CN108557836B - 一种BaB8O11(OH)4纳米阻燃材料及其制备方法 - Google Patents

一种BaB8O11(OH)4纳米阻燃材料及其制备方法 Download PDF

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CN108557836B
CN108557836B CN201810401616.8A CN201810401616A CN108557836B CN 108557836 B CN108557836 B CN 108557836B CN 201810401616 A CN201810401616 A CN 201810401616A CN 108557836 B CN108557836 B CN 108557836B
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刘志宏
苗静
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Abstract

本发明公开了一种BaB8O11(OH)4纳米阻燃材料及其制备方法，该方法以硝酸钡或醋酸钡为钡源，以八水合五硼酸铵或硼酸为硼源，直接一步水热或溶剂热反应即可制备成纳米片、纳米带、纳米盘结构的BaB8O11(OH)4纳米阻燃材料。本发明方法简单，反应条件温和，原料易得，所制备的BaB8O11(OH)4纳米材料分散性好，形貌均一，对聚丙烯等塑料具有良好的阻燃性，具有广阔的应用前景。

Description

一种BaB8O11(OH)4纳米阻燃材料及其制备方法
技术领域
本发明属于阻燃材料技术领域，具体涉及一种BaB8O11(OH)4纳米阻燃材料及其制备方法。
背景技术
硼酸盐是一种有效且价廉的无机阻燃剂，具有热稳定性好、无毒、抑烟、燃烧产物毒性小等优点，广泛应用于各种纤维、树脂、橡胶制品、电器绝缘材料、电线、电缆、木材及防锈漆等方面的阻燃。然而，通常制备的硼酸盐粒径较大，在聚合物中不易分散，还降低了高分子聚合物的机械性能，限制了其应用。由于纳米材料的形貌和尺寸对其阻燃性能有很大影响，对于等量的阻燃剂，其粒径愈小比表面积愈大，超细化、纳米化以后，增强了界面的相互作用，可以更均匀的分散于基质中，阻燃效果就愈好。如果将硼酸盐阻燃剂制备成纳米级，则有可能既可增大阻燃剂与基质材料的接触面和提高相容性，又可降低阻燃剂的用量。
发明人在研发过程中发现不少有关水合硼酸锌、水合硼酸钙、水合硼酸镁纳米结构的制备报道，如Lihong Bao等人提出采用水热法制备硼酸钙2CaO·B2O3·H2O 纳米带，本课题组也曾报道了4ZnO·B2O3·H2O纳米材料，椭球状、蚕蛹状 4CaO·5B2O3·7H2O纳米结构的制备，相转化法制备片状CaO·3B2O3·4H2O纳米材料，等。但未有人提出过关于组成为BaB8O11(OH)4的硼酸钡纳米材料制备的相关报道。
发明内容
本发明所要解决的技术问题在于提供一种粒径小、分散性好、阻燃性能优良的BaB8O11(OH)4纳米阻燃材料，以及该阻燃材料的制备方法。
解决上述技术问题所采用的BaB8O11(OH)4纳米阻燃材料由下述方法制备得到：按照钡元素与硼元素的摩尔比为1:2～20，将钡源和硼源加入溶剂中，混合均匀，所得混合物在密闭条件下120～220℃下反应8～36小时，将反应产物依次用60～80℃蒸馏水、乙醇洗涤后干燥，得到BaB8O11(OH)4纳米阻燃材料；
上述的钡源为硝酸钡或醋酸钡，硼源为八水合五硼酸铵或硼酸，溶剂为去离子水或乙二醇。
上述的钡源为硝酸钡、硼源为八水合五硼酸铵、溶剂为去离子水时，得到的BaB8O11(OH)4纳米阻燃材料为纳米片形貌，优选在密闭条件下170～190℃下反应10～12小时，进一步优选钡元素与硼元素的摩尔比为1:10～17。
上述的钡源为醋酸钡、硼源为硼酸、溶剂为去离子水时，在密闭条件下160～200℃下反应12～18小时，得到的BaB8O11(OH)4纳米阻燃材料为纳米带形貌，优选钡元素与硼元素的摩尔比为1:5～12。
上述的钡源为醋酸钡、硼源为硼酸、溶剂为乙二醇时，在密闭条件下160～200℃下反应12～18小时，得到的BaB8O11(OH)4纳米阻燃材料为纳米盘形貌，优选钡元素与硼元素的摩尔比为1:2～8。
