CN111763080B - 一种空心莫来石微球及其制备方法 - Google Patents

一种空心莫来石微球及其制备方法 Download PDF

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CN111763080B
CN111763080B CN202010572934.8A CN202010572934A CN111763080B CN 111763080 B CN111763080 B CN 111763080B CN 202010572934 A CN202010572934 A CN 202010572934A CN 111763080 B CN111763080 B CN 111763080B
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hollow mullite
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黎兆早
余恺为
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Shenzhen Cailianwei Technology Co.,Ltd.
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Abstract

本发明公开了一种空心莫来石微球，包括按质量百分比计的以下组分：氢氧化铝：30‑35％；氧化铝：20‑40％；二氧化硅：20‑25％；烧结助剂：1‑5％；粘合剂：3‑8％；保护剂：0.5‑2％；本发明还提供了对应的制备方法；本发明的方案，通过优化其配方配比，结合独特的制备方法，制得的空心莫来石微球，具有高强度、低密度及小孔径的优点。

Description

一种空心莫来石微球及其制备方法
技术领域
本发明涉及无机非金属材料领域，更具体地说，它涉及一种空心莫来石微球及其制备方法。
背景技术
莫来石材料因其具备耐腐蚀、比重小、熔点高、抗热震性好、热导率低和高温强度大等优点，广泛应用于冶金、机械、陶瓷、电子、建材、石化、航天航空等多个领域。
具有针状或纤维状显微结构的空心球状形貌的莫来石，因其拥有球壳内外疏松和较多的孔隙，加之其具有的较大比表面积和一定的耐压强度，在许多领域获得青睐和重视。
但目前的莫来石微球在制作过程中需要添加钠钙离子减低熔融温度，导致生成的微球壳层致密度差，外壳硬度偏低，为了单方面提升硬度和耐压以增厚玻璃微球壳层，导致密度增高，孔径大的缺点。
发明内容
针对现有技术存在的不足，本发明的目的在于提供一种空心莫来石微球，能提升微球的耐压力，减少微球密度，降低微球孔径，同时可减低制作成本等优点；本发明还提供了相应的制备方法。
本发明的上述技术目的是通过以下技术方案得以实现的：包括按质量百分比计的以下组分：氢氧化铝：30-35％；氧化铝：20-40％；二氧化硅：20-25％；烧结助剂：1-5％；粘合剂：3-8％；保护剂：0.5-2％。
进一步地，所述烧结助剂为氧化锌、二氧化钛、氧化锆、氧化镁中的至少一种。
进一步地，所述粘合剂为正硅酸乙酯、正硅酸甲酯、原硅酸钠中的至少一种。
进一步地，所述保护剂为葡萄糖、壳聚糖中的至少一种。
本发明还提供了上述空心莫来石微球的制备方法，包括以下步骤：
S1、按比例称各组分，混合后放入球磨罐中进行慢速球磨处理至分散均匀，得到混合物A；
S2、将有机溶剂、三乙醇胺、分散剂、交联剂、硅烷偶联剂和去离子水混合；在搅拌罐中恒温50℃搅拌3小时，得到混合物B；其中，混合物B中各组分的质量百分比如下：有机溶剂：10-15％；三乙醇胺：1-3％；分散剂：2-5％；交联剂：0.5-2％；硅烷偶联剂：30-40％；去离子水：30-40％；
S3、合并混合物A和混合物B于另一搅拌罐中，恒温50℃下搅拌6小时至混合均匀，得到混合物C；
S4、将混合物C转移至压力搅拌罐，调节PH值为7.5-9.0，在压力1.2-1.5Mpa下搅拌3小时；
S5、将压力罐的压力减至0.2-0.5Mpa，温度60℃下搅拌16小时，静置1小时后，升温至80℃并保持30分钟；
S6、过滤S5中得到的混合物，得到沉淀物和滤液；分三次用去离子水盥洗沉淀物，并收集盥洗后的滤液；
