CN106146887A - 一种耐氧化的双马来聚酰亚胺改性的碳酸钙填料 - Google Patents
一种耐氧化的双马来聚酰亚胺改性的碳酸钙填料 Download PDFInfo
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Abstract
一种耐氧化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、聚乙烯醇超细粉末3‑4份、丁基羟基茴香醚4‑5份、二丁基羟基甲苯3‑5份、石墨烯1‑2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、三聚磷酸钠3‑7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。本发明填料具有优异的耐氧化性能,能够增强塑料的耐氧化和耐候性能。
Description
技术领域
本发明涉及一种碳酸钙填料,具体涉及一种耐氧化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,提供一种耐氧化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:
一种耐氧化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、聚乙烯醇超细粉末3-4份、丁基羟基茴香醚4-5份、二丁基羟基甲苯3-5份、石墨烯1-2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、三聚磷酸钠3-7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。
所述的耐氧化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)碳酸钙粉、聚乙烯醇超细粉末、石墨烯研磨15-20min,过150-200目筛,得到混合料;
(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)将丁基羟基茴香醚、二丁基羟基甲苯、三聚磷酸钠加入步骤(3)得到的双马来聚酰亚胺预聚物-碳酸钙中,40-50℃搅拌10-20min作抗氧化处理,得到抗氧化的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(4)得到的抗氧化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,得到一种耐氧化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,丁基羟基茴香醚、二丁基羟基甲苯、三聚磷酸钠等原料还增加PVC的耐氧化性能和耐候性能,极具应用价值。
具体实施例
本实施例的耐氧化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、聚乙烯醇超细粉末4份、丁基羟基茴香醚4份、二丁基羟基甲苯3份、石墨烯2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0.5份、十六烷基三甲基溴化铵2份、二氧化钛2份、三聚磷酸钠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。
一种耐氧化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)碳酸钙粉、聚乙烯醇超细粉末、石墨烯研磨20min,过200目筛,得到混合料;
(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8h,得到双马来聚酰亚胺预聚物-碳酸钙;
(4)将丁基羟基茴香醚、二丁基羟基甲苯、三聚磷酸钠加入步骤(3)得到的双马来聚酰亚胺预聚物-碳酸钙中,40℃搅拌20min作抗氧化处理,得到抗氧化的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(4)得到的抗氧化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,得到一种耐氧化的双马来聚酰亚胺改性的碳酸钙填料。
本发明的耐氧化的双马来聚酰亚胺改性的碳酸钙填料的真密度为1.1-1.5g/cm3,堆积密度为0.13-0.24g/cm3,平均粒径小于等于6μm,比表面积80-170㎡/g,白度为90-95%。
Claims (3)
1.一种耐氧化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、聚乙烯醇超细粉末3-4份、丁基羟基茴香醚4-5份、二丁基羟基甲苯3-5份、石墨烯1-2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、三聚磷酸钠3-7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中所述的耐氧化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)碳酸钙粉、聚乙烯醇超细粉末、石墨烯研磨15-20min,过150-200目筛,得到混合料;
(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)将丁基羟基茴香醚、二丁基羟基甲苯、三聚磷酸钠加入步骤(3)得到的双马来聚酰亚胺预聚物-碳酸钙中,40-50℃搅拌10-20min作抗氧化处理,得到抗氧化的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(4)得到的抗氧化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,得到一种耐氧化的双马来聚酰亚胺改性的碳酸钙填料。
3.根据权利要求2中所述的耐氧化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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Cited By (3)
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CN106674609A (zh) * | 2016-12-16 | 2017-05-17 | 安徽北马科技有限公司 | 一种高分散性的双马来聚酰亚胺改性的碳酸钙填料 |
CN106752105A (zh) * | 2016-12-16 | 2017-05-31 | 安徽北马科技有限公司 | 一种二氧化钛包覆的双马来聚酰亚胺改性的碳酸钙填料 |
CN106833025A (zh) * | 2016-12-16 | 2017-06-13 | 安徽北马科技有限公司 | 一种高强度的双马来聚酰亚胺改性的碳酸钙填料 |
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CN106833025A (zh) * | 2016-12-16 | 2017-06-13 | 安徽北马科技有限公司 | 一种高强度的双马来聚酰亚胺改性的碳酸钙填料 |
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