CN111471320B - 一种碳酸钙粉体的制备方法 - Google Patents

一种碳酸钙粉体的制备方法 Download PDF

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CN111471320B
CN111471320B CN202010450125.XA CN202010450125A CN111471320B CN 111471320 B CN111471320 B CN 111471320B CN 202010450125 A CN202010450125 A CN 202010450125A CN 111471320 B CN111471320 B CN 111471320B
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黄俊俊
桂成梅
陈珍明
秦广超
赵娣芳
赵兴科
陆国庆
程兵
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Guangxi Hezhou Zhuoyuan New Material Co ltd
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Abstract

本发明公开了一种碳酸钙粉体的制备方法，包括以下步骤：（1）湿法研磨：采用湿法球磨工艺研磨高目数的碳酸钙粉体，体系温度为80℃，加入阴离子表面活性剂，研磨60‑600 min，压滤后即制备湿法研磨碳酸钙粉体；（2）碳酸钙表面原位包覆：将湿法研磨碳酸钙粉体浸入第一溶液，高速搅拌0.1‑10 min，压滤后即制备原位包覆碳酸钙粉体；（3）碳酸钙表面原位吸附：将原位包覆碳酸钙粉体浸入第二溶液，高速搅拌10‑600 min，压滤后即制备原位吸附的碳酸钙粉体；（4）精细分级：将原位吸附的碳酸钙粉体雾化干燥，并采用旋风分离即制备具有杀菌功能的透气膜用碳酸钙粉体。本发明的有益效果为：（1）制孔效果优秀，致孔效率高；（2）孔径小；（3）致孔剂功能化。

