CN115558176B - 一种高填充防火橡塑发泡保温材料及制备方法 - Google Patents
一种高填充防火橡塑发泡保温材料及制备方法 Download PDFInfo
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Abstract
本发明涉及保温材料技术领域，具体为一种高填充防火橡塑发泡保温材料，包括如下重量份的原料：丁腈橡胶10‑20份、PVC糊树脂3‑5份、复合催化剂3‑6份、复合碳基阻燃材料1‑4份、复合增粘材料1‑3份、磷酸酯10‑20份、氢氧化铝40‑50份、发泡剂6‑8份、硫磺0.1‑0.5份、硫化发泡助剂0.5‑2份、润滑剂1‑2份、防老剂1‑2份。本发明制备的橡塑发泡材料遇火时能够快速形成热稳定的碳化结构，燃烧性能达到不燃A级水平，同时具有低导热系数和较好的防火性能；能够同时满足石油化工、建筑、船舶等领域轻量化、防火和绝热保温的应用。
Description
技术领域
本发明涉及橡塑保温材料技术领域，具体为一种高填充防火橡塑发泡保温材料及制备方法。
背景技术
橡塑保温材料作为柔性闭孔弹性体材料，具有密度低、湿阻因子高、绝热性能好以及物理力学性能优良等特点，应用领域十分广泛。在建筑、石油化工、船舶、电器等各个领域的使用能够大大降低介质的冷损和热损失量，是具有高性能和高品质特点的新型保温材料。目前市场上的橡塑保温产品能够达到难燃B1级，但相比较于其它不燃A级保温材料，橡塑保温材料仍存在防火性级别还相对较低的缺点。
因此，在石油化工、液化气以及各类易燃易爆和火灾危险性较大的环境下，为了提高管道和设施的防火耐火性能和火灾安全性，橡塑发泡保温材料需要做进一步的技术升级，使其达到不燃A级水平；同时，还要兼顾制品的保温性能和管道主体结构的轻量化要求等。为了解决现有技术存在的问题，本发明提供的一种高填充防火橡塑发泡保温材料及制备方法，能够保证制品具有优异的防火性能和保温性能等，并且能够实现较好的加工性能。
发明内容
本发明的目的在于提供一种高填充防火橡塑发泡保温材料及制备方法，通过对制品的配方结构进行创新设计和工艺改进，使得橡塑发泡材料达到A级不燃水平，同时兼具了发泡材料的绝热保温性能，提升了产品性能和品质。
为实现上述目的，本发明提供如下技术方案：
一种高填充防火橡塑发泡保温材料，包括如下重量份的原料：丁腈橡胶10-20份、PVC糊树脂3-5份、复合催化剂3-6份、复合碳基阻燃材料1-4份、复合增粘材料1-3份、磷酸酯10-20份、氢氧化铝40-50份、发泡剂6-8份、硫磺0.1-0.5份、硫化发泡助剂0.5-2份、润滑剂1-2份、防老剂1-2份。
所述复合催化剂选自铁系化合物、钼系化合物、镍系化合物或稀土金属氧化物等至少其中一种原料组成。
优选复合催化剂由铁系化合物和钼系化合物组成。
进一步地，铁系化合物选自氧化铁、二茂铁等；钼系化合物选自二硫化钼、三氧化钼等；镍系化合物选自三氧化二镍、铝酸镍等；和/或稀土金属氧化物选自氧化镧等。
所述复合碳基阻燃材料由碳纳米管、碳纳米纤维、可膨胀石墨三种组分组成。
进一步地，碳纳米管∶碳纳米纤维∶可膨胀石墨三者重量用量比例为1∶1-2∶1-4。
所述复合增粘材料由树脂类、硅烷类组成。
进一步地，树脂类增粘材料优选烷基酚醛树脂，硅烷类增粘材料优选硅烷偶联剂。