S7、将沉淀物在80℃中烘烤保温3小时；
S8、将沉淀物转入高温炉进行烧结，升温至1200℃保温12小时至烧结，自然降温至室温；
S9、将烧结后的沉淀物雾化喷淋去离子水；
S10、将雾化喷淋后的沉淀物在80℃烤箱中烘烤1小时，得到空心的莫来石微球。
进一步地，所述步骤S8的升温过程中，包括以下步骤：先升温至400℃保温3小时，再升至600℃保温3小时，升至900℃保温3小时，再升至1200℃。
进一步地，所述有机溶剂为丙三醇、戊二醇、异丙醇、无水乙醇、甲醇中的至少一种。
进一步地，所述分散剂为硬脂酸钠、硬脂酸钙、硬脂酸锌中的至少一种。
进一步地，所述交联剂为乙烯基三乙氧基硅烷、乙烯基三甲氧基硅烷中的至少一种。
进一步地，所述硅烷偶联剂为巯基丙基三甲氧基硅烷、聚二甲基硅氧烷、氨丙基甲基二乙氧基硅烷中的至少一种。
综上所述，本发明具有以下有益效果：
其一，本发明的技术方案，通过优化其配方配比，筛选获得合适的及添加剂，制备过程中无需添加钠钙离子减低熔融温度，所制备的莫来石空心球材料具有高强度、低密度和小孔径的优点。
其二，本发明的方案，先将有机溶剂、三乙醇胺、分散剂、交联剂、硅烷偶联剂和去离子水在搅拌罐中混合，得到混合物B的乳化体系，再与混合物A在压力搅拌罐中升压搅拌，混合物B在混合物A的表面形成水包油的体系，在高温烧结过程中，不会破坏微球的内部结构，制得的空心莫来石微球，具有高强度、低密度及小孔径的优点，使其适应高压力注塑设备，能够提升各种塑料或橡胶材料轻量化等特性。
其三，步骤S3中，采用压力搅拌罐，控制反应条件在压力1.2-1.5Mpa进行，触发混合物A和混合B的反应条件，有利于形成水包油的体系。
其四，步骤S8的升温过程中，高温烧结过程采用曲线烧结，可对微球进行的孔径收缩约1/3,同时便于控制微球的空心率。
其五，本发明的工艺及设备简单，空心莫来石微球成分比现有的玻璃微球致密，而硬度比现有的玻璃微球高；具有提升微球的耐压力，减少产品密度，降低微球孔径，减低制作成本等优点。
附图说明
图1是本发明中实施例1所制空心莫来石微球的的扫描电镜照片。
具体实施方式
下面结合附图和实施例，对本发明进行详细描述。
实施例1：
一种空心莫来石微球，其组分的质量组成,如表1所示，
组分 质量(kg)
氢氧化铝 30
氧化铝 20
二氧化硅 20
氧化锌 1
正硅酸甲酯 3.6
聚壳糖 2
搅拌罐中各组分的质量组成，如表2所示，
Figure BDA0002550070770000041
Figure BDA0002550070770000051
制备方法包括以下步骤：
S1、按表1的百分比称取氢氧化铝、氧化铝、二氧化硅、氧化锌、正硅酸甲酯、聚壳糖，混合后放入球磨罐中进行慢速球磨处理12小时至分散均匀，得到混合物A；
S2、按表2中各组分的百分比，准确称取各组分并置于搅拌罐中；在搅拌罐中恒温50℃，转速400转/分钟，搅拌3小时，得到混合物B；
S3、合并混合物A和混合物B于另一搅拌罐中，恒温50℃下，转速200转/分钟，搅拌6小时至混合均匀，得到混合物C；
S4、将混合物C转移至压力搅拌罐，加入柠檬酸钠调节PH值为8，在压力1.2Mpa下搅拌3小时；
S5、加入柠檬酸钠调节混合物C的PH为8.5，将压力罐的压力减至0.2Mpa，温度60℃下搅拌16小时，静置1小时后，升温至80℃并保持30分钟；
S6、过滤S5中得到的混合物，得到沉淀物和滤液；分三次用去离子水盥洗沉淀物，并收集盥洗后的滤液；
S7、将沉淀物在80℃中烘烤保温3小时；
S8、将沉淀物转入高温炉烧结，升至400℃保温3小时，升至600℃保温3小时，升至900℃保温3小时，升至1200℃保温12小时至烧结，自然降温至室温；
S9、将烧结后的沉淀物雾化喷淋去离子水；
S10、将雾化喷淋后的沉淀物在80℃烤箱中烘烤1小时，得到空心的莫来石微球。
实施例2:
一种空心莫来石微球，其物料的质量组成,如表3所示。
表3：
组分 质量(kg)
氢氧化铝 50
二氧化硅 20
氧化锌 1
正硅酸甲酯 1.6
正硅酸已酯 2.2
葡萄糖 2
搅拌罐中各组分的质量组成，如表4所示。
表4：
Figure BDA0002550070770000061
Figure BDA0002550070770000071
制备方法如下：
