CN116550577A - 耐海洋气候工程零件表面涂层的涂覆处理工艺 - Google Patents
耐海洋气候工程零件表面涂层的涂覆处理工艺 Download PDFInfo
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- CN116550577A CN116550577A CN202310398694.8A CN202310398694A CN116550577A CN 116550577 A CN116550577 A CN 116550577A CN 202310398694 A CN202310398694 A CN 202310398694A CN 116550577 A CN116550577 A CN 116550577A
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- coating
- substrate
- resistant engineering
- marine climate
- climate resistant
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Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
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- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
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- B05D1/36—Successively applying liquids or other fluent materials, e.g. without intermediate treatment
- B05D1/38—Successively applying liquids or other fluent materials, e.g. without intermediate treatment with intermediate treatment
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B05D3/02—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by baking
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
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- B05D3/02—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by baking
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- B05D3/0272—After-treatment with ovens
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
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- B05D3/102—Pretreatment of metallic substrates
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B05D7/50—Multilayers
- B05D7/52—Two layers
- B05D7/54—No clear coat specified
- B05D7/544—No clear coat specified the first layer is let to dry at least partially before applying the second layer
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D151/00—Coating compositions based on graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Coating compositions based on derivatives of such polymers
- C09D151/08—Coating compositions based on graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Coating compositions based on derivatives of such polymers grafted on to macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- C09D151/085—Coating compositions based on graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Coating compositions based on derivatives of such polymers grafted on to macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds on to polysiloxanes
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/08—Anti-corrosive paints
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/16—Antifouling paints; Underwater paints
- C09D5/1656—Antifouling paints; Underwater paints characterised by the film-forming substance
- C09D5/1662—Synthetic film-forming substance
- C09D5/1675—Polyorganosiloxane-containing compositions
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C18/00—Alloys based on zinc
- C22C18/04—Alloys based on zinc with aluminium as the next major constituent
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C21/00—Alloys based on aluminium
- C22C21/10—Alloys based on aluminium with zinc as the next major constituent
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C30/00—Alloys containing less than 50% by weight of each constituent
- C22C30/06—Alloys containing less than 50% by weight of each constituent containing zinc
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
- C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
- C23G1/02—Cleaning or pickling metallic material with solutions or molten salts with acid solutions
- C23G1/08—Iron or steel
- C23G1/086—Iron or steel solutions containing HF
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
- C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
