CN104212139B - 硼砂-膨胀型阻燃剂协效改性聚甲基硅氧烷/聚甲基丙烯酸丁酯聚乳酸材料及其制备 - Google Patents
硼砂-膨胀型阻燃剂协效改性聚甲基硅氧烷/聚甲基丙烯酸丁酯聚乳酸材料及其制备 Download PDFInfo
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Abstract
本发明公开了一种硼砂-膨胀型阻燃剂协效改性聚甲基硅氧烷/聚甲基丙烯酸丁酯聚乳酸复合材料及其制备方法。按重量百分比,该生物材料由74%的聚乳酸,13~22%的双磷酸季戊四醇酯密胺盐,1%的硼砂,3~12%的核/壳聚甲基硅氧烷/聚甲基丙烯酸丁酯纳米粒子制成。先用种子乳液聚合法合成核/壳结构聚甲基硅氧烷/聚甲基丙烯酸丁酯纳米粒子,再将硼砂、双磷酸季戊四醇酯密胺盐、聚乳酸充分干燥后用转矩流变仪均匀混合,再注塑成为标准样条。
Description
技术领域
本发明属于阻燃技术领域,特别涉及到硼砂-膨胀型阻燃剂协效改性聚甲基硅氧烷/聚甲基丙烯酸丁酯聚乳酸材料的制备方法。
技术背景
随着人类对石油资源的掠夺性开发,石化高分子化合物对环境污染的日益加剧,使用非石油资源、对环境友好的材料已迫在眉睫。聚乳酸的原料乳酸可通过淀粉发酵而来,且聚乳酸的分解产物为水和二氧化碳,属于完全生物可降解材料。聚乳酸有着良好的热稳定性,加工温度在170-230℃,加工性能良好;但聚乳酸也存在着性脆,结晶度低,氧指数低,燃烧时易融滴并造成二次燃烧低的缺点。为扩大聚乳酸的应用范围,聚乳酸阻燃研究势在必行,中国专利201310008873.2公开了一种无卤阻燃聚乳酸纳米复合材料,其极限氧指数达到30-40,UL-94也达到了V-0级别,但是其拉伸强度均在20兆帕以下,断裂伸长率也极低。
膨胀性阻燃剂MPP是常见的高分子材料阻燃剂,何继辉等研究了含硅阻燃剂与膨胀性阻燃剂的协同,作用证明硼、磷、硅元素能形成陶瓷状化合物,对表面膨胀炭层起到增强作用,提高炭层的热氧稳定性和阻隔性能(高分子材料科学与工程,2010,26:31~34)。中国专利201210113969.0公开了一种水性膨胀性隧道防火防霉涂料,以硅丙乳液为成膜物,以改性聚磷酸胺、双季戊四醇、偶氮二甲酰胺为阻燃剂,得到了一种防火时限长的防霉防火保护涂层。
发明内容
本发明的目的是提供一种阻燃效果良好,抗融滴,力学性能较优、加工性能较好、耐热性好、结晶度高的硼砂-膨胀型阻燃剂协效改性的聚甲基硅氧烷/聚甲基丙烯酸丁酯聚乳酸复合材料及其制备。
本发明的一种硼砂-膨胀型阻燃剂协效改性的聚甲基硅氧烷/聚甲基丙烯酸丁酯聚乳酸复合材料由以下重量百分含量的组分组成:
其制备方法为:将聚乳酸、双磷酸季戊四醇酯密胺盐、硼砂、核/壳-聚甲基硅氧烷/聚甲基丙烯酸丁酯粒子混合,在170~175℃条件下,用转矩流变熔融共混,得到具有阻燃功能的聚乳酸复合材料,其中,转矩流变的三段温度分别为:170~172℃,172~174℃,173~175℃;转速为30rpm。
所述步骤中,聚甲基硅氧烷/聚甲基丙烯酸丁酯粒子为核壳结构粒子,粒径在100nm左右。
所述步骤中,所述的聚乳酸、核/壳-聚甲基硅氧烷/聚甲基丙烯酸丁酯粒子先在60~80℃下干燥6~10小时。
所述步骤中,所述的双磷酸季戊四醇酯密胺盐、硼砂先在60~80℃下干燥8~10小时,研磨后过80目筛。
本发明的聚乳酸复合材料的优点如下:
(1)本发明所提供的聚乳酸复合材料具有较高的阻燃级别。
(2)本发明所提供的聚乳酸复合材料所用阻燃剂双磷酸季戊四醇酯密胺盐和硼砂为无卤阻燃剂,改性添加剂核/壳-聚甲基硅氧烷/聚甲基丙烯酸丁酯粒子也无毒害,使得聚合材料在使用和燃烧过程中安全无毒,属于绿色环保材料。
