CN106700496A - 一种防火鞋的阻燃海绵及其制备方法 - Google Patents
一种防火鞋的阻燃海绵及其制备方法 Download PDFInfo
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Abstract
本发明申请提供了一种防火鞋的阻燃海绵，它由以下重量份数的原料制成：乙烯基聚合物接枝聚醚多元醇70～90份、异佛尔酮二异氰酸酯40～45份、双酚A‑双(二苯基磷酸酯)5～10份、活性碳纤维5～10份、碳粉10～30份、皂粉5～10份、滑石粉5～10份、二氧化硅1～5份、发泡剂1～3份、稳泡剂2～4份、氨水30～50份。配方组分相互间发生协同作用，海绵耐火阻燃性能优良，燃烧试验中氧指数达到35～38，燃点可达到1200～1300℃，用于消防鞋内不会发生变质。本发明申请还公开了一种防火鞋的阻燃海绵的制备方法。
Description
【技术领域】
本发明涉及防火鞋领域，具体涉及一种防火鞋的阻燃海绵及其制备方法。
【背景技术】
海绵具有优良的柔性、弹性、透气、保温等性能，在家居工业上有广泛的应用，如用作过滤材料、防震材料、装饰材料、包装材料及隔热保温材料等。然而，海绵遇火极易燃烧，并产生浓烟和有毒气体，危害人体。目前，阻燃海绵普遍采用添加各种阻燃剂来达到阻燃效果，现有的使用较多的是添加有机阻燃剂的海绵，主要添加卤系、磷酸酯、卤代磷酸酯等有机物，此类有机阻燃剂能起到一定的阻燃效果，但此类有机阻燃剂一般含有有害成分。CN103275293A公开了防火海绵及其制备方法，在传统海绵发泡原料中加入阻燃剂制作的阻燃性海绵，遇火不会燃烧，而是受热融化，可减少火灾隐患。但是因其遇火融化，只能一次性使用，融化过程中还可能损害其他部件。CN 105017502A公开了一种环保阻燃海绵及其制备方法，添加少量的可膨胀石墨，遇火时，可膨胀石墨由于高温而急剧膨胀，窒息了火焰，同时其生成的石墨膨体材料覆盖在基材表面，隔绝了热能辐射及氧化作用，其夹层内部的酸根在膨胀时释放出来，也促进了基材的碳化，从而通过多种阻燃方式达到良好的阻燃效果。但是，该方法阻燃过程会发生大面积膨胀，基材受影响变形，碳化后物质变质，无法继续利用。现有技术缺少用于防火鞋的承受火灾高温不变质的阻燃海绵。
【发明内容】
本发明所要解决的技术问题是，针对以上现有技术的缺点，提供一种防火鞋的阻燃海绵及其制备方法，能够用于防火鞋，承受火灾的高温。
本发明的技术方案是：一种防火鞋的阻燃海绵，它由以下重量份数的原料制成：乙烯基聚合物接枝聚醚多元醇70～90份、异佛尔酮二异氰酸酯40～45份、双酚A-双(二苯基磷酸酯)5～10份、活性碳纤维5～10份、碳粉10～30份、皂粉5～10份、滑石粉5～10份、二氧化硅1～5份、发泡剂1～3份、稳泡剂2～4份、氨水30～50份。