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- C23G1/19—Iron or steel
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D2518/00—Other type of polymers
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Wood Science & Technology (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Paints Or Removers (AREA)
Abstract
本发明公开了耐海洋气候工程零件表面涂层的涂覆处理工艺,涉及零件表面处理技术领域,包括:(1)依次采用碱液、酸液对基材表面进行浸泡处理得到预处理的基材;(2)取预处理后的基材浸泡于活化液中浸泡得到表面活化处理的基材;(3)将表面活化处理的基材浸入涂覆液中浸泡,然后高温固化处理获得涂覆处理的基材;(4)用有机硅复合树脂喷涂于涂覆处理的基材表面;活化液中包括表面处理剂,由L‑精氨酸甲酯二盐酸盐与二乙醇胺通过化学键连接获得。本发明提供的涂覆处理工艺获得的表面涂层,与基体结合力好,耐蚀性高,稳定性强,能够适于各种尺寸零件的处理,且具有更佳的抗污染能力,完全适用于海洋等极端恶劣的环境。
Description
技术领域
本发明属于零件表面处理技术领域,具体涉及耐海洋气候工程零件表面涂层的涂覆处理工艺。
背景技术
近海和海洋中的工程装备所处环境大气多雨、高温、多盐雾和强风流,其服役条件按ISO9225环境评价标准一般>C5级,属于极端恶劣环境。裸露在外的零件将受到强烈的大气腐蚀、电化学腐蚀以及气流冲刷侵蚀的综合作用,各种钢结构的使用寿命远低于一般内陆户外环境。如在海洋气候条件下服役的风力发电设备由于机组的外部构件如机舱、引擎罩、塔架、叶片根部法兰垫片、连接螺栓、连接弹簧等直接裸露于极端的腐蚀大气中,采用常规的防护措施,往往仅数个月便产生严重的腐蚀,因此,提供耐久性>15年的风电外部构件表面处理新材料与新工艺,已成为风电产业发展的迫切需求。
现代表面工程技术的快速发展,为钢铁表面的腐蚀防护提供了多种解决方法,如电镀、化学镀、热喷涂、气相沉积等。目前针对金属零件的表面防护主要方法是表面改性和表面涂覆。例如CN112521783A公开了一种防污防腐海洋涂料,该发明是由聚合邻对甲基苯胺等化学物质和定质量比制成的混合物,可有效保护船体不受海水侵蚀影响,并且有效阻止海洋赘生生物附着CN113774373A公开了一种同步超声喷丸辅助制备无缺陷耐磨蚀涂层的方法,该发明是同时开启高速激光熔覆系统和超声喷丸辅助系统获得无缺陷的耐磨蚀涂层,涂层的晶粒明显细化且硬度提高。但目前对面向海洋运输的增材制造金属零件的表面防护方法鲜有报道。
发明内容
本发明的目的在于提供耐海洋气候工程零件表面涂层的涂覆处理工艺,该涂覆处理工艺获得的表面涂层,与基体结合力好,耐蚀性高,稳定性强,能够适于各种尺寸零件的处理,且具有更佳的抗污染能力,完全适用于海洋等极端恶劣的环境。
本发明为实现上述目的所采取的技术方案为:
一种耐海洋气候工程零件表面涂层的涂覆处理工艺,包括:
(1)依次采用碱液、酸液对基材表面进行浸泡处理得到预处理的基材;
(2)取预处理后的基材浸泡于活化液中浸泡得到表面活化处理的基材;
(3)将表面活化处理的基材浸入涂覆液中浸泡,然后高温固化处理获得涂覆处理的基材;
(4)用有机硅复合树脂喷涂于涂覆处理的基材表面;
上述活化液中包括表面处理剂;表面处理剂由L-精氨酸甲酯二盐酸盐与二乙醇胺通过化学键连接获得。
本发明采用活化液在浸镀前对零件进行表面活化处理,能够基本消除活化液对零件产生腐蚀的风险,之后镀覆保护涂层,能够有效提升涂层与基材之间的结合能力,改善涂层的稳定性,且表现出较强的抗损伤能力。其原因可能在于,在经预处理后的基材表面进行活化处理,可能形成更多的有色活化中心,便于形成与基材表面紧密结合的纳米空洞,增加表面粗糙度,进而有效改善涂层与基材之间的结合能力,增强涂层稳定性以及抗冲击性能。
于具体实施方式中,表面处理剂的制备方法,包括:取L-精氨酸甲酯二盐酸盐与二乙醇胺在催化剂异丙醇钠作用下通过化学反应制备获得表面处理剂。
需要说明的是,上述表面处理剂的制备方法,具体包括:
取L-精氨酸甲酯二盐酸盐、二乙醇胺混合,加入催化剂异丙醇钠,85~120℃、70~90mmHg条件下搅拌反应1~2h,之后加入盐酸减压蒸馏得到表面处理剂。
于具体实施方式中,L-精氨酸甲酯二盐酸盐、二乙醇胺的摩尔比为1:2~2.5;异丙醇钠与L-精氨酸甲酯二盐酸盐的摩尔比为0.06~0.08:1。
进一步的,上述耐海洋气候工程零件表面涂层的涂覆处理工艺,具体包括:
(1)预处理,将基材放置于碱液中浸泡10~15min,水洗;然后再置于酸液中浸泡2~5min,水洗,获得预处理后的基材;
(2)表面活化处理,取预处理后的基材浸泡于活化液中,50~60℃下浸泡30~50min后取出水洗得到表面活化处理的基材;
(3)涂覆处理,将表面活化处理的基材浸入涂覆液中,3~5min后取出,沥干去除多余液体;之后先置于75~85℃下预烘10~20min,然后置于烧结炉中于120~200℃下烘烤20~35min;之后冷却至室温后,重复上述涂覆处理进行二次涂覆处理获得涂覆处理的基材;
(4)钝化处理,采用有机硅复合树脂涂料进行封闭钝化处理即可,具体包括:取丙二醇甲醚醋酸酯稀释有机硅复合树脂,浓度为22~27wt%,然后喷涂至涂覆处理的基材表面,室温固化30~50s即可,厚度为3~6μm。
于具体实施方式中,碱液包括:氢氧化钠25~40g/L,碳酸钠10~15g/L,十二烷基硫酸钠3~5g/L,余量水。
于具体实施方式中,酸液包括:氢氟酸4~6%、盐酸94~96%。
于具体实施方式中,活化液包括:乙二醇650~800mL/L,醋酸100~200mL/L,丙酮酸15~30mL/L,表面处理剂20~30g/L,酸性氟化铵30~40g/L,硼酸30~50g/L,氯化镍15~25g/L,余量水。
于具体实施方式中,涂覆液包括:按重量份计,金属复合物35~50份,乙二醇10~22份,去离子水15~25份,硅酸钠4~8份,羟乙基纤维素0.5~2份,聚羧酸铵盐分散剂0.2~1.5份。
于具体实施方式中,金属复合物包括:Zn 36~45wt%,Si 1.5~3.5wt%,Ti 0.5~3wt%,Ni1~3wt%,CeO2 0.2~1.5wt%,余量Al。
本发明还公开了上述有机硅复合树脂的制备方法,包括:
S1:取八甲基环四硅氧烷在碱催化剂条件下聚合得到有机硅中间产物A;
S2:取丙烯酸丁酯、甲基丙烯酸甲酯、乙酸丁香酚酯、丙烯酸以及有机硅中间产物A混合,通过自由基聚合反应制备获得有机硅复合树脂。
进一步具体的,上述有机硅复合树脂的制备方法,步骤为:
S1:取八甲基环四硅氧烷加热至95~105℃,然后加入碱催化剂反应1~3h,接着加入环四硅氧烷继续反应1~3h,旋蒸除去未反应单体,得到有机硅中间产物A;
S2:取丙烯酸丁酯、甲基丙烯酸甲酯、乙酸丁香酚酯、丙烯酸以及有机硅中间产物A混合,加入甲苯和AIBN,混合均匀后加热至90~110℃,反应1~3h,冷却减压蒸馏,提纯获得有机硅复合树脂。
于具体实施方式中,碱催化剂的加入量为八甲基环四硅氧烷的0.1~0.2wt%;环四硅氧烷与八甲基环四硅氧烷的质量比为0.15~0.3:1。
于具体实施方式中,丙烯酸丁酯、甲基丙烯酸甲酯、乙酸丁香酚酯、丙烯酸的摩尔比为1:0.9~1.1:0.4~0.6:0.1~0.3;有机硅中间产物A与丙烯酸丁酯的质量比为0.6~0.7:1;甲苯与丙烯酸丁酯的质量比为1.2~1.4:1;AIBN的加入量为丙烯酸丁酯的1.5~3wt%。
更优选地,步骤S2中采用左旋香芹酮替代丙烯酸。本发明采用左旋香芹酮作为聚合单体之一,与其它组分复合制备有机硅复合树脂,作为钝化处理材料涂覆于涂层表面,能够有效改善涂层的耐腐蚀性能,增强涂层表面的抗生物污染能力,抗生物附着效果明显提升,并且有效增强涂层的稳定性,其抗损伤性能显著改善。其原因可能在于,在有机硅复合树脂结构中引入左旋香芹酮,可能通过改善有机硅聚合物链结构,进而改善树脂的性能,涂覆于涂层表面,可能通过进一步增强表面疏水性能以及弥补涂层表面缺陷,使得表面涂层拥有更佳的综合性能。
本发明的又一目的在于,公开了上述涂覆处理获得的耐海洋气候工程零件表面涂层。
本发明还公开了上述耐海洋气候工程零件表面涂层在增强耐海洋气候工程零件耐腐蚀性能和抗污染性能中的应用。
相比于现有技术,本发明具有如下有益效果:
本发明采用活化液在浸镀前对零件进行表面活化处理,之后镀覆保护涂层,能够有效提升涂层与基材之间的结合能力,改善涂层的稳定性,且表现出较强的抗损伤能力。同时,本发明采用左旋香芹酮作为聚合单体之一,与其它组分复合制备有机硅复合树脂,作为钝化处理材料涂覆于涂层表面,能够有效改善涂层的耐腐蚀性能,增强涂层表面的抗生物污染能力,抗生物附着效果明显提升,并且有效增强涂层的稳定性,其抗损伤性能显著改善。本发明提供的涂覆处理工艺,操作简便,涂层厚度可调整,与基体结合牢固,且涂层的耐蚀性好,适于各种尺寸零件的处理,并且可在海洋气候条件下赋予其充分耐腐蚀性能和抗冲刷侵蚀性能,完全适用于海洋等极端恶劣的环境。
因此,本发明提供了耐海洋气候工程零件表面涂层的涂覆处理工艺,该涂覆处理工艺获得的表面涂层,与基体结合力好,耐蚀性高,稳定性强,能够适于各种尺寸零件的处理,且具有更佳的抗污染能力,完全适用于海洋等极端恶劣的环境。
附图说明
图1为本发明实施例1和实施例4中有机硅复合树脂的红外测试结果。
具体实施方式
为使本发明实施例的目的、技术方案和优点更加清楚,下面将结合实施例对本发明的各实施方式进行详细的阐述。然而,本领域的普通技术人员可以理解,在本发明各实施方式中,为了使读者更好地理解本申请而提出了许多技术细节。但是,即使没有这些技术细节和基于以下各实施方式的种种变化和修改,也可以实现本申请所要求保护的技术方案。
实施例1:
耐海洋气候工程零件表面涂层的涂覆处理工艺:
(1)预处理,将基材(材质40CrNiMo)放置于碱液(氢氧化钠32g/L,碳酸钠13g/L,十二烷基硫酸钠4g/L,余量水)中浸泡13min,水洗;然后再置于酸液(氢氟酸5%、盐酸95%)中浸泡3min,水洗,获得预处理后的基材;
(2)表面活化处理,取预处理后的基材浸泡于活化液(乙二醇735mL/L,醋酸155mL/L,丙酮酸22mL/L,表面处理剂26g/L,酸性氟化铵34g/L,硼酸40g/L,氯化镍20g/L,余量水)中,58℃下浸泡40min后取出水洗得到表面活化处理的基材;
(3)涂覆处理,将表面活化处理的基材浸入涂覆液(按重量份计,金属复合物40份,乙二醇16份,去离子水20份,硅酸钠6份,羟乙基纤维素1.2份,聚羧酸铵盐分散剂1份;其中,金属复合物包括:Zn 41.5wt%,Si 2.2wt%,Ti 1.6wt%,Ni 2.1wt%,CeO2 1.1wt%,余量Al)中,4min后取出,沥干去除多余液体;之后先置于80℃下预烘15min,然后置于烧结炉中于180℃下烘烤30min;之后冷却至室温后,重复上述涂覆处理进行二次涂覆处理获得涂覆处理的基材;
(4)钝化处理,采用有机硅复合树脂涂料进行封闭钝化处理即可,具体包括:取丙二醇甲醚醋酸酯稀释有机硅复合树脂,浓度为25wt%,然后喷涂至涂覆处理的基材表面,室温固化35s即可,厚度为4.3μm。
表面处理剂的制备:
按照摩尔比为1:2.3的比例取L-精氨酸甲酯二盐酸盐、二乙醇胺混合,加入催化剂异丙醇钠(与L-精氨酸甲酯二盐酸盐的摩尔比为0.07:1),105℃、82mmHg条件下搅拌反应1.5h,之后加入盐酸减压蒸馏得到表面处理剂;1H NMR(400MHz,CDCl3):δ:3.64(t,4H,-CH2),3.40(t,4H,-CH2),3.33(t,2H,-CH2),3.21(t,1H,-CH),1.78、1.49(m,4H,-CH2)。
有机硅复合树脂的制备:
S1:取八甲基环四硅氧烷加热至100℃,然后加入碱催化剂(氢氧化钾,加入量为八甲基环四硅氧烷的0.14wt%)反应2h,接着加入环四硅氧烷(与八甲基环四硅氧烷的质量比为0.21:1)继续反应2h,旋蒸除去未反应单体,得到有机硅中间产物A;
S2:取丙烯酸丁酯、甲基丙烯酸甲酯、乙酸丁香酚酯、丙烯酸以及有机硅中间产物A混合,加入甲苯和AIBN,混合均匀后加热至105℃,反应2h,冷却减压蒸馏,提纯获得有机硅复合树脂(Mn为2.31×104g/mol,Mw为4.36×104g/mol)。具体的,丙烯酸丁酯、甲基丙烯酸甲酯、乙酸丁香酚酯、丙烯酸的摩尔比为1:1:0.5:0.2;有机硅中间产物A与丙烯酸丁酯的质量比为0.66:1;甲苯与丙烯酸丁酯的质量比为1.3:1;AIBN的加入量为丙烯酸丁酯的2wt%。
实施例2:
耐海洋气候工程零件表面涂层的涂覆处理工艺与实施例1的不同在于:
活化液包括:乙二醇674mL/L,醋酸125mL/L,丙酮酸16mL/L,表面处理剂27g/L,酸性氟化铵32g/L,硼酸33g/L,氯化镍16g/L。
