CN114960208A - 一种应用于超高分子量聚乙烯纤维缆绳表面的耐磨树脂涂料及其涂覆工艺 - Google Patents
一种应用于超高分子量聚乙烯纤维缆绳表面的耐磨树脂涂料及其涂覆工艺 Download PDFInfo
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Abstract
本申请提供了一种应用于超高分子量聚乙烯纤维缆绳表面的耐磨树脂涂料及其涂覆工艺,所述的耐磨树脂涂料括以下质量配比的组分:4~10%的热塑性聚氨酯;0.5~2.5%的消泡剂;1~5%的金属氧化物纳米粒子;0.5~2.5%的流平剂;余量为有机溶剂。本发明提供的耐磨树脂涂料可提升超高分子量聚乙烯纤维的耐磨性能,同时具有较好的纤维附着力。实验显示,纤维经过表面改性之后超高分子量聚乙烯纤维表面的极性基团有大量提升,聚氨酯树脂在纤维表面的剪切强力能达到19mN,有利于纤维与树脂的结合。耐磨树脂涂层在纤维上涂覆之后,与未涂有耐磨树脂的纤维进行耐磨性能比较,纤维的耐磨性能提升了14%,利于应用。
Description
技术领域
本申请属于超高分子量聚乙烯纤维改性的技术领域,涉及一种应用于超高分子量聚乙烯纤维缆绳表面的耐磨树脂涂料及其涂覆工艺。
背景技术
超高分子量聚乙烯纤维(UHMWPE)高强缆绳在军事领域应用广泛,其具有很高的强力,且相较于钢丝绳,UHMWPE纤维缆绳具有自身重量小、存放更为方便、较难受到海水腐蚀等特点。目前,高强纤维主要被用于制作各种舰艇及各类船舶的抛锚绳、停泊索、抗风浪缆绳及码头的吊装卸绳索等,因此,这类产品被广泛应用于海上救援、船舶工业、海上作业勘测、海洋地球物探、船系泊等领域。
在缆绳使用过程中,摩擦是一种不可避免的现象,其产生的不良结果导致缆绳的磨损,使纤维表面受到物理和/或化学作用产生材料脱落、失效等现象,因此,摩擦现象对缆绳的使用寿命、使用安全性产生很大影响,还会给国民经济带来巨大损失。UHMWPE纤维制成的缆绳本身具有较好的耐磨性,然而,由于长时间在风吹日晒、海水浸泡、雨水冲刷、摩擦磨损等复杂环境下服役,缆绳表面容易受到损伤,这会破坏超高分子量聚乙烯纤维表面的惰性层,导致缆绳耐磨性急剧下降,进而降低缆绳的安全系数、使用寿命,为船只的安全航行带来极大的安全隐患。因此,针对UHMWPE纤维缆绳耐磨性能提升方面的工作具有重大意义。
其中,可利用树脂涂覆提升UHMWPE纤维耐磨性能,该方法具体是通过在UHMWPE纤维材料表面添加涂层,将纤维材料本身与复杂的外界环境隔离,从而达到牺牲涂层、保护纤维本体的目的。目前一般可应用的涂层主要分为橡胶类、环氧树脂类、有机硅树脂类、聚氨酯类、聚丙烯酸酯类,这些耐磨涂层的具体特点如下:橡胶类涂层弹性好,但容易老化;聚丙烯酸酯与基体粘附性好,但容易发生热黏冷脆现象。
环氧树脂类涂层中,环氧树脂是一种低聚合度的高分子预聚物,其分子链中含有多个环氧基团等活性基团,环氧基团在固化剂的作用下能够开环聚合同时形成紧密的网状结构。但环氧树脂反应交联后固化密度高、硬度过大、柔性差,在弯曲程度大的表面以及面积小的表面形成的涂层效果不好。有机硅树脂是一种含有硅氧基团的半有机型高聚物,硅原子和氧原子交替连结组成骨架,不同种类的有机基团与硅原子连结构成聚合物。有机硅树脂的耐热、耐高温性能优异,刚性高,在高温防护涂层中具有广泛应用,但常温性能反而不够理想,粘接力较差。
