CN1320189C - 氧化铝纤维聚集体及其制造方法 - Google Patents

氧化铝纤维聚集体及其制造方法 Download PDF

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CN1320189C
CN1320189C CNB028024591A CN02802459A CN1320189C CN 1320189 C CN1320189 C CN 1320189C CN B028024591 A CNB028024591 A CN B028024591A CN 02802459 A CN02802459 A CN 02802459A CN 1320189 C CN1320189 C CN 1320189C
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alumina
fiber
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short fibre
spinning solution
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CN1464924A (zh
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荘司守
池田宪雄
笹木利明
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Mitsubishi Kagaku Sanshi Corp
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Abstract

一种由平均纤维直径为4.0～10.0μm且最低纤维直径为3.0μm以上的氧化铝短纤维制成的氧化铝纤维聚集体、以及其制造方法，利用吹制法对含有碱性氯化铝、硅化合物、有机聚合物及水的纺丝液进行纺丝，然后对所得到的氧化铝短纤维前驱体的聚集体进行烧制，其特征在于：使用铝和硅之比换算成Al2O3和SiO2的重量比为99∶1～65∶35、碱性氯化铝的浓度为180～200g/L、有机聚合物的浓度为20～40g/L的纺丝液作为上述的纺丝液。上述的氧化铝纤维聚集体，因增大氧化铝短纤维直径从而抑制氧化铝短纤维飞散。

Description

氧化铝纤维聚集体及其制造方法
技术领域
本发明涉及氧化铝纤维聚集体及其制造方法。
背景技术
氧化铝纤维聚集体具有优良的耐热性，发挥它的这一特性，加工成氧化铝纤维支架等作为隔热材料等使用。这样的纤维支架，例如用下面这样的方法能制造出来。
即，利用吹制法对含有碱性氯化铝、硅化合物、有机聚合物及水的纺丝液进行纺丝，根据需要将所得到的氧化铝短纤维前驱体的聚集体(层压片)实施针刺后进行烧制。而且，在烧制工序中，除去挥发成份的同时，进行氧化铝和硅的结晶化，转换成氧化铝纤维。结果，得到了由氧化铝短纤维制成的氧化铝纤维聚集体。一般把这样的制造方法叫做前驱体纤维化法。
可是，当氧化铝短纤维直径小时，氧化铝短纤维容易飞散，操作性恶化，同时，工作环境卫生上也不好。也就是指出直径在数μm以下的纤维容易通过呼吸进入人体的肺泡等问题。
发明内容
本发明鉴于上述实际情况，其目的在于提供一种由氧化铝短纤维制成的纤维聚集体、即因增大氧化铝短纤维直径从而抑制氧化铝短纤维飞散的纤维聚集体及其制造方法。
本发明人经过反复深入地研究，结果发现：氧化铝短纤维的直径随着所使用的纺丝液的特性而变化，使用特定性状的纺丝液，而且在最佳的纺丝条件下，得到纤维直径大且纤维直径分布小的氧化铝短纤维。由此完成了本发明。
