CN106674597B - 一种氮磷协效阻燃剂改性层状无机物及其制备方法和应用 - Google Patents
一种氮磷协效阻燃剂改性层状无机物及其制备方法和应用 Download PDFInfo
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- CN106674597B CN106674597B CN201611269261.9A CN201611269261A CN106674597B CN 106674597 B CN106674597 B CN 106674597B CN 201611269261 A CN201611269261 A CN 201611269261A CN 106674597 B CN106674597 B CN 106674597B
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- Compositions Of Macromolecular Compounds (AREA)
Abstract
本发明公开了一种氮磷协效阻燃剂改性层状无机物及其制备方法和应用,属于阻燃剂改性层状无机物及其应用领域。该方法是将层状无机物、氮源阻燃剂、磷源阻燃剂按质量比20‑30:6‑9:3‑6,依次加入到三口烧瓶中,然后加入溶剂并升温至60‑100℃,在氮气氛围下搅拌反应3‑7h,经过滤、洗涤、干燥得氮磷协效阻燃剂改性层状无机物。将氮磷协效阻燃剂改性层状无机物与膨胀型阻燃剂复合,添加在硅橡胶中制备成阻燃性能优异、机械性能良好的复合材料。该改性层状无机物的加入能够明显提高复合材料的阻燃性能以及机械性能,这对无机物的表面改性和复合材料的阻燃增强,都具有深远的意义。
Description
技术领域
本发明属于阻燃剂改性层状无机物及其应用领域,具体涉及一种氮磷协效阻燃剂改性层状无机物及其制备方法和应用。
背景技术
硅橡胶具有生物相容性,耐高低温性、绝缘性、耐候性等优异的性能,经过70多年的开发利用发展,广泛运用于医疗卫生、航天航空、电线电缆、汽车工业等多个领域。但是硅橡胶本身易燃,一旦引燃更会持续燃烧,严重限制了硅橡胶的应用范围。因此对硅橡胶的阻燃改性显得尤为重要。
随着人们环保意识的加强,含卤素类阻燃剂由于燃烧时会释放出有毒气体,对环境危害较大而受到限制。氢氧化镁、氢氧化铝等金属氢氧化物阻燃剂在燃烧时无有害气体释放,燃烧后的残渣也不会污染环境,但只有添加量较大的时候才有明显的阻燃效果,而大量填充会严重恶化基体本身的物理机械性能。膨胀型阻燃剂具有低烟、无毒、阻燃效率高,燃烧时无熔融滴落物、无腐蚀性气体等特点,是一种环保高效的阻燃剂,广泛应用于各种聚合物阻燃体系。近年来,大量研究表明,膨胀型阻燃剂和层状无机化合物复配使用时,具有很好的协效阻燃作用,能显著提高聚合物基体阻燃性能。Wang D Y等(Preparation andburning behaviors of flame retarding biodegradable poly(lactic acid)nanocomposite based on zinc aluminum layered double hydroxide[J].PolymerDegradation and Stability,2010,95(12):2474-2480)复配膨胀型阻燃剂和铝镁水滑石复合使用制备出阻燃性能优异的聚乳酸纳米复合材料。Yang D等(Synergistic flameretardant effect ofα-zirconium phosphate in low-density polyethylene/ethylene–vinyl acetate/aluminum hydroxide hybrids[J].Journal of ThermalAnalysis and Calorimetry,2015,119(1):619-624.)将磷酸锆添加入LDPE/EVA杂化材料能显著提高基体的阻燃性能。但是层状无机物在聚合物基体里面较难分散,易团聚,使得制备的复合材料力学性能不佳,限制了层状无机物的使用。另外经过表面改性处理的层状无机物虽然能在基体有较好的分散但是因为改性剂本身的易燃性,使得对聚合物基体本身的阻燃性能会有影响。