对于聚氨酯树脂类,聚氨酯的全称为聚氨基甲酸酯(PU),在其主链上含有氨基甲酸酯基团(-NH-COO)。合成聚氨酯的原料主要包括:聚合二元醇、二异氰酸酯、二元醇。聚氨酯的形成过程是聚合二元醇与二异氰酸酯在合适的溶剂中反应形成预聚物,当预聚物制备完成后加入扩链剂,使预聚物发生聚合反应形成高分子量的聚氨酯,反应式示意如下:
从分子链结构来看,聚氨酯分子是由硬段和软段相间分布形成的一种高聚物,其中二异氰酸酯和扩链剂构成了硬段,而聚合二元醇构成了其中的软段。硬段之间吸引力较大,能够起到聚合物的增强作用,提高聚合物材料的力学性能,软段的柔性较大,能够影响聚合物材料的热学性能和弹性性能。因此,相对来说聚氨酯类涂层拥有密度低、耐磨性好的优点。
然而,目前的耐磨树脂涂层在耐磨性及粘结性等综合方面还有待进一步改善。
发明内容
有鉴于此,本申请提供一种应用于超高分子量聚乙烯纤维缆绳表面的耐磨树脂涂料及其涂覆工艺,本发明提供的耐磨树脂涂料可提升超高分子量聚乙烯纤维的耐磨性能,同时具有较好的纤维附着力。
本发明提供一种应用于超高分子量聚乙烯纤维缆绳表面的耐磨树脂涂料,包括以下质量配比的组分:
4~10%的热塑性聚氨酯;
0.5~2.5%的消泡剂;
1~5%的金属氧化物纳米粒子;
0.5~2.5%的流平剂;
余量为有机溶剂。
在本发明的优选实施例中,所述消泡剂为聚硅氧烷类消泡剂;所述流平剂为有机硅类流平剂。
在本发明的优选实施例中,所述金属氧化物纳米粒子的成分选自三氧化二铝和氧化锆中的一种或多种。
在本发明的优选实施例中,所述金属氧化物纳米粒子的粒径为20-250nm。
在本发明的优选实施例中,所述有机溶剂选自N,N-二甲基甲酰胺和二丙二醇丁醚中的一种或多种。
在本发明的优选实施例中,所述热塑性聚氨酯的硬度为85-90shore A。
本发明提供如前所述的耐磨树脂涂料的涂覆工艺,包括以下步骤:
将超高分子量聚乙烯纤维浸渍于前文所述的耐磨树脂涂料中,保持一定时间后取出固化,得到具有耐磨涂层的纤维材料。
在本发明的优选实施例中,在浸渍前,所述超高分子量聚乙烯纤维利用强氧化剂进行表面改性处理,使纤维表面引入含氧活性官能团。
在本发明的优选实施例中,所述强氧化剂选自重铬酸钾、高锰酸钾和硫酸中的一种或多种,优选为重铬酸钾和硫酸混合氧化液。
在本发明的优选实施例中,所述表面改性处理的温度为25-65℃,处理时间为0.5-3.5min。
与现有技术相比,本发明首先采用聚氨酯为耐磨树脂涂料的主要成分,并且配合使用一定比例的消泡剂、流平剂和金属氧化物纳米粒子,形成耐磨性提升的耐磨树脂涂料。本发明的耐磨树脂涂料配方中,聚氨酯大分子中既含有刚性链段和柔性链段,又含有强极性基团,使聚氨酯不仅能最大限度的吸收来自外部介质的冲击,且能同时维持自身足够的刚度与机械强度,从而使其应用的超高分子量聚乙烯纤维材料机械强度大、柔韧性好、界面相容性好、粘接性强、耐受性能优异。经所述的涂料配方各组分共同作用,应用于超高分子量聚乙烯纤维材料,本发明可提升耐磨树脂涂层及纤维材料的耐磨性能及粘结性能。
进一步地,本发明实施例优选将化学试剂处理法用于纤维表面改性,利用强氧化剂本身的氧化作用破坏纤维的界面层并且在纤维表面产生化学刻蚀,提升纤维表面的粗糙度,增加其与树脂的接触面积,也有利于与树脂发生机械啮合;同时,化学试剂可以在纤维表面引入-OH、-COOH等含氧活性官能团,改善纤维的润湿性,同时有利于纤维表面与树脂发生化学键结合,有助于提高其与树脂的粘结性能。
