CN114106643A - 改性壳聚糖在涂料中的应用 - Google Patents
改性壳聚糖在涂料中的应用 Download PDFInfo
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- CN114106643A CN114106643A CN202111499640.8A CN202111499640A CN114106643A CN 114106643 A CN114106643 A CN 114106643A CN 202111499640 A CN202111499640 A CN 202111499640A CN 114106643 A CN114106643 A CN 114106643A
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Abstract
本发明公开了一种壳聚糖改性水性阻尼涂料及其制备方法和应用，涉及水性阻尼涂料领域。通过加入三聚磷酸盐来使得壳聚糖产生离子交联网络，提高酸性和碱性环境中化学稳定性并提高耐水性，并在壳聚糖中加入纳米TiO2来提高其机械强度和阻隔性能。该壳聚糖改性水性阻尼涂料可以有效的起到长久防腐抗菌的作用，所用原料绿色环保，又提高了产品的环保性能，可使得阻尼涂层在保持原有阻尼性能的基础上，减少设备和基材在外部环境下被腐蚀和污染。而传统的防腐剂均为有毒物质，容易对环境造成污染。
Description
技术领域
本发明涉及涂料技术领域，尤其涉及改性壳聚糖在涂料中的应用。
背景技术
随着科技的不断发展，机械设备越来越自动化、高效化，而由此带来的振动和噪音问题也日益显著。剧烈的机械振动和过大的噪音不仅会对仪器设备本身带来损害，降低设备的精确度，减少设备的使用寿命，还会给人们的生活生产和身心带来伤害。减振降噪已成为机械和设备设计中要考虑的关键因素之一，而阻尼材料是解决振动和噪音问题的最有效的方法之一。水性阻尼涂料因其施工方便、环保、成本低廉成为人们首选的阻尼材料。现有的普通阻尼涂料不具有耐磨耐腐蚀等功能，暴露在高温高湿等环境下会发生涂层腐蚀或脱落，从而缩短设备使用寿命。
壳聚糖，是仅次于纤维素的第二丰富的天然生物聚合物，具有无毒性，生物相容性，pH值的敏感性的特点，并且生产成本低。壳聚糖有着胺基(-NH2)和羟基(-OH)基团，这些官能团有利于结构改性，增强壳聚糖的反应，以在化学交联网络中提供均相。此外，由于壳聚糖通过-NH2和-OH基团与金属表面配位，有着良好的抗腐蚀性，同时壳聚糖对细菌和真菌也有抑制作用。由于天然壳聚糖在许多有机酸中的溶解度高、在水中的溶胀指数高、低机械强度和低表面积而限制了这种材料的应用。三聚磷酸盐(TPP)是一种无毒的聚阴离子，可通过静电力与阳离子多糖壳聚糖相互作用。壳聚糖中的质子化胺基基团将与TPP的带负电荷的反离子相互作用，通过离子相互作用产生离子交联网络，从而提高壳聚糖提高酸性和碱性环境中化学稳定性并降低疏水性。
大多数无机抗菌物质是金属纳米颗粒和金属氧化物的纳米颗粒，如银、金、铜、氧化钛和氧化锌纳米颗粒。与纳米银、纳米氧化锌相比，纳米TiO2具有许多理想的特性，例如高化学稳定性、成本相对较低、无毒、环境友好、抗菌行为和光催化活性。将纳米TiO2分散在壳聚糖中可以结合无机材料(如硬度、热稳定性和韧性)和有机聚合物(如柔韧性、绝缘性、延展性和固化能力)的优点。可以利用壳聚糖和无机纳米粒子的优点延缓腐蚀现象来提高聚合物涂层的使用寿命。
目前，市场上的阻尼涂料均难以满足高温高湿度环境下的使用要求，限制了其在轨道交通和建筑工业上的应用。基于现有的水性阻尼涂料存在的缺陷，有必要对现有的水性阻尼涂料进行改进。
发明内容
针对现有技术中存在的不足，本发明的第一个目的提供了改性壳聚糖在涂料中的应用，使得涂料具有良好的防腐抗菌性，同时防污方面具有很大优势。
