CN112517355A - 一种换热管表面超双疏涂层及其制备工艺和在甲醇制烯烃装置中的应用 - Google Patents
一种换热管表面超双疏涂层及其制备工艺和在甲醇制烯烃装置中的应用 Download PDFInfo
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Abstract
本发明公开了一种换热管表面超双疏涂层及其制备方法和在甲醇制烯烃装置中的应用,属于甲醇制烯烃过程换热器除蜡技术领域。将含氟漆均匀喷涂于换热管的表面,形成的涂层能够增强其附着力,保证复合涂层粉末均匀附着于换热管的表面;在第二涂层制备过程中,将少量碳纳米管粉末均匀喷涂在涂层上,既可形成纳微结构增加双疏性,又可提高涂层的导热性能,加入聚苯胺可减弱电化学腐蚀,增加涂层的防腐时效性。喷涂两次涂层和梯度烘烤可增加涂层的耐高温、机械强度和附着力。本发明可以有效降低换热器管壁结蜡的速率,有效减缓管壁结蜡和堵塞问题以及后续设备的堵塞,进而显著降低换热器停车清洗的频率,从而能够有效提高甲醇制烯烃的生产效率。
Description
技术领域
本发明属于甲醇制烯烃过程换热器除蜡技术领域,涉及一种换热管表面超双疏涂层及其制备方法和在甲醇制烯烃装置中的应用。
背景技术
煤制烯烃作为新兴煤化工项目备受瞩目,其中甲醇制烯烃(MTO)是煤制烯烃最为核心的工艺过程。MTO煤制烯烃装置,是以粗甲醇或精甲醇为原料,通过MTO催化剂作用,反应生成低碳烯烃产品气,产品气在急冷水洗***中洗涤、冷却降温,脱除催化剂和水,再送至烯烃分离单元进行乙烯、丙烯、碳四等产品的提纯。MTO工艺在生成轻烯烃产品的同时副产56%的水,还有少部分油类物质,MTO装置水***存在结蜡主要体现在反应产物中的油类物质占产品气中总量的0.3%,由于其凝固点低,易在急冷水和水洗水中冷凝下来,冷凝下来的油蜡大部分为芳烃和长链烷烃,其中芳烃类物质占95%左右,并以三甲基苯、四甲基苯和五甲基苯为主。油类物质在水***温区凝固,碱洗塔***堵塞、附属废碱排放管线、黄油排放管线均堵塞,甚至无法正常排放,碱洗塔堵塞问题对产品气压缩机***的稳定运行带来极大影响,成为制约整个装置安全稳定长周期运行的最主要瓶颈问题之一,导致水洗塔、换热器、空冷器堵塞,水***换热效率下降,换热器淸洗频繁。甲醇制烯烃装置包括反应、再生***、急冷水洗和污水汽提***和余热回收***。其中,急冷水洗和污水汽提***普遍受催化剂和蜡状物的影响而经常堵塞冷换设备,在37℃左右特别容易在换热管内壁产生结蜡;合成气出口温度若提高,会影响水洗塔顶气体采出,从而会影响烯烃分离的压缩机;以E1205换热器为例,水洗塔上返塔线中的水洗水冷却器和水洗塔塔盘常被堵塞,特别容易在换热器壳程产生结蜡,堵塞冷换设备,需频繁定时清洗,四组换热器每周至少需要清洗一组换热器,不但影响生产的正常运行,还需增加人力劳动,浪费大量的清洗剂,从而会严重影响生产装置的长、满、优运行。
MTO结蜡问题是目前MTO工业装置普遍存在的问题。目前处理MTO结蜡的措施主要是注二甲苯等萃取剂进行洗涤,而二甲苯属于低毒化学品,这增加了装置的运行风险。因此,亟需发展一种新的处理措施解决MTO结蜡问题。
发明内容
