CN105862392A - 一种阻燃涂层胶及其应用 - Google Patents
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Abstract
本发明涉及一种阻燃涂层胶及其应用,所述阻燃涂层胶的成分包括:疏水化改性聚磷酸铵M‑APP、聚丙烯酸酯乳液、环状磷酸酯PES、季戊四醇PER和增稠剂。所述阻燃涂层胶应用于聚酯高铁内饰纺织品的阻燃:将阻燃涂层胶刮涂在织物的背面,烘焙,即得。本发明攻克了聚酯织物燃烧时阻燃效率低、熔融低落、烟雾密集、产生大量有毒性气体,以及涂层面料吸湿、发粘等技术难题。
Description
技术领域
本发明属于阻燃剂领域,特别涉及一种阻燃涂层胶及其应用。
背景技术
高速列车时代大发展和国产化进程的推进给了高铁广阔的市场前景,因此对环保型、功能性的内饰纺织品的多样化需求更加迫切。高速运行中的旅客列车,由于其内部空间封闭、可燃物相对多而且集中,一旦发生火灾,火势燃烧得非常快,火灾烟气迅速蔓延,并很快充满整个车厢,严重威胁人员生命和行车安全。而燃烧产生的毒烟,大大降低了人的能见度的同时更是造成伤亡的最大威胁。因此,低烟毒高性能阻燃安全高铁内饰纺织品的研发显得极其迫切和有必要。
高铁内饰纺织品主要为涤纶纤维等合成纤维。新的阻燃聚酯纤维产品,按生产工艺过程对其阻燃方法进行分类,则可归纳为以下五种:(1)反应型阻燃剂在酯交换或缩聚阶段加入,进行共缩聚;(2)添加型阻燃剂在熔融纺丝前往熔体中加入;(3)含有阻燃成份的聚酯与普通聚酯进行复合纺丝;(4)反应型阻燃剂与聚酯纤维或织物进行接枝共聚;(5)对聚酯纤维织物进行阻燃后整理。第(1)至(3)三种方法属于原丝的阻燃改性,工艺复杂、成本高;第(4)和(5)两种方法属于表面整理改性,其中后整理处理的优势在于成本低,操作方便。纺织品阻燃后整理法可具体分为:①浸轧—焙烘法,该方法适用普遍,是阻燃整理方法中应用最多的一种,但是用浸轧法整理有花纹、簇绒、绒头起毛等膨松性表面风格的织物会使表面绒毛、花纹受到损伤;②喷雾法,一些厚幕布和大型地毯商品都可在最后一道工序中做喷雾法的阻燃整理;③涂层—焙烘法,该法适用于需要保持织物绒面的风格的情况。
选择阻燃剂必须依据被阻燃材料的燃烧特性,即被阻燃材料的燃烧降解过程(分解、引发和燃烧)。选择阻燃剂时,必须考虑到以下两点:燃烧过程的阶段和阻燃功效的相态(气相或凝聚相)关系,明确燃烧过程的阶段(分解、引发或者燃烧),以及阻燃剂的相态在相应燃烧阶段所起的作用,即发挥气相阻燃机理,还是凝聚相阻燃机理,或者是几种机理的综合;阻燃剂必须在恰当的时间和恰当的地点发挥作用,即被阻燃物的分解温度与阻燃剂的分解温度匹配,采用混合阻燃剂复配达到最佳阻燃效果,一种阻燃剂在略低于被阻燃基材的分解温度时发挥阻燃作用,另一种则在基材分解失重50%和达到最大分解速率时发挥阻燃作用。此外,我国正处于一个高速发展和技术转型的过渡期,新型绿色环保阻燃剂已经成为开发的主要方向,阻燃剂结构正向阻燃、抑烟、低毒、环保方向发展。相对于其它类型的阻燃剂,膨胀阻燃剂无疑是目前最佳而且高效的、无卤的、环境友好型的阻燃剂,符合当前绿色环保的要求,且有着阻燃效率高、发烟量小、产生更少有毒性气体的优点。
