CN116396645B - 一种耐蚀耐磨的涂塑钢管及其制造工艺 - Google Patents
一种耐蚀耐磨的涂塑钢管及其制造工艺 Download PDFInfo
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Abstract
本发明涉及一种耐蚀耐磨的涂塑钢管及其制造工艺,属于涂塑钢管技术领域。本发明提供的涂塑钢管,采用氟化石墨烯和磷酸锆预复合,再与TiO2通过硅烷偶联剂复合,加入用环氧树脂补强的氟碳树脂中,制得一种具有高交联密度的涂塑层涂料用于涂塑钢管,有效提升了涂塑钢管的耐腐蚀性和耐磨性,其内部大分子交联网络,增加了涂层内部的稳定性以及致密性,分散体与基体有良好的相容性,延长了腐蚀介质的侵蚀路径,进而提升了涂层防腐性能,发挥保护金属基体的作用,使涂层具有优异的机械性能和耐化学品性。
Description
技术领域
本发明属于涂塑钢管技术领域,具体地,涉及一种耐蚀耐磨的涂塑钢管及其制造工艺。
背景技术
管材在输送介质中或放在大气、水土等环境条件中,管壁也会受到不同的侵蚀,直接关系到管材的使用寿命。食品、自来水管线、石化管道等诸多介质均不允许管壁锈蚀而使输送介质受到破坏,管道的防锈保护是重点课题。涂塑管材问题也随之而来,目前我国境内钢塑管从衬塑逐渐迈向了涂塑,而涂塑材质也大多使用了塑料粉状物质材质,当中特性较好的为聚丙烯树脂和环氧树脂,但由于它的施工条件较高,生产工艺困难度大,质量管理不易,生产设备投入较大,严重影响了涂塑管材的普及和使用,而中国境内目前只有生产孔径小于a250mm的涂塑管材。
涂塑管材,是指通过在管材内壁或外墙上以涂塑工艺热熔一层塑层起到防护管材内壁的一类管材,通常在涂塑以前就要先对管材的内壁和外墙面加以处理,如抛丸除锈等作业,使管材的内壁表面尽量光滑,以提高涂塑层与管材内部的结合紧密性,结合精密性不够,只是因为管材和涂塑层之间的热膨胀系数相差太大而导致的,由于现在的涂塑材质通常是聚乙烯和聚氯乙烯,易于老化,并且在温度变动相当大的情形下,由于管材无法弯曲、不可挤压,也不能冲刷和碰撞,因此,涂塑层很容易产生热剥落。而已有的涂塑层当管线切断时,涂塑切断面已无修复功效。
我国已研发出环氧树脂涂塑复合钢管,采用内外均有涂塑保护层,中间为增强焊接钢管或无缝承压钢管的复合结构,克服了钢管本身存在的易生锈、腐蚀、高污染及塑料管强度低、易变形的缺陷,整合了钢管和塑料产品的共同优点。由于环氧涂料分子结构的特殊结构,使其具有环氧树脂具有优异的耐化学品性能,耐磨性好、耐热性好、粘结力强和优异的电绝缘性能,在防腐涂料、粘结剂、绝缘材料等各个领域有广泛的应用。尤其在涂料领域,环氧树脂每年产量的40%以上被应用于涂料。但是对于纯环氧树脂,尤其工业应用广泛的双酚A型环氧树脂来说,其粘度较大,固化成膜后存在耐湿热性能差、耐冲击性能差、耐候性能差和脆性大等缺点。
发明内容
本发明涉及一种耐蚀耐磨的涂塑钢管及其制造工艺,属于涂塑钢管技术领域。本发明提供的涂塑钢管,采用氟化石墨烯和磷酸锆预复合,再与TiO2通过硅烷偶联剂复合,加入用环氧树脂补强的氟碳树脂中,制得一种具有高交联密度的涂塑层涂料用于涂塑钢管,有效提升了涂塑钢管的耐腐蚀性和耐磨性,其内部大分子交联网络,增加了涂层内部的稳定性以及致密性,分散体与基体有良好的相容性,延长了腐蚀介质的侵蚀路径,进而提升了涂层防腐性能,发挥保护金属基体的作用,使涂层具有优异的机械性能和耐化学品性。
本发明的目的可以通过以下技术方案实现:
一种耐蚀耐磨的涂塑钢管的制造工艺,其特征在于:所述制造工艺包括以下步骤:
(1)分别将氟化石墨烯、盐酸多巴胺、磷酸锆溶解在Tris缓冲溶液中,搅拌24h制得混合液,经离心、洗涤,直至上清液pH值为6.5-7.5,取下层沉淀冷干,得到预复合材料;