实验显示,纤维经过表面改性之后超高分子量聚乙烯纤维表面的极性基团有大量提升,聚氨酯树脂在纤维表面的剪切强力能达到19mN,有利于纤维与树脂的结合。耐磨树脂涂层在纤维上涂覆之后,与未涂有耐磨树脂的纤维进行耐磨性能比较,纤维的耐磨性能提升了14%。
附图说明
图1为本发明实施例中不同表面处理温度的UHMWPE纤维的红外谱图;
图2为本发明实施例中不同表面处理温度的UHMWPE纤维承受载荷结果;
图3为本发明实施例中不同表面处理时间的UHMWPE纤维的红外谱图;
图4为本发明实施例中不同表面处理时间的UHMWPE纤维承受载荷结果;
图5为本发明实施例的UHMWPE纤维浸胶前后对比情况。
具体实施方式
下面对本申请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申请一部分实施例,而不是全部的实施例。基于本申请中的实施例,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,都属于本申请保护的范围。
本发明提供了一种应用于超高分子量聚乙烯纤维缆绳表面的耐磨树脂涂料,包括以下质量配比的组分:
4~10%的热塑性聚氨酯;
0.5~2.5%的消泡剂;
1~5%的金属氧化物纳米粒子;
0.5~2.5%的流平剂;
余量为有机溶剂。
本发明提供的耐磨树脂涂料可应用于超高分子量聚乙烯纤维缆绳表面,提升超高分子量聚乙烯纤维的耐磨性能,同时与纤维的附着力较高。
本发明实施例所述的耐磨树脂涂料为聚氨酯树脂类,以热塑性聚氨酯 (TPU)为主要成分,其具体用量为4~10wt%,优选为4.5-6wt%;本发明对聚氨酯树脂的成分、配比优化有利于提升耐磨性。在本发明的实施例中,所述热塑性聚氨酯的分子链结构包括相间分布的硬段(刚性链段)和软段(柔性链段),该高聚物中硬段是二异氰酸酯和扩链剂结构,软段是聚合二元醇结构。具体地,所述热塑性聚氨酯的硬度为85-90shore A。
本发明一些实施例中采用型号TPU1185A(巴斯夫公司)的聚氨酯树脂,其密度1.12g/cm3,硬度87shore A。
并且,本发明实施例所述的耐磨树脂涂料还包含消泡剂、溶剂和消泡剂等组分,便于涂料制备和应用。其中,所述耐磨树脂涂料包括1~5%的金属氧化物纳米粒子,优选包括2~5%的金属氧化物纳米粒子,进一步增强涂料强度和耐磨性等。作为优选,所述金属氧化物纳米粒子的成分为三氧化二铝(Al2O3) 和氧化锆(ZrO2)中的一种或多种,更优选两者混用;所述金属氧化物纳米粒子的粒径可为20-250nm,进一步在50nm-200nm之间。在本发明的具体实施例中,加入Al2O3(α晶形,200nm)和ZrO2(50nm)纳米粒子,质量分数均为2.5%。
在本发明中,所述消泡剂优选为聚硅氧烷类消泡剂,包括但不限于消泡剂BYK024。所述流平剂优选有机硅类流平剂,包括但不限于流平剂BYK349。此外,所述有机溶剂优选选自N,N-二甲基甲酰胺和二丙二醇丁醚中的一种或多种,溶剂用量可为90~95wt%。本发明优选实施例采用TPU1185A聚氨酯作为主要原材料,并加入了一定比例的各类添加剂,使得涂层具有耐磨性能、流平性能、粘结性能优异的特点,利于应用。
本发明实施例提供了如前所述的耐磨树脂涂料的制备方法,优选包括以下步骤:
先将所述的热塑性聚氨酯与有机溶剂混合,溶解得到树脂溶液,然后加入消泡剂、流平剂和金属氧化物纳米粒子,得到所述耐磨树脂涂料。