乙烯基聚合物接枝聚醚多元醇，简称POP，常用作制备软质和半硬质聚氨酯泡沫塑料制品；异佛尔酮二异氰酸酯，简称IPDI，用作POP的胶黏剂，双酚A-双(二苯基磷酸酯)，简称BDP，作为无卤阻燃剂，具有低烟、低毒、环保等优点，此处适用POP和IPDI的阻燃。碳粉由树脂和炭黑、电荷剂、磁粉等组成，滑石粉即Mg3[Si4O10](OH)2多用于陶瓷，此处将滑石粉与碳粉混合，通过减少碳粉与空气的接触面积而防止碳粉燃烧变性，增加了碳粉的稳定性，成为了阻燃碳粉。而皂粉多用于清洁去渍，此处配合活性碳纤维对二氧化硅的负载，起到粘接作用，即增强粉末二氧化硅和活性碳纤维的粘结力，而不是吸附后很容易散落；并且皂粉增强了海绵的柔性，放在防火鞋内舒适柔软。碳粉、滑石粉、二氧化硅和皂粉均为固体粉末，填充到具高比表面积的活性碳纤维后，活性碳纤维会提供良好的孔隙环境，起到吸附作用。
优选地，一种防火鞋的阻燃海绵，它由以下重量份数的原料制成：乙烯基聚合物接枝聚醚多元醇75～85份、异佛尔酮二异氰酸酯40～45份、双酚A-双(二苯基磷酸酯)6～8份、活性碳纤维6～8份、碳粉15～25份、皂粉5～8份、滑石粉6～8份、二氧化硅1～5份、发泡剂1～3份、稳泡剂2～4份、氨水35～45份。
具体地，所述发泡剂为苏打粉、三聚氰胺、双氰胺、氯化石蜡、硼酸铵、三聚氰胺-甲醛树脂、氰二酞胺中的一种或几种。
具体地，所述稳泡剂为淀粉或纤维素。稳泡剂配合发泡剂作用，使得海绵的孔径大小可控，孔隙率可控，产品泡孔均匀。
一种防火鞋的阻燃海绵的制备方法，它包括以下步骤：
1)将活性碳纤维浸泡于氨水中5～10h；
2)将步骤1)浸泡后的活性碳纤维与二氧化硅、皂粉搅拌均匀，加压至25～35Mpa，45～50℃加热保持20～30min，得到阻燃活性碳纤维；
3)将碳粉和滑石粉混合，得到阻燃碳粉；
4)将阻燃碳粉与上述配方量的乙烯基聚合物接枝聚醚多元醇、异佛尔酮二异氰酸酯、双酚A-双(二苯基磷酸酯)投入混合器中混合，搅拌均匀，并50～60℃加热反应20～30min，得到初产品；
5)将初产品、阻燃活性碳纤维、发泡剂、稳泡剂投入混合器中混合，高速搅拌5～6min后倒入模具发泡并固化后，得到防火鞋的阻燃海绵。
活性碳纤维浸泡于氨水，有利于对活性碳纤维的表面改性，有助于吸附二氧化硅，增强吸附效果，降低活性碳纤维负载阻燃剂的对高压的要求。碳粉和滑石粉先与POP、IPDI、BDP混合反应，使其相互交联，形成初产品；再添加阻燃活性碳纤维，高速搅拌可进一步增强皂粉和二氧化硅的耐火阻燃性，发泡制得的海绵具有多孔结构，孔间穿插有改性的阻燃活性碳纤维，孔内填充有高效的阻燃碳粉，燃烧试验中氧指数达到35～38，燃点可达到1200～1300℃，可承载火灾全面燃烧时的高温800～1000℃，且用于消防鞋内不会发生化学反应、遇火融化、受热膨胀等变质现象，保持多孔海绵的初始状态。
优选地，所述步骤4)的混合、搅拌在体积分数为80～95％的N2环境中进行。N2氛围是为了保证交联反应的均匀稳定进行，不受外界空气影响，且有助于提升阻燃效果。
优选地，所述步骤5)的混合、搅拌在体积分数为90～98％的CO2环境中进行。CO2有利于海绵发泡成型，且活性碳纤维可吸收CO2于孔洞内，而不宜流失，为使用海绵奠定了基础。阻燃气体二氧化碳将孔洞填满，阻止海绵燃烧。皂粉遇水也会产生泡沫，会将周围的二氧化硅和二氧化碳包裹起来，这样再遇火泡沫破裂，便将囊内的二氧化硅喷出，破裂过程也会影响周围的阻燃碳粉的移动，海绵的阻燃效果显著增强。
本发明具有以下有益的技术效果：
1)配方组分相互间发生协同作用，海绵耐火阻燃性能优良，燃烧试验中氧指数达到35～38，燃点可达到1200～1300℃，用于消防鞋内不会发生变质；