(2)量取预复合材料、去离子水和乙醇,超声分散10-15min形成溶液A;将钛酸四丁酯溶解在乙醇中,分散均匀形成溶液B;边搅拌边将溶液B滴加到溶液A中,控制10min内添加完毕,室温下继续搅拌12-14h,静置陈化12-18h,离心并水洗醇洗各2-4次,70-80℃真空干燥6h得到TiO2复合粉体;
(3)将无水乙醇、硅烷偶联剂KH-560和去离子水配成均匀溶液,将TiO2复合粉体加入到溶液中,超声分散30-50min,一边搅拌一边在70-80℃反应8-9h,离心并水洗醇洗各2-4次,80℃真空干燥12-14h得到复合材料;
(4)将环氧树脂在二甲苯中与氟碳树脂超声、搅拌处理,得到0.5g/mL的混合溶液;
(5)将(3)制得的复合材料用二甲苯洗涤,然后均匀分散在二甲苯溶液中形成分散液,将分散液加入(4)制得的混合溶液中搅拌0.5-1h,得到组分A;
(6)将检验合格的钢管在喷砂除锈车间进行表面清理、除锈,用干燥的压缩空气对其进行清扫至表面无异物;通过中频加热方式对管件进行整体加热,将组分A与固化剂异氰酸酯混合均匀,涂覆在钢管内、外壁上,冷却固化,制得耐蚀耐磨的涂塑钢管。
其中,氟化石墨烯通过以下操作制得:称取氟化石墨,将其溶解在含有稳定剂聚乙烯吡咯烷酮的乙醇溶液中,进行超声分散10min,聚乙烯吡咯烷酮溶液浓度为10mg/mL;将配置好的0.8mg/mL的氟化石墨溶液进行高速机械剪切搅拌,转速为1200r/min连续搅拌10h,将溶液进行5000r/min离心处理10min,取上清液,抽滤洗去过量聚乙烯吡咯烷酮,之后将其放入真空干燥箱中60°干燥12h,得到氟化石墨烯。
作为本发明的一种优选方案,(1)中所述Tris缓冲溶液为pH=8.5,浓度为10mM的溶液。
作为本发明的一种优选方案,(1)中所述氟化石墨烯、盐酸多巴胺、磷酸锆在溶液中的浓度均为2mg/mL。
作为本发明的一种优选方案,(2)中所述预复合材料、去离子水和乙醇的用量比为1g:8-10mL:200-250mL。
作为本发明的一种优选方案,(2)中所述钛酸四丁酯和乙醇的体积比为0.8-1mL:2400-2500L。
作为本发明的一种优选方案,(3)中所述无水乙醇、硅烷偶联剂KH-560、去离子水和TiO2复合粉体的质量比为:3-4g:1g:0.4-0.5g:0.03-0.05g。
作为本发明的一种优选方案,(4)中所述环氧树脂和氟碳树脂的质量比为1:10-10.5。
作为本发明的一种优选方案,(5)中所述分散液的浓度为0.003-0.005g/mL。
作为本发明的一种优选方案,(6)中所述分散液、混合溶液与固化剂的用量比为2-3mL:10-12g:1g。
上述耐蚀耐磨的涂塑钢管的制造工艺制备得到的涂塑钢管。
本发明的有益效果:
1.本发明提供一种耐蚀耐磨的涂塑钢管,采用氟化石墨烯和磷酸锆预复合,再与TiO2通过硅烷偶联剂复合,加入用环氧树脂补强的氟碳树脂中,制得一种具有高交联密度,高耐磨性的涂塑层涂料用于涂塑钢管,有效提升了涂塑钢管的耐腐蚀性和耐磨性。
2.本发明中使用氟碳树脂作为基体,氟碳树脂有各种突出特性,包括耐化学品性、低介电常数和常温环境中可固化性等优点,本发明用将环氧树脂作为氟碳树脂的增强体,在涂层中引入含有大量的羟基或羧基等活性基团,加之在固化过程中活泼的环氧基能与界面金属原子反应形成牢固的化学键,保证了涂层与基材的优异附着力、低收缩率;并且其中的存在的羟基等活性基团,与氟碳树脂发生氢键反应,形成大分子交联网络,增加了涂层内部的稳定性以及致密性,延长了腐蚀介质的侵蚀路径,进而提升了涂层防腐性能,发挥保护金属基体的作用,使涂层具有优异的机械性能和耐化学品性。
3.本发明中氟化石墨烯纳米片增强了涂塑层的耐腐蚀性,这是由于氟化石墨烯纳米片具有的阻隔性能,在基体中分散均匀,可以为复合涂层提供一条曲折的路径,防止水、电解质和氧气穿透涂层表面,从而使纳米复合涂层的接触角增大,并且氟化石墨烯纳米片层自身具有优异阻隔作用,C-F键在石墨烯表层形成钝化层具有疏离腐蚀介质的特点,而适量氟化石墨烯在氟碳/环氧涂层中分散良好并与基体形成相容界面结构,这进一步可充分发挥氟化石墨烯纳米片的物理屏障防腐作用。