在所述耐磨树脂涂料的制备过程中,各原料试剂的内容如前所述,涂料组成满足100%。涂料制备优选在搅拌条件下进行,使混合均匀。
本发明提供了如前所述的耐磨树脂涂料的涂覆工艺,包括以下步骤:
将超高分子量聚乙烯纤维浸渍于前文所述的耐磨树脂涂料中,保持一定时间后取出固化,得到具有耐磨涂层的纤维材料。
超高分子量聚乙烯纤维(UHMWPE纤维)相对钢丝的重量小,强度高,耐海水腐蚀,纤维表面光滑,采用市售产品即可。在本发明的实施例中,所述超高分子量聚乙烯纤维的规格包括:1600D,纤维股数为440,单丝纤度为3.6d;单丝纤维强度可在50N左右。
由于超高分子量聚乙烯纤维表面光滑,树脂在纤维表面的附着力较差,导致纤维表面的树脂膜易脱落,因此提升聚氨酯树脂与纤维之间的附着力非常关键。在浸渍所述耐磨树脂涂料前,本发明实施例提供了所述超高分子量聚乙烯纤维的表面改性方法,具体利用强氧化剂对纤维进行表面改性处理,使纤维表面引入含氧活性官能团,得到改性的纤维材料。
在本发明的实施例中,所述强氧化剂选自重铬酸钾、高锰酸钾和硫酸中的一种或多种,优选为重铬酸钾和硫酸混合氧化液(K2Cr2O7/H2O/H2SO4混合,具体比例可为4.2wt%/7.1wt%/88.7wt%)。本发明实施例通过化学试剂处理法,在表面改性过程简便、有效提升了纤维表面的羟基数目,并且可以保证纤维强度。
具体地,本发明实施例配制强氧化剂溶液(简称氧化液),将超高分子量聚乙烯纤维浸没在所述强氧化剂溶液中并保持一定时间,之后取出纤维,可充分水洗以去除氧化液,经干燥,得到改性后的纤维。
作为优选,所述表面改性处理的温度为25-65℃,更优选为30-60℃,进一步优选为60℃,可通过恒温水浴控制处理温度。所述表面改性处理的时间优选为0.5-3.5min,更优选为1.5-2.5min,进一步优选为2min。本发明实施例优化所配氧化剂溶液和处理时间、处理温度等,可有效增加UHMWPE纤维表面的羟基等活性基团,有利于提升树脂在纤维表面的附着力。
按照纤维表面改性工艺对UHMWPE纤维进行表面改性后,本发明实施例将改性的纤维材料浸入上述制备的耐磨树脂涂料中,确保纤维完全浸没,避免浸胶不均匀的现象。所述改性的纤维在树脂涂料溶液中保持10-30s后,取出,垂直悬挂,可使之在室温(25℃)下自然风干1天,使纤维表面包覆的树脂充分固化,形成所需的耐磨涂层,得到涂覆了耐磨树脂的纤维材料。
与未涂有耐磨树脂的纤维相比,本发明所述的耐磨树脂涂层在纤维上涂覆之后,纤维的耐磨性能得到提升,且纤维与树脂结合较好。
为了更好理解本发明技术内容,下面提供具体实施例,对本发明做进一步的说明。如无特殊说明的,均为重量配比。以下实施例中,所用原料为市售产品。
所述的聚氨酯型号为TPU1185A,购于巴斯夫;二丙二醇丁醚(分析纯, 98.0%)购于陶氏;消泡剂BYK024和流平剂BYK349均购于毕克。重铬酸钾(分析纯,99%)购于阿拉丁;硫酸(分析纯)购于北京化工厂、N,N-二甲基甲酰胺(分析纯,99.5%)、3-氨丙基三乙氧基硅烷偶联剂KH550(分析纯,99%)、纳米二氧化硅(SiO2)(30±5nm)、纳米二氧化锆(ZrO2)(50nm) 和纳米氧化铝(Al2O3)(α晶形,200nm)均购于上海麦克林生化科技有限公司。所用的UHMWPE纤维为湖南中泰特种装备有限责任公司生产的ZTX98,产品规格为1600D,纤维股数为440,单丝纤度为3.6d。
