CN112376269A - 一种气凝胶复合纤维毡结构件及其制备方法 - Google Patents
一种气凝胶复合纤维毡结构件及其制备方法 Download PDFInfo
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Abstract
本发明提供一种气凝胶复合纤维毡结构件，由以下重量份的原料制成：气凝胶粉100份、润湿分散剂5‑10份、纤维毡90‑110份、增稠剂6‑9份、增韧剂8‑10份、热稳定剂2‑4份、阻燃剂3‑6份、防霉剂4‑8份、去离子水140‑150份。本发明还公开了该气凝胶复合纤维毡结构件的制备方法。本发明提供的气凝胶复合纤维毡结构件具有较高的强度，能制成异形结构件。
Description
技术领域
本发明涉及一种结构件，特别是涉及一种气凝胶复合纤维毡结构件及其制备方法。
背景技术
目前的保温绝热材料主要分为两大类：一类是有机类保温材料，如挤塑聚苯板，聚氨酯泡沫等，这类材料保温效果好、比重轻，且防水性和耐候性好，广泛应用于建筑外墙外保温及工业领域，但是有机保温材料易燃，燃烧时易释放大量有害物质，存在重大的安全隐患；另一类是传统无机类保温材料如膨胀珍珠岩，发泡水泥板等，这类材料的防火性能优异，在高温下不燃烧不分解，但保温效果不及传统有机材料，其导热系数普遍在0.04W/(m﹒K)以上。
二氧化硅气凝胶是三维空间网络结构的纳米多孔非晶固体材料，其低导热系数的优点使其在绝热保温领域有着广泛的应用前景，气凝胶保温绝热材料不但导热系数低、质量轻，同时兼具耐高温的特性，但超轻气凝胶还具有机械强度低、韧性差的特点，通常需使其与其他基材复合增强其力学性能，而与纤维复合制备的气凝胶毡由于其质量轻、柔韧性好、适用广泛的特点成为保温绝热领域的热门产品。现有的气凝胶毡主要以玻璃纤维作为骨架材料，柔性、强度不足，不能模压定型，不适合制作成异形结构件，限制了气凝胶复合制品在汽车等领域的使用。
发明内容
本发明要解决的技术问题是提供一种气凝胶复合纤维毡结构件，其具有较高的强度，能制成异形结构件。
为解决上述技术问题，本发明的技术方案是：
一种气凝胶复合纤维毡结构件，由以下重量份的原料制成：气凝胶粉100份、润湿分散剂5-10份、纤维毡90-110份、增稠剂6-9份、增韧剂8-10份、热稳定剂2-4份、阻燃剂3-6份、防霉剂4-8份、去离子水140-150份。
进一步地，本发明所述气凝胶粉为二氧化硅气凝胶粉，气凝胶粉的细度为10-50微米，密度为20-150克/升。
进一步地，本发明所述润湿分散剂为十二烷基磺酸钠、油酸丁酯、聚氧乙烯烷基醚、聚氧乙烯乙二醇烷基酯、聚磷酸盐中的其中一种。
进一步地，本发明所述纤维毡由聚乙烯纤维、聚丙烯纤维、聚氯乙烯纤维、聚苯乙烯纤维或聚酯纤维制成。
进一步地，本发明所述增稠剂为羟甲基纤维素。
进一步地，本发明所述增韧剂为聚乙烯蜡。
进一步地，本发明所述热稳定剂为硬脂酸锌。
进一步地，本发明所述阻燃剂为三氧化二锑。
进一步地，本发明所述防霉剂的制备步骤为：
A1.将西番莲果实的果皮60℃下干燥2小时，粉碎后过200目筛得到西番莲果皮粉，以1:25g/mL的比例将西番莲果皮粉加入70%浓度的乙醇溶液中，60℃下恒温提取1.5小时得到浸提液，将浸提液蒸除溶剂后冷冻干燥得到西番莲果皮提取物；
A2.将活性白土加入20倍重量的去离子水中，50℃下搅拌1小时后滴加入氢氧化钙，直至pH值稳定为止后抽滤得到滤饼一，将滤饼一100℃下干燥3小时，粉碎后过200目筛得到改性白土；
A3.将西番莲果皮提取物加入去离子水中，搅拌至混合均匀后加入改性白土，50℃下搅拌3小时后抽滤得到滤饼二，将滤饼二100℃下干燥2小时，粉碎后过200目筛得到防霉剂。
本发明要解决的另一技术问题是提供上述气凝胶复合纤维毡结构件的制备方法。
为解决上述技术问题，技术方案是：
