CN106317457A - 功能性填料及其制备方法 - Google Patents
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Abstract
本发明公开了一种功能性填料及其制备方法,所述功能性填料包括按重量份计的以下组分:有机酸钙盐40%‑95%,无机填料5%‑60%。所述功能性填料的制备方法包括如下步骤:(1)将所选填料加入可溶性有机酸盐溶液中,升至合适温度后,继续搅拌10‑30min;(2)在步骤(1)得到的混合液中加入可溶性表面活性剂和可溶性偶联剂,继续搅拌15‑40min;(3)在步骤(2)得到的混合液中快速加入可溶性钙盐溶液,继续搅拌20‑90min;(4)采用研磨机对步骤(3)得到的混合物进行细化处理,当物料的D90小于2μm时,过滤、洗涤、烘干,即得目标产品。本发明制备工艺简单易行,所制备的产品主要用于性能要求较高的材料中,不仅能提高制品的机械强度,还能改善耐热性能。
Description
技术领域
本发明涉及材料领域,具体涉及一种功能性填料及其制备方法。
背景技术
在高分子化工中,填料(填充剂)是用量最大的添加剂,几乎所有的塑料(包括热塑性和热固性塑料)、天然橡胶和涂料都填充大量的无机粉体,在改善性能的同时,还能降低配方成本。但无机粉体与高分子材料表面性能的差异,导致二者相容性,加工分散较为困难,而且所制备制品的性能差,难以达到较理想的效果。采用表面改性的方式可以在一定程度上改善无机粉体在高分子材料中的应用效果,较普遍的表面改性方式是对粉体进行后续的干法改性或者是经湿法改性后再烘干。干法改性相对湿法改性简单易行,但均匀性和应用效果往往较湿法改性差些;湿法改性效果更好,但工艺繁琐,一定程度上也增加了粉体生产的隐性成本。
发明内容
本发明的目的是提供一种分散性、与高分子材料相容性好的功能性填料及其制备方法,该制备工艺简单易行,且无须后续的专门改性环节,所制备的功能性填料主要用于性能要求较高的材料中,不仅能提高制品的机械强度,还能改善耐热性能。
为了实现上述目的,本发明通过如下技术方案实现:本发明的一种功能性填料,所述功能性填料包括按重量份计的以下组分:
有机酸钙盐40%-95%,无机填料5%-60%。
本发明所述的功能性填料的制备方法,包括以下步骤:
(1)将无机填料加入可溶性有机酸盐溶液中,加热至合适的温度后,继续搅拌10-30min;
(2)在步骤(1)得到的混合液中加入可溶性表面活性剂和可溶性偶联剂,继续搅拌15-40min;
(3)在步骤(2)得到的混合液中快速加入可溶性钙盐溶液,继续搅拌20-90min;
(4)采用研磨机对步骤(3)得到的混合物进行细化处理,当物料的D90小于2μm时,过滤、洗涤、烘干,即得目标产品。
进一步地,步骤(1)中所述的无机填料优选于陶土、滑石粉、碳酸钙、硫酸钙、硫酸钡中的一种或多种的组合物;
步骤(1)中所述的可溶性有机酸盐溶液优选于有机酸钠溶液或有机酸钾溶液中的一种,且其中溶质的重量百分含量为5%-15%;
步骤(1)中所述的温度为30-80℃;
步骤(2)中所述的可溶性表面活性剂优选于油酸钠、十二烷基苯磺酸钠、椰子油酸钠、十二烷基硫酸钠、硬质酸钠中的一种或多种的组合物,且其用量占有机酸钙盐的重量百分含量为0.5%-1.5%;可溶性偶联剂优选于硅烷偶联剂KH-560、螯合型钛酸酯偶联剂KR-238s中的一种,且其用量占有机酸钙盐的重量百分含量为0.5%-2%;
