CN108727545A - 一种防腐防污型涂料树脂及其制备方法 - Google Patents
一种防腐防污型涂料树脂及其制备方法 Download PDFInfo
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- CN108727545A CN108727545A CN201810604080.XA CN201810604080A CN108727545A CN 108727545 A CN108727545 A CN 108727545A CN 201810604080 A CN201810604080 A CN 201810604080A CN 108727545 A CN108727545 A CN 108727545A
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- Prior art keywords
- acrylate
- preparation
- corrosion
- anticorrosion
- coating resin
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- C08F293/005—Macromolecular compounds obtained by polymerisation on to a macromolecule having groups capable of inducing the formation of new polymer chains bound exclusively at one or both ends of the starting macromolecule using free radical "living" or "controlled" polymerisation, e.g. using a complexing agent
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- Polymers & Plastics (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
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Abstract
本发明公开了一种防腐防污型涂料树脂及其制备方法：将偏氯乙烯、丙烯酸酯、交联乳化单体、胶乳保护剂、亚硫酸氢钠和水加至容器中，搅匀得混合液A；丙烯酸甲硅烷酯、交联乳化单体和水混合得混合液B；反应器调温至15～30 ℃，氮气氛下加入过硫酸铵和亚硫酸氢钠水溶液，将混合液A在3～4 h内滴加至反应器后，继续滴加混合液B和引发剂，滴加时间1～2 h，滴完恒温2～3 h结束反应。采用常压低温无皂乳液聚合制备了高稳定、强附着、低表面能乳液。通过调节偏氯乙烯、不同丙烯酸酯、不同丙烯酸甲硅烷基酯、交联乳化单体的比例，可以调控树脂膜的附着力、耐水、耐候、耐盐、趋避污损生物等能力，从而提高了防腐防污涂料的综合性能。
Description
技术领域
本发明涉及海洋防腐防污涂料技术领域，具体涉及一种防腐防污型涂料树脂及其制备方法。
背景技术