4.本发明中通过聚多巴胺的交联和粘附作用,将层状磷酸锆组装到氟化石墨烯表面,使得涂塑层有优异的耐磨性。因为磷酸锆组合的氟化石墨烯和与氟碳/环氧树脂基体具有相同的C-F键,因此具有良好的相容性,可以增强界面相互作用抑制涂层的变形和开裂,发挥异质二维层状纳米结构的协同作用,提升了涂塑层的减摩耐磨性能。同时引入片状结构能提供一个额外的屏障来防止电解液的渗透,从而有效地防止腐蚀介质对底层金属的攻击,此外,将层状磷酸锆组装到氟化石墨烯表面并加入氟碳/环氧树脂基体增强了氟化石墨烯在氟碳涂层中的分散性,使得涂塑层更致密,分布均匀,能有效发挥片层协同阻隔作用,进而提升涂层的防腐性能。
5.本发明中经过盐酸多巴胺包覆后的氟化石墨烯表面具有-NH2,可以与环氧树脂反应,增强与环氧树脂的界面相互作用力,同时经过后续硅烷偶联剂KH560对粉体的修饰使其具有环氧官能团,增强了粉体与氟碳/环氧树脂体系的相容性,能够参与到整个涂塑层层固化成膜过程,形成均匀分布的有机无机互相交联的高致密度涂层。
具体实施方式
下面将结合本发明实施例,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它实施例,都属于本发明保护的范围。
实施例1
一种耐蚀耐磨的涂塑钢管,通过以下制造工艺制得:
(1)分别将氟化石墨烯、盐酸多巴胺、磷酸锆溶解在pH=8.5,浓度为10mM的Tris缓冲溶液中,其中氟化石墨烯、盐酸多巴胺、磷酸锆在溶液中的浓度均为2mg/mL,之后进行搅拌24h,制备好的溶液经离心、洗涤,直至上清液pH值为中性,取下层沉淀,进行冷干,得到预复合材料;
其中,氟化石墨烯通过以下操作制得:称取氟化石墨,将其溶解在含有稳定剂聚乙烯吡咯烷酮的乙醇溶液中,进行超声分散10min,聚乙烯吡咯烷酮溶液浓度为10mg/mL;将配置好的0.8mg/mL的氟化石墨溶液进行高速机械剪切搅拌,转速为1200r/min连续搅拌10h,将溶液进行5000r/min离心处理10min,取上清液,抽滤洗去过量聚乙烯吡咯烷酮,之后将其放入真空干燥箱中60°干燥12h,得到氟化石墨烯;
(2)在烧杯中准确称取预复合材料、去离子水和乙醇,其用量比为1g:8mL:200mL,超声分散10min形成均匀溶液A;在玻璃杯中,将钛酸四丁酯溶解在乙醇中,分散均匀形成均匀溶液B,钛酸四丁酯和乙醇的体积比为0.8mL:2400L,并将其转移至分液漏斗中;在磁力搅拌条件下,将溶液B缓慢滴加到溶液A中,10min滴加完毕,室温下继续搅拌12h促进水解,静置陈化12h,离心并水洗醇洗各2次,70℃真空干燥箱中干燥6h得到TiO2复合粉体;
(3)在四口烧瓶中加入无水乙醇,硅烷偶联剂KH-560和去离子水形成均匀溶液;将TiO2复合粉体加入到四口烧瓶中,超声分散30min,将四口烧瓶转移至油浴锅中,磁力搅拌,70℃反应8h,离心并水洗醇洗各2次,80℃真空干燥箱中干燥12h得到复合材料,其中,无水乙醇、硅烷偶联剂KH-560、去离子水和TiO2复合粉体的质量比为:3g:1g:0.4g:0.03g;
(4)将环氧树脂在二甲苯中与氟碳树脂超声、搅拌处理,得到0.5g/mL的混合溶液,其中环氧树脂和氟碳树脂的质量比为1:10.5;
(5)将(3)制得的复合材料用二甲苯洗涤,然后均匀分散在二甲苯溶液中形成分散液,其浓度为0.003g/mL,将分散液加入(4)制得的混合溶液中搅拌0.5h分散均匀,得到组分A;