2)废弃的产品可在强酸条件下降解，不会对环境造成污染；
3)制备方法简单方便，生产效率高，产品生产周期短；所采用原料成本低，易得，易合成；降低生产能耗，减少生产排放；
4)稳泡剂配合发泡剂作用，使得海绵的孔径大小可控，孔隙率可控，产品泡孔均匀；
5)皂粉配合活性碳纤维，粘接二氧化硅，遇水包裹二氧化硅和CO2，显著增强海绵的阻燃效果。
【具体实施方式】
以下结合具体实施例，对本发明做进一步描述。
以下所提供的实施例并非用以限制本发明所涵盖的范围，所描述的步骤也不是用以限制其执行顺序。本领域技术人员结合现有公知常识对本发明做显而易见的改进，亦落入本发明要求的保护范围之内。
实施例一
一种防火鞋的阻燃海绵，它由以下重量份数的原料制成：乙烯基聚合物接枝聚醚多元醇70份、异佛尔酮二异氰酸酯40份、碳粉10份、双酚A-双(二苯基磷酸酯)5份、活性碳纤维5份、滑石粉5份、二氧化硅1份、皂粉5份、苏打粉1份、淀粉2份、氨水30份。
一种防火鞋的阻燃海绵的制备方法，它包括以下步骤：
1)将活性碳纤维浸泡于氨水中5h；
2)将步骤1)浸泡后的活性碳纤维与二氧化硅、皂粉搅拌均匀，加压至25Mpa，45℃加热保持30min，得到阻燃活性碳纤维；
3)将碳粉和滑石粉混合，得到阻燃碳粉；
4)将阻燃碳粉与上述配方量的乙烯基聚合物接枝聚醚多元醇、异佛尔酮二异氰酸酯、双酚A-双(二苯基磷酸酯)投入含体积分数为80％N2混合器中混合，搅拌均匀，并50℃加热反应30min，得到初产品；
5)将初产品、阻燃活性碳纤维、发泡剂、稳泡剂投入含体积分数为90％CO2的混合器中混合，高速搅拌5min后倒入模具发泡并固化后，得到防火鞋的阻燃海绵。
实施例二
一种防火鞋的阻燃海绵，它由以下重量份数的原料制成：乙烯基聚合物接枝聚醚多元醇90份、异佛尔酮二异氰酸酯45份、碳粉30份、双酚A-双(二苯基磷酸酯)10份、活性碳纤维10份、滑石粉10份、二氧化硅5份、皂粉10份、三聚氰胺3份、淀粉4份、氨水50份。
一种防火鞋的阻燃海绵的制备方法，它包括以下步骤：
1)将活性碳纤维浸泡于氨水中10h；
2)将步骤1)浸泡后的活性碳纤维与二氧化硅、皂粉搅拌均匀，加压至35Mpa，50℃加热保持20min，得到阻燃活性碳纤维；
3)将碳粉和滑石粉混合，得到阻燃碳粉；
4)将阻燃碳粉与上述配方量的乙烯基聚合物接枝聚醚多元醇、异佛尔酮二异氰酸酯、双酚A-双(二苯基磷酸酯)投入含体积分数为95％N2混合器中混合，搅拌均匀，并60℃加热反应20min，得到初产品；
5)将初产品、阻燃活性碳纤维、发泡剂、稳泡剂投入含体积分数为98％CO2的混合器中混合，高速搅拌6min后倒入模具发泡并固化后，得到防火鞋的阻燃海绵。
实施例三
一种防火鞋的阻燃海绵，它由以下重量份数的原料制成：乙烯基聚合物接枝聚醚多元醇75份、异佛尔酮二异氰酸酯40份、碳粉15份、双酚A-双(二苯基磷酸酯)6份、活性碳纤维6份、滑石粉6份、二氧化硅1份、皂粉7份、双氰胺1份、淀粉2份、氨水35份。
一种防火鞋的阻燃海绵的制备方法，它包括以下步骤：
1)将活性碳纤维浸泡于氨水中8h；