涂覆液包括:按重量份计,金属复合物38份,乙二醇13份,去离子水16份,硅酸钠5份,羟乙基纤维素0.8份,聚羧酸铵盐分散剂0.5份。
金属复合物包括:Zn 37.8wt%,Si 1.6wt%,Ti 0.7wt%,Ni 1.4wt%,CeO20.4wt%,余量Al。
钝化处理过程中丙二醇甲醚醋酸酯稀释有机硅复合树脂的浓度为23wt%;厚度为3.4μm。
表面处理剂的制备与实施例1相同。
实施例3:
耐海洋气候工程零件表面涂层的涂覆处理工艺与实施例1的不同在于:
活化液包括:乙二醇780mL/L,醋酸118mL/L,丙酮酸28mL/L,表面处理剂34g/L,酸性氟化铵37g/L,硼酸46g/L,氯化镍22g/L。
涂覆液包括:按重量份计,金属复合物47份,乙二醇21份,去离子水23份,硅酸钠7份,羟乙基纤维素1.6份,聚羧酸铵盐分散剂1.3份。
金属复合物包括:Zn 43.4wt%,Si 3.1wt%,Ti 2.4wt%,Ni 2.6wt%,CeO21.1wt%,余量Al。
钝化处理过程中丙二醇甲醚醋酸酯稀释有机硅复合树脂的浓度为26wt%;厚度为5.2μm。
表面处理剂的制备与实施例1相同。
实施例4:
耐海洋气候工程零件表面涂层的涂覆处理工艺与实施例1的不同在于:有机硅复合树脂为本实施例制备的。
有机硅复合树脂的制备与实施例1的区别:步骤S2中采用等摩尔量的左旋香芹酮替代丙烯酸。
表面处理剂的制备与实施例1相同。
实施例5:
耐海洋气候工程零件表面涂层的涂覆处理工艺与实施例4的不同在于:活化液中不添加表面处理剂。
有机硅复合树脂的制备与实施例4相同。
实施例6:
耐海洋气候工程零件表面涂层的涂覆处理工艺与实施例1的不同在于:活化液中不添加表面处理剂。
试验例1:
红外表征
测试采用傅里叶变换红外光谱仪进行,测试方法为溴化钾压片法,测试范围4000~500cm-1。
对实施例1和实施例4中制备的有机硅复合树脂进行上述红外测试,结果如图1所示。从图中分析可知,相比于实施例1制备的有机硅复合树脂的红外测试结果,实施例4制备的有机硅复合树脂的红外光谱中,在1717cm-1附近出现酮羰基的特征吸收峰,表明实施例5中有机硅复合树脂成功制备。
试验例2:
结合力表征
测试参考GB1720规定的标准进行。
耐盐雾性能表征
测试采用浓度为5%的NaCl溶液,pH在6~7范围的盐雾试验箱进行,测试数天观察涂层腐蚀情况,记录涂层样品出现腐蚀现象的天数;试验温度为35±2℃。
对实施例1~6获得的表面涂层进行上述测试,结果如表1所示:
表1性能指标测试结果
样品 | 结合力 | 耐盐雾性能(d) |
实施例1 | 1级 | >19 |
实施例2 | 1级 | >18 |
实施例3 | 1级 | >20 |
实施例4 | 1级 | >30 |
实施例5 | 2级 | >28 |
实施例6 | 2级 | >18 |
从表1中的数据分析可知,实施例1制备的耐海洋气候工程零件表面涂层,与基材的结合力明显好于实施例6的,耐盐雾性能与实施例6的相当,表明采用L-精氨酸甲酯二盐酸盐、二乙醇胺制备获得表面处理剂,作为活化液组分应用于耐海洋气候工程零件表面处理工艺中,能够有效增强涂层与基材之间的结合能力。实施例4制备的耐海洋气候工程零件表面涂层,其耐盐雾性能明显好于实施例1的,且实施例5的效果好于实施例6的,表明采用左旋香芹酮作为聚合单体之一,与其它组分复配制备获得有机硅复合树脂,应用于耐海洋气候工程零件表面处理工艺中,能够有效增强工程零件表面的耐腐蚀性能。
抗菌性能测定
测试参照GBT 21866规定的标准进行,最后计算待测样品的抑菌率。
海洋生物附着情况探究
实验测试对象:海洋环境中典型硅藻舟形藻。
具体测试方法:取舟形藻置于(22±2)℃的恒温振荡培养箱中培养,以12h/12h(白天/黑夜)循环。取处于指数增长期的舟形藻作贴附实验,具体为:取浓度为5.5×106mL-1舟形藻海水悬浮液1mL淹没样品,然后置于(22±2)℃的恒温振荡培养箱中培养,以12h/12h(白天/黑夜)循环培养72h。之后取出样品,无菌人工海水冲洗,冲掉未附着上的舟形藻;之后采用人工海水配制的2.5%戊二醛在4℃条件下固定化处理4h,然后用扫描电镜观察统计舟形藻附着面积。
对实施例1~6获得的表面涂层进行上述测试,结果如表2所示:
表2抑菌性能测试结果
