CN104293062A - 水性软生质防污涂料及其制备方法 - Google Patents
水性软生质防污涂料及其制备方法 Download PDFInfo
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Abstract
本发明属于海洋保护技术领域，特别涉及一种水性软生质防污涂料及其制备方法。一种水性软生质防污涂料，该涂料包含A、B双组分，A、B组分的质量比为8-10:1，其中A组分为树脂基料载体，质量分数配比为：水性丙烯酸树脂60-66%、氧化铁红0-6%，氧化锌5%，活性二氧化硅0-3%，有机膨润土0-1%，吡啶硫酮锌3-4%，吡啶硫酮铜3-4%，防污剂9-10%，乙醇5%，水6%；B组分为交联剂。本发明采用的配方无毒无害，混合后得到的防污涂料防污效果好。
Description
技术领域
本发明属于海洋保护技术领域，特别涉及一种水性软生质防污涂料及其制备方法。
背景技术
众所周知，应对海洋生物污损最有效、最经济的办法是采用防污涂料。发展至今防污涂料已历经数代，形成了以自抛光型、低表面能型为代表的一整套涂料树脂制备技术，极大的促进了海洋涂料的发展。现有的各种防污涂料虽然防污性能较好，但是以有毒有害的居多，且具有较高的VOC排放，不利于环境保护。
发明内容
本发明提供一种既满足环保要求、又兼具高效的防污性能的水性软生质防污涂料。
本发明还提供所述水性软生质防污涂料的制备方法。
本发明解决其技术问题所采用的技术方案是：
一种水性软生质防污涂料，该涂料包含A、B双组分，A、B组分的质量比为8-10:1，其中A组分为树脂基料载体，质量分数配比为：水性丙烯酸树脂60-66％、氧化铁红0-6％，氧化锌5％，活性二氧化硅0-3％，有机膨润土0-1％，吡啶硫酮锌3-4％，吡啶硫酮铜3-4％，防污剂9-10％，乙醇5％，水6％；B组分为交联剂。本发明采用的配方无毒无害，混合后得到的防污涂料防污效果好。
作为优选，B组分选自30wt％的铜氨络合离子溶液，氮丙啶交联剂30wt％、乙醇40wt％和水30wt％的混合液，或正硅酸乙酯12wt％、氮丙啶交联剂18wt％、乙醇40wt％和水30wt％的混合液。
一种所述的水性软生质防污涂料的制备方法，包括如下步骤：
(1)水性丙烯酸树脂的合成
(2)水性软生质防污涂料的制备将步骤(1)制得的水性丙烯酸树脂按照权利要求1所述的配比制成树脂基料载体，即A组分，然后将A组分与B组分充分混合，得到所述水性软生质防污涂料。
步骤(1)的具体方法如下：将0.2重量份过氧化苯甲酰与200重量份乙醇混合后升温至78℃，然后向该混合物中加入包含12重量份丙烯酸、46重量份甲基丙烯酸甲酯、71重量份丙烯酸乙酯、63重量份丙烯酸丁酯、8重量份丙烯酸羟乙酯和1.6重量份过氧化苯甲酰的混合液，经3小时恒速滴加完毕，再加入0.2重量份过氧化苯甲酰，继续反应至充分，冷却至室温，加入氨水25重量份充分搅拌至反应完全，得到水性丙烯酸树脂。
步骤(1)的具体方法如下：将0.2重量份过氧化苯甲酰和200重量份乙醇混合后升温至78℃，然后向该混合物中加入包含12重量份丙烯酸、46重量份甲基丙烯酸甲酯、61重量份丙烯酸乙酯、63重量份丙烯酸丁酯、10重量份γ-(甲基丙烯酰氧基)丙基三甲氧基硅烷、8重量份丙烯酸羟乙酯和1.6重量份过氧化苯甲酰的混合液，经3小时恒速滴加完毕，加入0.2重量份过氧化苯甲酰，继续反应至充分，冷却至60℃，加入羟基硅油20重量份，继续反应12h以上，冷却至室温，加入氨水15重量份充分搅拌至反应完全，得到改性水性丙烯酸树脂。
步骤(1)的具体方法如下：将0.2重量份过氧化苯甲酰和200重量份乙醇混合后升温至78℃，然后向该混合物中加入包含20重量份丙烯酰胺、36重量份甲基丙烯酸甲酯、71重量份聚氧化乙烯醚甲基丙烯酸酯、65重量份丙烯酸丁酯、8重量份丙烯酸羟乙酯和1.6重量份过氧化苯甲酰的混合液，经3小时恒速滴加完毕，加入0.2重量份过氧化苯甲酰后继续反应至充分，冷却至室温后完成反应，得到水性丙烯酸树脂。