进一步地，树脂类、硅烷类重量用量比例通常为1-4∶1。
所述磷酸酯选自磷酸三乙酯(TEP)、磷酸三甲苯酯(TCP)、以及磷酸三(2-氯丙基)酯(TCPP)至少其中一种。
所述发泡剂优选发泡剂AC。
所述硫化发泡助剂通常由多功能橡胶助剂N,N’-间苯撑双马来酰亚胺(PDM)和硬脂酸锌组成。
进一步地，N,N’-间苯撑双马来酰亚胺(PDM)和硬脂酸锌重量用量比例优选为1-2∶1。
所述润滑剂由硬脂酸和聚乙烯蜡组成。
进一步地，硬脂酸和聚乙烯蜡重量用量比优选为1∶1-2。
所述防老剂由喹啉类和对苯二胺类组成。
进一步地，喹啉类防老剂优选防老剂RD，对苯二胺类防老剂优选4010。
进一步地，喹啉类和对苯二胺类重量用量比例优选为1-2∶1。
本发明还提供一种高填充防火橡塑发泡保温材料的制备方法，具体包括如下步骤：
(1)原料预分散
将按比例称取的复合碳基阻燃材料、复合增粘材料、磷酸酯、氢氧化铝、发泡剂、润滑剂、防老剂投入到高速混合机中进行混合，采用间歇式混合工艺，使各类原材料进行预分散处理。
(2)混炼胶料制备
(a)首先将丁腈橡胶和聚氯乙烯糊树脂投入密炼机混炼；
(b)接着将步骤(1)中的预分散混合料投入密炼机一起进行混炼；
(c)将混炼完成的胶料投入开炼机进行开炼，同时加入复合催化剂、硫磺、硫化发泡助剂,开炼结束后出条，凉置备用；
(3)挤出
将步骤(2)冷却后的胶条喂入挤出机，对胶料进行真空排气处理和产品定型，工艺参数根据产品规格进行设置；
(4)硫化发泡
将步骤(3)中经过挤出的胶料，输送到硫化发泡炉进行连续发泡生产，即可得到所述一种高填充防火橡塑发泡保温材料。
所述步骤(1)中间歇式混合时间通常为30-60min。
所述步骤(2)(a)中混炼转子转速通常为15-50r/min，时间通常为0.5-3min。
所述步骤(2)(b)中混炼时间通常为10-15min，温度通常为100℃-130℃。
所述步骤(2)(c)中开炼时间通常为10-15min，开炼温度通常为小于80℃。
与现有技术相比，本发明的有益效果是：
本发明提供的一种高填充防火橡塑发泡保温材料选用了具有成碳效果优异的复合催化剂和复合碳基阻燃材料，利用了丁腈橡胶和聚氯乙烯糊树脂极好的相容性和高填充特点，并结合复合增粘材料，使得复合催化剂、复合碳基阻燃材料和复合增粘材料的含量最高为骨架材料(丁腈橡胶和聚氯乙烯糊树脂)的100％。
本发明制备的材料中多种复合材料之间相互协同和增效，使得发泡材料具有优异的阻燃和成碳效果。具体地，本发明中复合催化剂中过渡金属离子如Fe3+、Mo4+、Ni3+、La3+等作为丁腈橡胶和聚氯乙烯糊树脂热分解的自由基捕捉剂和脱氢反应的催化剂，能够加速交联成碳、降低可燃物的释放。复合碳基阻燃材料的添加提高了制品的热稳定性，并且在其遇火焰燃烧或高温条件时能够迅速膨胀碳化，形成不燃且耐火性能极好的热稳定保护层结构，从而阻止火焰和热量的向内传播。磷酸酯和氢氧化铝遇火焰燃烧和高温能够迅速形成碳层保护。磷酸酯受热分解生成的粘稠状磷酸和聚磷酸在高温条件下生成多聚磷酸；多聚磷酸能催化聚合物成碳，同时粘附在其它材料表面，起到覆盖作用，隔绝热量和助燃气体；结合氢氧化铝阻燃机理，在受到外界持续燃烧条件下，能够生成热稳定极好的氧化铝和碳化产物。
本发明制备的材料中复合催化剂、复合碳基阻燃材料和复合增粘材料，以及磷酸酯和氢氧化铝的协同作用，使得橡塑发泡制品获得了意想不到的阻燃和防火性能。