Description

一种碳酸钙粉体的制备方法
技术领域
本发明涉及无机粉体功能化制备方法，特别是一种碳酸钙粉体的制备方法。
背景技术
透气膜是允许水蒸气扩散透过但阻隔液态水渗漏的一种微孔膜，主要用于制造卫生防护用品以及透气性防雨布等制品，在个人护理、建筑、农副产品包装等领域有广泛应用。超细碳酸钙是制备透气膜的主要填料，填充了碳酸钙粉体的树脂经过流延或吹塑方式制成薄膜，再通过对薄膜施加单向或双向拉伸作用，使聚酯基体与碳酸钙颗粒表面发生分离并在填料颗粒之间形成相互连通的微孔道，从而形成微孔透气膜，即碳酸钙在透气膜中起到“致孔剂”的作用。
据中国粉体网等权威网站发布的数据显示，当前国内具有高附加值的重质碳酸钙粉体品种还不足总产能的0.5％，碳酸钙高端市场(如透气膜、高端油墨、医用防护服等领域)基本被国外企业所垄断。目前国内医用防护服标准中缺少对微生物渗透的测试(如GB19082-2009标准)，而国外的医用防护服都对此类测试均有相关技术要求(如ANSI/AAMIPB70-2012、NFPA1999-2018和EN14126-2003标准)，其病毒防护的安全性更好，随着更高级别标准制定、实施，这都对透气膜中“致孔剂”碳酸钙提出精细化、功能化的要求。
发明内容
本发明的目的是提供一种碳酸钙粉体的制备方法，以解决现有技术中的不足，它能够在碳酸钙粉体表面原位形成柠檬酸钙，结合吸附银具有杀菌功能粒子，通过控制温度，在拉伸致孔过程中柠檬酸钙分解辅助界面脱粘致孔，在孔内形成杀菌功能粒子和阻隔物，降低孔径和赋予孔杀菌能力。
本发明提供了一种碳酸钙粉体的制备方法，包括以下步骤：
(1)湿法研磨：采用湿法球磨工艺研磨高目数的碳酸钙粉体，体系温度为80℃，加入阴离子表面活性剂，研磨60-600min，压滤后即制备湿法研磨碳酸钙粉体；
(2)碳酸钙表面原位包覆：将湿法研磨碳酸钙粉体浸入第一溶液，高速搅拌0.1-10min，压滤后即制备原位包覆碳酸钙粉体；
(3)碳酸钙表面原位吸附：将原位包覆碳酸钙粉体浸入第二溶液，高速搅拌10-600min，压滤后即制备原位吸附的碳酸钙粉体；
(4)精细分级：将原位吸附的碳酸钙粉体雾化干燥，并采用旋风分离即制备具有杀菌功能的透气膜专用碳酸钙粉体。
如上所述的一种碳酸钙粉体的制备方法，其中，优选的是，步骤(1)中所述阴离子表面活性剂为十二烷基苯磺酸钠、十二烷基硫酸钠和乙氧基化脂肪酸甲酯磺酸钠中的至少一种。
如上所述的一种碳酸钙粉体的制备方法，其中，优选的是，步骤(1)中所述阴离子表面活性剂的添加量为所述碳酸钙粉体质量的0.1-5％。
如上所述的一种碳酸钙粉体的制备方法，其中，优选的是，步骤(2)中所述第一溶液为柠檬酸和表面活性剂的溶液。
如上所述的一种碳酸钙粉体的制备方法，其中，优选的是，所述表面活性剂与柠檬酸的重量配比为：表面活性剂0.1-5％，柠檬酸1-20％，水为余量。
如上所述的一种碳酸钙粉体的制备方法，其中，优选的是，所述表面活性剂为卵磷脂，烷基葡糖苷，脂肪酸甘油酯，脂肪酸山梨坦和聚山梨酯中的至少一种。
如上所述的一种碳酸钙粉体的制备方法，其中，优选的是，所述第二溶液为硝酸银、硝酸锌和硝酸铜溶液中的至少一种。
如上所述的一种碳酸钙粉体的制备方法，其中，优选的是，所述第二溶液浓度为0.1-60g/L。
如上所述的一种碳酸钙粉体的制备方法，其中，优选的是，步骤(4)中所述雾化干燥温度为120-140℃。
如上所述的一种碳酸钙粉体的制备方法，其中，优选的是，粉体改性、密炼和挤出温度为160-170℃，拉伸温度为180-190℃。
与现有技术相比，本发明的有益效果为：(1)制孔效果优秀，致孔效率高：本发明制备的一种具有杀菌功能的透气膜专用碳酸钙粉体，通过表面原位同柠檬酸反应，结合对粉体纵向温度的控制，在碳酸钙粉体表面形成一层致密的柠檬酸钙层，在拉伸致孔过程中，柠檬酸钙分解，导致致孔剂/聚酯表面分离，进而形成孔结构，即依靠化学反应致孔，这种致孔的均匀性比传统依靠拉力破坏致孔剂/聚酯界面结构要好，且致孔工艺易控制、致孔效率高。(2)孔径小：柠檬酸钙分解除了形成气体外，还形成固体颗粒，这些颗粒残存在孔内部，分割孔成小孔。(3)致孔剂功能化：本发明依靠柠檬酸根离子吸附抗菌粒子，当柠檬酸钙分解后，这些抗菌粒子布满孔内部，赋予透气膜孔具有杀菌能力。
附图说明
图1是本发明实施例1的碳酸钙粉体制备示意图；
图2是本发明实施例1制备的碳酸钙在透气膜拉伸过程中的碳酸钙粉体/聚酯界面变化示意图；
图3是本发明实施例1制备的碳酸钙粉体制得的透气膜结构示意图。
具体实施方式
下面通过参考附图描述的实施例是示例性的，仅用于解释本发明，而不能解释为对本发明的限制。
一种碳酸钙粉体的制备方法，包括以下步骤：
(1)湿法研磨：采用湿法球磨工艺研磨高目数的碳酸钙粉体，体系温度为80℃，加入阴离子表面活性剂，研磨60-600min，压滤后即制备湿法研磨碳酸钙粉体；
(2)碳酸钙表面原位包覆：将湿法研磨碳酸钙粉体浸入第一溶液，高速搅拌0.1-10min，压滤后即制备原位包覆碳酸钙粉体；
(3)碳酸钙表面原位吸附：将原位包覆碳酸钙粉体浸入第二溶液，高速搅拌10-600min，压滤后即制备原位吸附的碳酸钙粉体；
(4)精细分级：将原位吸附的碳酸钙粉体雾化干燥，并采用旋风分离即制备具有杀菌功能的透气膜专用碳酸钙粉体。
步骤(1)中所述阴离子表面活性剂为十二烷基苯磺酸钠、十二烷基硫酸钠和乙氧基化脂肪酸甲酯磺酸钠中的至少一种。
步骤(1)中所述阴离子表面活性剂的添加量为所述碳酸钙粉体质量的0.1-5％。
步骤(2)中所述第一溶液为柠檬酸和表面活性剂的溶液。