本发明方法简单，原料易得，反应条件温和，所制备的BaB8O11(OH)4纳米阻燃材料分散性好、粒径小，且具有较好的阻燃效果和抑烟作用。
附图说明
图1是实施例1～3制备的BaB8O11(OH)4纳米片的XRD图。
图2是实施例1制备的BaB8O11(OH)4纳米片的SEM图。
图3是实施例2制备的BaB8O11(OH)4纳米片的SEM图。
图4是实施例3制备的BaB8O11(OH)4纳米带的SEM图。
图5是实施例4制备的BaB8O11(OH)4纳米带的SEM图。
图6是实施例5制备的BaB8O11(OH)4纳米盘的SEM图。
图7是实施例6制备的BaB8O11(OH)4纳米盘的SEM图。
具体实施方式
下面结合附图和实施例对本发明进一步详细说明，但本发明的保护范围不仅限于这些实施例。
实施例1
将2.61g(0.01mol)Ba(NO3)2、5.44g(0.01mol)(NH4)2B10O6·8H2O、60mL去离子水加入100mL高压反应釜中，室温搅拌混合均匀后，放置在160℃烘箱中密闭反应24小时，反应完成后自然冷却至室温，将反应产物依次用60～80℃蒸馏水、乙醇各洗涤2～3次后，60℃干燥12小时，得到BaB8O11(OH)4纳米片。
发明人采用X-射线衍射仪、扫描电子显微镜对所得样品进行表征，结果见图1～2。由图1的XRD表征结果可见，所得材料的衍射数据与BaB8O11(OH)4的JCPDS 标准卡片(FileNo.97-042-1417)的衍射数据相一致。由图2可见，BaB8O11(OH)4纳米片长约500nm、宽150～200nm、厚度约50nm左右。
实施例2
将2.61g(0.01mol)Ba(NO3)2、8.16g(0.015mol)(NH4)2B10O6·8H2O、60mL 去离子水加入100mL高压反应釜中，室温搅拌混合均匀后，在180℃下密闭反应 18小时，反应完成后自然冷却至室温，将反应产物依次用60～80℃蒸馏水、乙醇各洗涤2～3次后，60℃干燥12小时，得到BaB8O11(OH)4纳米片(见图3)。
实施例3
将2.55g(0.01mol)Ba(Ac)2、3.70g(0.058mol)H3BO3、10mL去离子水加入 50mL高压反应釜中，室温搅拌混合均匀后，在180℃下密闭反应12小时，反应完成后自然冷却至室温，将反应产物依次用60～80℃蒸馏水、乙醇各洗涤2～3次后，60℃干燥12小时，得到BaB8O11(OH)4纳米带。由图1的XRD表征结果可见，所得材料的衍射数据与BaB8O11(OH)4的JCPDS标准卡片(File No.97-042-1417)的衍射数据相一致。由图4可见，BaB8O11(OH)4纳米带厚度约50nm左右。
实施例4
将2.55g(0.01mol)Ba(Ac)2、6.18g(0.10mol)H3BO3、20mL去离子水加入 50mL高压反应釜中，室温搅拌混合均匀后，在160℃下密闭反应18小时，反应完成后自然冷却至室温，将反应产物依次用60～80℃蒸馏水、乙醇各洗涤2～3次后，60℃干燥12小时，得到BaB8O11(OH)4纳米带(见图5)。
实施例5
将2.55g(0.01mol)Ba(Ac)2、1.24g(0.02mol)H3BO3、5mL乙二醇加入50mL 高压反应釜中，室温搅拌混合均匀后，在180℃下密闭反应12小时，反应完成后自然冷却至室温，将反应产物依次用60～80℃蒸馏水、乙醇各洗涤2～3次后，60℃干燥12小时，得到BaB8O11(OH)4纳米盘。由图1的XRD表征结果可见，所得材料的衍射数据与BaB8O11(OH)4的JCPDS标准卡片(File No.97-042-1417)的衍射数据相一致。由图6可见，BaB8O11(OH)4纳米盘的直径为100～200nm、厚度约20nm 左右。
实施例6
将2.55g(0.01mol)Ba(Ac)2、4.96g(0.08mol)H3BO3、10mL乙二醇加入50 mL高压反应釜中，室温搅拌混合均匀后，在200℃下密闭反应12小时，反应完成后自然冷却至室温，将反应产物依次用60～80℃蒸馏水、乙醇各洗涤2～3次后， 60℃干燥12小时，得到BaB8O11(OH)4纳米盘(见图7)。