本发明的第二个目的提供一种应用了上述改性壳聚糖的水性阻尼涂料及其制备方法。
通过三聚磷酸盐和纳米TiO2联合改性壳聚糖得到改性壳聚糖，脱乙酰度为85-95％。其中，加入的三聚磷酸盐可使得壳聚糖产生离子交联网络，提高酸性和碱性环境中化学稳定性并提高耐水性，并在壳聚糖中加入纳米TiO2来提高其机械强度和阻隔性能。以壳聚糖作为主要的防腐抗菌原料，纳米TiO2可进一步提升其防腐抗菌效果。因此，上述改性壳聚糖可应用于涂料中以增加涂料的抗菌性，同时提升涂料的减震降噪的性能。
一种水性阻尼涂料，以重量份数计，包括水性乳液42-50份、改性壳聚糖8-16份、去离子水25-32份、功能性填料32-45份、分散剂1-2.5份、润湿剂1-2份、增稠剂1-2份、阻燃剂1-2.5份、消泡剂0.5-0.8份、成膜助剂1-2份。
本发明中，所述水性乳液包括纯丙乳液、苯丙乳液、氯偏乳液、丁苯乳液、水性聚氨酯中的一种或几种，水性乳液的固含量为35％-40％。
所述改性壳聚糖为壳聚糖用三聚磷酸盐(优选三聚磷酸钠)和纳米TiO2改性，脱乙酰度为85-95％。
所述功能性填料以片状云母粉为主，粒度为300-500目之间，还可以包括滑石粉、重质碳酸钙和贝壳粉的一种或几种。与普通云母粉相比，片层云母粉之间结构的滑动更加容易，因而在低温区即可滑动，可有效的提高阻尼性能，使有效阻尼温域相对扩宽，辅助填料的加入可以填补聚合物与片状云母粉之间的空缺，改善阻尼性能。
所述分散剂为聚羧酸盐类分散剂、聚氨酯类共聚物和脂肪酸衍生物的一种或几种。聚羧酸盐类分散剂常用的有聚羧酸钠、聚羧酸钾、聚羧酸钙等，聚氨酯盐类共聚物有有机硅改性聚氨酯、疏水改性聚氨酯、热塑性聚氨酯共聚物等，脂肪酸衍生物有脂肪酸聚氧乙烯醚、芥酸酰胺、脂肪胺等。三类分散剂具有优异的介电性、柔韧性、耐水性、透气性及生物相容性，同时又有良好的热稳定性、耐候性及耐腐蚀性。
所述润湿剂为改性有机硅类基材润湿剂和炔二醇类基材润湿剂的一种或几种。改性有机硅类基材润湿剂如聚醚改性有机硅、聚醚改性硅油，炔二醇类基材润湿剂如炔二醇改性表面活性剂、炔二醇环氧乙烷。两类润湿剂可适用于水性系统的低泡超强润湿剂，可提高体系对各种基材的动态润湿能力；静态和动态表面张力低，促进流平，且产品不起泡。
所述增稠剂为有机改性膨润土、气相二氧化硅、氢化蓖麻油中的一种或几种。
所述阻燃剂为无卤阻燃剂。
所述消泡剂为矿物油类消泡剂、聚醚改性有机硅类消泡剂和丙烯酸酯类消泡剂中的一种或几种。矿物油类消泡剂如HY-1040F、HY-7010、HY-7020，聚醚改性有机硅类消泡剂如Si-O-C型聚醚改性有机硅消泡剂乳液、Si-C型聚醚硅油、聚醚改性聚硅氧烷共聚物，丙烯酸酯类消泡剂，如甲基丙烯酸甲酯、2-三氟甲基丙烯酸甲酯、丙烯酸异冰片酯-甲基丙烯酸甲酯共聚物等。这几类消泡剂具有消泡性能好、表面张力低等优点，同时还具备耐高温、相容性好、抑泡性强的特点。
所述成膜助剂为
酯醇。
本发明还提供了一种壳聚糖改性水性阻尼涂料的制备方法，包括：
(1)将壳聚糖溶解在体积分数为1％的乙酸溶液中并在室温下搅拌24h，将1％三聚磷酸盐溶液加入到其中并将pH调至4-5，升温至60-70℃以200-300rpm搅拌加热5h得到壳聚糖溶液。将钛酸四丁酯、乙酰丙酮和无水乙醇按体积比例1：0.6：1混合，在室温下以400-500rpm搅拌2-3h，离心收集纳米颗粒并分散在无水乙醇和去离子水中，重复离心3-4次以洗去杂质，在100℃的烘箱干燥，然后在马弗炉中在500-600℃下煅烧2-3h，得到纳米TiO2。然后将纳米TiO2加入到壳聚糖溶液中以200-400rpm搅拌2h使其均匀分散并超声处理30min。最后，将混合液重复离心3-4次，用去离子水洗涤至中性，真空干燥，得到改性壳聚糖。
