CN114891402A - 一种钒与银纳米优化的低表面能防污涂料的制备方法 - Google Patents
一种钒与银纳米优化的低表面能防污涂料的制备方法 Download PDFInfo
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Abstract
本发明提供一种钒与银纳米优化的低表面能防污涂料的制备方法,属于防腐涂料技术领域。所述的制备方法包括以下步骤:将纳米钒酸铋分散到水中;再纳米钒酸铋溶液中加入硝酸银和蔗糖,超声处理再保温;离心固液分离烘干得到附银纳米钒酸铋;取聚四氟乙烯溶解在二甲苯中配成溶液A;将附银纳米钒酸铋、二氧化硅、纳米二氧化钛、分散剂、聚乙二醇辛基苯基醚、氟硅表面活性剂分散在二甲苯中形成液体B;将氟碳树脂溶解在二甲苯和醋酸丁酯的混合溶液中得到氟碳树脂溶液;将溶液A和溶液B倒入氟碳树脂溶液中,加入液体石蜡、疏水助剂、消泡剂和流平剂分散均匀;加入固化剂固化成膜。本发明的海洋防污涂料具有防污效果好、抑菌效果好、表面能低等特点。
Description
技术领域
本发明属于防腐涂料技术领域,具体涉及一种钒与银纳米优化的低表面能防污涂料的制备方法。
背景技术
众所周知,地球总面积约5.1亿平方千米,其中海洋面积约3.61亿平方千米,约占地球总面积的71%。海洋面积广大,孕育了丰富的物种,其中附着生物就多达几千种。这些附着生物会附着在船舶和海洋平台的表面,给船舶的航行安全,设备腐蚀等带来诸多问题。
人们使用海洋防污涂料有着十分悠久的历史。早在20世纪30年代。人们以沥青树脂、乙烯树脂及氯化橡胶为树脂,以氧化亚铜、***等金属氧化物作为防污剂制成海洋防污涂料。20世纪60年代。有机锡化合物(三丁基锡氧化物和三丁基锡氯化物)开始在防污涂料中得到广泛应用。这些防污涂料,依赖防污剂缓慢释放在海洋中,依赖对海洋生物的毒性,对海洋生物进行杀灭。20世纪80年代后,出现自抛光防污涂料,防污剂的渗出开始稳定。由于人们对环境保护的意识日益增强,21世纪初,人们开始禁止使用有机锡防污剂,氧化亚铜防污剂的使用也逐步减少。
BiVO4半导体材料具有无毒、稳定、光利用率高、杀菌效果好等优点广泛的应用于光催化和杀菌方面,但BiVO4具有较高的光生电子-空穴的复合效率等缺点,需要进一步提高其光催化杀菌活性,并将其应用于海洋防污涂料中。
发明内容
本发明通过提供一种钒与银纳米优化的低表面能防污涂料的制备方法,以解决上述技术问题。
为实现上述目的,本发明的技术解决方案是:
一种钒与银纳米优化的低表面能防污涂料的制备方法,包括以下步骤:
(1)将纳米钒酸铋分散到水中,加入分散剂,分散均匀得到纳米钒酸铋溶液;
(2)再纳米钒酸铋溶液中加入硝酸银和蔗糖,搅拌均匀,然后将溶液加热至60-75℃,边搅拌边超声0.5-1.5小时,再保温搅拌8-10小时;
(3)离心固液分离,再用清水洗涤固液分离三次,将获得的固体于80-85℃烘干得到附银纳米钒酸铋;
(4)取聚四氟乙烯溶解在二甲苯中配成溶液A;
(5)将附银纳米钒酸铋、二氧化硅、纳米二氧化钛、分散剂、聚乙二醇辛基苯基醚、氟硅表面活性剂分散在二甲苯中形成液体B;
(6)将氟碳树脂溶解在二甲苯和醋酸丁酯的混合溶液中得到氟碳树脂溶液;
(7)将溶液A和溶液B倒入氟碳树脂溶液中,加入液体石蜡、疏水助剂、消泡剂和流平剂在搅拌机中分散均匀;最后加入固化剂后固化成膜。