本发明是基于上述的想法而完成的。第一个要点在于纤维聚集体的特征，其特征是由平均纤维直径为4.0～10.0μm且最低纤维直径为3.0μm以上的氧化铝短纤维制成。
而且，本发明的第二个要点在于氧化铝纤维聚集体的制造方法，利用吹制法对含有碱性氯化铝、硅化合物、有机聚合物及水的纺丝液进行纺丝，然后对所得到的氧化铝短纤维前驱体的聚集体进行烧制，其特征在于：使用铝和硅之比换算成Al2O3和SiO2的重量比为99∶1～65∶35、碱性氯化铝的浓度为180～200g/L、有机聚合物的浓度为20～40g/L的纺丝液作为上述的纺丝液，由平均纤维直径为4.0～10.0μm且最低纤维直径为3.0μm以上的氧化铝短纤维制成氧化铝纤维聚集体。
以下详细说明本发明。因说明的方便，首先说明本发明的氧化铝纤维聚集体的制造方法。
本发明的制造方法是：利用吹制法对含有碱性氯化铝、硅化合物、有机聚合物及水的纺丝液进行纺丝，然后对所得到的氧化铝短纤维前驱体的聚集体进行烧制(前驱体纤维化法)。而且，主要由纺丝液的调制工序、纺丝工序、烧制工序构成，根据需要，在纺丝工序和烧制工序之间设置针刺工序。
<纺丝液的调制工序>
碱性氯化铝；Al(OH)3-XClX，例如可以通过使金属铝溶解于盐酸或氯化铝的水溶液中来进行调制。上述的化学式中的X的值通常为0.45～0.54，优选为0.50～0.53。作为硅化合物，以使用硅溶胶为宜，但也可以使用其它的四乙基硅酸盐或水溶性硅氧烷衍生物等水溶性硅化合物。作为有机聚合物，以使用例如聚乙烯醇、聚乙二醇、聚丙烯酰胺等水溶性高分子化合物。这些物质的聚合度通常为1000～3000。
在本发明中，使用铝和硅之比换算成Al2O3和SiO2的重量比为99∶1～65∶35、碱性氯化铝的浓度为180～200g/L、有机聚合物的浓度为20～40g/L的纺丝液作为上述的纺丝液是重要的。
硅化合物的量比上述的范围少时，构成短纤维的氧化铝容易产生α-氧化铝，而且，由于氧化铝微粒的粗大化容易引起短纤维的脆化。另一方面，硅化合物的量比上述的范围多时，与模来石(3Al2O3·2SiO2)同时生成的二氧化硅(SiO2)的量增加，耐热性低下。换算成Al2O3和SiO2的重量比的铝和硅之比通常为99∶1～65∶35，优选为99∶1～70∶30，更优选为98∶2～72∶28。
碱性氯化铝的浓度不足180g/L时或者有机聚合物的浓度不足20g/L时，都不能得到适应性的粘度，纤维直径减小。即，纺丝液中的游离水过多的结果，由于使用吹制法，纺丝时干燥速度慢，延伸过度，纺丝的前驱体纤维的纤维直径发生变化，不能得到纤维直径大且纤维直径分布小的短纤维。而且，碱性氯化铝的浓度不足180g/L时，生产性降低。另一方面，碱性氯化铝的浓度超过200g/L时或者有机聚合物的浓度超过40g/L时，都使粘度过高，形不成纺丝液。碱性氯化铝的优选浓度为185～195g/L，有机聚合物的优选浓度为30～40g/L。
通过把硅化合物及有机聚合物添加到碱性氯化铝的水溶液中，将碱性氯化铝及有机聚合物的浓度浓缩到上述的范围，调制成上述的纺丝液。在常温下，纺丝液的粘度通常为1～1000泊，优选为10～100泊。
<纺丝>
纺丝(纺丝液的纤维化)是通过将纺丝液供给于高速的纺丝气流中的吹制法进行的，由此，得到长度为数十mm～数百mm的氧化铝短纤维前驱体。
上述纺丝时使用的纺丝嘴的构造没有特别的限制，但优选例如欧洲专利第495466号公报(日本特许第2602460号公报)中记述的那样，由空气嘴吹出的空气流和由纺丝液供给嘴挤出的纺丝液流成为并行流，而且，空气的并行流被充分整流并与纺丝液接触的构造。这时，纺丝嘴的直径通常为0.1～0.5mm，每个纺丝液供给嘴的液量通常为1～120ml/h，优选为3～50ml/h；来自空气嘴的每个开口的气体流速通常为40～200m/s。
