CN106188622A - 一种耐磨阻燃的双马来聚酰亚胺改性的碳酸钙填料 - Google Patents
一种耐磨阻燃的双马来聚酰亚胺改性的碳酸钙填料 Download PDFInfo
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Abstract
一种耐磨阻燃的双马来聚酰亚胺改性的碳酸钙填料,由下列重量份原料制成:碳酸钙粉200份、十溴二苯醚4‑5份、三聚氰胺树脂3‑4份、滑石粉3‑4份、氧化镧2‑3份、双氧水80‑100份、聚乙二醇辛基苯基醚6‑8份、过氧化物酶8‑10份、二甲基甲酰胺200‑250份、5‑羟基乙酰丙酸1‑2份、4,4‑二苯基甲烷双马来酰亚胺2‑3份、丙二酸二乙酯2‑3份、催化剂0.5‑1份、十六烷基三甲基溴化铵1‑2份、二氧化钛1‑2份、二甲基二巯基乙酸异辛酯锡2‑3份、木质素磺酸钠2‑3份、羟基硅油2‑3份、丙酮适量、去离子水适量。本发明在碳酸钙表面接枝聚合双马来聚酰亚胺,表面改性均匀,有机化程度高,补强性能好。
Description
技术领域
本发明涉及一种碳酸钙填料,具体涉及一种耐磨阻燃的双马来聚酰亚胺改性的碳酸钙填料。
背景技术
碳酸钙是一类重要的功能性无机填料,具有价格低廉、储量丰富、性能稳定、易加工、无毒等优点,能够显著的改善材料的加工性能、物理性能以及降低生产成本等等,广泛应用于塑料、橡胶、涂料、造纸等领域,由于碳酸钙为亲水性化合物,导致在实际应用中存在与高聚物相容性不足,分散性差等缺陷,不能达到满意的填充补强效果,因此需要对碳酸钙进行改性处理,以提高其在各类材料中分散性和相容性,以达到改善产品性能的功效。
专利CN1400167A公开的一种表面改性纳米碳酸钙的制备方法,采用饱和脂肪酸钠盐作为表面处理剂;专利CN1654551A公开了一种纳米碳酸钙的改性方法,采用双子星表面活性剂二磷酸酯盐作为改性剂;都是在已碳酸化完成的碳酸钙乳液中加入表面处理剂在一定温度、浓度和比例下液相活化反应而得。此种方法得到的碳酸钙填料虽然分散性得到了提高,但是应用性能任然没得到改善。
发明内容
本发明的目的在于,提供一种耐磨阻燃的双马来聚酰亚胺改性的碳酸钙填料,为了实现上述目的,本发明采用的技术方案如下:
一种耐磨阻燃的双马来聚酰亚胺改性的碳酸钙填料,其特征在于,所述的碳酸钙由下列重量份的原料制成:碳酸钙粉200份、十溴二苯醚4-5份、三聚氰胺树脂3-4份、滑石粉3-4份、氧化镧2-3份、双氧水80-100份、过氧化物酶8-10份、聚乙二醇辛基苯基醚6-8份、二甲基甲酰胺200-250份、5-羟基乙酰丙酸1-2份、4,4-二苯基甲烷双马来酰亚胺2-3份、丙二酸二乙酯2-3份、催化剂0.5-1份、十六烷基三甲基溴化铵1-2份、二氧化钛1-2份、二甲基二巯基乙酸异辛酯锡2-3份、木质素磺酸钠2-3份、羟基硅油2-3份、丙酮适量、去离子水适量。
所述的耐磨阻燃的双马来聚酰亚胺改性的碳酸钙填料,其特征在于,所述的碳酸钙由如下步骤制备而成:
(1)将木质素磺酸钠溶入去离子水中,搅拌均匀后加入碳酸钙粉、三聚氰胺树脂、滑石粉、氧化镧,在3000-4000转/min下搅拌5-10min,70-100℃烘干,研磨15-20min,过150-200目筛,得到混合物料;
(2)将过氧化物酶、双氧水、聚乙二醇辛基苯基醚和步骤(1)所得的混合料混合均匀,30-40℃恒温搅拌30-40min,在其表面引入活性羟基,得到异化的活性羟基混合料;
(3)将活性羟基混合料超声分散在二甲基甲酰胺中,再加入5-羟基乙酰丙酸、4,4-二苯基甲烷双马来酰亚胺、丙二酸二乙酯、催化剂,70-80℃搅拌反应8-10h,得到双马来聚酰亚胺预聚物-碳酸钙;
(4)将其它剩余成分加入步骤(3)得到的双马来聚酰亚胺预聚物-碳酸钙中,超声2-3h,过滤,分别用去离子水、丙酮洗涤2-3次,50-60℃烘干,研磨20-30min,过150-200目筛,得到一种耐磨阻燃的双马来聚酰亚胺改性的碳酸钙填料。
所述的催化剂为(i)(IV)族金属的茂金属络合物,所述茂金属包含至少两个环戊二烯基型配体。
本发明的有益效果为:利用在碳酸钙表面接枝聚合双马来聚酰亚胺对碳酸钙进行改性处理,使得碳酸钙的性能发生改变,粉体的吸油值、粘度、活化率等性能指标均发生变化,更利于其在高分子聚合物中分散和相容,从而达到良好的填充补强效果,十溴二苯醚还增加了能够增加PVC的阻燃性能,三聚氰胺树脂、滑石粉、氧化镧等原料能够增加PVC的耐磨性能,极具应用价值。