步骤(3)中,所述的可溶性钙盐优选于氯化钙或硝酸钙中的一种,且其溶液中溶质的重量百分含量为15%-40%,可溶性钙盐与可溶性有机酸盐的摩尔比按照化学方程式的系数确定。
更进一步地,步骤(1)中所述的有机酸盐为含双键或苯环的羧酸盐,优选于丁烯二酸盐、富马酸盐、丙烯酸盐、甲基丙烯酸盐、柠檬酸盐、邻苯二甲酸盐、苯甲酸盐中的一种或多种的组合物。
有益效果:本发明通过简单、易行的方法制备得到一种功能性填料。反应过程中,无机填料的引入,起到异相成核的作用,有机酸钙盐包裹在无机填料表面。有机酸钙盐与高聚物之间有接枝共聚的化学结合,结构稳定,与高聚物间有良好的相容性;经过湿法研磨将颗粒磨细,同时添加了表面活性剂和偶联剂,改善表界面结构,提高粒子与聚合物分子间的有效结合,分散性好,在使用过程中可改善材料的力学性能、耐热性能等,是一种多功能性的填料。
具体实施方式
以下通过实施例进一步说明本发明。应该理解的是,这些实施例是本发明的阐释和举例,并不以任何形式限制本发明的范围。
实施例1:
本发明的一种功能性填料,所述功能性填料包括按重量份计的以下组分:
柠檬酸钙95%,碳酸钙5%。
本发明所述的功能性填料的制备方法,包括如下步骤:
(1)将碳酸钙加入柠檬酸钠溶液中,加热至30℃,继续搅拌10min,其中柠檬酸钠溶液中溶质的重量百分含量为5%;
(2)在步骤(1)得到的混合液中加入油酸钠和螯合型钛酸酯偶联剂KR-238s,继续搅拌15min,所用油酸钠和KR-238s的量分别占有机酸钙盐的重量百分含量为0.5%和2%;
(3)在步骤(2)得到的混合液中快速加入溶质重量百分含量为15%的氯化钙溶液,继续搅拌20min;
(4)采用研磨机对步骤(3)得到的混合物进行细化处理,当物料的D90小于2μm时,过滤、洗涤、烘干,即得目标产品1#。
实施例2:
本发明的一种功能性填料,所述功能性填料包括按重量份计的以下组分:
丁烯二酸钙35%,甲基丙烯酸钙33%,硫酸钙12%,硫酸钡20%。
本发明所述的功能性填料的制备方法,包括如下步骤:
(1)将硫酸钙和硫酸钡加入丁烯二酸钾和甲基丙烯酸钾的混合溶液中,加热至80℃,继续搅拌30min,其中混合溶液中丁烯二酸钾和甲基丙烯酸钾的总重量百分含量为15%;
(2)在步骤(1)得到的混合液中添加硬质酸钠和硅烷偶联剂KH-560,继续搅拌40min,所用硬质酸钠和硅烷偶联剂的量分别占有机酸钙盐的重量百分含量为1.5%和0.5%;
(3)在步骤(2)得到的混合液中快速加入溶质重量百分含量为40%的硝酸溶液,继续搅拌90min;
(4)采用研磨机对步骤(3)得到的混合物进行细化处理,当物料的D90小于2μm时,过滤、洗涤、烘干,即得目标产品2#。
实施例3:
本发明的一种功能性填料,所述功能性填料包括按重量份计的以下组分:
富马酸钙20%,丙烯酸钙20%,水滑石60%。
本发明所述的功能性填料的制备方法,包括如下步骤:
(1)将水滑石加入富马酸钠和丙烯酸钠的混合溶液中,加热至50℃,继续搅拌20min,其中混合溶液中富马酸钠和丙烯酸钠的总重量百分含量为10%;
(2)在步骤(1)得到的混合液中添加十二烷基苯磺酸钠和螯合型钛酸酯偶联剂KR-238s,继续搅拌25min,所用十二烷基苯磺酸钠和KR-238s的量分别占有机酸钙盐的重量百分含量为1.0%和1.2%;
(3)在步骤(2)得到的混合液中快速加入溶质重量百分含量为30%氯化钙溶液,继续搅拌50min;
(4)采用研磨机对步骤(3)得到的混合物进行细化处理,当物料的D90小于2μm时,过滤、洗涤、烘干,即得目标产品3#。
试验1
