CN110819222A - 一种防腐抗静电机床涂料制备方法 - Google Patents

一种防腐抗静电机床涂料制备方法 Download PDF

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CN110819222A
CN110819222A CN201911155613.1A CN201911155613A CN110819222A CN 110819222 A CN110819222 A CN 110819222A CN 201911155613 A CN201911155613 A CN 201911155613A CN 110819222 A CN110819222 A CN 110819222A
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王保军
拾振洪
李海洋
金传亮
回留柱
王家振
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Anhui Xindalu Special Paint Co Ltd
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Abstract

本发明公开了一种防腐抗静电机床涂料制备方法,具体涉及机床涂料技术领域,通过本发明方法制备的涂料具有较好的抗静电性能,同时,其耐酸碱腐蚀性能优异,附着力强,硬度高,适用于机床的抗静电防腐保护;利用氯化铝溶液、烷基酚聚氧乙烯醚对氧化石墨烯进行处理,其中烷基酚聚氧乙烯醚作为模板,碱性水热条件下,在氧化石墨烯表面负载氧化铝,通过煅烧除去烷基酚聚氧乙烯醚模板后,形成细微孔道,此操作大大提高了氧化石墨烯的比表面积,并赋予其多孔性质,增强其导电性能和防腐性能。

Description

一种防腐抗静电机床涂料制备方法
技术领域
本发明属于机床涂料技术领域,尤其是一种防腐抗静电机床涂料制备方法。
背景技术
机床是指以各种切削加工方法或非切削加工方法来将金属或非金属的原材料通过使用合适的刀具加工为需要的形状或尺寸、或为了附加更精密的加工为目的而使用的机器。为了其精密性,通常需要对机床进行涂层防护处理。
专利CN 107760082 A公开了一种机床用耐高温涂料,使用寿命长,并且具有耐高温性能,然而,其耐腐蚀性能、抗静电性能欠佳。
发明内容
针对上述问题,本发明旨在提供一种。
本发明通过以下技术方案实现:
(1)将以重量份计的15-17份氧化石墨烯加入到其体积5-7倍的无水乙醇中,在40-43KHz下超声处理10-12min,然后向其中加入20-30份浓度为0.8-1.2mol/L的氯化铝溶液、3-5份烷基酚聚氧乙烯醚,继续超声20-30min后,在50-55℃下静置2-3h,然后向其中加入质量分数为30-35%的氨水溶液,调节pH为8-8.5,将体系转移至反应釜中,在160-165℃下反应15-18h,冷却,过滤,洗涤后,在50-60℃下干燥10-12h,然后置于530-550℃下焙烧3-4h,研磨,备用;
(2)将15-20份步骤(1)所得物加入到40-50份质量分数为34-36%的氨基酸溶液中,在50-60℃、200-300rpm下搅拌10-20min后,向其中加入15-18份质量分数为30-33%的硫酸锌溶液,然后利用饱和氨水溶液调节pH为8.2-8.4,继续搅拌反应40-60min,过滤,洗涤后烘干,得到氨基酸锌-氧化铝-氧化石墨烯复合物;氨基酸可以为赖氨酸;
(3)将15-20份步骤(2)所得物加入到40-45份丙酮中,搅拌10-20min后,加入15-20份固含量为32-35%的环氧树脂E44的丙酮溶液,然后在63-65℃,300-500rpm下反应3-5h,冷却,在1500-2000rpm下离心15-17min,抽滤,将所得物在84-86℃下干燥12-16h;
(4)将15-20份步骤(3)所得物加入到40-50份聚四氢呋喃醚二醇中,然后加入0.5-1份三乙醇胺,在400-500rpm搅拌下加热至102-103℃,反应40-50min,然后向其中加入30-40份异佛尔酮二异氰酸酯、30-45份聚四氢呋喃醚二醇、0.5-0.8份有机锡催化剂,在70-76℃、200-300rpm下反应2-3h,然后向其中加入200-300份去离子水,在2200-2300rpm下高速剪切分散40-50min后,加入5-6份乙二醇,继续搅拌20-30min即可。
本发明的有益效果:通过本发明方法制备的涂料具有较好的抗静电性能,同时,其耐酸碱腐蚀性能优异,附着力强,硬度高,适用于机床的抗静电防腐保护;利用氯化铝溶液、烷基酚聚氧乙烯醚对氧化石墨烯进行处理,其中烷基酚聚氧乙烯醚作为模板,碱性水热条件下,在氧化石墨烯表面负载氧化铝,通过煅烧除去烷基酚聚氧乙烯醚模板后,形成细微孔道,此操作大大提高了氧化石墨烯的比表面积,并赋予其多孔性质,增强其导电性能和防腐性能;氨基酸溶液和锌离子通过络合反应在其表面继续负载,生成氨基酸锌-氧化铝-氧化石墨烯复合物,不仅引入金属锌离子,同时,也达到了氨基、羧基等官能团的接枝目的,可以利用氨基、羧基与聚氨酯单体中的异氰酸酯基和羟基进行反应,从而增强其与聚氨酯基底的交联作用,形成互联网络结构,显著提升了涂层附着力和硬度,同时增强其抗静电性能。
具体实施方式
下面用具体实施例说明本发明,但并不是对本发明的限制。
实施例1
(1)将以重量份计的16份氧化石墨烯加入到其体积6倍的无水乙醇中,在42KHz下超声处理11min,然后向其中加入25份浓度为1.0mol/L的氯化铝溶液、4份烷基酚聚氧乙烯醚,继续超声25min后,在52℃下静置3h,然后向其中加入质量分数为33%的氨水溶液,调节pH为8.3,将体系转移至反应釜中,在163℃下反应17h,冷却,过滤,洗涤后,在55℃下干燥11h,然后置于543℃下焙烧4h,研磨,备用;
