CN110396175B - 自乳化抗菌水性环氧树脂及在木竹材保护中的应用 - Google Patents
自乳化抗菌水性环氧树脂及在木竹材保护中的应用 Download PDFInfo
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Abstract
本发明公开了自乳化抗菌水性环氧树脂及在木竹材保护中的应用。由环氧树脂、二乙醇胺、有机溶剂、聚醚胺、冰乙酸、水以重量比100:21.5:100:14.7:20:364.5～624.8制备而成；以环氧树脂、聚醚胺、二乙醇胺为原料，丙二醇单甲醚为有机溶剂反应一定时间后，由旋蒸法除去有机溶剂，加入冰乙酸进行季铵盐化反应，并加水稀释至所需固含量，制得自乳化抗菌水性环氧树脂；使用时选用喷淋、涂刷、浸泡或加压、真空浸渍的方式处理木材和竹材。本发明制备的自乳化水性环氧树脂可以达到纳米尺度，粒径小，稳定性及渗透性好，同时，对木竹材具有很好的粘结和固着性，并且分子结构中的季铵基团抗菌效果明显。
Description
技术领域
本发明属于木竹材保护领域，具体涉及一种自乳化抗菌水性环氧树脂的制备及其在木竹材保护中的应用。
背景技术
环氧树脂俗称“万能胶”，对于各种金属材料如铝、钢、铁、铜和非金属材料如玻璃、陶瓷、木材、混凝土等都有很好的粘结性。环氧树脂高的粘结性和力学性能以及独特的光学特性使其在木竹材及其纤维的高值化利用方面作用显著。然而，环氧树脂通常粘度较高，用其改性木竹材一般需要借助醇、酮或芳烃类有机溶剂降低其粘度。有机溶剂的使用不仅使生产成本进一步提高，而且有机溶剂具有挥发性强、易燃易爆、污染环境等诸多缺点，使得环氧树脂的储存和施工过程中出现很多不便，严重限制其使用。
以水为分散介质或溶剂的水性环氧树脂不仅具有普通溶剂型环氧树脂的优点，且不含有机溶剂或挥发性有机化合物含量较低，安全环保。对施工环境没有严格要求，可以在室温或潮湿的环境下固化，固化时间比较合理并且易于存储，无火灾隐患，可操作性好，设备可用水清洗，方便。目前，水性环氧树脂的研究及应用主要在工业地坪和防腐涂料、防水和防渗堵漏材料、混凝土胶粘剂等领域，在木竹材保护方面的研究还未见报道。水性环氧树脂低粘度、高环保、易成膜及优良的粘结性等使其在木竹材保护方面具有明显优势。具有抗菌功能的纳米水性环氧树脂能够于木竹材中形成贯穿于细胞腔和细胞壁的三维网络结构，从根本上解决当前木竹材易变形和腐朽的缺陷。
发明内容
为了解决背景技术中的问题，本发明基于木竹材本身的结构特点及其易腐朽霉变和变形的缺陷研发了一种自乳化抗菌水性环氧树脂，应用于木竹材保护。
一、一种自乳化抗菌水性环氧树脂
主要由环氧树脂、二乙醇胺、有机溶剂、聚醚胺、冰乙酸和水制备而成，其中各组分重量比为：
所述环氧树脂为双酚A型E-51。
所述聚醚胺为D230。
所述有机溶剂为丙二醇单甲醚。
所述自乳化抗菌水性环氧树脂的制备方法包括以下步骤：
(1)将100重量份环氧树脂与21.5重量份二乙醇胺投入三口烧瓶中，并加入100份丙二醇单甲醚，在65-80℃下反应1h，反应过程中搅拌速度为300r-400r/min；
(2)在步骤(1)反应后的溶液中投入14.7重量份聚醚胺，继续在65-80℃反应1h；
(3)在50℃下，旋蒸除去溶剂，加入20.0重量份冰乙酸HAc进行季铵盐化反应，并在65℃下搅拌1h；
(4)在步骤(3)反应后的溶液中加水稀释至一定的固含量，并在65℃下搅拌均匀。
所述步骤(4)中一定的固含量为20％～30％的固含量。
二、自乳化抗菌水性环氧树脂的应用：