渔业设施装备，海洋资源勘探、开采、加工、储运等方面的大型工程装备和辅助装备等一系列海洋装备长期面临高盐、高湿、高温、暴晒、生物附着等恶劣环境，极易造成材料污损、腐蚀等。一方面，海洋高盐、高湿环境极易造成一些使用金属材料的船体、输油管道等的腐蚀，带来安全隐患，乃至产生灾难性的后果。另一方面，海洋生物能够附着在船舶、海洋工程以及水下设施表面形成生物污损层，造成船舶航行阻力增大、海洋装备表面漆膜受损、管道阻塞等。解决金属腐蚀的方法主要有表面镀层、表面钝化和涂覆防腐涂料等，其中涂覆防腐涂料应用最为广泛。解决海洋生物污损的方法包括人工或机械清除法、过滤法、加热法等物理防污法和电解法、涂覆防污涂料法等化学防污法，其中涂覆防污涂料由于施工容易、效果好而备受青睐。
防腐的机理是借助于树脂与基材强的作用力，在材料表面形成聚合物膜，阻隔水、无机盐及氧气等腐蚀物质与基材的接触，起到防腐作用。而目前防污的机理主要是利用涂层的疏水结构和低表面能等物理特性防污，使海洋污损生物难以在基材上面附着，或即使附着也不牢固，在水流或其他外力作用下易脱落，同时防污涂料在水中缓慢水解可以定期脱除表面层，从而及时清洗表面污染物。防污涂料具有表面光滑、极性低等特点才能起到较好的清洗表面污染物的作用，但是材料水解会造成涂料附着力降低，容易使基材腐蚀，而防腐涂料要求表面粗糙、具有大的极性才能和基材有较强的附着力，起到较好的阻隔、防腐作用。因此，防腐和防污性能对材料结构的要求是对立的，涂料很难兼有防腐和防污性能。为了满足海洋装备对防腐和防污的双重要求，基于重防腐树脂骨架引入防污单元是设计开发防腐防污涂料树脂的重要思路和途径。
发明内容
本发明针对现有技术的不足，提供一种兼具耐水、耐候、耐盐、趋避污损生物的防腐防污涂料树脂及其制备方法。
本发明解决上述技术问题采用的技术方案是：一种防腐防污型涂料树脂及其制备方法，其特征在于包括以下步骤：首先将偏氯乙烯、丙烯酸酯、交联乳化单体、胶乳保护剂、亚硫酸氢钠和水加至容器中，室温搅拌均匀得混合液A；丙烯酸甲硅烷酯、交联乳化单体和水混合得混合液B；体系固含量为55～60%，交联乳化单体占总单体质量的0.5～2%，水的加入量为总单体质量的67～82%，胶乳保护剂的用量为总单体质量的0.1～0.5%；然后将反应器抽真空、充氮气重复三次，调温至15～30 ℃，分别加入混合液A中单体质量0.2～1.0%和0.05～0.15%的过硫酸铵和亚硫酸氢钠水溶液，将混合液A在3～4 h内滴加至反应器后，继续滴加混合液B，同时向反应器中滴加混合液B中单体质量0.2～1%的过硫酸铵水溶液，滴加时间1～2 h，滴完恒温反应2～3 h结束反应，制得偏氯乙烯-丙烯酸酯-丙烯酸甲硅烷基酯乳液。
本发明所述丙烯酸酯为甲基丙烯酸甲酯、丙烯酸甲酯、丙烯酸乙酯、丙烯酸丁酯、丙烯酸-2-乙基己酯、丙烯酸、甲基丙烯酸的任意一种或任意两种及两种以上的混合物；丙烯酸甲硅烷基酯为丙烯酸三乙基甲硅烷基酯、丙烯酸三异丙基甲硅烷基酯、甲基丙烯酸三甲基硅酯、甲基丙烯酸三乙基甲硅烷基酯、甲基丙烯酸叔丁基二甲基甲硅烷基酯、甲基丙烯酸三异丙基甲硅烷基酯、甲基丙烯酸三苯基甲硅烷基酯的任意一种或任意两种及两种以上的混合物；交联乳化单体为N-羟甲基丙烯酰胺、N-羟乙基丙烯酰胺、N-羟丙基丙烯酰胺的任意一种或任意两种及两种以上的混合物。胶乳保护剂为碳酸氢钠、碳酸钠的任意一种或两种的混合物。
偏氯乙烯-丙烯酸酯-丙烯酸甲硅烷基酯的成膜固化：在表面经过砂纸打磨处理后的钢板上，涂上厚度为120 um左右厚的乳液，60 ℃烘干固化30 min后成膜，考察其各项性能。
与现有技术相比，本发明的有益效果是：