具体实施例
本实施例的耐磨阻燃的双马来聚酰亚胺改性的碳酸钙填料,由下列重量份的原料制成:碳酸钙粉200份、十溴二苯醚5份、三聚氰胺树脂3份、滑石粉3份、氧化镧3份、双氧水100份、过氧化物酶10份、聚乙二醇辛基苯基醚8份、二甲基甲酰胺250份、5-羟基乙酰丙酸2份、4,4-二苯基甲烷双马来酰亚胺3份、丙二酸二乙酯3份、催化剂1份、十六烷基三甲基溴化铵2份、二氧化钛2份、二甲基二巯基乙酸异辛酯锡3份、木质素磺酸钠3份、羟基硅油3份、丙酮适量、去离子水适量。
一种耐磨阻燃的双马来聚酰亚胺改性的碳酸钙填料,由如下步骤制备而成:
(1)将木质素磺酸钠溶入去离子水中,搅拌均匀后加入碳酸钙粉、三聚氰胺树脂、滑石粉、氧化镧,在3500转/min下搅拌10min,80℃烘干,研磨20min,过200目筛,得到混合物料;
(2)将过氧化物酶、双氧水、聚乙二醇辛基苯基醚和步骤(1)所得的混合料混合均匀,35℃恒温搅拌40min,在其表面引入活性羟基,得到异化的活性羟基混合料;
(3)将活性羟基混合料超声分散在二甲基甲酰胺中,再加入5-羟基乙酰丙酸、4,4-二苯基甲烷双马来酰亚胺、丙二酸二乙酯、催化剂,80℃搅拌反应10h,得到双马来聚酰亚胺预聚物-碳酸钙;
(4)将其它剩余成分加入步骤(3)得到的双马来聚酰亚胺预聚物-碳酸钙中,超声2h,过滤,分别用去离子水、丙酮洗涤3次,60℃烘干,研磨30min,过200目筛,得到一种耐磨阻燃的双马来聚酰亚胺改性的碳酸钙填料。
本发明的耐磨阻燃的双马来聚酰亚胺改性的碳酸钙填料的真密度为1.2-1.6g/cm3,堆积密度为0.14-0.24g/cm3,平均粒径小于等于6μm,比表面积80-170㎡/g,白度为90-95%。
Claims (3)
1.一种耐磨阻燃的双马来聚酰亚胺改性的碳酸钙填料,其特征在于,所述的碳酸钙由下列重量份的原料制成:碳酸钙粉200份、十溴二苯醚4-5份、三聚氰胺树脂3-4份、滑石粉3-4份、氧化镧2-3份、双氧水80-100份、过氧化物酶8-10份、聚乙二醇辛基苯基醚6-8份、二甲基甲酰胺200-250份、5-羟基乙酰丙酸1-2份、4,4-二苯基甲烷双马来酰亚胺2-3份、丙二酸二乙酯2-3份、催化剂0.5-1份、十六烷基三甲基溴化铵1-2份、二氧化钛1-2份、二甲基二巯基乙酸异辛酯锡2-3份、木质素磺酸钠2-3份、羟基硅油2-3份、丙酮适量、去离子水适量。
2.根据权利要求1中所述的耐磨阻燃的双马来聚酰亚胺改性的碳酸钙填料,其特征在于,所述的碳酸钙由如下步骤制备而成:
(1)将木质素磺酸钠溶入去离子水中,搅拌均匀后加入碳酸钙粉、三聚氰胺树脂、滑石粉、氧化镧,在3000-4000转/min下搅拌5-10min,70-100℃烘干,研磨15-20min,过150-200目筛,得到混合物料;
(2)将过氧化物酶、双氧水、聚乙二醇辛基苯基醚和步骤(1)所得的混合料混合均匀,30-40℃恒温搅拌30-40min,在其表面引入活性羟基,得到异化的活性羟基混合料;
(3)将活性羟基混合料超声分散在二甲基甲酰胺中,再加入5-羟基乙酰丙酸、4,4-二苯基甲烷双马来酰亚胺、丙二酸二乙酯、催化剂,70-80℃搅拌反应8-10h,得到双马来聚酰亚胺预聚物-碳酸钙;
(5)将其它剩余成分加入步骤(3)得到的双马来聚酰亚胺预聚物-碳酸钙中,超声2-3h,过滤,分别用去离子水、丙酮洗涤2-3次,50-60℃烘干,研磨20-30min,过150-200目筛,得到一种耐磨阻燃的双马来聚酰亚胺改性的碳酸钙填料。
3.根据权利要求2中所述的耐磨阻燃的双马来聚酰亚胺改性的碳酸钙填料的制备方法,其特征在于,所述的催化剂为(i)(IV)族金属的茂金属络合物,所述茂金属包含至少两个环戊二烯基型配体。
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CN111662572A (zh) * | 2020-06-19 | 2020-09-15 | 安徽雪城超细碳酸钙有限公司 | 一种提高耐磨性的碳酸钙填料及其制备方法 |
CN115570858A (zh) * | 2022-08-26 | 2023-01-06 | 浙江国泰萧星密封材料股份有限公司 | 一种耐高温复合垫片及其制备方法 |
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