(2)将18份步骤(1)所得物加入到45份质量分数为35%的赖氨酸溶液中,在55℃、260rpm下搅拌15min后,向其中加入17份质量分数为32%的硫酸锌溶液,然后利用饱和氨水溶液调节pH为8.3,继续搅拌反应50min,过滤,洗涤后烘干,得到氨基酸锌-氧化铝-氧化石墨烯复合物;
(3)将18份步骤(2)所得物加入到43份丙酮中,搅拌15min后,加入18份固含量为34%的环氧树脂E44的丙酮溶液,然后在64℃,400rpm下反应4h,冷却,在1800rpm下离心16min,抽滤,将所得物在85℃下干燥15h;
(4)将17份步骤(3)所得物加入到45份聚四氢呋喃醚二醇中,然后加入0.8份三乙醇胺,在450rpm搅拌下加热至103℃,反应45min,然后向其中加入35份异佛尔酮二异氰酸酯、40份聚四氢呋喃醚二醇、0. 6份有机锡催化剂,在73℃、240rpm下反应3h,然后向其中加入240份去离子水,在2200rpm下高速剪切分散45min后,加入6份乙二醇,继续搅拌25min即可。
经测试,涂层在5 wt.% H2SO4 下无变化,5 wt.% Na OH下无变化、3 wt.% Na Cl下无变化;附着力0级,铅笔硬度4H,表面电阻率为1.5×104%。
实施例2
(1)将以重量份计的16份氧化石墨烯加入到其体积6倍的无水乙醇中,在42KHz下超声处理11min,然后向其中加入25份浓度为1.0mol/L的氯化铝溶液、4份烷基酚聚氧乙烯醚,继续超声25min后,在52℃下静置3h,然后向其中加入质量分数为33%的氨水溶液,调节pH为8.3,将体系转移至反应釜中,在163℃下反应17h,冷却,过滤,洗涤后,在55℃下干燥11h,然后置于543℃下焙烧4h,研磨,备用;
(2)将18份步骤(1)所得物加入到43份丙酮中,搅拌15min后,加入18份固含量为34%的环氧树脂E44的丙酮溶液,然后在64℃,400rpm下反应4h,冷却,在1800rpm下离心16min,抽滤,将所得物在85℃下干燥15h;
(3)将17份步骤(2)所得物加入到45份聚四氢呋喃醚二醇中,然后加入0.8份三乙醇胺,在450rpm搅拌下加热至103℃,反应45min,然后向其中加入35份异佛尔酮二异氰酸酯、40份聚四氢呋喃醚二醇、0. 6份有机锡催化剂,在73℃、240rpm下反应3h,然后向其中加入240份去离子水,在2200rpm下高速剪切分散45min后,加入6份乙二醇,继续搅拌25min即可。
经测试,涂层在5 wt.% H2SO4 下发白起泡,5 wt.% Na OH下涂层破裂、3 wt.% NaCl下无变化;附着力2级,铅笔硬度2H,表面电阻率为3.7×105%。
实施例3
(1)将以重量份计的16份氧化石墨烯加入到其体积6倍的无水乙醇中,在42KHz下超声处理11min,然后向其中加入25份浓度为1.0mol/L的氯化铝溶液、4份烷基酚聚氧乙烯醚,继续超声25min后,在52℃下静置3h,然后向其中加入质量分数为33%的氨水溶液,调节pH为8.3,将体系转移至反应釜中,在163℃下反应17h,冷却,过滤,洗涤后,在55℃下干燥11h,然后置于543℃下焙烧4h,研磨,备用;
(2)将18份步骤(1)所得物加入到45份质量分数为35%的赖氨酸溶液中,在55℃、260rpm下搅拌15min后,向其中加入17份质量分数为32%的硫酸锌溶液,然后利用饱和氨水溶液调节pH为8.3,继续搅拌反应50min,过滤,洗涤后烘干,得到氨基酸锌-氧化铝-氧化石墨烯复合物;
(3)将17份步骤(2)所得物加入到45份聚四氢呋喃醚二醇中,然后加入0.8份三乙醇胺,在450rpm搅拌下加热至103℃,反应45min,然后向其中加入35份异佛尔酮二异氰酸酯、40份聚四氢呋喃醚二醇、0. 6份有机锡催化剂,在73℃、240rpm下反应3h,然后向其中加入240份去离子水,在2200rpm下高速剪切分散45min后,加入6份乙二醇,继续搅拌25min即可。
经测试,涂层在5 wt.% H2SO4 下发白起泡,5 wt.% Na OH下发白起泡、3 wt.% NaCl下无变化;附着力3级,铅笔硬度2H,表面电阻率为1.3×105%。
性能测试:
耐介质性能:按照 GB 9274—1988《色漆和清漆耐液体介质的测定》测试涂层的耐酸、耐碱和耐盐水性能,腐蚀介质分别为 5 wt.% H2SO4 溶液、5 wt.% Na OH 溶液、3 wt.% NaCl 溶液。具体方法如下:将试样涂层一面朝上水平放置,滴加数滴腐蚀介质,相邻液体中心保持至少20 mm间隔。试样在(23±2℃)条件下放置24 h,使其充分接触空气,但不受其他干扰。之后用清水彻底洗净涂层表面,并立即(1~2 min)检查涂层变化现象。若涂层表面无变化,不发生发白、起泡、腐蚀脱落等现象,认为涂层耐介质性能通过。
附着力:按照 GB/T 9286-1998《色漆和清漆漆膜的划格试验》测试涂层的附着力,使用刀具规格为 5×5,深度 2mm,胶带为 3M。具体过程如下:先将表面覆有涂层的试样固定,然后将刀具垂直于试样涂层一面,均匀用力在涂层上划出规定的格数。使用软毛刷清理后将胶带均匀完全粘附在划格上,5 min 内呈 60°角度用力平稳撕开,观察剥离网格数目,据此判断附着力等级。
铅笔硬度:按照GB/T 6739-1996《涂层硬度铅笔测定法》测试涂层的铅笔硬度,使用工具包括BY 型铅笔硬度计和中华牌绘图铅笔(硬度范围 6H~6B)。具体过程如下:先将试样涂层一面朝上、水平固定,然后调节平衡重锤使铅笔与待测平面成 45°,匀速推动小车使铅笔在涂层上划痕,用橡皮擦拭划痕后观察涂层表面,未被擦去的铅笔硬度为最终涂层实际硬度。
选用北京中航时代仪器设备有限公司生产的ZST-121 表面电阻测试仪测定各组所得涂料的表面电阻,以表征其抗静电性能。
以上测试,每组5组平行实验,重复5次,取平均值。