（1）在不加入小分子防污剂的基础上，制备了一种同时具有防腐和防污功能的涂料树脂。该树脂中偏氯乙烯-丙烯酸酯极性链段与基材有较强的吸附作用，可以在基材上形成稳定的树脂膜，赋予其较强的隔水、阻盐、阻气等性能，起到较好的防腐作用；树脂中聚丙烯酸甲硅烷基酯链段侧链的可控水解性能赋予其具有表面光滑的特点，通过自抛光作用实现防污功能。相比目前在防腐树脂上负载小分子防污剂的防腐防污涂料树脂，基于重防腐树脂骨架引入自抛光防污高分子链段既可以展现好的防污效果又不降低防腐链段与基材的附着力，不会造成海洋塑料污染，环保无毒。
（2）体系采用无皂乳液聚合制备了偏氯乙烯-丙烯酸酯-丙烯酸甲硅烷基酯树脂，相比传统乳液聚合制备的防腐树脂具有更好的防腐能力。因为传统乳液聚合体系中必须额外加入具有亲水基团的各种小分子助剂，这些亲水助剂在树脂成膜后还残留在树脂膜中，并且还会不断向膜表面迁移，从而增加了树脂膜的亲水性，不利于树脂膜对水、盐、氧气等腐蚀物质的阻隔。
（3）通过非活性聚合，常压低温（15～30 ℃）下实现了以沸点较低的偏氯乙烯为主体，具有防腐与防污功能“嵌段聚合物”的合成。活性聚合的本质是通过可逆的链终止或链转移反应降低体系中自由基的浓度，即降低真正链终止的几率，从而实现可控聚合。本发明通过调控还原剂的用量，采用较低的温度（15～30 ℃）降低自由基的产生速率，不仅做到接近活性聚合实现“嵌段聚合物”的合成，还能常压下保证沸点较低的偏氯乙烯具有较高的转化率，避免了高温高压反应对设备和操作工艺的苛刻要求。同时，相比目前通过高温高压制备的偏氯乙烯基防腐树脂，这种较低温度下的无皂乳液聚合还可以保证乳液具有较高的稳定性。
（4）不同反应时间加入不同种类的单体，在聚合前期主要是加入偏氯乙烯、丙烯酸酯等起防腐作用的单体，而聚合后期则主要加入丙烯酸甲硅烷基酯等起防污作用的单体，制备出兼有防腐、防污功能的“嵌段”乳液，具备强附着、低表面能等特点，大大提高了防腐防污涂料的性能。
（5）通过调节偏氯乙烯、不同种类丙烯酸酯、交联乳化单体的比例，可以调控树脂膜的附着力、耐盐雾性能等，从而提高了防腐防污涂料的综合性能。树脂在基材表面固化前为线形结构，利于均匀成膜；固化后借助于交联乳化单体的自交联作用形成疏水、耐溶剂的网状体形结构，可提高其防腐性能。同时，该树脂膜表面粘性小，不沾污，可提高其防污性能。
（6）将颜料浆、助剂等加入偏氯乙烯-丙烯酸酯-丙烯酸甲硅烷基酯乳液中，可制备具有优良耐水、耐候、耐盐、趋避污损生物特性的水性防腐防污涂料，且易于施工、绿色无毒。
附图说明
图1为本发明实施例1-3中的偏氯乙烯-丙烯酸酯-丙烯酸甲硅烷基酯乳液制备的防腐防污涂料喷涂在相同尺寸的钢板上，经过800小时耐盐雾实验后的钢板表面效果对比图。
具体实施方式
下面结合实施例对本发明作进一步的描述：
实施例1：
将0.6 kg N-羟甲基丙烯酰胺、0.09 kg 亚硫酸氢钠、0.15 kg 碳酸氢钠溶于30.0 kg去离子水中，全部溶解后，室温条件下加入42.0 kg 偏氯乙烯，7.5 kg甲基丙烯酸甲酯，2.5kg丙烯酸乙酯，8.0 kg丙烯酸丁酯，8.5 kg丙烯酸-2-乙基己酯，1.5 kg丙烯酸，充分搅拌得到混合液A；将0.2 kg N-羟甲基丙烯酰胺溶于10.0 kg 去离子水中，全部溶解后，加入25.0kg丙烯酸三乙基甲硅烷基酯、5.0 kg甲基丙烯酸三异丙基甲硅烷基酯，搅拌均匀得到混合液B。