本发明制备的材料优选的密度范围为50-90kg/m3，这样材料既具有很好的防火性能，又保留了橡塑发泡材料的绝热效果。密度越高，防火性能越好，但绝热保温效果会略有降低。
本发明制备的材料可达到A级不燃水平。根据GB/T 9978《建筑构件耐火试验方法》和GA/T 714-2007《构件用防火保护材料快速升温耐火试验方法》标准可知，发生火灾时需要保证被防护管道/构件在一定时间范围内保持其完整性、隔热性和稳定性。本发明制备的高填充防火橡塑发泡保温材料在1000℃以上火焰持续燃烧15min条件下，仍然能够保证其完整性和隔热效果。并且其具有密度低、柔性好、绝热性能优异以及防火性能佳等优点，将在未来绝热保温防火领域发挥重要作用。
具体实施方式
下面结合实施例，对本发明做进一步的描述，以下仅为本发明的较佳实施例而已，不能以此限定本发明的范围。即凡是依本发明申请专利范围所作的变化与修饰，皆应仍属本发明专利涵盖的范围内。
实施例1
称取以下重量份的原料：丁腈橡胶16份、PVC糊树脂4份、复合催化剂4份(由氧化铁和三氧化钼按照1∶1比例组成)、复合碳基阻燃材料3份(由碳纳米管、碳纳米纤维和可膨胀石墨按照1∶2∶4比例组成)、复合增粘材料2份(由烷基酚醛树脂和硅烷偶联剂按照1∶1比例组成)、磷酸三乙酯(TEP)11份、氢氧化铝44份、AC发泡剂7份、硫磺0.3份、PDM为0.5份、硬脂酸锌0.5份、硬脂酸0.5份，聚乙烯蜡1份、防老剂RD为1份，防老剂4010为0.5份。
按以下步骤制备高填充防火橡塑发泡保温材料：
(1)原料预分散
将按比例称取的复合碳基阻燃材料、复合增粘材料、磷酸酯、氢氧化铝、发泡剂、润滑剂、防老剂投入到高速混合机中进行混合，采用间歇式混合工艺，时间40min，使各类原材料进行预分散处理。
(2)混炼胶料制备
(a)首先将丁腈橡胶和聚氯乙烯糊树脂投入密炼机混炼，转子转速30r/min，时间2min；
(b)接着将步骤(1)中的预分散混合料投入密炼机一起进行混炼，时间为10min，温度为125℃；
(c)将混炼完成的胶料投入开炼机进行开炼，同时加入复合催化剂、硫磺、硫化发泡助剂。开炼时间12min，开炼温度60℃；开炼结束后出条，凉置备用；
(3)挤出
将步骤(2)冷却后的胶条喂入挤出机，对胶料进行真空排气处理和产品定型，工艺参数根据产品规格进行设置；
(4)硫化发泡
将步骤(3)中经过挤出的胶料，输送到硫化发泡炉进行连续发泡生产，制备高填充防火橡塑发泡保温材料。
实施例2
称取以下重量份的原料：丁腈橡胶18份、PVC糊树脂4.5份、复合催化剂5份(由氧化铁和三氧化钼按照1∶1比例组成)、复合碳基阻燃材料3份(由碳纳米管、碳纳米纤维和可膨胀石墨按照1∶2∶4比例组成)、复合增粘材料1.5份(由烷基酚醛树脂和硅烷偶联剂按照1∶1比例组成)、磷酸三乙酯(TEP)12份、氢氧化铝40份、AC发泡剂8份、硫磺0.4份、PDM为0.7份，硬脂酸锌0.7份、硬脂酸0.7份，聚乙烯蜡1份、防老剂RD为1份，防老剂4010为0.8份。
制备方式和实施例1一样。
实施例3