本发明的水性软生质防污涂料是新一代基于“积极防御”技术的高级污损防御型防污漆，是继自抛光、低表面能防污涂料之后出现的一种智能复合防污涂料。这种涂料，将国际上最前沿的涂料设计理念和仿生学的概念结为一体，是仿生学领域中又一次成功的应用典范。它充分利用了先进的柔性聚合物分子制备技术和有效的防污剂所叠合的效果，形成特殊的表面防污阻隔层可以有效地延长防污期效(≥5年)，同时具有很高的节约能源的潜力。
本发明的水性软生质防污涂料不同于以自抛光、低表面能防污涂料为代表的溶剂型硬生质防污涂料。在制备的过程中，水性软生质防污涂料主要以水为分散介质，极大地降低了环境的污染，是一类绿色健康型的防污涂料。在使用的过程中，软生质智能防污涂料与海水发生复杂的物理化学作用，在防污漆的表面形成一种类似于海藻吸水后的光滑柔性隔离层，有效地防止了海生物的附着。当意外碰撞发生后，柔性的智能防污涂料能够适时启动自修复机制，修复受损的涂层表面，持续有效地防止海生物的附着。因此，水性软生质防污涂料满足绿色环保的要求，同时又兼具高效的防污性能。
具体实施方式
下面通过具体实施例，对本发明的技术方案作进一步的具体说明。应当理解，本发明的实施并不局限于下面的实施例，对本发明所做的任何形式上的变通和/或改变都将落入本发明保护范围。
在本发明中，若非特指，所有的份、百分比均为重量单位，所采用的设备和原料等均可从市场购得或是本领域常用的。下述实施例中的方法，如无特别说明，均为本领域的常规方法。
以下实施例提供了四类水性软生质防污涂料的制备方法。
实施例1 水性软生质柔性交联防污涂料的制备
(1)水性丙烯酸树脂的合成
在装有搅拌器、回流冷凝管、恒压滴液漏斗的四口烧瓶中加入0.2g过氧化苯甲酰、200g乙醇，升温至78℃，然后向该混合物中加入包含12g丙烯酸、46g甲基丙烯酸甲酯、71g丙烯酸乙酯、63g丙烯酸丁酯、8g丙烯酸羟乙酯、1.6g过氧化苯甲酰的混合液，用恒压滴液漏斗经3小时恒速滴加完毕，加入0.2g过氧化苯甲酰，继续恒温反应(78℃，下同)3小时后，冷却至室温，加入氨水25g调节pH至中性，搅拌2h后完成反应，得到水性丙烯酸树脂。
(2)水性软生质柔性交联防污涂料的制备
涂料包含A、B双组分，A、B组分的质量之比为10:1，混合均匀即可。
其中A组分为树脂基料载体，具体成分如下：水性丙烯酸树脂60％、氧化铁红6％，氧化锌5％，吡啶硫酮锌4％，吡啶硫酮铜4％，防污剂Sea-Nine21110％，乙醇5％，水6％；
其中B组分为交联剂，具体成分如下：铜氨络合离子溶液(30wt％)；
具体合成路线如下：
经检测，改性树脂双键完全聚合，数均分子量Mn为28580，多分散系数Mw\Mn为2.12，附着力≤1级，粘度≤200S(涂四杯法)，固含量约为50％，实海挂板测试6个月证明具有优异的防污效果。海生物附着在2％以下。
实施例2 水性软生质自凝胶防污涂料的制备
(1)改性水性丙烯酸树脂的合成
在装有搅拌器、回流冷凝管、恒压滴液漏斗的四口烧瓶中加入0.2g过氧化苯甲酰、200g乙醇，升温至78℃，然后向该混合物中加入包含12g丙烯酸、46g甲基丙烯酸甲酯、61g丙烯酸乙酯、63g丙烯酸丁酯、10gγ-(甲基丙烯酰氧基)丙基三甲氧基硅烷、8g丙烯酸羟乙酯、1.6g过氧化苯甲酰的混合液，用恒压滴液漏斗经3小时恒速滴加完毕，加入0.2g过氧化苯甲酰，继续恒温反应3小时后，冷却至60℃，加入羟基硅油20g，反应12h，冷却至室温，加入氨水15g调节pH和树脂的亲水性，搅拌2h后完成反应，得到改性水性丙烯酸树脂。
(2)水性软生质自凝胶防污涂料的制备
涂料包含A、B双组分，A、B组分的质量之比为8:1，混合均匀即可。
其中A组分为树脂基料载体，具体成分如下：水性改性丙烯酸树脂60％、氧化铁红5％、有机膨润土1％，氧化锌5％，吡啶硫酮铜4％，吡啶硫酮锌4％，Sea-Nine 21110％，乙醇5％，水6％；
其中B组分为交联剂，具体成分如下：氮丙啶交联剂30％，乙醇40％，水30％。
具体合成路线如下：