优选地,所述步骤(1)中纳米钒酸铋、水和分散剂的质量份数分别为纳米钒酸铋15-20份、水80-110份、分散剂0.5-0.7份。
优选地,所述步骤(2)中硝酸银和蔗糖的质量份数分别为硝酸银0.6-1.2份、蔗糖1.5-3.0份。
优选地,所述步骤(2)中保温温度为60-75℃,搅拌时间9小时。
优选地,所述步骤(4)中聚四氟乙烯和二甲苯的质量份数分别为聚四氟乙烯6-9份、二甲苯12-14份。
优选地,所述步骤(5)中二氧化硅、纳米二氧化钛、分散剂、聚乙二醇辛基苯基醚、氟硅表面活性剂、二甲苯的质量份数分别为二氧化硅5-7份、纳米二氧化钛4-6份、分散剂0.5-0.8份、聚乙二醇辛基苯基醚1.2-1.6份、氟硅表面活性剂0.1-0.3份、二甲苯15-18份。
优选地,所述步骤(6)中氟碳树脂、二甲苯和醋酸丁酯的质量份数分别为氟碳树脂55-60份、二甲苯1-4份、醋酸丁酯3-5份。
优选地,所述步骤(7)中液体石蜡、疏水助剂、消泡剂、流平剂和固化剂的质量份数分别为液体石蜡3-4份、疏水助剂1-2份、消泡剂0.2-0.7份、流平剂0.1-0.2份、固化剂5-7份。
本发明的作用原理为:
1.钒酸铋的禁带宽度在2.4eV左右,吸收峰波长在517nm左右,在可见光的条件下可以具有光催化性能。钒酸铋可见光吸收能力强、化学稳定性强、具有较强的氧化还原能力,具备较强的杀菌能力,且本身无毒。钒酸铋对大肠杆菌,铜绿假单胞菌等许多菌种具有非常强的杀菌效果,能够有效的对船舶,海洋平台等表面附着生物进行杀灭,是海洋生物不能够长期有效的附着在船舶等的表面。
纳米TiO2在紫外光的情况下有着非常好的光催化效果,可以补充钨酸铋紫外波段的杀菌能力,ZnO本身具有强烈的杀菌效果。
2.钒酸铋的禁带宽度在2.4eV,对517nm左右的蓝光具有较好的吸收。钨酸铋的带吸收是一个较宽的吸收峰,可以从500nm到300nm均有较好的吸收。TiO2的禁带宽度在3.2eV,其光吸收曲线可以从3.2eV延伸到4.5eV,对276-388nm波段的紫外光有较强吸收。两种纳米材料的协同作用,可以吸收500-276nm波段较强能量的光,光吸收的范围比较宽。
3.钒酸铋与纳米银协同防污能力强
钒酸铋与纳米银协同作用,吸收波段可以从550-250nm,吸收波段比较宽。钒酸铋与纳米银协同防污能力强,当紫外光激发Ag-BiVO4后,电子从价带跃迁到导带上,此时催化剂表面的Ag粒子或AgO易捕获电子,在外部电场的作用下其不易出现复合,因此光电协同作用下,Ag-BiVO4的光电催化性能超过单一的钒酸铋。
其光电催化过程如下:
Ag-BiVO4+hν→[e-]+[h+]
[h+]+H2O→·OH+H+
O2+[e-]→·O2 -
因此附Ag钒酸铋会有良好的光催化效果,能够有效阻止海洋生物的附着。目前,附Ag钒酸铋应用于污染物降解,光催化产H2等方面,对于防污涂料中,防污剂方面的应用的报道十分少见。
4.在一定条件下,涂料中的钒酸铋能够与纳米二氧化钛形成多种类型光催化材料,包括Z型和II型等。这种材料能够有效的吸收可见光,在钒酸铋的导带中形成电子,价带中形成空穴,同时TiO2可以吸收紫外光,在导带中形成电子,价带中形成空穴。那么将发生以下反应:
BiVO4+hν→BiVO4([e–]–[h+])
TiO2[e–]+BiVO4→TiO2+BiVO4[e–]