称取以下重量份的原料：丁腈橡胶14份、PVC糊树脂3.5份、复合催化剂3.8份(由氧化铁和三氧化钼按照1∶1比例组成)、复合碳基阻燃材料2.5份(由碳纳米管、碳纳米纤维和可膨胀石墨按照1∶2∶4比例组成)、复合增粘材料2.8份(由烷基酚醛树脂和硅烷偶联剂按照1∶1比例组成)、磷酸三乙酯(TEP)14份、氢氧化铝42份、AC发泡剂7.5份、硫磺0.4份、PDM为0.9份，硬脂酸锌0.9份、硬脂酸0.6份，聚乙烯蜡1份、防老剂RD为0.6份，防老剂4010为0.6份。
制备方式和实施例1一样。
实施例4
称取以下重量份的原料：丁腈橡胶16份、PVC糊树脂4份、复合催化剂5份(由氧化铁和三氧化钼按照1∶1比例组成)、复合碳基阻燃材料4份(由碳纳米管、碳纳米纤维和可膨胀石墨按照1∶2∶4比例组成)、复合增粘材料2份(由烷基酚醛树脂和硅烷偶联剂按照1∶1比例组成)、磷酸三乙酯(TEP)11份、氢氧化铝42份、AC发泡剂7份、硫磺0.3份、PDM为0.5份，硬脂酸锌0.5份、硬脂酸0.5份，聚乙烯蜡1份、防老剂RD为1份，防老剂4010为0.5份。
制备方式和实施例1一样。
对比例1：采用与实施例1相同方法制备高填充橡塑发泡保温材料，不同之处在于，原料配方中不加复合催化剂，氢氧化铝48份。
对比例2：采用与实施例1相同方法制备高填充橡塑发泡保温材料，不同之处在于，原料配方中不加复合碳基阻燃材料，氢氧化铝47份。
对比例3：采用与实施例1相同方法制备高填充橡塑发泡保温材料，不同之处在于，原料配方中不加复合增粘材料，氢氧化铝46份。
测试试验：
针对实施例1-4以及对比例1-3提供的橡塑发泡保温材料试样进行性能测试，结果如表1所示。
表1
耐火性测试：样品尺寸为500mm长×500mm宽×30mm厚。样品用支架竖向垂直固定，采用火焰喷枪距离样品中心8cm距离点持续点燃15min；试验结束后，观察测试结果。其中火焰喷枪持续点燃5min后，表面温度应达到1093℃以上。
通过测试结果可知，本发明制备出的高填充防火橡塑发泡保温材料符合不燃A级标准要求，并且具有较低的导热系数和较好的防火性能。根据对比例可知，不加复合催化剂、复合碳基阻燃材料或复合增粘材料，燃烧等级效果均不太理想。
Claims (12)
1.一种高填充防火橡塑发泡保温材料，包括如下重量份的原料：丁腈橡胶10-20份、PVC糊树脂3-5份、复合催化剂3-6份、复合碳基阻燃材料1-4份、复合增粘材料1-3份、磷酸酯10-20份、氢氧化铝40-50份、发泡剂6-8份、硫磺0.1-0.5份、硫化发泡助剂0.5-2份、润滑剂1-2份、防老剂1-2份，其特征在于，复合催化剂由氧化铁和三氧化钼按照重量用量比例1∶1组成；复合碳基阻燃材料由碳纳米管、碳纳米纤维和可膨胀石墨按照重量用量比例1∶2∶4组成；复合增粘材料由烷基酚醛树脂和硅烷偶联剂按照重量用量比例为1∶1组成。
2.根据权利要求1所述橡塑发泡保温材料，其特征在于，磷酸酯选自磷酸三乙酯、磷酸三甲苯酯、以及磷酸三(2-氯丙基)酯至少其中一种。
3.根据权利要求1所述橡塑发泡保温材料，其特征在于，硫化发泡助剂由多功能橡胶助剂N,N’-间苯撑双马来酰亚胺和硬脂酸锌组成。
4.根据权利要求2所述橡塑发泡保温材料，其特征在于，硫化发泡助剂由多功能橡胶助剂N,N’-间苯撑双马来酰亚胺和硬脂酸锌组成。
5.根据权利要求3所述橡塑发泡保温材料，其特征在于，N,N’-间苯撑双马来酰亚胺和硬脂酸锌重量用量比例为1-2∶1。
6.根据权利要求4所述橡塑发泡保温材料，其特征在于，N,N’-间苯撑双马来酰亚胺和硬脂酸锌重量用量比例为1-2∶1。