S1、按表3中各组分的百分比，准确称取各组分，混合后放入球磨罐中进行慢速球磨处理12小时至分散均匀，得到混合物A；
S2、按表4中各组分的百分比，准确称取各组分并置于搅拌罐中；在搅拌罐中恒温50℃，转速400转/分钟，搅拌3小时，得到混合物B；
S3、合并混合物A和混合物B于另一搅拌罐中，恒温50℃下，转速200转/分钟，搅拌6小时至混合均匀，得到混合物C；
S4、将混合物C转移至压力搅拌罐，加入柠檬酸钠调节PH值为8.5，在压力1.2Mpa下搅拌3小时；
S5、加入柠檬酸钠调节混合物C的PH为8.5，将压力罐的压力减至0.2Mpa，温度60℃下搅拌16小时，静置1小时后，升温至80℃并保持30分钟；
S6、过滤S5中得到的混合物，得到沉淀物和滤液；分三次用去离子水盥洗沉淀物，并收集盥洗后的滤液；
S7、将沉淀物在80℃中烘烤保温3小时；
S8、将沉淀物转入高温炉烧结，升至400℃保温3小时，升至600℃保温3小时，升至900℃保温3小时，升至1200℃保温12小时至烧结，自然降温至室温；
S9、将烧结后的沉淀物雾化喷淋去离子水；
S10、将雾化喷淋后的沉淀物在80℃烤箱中烘烤1小时，得到空心的莫来石微球。
实施例3：
一种空心莫来石微球，其物料的质量组成,如表5所示，
表5：
组分 质量(kg)
氢氧化铝 50
二氧化硅 30
氧化锌 1
正硅酸甲酯 1.6
正硅酸已酯 2.2
葡萄糖 2
搅拌罐中各组分的质量组成，如表6所示。
表6：
Figure BDA0002550070770000081
Figure BDA0002550070770000091
制备方法包括以下步骤：
S1、按表5中各组分的百分比，准确称取各组分，混合后放入球磨罐中进行慢速球磨处理12小时至分散均匀，得到混合物A；
S2、按表6中各组分的百分比，准确称取各组分并置于搅拌罐中；在搅拌罐中恒温50℃，转速400转/分钟，搅拌3小时，得到混合物B；
S3、合并混合物A和混合物B于另一搅拌罐中，恒温50℃下，转速200转/分钟，搅拌6小时至混合均匀，得到混合物C；
S4、将混合物C转移至压力搅拌罐，加入柠檬酸钠调节PH值为8.5，在压力1.2Mpa下搅拌3小时；
S5、加入柠檬酸钠调节混合物C的PH为8.5，将压力罐的压力减至0.2Mpa，温度60℃下搅拌16小时，静置1小时后，升温至80℃并保持30分钟；
S6、过滤S5中得到的混合物，得到沉淀物和滤液；分三次用去离子水盥洗沉淀物，并收集盥洗后的滤液；
S7、将沉淀物在80℃中烘烤保温3小时；
S8、将沉淀物转入高温炉烧结，升至400℃保温3小时，升至600℃保温3小时，升至900℃保温3小时，升至1200℃保温12小时至烧结，自然降温至室温；
S9、将烧结后的沉淀物雾化喷淋去离子水；
S10、将雾化喷淋后的沉淀物在80℃烤箱中烘烤1小时，得到空心的莫来石微球。
以上实施例都可以制备获得最终产品空心莫来石微球，分别测试实施例1-3制得的空心莫来石微球的孔径、耐压力和微球密度。并对实施例1制得的空心莫来石微球进行电镜扫描，扫描结果见图1。
测试结果如表7所示。
表7：
测试项目 实施例1 实施例2 实施例3
孔径(um) 30 20 12
耐压力(psi) 20000 25000 30000
密度(t/m<sup>3</sup>) 0.5 0.6 0.6
根据表7及图1的数据可见，本发明的方案，通过优化其配方配比，结合独特的制备方法，制得的空心莫来石微球的孔径为在12-20um之间，耐压力可达20000-30000psi，密度为0.3-0.7t/m3。与现有技术相比，具有高强度、低密度及小孔径的优点，使其适应高压力注塑设备，提升各种塑料或橡胶材料轻量化等特性。
本发明采用压力搅拌罐，控制反应条件在压力1.2-1.5Mpa进行，触发混合物A和混合B的反应条件，混合物B在混合物A的表面形成水包油的体系，在后续的高温烧结过程中，不会破坏微球的内部结构，制得的空心莫来石微球，具有高强度、低密度及小孔径的优点。
以上所述仅是本发明的优选实施方式，本发明的保护范围并不仅局限于上述实施例，凡属于本发明思路下的技术方案均属于本发明的保护范围。应当指出，对于本技术领域的普通技术人员来说，在不脱离本发明原理前提下的若干改进和润饰，这些改进和润饰也应视为本发明的保护范围。