经检测，改性树脂双键完全聚合，数均分子量Mn为24370，多分散系数Mw\Mn为2.69，附着力≤1级，粘度≤200S(涂四杯法)，固含量约为50％，实海挂板测试6个月证明具有优异的防污效果。海生物附着在2％以下。
实施例3：水性软生质自修复防污涂料的制备
(1)改性水性丙烯酸树脂的合成
在装有搅拌器、回流冷凝管、恒压滴液漏斗的四口烧瓶中加入0.2g过氧化苯甲酰、200g乙醇，升温至78℃，然后向该混合物中加入包含12g丙烯酸、46g甲基丙烯酸甲酯、61g丙烯酸乙酯、63g丙烯酸丁酯、10gγ-(甲基丙烯酰氧基)丙基三甲氧基硅烷、8g丙烯酸羟乙酯、1.6g过氧化苯甲酰的混合液，用恒压滴液漏斗经3小时恒速滴加完毕，加入0.2g过氧化苯甲酰，继续恒温反应3小时后，冷却至60℃，加入羟基硅油20g，反应12h，冷却至室温，加入氨水15g调节pH和树脂的亲水性，搅拌2h后完成反应，得到水性丙烯酸树脂。
(2)水性软生质自修复防污涂料的制备
涂料包含A、B双组分，A、B组分的质量之比为10:1，混合均匀即可。
其中A组分为树脂基料载体，具体成分如下：水性丙烯酸树脂60％、氧化铁红6％，氧化锌5％，活性二氧化硅3％，吡啶硫酮锌3％，吡啶硫酮铜3％，防污剂Sea-Nine 2119％，乙醇5％，水6％；
其中B组分为交联剂，现配现用，具体成分如下：正硅酸乙酯12％，氮丙啶交联剂18％，乙醇40％，水30％。
合成路线可参照实施例2。
经检测，改性树脂双键完全聚合，数均分子量Mn为27470，多分散系数Mw\Mn为2.24，附着力≤1级，粘度≤200S(涂四杯法)，固含量约为50％，实海挂板测试6个月证明具有优异的防污效果。海生物附着在2％以下。
实施例4：水性软生质自适应防污涂料的制备
(1)改性水性丙烯酸树脂的合成
在装有搅拌器、回流冷凝管、恒压滴液漏斗的四口烧瓶中加入0.2g过氧化苯甲酰、200g乙醇，升温至78℃，然后向该混合物中加入包含20g丙烯酰胺、36g甲基丙烯酸甲酯、71g聚氧化乙烯醚甲基丙烯酸酯、65g丙烯酸丁酯、8g丙烯酸羟乙酯、1.6g过氧化苯甲酰的混合液，用恒压滴液漏斗经3小时恒速滴加完毕，加入0.2g过氧化苯甲酰，继续恒温反应3小时后，冷却至室温后完成反应，得到水性丙烯酸树脂。
(2)水性软生质自适应防污涂料的制备
涂料包含A、B双组分，A、B组分的质量之比为8:1，混合均匀即可。
其中A组分为树脂基料载体，具体成分如下：水性丙烯酸树脂66％、氧化锌5％，吡啶硫酮锌4％，吡啶硫酮铜4％，防污剂Sea-Nine 21110％，乙醇5％，水6％；
其中B组分为交联剂载体，具体成分如下：氮丙啶交联剂30％，乙醇40％，水30％。
具体合成路线如下：
经检测，改性树脂双键完全聚合，数均分子量Mn为38120，多分散系数Mw\Mn为2.98，附着力≤1级，粘度≤200S(涂四杯法)，固含量约为50％，实海挂板测试6个月证明具有优异的防污效果。海生物附着在2％以下。
以上所述的实施例只是本发明的一种较佳的方案，并非对本发明作任何形式上的限制，在不超出权利要求所记载的技术方案的前提下还有其它的变体及改型。
Claims (6)
1.一种水性软生质防污涂料，其特征在于：该涂料由A、B双组分混合而成，A、B组分的质量比为8-10:1，其中
A组分为树脂基料载体，质量分数配比为：水性丙烯酸树脂60-66%、氧化铁红0-6%，氧化锌5%，活性二氧化硅0-3%，有机膨润土0-1%，吡啶硫酮锌3-4%，吡啶硫酮铜3-4%，防污剂 9-10%，乙醇5%，水6%；
B组分为交联剂。
2.根据权利要求1所述的水性软生质防污涂料，其特征在于：B组分选自30 wt%的铜氨络合离子溶液，氮丙啶交联剂30 wt %、乙醇40 wt %和水30 wt %的混合液，或正硅酸乙酯12 wt %、氮丙啶交联剂18 wt %、乙醇40 wt %和水30 wt %的混合液。
3.一种权利要求1所述的水性软生质防污涂料的制备方法，其特征在于包括如下步骤：
（1）水性丙烯酸树脂的合成
