CN115538150A - 一种超疏水-超亲油织物及其制备方法 - Google Patents
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Abstract
本发明涉及一种超疏水‑超亲油织物的制备方法。本发明所述的一种超疏水‑超亲油织物的制备方法包括以下步骤：S1：将织物浸泡在碱液或酸液中刻蚀，然后水洗去除碱液或酸液，烘干；S2：将步骤S1得到的织物放入异氰酸酯或改性异氰酸酯溶液中浸泡，取出，加热固化，得到超疏水‑超亲油织物；所述改性异氰酸酯为异氰酸酯与含羟基聚硅氧烷反应得到。本发明提供的超疏水‑超亲油织物的制备方法，成本低廉，性能优异，有望广泛应用于织物防水、油水分离、染料污水处理等多个领域。
Description
技术领域
本发明涉及功能纺织材料领域，特别是涉及一种超疏水-超亲油织物及其制备方法。
背景技术
超疏水是指水在材料表面的静态接触角大于等于150°，使材料具有自清洁性，可用于织物防水领域。超疏水和超亲油织物在油水分离领域也得到了广泛的应用。
通常采用仿生学“荷叶效应”的方法制备超疏水表面，即在材料表面构建特定的微/纳米级分层结构和/或低表面能改性物质引入基材表面。通常将无机纳米材料引入到织物表面形成一定的粗糙度，然后接枝低表面能链段(如有机硅或含氟单体)。然而，无机纳米材料容易在使用过程中脱落而使材料失去超疏水效果。为提高耐用性，需在织物和无机纳米材料表面涂覆大量的有机低表面能涂层，但是，这会大大降低织物的透气性和柔韧性，从而不易通过水洗的方法去除织物表面的油污。并且含氟单体价格昂贵并且具有毒性限制了其使用。另外超疏水织物的制备工艺复杂、成本高也是限制其广泛应用的原因。
发明内容
为解决目前超疏水织物的制备工艺复杂、成本高、不易水洗除污以及透气性和柔韧性差等技术问题。本发明提供一种超疏水-超亲油织物及其制备方法：通过刻蚀织物表面，使其具有一定的表面粗糙度，然后接枝低表面能链段制备超疏水表面，制备的超疏水织物在外力作用下(如揉搓)变为超亲水，干燥后为超疏水的可逆转变。并且不改变原织物的透气性和柔韧性，另外，得到的超疏水织物超亲油，可应用于油水分离领域。该发明方法简便、成本低和无毒等优点，有利于大规模工业化生产。
一种超疏水-超亲油织物的制备方法，包括以下步骤：
S1：将织物浸泡在碱液或酸液中刻蚀，然后水洗去除碱液或酸液，烘干；
S2：将步骤S1得到的织物放入异氰酸酯或改性异氰酸酯溶液中浸泡，取出加热固化，得到超疏水-超亲油织物；
所述改性异氰酸酯为异氰酸酯与含羟基聚硅氧烷反应得到。
本发明通过碱液或酸液刻蚀织物，使其具有一定的表面粗糙度，当经异氰酸酯浸泡固化后，在棉织物表面进一步形成微/纳米的超疏水结构。当经改性异氰酸酯浸泡固化，因为异氰酸酯上接枝有低表面能的聚硅氧烷，使其在棉织物表面进一步形成微/纳米的超疏水结构的表面能进一步降低，进一步加强其超疏水性能。其中，加热固化的原理是：使异氰酸酯或改性异氰酸酯溶液中的-NCO基团与织物上的羟基反应，将异氰酸酯或改性异氰酸酯溶液接枝到织物表面，形成超疏水表面。制备得到的超疏水织物在外力作用下(如揉搓)变为超亲水，干燥后为超疏水的可逆转变。并且不改变原织物的透气性和柔韧性，另外，得到的超疏水织物超亲油，可应用于油水分离领域。该发明方法简便、成本低和无毒等优点，有利于大规模工业化生产。
进一步地，所述的碱液包括氢氧化钠、氢氧化钾、氢氧化钡、氨水、氢氧化钙中的一种或多种。
进一步地，所述的酸液包括硫酸、硝酸、盐酸、醋酸、氢氟酸和次氯酸中的一种或多种。
进一步地，所述碱液或酸液浓度为0.1～20mol/L。浓度过高对织物损伤过大，浓度过低刻蚀效果有限。
进一步地，所述碱液或酸液浓度为1～10mol/L。