本发明的目的在于克服上述现有技术中,甲醇制烯烃过程中换热器易结蜡而堵塞设备,需要频繁停车清蜡的缺点,提供一种换热管表面超双疏涂层及其制备方法和在甲醇制烯烃装置中的应用。
为了达到上述目的,本发明采用以下技术方案予以实现:
一种换热管表面超双疏涂层的制备工艺,包括如下步骤:
S1:将换热管置于0.3~1.0M NaOH溶液中浸泡洗涤3~4h,之后依次用酸液和清水冲洗换热管至表面为中性,冲洗完后依次进行干燥和喷砂处理;
S2:将含氟漆均匀喷涂在S1处理后的换热器表面,形成厚度为20~50μm的第一涂层;
S3:将乙烯-三氟氯乙烯共聚物、SiO2/ZnO复合粒子、聚苯胺和乙酸乙酯按照25g:5g:1g:750ml的投料比混合,进行溶解,超声搅拌1~3h,得到第二涂层混合溶液,将第二涂层混合溶液均匀喷涂在S2处理后的第一涂层上,再按照聚苯胺和碳纳米管的质量比为1:3喷涂一层碳纳米管,在换热管表面形成复合涂层;
S4:将S3处理后的具有复合涂层的换热管置于100~240℃下,梯度烘烤13~16h,冷却后得到具有超双疏涂层的换热管。
优选地,S1所述酸液为浓度为0.5mol/L的盐酸溶液。
优选地,S1所述的干燥是在氮气气氛中进行的;所述喷砂处理之后还包括对换热管表面进行粗糙化处理。
优选地,S2所述的喷涂是在0.5~0.7MPa下进行的静电喷涂;S3所述的喷涂是在3~8bar下进行的静电喷涂。
优选地,S4所述的烘烤过程具体为:首先将S3处理后的换热管置于100℃下烘烤7~8h,再依次置于140℃下烘烤1~2h、180℃下烘烤1~2h,220℃下烘烤1~2h,240℃下烘烤1~2h,之后置于室温下自然冷却。
优选地,S2所述的含氟漆是以乙烯-三氟氯乙烯共聚物为基础的树脂,含氟漆中的氟含量为25%~29%。
一种基于所述制备工艺得到的换热管表面超双疏涂层,所述超双疏涂层的结构为具有“高尔夫球”状的纳微结构;超双疏涂层对乙醇水溶液和浓硫酸的接触角分别为148°和141°。
优选地,所述超双疏涂层的总厚度为50~100μm。
一种超双疏涂层在甲醇制烯烃装置中的应用,所述甲醇制烯烃装置中包括换热器,超双疏涂层喷涂于换热器的内外表面,换热器底部设有用于收集催化剂和油类物质的过滤收集槽。
优选地,所述换热器包括管程和壳程,壳程中流通的为水洗水,壳程入口的温度为50~60℃,壳程出口的温度为35~43℃左右;管程中流通的为工艺循环水,管程入口的温度为20~28℃,管程出口的温度为27~32℃。
与现有技术相比,本发明具有以下有益效果:
本发明公开了一种换热管表面超双疏涂层的制备方法,首先用碱液清洗换热管表面,以清除换热管表面的杂质,之后利用酸液中和掉换热管表面的酸液,并用清水冲洗,干燥后进行喷砂处理,能够进一步去除换热管表面的杂质,将含氟漆均匀喷涂于换热管的表面,形成20-50μm厚的涂层,能够增强其附着力,同时,保证复合涂层粉末可以均匀附着于换热管的表面;在该第二涂层制备过程中,将少量碳纳米管粉末均匀喷涂在涂层上,既可形成纳微结构增加双疏性,又可提高涂层的导热性能,加入聚苯胺可减弱电化学腐蚀,增加涂层的防腐时效性。第一次喷涂底漆的是为了提高涂层的附着力,第二次喷涂复合涂层提高涂层的双疏性和防腐性。
进一步地,在氮气气氛中干燥,能够防止换热管表面在干燥过程中又沾染新的灰尘杂质;喷砂处理后进行表面粗糙化处理,能够防止因换热管表面粗糙而对影响涂层的喷涂效果。