同时,在纳米二氧化钛的导带上,氧气与导带的电子发生反应,形成O–自由基:
O2+[e–]→[·O2]–
[·O2]–+H+→[HO2·]–
[e–]+[HO2·]–+H+→H2O2
H2O2+[e–]→·OH+OH–
TiO2/BiVO4成的异质结主要应用于污染物降解,光催化产H2等方面,很少用于防污涂料。
本发明的有益效果是:
本发明同时结合附银纳米钒酸铋和低表面能防污材料的各自优势,制成的海洋防污涂料具有防污效果好、抑菌效果好、表面能低、与水接触角达到120°等特点。
具体实施方式
下面对本发明实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例仅仅是本发明的一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有作出创造性劳动前提下所获得的所有其他实施例,都属于本发明保护的范围。
另外,本发明各个实施例之间的技术方案可以相互结合,但是必须是以本领域普通技术人员能够实现为基础,当技术方案的结合出现相互矛盾或无法实现时应当认为这种技术方案的结合不存在,也不在本发明要求的保护范围之内。
实施例1
一种钒与银纳米优化的低表面能防污涂料的制备方法,包括以下步骤:
(1)将纳米钒酸铋20份分散到水110份中,加入分散剂0.6份,分散均匀得到纳米钒酸铋溶液;
(2)再纳米钒酸铋溶液中加入硝酸银0.6份和蔗糖2.0,搅拌均匀,然后将溶液加热至75℃,边搅拌边超声1.5小时,再于温度为60℃条件下保温搅拌9小时;
(3)离心固液分离,再用清水洗涤固液分离三次,将获得的固体于85℃烘干得到附银纳米钒酸铋;
(4)取聚四氟乙烯6份溶解在二甲苯14份中配成溶液A;
(5)将步骤(3)的附银纳米钒酸铋以及二氧化硅6份、纳米二氧化钛4-6份、分散剂0.7份、聚乙二醇辛基苯基醚1.2份、氟硅表面活性剂0.1份分散在二甲苯16份中形成液体B;
(6)将氟碳树脂55份溶解在二甲苯1份和醋酸丁酯3份的混合溶液中得到氟碳树脂溶液;
(7)将溶液A和溶液B倒入氟碳树脂溶液中,加入液体石蜡3份、疏水助剂1份、消泡剂0.5份和流平剂0.2份在搅拌机中分散均匀;最后加入固化剂6份后固化成膜。
实施例2
一种钒与银纳米优化的低表面能防污涂料的制备方法,包括以下步骤:
(1)将纳米钒酸铋15份分散到水80份中,加入分散剂0.7份,分散均匀得到纳米钒酸铋溶液;
(2)再纳米钒酸铋溶液中加入硝酸银1份和蔗糖3.0,搅拌均匀,然后将溶液加热至60℃,边搅拌边超声0.5小时,再于温度为65℃条件下保温搅拌10小时;
(3)离心固液分离,再用清水洗涤固液分离三次,将获得的固体于80℃烘干得到附银纳米钒酸铋;
(4)取聚四氟乙烯7份溶解在二甲苯12份中配成溶液A;
(5)将步骤(3)的附银纳米钒酸铋以及二氧化硅7份、纳米二氧化钛5份、分散剂0.8份、聚乙二醇辛基苯基醚1.4份、氟硅表面活性剂0.2份分散在二甲苯18份中形成液体B;
(6)将氟碳树脂58份溶解在二甲苯2份和醋酸丁酯4份的混合溶液中得到氟碳树脂溶液;
(7)将溶液A和溶液B倒入氟碳树脂溶液中,加入液体石蜡3.5份、疏水助剂1.5份、消泡剂0.7份和流平剂0.1份在搅拌机中分散均匀;最后加入固化剂7份后固化成膜。
实施例3
一种钒与银纳米优化的低表面能防污涂料的制备方法,包括以下步骤:
(1)将纳米钒酸铋18份分散到水100份中,加入分散剂0.5份,分散均匀得到纳米钒酸铋溶液;
(2)再纳米钒酸铋溶液中加入硝酸银1.2份和蔗糖1.5,搅拌均匀,然后将溶液加热至70℃,边搅拌边超声1小时,再于温度为75℃条件下保温搅拌8小时;
(3)离心固液分离,再用清水洗涤固液分离三次,将获得的固体于85℃烘干得到附银纳米钒酸铋;
(4)取聚四氟乙烯9份溶解在二甲苯13份中配成溶液A;
(5)将步骤(3)的附银纳米钒酸铋以及二氧化硅5份、纳米二氧化钛6份、分散剂0.5份、聚乙二醇辛基苯基醚1.6份、氟硅表面活性剂0.3份分散在二甲苯15份中形成液体B;
(6)将氟碳树脂60份溶解在二甲苯3份和醋酸丁酯4.5份的混合溶液中得到氟碳树脂溶液;
(7)将溶液A和溶液B倒入氟碳树脂溶液中,加入液体石蜡4份、疏水助剂2份、消泡剂0.2份和流平剂0.1份在搅拌机中分散均匀;最后加入固化剂5份后固化成膜。
实施例4
一种钒与银纳米优化的低表面能防污涂料的制备方法,包括以下步骤:
(1)将纳米钒酸铋19份分散到水90份中,加入分散剂0.6份,分散均匀得到纳米钒酸铋溶液;
(2)再纳米钒酸铋溶液中加入硝酸银1份和蔗糖2.5,搅拌均匀,然后将溶液加热至70℃,边搅拌边超声0.8小时,再于温度为65℃条件下保温搅拌9小时;
(3)离心固液分离,再用清水洗涤固液分离三次,将获得的固体于80℃烘干得到附银纳米钒酸铋;
(4)取聚四氟乙烯7份溶解在二甲苯13份中配成溶液A;
(5)将步骤(3)的附银纳米钒酸铋以及二氧化硅6份、纳米二氧化钛5份、分散剂0.6份、聚乙二醇辛基苯基醚1.4份、氟硅表面活性剂0.2份分散在二甲苯17份中形成液体B;
(6)将氟碳树脂58份溶解在二甲苯4份和醋酸丁酯5份的混合溶液中得到氟碳树脂溶液;
(7)将溶液A和溶液B倒入氟碳树脂溶液中,加入液体石蜡3份、疏水助剂1份、消泡剂0.4份和流平剂0.1份在搅拌机中分散均匀;最后加入固化剂6份后固化成膜。
检测试验
采用水滴方式对实施例1-4所得的防污涂料的涂层接触角进行测量。
具体为将一定量实施例1-4所得的防污涂料,分别滴在大肠杆菌培养皿中,恒温37℃条件下培养36h小时后取出,用照相机拍照,划定抑菌环,并用游标卡尺测量其尺寸。引用标准:根据国家标准GB/T4789.37-2008Baird-Parker平板计数实现金黄色葡萄球菌检测计数,计算抑菌率,结果见下表。
防污涂料的涂层接触角实验结果表
实施例 | 接触角 | 抑菌直径 | 抑菌率 |
实施例1 | 121.2° | 12.7mm | 97.3% |
实施例2 | 123.1° | 14.6mm | 98.2% |
实施例3 | 125.7° | 15.8mm | 98.5% |
实施例4 | 128.5° | 17.9mm | 98.7% |
从上表可知,本发明中防污涂料的涂层接触角大于121.2°,抑菌率高于97.3%,这是因为:大颗粒SiO2与纳米填料可以的相互作用,可以在涂层表面形成微小凸起,这种微小凸起可以起到类似荷叶的效应,有效降低材料本身的表面能。此外氟碳涂料本身表面能小,添加液体石蜡、疏水助剂后进一步降低涂料的表面能,增加接触角,所以涂料表面的接触角大于120°,具有良好的疏水性。TiO2和BiVO4,以及部分TiO2/BiVO4异质结在光照条件下,产生光生e–或h+,并进一步与H2O或O2反应氧化还原反应,生成具有强氧化性的·OH、·O2和H2O2等活性自由基。这些光生自由基可与细胞壁、细胞膜或胞内物质发生反应,导致细胞膜和细胞壁的破坏以及胞内功能分子的变性能够对海洋生物等进行良好的抑制作用。Ag一方面可以直接杀灭海洋生物,另一方面可以促进导带电子与价带空穴的分离,促进涂料良好的阻止海洋生物的性能,所以涂料的抑菌率效果好,大于97.3%。