按照上述那样的纺丝管嘴，由于从纺丝液供给嘴挤出的纺丝液不会成为雾状而被充分延伸，纤维相互难以熔融粘合，所以通过将纺丝条件最佳化，可得到纤维直径分布狭窄均匀的氧化铝纤维前驱体。
另外，在纺丝时，首先优选为，在抑制水分蒸发和纺丝液分解的条件下，形成从纺丝液充分延伸的纤维，接着，迅速干燥这种纤维。因此，在从纺丝液形成纤维至到达纤维捕集器的过程中，优选使氛围气体从抑制水分蒸发的状态变化到促进水分蒸发的状态。因此，纺丝液与空气流开始接触的附近的温度优选为10～20℃，纤维捕集器附近的空气流的温度优选为40～50℃，相对湿度优选为不足30％。
在由纺丝液应形成充分延伸的纤维的阶段，氛围气体的温度过高时，由于水分急剧蒸发等，难以形成充分延伸的纤维，另外，在形成的纤维中产生缺陷，最终取得的无机氧化物纤维脆化。另一方面，为了抑制蒸发，在低温或高湿度氛围气体中，由纺丝液形成纤维时，因为纤维形成后还继续在同一氛围气体中，纤维相互粘附，又由于弹性回复而液滴化，容易发生喷丸(shot)，所以不可取。
以与纺丝气流近乎呈直角的方式设置金属网制的无端带子，一边使无端带子转动，一边使它与含有氧化铝短纤维前驱体的纺丝气流在此处冲撞，通过如上这样构造的收集装置，可以回收氧化铝短纤维前驱体的聚集体作为连续片(薄层片)。
由上述的收集装置回收的薄层片，连续引出并送到折叠装置，一边按规定的宽度折叠摞起来，一边相对于折叠方向呈直角方向连续移动，由此能形成层压片。由此，因为薄层片宽度方向的两端部配置在所形成的层压片的内侧，所以层压片的观察量成为片全体均匀。可以使用欧洲公开专利第971057号公报(日本公开特许2000-80547号公报)中记述的装置作为上述的折叠装置。
<针刺工序>
通过在氧化铝短纤维前驱体的聚集体(层压片)上施行针刺，可以成为在厚度方向也定向的机械强度大的氧化铝纤维聚集体。针刺的打数通常为1～50打/cm2，一般来说，打数越多，所得到的氧化铝纤维聚集体的体积密度和剥离强度越大。
<烧制工序>
烧制通常在500℃以上、优选为700～1400℃的温度下进行。烧制温度不足500℃时，只能得到结晶不充分、强度小且脆弱的氧化铝短纤维，烧制温度超过1400℃时，只能得到纤维结晶的颗粒正在成长、强度小且脆弱的氧化铝短纤维。
下面，说明本发明的氧化铝短纤维聚集体。本发明的氧化铝纤维聚集体，例如可以用上述那样的制造方法得到，其构造由氧化铝短纤维构成。而且，构成氧化铝纤维聚集体的氧化铝短纤维的纤维直径大且纤维直径分布小。即，本发明的氧化铝纤维集合具有如下特征：氧化铝短纤维的平均纤维直径为4.0～10.0μm、且最低纤维直径在3.0μm以上。氧化铝短纤维的平均纤维直径的下限优选为4.0μm，更优选为5.0μm。另外，氧化铝短纤维的平均纤维直径优选为5.0～8.0μm，更优选为6.0～8.0μm。
纤维直径小的物质多时，纤维容易飞散，操作性恶化，同时工作环境卫生上也不好。另外，纤维直径太大时，一般来说，氧化铝短纤维的聚集体的隔热性、弹力性等降低，因此不可取。以上的度数分布是指根据后述的纤维直径分布的测定方法测定的值。另外，由此得到的氧化铝短纤维的长度通常为10～500mm。
本发明的氧化铝纤维聚集体具有上述这样的特征，因此例如在氧化铝纤维毯子的制造工序等中的操作处理时，纤维飞散少，操作性及工作环境卫生方面优良。
具体实施方式
以下，根据实施例更详细地说明本发明。就本发明来说，只要不超过其要点，就不局限于以下的实施例。另外，在以下的各个实施例中，测定氧化铝单纤维的纤维直径分布是按下面所示的次序进行的。