一种气凝胶复合纤维毡结构件的制备方法，包括以下步骤：
B1.按重量份称取各原料，将除了纤维毡之外的原料混合，搅拌至混合均匀得到气凝胶溶液；
B2.将纤维毡浸泡于气凝胶溶液中10-12小时后取出，100-150℃下干燥2小时得到气凝胶复合纤维毡；
B3.将气凝胶复合纤维毡置于平面模腔中，200℃下预热软化2分钟，然后转移至冷模中冷却定型即得气凝胶复合纤维毡结构件。
与现有技术相比，本发明具有以下有益效果：
1）本发明是先将气凝胶与其他助剂混合配制成气凝胶溶液，然后将纤维毡浸泡于气凝胶溶液中进行复合，再经过高温软化冷却模压成型制得强度较高、可以制成异形结构件的气凝胶复合纤维结构件。
2)本发明将西番莲果实的果皮部分通过乙醇提取法提取得到西番莲果皮提取物，其具有较强的防霉抑菌活性，不过其热稳定性不佳，因而本发明将活性白土用氢氧化钙改性后再与西番莲果皮提取物混合制得主要成分是改性白土负载西番莲果皮提取物的防霉剂，改性白土的热稳定性较好，能对西番莲果皮提取物提供较好的热保护作用，因此该防霉剂能有效提高气凝胶复合纤维毡结构件的防霉性能。
具体实施方式
下面将结合具体实施例来详细说明本发明，在此本发明的示意性实施例以及说明用来解释本发明，但并不作为对本发明的限定。
实施例1
气凝胶复合纤维毡结构件，由以下重量份的原料制成：气凝胶粉100份、十二烷基磺酸钠8份、纤维毡100份、羟甲基纤维素7份、聚乙烯蜡9份、硬脂酸锌3份、三氧化二锑5份、防霉剂6份、去离子水145份。其中，气凝胶粉为二氧化硅气凝胶粉，二氧化硅气凝胶粉的细度为10-50微米，密度为20-150克/升；纤维毡由聚乙烯纤维制成；防霉剂的制备步骤为：
A1.将西番莲果实的果皮60℃下干燥2小时，粉碎后过200目筛得到西番莲果皮粉，以1:25g/mL的比例将西番莲果皮粉加入70%浓度的乙醇溶液中，60℃下恒温提取1.5小时得到浸提液，将浸提液蒸除溶剂后冷冻干燥得到西番莲果皮提取物；
A2.将活性白土加入20倍重量的去离子水中，50℃下搅拌1小时后滴加入氢氧化钙，直至pH值稳定为止后抽滤得到滤饼，将滤饼100℃下干燥3小时，粉碎后过200目筛得到改性白土；
A3.将西番莲果皮提取物加入去离子水中，搅拌至混合均匀后加入改性白土，50℃下搅拌3小时后抽滤得到滤饼，将滤饼100℃下干燥2小时，粉碎后过200目筛得到防霉剂。
该气凝胶复合纤维毡结构件的制备方法包括以下步骤：
B1.按重量份称取各原料，将除了纤维毡之外的原料混合，搅拌至混合均匀得到气凝胶溶液；
B2.将纤维毡浸泡于气凝胶溶液中11小时后取出，120℃下干燥2小时得到气凝胶复合纤维毡；
B3.将气凝胶复合纤维毡置于平面模腔中，200℃下预热软化2分钟，然后转移至冷模中冷却定型即得气凝胶复合纤维毡结构件。
对比例1
与实施例1的主要区别在于组分中不包括防霉剂。
对比例2
与实施例1的主要区别在于防霉剂替换为西番莲果皮提取物，省去步骤A2、A3。
对比例3：市售气凝胶毡，由二氧化硅气凝胶与玻璃纤维复合而成
试验例一：
使用万能试验机分别测试实施例1、对比例1-3的抗压强度，加载速度为15mm/分，抗压强度为测试样品在应变50%时的应力值。测试结果如下表所示：
| 样品 | 抗压强度（MPa） |
| 实施例1 | 1.324 |
| 对比例1 | 1.323 |
| 对比例2 | 1.324 |
| 对比例3 | 0.347 |
由上表可以看出，本发明实施例1的抗压强度明显高于对比例3，表明本发明制得的气凝胶复合纤维毡结构件具有较高的抗压强度。
试验例二：
参考ASTM G21-1996分别测试实施例1、对比例1-3的防霉等级，测试菌种为黑曲霉、球毛壳霉、绿粘帚霉、绳状青霉、出芽短梗霉，防霉等级分为0级、1级、2级、3级、4级，0级表示防霉性能最好，等级越高防霉性能越差。测试结果如下表所示：
| 样品 | 防霉等级 |
| 实施例1 | 0级 |
| 对比例1 | 2级 |
