CN106752094A - 一种含硼酸酯的二氧化钛包覆碳酸钙无机填料及其制备方法 - Google Patents

一种含硼酸酯的二氧化钛包覆碳酸钙无机填料及其制备方法 Download PDF

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CN106752094A
CN106752094A CN201610914014.3A CN201610914014A CN106752094A CN 106752094 A CN106752094 A CN 106752094A CN 201610914014 A CN201610914014 A CN 201610914014A CN 106752094 A CN106752094 A CN 106752094A
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王文杰
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Abstract

本发明公开了一种含硼酸酯的二氧化钛包覆碳酸钙无机填料及其制备方法，其特征在于，由以下重量份的原料制成：硼酸酯2‑4，氧化钙40‑50，海泡石1‑2，CO2适量，乙酰丙酮5‑10，硬脂酸钠6‑12，钛酸丁酯15‑25，氯化钙1‑3，聚乙烯树脂25‑35，二甲基硅油8‑12，去离子水200‑250。本发明利用二氧化钛和聚乙烯树脂对碳酸钙粉体进行双重包覆，不仅增强了碳酸钙粉体的耐酸度、白度和耐火性能，同时改善了其与有机基底的融合性，使其满足更广泛的应用要求；配合添加的硼酸酯，增强了纳米碳酸钙的亲油性。

Description

一种含硼酸酯的二氧化钛包覆碳酸钙无机填料及其制备方法
技术领域
本发明涉及一种复合改性碳酸钙粉体及其制备，尤其涉及一种含硼酸酯的二氧化钛包覆碳酸钙无机填料及其制备方法。
背景技术
粉体的表面改性处理就是根据粉体材料应用的需要，利用物理、化学、机械等方法有目的地改变粉体材料表面的物理化学性质，如表面组成、结构和官能团、表面能、表面润湿性、电性、光性、吸附和反应特性等等，以满足现代材料和新技术发展的需要。在塑料、人造大理石等高分子材料工业及高聚物基复合材料应用领域中，碳酸钙粉体填料占有很重要的地位。碳酸钙填料不仅可以减低材料的生产成本，还能提高材料的硬度、刚性或尺寸稳定性，改善材料的力学性能并赋予材料某些特殊的物理化学性能，如耐腐蚀性、耐候性、阻燃性和绝缘性等。但由于碳酸钙填料与基质，即有机高聚物的表面或界面性质不同，相容性较差，因而,难以在基质中均匀分散，直接或过多地填充往往容易导致材料的某些力学性能下降以及易脆化等缺点。因此，除了对碳酸钙填料的粒度和粒度分布的要求之外，还必须对其表面进行改性，以改善其表面的物理化学特性，增强其与有机聚合物或树脂等基体的相容性和在有机基体中的分散性，以提高材料的机械性能及综合性能。
段好在其硕士学位论文《超细碳酸钙粉体的干法表面改性研究》中，利用油酸-马来酸酐复合改性剂对碳酸钙粉体进行改性，但是当碳酸钙作为塑料、涂料等填料时，还存在着耐酸度不佳，与有机基底的融合性欠缺等缺点。
发明内容
基于以上的思考，本发明旨在提供一种复合改性碳酸钙无机填料及其制备方法，用以解决当碳酸钙作为塑料、涂料等填料时，存在的耐酸度不佳，与有机基底的融合性欠缺等缺点。
本发明所要解决的技术问题采用以下的技术方案来实现 ：
一种含硼酸酯的二氧化钛包覆碳酸钙无机填料，其特征在于，由以下重量份的原料制成：
硼酸酯2-4，氧化钙40-50，海泡石1-2，CO2适量，乙酰丙酮5-10，硬脂酸钠6-12，钛酸丁酯15-25，氯化钙1-3，聚乙烯树脂25-35，二甲基硅油8-12，去离子水200-250。
所述的一种含硼酸酯的二氧化钛包覆碳酸钙无机填料及其制备方法，其特征在于，由以下步骤制成：
a. 将氧化钙固体粉碎成粉末状，加入去离子水，60-100℃下搅拌反应2-3h，反应后的浆液陈化1-3h后，将浆液转入到碳化反应釜中，CO2和空气通过转子流量计计量后混合，通入碳化反应釜底部的气体分布器；当 pH＜7 时，结束反应，得碳酸钙浆液；
b. 70-90℃下，向步骤a所得碳酸钙浆液中加入硼酸酯、海泡石、乙酰丙酮、硬脂酸钠，在研磨机中研磨搅拌均匀后，边研磨边缓慢滴加钛酸丁酯，结束后继续研磨0.5-1h，钛酸丁酯在乙酰丙酮的作用下，水解生成二氧化钛微粒，并在硬脂酸钠的活化作用下，包覆在碳酸钙、海泡石颗粒表面；对已包覆二氧化钛微粒的碳酸钙、海泡石粉进行过滤，烘干，然后粉碎，得混合物；
c. 将步骤b所得混合物投入高速混料机中，加入聚乙烯树脂、氯化钙、二甲基硅油，搅拌升温至90-110℃，保温搅拌10-30min后，经双螺杆挤出机挤出造粒即可。
所述的一种含硼酸酯的二氧化钛包覆碳酸钙无机填料及其制备方法，其特征在于，步骤a中CO2流量为0.04-0.40L/g(CaO)·min，反应温度为15-45℃。
本发明的有益效果是：钛酸丁酯在乙酰丙酮的作用下，水解生成二氧化钛微粒，并在硬脂酸钠的活化作用下，包覆在碳酸钙颗粒表面，增强了碳酸钙粉体的耐酸度、白度和耐火性能，使其满足更广泛的应用要求；之后再用聚乙烯对包覆二氧化钛的碳酸钙粉体进行再次包覆，将所得粉体亲水的特性转变为亲油性，促进了其与有机基底的融合，使所得碳酸钙粉体能更好的应用到塑料、涂料等领域；其间加入的二甲基硅油，防止碳酸钙之间的团聚，同时促进了碳酸钙在聚乙烯树脂中的分散，使其包裹的更加均匀；配合添加的硼酸酯，增强了纳米碳酸钙的亲油性。
具体实施方式
下面结合实施例， 对本发明的具体实施方式作进一步描述。
实施例
一种含硼酸酯的二氧化钛包覆碳酸钙无机填料，其特征在于，由以下重量份的原料制成：
硼酸酯4，氧化钙50，海泡石2，CO2适量，乙酰丙酮10，硬脂酸钠12，钛酸丁酯25，氯化钙3，聚乙烯树脂35，二甲基硅油12，去离子水250。
所述的一种含硼酸酯的二氧化钛包覆碳酸钙无机填料及其制备方法，其特征在于，由以下步骤制成：
a. 将氧化钙固体粉碎成粉末状，加入去离子水，60-100℃下搅拌反应2-3h，反应后的浆液陈化1-3h后，将浆液转入到碳化反应釜中，CO2和空气通过转子流量计计量后混合，通入碳化反应釜底部的气体分布器；当 pH＜7 时，结束反应，得碳酸钙浆液；
b. 70-90℃下，向步骤a所得碳酸钙浆液中加入硼酸酯、海泡石、乙酰丙酮、硬脂酸钠，在研磨机中研磨搅拌均匀后，边研磨边缓慢滴加钛酸丁酯，结束后继续研磨0.5-1h，钛酸丁酯在乙酰丙酮的作用下，水解生成二氧化钛微粒，并在硬脂酸钠的活化作用下，包覆在碳酸钙、海泡石颗粒表面；对已包覆二氧化钛微粒的碳酸钙、海泡石粉进行过滤，烘干，然后粉碎，得混合物；
c. 将步骤b所得混合物投入高速混料机中，加入聚乙烯树脂、氯化钙、二甲基硅油，搅拌升温至90-110℃，保温搅拌10-30min后，经双螺杆挤出机挤出造粒即可。
所述的一种含硼酸酯的二氧化钛包覆碳酸钙无机填料及其制备方法，其特征在于，步骤a中CO2流量为0.04-0.40L/g(CaO)·min，反应温度为15-45℃。
本发明的技术参数为：活化度≥90%；吸油值≥0.25mL/g。