2)将步骤1)浸泡后的活性碳纤维与二氧化硅、皂粉搅拌均匀，加压至30Mpa，48℃加热保持25min，得到阻燃活性碳纤维；
3)将碳粉和滑石粉混合，得到阻燃碳粉；
4)将阻燃碳粉与上述配方量的乙烯基聚合物接枝聚醚多元醇、异佛尔酮二异氰酸酯、双酚A-双(二苯基磷酸酯)投入含体积分数为88％N2混合器中混合，搅拌均匀，并55℃加热反应25min，得到初产品；
5)将初产品、阻燃活性碳纤维、发泡剂、稳泡剂投入含体积分数为95％CO2的混合器中混合，高速搅拌5min后倒入模具发泡并固化后，得到防火鞋的阻燃海绵。
实施例四
一种防火鞋的阻燃海绵，它由以下重量份数的原料制成：乙烯基聚合物接枝聚醚多元醇85份、异佛尔酮二异氰酸酯45份、碳粉25份、双酚A-双(二苯基磷酸酯)8份、活性碳纤维8份、滑石粉8份、二氧化硅5份、皂粉5份、氯化石蜡3份、纤维素4份、氨水45份。
一种防火鞋的阻燃海绵的制备方法，它包括以下步骤：
1)将活性碳纤维浸泡于氨水中9h；
2)将步骤1)浸泡后的活性碳纤维与二氧化硅、皂粉搅拌均匀，加压至30Mpa，48℃加热保持23min，得到阻燃活性碳纤维；
3)将碳粉和滑石粉混合，得到阻燃碳粉；
4)将阻燃碳粉与上述配方量的乙烯基聚合物接枝聚醚多元醇、异佛尔酮二异氰酸酯、双酚A-双(二苯基磷酸酯)投入含体积分数为90％N2混合器中混合，搅拌均匀，并58℃加热反应23min，得到初产品；
5)将初产品、阻燃活性碳纤维、发泡剂、稳泡剂投入含体积分数为96％CO2的混合器中混合，高速搅拌5min后倒入模具发泡并固化后，得到防火鞋的阻燃海绵。
实施例五
一种防火鞋的阻燃海绵，它由以下重量份数的原料制成：乙烯基聚合物接枝聚醚多元醇80份、异佛尔酮二异氰酸酯42份、碳粉20份、双酚A-双(二苯基磷酸酯)7份、活性碳纤维7份、滑石粉7份、二氧化硅3份、皂粉8份、硼酸铵2份、纤维素3份、氨水40份。
一种防火鞋的阻燃海绵的制备方法，它包括以下步骤：
1)将活性碳纤维浸泡于氨水中8h；
2)将步骤1)浸泡后的活性碳纤维与二氧化硅、皂粉搅拌均匀，加压至30Mpa，48℃加热保持25min，得到阻燃活性碳纤维；
3)将碳粉和滑石粉混合，得到阻燃碳粉；
4)将阻燃碳粉与上述配方量的乙烯基聚合物接枝聚醚多元醇、异佛尔酮二异氰酸酯、双酚A-双(二苯基磷酸酯)投入含体积分数为90％N2混合器中混合，搅拌均匀，并55℃加热反应25min，得到初产品；
5)将初产品、阻燃活性碳纤维、发泡剂、稳泡剂投入含体积分数为95％CO2的混合器中混合，高速搅拌5min后倒入模具发泡并固化后，得到防火鞋的阻燃海绵。
产品测试
测试产品密度30～35kg/m3，回弹性30～35％。
将实施例1～5制得的海绵材料置于氧氮混合气体，测试其维持稳定燃烧所需的最低氧浓度，以氧在混合气体中所占的百分数表示。
测试实施例1～5制得的海绵开始并继续燃烧的最低温度。
| 实施例1 | 实施例2 | 实施例3 | 实施例4 | 实施例5 | |
| 氧指数/％ | 35 | 38 | 35.6 | 37 | 36.5 |
| 燃点/℃ | 1210 | 1300 | 1240 | 1290 | 1270 |
通过测试结果发现，采用本发明申请的配方制得的阻燃海绵，氧指数、燃点均达到火灾的高温标准，即将该海绵用于防火鞋，可有效起到防火作用。并且，活性碳纤维对产品的影响较大，对海绵的阻燃效果发挥了重要作用。