实施例1
耐磨树脂涂料制备:
(1)将4.5wt%的TPU1185A与90.5wt%的N,N-二甲基甲酰胺混合;
(2)70℃恒温水浴下保温1小时,得到树脂溶液;
(3)向所述树脂溶液中加入1.5wt%的消泡剂BYK024,充分搅拌;
(4)将搅拌后的混合溶液于70℃下继续保温1小时;
(5)向上述样品中加入2wt%的二丙二醇丁醚、流平剂BYK349 1.5wt%,混合均匀;
(6)向混合均匀的样品中加入Al2O3(α晶形,200nm)和ZrO2(50nm) 纳米粒子,二者质量分数均为2.5%;
(7)搅拌0.5小时,得到所需耐磨树脂涂料。
实施例2
UHMWPE纤维表面改性工艺:
(1)配置K2Cr2O7/H2O/H2SO4比例为4.2wt%/7.1wt%/88.7wt%的重铬酸钾酸性溶液,以此为氧化液;
(2)超声0.5h;
(3)将超声后的氧化液置于60℃恒温水浴环境中;
(4)将UHMWPE纤维浸没在上述氧化液中,保持2min;
(5)取出纤维,充分水洗;
(6)将水洗后的纤维悬挂,自然风干1天,得到改性后的纤维。
实施例3
与实施例2的基本工艺步骤相同,区别在于,替换处理温度为30℃、40℃、 50℃、70℃,分别得到改性后的纤维。
不同表面处理温度的UHMWPE纤维的红外谱图参见图1,纤维承受载荷结果参见图2。
实施例4
与实施例2的基本工艺步骤相同,区别在于,替换处理时间为1min、3min、 4min、5min,分别得到改性后的纤维。
不同表面处理时间的UHMWPE纤维的红外谱图参见图3,纤维承受载荷结果参见图4。
表面改性过程虽然有效提升了纤维表面的羟基数目,但也有可能降低纤维的剪切强度,影响纤维的使用性能。本发明实施例对不同温度下处理表面改性过后的纤维进行了力学性能测试。采用电子万能材料试验机对不同处理温度或不同处理时间后的纤维进行拉伸测试。纤维拉伸测试采用5KN Instron5565电子万能材料试验机,测试采用10根单丝纤维组成的纤维束,试样原始长度为15.0cm,试样拉伸速率为10mm/s,数据采集间隔为0.02s,力值精确度为0.01mN,位移精确度为0.01μm。
根据红外谱图,相比于未被处理的样品,经过酸处理的样品在3352cm-1处出现了非常明显的特征O-H震动峰,并且在900-1200cm-1之间也出现了相对较小的吸收峰,这些峰为C-O伸缩震动峰,这两个峰的强度随着温度的升高逐渐增强。以60℃为氧化液表面处理温度,不同的处理时间下酸处理的样品的FT-IR图表明,随着处理时间的增加,O-H和C-O的特征峰也呈现出明显增强的趋势。以上结果表明,随着温度的升高及处理时间的增长,纤维表面产生的羟基数目得到了明显的提升。
实验结果表明,表面处理温度为30℃、处理一分钟后,单丝纤维的承受载荷可以达到51.23N,随着温度升高至70℃,单丝纤维的承受载荷降低至 41.1N(图2)。通过改变表面处理时间,单丝纤维的承受载荷由49.31N下降至41.52N(图4),尤其在氧化时间为3min及以上时,相较于未改性纤维(pristine) 的51.35N下降超过了14%。
由上述结果可知,K2Cr2O7/H2O/H2SO4混合酸处理,改性时间为2min,改性温度为60℃,性能最佳。
实施例5
按照纤维表面最佳改性工艺对UHMWPE纤维进行表面改性后,再将纤维浸入实施例1制备的耐磨树脂涂料中,纤维在树脂溶液中保持10s后,取出,垂直悬挂,在室温(25℃)下自然风干1天,形成所需的耐磨涂层,得到涂覆了耐磨树脂的纤维材料。