(2)将水性乳液、改性壳聚糖和去离子水加入到三口烧瓶中，打开冷凝水，在60-70℃下以600-800rpm搅拌3-4h。再加入分散剂、消泡剂并以500-600rpm搅拌1-1.5h得到混合液。
(3)将功能型填料、润湿剂和阻燃剂加入到混合液中以400-500rpm搅拌0.5-1h，再继续加入增稠剂和成膜助剂以600-700rpm搅拌20-30min，过滤得到水性阻尼涂料，即壳聚糖改性水性阻尼涂料。
本发明的改性壳聚糖应用在水性阻尼涂料制备中时，可使得涂料具有良好防腐抗菌性，同时在在减震抗噪方面具有很大优势，因此，制得的涂料可在轨道交通和机械设备中作为金属表面涂层。
本发明的壳聚糖改性水性阻尼涂料相对于现有技术具有以下有益效果：
通过加入三聚磷酸盐来使得壳聚糖产生离子交联网络，提高酸性和碱性环境中化学稳定性并提高耐水性，并在壳聚糖中加入纳米TiO2来提高其机械强度和阻隔性能。以壳聚糖作为主要的防腐抗菌原料，纳米TiO2可进一步提升其防腐抗菌效果。包含改性壳聚糖的水性阻尼涂料可以有效的起到长久防腐抗菌的作用，所用原料绿色环保，又提高了产品的环保性能，可使得阻尼涂层在保持原有阻尼性能的基础上，减少设备和基材在外部环境下被腐蚀和污染。
具体实施方式
为更好理解本发明，下面结合实施例对本发明作进一步详细的描述，但本发明要求保护范围并不局限于此。
实施例1
(1)将1g壳聚糖溶解在100mL体积分数为1％的乙酸溶液中并在室温下搅拌24h，将90mL体积分数为1％的三聚磷酸钠溶液加入到其中并将pH调至4-5，升温至60-70℃以200-300rpm搅拌加热5h得到壳聚糖溶液。将钛酸四丁酯、乙酰丙酮和无水乙醇按体积比例1：0.6：1混合，在室温下以400-500rpm搅拌2-3h，离心收集纳米颗粒并分散在100mL无水乙醇和50mL去离子水的混合液中，重复离心3-4次以洗去杂质，在100℃的烘箱干燥，在马弗炉中在500-600℃下煅烧2-3h，得到纳米TiO2。然后将1g纳米TiO2加入到壳聚糖溶液中以200-400rpm搅拌2h使其均匀分散并超声处理30min。最后，将混合液重复离心3-4次，用去离子水洗涤至中性，真空干燥，得到改性壳聚糖。
(2)将25份纯丙乳液，22份苯丙乳液、10份改性壳聚糖和25份去离子水加入到三口烧瓶中，打开冷凝水，在60-70℃下以600-800rpm搅拌4-5h。再加入1.5份聚羧酸钠分散剂、0.5份HY-1040F矿物油类消泡剂并以500-600rpm搅拌1-1.5h得到混合液。
(3)将24份片状云母粉，5份滑石粉，3份贝壳粉、1份聚醚改性硅油润湿剂和2份无卤阻燃剂加入到混合液中以400-500rpm搅拌0.5-1h，再继续加入1份氢化蓖麻油和1份
酯醇并以600-700rpm搅拌20-30min，过滤得到水性阻尼涂料，即壳聚糖改性水性阻尼涂料。
实施例2
(1)改性壳聚糖的制备方法同实施例1。
(2)将28份纯丙乳液，20份水性聚氨酯、15份改性壳聚糖和30份去离子水加入到三口烧瓶中，打开冷凝水，在60-70℃下以600-800rpm搅拌4-5h。再加入1份有机硅改性聚氨酯分散剂、0.8份甲基丙烯酸甲酯消泡剂并以500-600rpm搅拌1-1.5h得到混合液。
(3)将30份片状云母粉，4份重质碳酸钙，4份贝壳粉、1.5份炔二醇环氧乙烷润湿剂和1.5份无卤阻燃剂加入到混合液中以400-500rpm搅拌0.5-1h，再继续加入1.5份有机改性膨润土和2份
酯醇并以600-700rpm搅拌20-30min，过滤得到水性阻尼涂料，即壳聚糖改性水性阻尼涂料。
实施例3
(1)改性壳聚糖的制备方法同实施例1。
(2)将23份氯偏乳液，26份丁苯乳液、12份改性壳聚糖和32份去离子水加入到三口烧瓶中，打开冷凝水，在60-70℃下以600-800rpm搅拌4-5h。再加入1.8份脂肪酸聚氧乙烯醚分散剂、0.6份Si-O-C型聚醚改性有机硅消泡剂乳液并以500-600rpm搅拌1-1.5h得到混合液。
