CN103772966A - 微硅粉增强尼龙材料及其制备方法 - Google Patents

微硅粉增强尼龙材料及其制备方法 Download PDF

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CN103772966A
CN103772966A CN201310719035.6A CN201310719035A CN103772966A CN 103772966 A CN103772966 A CN 103772966A CN 201310719035 A CN201310719035 A CN 201310719035A CN 103772966 A CN103772966 A CN 103772966A
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silica fume
nylon
nylon material
reinforced nylon
antioxidant
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石文建
杨再祥
吴毅
雷勇
魏喜苹
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GUIZHOU LANTU NEW MATERIALS CO Ltd
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Abstract

本发明公开了一种微硅粉增强尼龙材料及其制备方法，按重量份数计算，包括40～98份尼龙、1～50份微硅粉、0.1～5份表面改性剂以及0.1～0.5份抗氧化剂。本发明将微硅粉进行表面改性后，再尼龙混合，并在混合过程中加入抗氧化剂，在设定好挤出机螺杆的转速及挤出温度下进行熔融挤出造粒，以获得性能优异的微硅粉改性尼龙母粒。本发明能有效解决尼龙拉伸强度和抗冲击性能差等缺点，改善了尼龙材料的抗蠕变性能和耐热性能，微硅粉改性尼龙复合材料综合性能优良，可进行连续生产。