(6)将检验合格的钢管在喷砂除锈车间进行表面清理、除锈,用干燥的压缩空气对其进行清扫至表面无异物;通过中频加热方式对管件进行整体加热,再在组分A中加入异氰酸酯固化剂,搅拌30min,分散液、混合溶液与固化剂的用量比为2mL:10g:1g,随后在-0.09MPa的真空烘箱中去除气泡,得到涂塑层涂料,涂覆在钢管内、外壁上,冷却固化,制得耐蚀耐磨的涂塑钢管。
实施例2
一种耐蚀耐磨的涂塑钢管,通过以下制造工艺制得:
(1)分别将氟化石墨烯、盐酸多巴胺、磷酸锆溶解在pH=8.5,浓度为10mM的Tris缓冲溶液中,其中氟化石墨烯、盐酸多巴胺、磷酸锆在溶液中的浓度均为2mg/mL,之后进行搅拌24h,制备好的溶液经离心、洗涤,直至上清液pH值为中性,取下层沉淀,进行冷干,得到预复合材料;
其中,氟化石墨烯通过以下操作制得:称取氟化石墨,将其溶解在含有稳定剂聚乙烯吡咯烷酮的乙醇溶液中,进行超声分散10min,聚乙烯吡咯烷酮溶液浓度为10mg/mL;将配置好的0.8mg/mL的氟化石墨溶液进行高速机械剪切搅拌,转速为1200r/min连续搅拌10h,将溶液进行5000r/min离心处理10min,取上清液,抽滤洗去过量聚乙烯吡咯烷酮,之后将其放入真空干燥箱中60°干燥12h,得到氟化石墨烯;
(2)在烧杯中准确称取预复合材料、去离子水和乙醇,其用量比为1g:9mL:225mL,超声分散12min形成均匀溶液A;在玻璃杯中,将钛酸四丁酯溶解在乙醇中,分散均匀形成均匀溶液B,钛酸四丁酯和乙醇的体积比为0.9mL:2450L,并将其转移至分液漏斗中;在磁力搅拌条件下,将溶液B缓慢滴加到溶液A中,10min滴加完毕,室温下继续搅拌13h促进水解,静置陈化15h,离心并水洗醇洗各3次,75℃真空干燥箱中干燥6h得到TiO2复合粉体;
(3)在四口烧瓶中加入无水乙醇,硅烷偶联剂KH-560和去离子水形成均匀溶液;将TiO2复合粉体加入到四口烧瓶中,超声分散40min,将四口烧瓶转移至油浴锅中,磁力搅拌,75℃反应8.5h,离心并水洗醇洗各3次,80℃真空干燥箱中干燥13h得到复合材料,其中,无水乙醇、硅烷偶联剂KH-560、去离子水和TiO2复合粉体的质量比为:3.5g:1g:0.45g:0.04g;
(4)将环氧树脂在二甲苯中与氟碳树脂超声、搅拌处理,得到0.5g/mL的混合溶液,其中环氧树脂和氟碳树脂的质量比为1:10.3;
(5)将(3)制得的复合材料用二甲苯洗涤,然后均匀分散在二甲苯溶液中形成分散液,其浓度为0.004g/mL,将分散液加入(4)制得的混合溶液中搅拌45min分散均匀,得到组分A;
(6)将检验合格的钢管在喷砂除锈车间进行表面清理、除锈,用干燥的压缩空气对其进行清扫至表面无异物;通过中频加热方式对管件进行整体加热,再在组分A中加入异氰酸酯固化剂,搅拌30min,分散液、混合溶液与固化剂的用量比为2.5mL:11g:1g,随后在-0.09MPa的真空烘箱中去除气泡,得到涂塑层涂料,涂覆在钢管内、外壁上,冷却固化,制得耐蚀耐磨的涂塑钢管。
实施例3
一种耐蚀耐磨的涂塑钢管,通过以下制造工艺制得:
(1)分别将氟化石墨烯、盐酸多巴胺、磷酸锆溶解在pH=8.5,浓度为10mM的Tris缓冲溶液中,其中氟化石墨烯、盐酸多巴胺、磷酸锆在溶液中的浓度均为2mg/mL,之后进行搅拌24h,制备好的溶液经离心、洗涤,直至上清液pH值为中性,取下层沉淀,进行冷干,得到预复合材料;
其中,氟化石墨烯通过以下操作制得:称取氟化石墨,将其溶解在含有稳定剂聚乙烯吡咯烷酮的乙醇溶液中,进行超声分散10min,聚乙烯吡咯烷酮溶液浓度为10mg/mL;将配置好的0.8mg/mL的氟化石墨溶液进行高速机械剪切搅拌,转速为1200r/min连续搅拌10h,将溶液进行5000r/min离心处理10min,取上清液,抽滤洗去过量聚乙烯吡咯烷酮,之后将其放入真空干燥箱中60°干燥12h,得到氟化石墨烯;
