CN105408009B - 具有改善的机械特性的陶瓷空心纤维膜 - Google Patents
具有改善的机械特性的陶瓷空心纤维膜 Download PDFInfo
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Abstract
本发明涉及一种用于制备基于氧化铝的陶瓷空心纤维膜的方法，其通过湿式纺丝工艺由纺丝原液制备。为此在该纺丝原液中加入二次相。
Description
技术领域
本发明一般性涉及陶瓷空心纤维膜。本发明具体涉及具有改善的机械特性的这类空心纤维膜。本发明还涉及用于制备这类空心纤维膜的方法。
背景技术
过滤法或分离法对气体和液体的浓缩和分离具有很大的经济意义。在此领域越来越多地应用膜技术。在此情况下，空心纤维膜在过滤工艺或浓缩工艺中的应用随之带来一系列的优点。
因为面积对体积之比相对高，所以浓缩工艺或过滤工艺的效率也高；此外该方法也易于实施，并适合于各类需求。
早期的商用空心纤维膜由聚合物材料制成，所以对腐蚀条件和较高温度是敏感的。因此很快制备出陶瓷空心纤维膜，例如通过在碳丝上的蒸汽冷凝和接着去除该碳丝来制备。
用于制备陶瓷型空心纤维的现今已知的方法包括纺丝工艺，在该工艺的第一步骤中，由含陶瓷材料前体的可纺丝原液和聚合物来制备弹性的生纤维（Grünfaser）。接着在高温下烧去该聚合物成分，并形成纯的陶瓷型空心纤维。
基于金属氧化物如Al2O3的陶瓷空心纤维膜由于结构特性及其几何形态仅达到低的强度值。如在3-点-弯曲试验中的断裂力仅为约6 N，这换算成弯曲断裂强度相当于约为33 MPa。
该空心纤维膜的高机械应力主要在操作时和在进一步加工中(如在模块结构中)以及在空心纤维运输中 (作为单部件或以模块形式) 和在压力冲击或压力梯度下的运行中出现，以致有时会出现高的废品率。如果该空心纤维已构建到模块中，则要消除例如由运输造成的纤维断裂的缺陷是特别复杂的。
有关这方面，DE 102009038814 A1公开了一种模块元件，其包括一个具有用于引入陶瓷毛细管膜的至少一个通孔的耐高温的基体，EP 0941759 A1描述了一种用于制备空心纤维膜模块的方法。
由CN 102515817 A已知制备具有高过滤流量的陶瓷空心纤维膜。该纤维的组成(以重量%计)为40-80份粉末状的硅酸铝水合物、10-20份粉末状的塑性耐火粘土、1-10份粉末状的钠长石、1-10份粉末状的白云石、6-10份粉末状的硅酸硼玻璃粉、1-7份羧甲基纤维素和1-3份甘油。该纤维的外径为3-6 mm，内径为1-2 mm，该纤维长度为100-1000 mm。总孔隙度为50-56 %，水流量为10000-12500 L/m2hMPa和弯曲断裂强度为35-85 MPa。
发明内容
因此，本发明的目的在于提供陶瓷空心纤维膜，其在保持迄今的空心纤维膜的孔隙度和流量效率下具有改善的机械特性。
本发明的上述目的通过本发明的方法和空心纤维膜实现。本发明的用于由纺丝原液制备陶瓷空心纤维膜的方法的特征在于包括下列步骤：
-由溶剂、聚合物和陶瓷粉末制备纺丝原液；
-向纺丝原液中加入二次相；
-将纺丝原液喷入沉淀浴中，其中聚合物通过与沉淀剂接触而凝固；和
-烧结所获得的生坯，
其中所述陶瓷空心纤维膜的制备基于氧化物陶瓷材料进行或者基于非氧化物陶瓷材料进行，
其中该二次相是由纳米级伊利石组成的玻璃相。
本发明的陶瓷空心纤维膜基于氧化物陶瓷材料或者基于非氧化物陶瓷材料，其特征在于，其具有由纳米级伊利石组成的二次玻璃相。
在本发明的一个特别的实施方案中，该二次相是玻璃相。
在本发明的一个优选实施方案中，该玻璃相是纳米级的lllit。
本发明的空心纤维膜主要适用于微滤、超滤、纳滤和气体分离，特别是适用于水净化 (废水净化、饮用水处理等) 领域或油-水分离领域，如其在石油-和天然气工业中应用。
具体实施方案
通过使用纺丝原液的纺丝工艺制备空心纤维膜，其中作为基础配剂的纺丝原液由溶剂、聚合物和陶瓷粉末 (氧化铝) 以及用于稳定悬浮体的分散剂组成。通常，这类空心纤维膜的强度的升高导致较低的孔隙度和由此也造成较低的过滤效率。
已经发现，在用于制备基于氧化物陶瓷材料如氧化铝、ZrO2或TiO2，或基于非-氧化物陶瓷材料如Si3N4、AlN或WC的陶瓷空心纤维膜的陶瓷空心纤维的基础配剂中加入二次相却抵消这种发展。该二次相优选由玻璃相组成，其加入量为基于总固体计约0.5-10 %。
纳米级 (即1-200 nm数量级) 的lllit即天然存在的三层式层状硅酸盐特别适合作为玻璃相，其化学主成分为：47.0 % ± 3.5 % SiO2、21.0 % ± 2.0 % Al2O3、7.0 % ±1.0 % Fe2O3、4.0 % ± 2.0 % CaO、5.5 % ± 0.7 % K2O、3.0 % ±0.75 % MgO、0.15 % ±0.05 % Na2O、0.8 % ± 0.1 % TiO2、0.3 % ± 0.08 % P2O5、11.0 % ± 2.0 % GV (总杂质)。也可使用合成的玻璃粉或天然粘土矿物替代lllit。