所述表面活性剂与柠檬酸的重量配比为：表面活性剂0.1-5％，柠檬酸1-20％，水为余量。
所述表面活性剂为卵磷脂，烷基葡糖苷，脂肪酸甘油酯，脂肪酸山梨坦和聚山梨酯中的至少一种。
所述第二溶液为硝酸银、硝酸锌和硝酸铜溶液中的至少一种。
所述第二溶液浓度为0.1-60g/L。
步骤(4)中所述雾化干燥温度为120-140℃。
粉体改性、密炼和挤出温度为160-170℃，拉伸温度为180-190℃。
本发明的实施例1：
一种碳酸钙粉体的制备方法，包括以下步骤：
(1)湿法研磨：采用湿法球磨工艺研磨高目数的碳酸钙粉体，体系温度为80℃，加入卵磷脂阴离子溶液，研磨60min，卵磷脂阴离子溶液的添加量为碳酸钙质量的0.1％，压滤后即制备湿法研磨碳酸钙粉体；
(2)碳酸钙表面原位包覆：将湿法研磨碳酸钙粉体采用微波加热至600℃，再浸入柠檬酸和卵磷脂表面活性剂的混合溶液，卵磷脂表面活性剂0.1％，柠檬酸10％，水为余量，溶液pH为6，温度为0℃，高速搅拌0.1min，压滤后即制备原位包覆碳酸钙粉体；
(3)碳酸钙表面原位吸附：将原位包覆碳酸钙粉体浸入0.1g/L的硝酸银溶液，高速搅拌10min，压滤后即制备原位吸附的碳酸钙粉体；
(4)精细分级：将原位吸附的碳酸钙粉体雾化干燥，雾化干燥温度为120℃，并采用旋风分离即制备具有杀菌功能的透气膜专用碳酸钙粉体。
本实施例的方法制备的碳酸钙粉体参数为：中位粒径(D50)在1.8μm，97％颗粒粒径(D97)为6.5μm，1～5μm颗粒占60％，10μm以上颗粒＜100ppm，BET比表面积为5m2/g。
制备透气膜过程涉及到粉体改性、密炼和挤出温度为160℃，拉伸温度为180℃，透气膜拉伸过程中碳酸钙粉体/聚酯界面变化示意图如图2所示，依靠柠檬酸根离子吸附抗菌粒子，当柠檬酸钙分解后，这些抗菌粒子布满孔内部，赋予透气膜孔具有杀菌能力，透气膜结构示意图如图3所示。制备的透气膜性能如表1。
表1透气膜性能
指标明细 数值
细菌过滤效率 98.5％
非油性颗粒过滤效率 98.5％
合成血液穿透 160mmHg
呼吸阻力 5.5mm H<sub>2</sub>O/cm<sup>2</sup>
透气膜平均孔径 5μm
本发明的实施例2：
一种碳酸钙粉体的制备方法，包括以下步骤：
(1)湿法研磨：采用湿法球磨工艺研磨高目数的碳酸钙粉体，体系温度为80℃，加入烷基葡糖苷阴离子溶液，研磨600min，其中烷基葡糖苷阴离子溶液的添加量为碳酸钙质量的5％，压滤后即制备湿法研磨碳酸钙粉体；
(2)碳酸钙表面原位包覆：将湿法研磨碳酸钙粉体采用微波加热至600-800℃，再浸入柠檬酸和脂肪酸甘油酯阴离子表面活性剂的混合溶液，其中脂肪酸甘油酯阴离子表面活性剂5％，柠檬酸20％，水为余量，溶液pH为6，温度为10℃，高速搅拌10min，压滤后即制备原位包覆碳酸钙粉体；
(3)碳酸钙表面原位吸附：将原位包覆碳酸钙粉体浸入60g/L的硝酸锌溶液，高速搅拌600min，压滤后即制备原位吸附的碳酸钙粉体，压滤后即制备原位吸附的碳酸钙粉体；
(4)精细分级：将原位吸附的碳酸钙粉体雾化干燥，雾化干燥温度为140℃，并采用旋风分离即制备具有杀菌功能的透气膜专用碳酸钙粉体。
本实施例的方法制备的碳酸钙粉体参数为：中位粒径(D50)在2.2μm，97％颗粒粒径(D97)为5.5μm，1～5μm颗粒占65％，10μm以上颗粒为90ppm，BET比表面积为15m2/g。
制备透气膜过程涉及到粉体改性、密炼和挤出温度为170℃，拉伸温度为190℃，制备的透气膜性能如表2。
表2透气膜性能
指标明细 数值
细菌过滤效率 98.1％
非油性颗粒过滤效率 98.1％
合成血液穿透 80mmHg
呼吸阻力 3.5mm H<sub>2</sub>O/cm<sup>2</sup>
透气膜平均孔径 8μm
本发明的实施例3：
一种碳酸钙粉体的制备方法，包括以下步骤：
(1)湿法研磨：采用湿法球磨工艺研磨高目数的碳酸钙粉体，体系温度为80℃，加入脂肪酸甘油酯，脂肪酸山梨坦阴离子溶液，研磨400min，其中表面活性剂的添加量为碳酸钙质量的3％，压滤后即制备湿法研磨碳酸钙粉体；
(2)碳酸钙表面原位包覆：将湿法研磨碳酸钙粉体采用微波加热至600-800℃，再浸入柠檬酸和聚山梨酯阴离子表面活性剂的混合溶液，聚山梨酯阴离子表面活性剂2％，柠檬酸10％，水为余量，其中溶液pH为6，温度为5℃，高速搅拌5min，压滤后即制备原位包覆碳酸钙粉体；
(3)碳酸钙表面原位吸附：将原位包覆碳酸钙粉体浸入30g/L的硝酸铜溶液，高速搅拌100min，压滤后即制备原位吸附的碳酸钙粉体；
(4)精细分级：将原位吸附的碳酸钙粉体雾化干燥，雾化干燥温度为130℃，并采用旋风分离即制备具有杀菌功能的透气膜专用碳酸钙粉体。
本实施例的方法制备的碳酸钙粉体参数为：中位粒径(D50)在2μm，97％颗粒粒径(D97)为6.1μm，1～5μm颗粒占65％，10μm以上颗粒800ppm，BET比表面积为11m2/g。
制备透气膜过程涉及到粉体改性、密炼和挤出温度为165℃，拉伸温度为185℃，制备的透气膜性能如表3所示。
表3透气膜性能
指标明细 数值
细菌过滤效率 99％
非油性颗粒过滤效率 99％
合成血液穿透 80mmHg
呼吸阻力 3.0mm H<sub>2</sub>O/cm<sup>2</sup>
透气膜平均孔径 3μm
以上依据图式所示的实施例详细说明了本发明的构造、特征及作用效果，以上所述仅为本发明的较佳实施例，但本发明不以图面所示限定实施范围，凡是依照本发明的构想所作的改变，或修改为等同变化的等效实施例，仍未超出说明书与图示所涵盖的精神时，均应在本发明的保护范围内。