发明内容
本发明所要解决的技术问题是提供一种阻燃涂层胶及其应用,攻克了聚酯织物燃烧时阻燃效率低、熔融低落、烟雾密集、产生大量有毒性气体等技术难题。
本发明的一种阻燃涂层胶,所述阻燃涂层胶的成分包括:疏水化改性聚磷酸铵M-APP、聚丙烯酸酯乳液、环状磷酸酯PES、季戊四醇PER和增稠剂;其中,PES、M-APP与PER的质量比例为1~40:1~20:1~20,PES、M-APP和PER的质量百分比之和与聚丙烯酸酯乳液的质量百分比的比例为30~70%:70~30%。
所述M-APP的制备方法:将聚磷酸铵APP加到聚硅氧烷溶胶中,搅拌,干燥,凝胶化并除去溶剂,得到疏水化改性聚磷酸铵M-APP。
所述聚硅氧烷溶胶的制备方法:将无水乙醇、甲基三甲氧基硅烷MS、正硅酸四乙酯TEOS以及氨水混合,使反应体系pH值为9~10之间,升温至10~80℃;在搅拌条件下滴加水,时间1~5h,水滴完后继续搅1~5h,得到聚硅氧烷溶胶;其中,TEOS与MS的摩尔比为1:2~1:6。
所述聚硅氧烷溶胶的质量为APP质量的1~50%。
所述增稠剂为ASE-60,用量为阻燃涂层胶总质量的2%。
所述阻燃涂层胶应用于聚酯高铁内饰纺织品的低烟毒高效率阻燃方法,包括:
(1)将聚磷酸铵APP加入到聚硅氧烷溶胶中,高速搅拌至完全均匀分散,放入恒温干燥箱干燥,凝胶化并除去溶剂,得到疏水化改性聚磷酸铵M-APP;硅烷水解形成的聚硅氧烷溶胶在表面能较高的聚磷酸铵(APP)表面吸附生长,羟基化的一面吸附在聚磷酸铵表面,甲基疏水面则向外排列,逐步缩聚形成疏水表面;
(2)将步骤(1)中得到的M-APP、聚丙烯酸酯乳液、环状磷酸酯PES、季戊四醇PER和增稠剂混合,研磨,得到阻燃涂层胶;其中,PES、M-APP与PER的质量比例为1~40:1~20:1~20,PES、M-APP和PER的质量百分比之和与聚丙烯酸酯乳液的质量百分比的比为30~70%:70~30%;
(3)将步骤(2)中得到的阻燃涂层胶刮涂在织物的背面,烘焙,得到低烟毒高效率阻燃的聚酯高铁内饰纺织品。
所述步骤(1)中聚硅氧烷溶胶的制备方法:在装有搅拌棒、温度计、冷凝管、针筒的500mL四口烧瓶中先后加入10~100mL无水乙醇、一定质量的甲基三甲氧基硅烷(MS)、正硅酸四乙酯(TEOS)以及一定量的氨水,使反应体系pH值为9~10之间,升温至10~80℃;再在搅拌条件下逐渐滴入一定量的水,时间1~5h,水滴完后继续搅1~5h,制得稳定均一透明的聚硅氧烷溶胶;其中,TEOS与MS的摩尔比为1:2~1:6。
改变TEOS与MS的摩尔比,添加混合液的质量为APP质量的10~50%,进行润湿性实验测定改性后聚磷酸铵粉末的接触角,确定最合适TEOS与MS摩尔比。
所述步骤(1)中聚硅氧烷溶胶的质量为APP质量的1~50%。
所述步骤(3)中织物为聚酯提花绒织物。
所述步骤(3)中涂覆量为100~400g/m2。
所述步骤(3)中烘焙的条件为:焙烘温度为100~200℃,焙烘时间为1~10min。
所述步骤(3)中阻燃涂层胶中加入氢氧化铝,氢氧化铝的加入量为阻燃涂层胶质量的1~20%。
