CN105924675B - 一种聚合物透气膜及其填料重质碳酸钙制备方法 - Google Patents

一种聚合物透气膜及其填料重质碳酸钙制备方法 Download PDF

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CN105924675B
CN105924675B CN201610339951.0A CN201610339951A CN105924675B CN 105924675 B CN105924675 B CN 105924675B CN 201610339951 A CN201610339951 A CN 201610339951A CN 105924675 B CN105924675 B CN 105924675B
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董绍宏
郑家伟
郑水林
刘立新
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Yunnan Macro Innovation Mstar Technology Ltd
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Abstract

一种聚合物透气膜及其填料重质碳酸钙制备方法。本发明属于吸水材料领域，具体涉及一种聚合物透气膜用低含水量重质碳酸钙填料及其制备方法。本发明是将重质碳酸钙粉磨至粒度325目筛余小于3%，然后调浆，进行湿式研磨，压滤脱水成滤饼，在超微干燥粉碎机中同时进行干燥和表面有机改性，真空包装，与有机聚合物的结合制得微孔透气膜。本发明所用重质碳酸钙填料的水分含量低，粒度分布细，与聚合物的相容性好，容易分散，且与有机聚合物的结合力强，用其制备的透气膜，透湿性能好，拉伸强度高和伸长率高，生产成本较低。