因此本发明公开了一种层状无机物的改性方法。按照这种方法制备的氮磷协效阻燃剂改性层状无机物在聚合物基体里面有很好的分散,不仅能显著提高聚合物基体的阻燃性能,更能起到良好的补强效果。这种氮磷协效阻燃剂改性层状无机物及其制备方法和应用迄今未见国内外文献报道。
发明内容
本发明的目的在于克服目前层状无机物在聚合物基体中分散性不好,以及改性剂处理后聚合物基体阻燃性能受影响的缺点,提供一种氮磷协效阻燃剂改性层状无机物及其制备方法和应用,该氮磷协效阻燃剂改性层状无机物具有良好分散效果,以其制备具有高阻燃性能的复合材料,扩大层状无机物的应用范围。
本发明的目的通过以下技术方案实现。
本发明的氮磷协效阻燃剂改性层状无机物是利用常用的氮源阻燃剂和磷源阻燃剂***层状无机物层间进行原位反应,得到一种改性层状无机物。
以磷酸锆,双氰胺,六氯环三磷腈为例,其制备原理如下:
一种氮磷协效阻燃剂改性层状无机物的制备方法,包括以下步骤:
(1)将层状无机物、氮源阻燃剂、磷源阻燃剂依次加入到三口烧瓶中,然后加入溶剂并升温至60-100℃,在氮气氛围下搅拌反应,反应后经过滤、洗涤、干燥得氮磷协效阻燃剂改性层状无机物。
优选的,所述层状无机物、氮源阻燃剂、磷源阻燃剂的质量比(20-30):(6-9):(3-6);所述反应的时间为3-7h。
优选的,所述的层状无机物为蒙脱土、云母、高岭土、水滑石和磷酸锆等中的一种以上;所述的氮源阻燃剂为单氰胺、双氰胺、三聚氰胺和尿素等中的一种以上。所述的磷源阻燃剂为六氯环三磷腈、9,10-二氢-9-氧杂-10-磷杂菲-10-氧化物和二氯三苯基磷等中的一种以上;所述的溶剂为N,N-二甲基甲酰胺、二甲基亚砜、N,N-二甲基乙酰胺、甲苯和二氯甲烷等中的任意一种或多种。
由以上所述的制备方法制得的一种氮磷协效阻燃剂改性层状无机物。
以上所述的一种氮磷协效阻燃剂改性层状无机物在制备无卤阻燃硅橡胶复合材料中的应用,所述无卤阻燃硅橡胶复合材料的组分和各组分的质量百分比如下:
硅橡胶:68.5-80%,进一步优选为70.5-80%;
硫化剂:0.4-4%,进一步优选为0.4-3%;
复合膨胀型阻燃剂:17-28.5%,进一步优选为18-27.5%;
所述复合膨胀型阻燃剂是膨胀型阻燃剂和氮磷协效阻燃剂改性层状无机物的均匀混合物。
优选的,所述膨胀型阻燃剂和氮磷协效阻燃剂改性层状无机物的质量比(17-27):(0.5-5)。
优选的,所述的膨胀型阻燃剂为单体膨胀型阻燃剂和复配膨胀型阻燃剂中的至少一种。
进一步优选的,所述的单体膨胀型阻燃剂为2,4,8,10-四氧-3,9二磷螺环[5,5]十一烷-3.9二氧-3,9-二三聚氰胺盐、双(2,6,7-三氧-1-磷-双环[2,2,2]辛烷-1-氧甲基)磷酸酯三聚氰胺盐、三(新戊二醇磷酸酯-磷-亚甲基)胺和新戊二醇磷酸酯三聚氰铵盐等中的至少一种;所述的复配膨胀型阻燃剂为季戊四醇和聚磷酸胺复配体系、三聚氰胺聚磷酸盐和季戊四醇体系、三聚氰胺磷酸盐和季戊四醇复配体系等中的至少一种体系。
优选的,所述的硅橡胶为二甲基硅橡胶、甲基乙烯基硅橡胶、甲基苯基乙烯基硅橡胶、氟硅橡胶、腈硅橡胶和二乙基硅橡胶等中的一种以上;所述的硫化剂为2,4-二氯过氧化苯甲酰、2,5-二甲基-2,5-双(叔丁基过氧基)己烷、过氧化苯甲酰和过氧化二异苯丙等中的一种以上。
优选的,该无卤阻燃硅橡胶复合材料的制备方法如下:将硅橡胶、复合膨胀型阻燃剂和硫化剂在开炼机或密炼机中15-40℃下混炼15-20min,然后在平板硫化仪中100-140℃下进行平板硫化10-20min,得无卤阻燃硅橡胶复合材料。