将反应器抽真空、充氮气重复三次，调温至25 ℃，加入15.0 kg溶有0.35 kg过硫酸铵和0.07 kg亚硫酸氢钠的去离子水溶液，3.5 h内将混合液A滴加至反应器中，滴完恒温反应10 min。继续滴加混合液B和10.0 kg溶有0.15 kg过硫酸铵的去离子水溶液，控制滴加时间1.5 h，滴完恒温反应2.0 h后结束反应，制得偏氯乙烯-丙烯酸酯-丙烯酸甲硅烷基酯乳液：固含量为59%左右，粘度为860 mpa·s。该乳液储存1年后保持稳定，涂膜硬度高，可有效趋避污损生物，耐水、耐盐雾性能好，可应用于水性防腐防污涂料。
实施例2：
将0.8 kg N-羟甲基丙烯酰胺、0.09 kg 亚硫酸氢钠、0.15 kg 碳酸氢钠溶于35.0 kg去离子水中，全部溶解后，室温条件下加入42.0 kg 偏氯乙烯，7.5 kg甲基丙烯酸甲酯，2.5kg丙烯酸乙酯，8.0 kg丙烯酸丁酯，8.5 kg丙烯酸-2-乙基己酯，1.5 kg丙烯酸，充分搅拌得到混合液A；将0.2 kg N-羟甲基丙烯酰胺溶于10.0 kg 去离子水中，全部溶解后，加入25.0kg丙烯酸三乙基甲硅烷基酯、5.0 kg甲基丙烯酸三异丙基甲硅烷基酯，搅拌均匀得到混合液B。
将反应器抽真空、充氮气重复三次，调温至25 ℃，加入20.0 kg溶有0.35 kg过硫酸铵和0.07 kg亚硫酸氢钠的去离子水溶液，3.5 h内将混合液A滴加至反应器中，滴完恒温反应10 min。继续滴加混合液B和10.0 kg溶有0.15 kg过硫酸铵的去离子水溶液，控制滴加时间1.5 h，滴完恒温反应2.0 h后结束反应，制得偏氯乙烯-丙烯酸酯-丙烯酸甲硅烷基酯乳液：固含量为56%左右，粘度为950 mpa·s。该乳液储存1年后保持稳定，涂膜硬度高，可有效趋避污损生物，耐水、耐盐雾性能好，可应用于水性防腐防污涂料。
实施例3：
将0.8 kg N-羟甲基丙烯酰胺、0.09 kg 亚硫酸氢钠、0.15 kg 碳酸氢钠溶于35.0 kg去离子水中，全部溶解后，室温条件下加入38.0 kg 偏氯乙烯，7.5 kg甲基丙烯酸甲酯，2.5kg丙烯酸乙酯，10.0 kg丙烯酸丁酯，10.5 kg丙烯酸-2-乙基己酯，1.5 kg丙烯酸，充分搅拌得到混合液A；将0.2 kg N-羟甲基丙烯酰胺溶于10.0 kg 去离子水中，全部溶解后，加入15.0 kg丙烯酸三乙基甲硅烷基酯、5.0 kg甲基丙烯酸三甲基硅酯、5.0 kg丙烯酸三异丙基甲硅烷基酯、5.0 kg甲基丙烯酸三异丙基甲硅烷基酯，搅拌均匀得到混合液B。
将反应器抽真空、充氮气重复三次，调温至30 ℃，加入20.0 kg溶有0.35 kg过硫酸铵和0.07 kg亚硫酸氢钠的去离子水溶液，3.5 h内将混合液A滴加至反应器中，滴完恒温反应10 min。继续滴加混合液B和10.0 kg溶有0.15 kg过硫酸铵的去离子水溶液，控制滴加时间1.5 h，滴完恒温反应2.0 h后结束反应，制得偏氯乙烯-丙烯酸酯-丙烯酸甲硅烷基酯乳液：固含量为57%左右，粘度为780 mpa·s。该乳液储存1年后保持稳定，涂膜硬度高，可有效趋避污损生物，耐水、耐盐雾性能好，可应用于水性防腐防污涂料。