<纤维直径分布的测定方法>
(1)从氧化铝纤维垫上用小镊子摘取约1掏耳勺量的纤维。
(2)把上述(1)摘取的纤维尽量不重叠地放置在碳制导电带上，该碳制导电带贴在扫描型电子显微镜(SEM)观察用试样台上。
(3)为了使上述(2)的纤维表面具有导电性，在试样表面蒸镀1～3nm厚的铂-钯膜。
(4)把蒸镀的分析试样放入到SEM的测定室，在适当的倍率下进行观察，并拍摄观察图像，测定纤维直径。作为装置，使用日本电子社制的扫描型电子显微镜“JSM-6320F”，作为观察条件，采用加速电压15KV、工作距离(WD)15mm。另外，适宜选择的倍率范围为1000～3000。
(5)上述(4)拍摄的SEM照片，用游标卡尺或直尺测量到单位为0.1mm。而且测定任意合计100根的纤维直径。
(6)用下面的式子计算平均纤维直径。这时，计算值在小数点以下2位四舍五入，保留小数点以下1位。
(7)另外，在此从纤维直径的度数分布的倾向看，对下限的纤维直径产生疑义时，通常反复测定2～4次，把度数分布在平均1％以上的直径当作最低纤维直径。
平均纤维直径(μm)＝{100点的合计测定值/(100×观察倍率)}
                   ×1,000
实施例1
<纺丝液的调制>
首先，在每1.0L的铝浓度为165g/L的碱性氯化铝：Al(OH)3-XClX(X＝0.51)的水溶液中添加20重量％硅溶胶溶液606g、5重量％聚乙烯醇(聚合度1700)水溶液608g并进行混合后，在50℃下减压浓缩，得到纺丝液。纺丝液的粘度为60泊(25℃下由旋转粘度计测定的测定值)，铝和硅之比(Al2O3和SiO2的重量比)为72.0∶28.0，碱性氯化铝的浓度为190g/L，有机聚合物的浓度为35.0g/L。
<纺丝>
用吹制法对上述的纺丝液进行纺丝。纺丝嘴是使用与欧洲专利第495466号公报(日本特许第2602460号公报)图6记述的构造相同的纺丝嘴。而且，纺丝在下述条件下进行：纺丝液供给嘴的直径为0.3mm，每根纺丝液供给嘴的液量为5ml/h，空气流速(空气嘴的开口部)：54m/s(压力：2kg/cm2、温度：18℃、相对湿度40％)。另外，集棉时，通过将干燥的150℃的温风与高速空气流并行地导入到屏(screen)上，将纤维捕集器附近的空气流调节至温度为40℃、相对湿度为20％。而且，以与纺丝气流近乎呈直角的方式设置金属网制的无端带子，一边使无端带子转动，一边使它与含有氧化铝短纤维前驱体的纺丝气流在此处冲撞，通过如上这样构造的收集装置，可以回收氧化铝短纤维前驱体的聚集体作为连续片(薄层片)。
由收集装置回收的薄层片，连续引出并送到折叠装置，一边按规定的宽度折叠摞起来，一边相对于折叠方向呈直角方向连续移动，由此能形成层压片。可以使用欧洲公开专利第971057号公报(日本公开特许2000-80547号公报)中记述的装置作为上述的折叠装置。
<氧化铝纤维聚集体的制造>
对上述的层压片(氧化铝短纤维前驱体的聚集体)实施针刺后，在1250℃的空气中烧制1小时，得到氧化铝纤维聚集体。上述的针刺由针刺机进行8次/cm2的穿刺。测定所得到的氧化铝纤维聚集体的构成氧化铝短纤维的纤维直径分布，结果如表1所示。平均纤维直径为6.9μm，最低纤维直径为5.2μm。
实施例2
<纺丝液的调制>
首先，在每1.0L的铝浓度为165g/L的碱性氯化铝：Al(OH)3-XClX(X＝0.51)的水溶液中添加20重量％硅溶胶溶液606g、5重量％聚乙烯醇(聚合度1700)水溶液608g并进行混合后，在50℃下减压浓缩，得到纺丝液。纺丝液的粘度为40泊(25℃下由旋转粘度计测定的测定值)，铝和硅之比(Al2O3和SiO2的重量比)为72.0∶28.0，碱性氯化铝的浓度为180g/L，有机聚合物的浓度为33.2g/L。