进一步地,采用静电喷涂,能够构筑粗糙表面增加双疏性。采用梯度烘烤,能够增加涂层的机械强度,减少涂层的脆性。
本发明还公开了一种换热管表面超双疏涂层,是基于上述制备工艺得到的,具有“高尔夫球”状的纳微结构,可以增强涂层的疏水疏油性,该涂层对乙醇水溶液和浓硫酸的接触角分别高达148°和141°;十字胶带测试,评估涂层的附着力,结果表明该涂层的附着力良好。即该超双疏涂层附着力好、机械强度高、耐高温,且具有一定的防腐蚀性。将该换热管表面超双疏涂层应用于甲醇制烯烃装置中,采用在换热管外和换热器壳体内壁喷涂超双疏涂层,与现有的注二甲苯等萃取剂进行洗涤的方法相比,该工艺方法不但无毒,而且可以有效降低换热器管壁结蜡的速率,有效减缓管壁结蜡和堵塞问题以及后续设备的堵塞,进而显著降低换热器停车清洗的频率,从而能够有效提高甲醇制烯烃的生产效率。
附图说明
图1为E1205水洗水冷却换热器流程图;
图2为水洗水合成气的组成图;
图3为本发明实施例1制备的超双疏涂层的形貌表征SEM图,其中(a)为放大10000倍的SEM图,(b)为放大30000倍的SEM图。
具体实施方式
为了使本技术领域的人员更好地理解本发明方案,下面将结合本发明实施例中的附图,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的实施例,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做出创造性劳动前提下所获得的所有其他实施例,都应当属于本发明保护的范围。
下面结合附图对本发明做进一步详细描述:
一种基于构筑疏水疏油自清洁表面涂层除蜡的高效管式换热器装置,如图1所示,包括换热器管程和换热器壳程,水洗塔,压缩机,水洗塔底泵;所述管式换热器壳程介质是水洗水,入口温度55℃左右,出口温度39℃左右;所述管式换热器管程介质是工艺循环水,入口温度24℃左右,出口温度30℃左右;MTO煤制烯烃装置,是以粗甲醇或精甲醇为原料,通过MTO催化剂作用,反应生成低碳烯烃产品气,产品气在急冷水洗***中洗涤、冷却降温,脱除催化剂和水;所述换热器换热管内管外壁涂有超双疏涂层,冷却过程中催化剂和蜡状物不容易附着在内管管壁,在换热器底部设置有过滤收集槽,将催化剂和油类物质收集起来,有效减缓管壁结蜡和堵塞问题以及后续设备的堵塞。水洗水换热器的主体材料为Q345R,压力在0.45-1.347Mpa,温度在30-70℃,反应气的组成如图2所示。
换热管表面需要做处理,采用性能好疏水疏油的涂层。涂层必须满足附着力好、机械强度高和耐高温,同时具有一定的防腐蚀性。
一种换热管表面超双疏涂层的制备工艺做了以下几种试验:
实施例1
(1)将换热管放入1mol/L的NaOH溶液中,浸洗3h,用0.5mol/L的盐酸溶液中和,用自来水冲洗5次,在氮气氛围干燥;
(2)将换热管外表面放置于高速喷砂机下,进行喷砂处理,去除表面杂质,同时将表面进行粗糙化处理;
(3)将含氟漆在0.5MPa下均匀喷涂于换热管外表面,形成20-50μm厚的涂层,增强其附着力,同时,保证复合涂层粉末可以均匀附着于换热管外表面;含氟漆中的氟含量为25%;