Claims (5)

1.一种碳酸钙粉体的制备方法，其特征在于：包括以下步骤：
(1)湿法研磨：采用湿法球磨工艺研磨高目数的碳酸钙粉体，体系温度为80℃，加入阴离子表面活性剂，研磨60-600 min，压滤后即制备湿法研磨碳酸钙粉体；
(2)碳酸钙表面原位包覆：将湿法研磨碳酸钙粉体浸入第一溶液，高速搅拌0.1-10min，压滤后即制备原位包覆碳酸钙粉体；所述第一溶液为柠檬酸和表面活性剂的溶液；所述第一溶液的重量配比为：表面活性剂0.1-5％，柠檬酸1-20％，水为余量；所述表面活性剂为卵磷脂，烷基葡糖苷，脂肪酸甘油酯，脂肪酸山梨坦和聚山梨酯中的至少一种；
(3)碳酸钙表面原位吸附：将原位包覆碳酸钙粉体浸入第二溶液，高速搅拌10-600min，压滤后即制备原位吸附的碳酸钙粉体；所述第二溶液为硝酸银、硝酸锌和硝酸铜溶液中的至少一种；
(4)精细分级：将原位吸附的碳酸钙粉体雾化干燥，并采用旋风分离即制备具有杀菌功能的透气膜用碳酸钙粉体。
2.根据权利要求1所述的碳酸钙粉体的制备方法，其特征在于：步骤（1）中所述阴离子表面活性剂为十二烷基苯磺酸钠、十二烷基硫酸钠和乙氧基化脂肪酸甲酯磺酸钠中的至少一种。
3.根据权利要求1所述的碳酸钙粉体的制备方法，其特征在于：步骤（1）中所述阴离子表面活性剂的添加量为所述碳酸钙粉体质量的0.1-5% 。
4.根据权利要求1所述的碳酸钙粉体的制备方法，其特征在于：所述第二溶液浓度为0.1-60 g/L。
5.根据权利要求1所述的碳酸钙粉体的制备方法，其特征在于：步骤（4）中所述雾化干燥温度为120-140℃。
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