(3)将28份片状云母粉，5份滑石粉，7份重质碳酸钙、1.6份炔二醇改性表面活性剂和1.8份无卤阻燃剂加入到混合液中以400-500rpm搅拌0.5-1h，再继续加入1.6份气相二氧化硅和1.5份
酯醇并以600-700rpm搅拌20-30min，过滤得到水性阻尼涂料，即壳聚糖改性水性阻尼涂料。
实施例4
(1)改性壳聚糖的制备方法同实施例1。
(2)将25份苯丙乳液，25份氯偏乳液、16份改性壳聚糖和28份去离子水加入到三口烧瓶中，打开冷凝水，在60-70℃下以600-800rpm搅拌4-5h。再加入1.2份疏水改性聚氨酯共聚物分散剂、0.7份Si-C型聚醚硅油消泡剂并以500-600rpm搅拌1-1.5h得到混合液。
(3)将30份片状云母粉，7份重质碳酸钙，5份贝壳粉、2份聚醚改性硅油润湿剂和1.4份无卤阻燃剂加入到混合液中以400-500rpm搅拌0.5-1h，再继续加入1.2份有机改性膨润土和1.8份
酯醇并以600-700rpm搅拌20-30min，过滤得到水性阻尼涂料，即壳聚糖改性水性阻尼涂料。
对比例1
(1)将1g壳聚糖溶解在100mL体积分数为1％的乙酸溶液中并在室温下搅拌24h，得到壳聚糖溶液。将钛酸四丁酯、乙酰丙酮和无水乙醇按体积比例1：0.6：1混合，在室温下以400-500rpm搅拌2-3h，离心收集纳米颗粒并分散在100mL无水乙醇和50mL去离子水的混合液中，重复离心3-4次以洗去杂质，在100℃的烘箱干燥，在马弗炉中在500-600℃下煅烧2-3h，得到纳米TiO2。然后将1g纳米TiO2加入到壳聚糖溶液中以200-400rpm搅拌2h使其均匀分散并超声处理30min。最后，将混合液重复离心3-4次，用去离子水洗涤至中性，真空干燥，得到改性壳聚糖。
(2)将25份纯丙乳液，22份苯丙乳液、10份改性壳聚糖和25份去离子水加入到三口烧瓶中，打开冷凝水，在60-70℃下以600-800rpm搅拌4-5h。再加入1.5份聚羧酸盐类分散剂、0.5份矿物油类消泡剂并以500-600rpm搅拌1-1.5h得到混合液。
(3)将24份片状云母粉，5份滑石粉，3份贝壳粉、1份改性有机硅类基材润湿剂和2份无卤阻燃剂加入到混合液中以400-500rpm搅拌0.5-1h，再继续加入1份氢化蓖麻油和1份
酯醇并以600-700rpm搅拌20-30min，过滤得到水性阻尼涂料，即壳聚糖改性水性阻尼涂料。
对比例2
(1)将1g壳聚糖溶解在100mL体积分数为1％的乙酸溶液中并在室温下搅拌24h，将90mL体积分数为1％的三聚磷酸钠溶液加入到其中并将pH调至4-5，升温至60-70℃以200-300rpm搅拌加热5h得到壳聚糖溶液。最后，将溶液重复离心3-4次，用去离子水洗涤至中性，真空干燥，得到改性壳聚糖。
(2)将25份纯丙乳液，22份苯丙乳液、10份改性壳聚糖和25份去离子水加入到三口烧瓶中，打开冷凝水，在60-70℃下以600-800rpm搅拌4-5h。再加入1.5份聚羧酸盐类分散剂、0.5份矿物油类消泡剂并以500-600rpm搅拌1-1.5h得到混合液。
(3)将24份片状云母粉，5份滑石粉，3份贝壳粉、1份改性有机硅类基材润湿剂和2份无卤阻燃剂加入到混合液中以400-500rpm搅拌0.5-1h，再继续加入1份氢化蓖麻油和1份
酯醇并以600-700rpm搅拌20-30min，过滤得到水性阻尼涂料，即壳聚糖改性水性阻尼涂料。
将上述实施例1-4和对比例1-2制备得到的水性阻尼涂料覆盖在不锈钢金属板上分别测试其性能，结果如下表1所示。
表1
所述耐酸性测试是样品在0.1mol/L的H2SO4溶液浸泡24h，所述耐碱性测试是样品在0.1mol/L的NaOH溶液浸泡24h，所述耐盐水性测试是样品在3.5wt％的NaCl溶液浸泡240h。