比较功能性填料1#、2#、3#与不同碳酸钙的分散性,通过旋转粘度仪测定的粘度进行比较,粘度越小,分散性越好。试验方法:取样品:液体石蜡为1:4在烧杯中预混合,再超声10min,同一温度下测定其粘度,测得数据如表1所示。
表1:
通过表1中粘度数据的比较可知:本发明制备的功能性填料分散性比轻质碳酸钙和纳米碳酸钙的好,且随着有机酸钙含量的增加,分散性更好。
试验2
采用配方(按重量份计):CPVC 50份、PVC 50份、有机锡稳定剂 2份、硬脂酸钙1.0-1.5份、58号精炼石蜡1份、PA20 1份、填料(变品种)20份。在高速搅拌机中混合均匀,用双辊开炼机将干混料塑化,工艺参数为前辊温度180-190℃、转速35r/min,后辊温度175-185℃、转速30r/min,开炼时间5min。开炼结束后,于180-190℃平板硫化机上压片。按国家标准进行测试,所得性能如表2所示。
表2:
从表2的数据比较中看出,添加本发明制备的功能性填料后,材料具有优异的力学性能和良好的耐热性。
以上所述依据本发明的理想实施例为启示,通过上述的说明内容,相关工作人员完全可以在不偏离本想发明技术思想的范围内,进行多样的变更以及修改。本项发明的技术性范围并不局限于说明书上的内容,必须要根据权利要求范围来确定其技术性范围。
Claims (8)
1.一种功能性填料,其特征在于,所述功能性填料包括按重量份计的以下组分:有机酸钙盐40%-95%,无机填料5%-60%。
2.权利要求1所述的功能性填料的制备方法,其特征在于包括如下步骤:
(1)将无机填料加入可溶性有机酸盐溶液中,加热至合适的温度后,继续搅拌10-30min;
(2)在步骤(1)得到的混合液中加入可溶性表面活性剂和可溶性偶联剂,继续搅拌15-40min;
(3)在步骤(2)得到的混合液中快速加入可溶性钙盐溶液,继续搅拌20-90min;
(4)采用研磨机对步骤(3)得到的混合物进行细化处理,当物料的D90小于2μm时,过滤、洗涤、烘干,即得目标产品。
3.根据权利要求2所述的功能性填料的制备方法,其特征在于:步骤(1)中所述的可溶性有机酸盐溶液优选于有机酸钠或有机酸钾溶液中的一种,且其中溶质的重量百分含量为5%-15%。
4.根据权利要求2或3所述的功能性填料的制备方法,其特征在于:所述的有机酸盐为含双键或苯环的羧酸盐,优选于丁烯二酸盐、富马酸盐、丙烯酸盐、甲基丙烯酸盐、柠檬酸盐、邻苯二甲酸盐、苯甲酸盐中的一种或多种的组合物。
5.根据权利要求2所述的功能性填料的制备方法,其特征在于:步骤(1)中所述的无机填料优选于陶土、滑石粉、碳酸钙、硫酸钙、硫酸钡中的一种或多种的组合物。
6.根据权利要求2所述的功能性填料的制备方法,其特征在于:步骤(1)中所述的温度为30-80℃。
7.根据权利要求2所述的功能性填料的制备方法,其特征在于:步骤(2)中所述的可溶性表面活性剂优选于油酸钠、十二烷基苯磺酸钠、椰子油酸钠、十二烷基硫酸钠、硬质酸钠中的一种或多种的组合物,且其用量占有机酸钙盐的重量百分含量为0.5%-1.5%;可溶性偶联剂优选于硅烷偶联剂KH-560、螯合型钛酸酯偶联剂KR-238s中的一种,且其用量占有机酸钙盐的重量百分含量为0.5%-2%。
8.根据权利要求2所述的功能性填料的制备方法,其特征在于:步骤(3)中所述的可溶性钙盐优选于氯化钙或硝酸钙中的一种,且其溶液中溶质的重量百分含量为15%-40%,可溶性钙盐与可溶性有机酸盐的摩尔比按照化学方程式的系数确定。
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