Description

微硅粉增强尼龙材料及其制备方法
技术领域
本发明涉及高分子科学领域，尤其是一种微硅粉增强尼龙材料及其制备方法。
背景技术
尼龙又称聚酰胺，是分子主链上含有重复酰胺基团的热塑性树脂总称。包括脂肪族尼龙，脂肪芳香族尼龙和芳香族尼龙。其中，脂肪族尼龙品种多，产量大，应用广泛，其命名由合成单体具体的碳原子数而定。尼龙与其他聚合物共混物和合金等，满足不同特殊要求，广泛用作金属，木材等传统材料代用品，作为各种结构材料。
尼龙是最重要的工程塑料，产量在五大通用工程塑料中居首位。尼龙为韧性角状半透明或乳白色结晶性树脂，作为工程塑料的尼龙分子量一般为1.5～3万，尼龙具有很高的机械强度，软化点高，耐热，磨擦系数低，耐磨损，自润滑性，吸震性和消音性，耐油，耐弱酸，耐碱和一般溶剂，电绝缘性好，有自熄性，无毒，无臭，耐候性好，染色性差。尼龙缺点是吸水性大，影响尺寸稳定性和电性能，本专利采用工业废物微硅粉对尼龙进行填充改性，能改善尼龙的吸水性能、耐寒性能、尺寸收缩性以及缺口冲击强度。 
微硅粉又称硅灰或凝聚硅灰，外观为灰色或灰白色粉末。其平均粒径在0.1～0.3um，比表面积较大。其细度和比表面积约为水泥的80～100倍，粉煤灰的50～70倍。微硅粉是冶炼硅铁和工业硅（金属硅）的副产物，矿热电炉内产生出大量挥发性很强的SiO2和Si气体，气体排放后与空气迅速氧化冷凝沉淀而生成的。它是大工业冶炼中，整个过程需要用除尘环保设备进行回收，因为质量比较轻，还需要用加密设备进行加密。微硅粉在形成过程中受表面张力的作用，形成了非结晶相无定形圆球状颗粒，表面较为光滑，有些则是多个圆球颗粒粘在一起的团聚体，微小的球状体可以起到润滑的作用。
中国专利公开号CN103232718A，于2013年8月7日公开了“微硅粉/SBS复合改性沥青及其制备方法”。该专利是采用微硅粉填充到沥青中，得到复合改性的沥青，提高沥青基材的粘合性、耐热性和抗老化性，可节约沥青的使用量，降低生产成本。
中国专利公开号CN102775913A，于2012年11月14日公开了“ 一种利用工业废料微硅粉制作的涂料及其制备方法”。该发明涉及一种利用工业废料微硅粉制作的涂料及其制备方法，该发明充分利用工业废料微硅粉，使其变废为宝，减轻环境压力；且因原料廉价，涂料具有较好的成本优势，同时具有结构致密、填隙良好、附着牢固、色泽雅致的优点。
可见，现有技术主要是将微硅粉作为填料添加到沥青或涂料中，并未涉及到作为增强尼龙材料内。
发明内容
本发明的目的是：提供一种微硅粉增强尼龙材料及其制备方法，它不仅能降低生产成本，还改善了尼龙材料的抗蠕变性能和耐热性能，以克服现有技术的不足。
本发明是这样实现的：微硅粉增强尼龙材料，按重量份数计算，包括40～98份尼龙、1～50份微硅粉、0.1～5份表面改性剂以及0.1～0.5份抗氧化剂。
所述的表面改性剂为硅烷偶联剂、钛酸酯偶联剂或硬脂酸中的一种或几种的任意组合。
所述的抗氧化剂为对苯二酚或对苯二胺。
还包括0.1～5份抗老化剂。
微硅粉增强尼龙材料的制备方法，按上述重量份数取各组分，将微硅粉与表面改性剂进行混合，混合温度为50℃，混合2h后，获得改性的微硅粉；将改性的微硅在温度为100℃的条件下真空干燥6h，获得干燥的改性微硅粉；将干燥的改性微硅粉与尼龙及抗氧化剂充分混合均匀后，加入挤出机熔融挤出造粒并干燥后，获得微硅粉改性尼龙母粒。
挤出机螺杆的转速为200rpm及挤出温度分别为一区240℃、二区250℃、三区260℃、四区270℃、五区270℃、机头260℃。
将干燥的改性微硅粉与尼龙、抗氧化剂进行混合时，同时还加入0.1～5份抗老化剂。
由于采用了上述的技术方案，本发明将微硅粉进行表面改性后，再尼龙混合，并在混合过程中加入抗氧化剂和抗老化剂，在设定好挤出机螺杆的转速及挤出温度下进行熔融挤出造粒，以获得性能优异的微硅粉改性尼龙母粒。加工过程中，通过控制微硅粉、改性剂、抗氧化剂的添加量，以及混合挤出时的温度及螺杆转速来有效控制改性尼龙的力学性能，通过改性微硅粉添加到尼龙材料中，一定程度上能有效解决尼龙拉伸强度和抗冲击性能差等缺点。本发明生产方法简单，制备出的微硅粉改性尼龙复合材料强度和韧性得到了大幅提高，通过填充微硅粉，降低了生产成本，改善了尼龙材料的抗蠕变性能和耐热性能，微硅粉改性尼龙复合材料综合性能优良，可进行连续生产。采用微硅粉作为一种填料添加到尼龙材料中，可以减轻工业废物微硅粉对环境的压力，能达到变废为宝的目的。本发明可广泛的应用于建材、家电、建筑及土工材料等领域，综合性能较好，具有一定的市场竞争力。
具体实施方式
本发明的实施例1：微硅粉增强尼龙材料，按重量份数计算，包括70份尼龙、25份微硅粉、1.75份表面改性剂、0.25份抗氧化剂以及3份抗老化剂；表面改性剂为钛酸酯偶联剂；抗氧化剂为对苯二胺；抗老化剂为纳米二氧化钛。
微硅粉增强尼龙材料的制备方法，按上述重量份数取各组分，将微硅粉与表面改性剂进行混合，混合温度为50℃，混合2h后，获得改性的微硅粉；将改性的微硅在温度为100℃的条件下真空干燥6h，获得干燥的改性微硅粉；将干燥的改性微硅粉与尼龙及抗氧化剂充分混合均匀后，加入挤出机熔融挤出造粒并干燥后，获得微硅粉改性尼龙母粒；挤出机螺杆的转速为200rpm及挤出温度分别为一区240℃、二区250℃、三区260℃、四区270℃、五区270℃、机头260℃。
将干燥的改性微硅粉与尼龙及抗氧化剂进行混合时，同时还加入3份抗老化剂。
实验结果表明：纯尼龙材料冲击强度为31.5kJ/m2，抗拉强度为56.5MPa，添加25份微硅粉后，复合材料的冲击强度提高43.8%，抗拉强度增加32.3%。
本发明的实施例2：微硅粉增强尼龙材料，按重量份数计算，包括80份尼龙、15份微硅粉、0.75份表面改性剂、0.25份抗氧化剂以及4份抗老化剂；表面改性剂为硅烷偶联剂；抗氧化剂为对苯二酚；抗老化剂为纳米二氧化钛。
制备方法同实施例1。
实验结果表明：纯尼龙材料冲击强度为31.5kJ/m2，抗拉强度为56.5MPa，添加15份微硅粉后，复合材料的冲击强度提高65.7%，抗拉强度增加48.2%。
本发明的实施例3：微硅粉增强尼龙材料，按重量份数计算，包括98份尼龙、1份微硅粉、0.1份表面改性剂、0.5份抗氧化剂以及3.4份抗老化剂；表面改性剂为硬脂酸；抗老化剂为纳米二氧化钛。
实验结果表明：纯尼龙材料冲击强度为31.5kJ/m2，抗拉强度为56.5MPa，添加1份微硅粉后，复合材料的冲击强度提高10.6%，抗拉强度增加19.8%。
本发明的实施例4：微硅粉增强尼龙材料，按重量份数计算，包括60份尼龙、30份微硅粉、1.5份表面改性剂、0.2份抗氧化剂以及3.3份抗老化剂；表面改性剂为等量的硅烷偶联剂、钛酸酯偶联剂或硬脂酸组成；抗老化剂为纳米二氧化钛。
实验结果表明：纯尼龙材料冲击强度为31.5kJ/m2，抗拉强度为56.5MPa，添加1份微硅粉后，复合材料的冲击强度提高38.5%，抗拉强度增加26.7%。