复配合适的无机协效剂对膨胀型阻燃涂层产生阻燃增效作用:兼顾阻燃剂的不同特点与性能,将有机无机阻燃剂协同增效使用,优化选择阻燃剂的种类,提高阻燃效果,同时降低有机磷用量,改善吸湿返霜的问题;选择不同无机协效剂对涤纶织物阻燃测试,对比复配效果,确定最高效无机协效剂为氢氧化铝,进而探讨其用量对阻燃效果影响,确定1~20%(相对涂层胶质量)的氢氧化铝用量可使整理织物阻燃效果达到最佳,无融滴现象,且手感干爽。
所述步骤(1)得到疏水化改性聚磷酸铵M-APP之前的预备工作:
A.膨胀阻燃体系组分、比例及用量的确定:
(i)按照一定的配比和顺序将膨胀阻燃体系组分、水性聚聚丙烯酸酯加入到调和容器中,聚丙烯酸酯乳液30~70%,膨胀阻燃剂30~70%,保证膨胀阻燃剂总量为10~70g,高速研磨分散均匀,制得阻燃涂层胶。
(ii)用瑞士MathisBA涂层机将阻燃胶均匀地涂敷在织物的背面,涂覆量为100~400g/m2,用烘箱焙烘,焙烘温度100~200℃,焙烘时间1~10min。然后用YG815A型垂直法织物燃烧性能测试仪,将300×80(mm)试样置于规定的燃烧器下点燃,稳定火苗30s,在规定点燃时间12s后,测量试样的续燃时间、阴燃时间、损毁长度等。
(iii)对环状磷酸酯(PES)、聚磷酸铵(APP)、季戊四醇(PER)三组分用量正交试验分析,涂覆量为100~400g/m2,焙烘温度为100~200℃,焙烘时间为1~10min,改变PES、APP、PER的用量,测试阻燃性能,根据续燃时间和损毁长度综合考虑确定PES、APP、PER三者最佳的比例为1~40:1~20:1~20。
(iv)按照确定阻燃体系组分的最佳比例,改变阻燃胶在整理中的涂覆量,测试其阻燃性能,考虑阻燃效果及成本两方面,确定总涂覆量为100~400g/m2,阻燃效果最佳。
B.疏水改性聚磷酸铵(APP)改善涂层的吸湿发粘问题:
膨胀型阻燃剂阻燃效率低、耐水性差,导致其涂层体系应用时存在添加量大,吸湿返霜、发粘的问题。将正硅酸四乙酯(TEOS)和甲基三甲氧基硅烷(MS)水解缩合生成聚硅氧烷,利用聚硅氧烷对聚磷酸铵(APP)进行疏水化改性。
本发明的高铁内饰纺织品为聚酯提花绒织物,后整理为从涂层—焙烘整理的方法对其进行阻燃研究。
C.测试方法:
(i)织物阻燃性测试按照《GBT 5454-1997纺织品燃烧性能试验氧指数法》和《GBT 5455-2014纺织品燃烧性能垂直方向损毁长度阴燃和续燃时间的测定》的规定进行。
(ii)阻燃涂膜吸水率按照《FZT 10019-2011纺织上浆用聚丙烯酸类浆料试验方法浆膜吸水率测定》的规定进行。
(iii)涂层整织物的粘连性按照《FZT 01063-2008涂层织物抗粘连性的测定》的规定进行。
有益效果
本发明研究高铁内饰纺织品的阻燃体系、疏水化改性、无机有机阻燃剂协同增效等技术,攻克了聚酯织物燃烧时阻燃效率低、熔融低落、烟雾密集、产生大量有毒性气体等技术以及涂层织物吸湿、发粘等问题。
附图说明
图1为膨胀系阻燃体系阻燃原理示意图;
图2为本明主要内容示意图。
具体实施方式