(4)将2g乙烯三氟氯乙烯共聚物加入到60ml的乙酸乙酯溶液中,超声搅拌20min,再加入0.4g SiO2/ZnO复合粒子和0.08g聚苯胺,超声搅拌1h,使混合液均匀分散,得到混合溶液。然后用喷枪以3bar的压力将混合溶液均匀的喷涂在有第一涂层(即底漆)的不锈钢换热管表面,采用静电喷涂仪将0.24g碳纳米管粉末均匀喷涂在涂层上
(5)将Q345R钢换热器换热管处于100℃下烘烤7h,140℃下烘烤1h,180℃下烘烤2h,220℃下烘烤2h,240℃下放置1h,梯度固化,自然冷却,得到厚度为50-100μm厚的超双疏涂层。
实施例2
(1)将换热管放入0.3mol/L的NaOH溶液中,浸洗4h,用0.5mol/L的盐酸溶液中和,用自来水冲洗4次,在氮气氛围干燥;
(2)将换热管外表面放置于高速喷砂机下,进行喷砂处理,去除表面杂质,同时将表面进行粗糙化处理;
(3)将含氟漆在0.7MPa下均匀喷涂于换热管外表面,形成20-50μm厚的涂层,增强其附着力,同时,保证复合涂层粉末可以均匀附着于换热管外表面;含氟漆中的氟含量为27%;
(4)将5g乙烯三氟氯乙烯共聚物加入到150ml的乙酸乙酯溶液中,超声搅拌20min,再加入1.0g SiO2/ZnO复合粒子和0.2g聚苯胺,超声搅拌3h,使混合液均匀分散,得到混合溶液。然后用喷枪以5bar的压力将混合溶液均匀的喷涂在有第一涂层(即底漆)的不锈钢管热管表面,采用静电喷涂仪将0.6g碳纳米管粉末均匀喷涂在涂层上
(5)将Q345R钢换热器换热管处于100℃下烘烤8h,140℃下烘烤2h,180℃下烘烤2h,220℃下烘烤1h,240℃下放置2h,梯度固化,自然冷却,得到厚度为50-100μm厚的超双疏涂层。
实施例3
(1)将换热管放入0.7mol/L的NaOH溶液中,浸洗3.5h,用0.5mol/L的盐酸溶液中和,用自来水冲洗3次,在氮气氛围干燥;
(2)将换热管外表面放置于高速喷砂机下,进行喷砂处理,去除表面杂质,同时将表面进行粗糙化处理;
(3)将含氟漆在0.6MPa下均匀喷涂于换热管外表面,形成20-50μm厚的涂层,增强其附着力,同时,保证复合涂层粉末可以均匀附着于换热管外表面;含氟漆中的氟含量为29%;
(4)将10g乙烯三氟氯乙烯共聚物加入到150ml的乙酸乙酯溶液中,超声搅拌30min,再加入2.0g SiO2/ZnO复合粒子和0.4g聚苯胺,超声搅拌2h,使混合液均匀分散,得到混合溶液。然后用喷枪以6bar的压力将混合溶液均匀的喷涂在有第一涂层(即底漆)的不锈钢换热管表面,采用静电喷涂仪将1.2g碳纳米管粉末均匀喷涂在涂层上
(5)将Q345R钢换热器换热管处于100℃下烘烤8h,140℃下烘烤2h,180℃下烘烤2h,220℃下烘烤2h,240℃下放置2h,梯度固化,自然冷却,得到厚度为50-100μm厚的超双疏涂层。
对实施例1制备的超双疏涂层进行性能测试:
利用扫描电镜分析超双疏涂层的表面形貌,结果如图(3)所示,表明低表面能涂层表面,具有“高尔夫球”状的纳微结构,可以增强涂层的疏水疏油性,该涂层对乙醇水溶液和浓硫酸的接触角分别高达148°和141°;
采用GB/T 9286对超双疏涂层进行十字胶带测试,评估涂层的附着力,用壁纸刀将超双疏涂层划成方格,直至暴露金属基底,然后用胶带按压样品2min后撕开,重复多次胶带表面均未有发现基底脱落,该超双疏涂层的附着力良好。
换热管表面采用超双疏涂层改进后,与原换热管的除蜡效果进行对比,涂镀超双疏涂层后,换热器由原来的一周清洗一次推迟到现在的两月清洗一次。显著节省了人力和清洗原料。