Claims (3)

1.一种含硼酸酯的二氧化钛包覆碳酸钙无机填料，其特征在于，由以下重量份的原料制成：
硼酸酯2-4，氧化钙40-50，海泡石1-2，CO2适量，乙酰丙酮5-10，硬脂酸钠6-12，钛酸丁酯15-25，氯化钙1-3，聚乙烯树脂25-35，二甲基硅油8-12，去离子水200-250。
2.根据权利要求1所述的一种含硼酸酯的二氧化钛包覆碳酸钙无机填料及其制备方法，其特征在于，由以下步骤制成：
a. 将氧化钙固体粉碎成粉末状，加入去离子水，60-100℃下搅拌反应2-3h，反应后的浆液陈化1-3h后，将浆液转入到碳化反应釜中，CO2和空气通过转子流量计计量后混合，通入碳化反应釜底部的气体分布器；当 pH＜7 时，结束反应，得碳酸钙浆液；
b. 70-90℃下，向步骤a所得碳酸钙浆液中加入硼酸酯、海泡石、乙酰丙酮、硬脂酸钠，在研磨机中研磨搅拌均匀后，边研磨边缓慢滴加钛酸丁酯，结束后继续研磨0.5-1h，钛酸丁酯在乙酰丙酮的作用下，水解生成二氧化钛微粒，并在硬脂酸钠的活化作用下，包覆在碳酸钙、海泡石颗粒表面；对已包覆二氧化钛微粒的碳酸钙、海泡石粉进行过滤，烘干，然后粉碎，得混合物；
c. 将步骤b所得混合物投入高速混料机中，加入聚乙烯树脂、氯化钙、二甲基硅油，搅拌升温至90-110℃，保温搅拌10-30min后，经双螺杆挤出机挤出造粒即可。
3.根据权利要求2所述的一种含硼酸酯的二氧化钛包覆碳酸钙无机填料及其制备方法，其特征在于，步骤a中CO2流量为0.04-0.40L/g(CaO)·min，反应温度为15-45℃。
CN201610914014.3A 2016-10-20 2016-10-20 一种含硼酸酯的二氧化钛包覆碳酸钙无机填料及其制备方法 Pending CN106752094A (zh)

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