Claims (7)

1.一种微硅粉增强尼龙材料，其特征在于：按重量份数计算，包括40～98份尼龙、1～50份微硅粉、0.1～0.5份抗氧化剂以及0.1～5份表面改性剂。
2.根据权利要求1所述的微硅粉增强尼龙材料，其特征在于：所述的表面改性剂为硅烷偶联剂、钛酸酯偶联剂或硬脂酸中的一种或几种的任意组合。
3.根据权利要求1所述的微硅粉增强尼龙材料，其特征在于：所述的抗氧化剂为对苯二酚或对苯二胺。
4.根据权利要求1所述的微硅粉增强尼龙材料，其特征在于：还包括0.1～5份抗老化剂，抗老化剂为纳米二氧化钛。
5.一种如权利要求1所述的微硅粉增强尼龙材料的制备方法，其特征在于：按上述重量份数取各组分，将微硅粉与表面改性剂进行混合,混合温度为50℃，混合2h后，获得改性的微硅粉；将改性的微硅在温度为100℃的条件下真空干燥6h，，获得干燥的改性微硅粉；将干燥的改性微硅粉与尼龙及抗氧化剂充分混合均匀后，加入挤出机熔融挤出造粒并干燥后，获得微硅粉改性尼龙母粒。
6.根据权利要求5所述的微硅粉增强尼龙材料的制备方法，其特征在于：挤出机螺杆的转速为200rpm及挤出温度分别为一区240℃、二区250℃、三区260℃、四区270℃、五区270℃、机头260℃。
7.根据权利要求5所述的微硅粉增强尼龙材料的制备方法，其特征在于：将干燥的改性微硅粉与尼龙及抗氧化剂进行混合时，同时还加入0.1～5份抗老化剂。
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