需要说明的是,本发明实施例中使用的换热器具为Q345R钢换热器,所述的含氟漆是以乙烯-三氟氯乙烯共聚物为基础的树脂。
以上内容仅为说明本发明的技术思想,不能以此限定本发明的保护范围,凡是按照本发明提出的技术思想,在技术方案基础上所做的任何改动,均落入本发明权利要求书的保护范围之内。
Claims (10)
1.一种换热管表面超双疏涂层的制备工艺,其特征在于,包括如下步骤:
S1:将换热管置于0.3~1.0M NaOH溶液中浸泡洗涤3~4h,之后依次用酸液和清水冲洗换热管至表面为中性,冲洗完后依次进行干燥和喷砂处理;
S2:将含氟漆均匀喷涂在S1处理后的换热器表面,形成厚度为20~50μm的第一涂层;
S3:将乙烯-三氟氯乙烯共聚物、SiO2/ZnO复合粒子、聚苯胺和乙酸乙酯按照25g:5g:1g:750ml的投料比混合,进行溶解,超声搅拌1~3h,得到第二涂层混合溶液,将第二涂层混合溶液均匀喷涂在S2处理后的第一涂层上,再按照聚苯胺和碳纳米管的质量比为1:3喷涂一层碳纳米管,在换热管表面形成复合涂层;
S4:将S3处理后的具有复合涂层的换热管置于100~240℃下,梯度烘烤13~16h,冷却后得到具有超双疏涂层的换热管。
2.根据权利要求1所述的换热管表面超双疏涂层的制备工艺,其特征在于,S1所述酸液为浓度为0.5mol/L的盐酸溶液。
3.根据权利要求1所述的换热管表面超双疏涂层的制备工艺,其特征在于,S1所述的干燥是在氮气气氛中进行的;所述喷砂处理之后还包括对换热管表面进行粗糙化处理。
4.根据权利要求1所述的换热管表面超双疏涂层的制备工艺,其特征在于,S2所述的喷涂是在0.5~0.7MPa下进行的静电喷涂;S3所述的喷涂是在3~8bar下进行的静电喷涂。
5.根据权利要求1所述的换热管表面超双疏涂层的制备工艺,其特征在于,S4所述的烘烤过程具体为:首先将S3处理后的换热管置于100℃下烘烤7~8h,再依次置于140℃下烘烤1~2h、180℃下烘烤1~2h,220℃下烘烤1~2h,240℃下烘烤1~2h,之后置于室温下自然冷却。
6.根据权利要求1所述的换热管表面超双疏涂层的制备工艺,其特征在于,S2所述的含氟漆是以乙烯-三氟氯乙烯共聚物为基础的树脂,含氟漆中的氟含量为25%~29%。
7.一种基于权利要求1~6任一项所述制备工艺得到的换热管表面超双疏涂层,其特征在于,所述超双疏涂层的结构为具有“高尔夫球”状的纳微结构;超双疏涂层对乙醇水溶液和浓硫酸的接触角分别为148°和141°。
8.根据权利要求7所述的换热管表面超双疏涂层,其特征在于,所述超双疏涂层的总厚度为50~100μm。
9.一种超双疏涂层在甲醇制烯烃装置中的应用,其特征在于,所述甲醇制烯烃装置中包括换热器,超双疏涂层喷涂于换热器的内外表面,换热器底部设有用于收集催化剂和油类物质的过滤收集槽。
10.根据权力要求9所述的应用,其特征在于,所述换热器包括管程和壳程,壳程中流通的为水洗水,壳程入口的温度为50~60℃,壳程出口的温度为35~43℃左右;管程中流通的为工艺循环水,管程入口的温度为20~28℃,管程出口的温度为27~32℃。
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