Claims (9)

1.一种空心莫来石微球的制备方法，其特征在于,包括以下步骤：
S1、按比例称取空心莫来石微球各组分，混合后放入球磨罐中进行慢速球磨处理至分散均匀，得到混合物A; 其中所述空心莫来石微球各组分包括以下原料: 氢氧化铝、氧化铝、二氧化硅、烧结助剂、粘合剂、及保护剂；所述粘合剂为正硅酸乙酯、正硅酸甲酯、原硅酸钠中的至少一种；所述保护剂为葡萄糖、壳聚糖中的至少一种；
S2、将有机溶剂、三乙醇胺、分散剂、交联剂、硅烷偶联剂和去离子水混合；在搅拌罐中恒温50℃搅拌3小时，得到混合物B;其中，混合物B中各组分的质量百分比如下：有机溶剂：10-15%；三乙醇胺：1-3%；分散剂：2-5%；交联剂：0.5-2%；硅烷偶联剂：30-40%；去离子水：30-40%；
S3、合并混合物A和混合物B于另一搅拌罐中，恒温50℃下搅拌6小时至混合均匀，得到混合物C；
S4、将混合物C转移至压力搅拌罐，调节pH值为7.5-9.0，在压力1.2-1.5Mpa下搅拌3小时；
S5、将压力罐的压力减至0.2-0.5Mpa，温度60℃下搅拌16小时，静置1小时后，升温至80℃并保持30分钟；
S6、过滤S5中得到的混合物，得到沉淀物和滤液；分三次用去离子水盥洗沉淀物，并收集盥洗后的滤液；
S7、将沉淀物在80℃中烘烤保温3小时；
S8、将沉淀物转入高温炉进行烧结，升温至1200℃保温12小时至烧结，自然降温至室温；
S9、将烧结后的沉淀物雾化喷淋去离子水；
S10、将雾化喷淋后的沉淀物在80℃烤箱中烘烤1小时，得到空心的莫来石微球。
2.根据权利要求1所述的空心莫来石微球的制备方法，其特征在于，所述步骤S8的升温过程中，包括以下步骤：先升温至400℃保温3小时，再升至600℃保温3小时，升至900℃保温3小时，再升至1200℃。
3.根据权利要求1所述的空心莫来石微球的制备方法，其特征在于，所述有机溶剂为丙三醇、戊二醇、异丙醇、无水乙醇、甲醇中的至少一种。
4.根据权利要求1所述的空心莫来石微球的制备方法，其特征在于，所述分散剂为硬脂酸钠、硬脂酸钙、硬脂酸锌中的至少一种。
5.根据权利要求1所述的空心莫来石微球的制备方法，其特征在于，所述交联剂为乙烯基三乙氧基硅烷、乙烯基三甲氧基硅烷中的至少一种。
6.根据权利要求1所述的空心莫来石微球的制备方法，其特征在于，所述硅烷偶联剂为巯基丙基三甲氧基硅烷、聚二甲基硅氧烷、氨丙基甲基二乙氧基硅烷中的至少一种。
7.根据权利要求1所述的空心莫来石微球的制备方法，其特征在于，步骤S1中所述的空心莫来石微球各组分包括以下质量百分比原料：氢氧化铝：30-35%；氧化铝：20-40%；二氧化硅：20-25%；烧结助剂：1-5%；粘合剂：3-8%；保护剂：0.5-2%。
8.根据权利要求7所述的空心莫来石微球的制备方法，其特征在于，所述烧结助剂为氧化锌、二氧化钛、氧化锆、氧化镁中的至少一种。
9.一种根据权利要求1-8任一项所述的空心莫来石微球的制备方法制备得到的空心莫来石微球。
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