进一步地，所述异氰酸酯包括对苯二异氰酸酯、1,4-环己烷二异氰酸酯、甲苯二异氰酸酯、二甲基联苯二异氰酸酯、多亚甲基多苯基异氰酸酸酯、异佛尔酮二异氰酸酯、二环己基二异氰酸酯、环己烷二亚甲基二异氰酸酯、1,6-六亚甲基二异氰酸酯、HDI三聚体、异佛尔酮二异氰酸酯三聚体、L-赖氨酸三异氰酸酯中的一种或多种。
进一步地，所述改性异氰酸酯由以下方法制备：将异氰酸酯与含羟基聚硅氧烷按摩尔比0.5～10:1混合，在60～120℃下反应0.5～5h，得到改性异氰酸酯。异氰酸酯中的-NCO与含羟基聚硅氧烷中的羟基反应，将低表面能的聚硅氧烷接枝到异氰酸酯，得到低表面能的改性异氰酸酯。
进一步地，所述含羟基聚硅氧烷包括单末端单羟基改性硅油、单末端双羟基改性硅油、两末端羟基改性硅油中的一种或多种，分子量为100～20000。
进一步地，所述的加热固化温度为40～150℃，加热时间为0.1～5h。
一种超疏水-超亲油织物，采用上述超疏水-超亲油织物的制备方法制备得到。
本发明提供一种超疏水-超亲油织物及其制备方法。该方法通过刻蚀织物表面，使其具有一定的表面粗糙度，然后接枝低表面能链段制备超疏水表面。水接触角大于150°，并且在水中外力揉搓可变为超亲水表面，方便通过水洗去除织物表面油污，干燥后仍为超疏水表面。并且不改变原织物的透气性和柔韧性。另外，该方法制备的超疏水织物超亲油，可在水面上和水面下快速吸取油类、有机溶剂和染料，吸取后可通过挤压、溶剂清洗和蒸发后重复使用。本发明制备工艺简便可行，成本低廉，性能优异，有望广泛应用于织物防水、油水分离、染料污水处理等多个领域。
为了更好地理解和实施，下面结合附图详细说明本发明。
附图说明
图1为实施例1未刻蚀前棉织物的电镜图。
图2为实施例1碱刻蚀后棉织物的电镜图。
图3为实施例1HDI三聚体固化后的电镜图。
图4为实施例1改性织物对水中苏丹红染色的石蜡油选择性吸收清除的过程图。
具体实施方式
实施例1
首先，用去离子水清洗棉织物，在100℃下干燥后，在8mol/L氨水中浸渍90分钟。将刻蚀后的棉织物经过三次水洗除去碱液，然后烘干棉织物浸泡在HDI三聚体中。3小时后取出，在60℃加热固化3小时得到功能化织物。水接触角测试结果为152°。
参见图1-3。由图2和图1的电镜图对比可知，碱刻蚀后棉织物表面形成一定的表面粗糙度。由图3和图2的电镜图对比可知，经HDI三聚体浸泡固化后在棉织物表面进一步形成微/纳米的超疏水结构。参见图4，其为改性织物对水中苏丹红染色的石蜡油选择性吸收清除的过程图，图中石蜡油和染料极易吸附在改性织物，由于具有超疏水效果，吸取后织物没有被水润湿。
实施例2
首先，用去离子水清洗棉织物，在100℃下干燥后，在8mol/L NaOH溶液中浸渍30分钟。将刻蚀后的棉织物经过三次水洗除去碱液，然后烘干棉织物浸泡在1,4-环己烷二异氰酸酯中。4小时后取出，在120℃加热固化2小时得到功能化织物。水接触角测试结果为156°。
实施例3
首先，用去离子水清洗棉织物，在100℃下干燥后，在1mol/L KOH溶液中浸渍120分钟。将刻蚀后的棉织物经过三次水洗除去碱液，然后烘干棉织物浸泡在环己烷二亚甲基二异氰酸酯中。5小时后取出，在120℃加热固化4小时得到功能化织物。水接触角测试结果为155°。
实施例4
首先，将异佛尔酮二异氰酸酯与单末端单羟基改性硅油(如信越X-22-170DX)，按摩尔比0.5:1混合，在60℃下反应4小时，得到改性的异氰酸酯。
然后，用去离子水清洗棉织物，在100℃下干燥后，在2mol/L KOH溶液中浸渍100分钟。将刻蚀后的棉织物经过三次水洗除去碱液，然后烘干棉织物浸泡在上述改性的异氰酸酯中。4小时后取出，在130℃加热固化3小时得到功能化织物。水接触角测试结果为160°。