<纺丝及氧化铝纤维聚集体的制造>
与实施例1同样地进行。测定所得到的氧化铝纤维聚集体的构成氧化铝短纤维的纤维直径分布，结果如表1所示。平均纤维直径为4.9μm，最低纤维直径为3.3μm。
比较例1
<纺丝液的调制>
在每1.0L的铝浓度为75g/L的碱性氯化铝：Al(OH)3-XClX(X＝0.56)的水溶液中添加20重量％硅溶胶溶液276g、5重量％聚乙烯醇(聚合度1700)水溶液315g并进行混合后，在50℃下减压浓缩，得到纺丝液。纺丝液的粘度为40泊(25℃下由旋转粘度计测定的测定值)，铝和硅之比(Al2O3和SiO2的重量比)为72.0∶28.0，碱性氯化铝的浓度为160g/L，有机聚合物的浓度为33.6g/L。
<纺丝及氧化铝纤维聚集体的制造>
使用与实施例1相同的纺丝嘴。而且，纺丝在如下条件下进行：纺丝液供给嘴的直径为0.3mm，每根纺丝液供给嘴的液量为5ml/h，空气流速(空气嘴的开口部)：54m/s(压力：2kg/cm2、温度：18℃、相对湿度40％)。另外，集棉时，通过将干燥的90℃的温风与高速空气流并行地导入到屏(screen)上，将纤维捕集器附近的空气流调节至温度为35℃、相对湿度为30％。而且，由与实施例1同样的集绵装置、收集装置回收连续片(薄层片)。测定所得到的氧化铝纤维聚集体的构成氧化铝短纤维的纤维直径分布，结果如表1所示。平均纤维直径为6.6μm，最低纤维直径为2.2μm。
比较例2
<纺丝液的调制>
在每1.0L的铝浓度为165g/L的碱性氯化铝：Al(OH)3-XClX(X＝0.51)的水溶液中添加20重量％硅溶胶溶液606g、5重量％聚乙烯醇(聚合度1700)水溶液260g并进行混合后，在50℃下减压浓缩，得到纺丝液。纺丝液的粘度为8泊(25℃下由旋转粘度计测定的测定值)，铝和硅之比(Al2O3和SiO2的重量比)为72.0∶28.0，碱性氯化铝的浓度为190g/L，有机聚合物的浓度为15.0g/L。
<纺丝及氧化铝纤维聚集体的制造>
与实施例1同样地进行。测定所得到的氧化铝纤维聚集体的构成氧化铝短纤维的纤维直径分布，结果如表1所示。平均纤维直径为2.3μm，最低纤维直径为0.4μm。
比较例3
<纺丝液的调制>
在每1.0L的铝浓度为165g/L的碱性氯化铝：Al(OH)3-XClX(X＝0.51)的水溶液中添加20重量％硅溶胶溶液606g、5重量％聚乙烯醇(聚合度1700)水溶液550g并进行混合后，在50℃下减压浓缩，将铝和硅之比(Al2O3和SiO2的重量比)调节为72.0∶28.0，将碱性氯化铝的浓度调节为210g/L，将有机聚合物的浓度调节为35.0g/L。但是，所得到的组合物在浓缩阶段呈现固化状态，得不到纺丝液。
比较例4
<纺丝液的调制>
在每1.0L的铝浓度为165g/L的碱性氯化铝：Al(OH)3-XClX(X＝0.51)的水溶液中添加20重量％硅溶胶溶液606g、5重量％聚乙烯醇(聚合度1700)水溶液868g并进行混合后，在50℃下减压浓缩，将铝和硅之比(Al2O3和SiO2的重量比)调节为72.0∶28.0，将碱性氯化铝的浓度调节为190g/L，将有机聚合物的浓度调节为50.0g/L。但是，所得到的组合物在浓缩阶段粘度过高，成为不能用旋转粘度计进行适当粘度测定的状态，不是能纺丝的性状。
表1
<度数分布>
 纤维直径(μm)   实施例1   实施例2   比较例1   比较例2
 0.0≤   -   -   -   2
 0.5≤   -   -   -   9
 1.0≤   -   -   -   18
