液pH调节为9，冷却、过滤后；将产物分散于10kg水中，然后加入质量分数10％硝酸水溶液0.02kg，待用。
2)将1kg聚苯乙烯磺酸钠和100kg去离子水搅拌均匀，然后加入100kg蒙脱土，35℃条件下反应3h后，再经冷却、过滤、待用。
3)将2kg正硅酸乙酯和1kg无水乙醇加入到1kg去离子水中，然后加入步骤1)产物2kg、步骤2)产物2kg，再用质量分数10％盐酸水溶液使溶液pH调节为3.5，35℃条件下反应3h后，获得阻燃抑烟溶胶。
所得的阻燃抑烟溶胶的光学显微镜照片如图3所示，此阻燃抑烟溶胶粒径分布均匀，无团聚体出现，说明分散性优异。
对比例1
将1kg蒙脱土与100kg去离子水均匀分散，得到溶胶产物。所得的产物的光学显微镜照片如图4所示，此阻燃抑烟溶胶粒径分布不均匀，大量团聚体出现，说明分散性差。
对比例2
将1kg聚磷酸铵与100kg去离子水均匀分散，得到溶胶产物。所得的产物的光学显微镜照片如图5所示，此阻燃抑烟溶胶粒径分布不均匀，大量团聚体出现，说明分散性差。
阻燃性能和抑烟性能：
采用实施例1～3和对比例1～2中的产品，将其应用于PET/PA6纺粘水刺非织造材料。
分别取上述PET/PA6纺粘水刺非织造材料在实施例1～3和对比例1～2中浸渍，二浸二轧，60℃干燥30min，160℃高温烘培5min，得到涂层整理的PET/PA6纺粘水刺非织造材料，测试其阻燃性能和抑烟性能，部分试验结果如表1所示。
表1为实施例1～3及对比例1～2分别制备的材料的阻燃性能和抑烟性能
对比例1中是使用纯蒙脱土，单一使用阻燃效率低，填充质量大于50％才能有效果。对比例2中是使用纯聚磷酸铵，单一使用阻燃效率低，不能满足阻燃等级要求。
根据表1可以看出，本发明专利制备的阻燃抑烟的溶胶应用于PET/PA6纺粘水刺非织造材料中，它具有高效的阻燃和抑烟性能以及优异的抗熔滴、自熄性能，也解决由于单一阻燃剂效率低和添加量大带来的成本问题。
Claims (9)
1.一种用于纺织品的阻燃抑烟溶胶的制备方法，其特征在于，包括如下步骤：
1)将铝盐和聚磷酸铵加入到水中混合，调节pH为7-10，分离后得到絮状沉淀物；将絮状沉淀物分散于水中，加入稀酸溶液待用；
2)将蒙脱土加入到聚苯乙烯磺酸钠水溶液中反应，分离后得到改性的蒙脱土；
3)将正硅酸乙酯加入到乙醇水溶液中混合，继续加入步骤1)产物和步骤2)产物混合，调节pH为1-5进行反应，得到阻燃抑烟溶胶。
2.根据权利要求1所述的用于纺织品的阻燃抑烟溶胶的制备方法，其特征在于，所述步骤1)铝盐为硝酸铝或硫酸铝。
3.根据权利要求1所述的用于纺织品的阻燃抑烟溶胶的制备方法，其特征在于，所述步骤1)铝盐和聚磷酸铵的质量比为1:1-10。
4.根据权利要求1所述的用于纺织品的阻燃抑烟溶胶的制备方法，其特征在于，所述步骤1)稀酸溶液的质量分数为5-15％，所述稀酸溶液为冰醋酸、硫酸、硝酸或盐酸溶液；所述稀酸溶液与铝盐的质量比为1:50-100。
5.根据权利要求1所述的用于纺织品的阻燃抑烟溶胶的制备方法，其特征在于，所述步骤2)聚苯乙烯磺酸钠水溶液中聚苯乙烯磺酸钠与水的质量比为1:50-100。
6.根据权利要求1所述的用于纺织品的阻燃抑烟溶胶的制备方法，其特征在于，所述步骤2)聚苯乙烯磺酸钠与蒙脱土的质量比为1:50-100。
7.根据权利要求1所述的用于纺织品的阻燃抑烟溶胶的制备方法，其特征在于，所述步骤3)中步骤1)产物与步骤2)产物的质量比为1:1-10。
8.根据权利要求1所述的用于纺织品的阻燃抑烟溶胶的制备方法，其特征在于，所述步骤3)中正硅酸乙酯与步骤1)产物和步骤2)产物的总质量之比为1:1-10。
9.一种如权利要求1～8任一所述的制备方法制备得到的用于纺织品的阻燃抑烟溶胶。
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