实施例5
首先，将甲苯二异氰酸酯与单末端双羟基改性硅油(本实施例采用的单末端双羟基改性硅油为信越X-22-170BX)，按摩尔比4:1混合，在120℃下反应5小时，得到改性的异氰酸酯。
然后，用去离子水清洗棉织物，在100℃下干燥后，在8mol/L NaOH溶液中浸渍100分钟。将刻蚀后的棉织物经过三次水洗除去碱液，然后烘干棉织物浸泡在上述改性的异氰酸酯中。4小时后取出，在120℃加热固化3小时得到功能化织物。水接触角测试结果为162°。
实施例6
首先，将甲苯二异氰酸酯与两末端羟基改性硅油(本实施例采用的单末端单羟基改性硅油为道康宁0156)，按摩尔比2:1混合，在120℃下反应5小时，得到改性的异氰酸酯。
然后，用去离子水清洗棉织物，在100℃下干燥后，在1mol/L NaOH溶液中浸渍100分钟。将刻蚀后的棉织物经过三次水洗除去碱液，然后烘干棉织物浸泡在上述改性的异氰酸酯中。4小时后取出，在120℃加热固化2小时得到功能化织物。水接触角测试结果为151°。
本发明提供的一种超疏水-超亲油织物的制备方法还可以应用于表面带有羟基的基材超疏水-超亲油层的制备，如无纺布、经特殊处理后的金属基材等。
以上所述实施例仅表达了本发明的几种实施方式，其描述较为具体和详细，但并不能因此而理解为对发明专利范围的限制。应当指出的是，对于本领域的普通技术人员来说，在不脱离本发明构思的前提下，还可以做出若干变形和改进，则本发明也意图包含这些改动和变形。
Claims (10)
1.一种超疏水-超亲油织物的制备方法，其特征在于，包括以下步骤：
S1：将织物浸泡在碱液或酸液中刻蚀，然后水洗去除碱液或酸液，烘干；
S2：将步骤S1得到的织物放入异氰酸酯或改性异氰酸酯溶液中浸泡，取出，加热固化，得到超疏水-超亲油织物；
所述改性异氰酸酯为异氰酸酯与含羟基聚硅氧烷反应得到。
2.根据权利要求1所述的超疏水-超亲油织物的制备方法，其特征在于：所述的碱液包括氢氧化钠、氢氧化钾、氢氧化钡、氨水、氢氧化钙中的一种或多种。
3.根据权利要求1所述的超疏水-超亲油织物的制备方法，其特征在于：所述的酸液包括硫酸、硝酸、盐酸、醋酸、氢氟酸和次氯酸中的一种或多种。
4.根据权利要求1所述的超疏水-超亲油织物的制备方法，其特征在于：所述碱液或酸液浓度为0.1～20mol/L。
5.根据权利要求4所述的超疏水-超亲油织物的制备方法，其特征在于：所述碱液或酸液浓度为0.1～20mol/L。
6.根据权利要求1所述的超疏水-超亲油织物的制备方法，其特征在于：所述异氰酸酯包括对苯二异氰酸酯、1,4-环己烷二异氰酸酯、甲苯二异氰酸酯、二甲基联苯二异氰酸酯、多亚甲基多苯基异氰酸酸酯、异佛尔酮二异氰酸酯、二环己基二异氰酸酯、环己烷二亚甲基二异氰酸酯、1,6-六亚甲基二异氰酸酯、HDI三聚体、异佛尔酮二异氰酸酯三聚体、L-赖氨酸三异氰酸酯中的一种或多种。
7.根据权利要求6所述的超疏水-超亲油织物的制备方法，其特征在于：所述改性异氰酸酯由以下方法制备：将异氰酸酯与含羟基聚硅氧烷按摩尔比0.5～10:1混合，在60～120℃下反应0.5～5h，得到改性异氰酸酯。
8.根据权利要求7所述的超疏水-超亲油织物的制备方法，其特征在于：所述含羟基聚硅氧烷包括单末端单羟基改性硅油、单末端双羟基改性硅油、两末端羟基改性硅油中的一种或多种，分子量为100～20000。
9.根据权利要求1所述的超疏水-超亲油织物的制备方法，其特征在于：所述的加热固化温度为40～150℃，加热时间为0.1～5h。
10.一种超疏水-超亲油织物，其特征在于：采用权利要求1-9任一所述超疏水-超亲油织物的制备方法制备得到。
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