| 对比例2 | 1级 |
| 对比例3 | 2级 |
由上表可以看出，本发明实施例1的防霉等级明显低于对比例3，表明本发明制得的气凝胶复合纤维毡结构件具有较好的防霉性能。对比例1的防霉等级上升至2级，表明本发明使用的防霉剂能有效提高气凝胶复合纤维毡结构件的防霉性能；对比例2的防霉等级上升至1级，表明在没有改性白土负载保护的情况下，西番莲果皮提取物对气凝胶复合纤维毡结构件防霉性能的提高效果比较有限，改性白土能对西番莲果皮提取物起到有效的热保护作用。
实施例2
气凝胶复合纤维毡结构件，由以下重量份的原料制成：气凝胶粉100份、油酸丁酯10份、纤维毡90份、羟甲基纤维素8份、聚乙烯蜡8份、硬脂酸锌2.5份、三氧化二锑4份、防霉剂5份、去离子水140份。其中，气凝胶粉为二氧化硅气凝胶粉，二氧化硅气凝胶粉的细度为10-50微米，密度为20-150克/升；纤维毡由聚丙烯纤维制成；防霉剂的制备步骤与实施例1相同。
该气凝胶复合纤维毡结构件的制备方法包括以下步骤：
B1.按重量份称取各原料，将除了纤维毡之外的原料混合，搅拌至混合均匀得到气凝胶溶液；
B2.将纤维毡浸泡于气凝胶溶液中10小时后取出，100℃下干燥2小时得到气凝胶复合纤维毡；
B3.将气凝胶复合纤维毡置于平面模腔中，200℃下预热软化2分钟，然后转移至冷模中冷却定型即得气凝胶复合纤维毡结构件。
实施例3
气凝胶复合纤维毡结构件，由以下重量份的原料制成：气凝胶粉100份、聚氧乙烯烷基醚5份、纤维毡110份、羟甲基纤维素9份、聚乙烯蜡8.5份、硬脂酸锌4份、三氧化二锑3份、防霉剂4份、去离子水150份。其中，气凝胶粉为二氧化硅气凝胶粉，二氧化硅气凝胶粉的细度为10-50微米，密度为20-150克/升；纤维毡由聚氯乙烯纤维制成；防霉剂的制备步骤与实施例1相同。
该气凝胶复合纤维毡结构件的制备方法包括以下步骤：
B1.按重量份称取各原料，将除了纤维毡之外的原料混合，搅拌至混合均匀得到气凝胶溶液；
B2.将纤维毡浸泡于气凝胶溶液中10.5小时后取出，110℃下干燥2小时得到气凝胶复合纤维毡；
B3.将气凝胶复合纤维毡置于平面模腔中，200℃下预热软化2分钟，然后转移至冷模中冷却定型即得气凝胶复合纤维毡结构件。
实施例4
气凝胶复合纤维毡结构件，由以下重量份的原料制成：气凝胶粉100份、聚氧乙烯乙二醇烷基酯6份、纤维毡105份、羟甲基纤维素6份、聚乙烯蜡10份、硬脂酸锌2份、三氧化二锑6份、防霉剂8份、去离子水147份。其中，气凝胶粉为二氧化硅气凝胶粉，二氧化硅气凝胶粉的细度为10-50微米，密度为20-150克/升；纤维毡由聚苯乙烯纤维制成；防霉剂的制备步骤与实施例1相同。
该气凝胶复合纤维毡结构件的制备方法包括以下步骤：
B1.按重量份称取各原料，将除了纤维毡之外的原料混合，搅拌至混合均匀得到气凝胶溶液；
B2.将纤维毡浸泡于气凝胶溶液中10.5小时后取出，110℃下干燥2小时得到气凝胶复合纤维毡；
B3.将气凝胶复合纤维毡置于平面模腔中，200℃下预热软化2分钟，然后转移至冷模中冷却定型即得气凝胶复合纤维毡结构件。
实施例5
气凝胶复合纤维毡结构件，由以下重量份的原料制成：气凝胶粉100份、聚磷酸盐6份、纤维毡105份、羟甲基纤维素6份、聚乙烯蜡10份、硬脂酸锌2份、三氧化二锑6份、防霉剂8份、去离子水147份。其中，气凝胶粉为二氧化硅气凝胶粉，二氧化硅气凝胶粉的细度为10-50微米，密度为20-150克/升；纤维毡由聚酯纤维制成；防霉剂的制备步骤与实施例1相同。
该气凝胶复合纤维毡结构件的制备方法包括以下步骤：
B1.按重量份称取各原料，将除了纤维毡之外的原料混合，搅拌至混合均匀得到气凝胶溶液；
B2.将纤维毡浸泡于气凝胶溶液中10.5小时后取出，110℃下干燥2小时得到气凝胶复合纤维毡；
B3.将气凝胶复合纤维毡置于平面模腔中，200℃下预热软化2分钟，然后转移至冷模中冷却定型即得气凝胶复合纤维毡结构件。