遇水测试
将实施例1～5制得的海绵材料喷洒10～20ml水，测试其氧指数和燃点。
| 实施例1 | 实施例2 | 实施例3 | 实施例4 | 实施例5 | |
| 氧指数/％ | 37 | 42 | 37.9 | 39.2 | 38.3 |
| 燃点/℃ | 1240 | 1320 | 1270 | 1300 | 1280 |
比较发现，添加适量的皂粉，海绵遇水后阻燃效果更佳，氧指数和燃点都有提高。
可观察到海绵内有白色粉末喷出，粘附于海绵外表面，进而降低海绵的燃点。
对比例
参照实施例5，配方中改变活性碳纤维的用量，其余相同，进行对比例1～6的产品测试。
通过测试结果发现，与对比例1～6相比，采用本发明申请的实施例5配方及其制备方法制得的海绵阻燃效果最佳。但是，若增加或减少活性碳纤维的用量，都会显著降低海绵的阻燃性能，且影响较大。
Claims (7)
1.一种防火鞋的阻燃海绵，其特征在于，它由以下重量份数的原料制成：乙烯基聚合物接枝聚醚多元醇70～90份、异佛尔酮二异氰酸酯40～45份、双酚A-双(二苯基磷酸酯)5～10份、活性碳纤维5～10份、碳粉10～30份、皂粉5～10份、滑石粉5～10份、二氧化硅1～5份、发泡剂1～3份、稳泡剂2～4份、氨水30～50份。
2.根据权利要求1所述的防火鞋的阻燃海绵，其特征在于，它由以下重量份数的原料制成：乙烯基聚合物接枝聚醚多元醇75～85份、异佛尔酮二异氰酸酯40～45份、双酚A-双(二苯基磷酸酯)6～8份、活性碳纤维6～8份、碳粉15～25份、皂粉5～8份、滑石粉6～8份、二氧化硅1～5份、发泡剂1～3份、稳泡剂2～4份、氨水35～45份。
3.根据权利要求1所述的防火鞋的阻燃海绵，其特征在于，所述发泡剂为苏打粉、三聚氰胺、双氰胺、氯化石蜡、硼酸铵、三聚氰胺-甲醛树脂、氰二酞胺中的一种或几种。
4.根据权利要求1所述的防火鞋的阻燃海绵，其特征在于，所述稳泡剂为淀粉或纤维素。
5.一种根据权利要求1所述的防火鞋的阻燃海绵的制备方法，其特征在于，它包括以下步骤：
1)将活性碳纤维浸泡于氨水中5～10h；
2)将步骤1)浸泡后的活性碳纤维与二氧化硅、皂粉搅拌均匀，加压至25～35Mpa，45～50℃加热保持20～30min，得到阻燃活性碳纤维；
3)将碳粉和滑石粉混合，得到阻燃碳粉；
4)将阻燃碳粉与上述配方量的乙烯基聚合物接枝聚醚多元醇、异佛尔酮二异氰酸酯、双酚A-双(二苯基磷酸酯)投入混合器中混合，搅拌均匀，并50～60℃加热反应20～30min，得到初产品；
5)将初产品、阻燃活性碳纤维、发泡剂、稳泡剂投入混合器中混合，高速搅拌5～6min后倒入模具发泡并固化后，得到防火鞋的阻燃海绵。
6.根据权利要求5所述的防火鞋的阻燃海绵的制备方法，其特征在于，所述步骤4)的混合、搅拌在体积分数为80～95％的N2环境中进行。
7.根据权利要求5所述的防火鞋的阻燃海绵的制备方法，其特征在于，所述步骤5)的混合、搅拌在体积分数为90～98％的CO2环境中进行。
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