(3)本发明所提供的聚乳酸复合材料采用了多种改性剂,且不同阻燃剂之间存在协同作用:硼、硅元素有支撑碳层,增加碳层表面致密度的作用;硼、磷、硅元素能形成陶瓷状化合物,对表面膨胀炭层起到增强作用,提高炭层的热氧稳定性和阻隔性能。相比添加单一阻燃剂的聚乳酸材料,该聚乳酸复合材料有着更好的阻燃效果。
(4)本发明所提供的聚乳酸复合材料中添加了弹性预定体核/壳-聚甲基硅氧烷/聚甲基丙烯酸丁酯粒子,硼砂等改性填料,充分利用了核/壳-聚甲基硅氧烷/聚甲基丙烯酸丁酯粒子内核聚甲基硅氧烷主链Si-O-Si的链段柔性,与单一添加双磷酸季戊四醇酯密胺盐的聚乳酸材料,有着更好的拉伸强度和加工性能。
(5)本发明所提供的聚乳酸复合材料采用了核/壳-聚甲基硅氧烷/聚甲基丙烯酸丁酯粒子,其外壳层聚甲基丙烯酸甲酯的溶解度参数介于聚甲基硅氧烷和基体聚乳酸之间,改善了聚甲基硅氧烷粒子和基体聚乳酸之间的相容性,增加了聚乳酸复合材料的耐候性、耐久性。
(6)本发明所提供的聚乳酸复合材料中添加了硼砂,以及聚甲基硅氧烷,与纯聚乳酸相比,有着更好的耐热性能。
(7)本发明所提供的聚乳酸复合材料的阻燃剂、增韧改性剂、成核剂、耐热改性剂、加工助剂为聚乳酸、双磷酸季戊四醇酯密胺盐、硼砂、核/壳聚甲基硅氧烷/聚甲基丙烯酸丁酯中的一种或多种。
具体实施方法
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,对本发明内容的修改和改动同样落于本发明所附权利要求书所限定的范围内。
本发明所使用改性填料核/壳结构聚甲基硅氧烷/聚甲基丙烯酸丁酯材料的制备方法如下:
(1)将八甲基环四硅氧烷(48.5g),正硅酸四乙酯(1g),甲基丙烯酰氧基丙基甲基二甲氧基硅烷(0.25g),十二烷基苯磺酸钠(0.5g),水(100ml)通过超声分散10min,再以高速乳化机以10000rpm*15min高速乳化成稳定乳液。
(2)将所得稳定乳液倒入装有搅拌、冷凝回流装置,温度计的四口烧瓶反应装置中,加预先备好的硫酸溶液(98%H2SO4:H2O=4:1),搅拌,80℃水浴中反应5h。
(3)取所得乳液,二甲基丙烯酸乙二醇酯(0.75g),甲基丙烯酸丁酯(31.75g),十二烷基苯磺酸钠(0.35g),水110ml通过超声分散10min,倒入装有搅拌、冷凝回流装置、温度计的四口烧瓶中,置于水浴装置中,并通氮气保护10min。
(4)在置于水浴装置中,装有搅拌、冷凝回流装置、温度计的四口烧瓶反应装置中,分两步加入氧化还原引发体系:亚硫酸钠溶液(0.1g:10mlH2O),过硫酸钾溶液(0.3g:10mlH2O),再以500r/min高速搅拌10min,升温至65℃反应5小时。
(5)将所得目标乳液转移,用氯化钙水溶液破乳并离心,再用50ml去离子水润洗三遍,在60℃下烘干24h至重量不再变化。粉碎后过80目筛。
实施例1:
取核/壳-聚甲基硅氧烷/聚甲基丙烯酸丁酯6g,硼砂0.5g,双磷酸季戊四醇酯密胺盐6.5g,于60℃下烘干8h并过80目筛,聚乳酸37g于60℃下烘干8h,将四种材料物理共混,放入转矩流变仪中,三段温度分别为:170~172℃,172~174℃,173~175℃;转速30rpm,共混5~8min。得到目标材料。
实施例2:
取核/壳-聚甲基硅氧烷/聚甲基丙烯酸丁酯4.5g,硼砂0.5g,双磷酸季戊四醇酯密胺盐8g,于60℃下烘干8h并过80目筛,聚乳酸37g于60℃下烘干8h,将四种材料物理共混,放入转矩流变仪中,三段温度分别为:170~172℃,172~174℃,173~175℃;转速30rpm,共混5~8min。得到目标材料。
实施例3:
取核/壳-聚甲基硅氧烷/聚甲基丙烯酸丁酯3g,硼砂0.5g,双磷酸季戊四醇酯密胺盐9.5g,于60℃下烘干8h并过80目筛,聚乳酸37g于60℃下烘干8h,将四种材料物理共混,放入转矩流变仪中,三段温度分别为:170~172℃,172~174℃,173~175℃;转速30rpm,共混5~8min。得到目标材料。
实施例4:
取核/壳-聚甲基硅氧烷/聚甲基丙烯酸丁酯1.5g,硼砂0.5g,双磷酸季戊四醇酯密胺盐11g,于60℃下烘干8h并过80目筛,聚乳酸37g于60℃下烘干8h,将四种材料物理共混,放入转矩流变仪中,三段温度分别为:170~172℃,172~174℃,173~175℃;转速30rpm,共混5~8min。得到目标材料。
对比例1:
取双磷酸季戊四醇酯密胺盐12.5g,于60℃下烘干8h并过80目筛,聚乳酸37.5g于60℃下烘干8h,将两种材料物理共混后放入转矩流变仪中,三段温度分别为:170~172℃,172~174℃,173~175℃;转速30rpm,共混5~8min。得到目标材料。
对比例2:
取核/壳-聚甲基硅氧烷/聚甲基丙烯酸丁酯6g,于60℃下烘干8h并过80目筛,聚乳酸44g于60℃下烘干8h,将两种材料物理共混后放入转矩流变仪中,三段温度分别为:170~172℃,172~174℃,173~175℃;转速30rpm,共混5~8min。得到目标材料。
对比例3:
取纯聚乳酸50g,于60℃下烘干8h后放入转矩流变仪中,三段温度分别为:170~172℃,172~174℃,173~175℃;转速30rpm,共混5~8min。得到目标材料。
目标材料的拉伸强度、断裂伸长率、极限氧指数、垂直燃烧等性能如表1所示:
表1目标材料的拉伸强度、断裂伸长率、极限氧指数、垂直燃烧性能:
测试项目 | 拉伸强度 | 断裂伸长率 | 极限氧指数 | UL-94 |
单位 | MPa | % | % | -- |
实施例1 | 36.91 | 10.62 | 23.1 | V-2能 |
实施例2 | 30.61 | 10.37 | 24.3 | V-0能 |
实施例3 | 22.39 | 5.62 | 25.6 | V-0否 |
实施例4 | 22.10 | 4.05 | 28.8 | V-0否 |
对比例1 | 17.64 | 3.13 | 30.5 | V-0否 |
对比例2 | 56.61 | 48.81 | 19.5 | fail |
对比例3 | 64.22 | 15.40 | 20.0 | fail |
Claims (5)
1.一种硼砂-膨胀型阻燃剂协效改性的聚甲基硅氧烷/聚甲基丙烯酸丁酯聚乳酸复合材料,其特征在于,由以下重量百分含量的组分组成:
2.制备如权利要求1所述的硼砂-膨胀型阻燃剂协效改性的聚甲基硅氧烷/聚甲基丙烯酸丁酯聚乳酸复合材料的方法,其特征在于将聚乳酸、双磷酸季戊四醇酯密胺盐、硼砂、核/壳-聚甲基硅氧烷/聚甲基丙烯酸丁酯粒子混合,在170~175℃条件下,用转矩流变熔融共混,得到具有阻燃功能的聚乳酸复合材料,其中,转矩流变的三段温度分别为:170~172℃,172~174℃,173~175℃;转速为30rpm。
3.如权利要求2所述的聚乳酸复合材料的制备方法,其特征在于,聚甲基硅氧烷/聚甲基丙烯酸丁酯粒子为核壳结构粒子,平均粒径为100nm。
4.如权利要求2所述的聚乳酸复合材料的制备方法,其特征在于,先将所述的聚乳酸、核/壳-聚甲基硅氧烷/聚甲基丙烯酸丁酯粒子在60~80℃下干燥6~10小时。
5.如权利要求2所述的聚乳酸复合材料的制备方法,其特征在于,先将所述的双磷酸季戊四醇酯密胺盐、硼砂在60~80℃下干燥8~10小时,研磨后过80目筛。
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