Description

一种聚合物透气膜及其填料重质碳酸钙制备方法
技术领域
本发明属于吸水材料领域，具体涉及一种聚合物透气膜用低含水量重质碳酸钙填料及其制备方法。
背景技术
微孔透气膜是一种具有微细孔道结构的无机填料填充聚合物复合薄膜材料，微孔允许气体通过，但由于液体直径大于微孔直径而被阻挡，从而具有“透气不透水”的特性。透气膜的制造过程是将无机填料与聚合物复合制得透气膜专用料；后将专用料流延或吹塑成薄膜；最后对薄膜进行拉伸，使聚合物基体与填料颗粒表面分离形成微孔，并在填料颗粒之间产生相互连通的微细孔道，从而制得微孔透气膜。透气膜广泛应用于婴儿纸尿布、卫生巾、卫生护垫、成人纸尿裤及失禁用品等领域。
现有技术中已有在微孔透气中加入纳米碳酸钙来制备吸水材料卫生用品的方案，如中国专利文献公开的201410353792.0号申请申请，该技术是将纳米碳酸钙的加入到丙烯酸酯泡沫材料中，从而取代部分价格昂贵的填充料及助剂，同时使透气性能得到显著改善。然而在该技术方案中，CaCO3表面多余的水分会在较高的加工温度下蒸发产生水蒸气，使得最终得到透气膜表面产生大孔甚至孔洞，从而对透气膜的透湿性能和力学性能产生影响；纳米碳酸钙的干燥和表面改性过程是分开进行，在干燥和表面改性的生产间隙中CaCO3会吸收空气中的水分，使得最终产出的CaCO3填料水分含量不能达到使用要求；纳米碳酸钙的制备方法较复杂，产品的成本还较高，也就不能较显著的降低吸水材料卫生用品的成本。
发明内容
本发明所要解决的技术问题是提供一种聚合物透气膜用重质碳酸钙填料及其制备方法，其生产容易，成本较低，水分含量能达到使用要求，粒度分布细，与聚合物的相容性好。
实现本发明上述目的所采取的技术方案是：无机填料CaCO3的粒度为d50=0.7～2μm和d97=5～8μm（分别表示重质碳酸钙的中位粒度和97%累积粒度分布），吸油值为0.14～0.18ml/g，水分含量为0.04wt%～0.09wt%，制得的透气膜水蒸气透过率（WVTR）为6900～7300g/m2 .day，纵向拉伸强度39～43MPa，横向拉伸强度12～14MPa，纵向伸长率=150%～190%，横向伸长率410%～450%，润湿张力=38～39，热收缩率=3.8%～4.0%。、
本发明所述聚合物透气膜的填料重质碳酸钙制备方法为：
①将破碎和粉磨至粒度325目筛余小于3%的重质碳酸钙粉体加水和分散剂调浆，浆料的粉体质量浓度为30%～50%；
②将步骤①制备的重质碳酸钙粉体浆料给入密闭卧式砂磨机中进行湿式研磨，研磨至d50=0.7～2μm和d97=5～8μm；
③将步骤②研磨后的重质碳酸钙浆料进行压滤脱水成滤饼；
④将步骤③脱水后的滤饼给入（WFG）超微干燥粉碎机中同时进行干燥和表面有机改性，改性剂为硬脂酸、铝酸酯、钛酸酯或聚乙二醇，用量为重钙粉体质量的1.0%～1.8%；
⑤将步骤④所得粉体采用真空包装机进行包装储存。
所述的聚合物透气膜的填料重质碳酸钙制备方法还包括：给入超微干燥粉碎机的脱水滤饼含水量为10wt%～20wt%，超微干燥粉碎机中的温度为180℃～360℃，出口温度120℃～150℃，物料干燥时间为9s～18s，加工所得粉体的含水量为0.04wt%～0.09wt%。
本发明的有益技术效果是：用本发明方法制备的透气膜用重质碳酸钙填料的水分含量低，粒度分布细，与聚合物的相容性好，容易分散，且与有机聚合物的结合力强；用其制备的透气膜，透湿性能好，拉伸强度高和伸长率高，而且生产成本较低。
具体实施方式
实施例1：取破碎和粉磨至筛余为3%的325目的重质碳酸钙粉体100kg，加160kg水和0.5%的六偏磷酸钠调浆分散；将分散好的重质碳酸钙粉体浆料给入HDM-200密闭卧式砂磨机中进行超细研磨；然后将超细研磨好的重质碳酸钙浆料进行压滤脱水；将脱水后的滤饼给入WFG500超微干燥粉碎机同时进行干燥和表面有机改性，表面改性剂为硬脂酸1801，用量为重质碳酸钙粉体质量的1.4%；采用真空包装机将改性好的重钙粉体进行包装。取干燥改性后的重质碳酸钙样品填充LLDPE制得透气膜专用料，后经流延和拉伸制成透气膜，透气膜性能检测结果列于表1。
实施例2：取破碎和粉磨至筛余为3%的325目的重质碳酸钙粉体100kg，加180kg水和0.5%的六偏磷酸钠调浆分散；将分散好的重质碳酸钙粉体浆料给入HDM-200密闭卧式砂磨机中进行超细研磨；然后将超细研磨好的重质碳酸钙浆料进行压滤脱水；将脱水后的滤饼给入WFG500超微干燥粉碎机同时进行干燥和表面有机改性，表面改性剂为硬脂酸1801，用量为重质碳酸钙粉体质量的1.2%；采用真空包装机将改性好的重钙粉体进行包装。取干燥改性后的重钙样品填充LLDPE制得透气膜专用料，后经流延和拉伸制成透气膜，透气膜性能检测结果列于表1。
实施例3：取破碎和粉磨至筛余为3%的325目的重质碳酸钙粉体100kg，加140kg水和0.5%的六偏磷酸钠调浆分散；将分散好的重质碳酸钙粉体浆料给入HDM-200密闭卧式砂磨机中进行超细研磨；然后将超细研磨好的重质碳酸钙浆料进行压滤脱水；将脱水后的滤饼给入WFG500超微干燥粉碎机同时进行干燥和表面有机改性，表面改性剂为铝酸酯，用量为重钙粉体质量的1.4%；采用真空包装机将改性好的重质碳酸钙粉体进行包装。取干燥改性后的重钙样品填充LLDPE制得透气膜专用料，后经流延和拉伸制成透气膜，透气膜性能检测结果列于表1。
实施例4：取破碎和粉磨至筛余为3%的325目的重质碳酸钙粉体100kg，加160kg水和0.5%的六偏磷酸钠调浆分散；将分散好的重质碳酸钙粉体浆料给入HDM-200密闭卧式砂磨机中进行超细研磨；然后将超细研磨好的重质碳酸钙浆料进行压滤脱水；将脱水后的滤饼给入WFG500超微干燥粉碎机同时进行干燥和表面有机改性，表面改性剂为钛酸酯，用量为重质碳酸钙粉体质量的1.2%；采用真空包装机将改性好的重质碳酸钙粉体进行包装。取干燥改性后的重钙样品填充LLDPE制得透气膜专用料，后经流延和拉伸制成透气膜，透气膜性能检测结果列于表1。
实施例5：取破碎和粉磨至筛余为3%的325目的重质碳酸钙粉体100kg，加200kg水和0.5%的六偏磷酸钠调浆分散；将分散好的重质碳酸钙粉体浆料给入HDM-200密闭卧式砂磨机中进行超细研磨；然后将超细研磨好的重质碳酸钙浆料进行压滤脱水；将脱水后的滤饼给入WFG500超微干燥粉碎机同时进行干燥和表面有机改性，表面改性剂为聚乙二醇200，用量为重质碳酸钙粉体质量的1.2%；采用真空包装机将改性好的重钙粉体进行包装。取干燥改性后的重钙样品填充LLDPE制得透气膜专用料，后经流延和拉伸制成透气膜，透气膜性能检测结果列于表1。
实施例6：取破碎和粉磨至筛余为3%的325目的重质碳酸钙粉体100kg，加200kg水和0.5%的六偏磷酸钠调浆分散；将分散好的重质碳酸钙粉体浆料给入HDM-200密闭卧式砂磨机中进行超细研磨；然后将超细研磨好的重质碳酸钙浆料进行压滤脱水；将脱水后的滤饼给入WFG500超微干燥粉碎机同时进行干燥和表面有机改性，表面改性剂为聚乙二醇400，用量为重质碳酸钙粉体质量的1.0%；采用真空包装机将改性好的重质碳酸钙粉体进行包装。取干燥改性后的重质碳酸钙样品填充LLDPE制得透气膜专用料，后经流延和拉伸制成透气膜，透气膜性能检测结果列于表1。
表1
。
矿物水分含量依据GB/T7702.1-1997测定；拉伸强度和断裂伸长率依据GB/T1040.3-2006标准测试；透气量（WVTR）依据ASTME398测定；润湿张力依据GB/T14216-2008测定；热收缩率依据GB/T12027-2004测定。