本发明制备氮磷协效阻燃剂改性层状无机物的方法可进一步推广到其他无机物的表面改性领域,与此同时,该改性层状无机物的加入能够明显提高复合材料的阻燃性能以及机械性能,这对无机物的表面改性和复合材料的阻燃增强,都具有深远的意义。
与现有技术相比,本发明具有如下优点与技术效果:
(1)本发明的制备工艺简单,不需要复杂的后处理步骤,便于工业化的实现。
(2)本发明的改性层状无机物通过氮磷协效阻燃剂改性,避免传统改性剂本身易燃性的缺点,为无机物的表面处理提供了另一种思路。
(3)本发明的改性层状无机物在聚合物基体里面能够很好的分散,不易团聚,而且能够显著提高聚合物基体的阻燃性能和机械性能,应用前景广阔。
附图说明
图1是实施例1中氮磷协效阻燃剂改性层状无机物和未改性层状无机物的XRD谱图。
图2a、图2b分别是实施例2中氮磷协效阻燃剂改性层状无机物和未改性层状无机物的SEM照片。
图3是实施例3中氮磷协效阻燃剂改性层状无机物和未改性层状无机物在硅橡胶基体分散的XRD谱图。
图4a、图4b分别是实施例5中氮磷协效阻燃剂改性层状无机物和未改性层状无机物在硅橡胶基体分散的TEM谱图。
具体实施方式
为了更好地叙述和理解本发明,下面结合实施例和附图对本发明的具体实施作进一步说明,但是本发明要求保护的范围并不局限于实施例表述的范围。
实施例1
将20g云母、9g单氰胺、3g 9,10-二氢-9-氧杂-10-磷杂菲-10-氧化物依次加入到三口烧瓶中,然后加入N,N-二甲基甲酰胺并升温至60℃,在氮气氛围下搅拌反应7h,经过滤、洗涤、干燥得氮磷协效阻燃剂改性层状无机物。图1是本实施例制备的氮磷协效阻燃剂改性层状无机物和未改性层状无机物的XRD谱图。从图可以发现特征衍射峰向小角度偏移,说明层间距变大,片层被打开,有利于在聚合物基体的分散。
实施例2
将24磷酸锆、8g双氰胺、5g六氯环三磷腈依次加入到三口烧瓶中,然后加入N,N-二甲基乙酰胺并升温至70℃,在氮气氛围下搅拌反应6h,经过滤、洗涤、干燥得氮磷协效阻燃剂改性层状无机物。图2a、图2b是本实施例制备的氮磷协效阻燃剂改性层状无机物和未改性层状无机物的SEM照片,从图可以明显发现磷酸锆片层层间距变大,层间作用减弱。
实施例3
将30g蒙脱土、6g三聚氰胺、6g二氯三苯基磷依次加入到三口烧瓶中,然后加入二甲基亚砜并升温至80℃,在氮气氛围下搅拌反应5h,经过滤、洗涤、干燥得氮磷协效阻燃剂改性层状无机物。然后将22g新戊二醇磷酸酯三聚氟铵盐和3g改性层状无机物均匀混合制得复合膨胀型阻燃剂,再将70.5g甲基乙烯基硅橡胶、27.5g复合膨胀型阻燃剂、0.4g 2,5-二甲基-2,5-双(叔丁基过氧基)己烷在15℃下于开炼机中混炼15min,然后用平板硫化仪于100℃下进行平板硫化10min得到产品。图3是本实施例制备的氮磷协效阻燃剂改性层状无机物和未改性层状无机物在硅橡胶基体中分散的XRD谱图。对比发现未改性的样品仍然有尖锐的特征衍射峰,说明有部分蒙脱土仍然团聚在一起。而改性后的样品特征衍射峰基本消失,说明分散较好。
实施例4
将25g高岭土、7.5g尿素、4.5g六氯环三磷腈依次加入到三口烧瓶中,然后加入甲苯并升温至90℃,在氮气氛围下搅拌反应4h,经过滤、洗涤、干燥得氮磷协效阻燃剂改性层状无机物。然后将27g季戊四醇和聚磷酸胺复配体系(质量比为3:1)和5g改性层状无机物均匀混合制得复合膨胀型阻燃剂,再将80g二甲基硅橡胶、18g复合膨胀型阻燃剂、3g过氧化二异苯丙在25℃下于开炼机中混炼17min,然后用平板硫化仪于120℃下进行平板硫化15min得到产品。表1是改性层状无机物和未改性层状无机物阻燃性能对比数据。
表1
从表1中可以发现经氮磷协效阻燃剂改性的层状无机物能赋予复合材料更好的阻燃性能。
实施例5