自乳化抗菌水性环氧树脂应用于木竹材保护，采用喷淋、涂刷、浸泡或加压、真空浸渍的方式处理木材和竹材。
测试处理材的尺寸稳定性，并根据《防霉剂对木材霉菌及变色菌防治效力的试验方法》(GB T18261-2013)处理木竹材试块，测定抗菌效果。
本发明的有益效果：
本发明所制自乳化抗菌水性环氧树脂其粒径具有可调控性，尺寸小且稳定性好，可以长期保持不发生分层现象。渗透性较好，从而起到稳定木竹材尺寸和减少真菌侵袭的作用。水性环氧分子上的羟基、环氧等基团又可与木竹材内部反应或构成氢键，提高了固着和粘附性以及提高改性剂抗流失性，同时季铵基团可以提供抗菌性。具有抗菌功能的纳米水性环氧树脂能够很好的在木竹材中渗透，并形成交联贯穿于细胞腔和细胞壁的三维网络结构，从根本上解决木材和竹材易变形和腐朽的缺陷。
附图说明
图1为实施例1(A1,A2)和实施例2(B1,B2)在室温静置3个月前后稳定性的对照。
图2为不同实施例中处理木材的抗胀率。
图3为未处理木材(对照组)和不同实施例处理木材的抗菌效果。
图4为未处理竹材(对照组)和不同实施例处理竹材抗菌效果。
图5为未处理(对照组)的木材试块和不同实施例处理的木材试块在黑曲霉培养皿中不同时间的感染状态显示。
图6未处理(对照组)和不同实施例处理竹材试块在黑曲霉培养皿中不同时间的感染状态显示。
具体实施方式
下面结合附图和实施例对本发明作进一步说明。
通过本发明的配方和制备工艺制备自乳化抗菌水性环氧环氧树脂，测定其稳定性；根据《防霉剂对木材霉菌及变色菌防治效力的试验方法》(GB T18261-2013)的方法处理木竹材试块，测试抗菌效果，并测定处理材尺寸稳定性。
实施例1：
自乳化抗菌水性环氧树脂的物料配比：
(1)取100重量份环氧树脂E-51，加入21.5重量份的二乙醇胺和100重量份的有机溶剂丙二醇单甲醚，在65℃-80℃下搅拌反应1h；之后，称取14.7重量份的聚醚胺D230加入其中，在相同的温度下反应1h；然后采用旋蒸法除去溶剂，加入20重量份冰乙酸(HAc)，搅拌反应1h；之后，加入624.8重量份的水配成所需固含量(20％)的季铵盐型自乳化水性环氧树脂。
(2)测定离心静置稳定性，如图1所示，稳定性较好，离心后静置3个月仍然均一透明，未见分层。
(3)将所得水性环氧树脂加压浸渍到杨木和竹材试块(杨木试块尺寸：50*20*5mm，毛竹材试块尺寸：50*20*5mm)中，采用三步法(60℃/1h-80℃/4h-120℃/2h)固化处理，将干燥后的试块完全浸没在水中浸泡72h，取出后立即测体积。根据所得数据计算进行尺寸稳定性分析，结果见图2。
(4)根据标准《防霉剂对木材霉菌及变色菌防治效力的试验方法》(GB T18261-2013)处理木竹材试块，测试抗菌效果，结果见图3-6。
实施例2
自乳化纳米抗菌水性环氧树脂的物料配比：
(1)取100重量份环氧树脂E-51，加入21.5重量份的二乙醇胺和100重量份的有机溶剂丙二醇单甲醚，在65℃-80℃下搅拌反应1h；之后，称取14.7重量份的聚醚胺D230加入其中，在相同温度下反应1h；然后采用旋蒸法除去溶剂，加入20重量份乙酸(HAc)，搅拌反应1h；之后，加入一定量的水配成所需固含量(30％)的季铵盐型自乳化水性环氧树脂。
(2)测定离心静置稳定性，如图1所示，稳定性较好，离心后静置3个月仍然均一透明，未见分层。
(3)将所得水性环氧树脂加压浸渍到杨木和竹材试块(杨木试块尺寸：50*20*5mm，毛竹材试块尺寸：50*20*5mm)中，采用三步法(60℃/1h-80℃/4h-120℃/2h)固化处理，将干燥后的试块完全浸没在水中浸泡72h，取出后立即测体积。根据所得数据计算进行尺寸稳定性分析，结果见图2。