Claims (3)

1.一种聚合物透气膜，其特征在于：重质碳酸钙CaCO3的粒度为d50=0.7～2μm和d97=5～8μm，吸油值为0.14～0.18 ml/g，水分含量为0.04wt%～0.09wt%，制得的透气膜水蒸气透过率为6900～7300g/m2 .day，纵向拉伸强度39～43MPa，横向拉伸强度12～14MPa，纵向伸长率=150%～190%，横向伸长率410%～450%，润湿张力=38～39，热收缩率=3.8%～4.0%；
所述聚合物透气膜由重质碳酸钙与有机聚合物组成；
所述聚合物透气膜的填料重质碳酸钙的制备方法为：
①将破碎和粉磨至粒度325目筛余小于3%的重质碳酸钙粉体加水和分散剂调浆，浆料的粉体质量浓度为30%～50%；
②将步骤①制备的重质碳酸钙粉体浆料给入密闭卧式砂磨机中进行湿式研磨，研磨至d50=0.7～2μm和d97=5～8μm；
③将步骤②研磨后的重质碳酸钙浆料进行压滤脱水成滤饼；
④将步骤③脱水后的滤饼给入超微干燥粉碎机中同时进行干燥和表面有机改性，改性剂为硬脂酸、铝酸酯、钛酸酯或聚乙二醇，用量为重钙粉体质量的1.0%～1.8%，超微干燥粉碎机中的温度为180℃～360℃，出口温度120℃～150℃；
⑤将步骤④所得粉体采用真空包装机进行包装储存。
2.一种权利要求1所述聚合物透气膜的制备方法，其特征在于，制备方法为：
所述聚合物透气膜是按照下述方法制备得到的：取干燥改性后的重质碳酸钙样品填充LLDPE制得透气膜专用料，后经流延和拉伸制成透气膜；
所述重质碳酸钙的制备方法为：
①将破碎和粉磨至粒度325目筛余小于3%的重质碳酸钙粉体加水和分散剂调浆，浆料的粉体质量浓度为30%～50%；
②将步骤①制备的重质碳酸钙粉体浆料给入密闭卧式砂磨机中进行湿式研磨，研磨至d50=0.7～2μm和d97=5～8μm；
③将步骤②研磨后的重质碳酸钙浆料进行压滤脱水成滤饼；
④将步骤③脱水后的滤饼给入超微干燥粉碎机中同时进行干燥和表面有机改性，改性剂为硬脂酸、铝酸酯、钛酸酯或聚乙二醇，用量为重钙粉体质量的1.0%～1.8%，超微干燥粉碎机中的温度为180℃～360℃，出口温度120℃～150℃；
⑤将步骤④所得粉体采用真空包装机进行包装储存。
3.根据权利要求2所述的聚合物透气膜的制备方法，其特征在于：给入超微干燥粉碎机的脱水滤饼含水量为10wt%～20wt%，物料干燥时间为9s～18s，加工所得粉体的含水量为0.04wt%～ 0.09wt%。
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