下面结合具体实施例,进一步阐述本发明。应理解,这些实施例仅用于说明本发明而不用于限制本发明的范围。此外应理解,在阅读了本发明讲授的内容之后,本领域技术人员可以对本发明作各种改动或修改,这些等价形式同样落于本申请所附权利要求书所限定的范围。
实施例1
(1)疏水改性聚磷酸铵(APP)
(i)聚硅氧烷改性溶胶的制备
在装有搅拌棒、温度计、冷凝管、针筒的500mL四口烧瓶中先后加入30mL无水乙醇、5g甲基三甲氧基硅烷(MS)、10g正硅酸四乙酯(TEOS),用氨水调节使反应体系pH值为9~10之间,升温至80℃;再在搅拌条件下逐渐滴入50ml的水,所需时间1h,水滴完后继续搅1h,制得稳定均一透明的聚硅氧烷溶胶。
(ii)聚磷酸铵(APP)的疏水化改性
按聚硅氧烷改性溶胶与聚磷酸铵(APP)的质量比为4:100的量添加在调和容器中,高速搅拌至完全均匀分散。将此混合物放入100℃恒温干燥箱干燥,凝胶并除去溶剂,得到疏水化改性聚磷酸铵(M-APP)。
(2)将环状磷酸酯(PES)、疏水化改性聚磷酸铵(M-APP),季戊四醇(PER)按照30:10:3的质量配比,总用量为50%,和成膜物丙烯酸酯混合乳(BLJ-733D:BLJ-716=3:2)总用量为50%,加入到调和容器中,高速研磨分散均匀,制得阻燃涂层胶。
(3)将相对涂层胶质量15%的无机协效剂氢氧化铝加入涂层胶中,高速研磨分散均匀。
(4)将步骤(3)中得到的阻燃涂层胶刮涂在织物的背面,烘焙(160℃,120s),得到低烟毒高效率阻燃的聚酯高铁内饰纺织品织物。
(iii)性能测试结果:
试样置于规定的燃烧器下点燃,稳定火苗30s,在规定点燃时间12s后,测量试样的阻燃性能为:续燃时间3.2s、阴燃时间0s、损毁长度4cm。
胶膜吸水率测试表明:疏水化改性后聚磷酸铵的阻燃胶膜的吸水率下降55.6%,可见疏水化改性后涂层胶的吸水率大大降低。
涂层面料连性测试表明:涂层座椅面料放置一段时间后,基本无粘连现象。
综上可见:疏水化改性后的阻燃性能没有下降,耐水性有较大提高,其阻燃涂层吸湿发粘缺陷得到明显改善。
实施例2
(1)疏水改性聚磷酸铵(APP)
(i)聚硅氧烷改性溶胶的制备
在装有搅拌棒、温度计、冷凝管、针筒的500mL四口烧瓶中先后加入60mL无水乙醇、5g甲基三甲氧基硅烷(MS)、12g正硅酸四乙酯(TEOS),用氨水调节使反应体系pH值为9~10之间,升温至70℃;再在搅拌条件下逐渐滴入60ml的水,所需时间1h,水滴完后继续搅1h,制得稳定均一透明的聚硅氧烷溶胶。
(ii)聚磷酸铵(APP)的疏水化改性
按聚硅氧烷改性凝胶与聚磷酸铵(APP)的质量比为6:100的量添加在调和容器中,高速搅拌至完全均匀分散。将此混合物放入80℃恒温干燥箱干燥,凝胶并除去溶剂,得到疏水化改性聚磷酸铵(M-APP)。
(2)将环状磷酸酯(PES)、疏水化改性聚磷酸铵(M-APP),季戊四醇(PER)按照25:10:3的质量配比,总用量为60%,和成膜物丙烯酸酯混合乳(BLJ-733D:BLJ-716=3:2)总用量为40%,加入到调和容器中,高速研磨分散均匀,制得阻燃涂层胶。
(3)将相对涂层胶质量10%的无机协效剂氢氧化铝加入涂层胶中,高速研磨分散均匀。