应用实施例：适用实施例1-3中的偏氯乙烯-丙烯酸酯-丙烯酸甲硅烷基酯乳液，制备水性防腐防污涂料分别编号1-3。制备方法如下：按照质量百分比，先将15份颜料浆、0.3份润湿分散剂、0.1份流平剂、0.05份消泡剂，19.55份去离子水加入到搅拌釜中，用高速分散机分散50 min，然后将65份实施例1-3中制备的乳液缓慢加入到搅拌釜中，中速搅拌40min，然后过滤、出料、包装，制备出水性防腐防污涂料。按照既定单组分水性箱漆箱厂喷涂工艺和设计膜厚进行喷涂耐盐雾试验测试板。封边并养护干燥7天；待封边漆7天完全干燥后，编号并测试防腐防污性能。按国标T-1771-1991“色漆和清漆耐中性盐雾性能的测定”规定，划加速线并投板开始耐盐雾试验；每天查板一次，着重留意加速线和板面的起泡、锈蚀情况，800小时后拍照（图1）并记录评价结果（表1）。按国标GB/T6822-2007对应用实施例1-3涂料进行防污性能评价，于仿生海水中浸泡8周，记录其防污效果（表1）。
表1防腐防污涂料性能评价
| 编号 | 加速线 | 锈蚀 | 起泡 | 防污结果 |
| 1 | 10 | 10 | 无 | 表面光滑 |
| 2 | 10 | 10 | 无 | 表面光滑 |
| 3 | 10 | 10 | 无 | 表面光滑 |
备注：加速线分级0-10级，10级最好，无扩展。
锈蚀等级分0-10级，10级最好，无锈蚀。
起泡分F微量、M少量、MD中量、D大量四级。
由表1数据可知，本发明制得的水性防腐防污涂料所评价样板加速线扩展在0.5mm内，按ASTM D1654标准为10级；板面均未发生大面积锈蚀，锈蚀等级均能达到10级；未出现起泡现象；表面光滑；即该涂料具有良好的防腐、防污性能，应用前景广阔。
单体种类、引发剂用量、反应温度、单体浓度及反应时间的改变等因素都能影响本发明的实现，在此不再一一举实施例。
Claims (6)
1.一种防腐防污型涂料树脂及其制备方法，其特征在于包括以下步骤：首先将偏氯乙烯、丙烯酸酯、交联乳化单体、胶乳保护剂、亚硫酸氢钠和水加至容器中，室温搅拌均匀得混合液A；丙烯酸甲硅烷酯、交联乳化单体和水混合得混合液B；体系固含量为55～60%，交联乳化单体占总单体质量的0.5～2%，水的加入量为总单体质量的67～82%，胶乳保护剂的用量为总单体质量的0.1～0.5%；然后将反应器抽真空、充氮气重复三次，调温至15～30 ℃，分别加入混合液A中单体质量0.2～1.0%和0.05～0.15%的过硫酸铵和亚硫酸氢钠水溶液，将混合液A在3～4 h内滴加至反应器后，继续滴加混合液B，同时向反应器中滴加混合液B中单体质量0.2～1%的过硫酸铵水溶液，滴加时间1～2 h，滴完恒温反应2～3 h结束反应，制得偏氯乙烯-丙烯酸酯-丙烯酸甲硅烷基酯乳液。
2.根据权利要求1所述的防腐防污型涂料树脂及其制备方法，其特征在于所说的交联乳化单体为N-羟甲基丙烯酰胺、N-羟乙基丙烯酰胺、N-羟丙基丙烯酰胺的任意一种或任意两种及两种以上的混合物。
3.根据权利要求1所述的防腐防污型涂料树脂及其制备方法，其特征在于所说的丙烯酸酯为甲基丙烯酸甲酯、丙烯酸甲酯、丙烯酸乙酯、丙烯酸丁酯、丙烯酸-2-乙基己酯、丙烯酸、甲基丙烯酸的任意一种或任意两种及两种以上的混合物。
4.根据权利要求1所述的防腐防污型涂料树脂及其制备方法，其特征在于所说的丙烯酸甲硅烷基酯为丙烯酸三乙基甲硅烷基酯、丙烯酸三异丙基甲硅烷基酯、甲基丙烯酸三甲基硅酯、甲基丙烯酸三乙基甲硅烷基酯、甲基丙烯酸叔丁基二甲基甲硅烷基酯、甲基丙烯酸三异丙基甲硅烷基酯、甲基丙烯酸三苯基甲硅烷基酯的任意一种或任意两种及两种以上的混合物。
5.根据权利要求1所述的防腐防污型涂料树脂及其制备方法，其特征在于所说的反应温度为15～30 ℃。
6.根据权利要求1所述的防腐防污型涂料树脂及其制备方法，其特征在于所说的引发剂为过硫酸铵和亚硫酸氢钠。
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