Claims (4)

1.一种防腐抗静电机床涂料制备方法,其特征在于,包括以下步骤:
(1)将以重量份计的15-17份氧化石墨烯加入到其体积5-7倍的无水乙醇中,在40-43KHz下超声处理10-12min,然后向其中加入20-30份浓度为0.8-1.2mol/L的氯化铝溶液、3-5份烷基酚聚氧乙烯醚,继续超声20-30min后,在50-55℃下静置2-3h,然后向其中加入质量分数为30-35%的氨水溶液,调节pH为8-8.5,将体系转移至反应釜中,在160-165℃下反应15-18h,冷却,过滤,洗涤后,在50-60℃下干燥10-12h,然后置于530-550℃下焙烧3-4h,研磨,备用;
(2)将步骤(1)所得物进行进一步处理,得到氨基酸锌-氧化铝-氧化石墨烯复合物;
(3)将15-20份步骤(2)所得物加入到40-45份丙酮中,搅拌10-20min后,加入15-20份环氧树脂E44的丙酮溶液,然后在63-65℃,300-500rpm下反应3-5h,冷却,在1500-2000rpm下离心15-17min,抽滤,将所得物在84-86℃下干燥12-16h;
(4)将15-20份步骤(3)所得物加入到40-50份聚四氢呋喃醚二醇中,然后加入0.5-1份三乙醇胺,在400-500rpm搅拌下加热至102-103℃,反应40-50min,然后向其中加入30-40份异佛尔酮二异氰酸酯、30-45份聚四氢呋喃醚二醇、0.5-0.8份有机锡催化剂,在70-76℃、200-300rpm下反应2-3h,然后向其中加入200-300份去离子水,在2200-2300rpm下高速剪切分散40-50min后,加入5-6份乙二醇,继续搅拌20-30min即可。
2.根据权利要求1所述的一种防腐抗静电机床涂料制备方法,其特征在于,步骤(2)所述具体处理方法为:将15-20份步骤(1)所得物加入到40-50份质量分数为34-36%的氨基酸溶液中,在50-60℃、200-300rpm下搅拌10-20min后,向其中加入15-18份质量分数为30-33%的硫酸锌溶液,然后利用饱和氨水溶液调节pH为8.2-8.4,继续搅拌反应40-60min,过滤,洗涤后烘干,得到氨基酸锌-氧化铝-氧化石墨烯复合物。
3.根据权利要求1所述的一种防腐抗静电机床涂料制备方法,其特征在于,步骤(3)所述步骤(3)所述氨基酸为赖氨酸。
4.根据权利要求1所述的一种防腐抗静电机床涂料制备方法,其特征在于,步骤(3)所述环氧树脂E44的丙酮溶液固含量为32-35%。
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