(4)将步骤(3)中得到的阻燃涂层胶刮涂在织物的背面,烘焙(130℃,120s),得到低烟毒高效率阻燃的聚酯高铁内饰纺织品织物。
(5)(iii)性能测试结果:试样置于规定的燃烧器下点燃,稳定火苗30s,在规定点燃时间12s后,测量试样的阻燃性能为:续燃时间3s、阴燃时间0、损毁长度3.7cm。
胶膜吸水率测试表明:疏水化改性后聚磷酸铵的阻燃胶膜的吸水率下降58.1%,可见疏水化改性后涂层胶的吸水率大大降低。
涂层面料连性测试表明:涂层座椅面料放置一段时间后,基本无粘连现象。
综上可见:疏水化改性后的阻燃性能没有下降,耐水性有较大提高,其阻燃涂层吸湿发粘缺陷得到明显改善。
实施例3
(1)疏水改性聚磷酸铵(APP)
(i)聚硅氧烷改性溶胶的制备
在装有搅拌棒、温度计、冷凝管、针筒的500mL四口烧瓶中先后加入80mL无水乙醇、8g甲基三甲氧基硅烷(MS)、5g正硅酸四乙酯(TEOS),用氨水调节反应体系pH值为9~10之间,升温至70℃;再在搅拌条件下逐渐滴入50ml的水,所需时间1h,水滴完后继续搅1h,制得稳定均一透明的聚硅氧烷溶胶。
(ii)聚磷酸铵(APP)的疏水化改性
按聚硅氧烷改性凝胶与聚磷酸铵(APP)的质量比为8:100的量添加在调和容器中,高速搅拌至完全均匀分散。将此混合物放入90℃恒温干燥箱干燥,凝胶并除去溶剂,得到疏水化改性聚磷酸铵(M-APP)。
(2)将环状磷酸酯(PES)、疏水化改性聚磷酸铵(M-APP),季戊四醇(PER)按照25:12:3的质量配比,总用量为50%,和成膜物丙烯酸酯混合乳(BLJ-733D:BLJ-716=3:2)总用量为50%,加入到调和容器中,高速研磨分散均匀,制得阻燃涂层胶。
(3)将相对涂层胶质量10%的无机协效剂氢氧化铝加入涂层胶中,高速研磨分散均匀。
(4)将步骤(3)中得到的阻燃涂层胶刮涂在织物的背面,烘焙(150℃,120s),得到低烟毒高效率阻燃的聚酯高铁内饰纺织品织物。
(iii)性能测试结果:
试样置于规定的燃烧器下点燃,稳定火苗30s,在规定点燃时间12s后,测量试样的阻燃性能为:续燃时间3.3s、阴燃时间0s、损毁长度3.5cm。
胶膜吸水率测试表明:疏水化改性后聚磷酸铵的阻燃胶膜的吸水率下降57.3%,可见疏水化改性后涂层胶的吸水率大大降低。
涂层面料连性测试表明:涂层座椅面料放置一段时间后,基本无粘连现象。
综上可见:疏水化改性后的阻燃性能没有下降,耐水性有较大提高,其阻燃涂层吸湿发粘缺陷得到明显改善。
实施例4
(1)疏水改性聚磷酸铵(APP)
(i)聚硅氧烷改性溶胶的制备
在装有搅拌棒、温度计、冷凝管、针筒的500mL四口烧瓶中先后加入60mL无水乙醇、10g甲基三甲氧基硅烷(MS)、5g正硅酸四乙酯(TEOS),用氨水调节反应体系pH值为9~10之间,升温至70℃;再在搅拌条件下逐渐滴入50ml的水,所需时间1h,水滴完后继续搅1h,制得稳定均一透明的聚硅氧烷溶胶。
(ii)聚磷酸铵(APP)的疏水化改性
按聚硅氧烷改性凝胶与聚磷酸铵(APP)的质量比为7:100的量添加在调和容器中,高速搅拌至完全均匀分散。将此混合物放入85℃恒温干燥箱干燥,凝胶并除去溶剂,得到疏水化改性聚磷酸铵(M-APP)。