 1.5≤   -   -   -   25
 2.0≤   -   -   1   15
 2.5≤   -   -   5   5
 3.0≤   -   1   8   6
 3.5≤   -   6   3   7
 4.0≤   -   13   8   3
 4.5≤   -   33   18   2
 5.0≤   5   18   11   2
 5.5≤   13   21   9   3
 6.0≤   32   1   7   1
 6.5≤   21   4   3   -
 7.0≤   8   -   5   1
 7.5≤   7   -   3   -
 8.0≤   5   -   2   1
 8.5≤   3   -   5   -
 9.0≤   1   -   2   -
 9.5≤   1   -   4   -
 10.0≤   4   -   6   -
 点数   100   100   100   100
 平均   6.9   4.9   6.6   2.3
 下限   5.2   3.3   2.2   0.4
参考例1
现有的氧化铝纤维的平均纤维直径一般为2～5μm，对三个公司市售的氧化铝纤维进行了分析。结果如表2所示。
表2
 平均纤维直径(μm)  最低纤维直径(μm)
A公司产品   第一组  3.6  1.1
  第二组  3.7  1.4
  第三组  4.6  1.8
  第四组  3.0  0.7
 B公司产品  3.0  1.3
 C公司产品   第一组  3.5  1.1
  第二组  4.2  1.8
  第三组  4.7  2.2
产业上的可利用性
根据以上所说明的本发明，提供一种由氧化铝短纤维制成的氧化铝纤维聚集体、即因增大氧化铝短纤维直径从而抑制氧化铝短纤维飞散的氧化铝纤维聚集体及其制造方法。在操作处理这样的氧化铝聚集体时，纤维飞散少，操作性和工作环境卫生方面优良。因此，本发明的工业价值显著。

Claims (8)

1.一种氧化铝纤维聚集体，其特征在于：由平均纤维直径为4.0～10.0μm且最低纤维直径为3.0μm以上的氧化铝短纤维制成。
2.如权利要求1所述的氧化铝纤维聚集体，其特征在于：由最低纤维直径为4.0μm以上的氧化铝短纤维制成。
3.如权利要求1所述的氧化铝纤维聚集体，其特征在于：由最低纤维直径为5.0μm以上的氧化铝短纤维制成。
4.如权利要求1～3中任一项所述的氧化铝纤维聚集体，其特征在于：由平均纤维直径为5.0～8.0μm的氧化铝短纤维制成。
5.如权利要求1～3中任一项所述的氧化铝纤维聚集体，其特征在于：由平均纤维直径为6.0～8.0μm的氧化铝短纤维制成。
6.如权利要求1～3中任一项所述的氧化铝纤维聚集体，其特征在于：氧化铝短纤维的组成用Al2O3和SiO2的重量比来表示为99∶1～65∶35。
7.一种权利要求1～3中任一项所述的氧化铝纤维聚集体的制造方法，利用吹制法对含有碱性氯化铝、硅化合物、水溶性高分子化合物及水的纺丝液进行纺丝，然后对所得到的氧化铝短纤维前驱体的聚集体以500℃～1400℃的温度进行烧制，所述硅化合物是硅溶胶或水溶性硅化合物，其特征在于：使用铝和硅之比换算成Al2O3和SiO2的重量比为99∶1～65∶35、碱性氯化铝的浓度为180～200g/L、水溶性高分子化合物的浓度为20～40g/L的纺丝液作为所述的纺丝液。
8.如权利要求7所述的氧化铝纤维聚集体的制造方法，其特征在于：在所述纺丝工序和所述烧制工序之间具有针刺工序。
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