以上所述仅为本发明的实施例,并非因此限制本发明的专利范围,凡是利用本发明说明书所作的等效变换,或直接或间接运用在其它相关的技术领域,均同理包括在本发明的专利保护范围内。
Claims (8)
1.一种钒与银纳米优化的低表面能防污涂料的制备方法,其特征在于,包括以下步骤:
(1)将纳米钒酸铋分散到水中,加入分散剂,分散均匀得到纳米钒酸铋溶液;
(2)再纳米钒酸铋溶液中加入硝酸银和蔗糖,搅拌均匀,然后将溶液加热至60-75℃,边搅拌边超声0.5-1.5小时,再保温搅拌8-10小时;
(3)离心固液分离,再用清水洗涤固液分离三次,将获得的固体于80-85℃烘干得到附银纳米钒酸铋;
(4)取聚四氟乙烯溶解在二甲苯中配成溶液A;
(5)将附银纳米钒酸铋、二氧化硅、纳米二氧化钛、分散剂、聚乙二醇辛基苯基醚、氟硅表面活性剂分散在二甲苯中形成液体B;
(6)将氟碳树脂溶解在二甲苯和醋酸丁酯的混合溶液中得到氟碳树脂溶液;
(7)将溶液A和溶液B倒入氟碳树脂溶液中,加入液体石蜡、疏水助剂、消泡剂和流平剂在搅拌机中分散均匀;最后加入固化剂后固化成膜。
2.根据权利要求1所述的钒与银纳米优化的低表面能防污涂料的制备方法,其特征在于,所述步骤(1)中纳米钒酸铋、水和分散剂的质量份数分别为纳米钒酸铋15-20份、水80-110份、分散剂0.5-0.7份。
3.根据权利要求1所述的钒与银纳米优化的低表面能防污涂料的制备方法,其特征在于,所述步骤(2)中硝酸银和蔗糖的质量份数分别为硝酸银0.6-1.2份、蔗糖1.5-3.0份。
4.根据权利要求1所述的钒与银纳米优化的低表面能防污涂料的制备方法,其特征在于,所述步骤(2)中保温温度为60-75℃,搅拌时间9小时。
5.根据权利要求1所述的钒与银纳米优化的低表面能防污涂料的制备方法,其特征在于,所述步骤(4)中聚四氟乙烯和二甲苯的质量份数分别为聚四氟乙烯6-9份、二甲苯12-14份。
6.根据权利要求1所述的钒与银纳米优化的低表面能防污涂料的制备方法,其特征在于,所述步骤(5)中二氧化硅、纳米二氧化钛、分散剂、聚乙二醇辛基苯基醚、氟硅表面活性剂、二甲苯的质量份数分别为二氧化硅5-7份、纳米二氧化钛4-6份、分散剂0.5-0.8份、聚乙二醇辛基苯基醚1.2-1.6份、氟硅表面活性剂0.1-0.3份、二甲苯15-18份。
7.根据权利要求1所述的钒与银纳米优化的低表面能防污涂料的制备方法,其特征在于,所述步骤(6)中氟碳树脂、二甲苯和醋酸丁酯的质量份数分别为氟碳树脂55-60份、二甲苯1-4份、醋酸丁酯3-5份。
8.根据权利要求1所述的钒与银纳米优化的低表面能防污涂料的制备方法,其特征在于,所述步骤(7)中液体石蜡、疏水助剂、消泡剂、流平剂和固化剂的质量份数分别为液体石蜡3-4份、疏水助剂1-2份、消泡剂0.2-0.7份、流平剂0.1-0.2份、固化剂5-7份。
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