CN106566284A - 一种阻燃的二氧化钛、聚乙烯双重包覆碳酸钙无机填料及其制备方法 - Google Patents

一种阻燃的二氧化钛、聚乙烯双重包覆碳酸钙无机填料及其制备方法 Download PDF

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CN106566284A
CN106566284A CN201610911113.6A CN201610911113A CN106566284A CN 106566284 A CN106566284 A CN 106566284A CN 201610911113 A CN201610911113 A CN 201610911113A CN 106566284 A CN106566284 A CN 106566284A
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陈永忠
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QINGYANG HENGYUAN CHEMICAL MATERIALS Co Ltd
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Abstract

本发明公开了一种阻燃的二氧化钛、聚乙烯双重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：氢氧化铝2‑3，氧化钙40‑50，硼砂1‑2，CO2适量，乙酰丙酮5‑10，硬脂酸钠6‑12，钛酸丁酯15‑25，纳米二氧化硅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；氢氧化铝、硼砂等原料的添加，使该改性碳酸钙粉体具备良好的阻燃耐火效果。

Description

一种阻燃的二氧化钛、聚乙烯双重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，尤其涉及一种阻燃的二氧化钛、聚乙烯双重包覆碳酸钙无机填料及其制备方法。
背景技术
碳酸钙（包括重钙和轻钙）具有原料易得，价格低廉，稳定性好，色泽单纯，无毒等诸多优点，而被广泛用于塑料，橡胶，造纸，油墨，建材，电线电缆等领域，成为用量最大的填充材料。但由于碳酸钙属无机粉体，粒子表面是亲水疏油的，呈强极性，在有机介质中难以分散均匀，与基材之间结合力低，在受外力冲击时，易造成界面缺陷，导致材料性能下降。纳米级的碳酸钙粉末，表面能高，吸附作用越强，粒子互相团聚，无法在聚合物基体中很好分散，从而影响其使用的实际效果。因此，只有对碳酸钙进行改性才能获得高性能且满足实际应用的功能性改性填充专用料。
梁锦在其硕士学位论文《纳米碳酸钙的制备与表面改性研究》中，利用碳化法制备了纳米碳酸钙，并用硬脂酸钠对其进行改性，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 ：
一种阻燃的二氧化钛、聚乙烯双重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：
氢氧化铝2-3，氧化钙40-50，硼砂1-2，CO2适量，乙酰丙酮5-10，硬脂酸钠6-12，钛酸丁酯15-25，纳米二氧化硅1-3，聚乙烯树脂25-35，二甲基硅油8-12，去离子水200-250。
所述的一种阻燃的二氧化钛、聚乙烯双重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乙酰丙酮、纳米二氧化硅、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，二氧化钛和纳米二氧化硅包覆在碳酸钙颗粒表面；对已包覆二氧化钛、纳米二氧化硅微粒的碳酸钙进行过滤，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、硼砂、氢氧化铝、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。
所述的一种阻燃的二氧化钛、聚乙烯双重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；氢氧化铝、硼砂等原料的添加，使该改性碳酸钙粉体具备良好的阻燃耐火效果。
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
一种阻燃的二氧化钛、聚乙烯双重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：
氢氧化铝3，氧化钙40，硼砂2，CO2适量，乙酰丙酮10，硬脂酸钠6，钛酸丁酯25，纳米二氧化硅1，聚乙烯树脂35，二甲基硅油12，去离子水250。
所述的一种阻燃的二氧化钛、聚乙烯双重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乙酰丙酮、纳米二氧化硅、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，二氧化钛和纳米二氧化硅包覆在碳酸钙颗粒表面；对已包覆二氧化钛、纳米二氧化硅微粒的碳酸钙进行过滤，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、硼砂、氢氧化铝、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。
所述的一种阻燃的二氧化钛、聚乙烯双重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)

1.一种阻燃的二氧化钛、聚乙烯双重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：
氢氧化铝2-3，氧化钙40-50，硼砂1-2，CO2适量，乙酰丙酮5-10，硬脂酸钠6-12，钛酸丁酯15-25，纳米二氧化硅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所述的一种阻燃的二氧化钛、聚乙烯双重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乙酰丙酮、纳米二氧化硅、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，二氧化钛和纳米二氧化硅包覆在碳酸钙颗粒表面；对已包覆二氧化钛、纳米二氧化硅微粒的碳酸钙进行过滤，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、硼砂、氢氧化铝、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所述的一种阻燃的二氧化钛、聚乙烯双重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℃。
CN201610911113.6A 2016-10-20 2016-10-20 一种阻燃的二氧化钛、聚乙烯双重包覆碳酸钙无机填料及其制备方法 Pending CN106566284A (zh)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112898942A (zh) * 2021-01-23 2021-06-04 广西碳酸钙产业化工程院有限公司 一种赋予单组份脱醇型硅酮密封胶良好阻燃性能专用重质碳酸钙及其制备方法
CN115873423A (zh) * 2022-12-29 2023-03-31 贺州学院 一种利用钛酸四丁酯制备改性碳酸钙粉体的方法

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112898942A (zh) * 2021-01-23 2021-06-04 广西碳酸钙产业化工程院有限公司 一种赋予单组份脱醇型硅酮密封胶良好阻燃性能专用重质碳酸钙及其制备方法
CN115873423A (zh) * 2022-12-29 2023-03-31 贺州学院 一种利用钛酸四丁酯制备改性碳酸钙粉体的方法

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