将22g水滑石、7g尿素、4g六氯环三磷腈,依次加入到三口烧瓶,然后加入二甲基亚砜并升温至100℃,在氮气氛围下搅拌反应3h,经过滤、洗涤、干燥得氮磷协效阻燃剂改性层状无机物。然后将17g双(2,6,7-三氧-1-磷-双环[2,2,2]辛烷-1-氧甲基)磷酸酯三聚氰胺盐和0.5g改性层状无机物均匀混合制得复合膨胀型阻燃剂,再将77.5g甲基苯基乙烯基硅橡胶、23.5g复合膨胀型阻燃剂、1.5g 2,4-二氯过氧化苯甲酰在40℃下于开炼机中混炼20min,然后用平板硫化仪于140℃下进行平板硫化20min得到产品。图4a、图4b是本实施例制备的氮磷协效阻燃剂改性层状无机物和未改性层状无机物在硅橡胶基体分散的TEM谱图。从图4a、图4b中可以发现改性无机物在硅橡胶基体分散的更好。表2是改性层状无机物和未改性层状无机物机械性能对比数据。
表2
从表2中可以发现经氮磷协效阻燃剂改性的层状无机物能赋予复合材料更好的机械性能。
Claims (10)
1.一种氮磷协效阻燃剂改性层状无机物的制备方法,其特征在于,包括以下步骤:将层状无机物、氮源阻燃剂、磷源阻燃剂依次加入到三口烧瓶中,然后加入溶剂并升温至60-100℃,在氮气氛围下搅拌反应,反应后经过滤、洗涤、干燥得氮磷协效阻燃剂改性层状无机物;所述的氮源阻燃剂为单氰胺、双氰胺、三聚氰胺和尿素中的一种以上;所述的磷源阻燃剂为六氯环三磷腈、9,10-二氢-9-氧杂-10-磷杂菲-10-氧化物和二氯三苯基磷中的一种以上。
2.根据权利要求1所述的制备方法,其特征在于,所述层状无机物、氮源阻燃剂、磷源阻燃剂的质量比为(20-30):(6-9):(3-6);所述反应的时间为3-7h。
3.根据权利要求1所述的制备方法,其特征在于,所述的层状无机物为蒙脱土、云母、高岭土、水滑石和磷酸锆中的一种以上;所述的溶剂为N,N-二甲基甲酰胺、二甲基亚砜、N,N-二甲基乙酰胺、甲苯和二氯甲烷中的任意一种或多种。
4.由权利要求1-3任一项所述的制备方法制得的一种氮磷协效阻燃剂改性层状无机物。
5.权利要求4所述的一种氮磷协效阻燃剂改性层状无机物在制备无卤阻燃硅橡胶复合材料中的应用,其特征在于,所述无卤阻燃硅橡胶复合材料的组分和各组分的质量百分比如下:
硅橡胶:68.5-80%,
硫化剂:0.4-4%,
复合膨胀型阻燃剂:17-28.5%;
所述复合膨胀型阻燃剂是膨胀型阻燃剂和氮磷协效阻燃剂改性层状无机物的均匀混合物。
6.根据权利要求5所述的应用,其特征在于,所述膨胀型阻燃剂和氮磷协效阻燃剂改性层状无机物的质量比为(17-27):(0.5-5)。
7.根据权利要求5所述的应用,其特征在于,所述的膨胀型阻燃剂为单体膨胀型阻燃剂和复配膨胀型阻燃剂中的至少一种。
8.根据权利要求7所述的应用,其特征在于,所述的单体膨胀型阻燃剂为2,4,8,10-四氧-3,9二磷螺环[5,5]十一烷-3.9二氧-3,9-二三聚氰胺盐、双(2,6,7-三氧-1-磷-双环[2,2,2]辛烷-1-氧甲基)磷酸酯三聚氰胺盐、三(新戊二醇磷酸酯-磷-亚甲基)胺和新戊二醇磷酸酯三聚氰铵盐中的至少一种;所述的复配膨胀型阻燃剂为季戊四醇和聚磷酸胺复配体系、三聚氰胺聚磷酸盐和季戊四醇体系、三聚氰胺磷酸盐和季戊四醇复配体系中的至少一种体系。
9.根据权利要求5所述的应用,其特征在于,所述的硅橡胶为二甲基硅橡胶、甲基乙烯基硅橡胶、甲基苯基乙烯基硅橡胶、氟硅橡胶、腈硅橡胶和二乙基硅橡胶中的一种以上;所述的硫化剂为2,4-二氯过氧化苯甲酰、2,5-二甲基-2,5-双(叔丁基过氧基)己烷、过氧化苯甲酰和过氧化二异苯丙中的一种以上。
10.根据权利要求5-9任一项所述的应用,其特征在于,该无卤阻燃硅橡胶复合材料的制备方法如下:将硅橡胶、复合膨胀型阻燃剂和硫化剂在开炼机或密炼机中15-40℃下混炼15-20min,然后在平板硫化仪中100-140℃下进行平板硫化10-20min,得无卤阻燃硅橡胶复合材料。
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