(4)根据标准《防霉剂对木材霉菌及变色菌防治效力的试验方法》(GB T18261-2013)处理木竹材试块，测试抗菌效果，结果见图3-6。
实验结果：
1)自乳化水性环氧树脂稳定性：
如图1所示为实施例1(A1,A2)和实施例2(B1,B2)在室温静置3个月前后稳定性的对照；其中A1、B1静置时间为0天，A2、B2静置时间为90天。由图1可以明显看到实施例1和实施例2的自乳化水性环氧树脂稳定性较好，离心后静置3个月仍然均一透明，未见分层。
2)经水性环氧树脂处理后的木材尺寸稳定性：
如图2所示为不同实施例中处理木材的抗胀率。由图2可知，经实施例1处理的木材抗胀率为27.9％，能够使材料尺寸稳定性提高。经实施例2处理木材的抗胀率可达41.7％，能够使材料尺寸稳定性明显提高。
3)未处理的木竹材试块(对照组)和经水性环氧树脂处理后的木竹材试块的抗菌结果：
图3所示为未处理木材(对照组)和不同实施例处理木材的抗黑曲霉效果；图4为未处理竹材(对照组)和不同实施例处理竹材抗黑曲霉效果。
图5所示为未处理(对照组)的木材试块和不同实施例处理的木材试块在黑曲霉培养皿中不同时间的感染状态显示，其中A1,A2,A3为对照组；B1,B2,B3为实施例1；C1,C2,C3为实施例2；A1,B1,C1为第1天时初始状态，A2,B2,C2为第8天时的状态(此时未处理材开始出现感染)，A3,B3,C3为第30天时的状态。A21为A2的放大图。
图6所示为未处理(对照组)和不同实施例处理竹材试块在黑曲霉培养皿中不同时间的感染状态显示。A1,A2,A3为对照组；B1,B2,B3为实施例1；C1,C2,C3为实施例2；A1,B1,C1为第1天时初始状态，A2,B2,C2为第5天时的状态(此时未处理材开始出现感染)，A3,B3,C3为第30天时的状态。
结果表明，未经任何处理的木材和竹材试块(对照组)分别在第5天和第8天被黑曲霉感染，之后迅速发展，大约在12天作为被完全覆盖，被害值达到4。处理后的木材和竹材对黑曲霉的抗菌效果均得到明显改善，经实施例1处理后木材和竹材试块1个月(30天)室内测试的最终被害值分别为1.3和0.38，经实施例2处理后木材和竹材试块1个月(30天)室内测试的最终被害值分别为0.38和0.17。
Claims (3)
1.一种自乳化抗菌水性环氧树脂，其特征在于，主要由环氧树脂、二乙醇胺、有机溶剂、聚醚胺、冰乙酸和水制备而成，其中各组分重量比为：
所述聚醚胺为D230；
所述环氧树脂为双酚A型E-51；
所述有机溶剂为丙二醇单甲醚；
自乳化抗菌水性环氧树脂的制备方法包括以下步骤：
(1)将100重量份环氧树脂与21.5重量份二乙醇胺投入三口烧瓶中，并加入100份丙二醇单甲醚，在65-80℃下反应1h，反应过程中搅拌速度为300r-400r/min；
(2)在步骤(1)反应后的溶液中投入14.7重量份聚醚胺，继续在65-80℃反应1h；
(3)在50℃下，旋蒸除去溶剂，加入20.0重量份冰乙酸进行季铵盐化反应，并在65℃下搅拌1h；
(4)在步骤(3)反应后的溶液中加水稀释至一定的固含量，并在65℃下搅拌均匀。
2.根据权利要求1所述的自乳化抗菌水性环氧树脂，其特征在于，所述步骤(4)中一定的固含量为20％～30％的固含量。
3.根据权利要求1所述的自乳化抗菌水性环氧树脂的应用，其特征在于，自乳化抗菌水性环氧树脂应用于木竹材保护，采用喷淋、涂刷、浸泡或加压、真空浸渍的方式处理木材和竹材。
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