从表1中可以看出，本发明制备得到的壳聚糖改性水性阻尼涂料具有良好的柔韧性、阻燃性、耐酸性、耐碱性、耐水性、耐盐水腐蚀、抗细菌性、抗霉菌性、且使用温域范围宽，并且与基材之间具有良好的附着力；本发明制备得到的壳聚糖改性水性阻尼涂料不仅可以减少在生活生产中的表面污染，还可以起到防腐抗菌的作用，适合在高温高湿度情况下使用。
以上所述仅为本发明的具体实施方式而已，并不用于限制本发明，对于本领域的技术人员来说，本发明可以有各种更改和变化。凡在本发明的精神和原则之内所作的任何修改、等同替换、改进等，均应包含在本发明的保护范围之内。
Claims (10)
1.改性壳聚糖在涂料中的应用，其特征在于，所述改性壳聚糖为三聚磷酸盐和纳米TiO2联合改性壳聚糖得到，改性壳聚糖的脱乙酰度为85-95％。
2.一种水性阻尼涂料，其特征在于，以重量份数计，包括水性乳液42-50份、改性壳聚糖8-16份、去离子水25-32份、功能性填料32-45份、分散剂1-2.5份、润湿剂1-2份、增稠剂1-2份、阻燃剂1-2.5份、消泡剂0.5-0.8份、成膜助剂1-2份；
所述改性壳聚糖为三聚磷酸盐和纳米TiO2联合改性壳聚糖得到，改性壳聚糖的脱乙酰度为85-95％。
3.根据权利要求2所述的水性阻尼涂料，其特征在于，所述消泡剂为矿物油类消泡剂、聚醚改性有机硅类消泡剂、丙烯酸酯类消泡剂中的一种或几种。
4.根据权利要求2所述的水性阻尼涂料，其特征在于，所述阻燃剂为无卤阻燃剂；所述成膜助剂为
酯醇。
5.根据权利要求2所述的水性阻尼涂料，其特征在于，所述水性乳液包括纯丙乳液、苯丙乳液、氯偏乳液、丁苯乳液、水性聚氨酯中的一种或几种，固含量为35％-40％。
6.根据权利要求2所述的水性阻尼涂料，其特征在于，所述功能性填料以片状云母粉为主，粒度为300-500目之间，或还包括滑石粉、重质碳酸钙和贝壳粉的一种或几种作为辅填料。
7.根据权利要求2所述的水性阻尼涂料，其特征在于，所述分散剂为聚羧酸盐类、聚氨酯类共聚物和脂肪酸衍生物的一种或几种。
8.根据权利要求2所述的水性阻尼涂料，其特征在于，所述润湿剂为改性有机硅类基材润湿剂、炔二醇类基材润湿剂中的一种或几种。
9.根据权利要求2所述的水性阻尼涂料，其特征在于，所述增稠剂为有机改性膨润土、气相二氧化硅、氢化蓖麻油中的一种或几种。
10.根据权利要求2所述的壳聚糖改性水性阻尼涂料的制备方法，其特征在于，包含以下步骤：
(1)将壳聚糖溶解在体积分数为1％的乙酸溶液中并在室温下搅拌24h，将体积分数为1％的三聚磷酸盐溶液加入到其中并将pH调至4-5，升温至60-70℃以200-300rpm搅拌加热5h得到壳聚糖溶液；将钛酸四丁酯、乙酰丙酮和无水乙醇按体积比例1：0.6：1混合，在室温下以400-500rpm搅拌2-3h，离心收集纳米颗粒并分散在无水乙醇和去离子水中，重复离心3-4次以洗去杂质，在100℃的烘箱干燥，然后在马弗炉中在500-600℃下煅烧2-3h，得到纳米TiO2；然后将纳米TiO2加入到壳聚糖溶液中以400-600rpm搅拌3-4h使其均匀分散并超声处理30min；最后，将混合液离心，用去离子水洗涤至中性，真空干燥，得到改性壳聚糖；
(2)将水性乳液、改性壳聚糖和去离子水加入到三口烧瓶中，打开冷凝水，在60-70℃下以600-800rpm搅拌3-4h；再加入分散剂、消泡剂并以500-600rpm搅拌1-1.5h得到混合液；
(3)将功能性填料、润湿剂和阻燃剂加入到混合液中以400-500rpm搅拌0.5-1h，再继续加入增稠剂和成膜助剂并以600-700rpm搅拌20-30min，过滤得到水性阻尼涂料，即壳聚糖改性水性阻尼涂料。
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