(2)在烧杯中准确称取预复合材料、去离子水和乙醇,其用量比为1g:10mL:250mL,超声分散15min形成均匀溶液A;在玻璃杯中,将钛酸四丁酯溶解在乙醇中,分散均匀形成均匀溶液B,钛酸四丁酯和乙醇的体积比为1mL:2500L,并将其转移至分液漏斗中;在磁力搅拌条件下,将溶液B缓慢滴加到溶液A中,10min滴加完毕,室温下继续搅拌14h促进水解,静置陈化18h,离心并水洗醇洗各4次,80℃真空干燥箱中干燥6h得到TiO2复合粉体;
(3)在四口烧瓶中加入无水乙醇,硅烷偶联剂KH-560和去离子水形成均匀溶液;将TiO2复合粉体加入到四口烧瓶中,超声分散50min,将四口烧瓶转移至油浴锅中,磁力搅拌,80℃反应9h,离心并水洗醇洗各4次,80℃真空干燥箱中干燥14h得到复合材料,其中,无水乙醇、硅烷偶联剂KH-560、去离子水和TiO2复合粉体的质量比为:4g:1g:0.5g:0.05g;
(4)将环氧树脂在二甲苯中与氟碳树脂超声、搅拌处理,得到0.5g/mL的混合溶液,其中环氧树脂和氟碳树脂的质量比为1:10;
(5)将(3)制得的复合材料用二甲苯洗涤,然后均匀分散在二甲苯溶液中形成分散液,其浓度为0.005g/mL,将分散液加入(4)制得的混合溶液中搅拌1h分散均匀,得到组分A;
(6)将检验合格的钢管在喷砂除锈车间进行表面清理、除锈,用干燥的压缩空气对其进行清扫至表面无异物;通过中频加热方式对管件进行整体加热,再在组分A中加入异氰酸酯固化剂,搅拌30min,分散液、混合溶液与固化剂的用量比为3mL:12g:1g,随后在-0.09MPa的真空烘箱中去除气泡,得到涂塑层涂料,涂覆在钢管内、外壁上,冷却固化,制得耐蚀耐磨的涂塑钢管。
对比例1
一种耐蚀耐磨的涂塑钢管,与实施例3相比,不添加氟碳树脂,通过以下制造工艺制得:
(1)分别将氟化石墨烯、盐酸多巴胺、磷酸锆溶解在pH=8.5,浓度为10mM的Tris缓冲溶液中,其中氟化石墨烯、盐酸多巴胺、磷酸锆在溶液中的浓度均为2mg/mL,之后进行搅拌24h,制备好的溶液经离心、洗涤,直至上清液pH值为中性,取下层沉淀,进行冷干,得到预复合材料;
(2)在烧杯中准确称取预复合材料、去离子水和乙醇,其用量比为1g:10mL:250mL,超声分散15min形成均匀溶液A;在玻璃杯中,将钛酸四丁酯溶解在乙醇中,分散均匀形成均匀溶液B,钛酸四丁酯和乙醇的体积比为1mL:2500L,并将其转移至分液漏斗中;在磁力搅拌条件下,将溶液B缓慢滴加到溶液A中,10min滴加完毕,室温下继续搅拌14h促进水解,静置陈化18h,离心并水洗醇洗各4次,80℃真空干燥箱中干燥6h得到TiO2复合粉体;
(3)在四口烧瓶中加入无水乙醇,硅烷偶联剂KH-560和去离子水形成均匀溶液;将TiO2复合粉体加入到四口烧瓶中,超声分散50min,将四口烧瓶转移至油浴锅中,磁力搅拌,80℃反应9h,离心并水洗醇洗各4次,80℃真空干燥箱中干燥14h得到复合材料,其中,无水乙醇、硅烷偶联剂KH-560、去离子水和TiO2复合粉体的质量比为:4g:1g:0.5g:0.05g;
(4)将环氧树脂在二甲苯中超声、搅拌处理,得到0.5g/mL的混合溶液;
其余步骤与实施例3相同。
对比例2
一种耐蚀耐磨的涂塑钢管,与实施例3相比,不添加环氧树脂,通过以下制造工艺制得:
(1)分别将氟化石墨烯、盐酸多巴胺、磷酸锆溶解在pH=8.5,浓度为10mM的Tris缓冲溶液中,其中氟化石墨烯、盐酸多巴胺、磷酸锆在溶液中的浓度均为2mg/mL,之后进行搅拌24h,制备好的溶液经离心、洗涤,直至上清液pH值为中性,取下层沉淀,进行冷干,得到预复合材料;
(2)在烧杯中准确称取预复合材料、去离子水和乙醇,其用量比为1g:10mL:250mL,超声分散15min形成均匀溶液A;在玻璃杯中,将钛酸四丁酯溶解在乙醇中,分散均匀形成均匀溶液B,钛酸四丁酯和乙醇的体积比为1mL:2500L,并将其转移至分液漏斗中;在磁力搅拌条件下,将溶液B缓慢滴加到溶液A中,10min滴加完毕,室温下继续搅拌14h促进水解,静置陈化18h,离心并水洗醇洗各4次,80℃真空干燥箱中干燥6h得到TiO2复合粉体;