UHMWPE纤维浸胶前后对比情况参见图5,图5是光学照片,上方是浸胶前的纤维,下方是浸涂后的纤维;浸涂后纤维增重为19.18%。
聚氨酯树脂在纤维表面的剪切强力能达到19mN,有利于纤维与树脂的结合。耐磨树脂涂层在纤维上涂覆之后,与未涂有耐磨树脂的纤维进行耐磨性能比较,纤维的耐磨性能提升了14%。
耐磨性能测试方法如下:实验室自主研发的摩擦磨损仪,在1KG负载的拉引下摩擦1000次,磨损介质为2000目的砂纸,磨损段长度:4.5cm;
负载:1KG;
涂膜前的磨损率为4.09×10-3mm3/(Nm),涂膜后的磨损率为3.52×10-3 mm3/(Nm)。
由以上实施例可知,本发明所述的涂料配方各组分共同作用,应用于超高分子量聚乙烯纤维材料,可提升耐磨树脂涂层及纤维材料的耐磨性能及粘结性能。进一步地,本发明实施例优选将化学试剂处理法用于纤维表面改性,有助于提高其与树脂的粘结性能。实验显示,纤维经过表面改性之后超高分子量聚乙烯纤维表面的极性基团有大量提升,聚氨酯树脂在纤维表面的剪切强力能达到19mN,有利于纤维与树脂的结合。耐磨树脂涂层在纤维上涂覆之后,与未涂有耐磨树脂的纤维进行耐磨性能比较,纤维的耐磨性能提升了14%。本申请优化出耐磨性能较好的树脂之后,采用了最优的配方应用于纤维,达到了项目要求的指标。
以上所述的实施例仅是对本发明的优选方式进行描述,并非对本发明的范围进行限定,在不脱离本发明设计精神的前提下,本领域普通技术人员对本发明的技术方案做出的各种变形和改进,均应落入本发明权利要求书确定的保护范围内。
Claims (10)
1.一种应用于超高分子量聚乙烯纤维缆绳表面的耐磨树脂涂料,其特征在于,包括以下质量配比的组分:
4~10%的热塑性聚氨酯;
0.5~2.5%的消泡剂;
1~5%的金属氧化物纳米粒子;
0.5~2.5%的流平剂;
余量为有机溶剂。
2.根据权利要求1所述的耐磨树脂涂料,其特征在于,所述消泡剂为聚硅氧烷类消泡剂;所述流平剂为有机硅类流平剂。
3.根据权利要求1所述的耐磨树脂涂料,其特征在于,所述金属氧化物纳米粒子的成分选自三氧化二铝和氧化锆中的一种或多种。
4.根据权利要求3所述的耐磨树脂涂料,其特征在于,所述金属氧化物纳米粒子的粒径为20-250nm。
5.根据权利要求1所述的耐磨树脂涂料,其特征在于,所述有机溶剂选自N,N-二甲基甲酰胺和二丙二醇丁醚中的一种或多种。
6.根据权利要求1-5任一项所述的耐磨树脂涂料,其特征在于,所述热塑性聚氨酯的硬度为85-90shore A。
7.如权利要求1-6任一项所述的耐磨树脂涂料的涂覆工艺,包括以下步骤:
将超高分子量聚乙烯纤维浸渍于权利要求1-6任一项所述的耐磨树脂涂料中,保持一定时间后取出固化,得到具有耐磨涂层的纤维材料。
8.根据权利要求7所述的涂覆工艺,其特征在于,在浸渍前,所述超高分子量聚乙烯纤维利用强氧化剂进行表面改性处理,使纤维表面引入含氧活性官能团。
9.根据权利要求8所述的涂覆工艺,其特征在于,所述强氧化剂选自重铬酸钾、高锰酸钾和硫酸中的一种或多种,优选为重铬酸钾和硫酸混合氧化液。
10.根据权利要求9所述的涂覆工艺,其特征在于,所述表面改性处理的温度为25-65℃,处理时间为0.5-3.5min。
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