（2）水性软生质防污涂料的制备 将步骤（1）制得的水性丙烯酸树脂按照权利要求1所述的配比制成树脂基料载体，即A组分，然后将A组分与B组分充分混合，得到所述水性软生质防污涂料。
4.根据权利要求3所述的制备方法，其特征在于步骤（1）的具体方法如下：将0.2重量份过氧化苯甲酰与200重量份乙醇混合后升温至78℃，然后向该混合物中加入包含12重量份丙烯酸、46重量份甲基丙烯酸甲酯、71重量份丙烯酸乙酯、63重量份丙烯酸丁酯、8重量份丙烯酸羟乙酯和1.6重量份过氧化苯甲酰的混合液，经3小时恒速滴加完毕，再加入0.2重量份过氧化苯甲酰，继续反应至充分，冷却至室温，加入氨水25重量份充分搅拌至反应完全，得到水性丙烯酸树脂。
5.根据权利要求3所述的制备方法，其特征在于步骤（1）的具体方法如下：将0.2重量份过氧化苯甲酰和200重量份乙醇混合后升温至78℃，然后向该混合物中加入包含12重量份丙烯酸、46重量份甲基丙烯酸甲酯、61重量份丙烯酸乙酯、63重量份丙烯酸丁酯、10重量份γ-（甲基丙烯酰氧基）丙基三甲氧基硅烷、8重量份丙烯酸羟乙酯和1.6重量份过氧化苯甲酰的混合液，经3小时恒速滴加完毕，加入0.2重量份过氧化苯甲酰，继续反应至充分，冷却至60℃，加入羟基硅油20 重量份，继续反应12 h以上，冷却至室温，加入氨水15重量份充分搅拌至反应完全，得到改性水性丙烯酸树脂。
6.根据权利要求3所述的制备方法，其特征在于步骤（1）的具体方法如下：将0.2重量份过氧化苯甲酰和200重量份乙醇混合后升温至78℃，然后向该混合物中加入包含20重量份丙烯酰胺、36重量份甲基丙烯酸甲酯、71重量份聚氧化乙烯醚甲基丙烯酸酯、65重量份丙烯酸丁酯、8重量份丙烯酸羟乙酯和1.6重量份过氧化苯甲酰的混合液，经3小时恒速滴加完毕，加入0.2重量份过氧化苯甲酰后继续反应至充分，冷却至室温后完成反应，得到水性丙烯酸树脂。
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| CN103525218A (zh) * | 2013-09-30 | 2014-01-22 | 中国船舶重工集团公司第七二五研究所 | 一种环保型防污涂料及其制备方法 |
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| CN105367706A (zh) * | 2015-12-11 | 2016-03-02 | 舟山市恒泰漆业有限责任公司 | 一种丙烯酸防污树脂的制备方法及降低防污剂用量的环境友好型船底防污漆及其制备方法 |
| CN105949382A (zh) * | 2016-06-21 | 2016-09-21 | 浙江省海洋开发研究院 | 一种生物杀菌型丙烯酸树脂及采用其制备的新型海洋防污涂料组合物 |
| CN105949382B (zh) * | 2016-06-21 | 2018-06-05 | 浙江省海洋开发研究院 | 一种生物杀菌型丙烯酸树脂及采用其制备的海洋防污涂料组合物 |
| CN107286794A (zh) * | 2017-08-03 | 2017-10-24 | 厦门双瑞船舶涂料有限公司 | 一种不含铜类防污剂的减阻防污涂料及其制备方法 |
| CN112175434A (zh) * | 2020-08-24 | 2021-01-05 | 中国船舶重工集团公司第七二五研究所 | 一种含稀土/防污剂的防污凝胶粒子及其制备方法 |
| CN112175434B (zh) * | 2020-08-24 | 2021-07-27 | 中国船舶重工集团公司第七二五研究所 | 一种含稀土/防污剂的防污凝胶粒子及其制备方法 |
| WO2022041429A1 (zh) * | 2020-08-24 | 2022-03-03 | 中国船舶重工集团公司第七二五研究所 | 一种含稀土/防污剂的防污凝胶粒子及其制备方法 |
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