(3)在四口烧瓶中加入无水乙醇,硅烷偶联剂KH-560和去离子水形成均匀溶液;将TiO2复合粉体加入到四口烧瓶中,超声分散50min,将四口烧瓶转移至油浴锅中,磁力搅拌,80℃反应9h,离心并水洗醇洗各4次,80℃真空干燥箱中干燥14h得到复合材料,其中,无水乙醇、硅烷偶联剂KH-560、去离子水和TiO2复合粉体的质量比为:4g:1g:0.5g:0.05g;
(4)将氟碳树脂在二甲苯中超声、搅拌处理,得到0.5g/mL的混合溶液;
其余步骤与实施例3相同。
对比例3
一种耐蚀耐磨的涂塑钢管,与实施例3相比,不添加磷酸锆,通过以下制造工艺制得:
(1)分别将氟化石墨烯、盐酸多巴胺溶解在pH=8.5,浓度为10mM的Tris缓冲溶液中,其中氟化石墨烯、盐酸多巴胺在溶液中的浓度均为2mg/mL,之后进行搅拌24h,制备好的溶液经离心、洗涤,直至上清液pH值为中性,取下层沉淀,进行冷干,得到预复合材料;
其中,氟化石墨烯通过以下操作制得:称取氟化石墨,将其溶解在含有稳定剂聚乙烯吡咯烷酮的乙醇溶液中,进行超声分散10min,聚乙烯吡咯烷酮溶液浓度为10mg/mL;将配置好的0.8mg/mL的氟化石墨溶液进行高速机械剪切搅拌,转速为1200r/min连续搅拌10h,将溶液进行5000r/min离心处理10min,取上清液,抽滤洗去过量聚乙烯吡咯烷酮,之后将其放入真空干燥箱中60°干燥12h,得到氟化石墨烯;
(2)在烧杯中准确称取预复合材料、去离子水和乙醇,其用量比为1g:10mL:250mL,超声分散15min形成均匀溶液A;在玻璃杯中,将钛酸四丁酯溶解在乙醇中,分散均匀形成均匀溶液B,钛酸四丁酯和乙醇的体积比为1mL:2500L,并将其转移至分液漏斗中;在磁力搅拌条件下,将溶液B缓慢滴加到溶液A中,10min滴加完毕,室温下继续搅拌14h促进水解,静置陈化18h,离心并水洗醇洗各4次,80℃真空干燥箱中干燥6h得到TiO2复合粉体;
(3)在四口烧瓶中加入无水乙醇,硅烷偶联剂KH-560和去离子水形成均匀溶液;将TiO2复合粉体加入到四口烧瓶中,超声分散50min,将四口烧瓶转移至油浴锅中,磁力搅拌,80℃反应9h,离心并水洗醇洗各4次,80℃真空干燥箱中干燥14h得到复合材料,其中,无水乙醇、硅烷偶联剂KH-560、去离子水和TiO2复合粉体的质量比为:4g:1g:0.5g:0.05g;
(4)将环氧树脂在二甲苯中与氟碳树脂超声、搅拌处理,得到0.5g/mL的混合溶液,其中环氧树脂和氟碳树脂的质量比为1:10;
其余步骤与实施例3相同。
对比例4
一种耐蚀耐磨的涂塑钢管,与实施例3相比,不添加氟化石墨烯,通过以下制造工艺制得:
(1)分别将盐酸多巴胺、磷酸锆溶解在pH=8.5,浓度为10mM的Tris缓冲溶液中,其中盐酸多巴胺、磷酸锆在溶液中的浓度均为2mg/mL,之后进行搅拌24h,制备好的溶液经离心、洗涤,直至上清液pH值为中性,取下层沉淀,进行冷干,得到预复合材料;
(2)在烧杯中准确称取预复合材料、去离子水和乙醇,其用量比为1g:10mL:250mL,超声分散15min形成均匀溶液A;在玻璃杯中,将钛酸四丁酯溶解在乙醇中,分散均匀形成均匀溶液B,钛酸四丁酯和乙醇的体积比为1mL:2500L,并将其转移至分液漏斗中;在磁力搅拌条件下,将溶液B缓慢滴加到溶液A中,10min滴加完毕,室温下继续搅拌14h促进水解,静置陈化18h,离心并水洗醇洗各4次,80℃真空干燥箱中干燥6h得到TiO2复合粉体;