(2)将环状磷酸酯(PES)、疏水化改性聚磷酸铵(M-APP),季戊四醇(PER)按照30:10:7的质量配比,总用量为70%,和成膜物丙烯酸酯混合乳(BLJ-733D:BLJ-716=2:1)总用量为30%,加入到调和容器中,高速研磨分散均匀,制得阻燃涂层胶。
(3)将相对涂层胶质量8%的无机协效剂氢氧化铝加入涂层胶中,高速研磨分散均匀。
(4)将步骤(3)中得到的阻燃涂层胶刮涂在织物的背面,烘焙(150℃,180s),得到低烟毒高效率阻燃的聚酯高铁内饰纺织品织物。
(iii)性能测试结果:
试样置于规定的燃烧器下点燃,稳定火苗30s,在规定点燃时间12s后,测量试样的续燃时间2.9s、阴燃时间0s、损毁长度3.3cm。
胶膜吸水率测试表明:疏水化改性后聚磷酸铵的阻燃胶膜的吸水率下降60.2%,可见疏水化改性后涂层胶的吸水率大大降低。
涂层面料连性测试表明:涂层座椅面料放置一段时间后,基本无粘连现象。
综上可见:疏水化改性后的阻燃性能没有下降,耐水性有较大提高,其阻燃涂层吸湿发粘缺陷得到明显改善。
Claims (10)
1.一种阻燃涂层胶,其特征在于,所述阻燃涂层胶的成分包括:疏水化改性聚磷酸铵M-APP、聚丙烯酸酯乳液、环状磷酸酯PES、季戊四醇PER和增稠剂;其中,PES、M-APP与PER的质量比例为1~40:1~20:1~20,PES、M-APP和PER的质量百分比之和与聚丙烯酸酯乳液的质量百分比的比例为30~70%:70~30%。
2.根据权利要求1所述的一种阻燃涂层胶,其特征在于,所述M-APP的制备方法:将聚磷酸铵APP加到聚硅氧烷溶胶中,搅拌,干燥,凝胶化并除去溶剂,得到疏水化改性聚磷酸铵M-APP。
3.根据权利要求2所述的一种阻燃涂层胶,其特征在于,所述聚硅氧烷溶胶的制备方法:将无水乙醇、甲基三甲氧基硅烷MS、正硅酸四乙酯TEOS以及氨水混合,使反应体系pH值为9~10之间,升温至10~80℃;在搅拌条件下滴加水,时间1~5h,水滴完后继续搅1~5h,得到聚硅氧烷溶胶;其中,TEOS与MS的摩尔比为1:2~1:6。
4.根据权利要求2所述的一种阻燃涂层胶,其特征在于,所述聚硅氧烷溶胶的质量为APP质量的1~50%。
5.根据权利要求1所述的一种阻燃涂层胶,其特征在于,所述增稠剂为ASE-60,用量为阻燃涂层胶总质量的2%。
6.一种如权利要求1所述的阻燃涂层胶的应用,其特征在于,应用于聚酯高铁内饰纺织品的阻燃:将阻燃涂层胶刮涂在织物的背面,烘焙,即得。
7.根据权利要求6所述的一种阻燃涂层胶的应用,其特征在于,所述织物为聚酯提花绒织物;涂覆量为100~400g/m2。
8.根据权利要求6所述的一种阻燃涂层胶的应用,其特征在于,所述烘焙的条件为:焙烘温度为100~200℃,焙烘时间为1~10min。
9.根据权利要求6所述的一种阻燃涂层胶的应用,其特征在于,所述阻燃涂层胶中加入无机协效剂,加入量为阻燃涂层胶质量的1~20%。
10.根据权利要求9所述的一种阻燃涂层胶的应用,其特征在于,所述无机协效剂为氢氧化铝。
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