7.根据权利要求1-6所述任意一种橡塑发泡保温材料，其特征在于，润滑剂由硬脂酸和聚乙烯蜡组成。
8.根据权利要求1-6所述任意一种橡塑发泡保温材料，其特征在于，防老剂由喹啉类和对苯二胺类组成。
9.根据权利要求1-8所述任意一种高填充防火橡塑发泡保温材料的制备方法，具体包括如下步骤：
(1)原料预分散
将按比例称取的复合碳基阻燃材料、复合增粘材料、磷酸酯、氢氧化铝、发泡剂、润滑剂、防老剂投入到高速混合机中进行混合，采用间歇式混合工艺，使各类原材料进行预分散处理；
(2)混炼胶料制备
(a)首先将丁腈橡胶和聚氯乙烯糊树脂投入密炼机混炼；
(b)接着将步骤(1)中的预分散混合料投入密炼机一起进行混炼；
(c)将混炼完成的胶料投入开炼机进行开炼，同时加入复合催化剂、硫磺、硫化发泡助剂,开炼结束后出条，凉置备用；
(3)挤出
将步骤(2)冷却后的胶条喂入挤出机，对胶料进行真空排气处理和产品定型，工艺参数根据产品规格进行设置；
(4)硫化发泡
将步骤(3)中经过挤出的胶料，输送到硫化发泡炉进行连续发泡生产，即可得到所述高填充防火橡塑发泡保温材料。
10.根据权利要求9所述橡塑发泡保温材料的制备方法，其特征在于，步骤(2)(b)中混炼时间为10-15min，温度为100℃-130℃。
11.根据权利要求9所述橡塑发泡保温材料的制备方法，其特征在于，步骤(2)(c)中开炼时间为10-15min，开炼温度小于80℃。
12.根据权利要求10所述橡塑发泡保温材料的制备方法，其特征在于，步骤(2)(c)中开炼时间为10-15min，开炼温度小于80℃。
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| CN114149626A (zh) * | 2022-01-04 | 2022-03-08 | 神州节能科技集团有限公司 | 一种难燃的轻量型橡塑发泡制品及其制造方法 |
| CN114437428A (zh) * | 2021-12-30 | 2022-05-06 | 易宝（福建）高分子材料股份公司 | 一种改性nbr/pvc发泡材料及其制备方法 |
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| JPH0747658B1 (zh) * | 1988-04-05 | 1995-05-24 | Kanegafuchi Chemical Ind | |
| JPH11117425A (ja) * | 1997-10-09 | 1999-04-27 | Sekisui Chem Co Ltd | 耐火積層体及び耐火鉄骨被覆材 |
| JP2002294078A (ja) * | 2001-03-29 | 2002-10-09 | Kanegafuchi Chem Ind Co Ltd | 耐水性を有する発泡型防火性組成物 |
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| CN114149626A (zh) * | 2022-01-04 | 2022-03-08 | 神州节能科技集团有限公司 | 一种难燃的轻量型橡塑发泡制品及其制造方法 |
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