(3)在四口烧瓶中加入无水乙醇,硅烷偶联剂KH-560和去离子水形成均匀溶液;将TiO2复合粉体加入到四口烧瓶中,超声分散50min,将四口烧瓶转移至油浴锅中,磁力搅拌,80℃反应9h,离心并水洗醇洗各4次,80℃真空干燥箱中干燥14h得到复合材料,其中,无水乙醇、硅烷偶联剂KH-560、去离子水和TiO2复合粉体的质量比为:4g:1g:0.5g:0.05g;
(4)将环氧树脂在二甲苯中与氟碳树脂超声、搅拌处理,得到0.5g/mL的混合溶液,其中环氧树脂和氟碳树脂的质量比为1:10;
其余步骤与实施例3相同。
对比例5
一种耐蚀耐磨的涂塑钢管,与实施例3相比,不添加TiO2,通过以下制造工艺制得:
(1)分别将氟化石墨烯、盐酸多巴胺、磷酸锆溶解在pH=8.5,浓度为10mM的Tris缓冲溶液中,其中氟化石墨烯、盐酸多巴胺、磷酸锆在溶液中的浓度均为2mg/mL,之后进行搅拌24h,制备好的溶液经离心、洗涤,直至上清液pH值为中性,取下层沉淀,进行冷干,得到预复合材料;
(2)在四口烧瓶中加入无水乙醇,硅烷偶联剂KH-560和去离子水形成均匀溶液;将预复合材料加入到四口烧瓶中,超声分散50min,将四口烧瓶转移至油浴锅中,磁力搅拌,80℃反应9h,离心并水洗醇洗各4次,80℃真空干燥箱中干燥14h得到复合材料,其中,无水乙醇、硅烷偶联剂KH-560、去离子水和预复合材料的质量比为:4g:1g:0.5g:0.05g;
(4)将环氧树脂在二甲苯中与氟碳树脂超声、搅拌处理,得到0.5g/mL的混合溶液,其中环氧树脂和氟碳树脂的质量比为1:10;
其余步骤与实施例3相同。
对比例6
一种耐蚀耐磨的涂塑钢管,与实施例3相比,不添加硅烷偶联剂,通过以下制造工艺制得:
(1)分别将氟化石墨烯、盐酸多巴胺、磷酸锆溶解在pH=8.5,浓度为10mM的Tris缓冲溶液中,其中氟化石墨烯、盐酸多巴胺、磷酸锆在溶液中的浓度均为2mg/mL,之后进行搅拌24h,制备好的溶液经离心、洗涤,直至上清液pH值为中性,取下层沉淀,进行冷干,得到预复合材料;
其中,氟化石墨烯通过以下操作制得:称取氟化石墨,将其溶解在含有稳定剂聚乙烯吡咯烷酮的乙醇溶液中,进行超声分散10min,聚乙烯吡咯烷酮溶液浓度为10mg/mL;将配置好的0.8mg/mL的氟化石墨溶液进行高速机械剪切搅拌,转速为1200r/min连续搅拌10h,将溶液进行5000r/min离心处理10min,取上清液,抽滤洗去过量聚乙烯吡咯烷酮,之后将其放入真空干燥箱中60°干燥12h,得到氟化石墨烯;
(2)在烧杯中准确称取预复合材料、去离子水和乙醇,其用量比为1g:10mL:250mL,超声分散15min形成均匀溶液A;在玻璃杯中,将钛酸四丁酯溶解在乙醇中,分散均匀形成均匀溶液B,钛酸四丁酯和乙醇的体积比为1mL:2500L,并将其转移至分液漏斗中;在磁力搅拌条件下,将溶液B缓慢滴加到溶液A中,10min滴加完毕,室温下继续搅拌14h促进水解,静置陈化18h,离心并水洗醇洗各4次,80℃真空干燥箱中干燥6h得到TiO2复合粉体;
(3)在四口烧瓶中加入无水乙醇和去离子水形成均匀溶液;将TiO2复合粉体加入到四口烧瓶中,超声分散50min,将四口烧瓶转移至油浴锅中,磁力搅拌,80℃反应9h,离心并水洗醇洗各4次,80℃真空干燥箱中干燥14h得到复合材料,其中,无水乙醇、去离子水和TiO2复合粉体的质量比为:4g:1g:0.5g:0.05g;
(4)将环氧树脂在二甲苯中与氟碳树脂超声、搅拌处理,得到0.5g/mL的混合溶液,其中环氧树脂和氟碳树脂的质量比为1:10;
其余步骤与实施例3相同。
对实施例1-3和对比例1-6所制得的涂塑钢管进行如下测试:
1.按照SY/T0457-2010要求进行性能检测,所得结果见表1。
2.将涂塑钢管在盐水中浸泡1920h,测试其耐腐蚀性能,所得结果见表1。
3.使用CFT-I型材料表面综合性能测试仪对涂塑钢管的耐磨性进行测试。在试验中,采用球-盘式往复摩擦,摩擦球为直径4mm的GCr 15钢球,在垂直方向上加载3N的力,以300r/min的速度来回摩擦,运行时间30min。在测试前,使用丙酮清洗对偶面表面,并重复3次,保证结果测试的准确性,测得的摩擦系数见表1。