从表2中的数据分析可知,实施例1制备的耐海洋气候工程零件表面涂层,其对大肠杆菌以及金黄色葡萄球菌的抑菌率与实施例6的相当,而实施例5制备的耐海洋气候工程零件表面涂层,其对大肠杆菌以及金黄色葡萄球菌的抑菌率均明显好于实施例1的,且实施例5的效果好于实施例6的,表明采用左旋香芹酮作为聚合单体之一,与其它组分复配制备获得有机硅复合树脂,应用于耐海洋气候工程零件表面处理工艺中,能够有效增强工程零件表面的抗生物污染性能。
同时,实施例5制备的耐海洋气候工程零件表面涂层,其表面藻类微生物附着面积明显低于实施例1的,且实施例5的效果好于实施例6的,表明采用左旋香芹酮作为聚合单体之一,与其它组分复配制备获得有机硅复合树脂,应用于耐海洋气候工程零件表面处理工艺中,能够有效改善工程零件表面的抗生物附着性能。
防污稳定性探究
测试参考GB5370规定的方法进行挂板制备,并置于海域进行浅海挂板试验,评价涂层的防污表现。需要说明的是,测试过程中将制备挂板垂直浸没于距海平面2m的海水中,3个月后进行挂板观察检查,并采用全自动清洗机对板面进行清洗,压力5MPa,喷嘴距离样板表面20cm,冲洗表面的附着污损物,评价清洗后涂层表面状态。
对实施例1~6获得的表面涂层进行上述测试,结果如表3所示:
表3防污稳定性测试结果
样品 | 清洗后涂层表面状态 |
实施例1 | 较光洁 |
实施例2 | 较光洁 |
实施例3 | 较光洁 |
实施例4 | 光洁 |
实施例5 | 光洁 |
实施例6 | 涂层局部脱落 |
从表3中的数据分析可知,实施例1制备的耐海洋气候工程零件表面涂层清洗后,其表面状态明显好于实施例6的,表明采用L-精氨酸甲酯二盐酸盐、二乙醇胺制备获得表面处理剂,作为活化液组分应用于耐海洋气候工程零件表面处理工艺中,能够有效改善涂层的稳定性,表现出较强的抗损伤能力。实施例4制备的耐海洋气候工程零件表面涂层的效果明显好于实施例1的,且实施例5的效果好于实施例6的,表明采用左旋香芹酮作为聚合单体之一,与其它组分复配制备获得有机硅复合树脂,应用于耐海洋气候工程零件表面处理工艺中,能够有效增强工程零件表面涂层的稳定性,提升抗损伤性能。
上述实施例中的常规技术为本领域技术人员所知晓的现有技术,故在此不再详细赘述。
以上所述,仅为本发明的具体实施方式,但本发明的保护范围并不局限于此,任何熟悉本技术领域的技术人员在本发明揭露的技术范围内,可轻易想到变化或替换,都应涵盖在本发明的保护范围之内。因此,本发明的保护范围应以所述权利要求的保护范围为准。
Claims (8)
1.一种耐海洋气候工程零件表面涂层的涂覆处理工艺,包括:
(1)依次采用碱液、酸液对基材表面进行浸泡处理得到预处理的基材;
(2)取预处理后的基材浸泡于活化液中浸泡得到表面活化处理的基材;
(3)将表面活化处理的基材浸入涂覆液中浸泡,然后高温固化处理获得涂覆处理的基材;
(4)用有机硅复合树脂喷涂于涂覆处理的基材表面;
其特征在于,所述活化液中包括表面处理剂;所述表面处理剂由L-精氨酸甲酯二盐酸盐与二乙醇胺通过化学键连接获得。
2.根据权利要求1所述的耐海洋气候工程零件表面涂层的涂覆处理工艺,其特征在于,所述碱液包括:氢氧化钠25~40g/L,碳酸钠10~15g/L,十二烷基硫酸钠3~5g/L。
3.根据权利要求1所述的耐海洋气候工程零件表面涂层的涂覆处理工艺,其特征在于,所述酸液包括:氢氟酸4~6%、盐酸94~96%。
4.根据权利要求1所述的耐海洋气候工程零件表面涂层的涂覆处理工艺,其特征在于,所述活化液包括:乙二醇650~800mL/L,醋酸100~200mL/L,丙酮酸15~30mL/L,表面处理剂20~30g/L,酸性氟化铵30~40g/L,硼酸30~50g/L,氯化镍15~25g/L。
5.根据权利要求1所述的耐海洋气候工程零件表面涂层的涂覆处理工艺,其特征在于,所述涂覆液包括:按重量份计,金属复合物35~50份,乙二醇10~22份,去离子水15~25份,硅酸钠4~8份,羟乙基纤维素0.5~2份,聚羧酸铵盐分散剂0.2~1.5份。
6.根据权利要求5所述的耐海洋气候工程零件表面涂层的涂覆处理工艺,其特征在于,所述金属复合物包括:Zn 36~45wt%,Si 1.5~3.5wt%,Ti 0.5~3wt%,Ni1~3wt%,CeO2 0.2~1.5wt%,余量Al。
7.权利要求1所述的涂覆处理获得的耐海洋气候工程零件表面涂层。
8.权利要求7所述的耐海洋气候工程零件表面涂层在增强耐海洋气候工程零件耐腐蚀性能和抗污染性能中的应用。
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