Claims (1)

1.一种BaB8O11(OH)4纳米阻燃材料的制备方法，其特征在于：将钡源和硼源加入溶剂中，混合均匀，所得混合物在密闭条件下反应，将反应产物依次用60～80℃蒸馏水、乙醇洗涤后干燥，得到BaB8O11(OH)4纳米阻燃材料；
所述的钡源为硝酸钡、硼源为八水合五硼酸铵、溶剂为去离子水，钡元素与硼元素的摩尔比为1:10～17，在密闭条件下150～180℃下反应12～24小时时，得到的BaB8O11(OH)4纳米阻燃材料为纳米片形貌；
所述的钡源为醋酸钡、硼源为硼酸、溶剂为去离子水，钡元素与硼元素的摩尔比为1:5～12，在密闭条件下160～200℃下反应12～18小时时，得到的BaB8O11(OH)4纳米阻燃材料为纳米带形貌；
所述的钡源为醋酸钡、硼源为硼酸、溶剂为乙二醇，钡元素与硼元素的摩尔比为1:2～8，在密闭条件下160～200℃下反应12～18小时时，得到的BaB8O11(OH)4纳米阻燃材料为纳米盘形貌。
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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH04243998A (ja) * 1991-01-28 1992-09-01 Sumitomo Metal Mining Co Ltd β−メタホウ酸バリウム単結晶の製造方法
CN1669923A (zh) * 2004-03-16 2005-09-21 中国科学院福建物质结构研究所 一种低温相偏硼酸钡纳米粉体的制备方法
CN101781571A (zh) * 2009-12-18 2010-07-21 苏州科技学院 一种复合膨胀型阻燃剂

Family Cites Families (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2002020695A1 (de) * 2000-09-08 2002-03-14 Nanosolutions Gmbh Dotierte nanopartikel
CN1183035C (zh) * 2000-12-07 2005-01-05 中国科学院福建物质结构研究所 低温相偏硼酸钡纳米粉的制备方法
KR100813601B1 (ko) * 2006-09-28 2008-03-17 삼성전기주식회사 저온 소결용 나노글라스 분말의 제조방법
CN101186307B (zh) * 2007-11-28 2011-03-02 华南理工大学 水热反应制备偏硼酸钡纳米线的方法
CN101913619B (zh) * 2010-09-29 2012-09-05 河北大学 一种偏硼酸钡纳米粉体的制备方法
CN103738996B (zh) * 2013-12-13 2015-07-01 绵阳市远达新材料有限公司 一种纳米碳酸钡的制备方法
CN104017336A (zh) * 2014-06-20 2014-09-03 曲铭海 一种纳米硼酸钡溶胶的制备方法及其在聚酯阻燃中的应用

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH04243998A (ja) * 1991-01-28 1992-09-01 Sumitomo Metal Mining Co Ltd β−メタホウ酸バリウム単結晶の製造方法
CN1669923A (zh) * 2004-03-16 2005-09-21 中国科学院福建物质结构研究所 一种低温相偏硼酸钡纳米粉体的制备方法
CN101781571A (zh) * 2009-12-18 2010-07-21 苏州科技学院 一种复合膨胀型阻燃剂

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
"Role of reaction time in tuning the morphology and third order nonlinear optical properties of barium borate";T.C.Sabari Girisun et al;《Optics and Laser Technology》;20161013;第89卷;第54-58页 *

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