表1
由表1可得,本发明所有提供的涂塑钢管实施例1-3具有良好耐腐蚀性和耐磨性,而对比例1-6所得的涂塑钢管在耐腐蚀性和耐磨性有不同程度的下降。
在说明书的描述中,参考术语“一个实施例”、“示例”、“具体示例”等的描述意指结合该实施例或示例描述的具体特征、结构、材料或者特点包含于本发明的至少一个实施例或示例中。在本说明书中,对上述术语的示意性表述不一定指的是相同的实施例或示例。而且,描述的具体特征、结构、材料或者特点可以在任何的一个或多个实施例或示例中以合适的方式结合。
以上内容仅仅是对本发明所作的举例和说明,所属本技术领域的技术人员对所描述的具体实施例做各种各样的修改或补充或采用类似的方式替代,只要不偏离发明或者超越本权利要求书所定义的范围,均应属于本发明的保护范围。
Claims (7)
1.一种耐蚀耐磨的涂塑钢管的制造工艺,其特征在于:所述制造工艺包括以下步骤:
(1)分别将氟化石墨烯、盐酸多巴胺、磷酸锆溶解在Tris缓冲溶液中,搅拌24h制得混合液,经离心、洗涤,直至上清液pH值为6.5-7.5,取下层沉淀冷干,得到预复合材料;
(2)量取预复合材料、去离子水和乙醇,超声分散10-15min形成溶液A;将钛酸四丁酯溶解在乙醇中,分散均匀形成溶液B;边搅拌边将溶液B滴加到溶液A中,控制10min内添加完毕,室温下继续搅拌12-14h,静置陈化12-18h,离心并水洗醇洗各2-4次,70-80℃真空干燥6h得到TiO2复合粉体;
(3)将无水乙醇、硅烷偶联剂KH-560和去离子水配成均匀溶液,将Ti O2复合粉体加入到溶液中,超声分散30-50min,一边搅拌一边在70-80℃反应8-9h,离心并水洗醇洗各2-4次,80℃真空干燥12-14h得到复合材料;
(4)将环氧树脂在二甲苯中与氟碳树脂超声、搅拌处理,得到0.5g/mL的混合溶液;
(5)将(3)制得的复合材料用二甲苯洗涤,然后均匀分散在二甲苯溶液中形成分散液,将分散液加入(4)制得的混合溶液中搅拌0.5-1h,得到组分A;
(6)将检验合格的钢管在喷砂除锈车间进行表面清理、除锈,用干燥的压缩空气对其进行清扫至表面无异物;通过中频加热方式对管件进行整体加热,将组分A与固化剂异氰酸酯混合均匀,涂覆在钢管内、外壁上,冷却固化,制得耐蚀耐磨的涂塑钢管;
(2)中所述预复合材料、去离子水和乙醇的用量比为1g:8-10mL:200-250mL;
(2)中所述钛酸四丁酯和乙醇的体积比为0.8-1mL:2400-2500L;
(3)中所述无水乙醇、硅烷偶联剂KH-560、去离子水和Ti O2复合粉体的质量比为:3-4g:1g:0.4-0.5g:0.03-0.05g。
2.根据权利要求1所述的一种耐蚀耐磨的涂塑钢管的制造工艺,其特征在于:(1)中所述Tri s缓冲溶液为pH=8.5,浓度为10mM的溶液。
3.根据权利要求1所述的一种耐蚀耐磨的涂塑钢管的制造工艺,其特征在于:(1)中所述氟化石墨烯、盐酸多巴胺、磷酸锆在溶液中的浓度均为2mg/mL。
4.根据权利要求1所述的一种耐蚀耐磨的涂塑钢管的制造工艺,其特征在于:(4)中所述环氧树脂和氟碳树脂的质量比为1:10-10.5。
5.根据权利要求1所述的一种耐蚀耐磨的涂塑钢管的制造工艺,其特征在于:(5)中所述分散液的浓度为0.003-0.005g/mL。
6.根据权利要求1所述的一种耐蚀耐磨的涂塑钢管的制造工艺,其特征在于:(6)中所述分散液、混合溶液与固化剂的用量比为2-3mL:10-12g:1g。
7.一种如权利要求1-6任一项所述的耐蚀耐磨的涂塑钢管的制造工艺制备得到的涂塑钢管。
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