常用的基于氧化铝的陶瓷型空心纤维大多通过湿式纺丝法制备，其中所用的由溶剂、使用的聚合物和沉淀剂组成的三物质体系具有混合缺陷，由此溶于纺丝原液中的聚合物通过与沉淀剂的接触而凝固。该陶瓷颗粒通过此过程嵌入聚合物基质中。经干燥步骤后，该所制备的生坯仍由聚合物和氧化铝组成。接着实施烧结过程，以通过形成烧结颈结合陶瓷颗粒并烧去聚合物，由此制备多孔型陶瓷膜。
通过按本发明将二次相 (玻璃相) 引入纺丝原液中，成功制备了由聚合物、氧化铝和玻璃相组成的生坯。通过随后的烧结工艺制备的空心纤维膜的强度值约为13 N，其是按通常制备的空心纤维膜的强度值的两倍多，其中可保留无玻璃体系的纤维几何形状尺寸(外径0.8-5.0 mm，内径0.5-4.8 mm)、孔结构、总孔隙度 (40-60 %) 和纯水渗透率(10000-30000 l/m2/h/bar)。由此，例如与通过加入由研磨玻璃粉合成制备的玻璃料相比，甚至可实现明显更高的强度值 (＞ 30 %)。
由于以本发明可实现的机械稳定性的明显提高，可大大降低废品率，并由此大大降低由操作、再加工以及运输所产生的成本。
本发明的这类空心纤维膜主要适用于微滤、超滤、纳滤和气体分离，特别是适用于水净化 (废水净化、饮用水处理等) 领域。其它的应用领域是食品工业和饮料工业以及化学工业或石油天然气工业中的过滤。
在制备时的烧结温度可降低至多约200 ℃，在此，该机械稳定性仍处于纯陶瓷体系的相应水平。在制备其机械特性与不加玻璃相时所得的机械特性相当的空心纤维膜时，可以以此方式节省能量。
如果在该空心纤维膜的结构中的玻璃相在其后的运行中由于侵蚀 (例如pH 14的热碱液) 而局部或甚至全部溶出，该基础机械强度仍保持在无玻璃体系的水平，即该机械稳定性不会降低到低于不加玻璃相时所得的机械稳定性。
Claims (10)
1.用于由纺丝原液制备陶瓷空心纤维膜的方法，其特征在于下列步骤：
-由溶剂、聚合物和陶瓷粉末制备纺丝原液；
-向纺丝原液中加入二次相；
-将纺丝原液喷入沉淀浴中，其中聚合物通过与沉淀剂接触而凝固；和
-烧结所获得的生坯，
其中所述陶瓷空心纤维膜的制备基于氧化物陶瓷材料进行或者基于非氧化物陶瓷材料进行，
其中该二次相是由纳米级伊利石组成的玻璃相。
2.根据权利要求1的方法，其特征在于，所述氧化物陶瓷材料为氧化铝、ZrO2或TiO2。
3.根据权利要求1的方法，其特征在于，所述非氧化物陶瓷材料为Si3N4、AlN或WC。
4.根据权利要求1-3之一的方法，其特征在于，该二次相的加入量为基于总固体计0.5-10 %。
5.通过权利要求1-4之一的方法获得的陶瓷空心纤维膜，其基于氧化物陶瓷材料或者基于非氧化物陶瓷材料，其特征在于，其具有由纳米级伊利石组成的二次玻璃相。
6.根据权利要求5的陶瓷空心纤维膜，其特征在于，所述氧化物陶瓷材料为氧化铝、ZrO2或TiO2。
7.根据权利要求5的陶瓷空心纤维膜，其特征在于，所述非氧化物陶瓷材料为Si3N4、AlN或WC。
8.根据权利要求5-7之一的陶瓷空心纤维膜在微滤、超滤或气体分离中的应用。
9.根据权利要求5-7之一的陶瓷空心纤维膜在水处理中的应用。
10.根据权利要求9的应用，用于废水处理。
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| CN109731553A (zh) * | 2019-03-12 | 2019-05-10 | 海安县中丽化工材料有限公司 | 一种TiO2@Mofs改性玻璃纤维膜的制备方法 |
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| EP3027299A1 (de) | 2016-06-08 |
| US20160136582A1 (en) | 2016-05-19 |
| US10857505B2 (en) | 2020-12-08 |
| ES2792223T3 (es) | 2020-11-10 |
| CN108452686A (zh) | 2018-08-28 |
| EP3027299B1 (de) | 2020-04-08 |
| US10029214B2 (en) | 2018-07-24 |
| US20190015791A1 (en) | 2019-01-17 |
| CN105408009A (zh) | 2016-03-16 |
| WO2015014624A1 (de) | 2015-02-05 |
| CN108452686B (zh) | 2021-06-29 |
| DE102013012671A1 (de) | 2015-02-05 |
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