实施例6
气凝胶复合纤维毡结构件，由以下重量份的原料制成：气凝胶粉100份、硅酸盐6份、纤维毡105份、羟甲基纤维素6份、聚乙烯蜡10份、硬脂酸锌2份、三氧化二锑6份、防霉剂8份、去离子水147份。其中，气凝胶粉为二氧化硅气凝胶粉，二氧化硅气凝胶粉的细度为10-50微米，密度为20-150克/升；纤维毡由聚酯纤维制成；防霉剂的制备步骤与实施例1相同。
该气凝胶复合纤维毡结构件的制备方法包括以下步骤：
B1.按重量份称取各原料，将除了纤维毡之外的原料混合，搅拌至混合均匀得到气凝胶溶液；
B2.将纤维毡浸泡于气凝胶溶液中10.5小时后取出，110℃下干燥2小时得到气凝胶复合纤维毡；
B3.将气凝胶复合纤维毡置于平面模腔中，200℃下预热软化2分钟，然后转移至冷模中冷却定型即得气凝胶复合纤维毡结构件。
上述实施例仅例示性说明本发明的原理及其功效，而非用于限制本发明。任何熟悉此技术的人士皆可在不违背本发明的精神及范畴下，对上述实施例进行修饰或改变。因此，举凡所属技术领域中具有通常知识者在未脱离本发明所揭示的精神与技术思想下所完成的一切等效修饰或改变，仍应由本发明的权利要求所涵盖。
Claims (10)
1.一种气凝胶复合纤维毡结构件，其特征在于：由以下重量份的原料制成：气凝胶粉100份、润湿分散剂5-10份、纤维毡90-110份、增稠剂6-9份、增韧剂8-10份、热稳定剂2-4份、阻燃剂3-6份、防霉剂4-8份、去离子水140-150份。
2.根据权利要求1所述的一种气凝胶复合纤维毡结构件，其特征在于：所述气凝胶粉为二氧化硅气凝胶粉，气凝胶粉的细度为10-50微米，密度为20-150克/升。
3.根据权利要求1所述的一种气凝胶复合纤维毡结构件，其特征在于：所述润湿分散剂为十二烷基磺酸钠、油酸丁酯、聚氧乙烯烷基醚、聚氧乙烯乙二醇烷基酯、聚磷酸盐中的其中一种。
4.根据权利要求1所述的一种气凝胶复合纤维毡结构件，其特征在于：所述纤维毡由聚乙烯纤维、聚丙烯纤维、聚氯乙烯纤维、聚苯乙烯纤维或聚酯纤维制成。
5.根据权利要求1所述的一种气凝胶复合纤维毡结构件，其特征在于：所述增稠剂为羟甲基纤维素。
6.根据权利要求1所述的一种气凝胶复合纤维毡结构件，其特征在于：所述增韧剂为聚乙烯蜡。
7.根据权利要求1所述的一种气凝胶复合纤维毡结构件，其特征在于：所述热稳定剂为硬脂酸锌。
8.根据权利要求1所述的一种气凝胶复合纤维毡结构件，其特征在于：所述阻燃剂为三氧化二锑。
9.根据权利要求1所述的一种气凝胶复合纤维毡结构件，其特征在于：所述防霉剂的制备步骤为：
A1.将西番莲果实的果皮60℃下干燥2小时，粉碎后过200目筛得到西番莲果皮粉，以1:25g/mL的比例将西番莲果皮粉加入70%浓度的乙醇溶液中，60℃下恒温提取1.5小时得到浸提液，将浸提液蒸除溶剂后冷冻干燥得到西番莲果皮提取物；
A2.将活性白土加入20倍重量的去离子水中，50℃下搅拌1小时后滴加入氢氧化钙，直至pH值稳定为止后抽滤得到滤饼一，将滤饼一100℃下干燥3小时，粉碎后过200目筛得到改性白土；
A3.将西番莲果皮提取物加入去离子水中，搅拌至混合均匀后加入改性白土，50℃下搅拌3小时后抽滤得到滤饼二，将滤饼二100℃下干燥2小时，粉碎后过200目筛得到防霉剂。
10.根据权利要求1-9任意一项所述的气凝胶复合纤维毡结构件的制备方法，其特征在于：包括以下步骤：
B1.按重量份称取各原料，将除了纤维毡之外的原料混合，搅拌至混合均匀得到气凝胶溶液；
B2.将纤维毡浸泡于气凝胶溶液中10-12小时后取出，100-150℃下干燥2小时得到气凝胶复合纤维毡；
B3.将气凝胶复合纤维毡置于平面模腔中，200℃下预热软化2分钟，然后转移至冷模中冷却定型即得气凝胶复合纤维毡结构件。
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