CN103410003B - 一种含氟自润滑型织物涂层材料及其制备方法 - Google Patents
一种含氟自润滑型织物涂层材料及其制备方法 Download PDFInfo
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Abstract
一种含氟自润滑型织物涂层材料及其制备方法,涉及涂层材料及其制备方法。其配方为:含氟树脂30~70g、固化剂10~40g、活性稀释剂5~25g、硅烷偶联剂0.5~5g、硅表面活性剂0.5~3g。本发明含氟量高,含氟聚合物稳定性好,涂层材料为无溶剂环保体系,应用范围广;该涂层材料制备工艺简单,耐候性佳,具有突出的自润滑特性。
Description
技术领域
本发明属于涂层技术领域,涉及一种含氟自润滑涂层材料及其制备方法,尤其是一种用于自润滑关节轴承织物衬垫的涂层材料及其制备方法。
背景技术
关节轴承又称为球面滑动轴承,其结构由一个带球面的外圈和一个带外球面的内圈组成,自润滑关节轴承是一种无需补充润滑剂的特殊形式的关节轴承。其特点是结构简单、体积小、承载力大,而且还具有摩擦系数小、耐冲击、耐腐蚀、减少振动、适用温度范围广、寿命长,在工作过程中可以免维修和无需添加润滑剂等优异特性,广泛应用于工程机械、载重汽车、水利设施、军工机械等方面。因此,在美、法、德、英等一些航空工业发达国家,自润滑关节轴承的研究工作起步很早,经过多年的***研究和试验,现已形成适应多种工况的多品种系列产品。我国关于自润滑关节轴承的研究起步晚,基础研究薄弱,虽然在一些领域部分国内产品能够替代国外产品,但是总体上,从产品质量、性能以及产品系列化上与国外同类产品还存在较大差距,尤其是在航空航天等一些尖端领域应用的自润滑关节轴承技术接近于空白,这已成为影响我国在这些领域获取突破的一个重要瓶颈。
近年来,织物衬垫型自润滑关节轴掀起了一股研究热潮。织物衬垫自润滑关节轴承是指内、外圈间含有织物衬垫形式自润滑材料的关节轴承,具有结构简单紧凑,易于装拆,承载能力高,寿命长,转动灵活,免维护等特点,因此在航空、航天、电力、交通、生物医药和纺织等装备中获得了愈来愈广泛的应用,已经成为这些装备中不可或缺的关键零部件。
织物衬垫自润滑关节轴承的主要失效形式是磨损,磨损使内、外圈间隙过大,衬垫失去正常润滑能力,严重时会造成相关机构咬合卡死。在诸如飞机起落架***等场合,这种失效常导致灾难性后果。故而,织物衬垫表面往往需要涂覆一些涂层,固化以后不仅能够有效固定织物、防止走位,而且具有自润滑性质的涂层将进一步降低摩擦系数。
研究发现,含氟聚合物,具有耐热、耐腐蚀、憎水憎油、电绝缘、低摩擦系数及生物体适应性、不燃性等多种优异性能,使得它在许多应用领域中独领风骚,愈来愈受到人们的关注。氟元素的电负性最大,原子半径很小、形成的碳氟键键长较短、键能大,将氟元素引入环氧树脂中而赋予含氟环氧树脂优异的耐溶剂性、耐油、耐摩擦、表面自洁等性能。
在自润滑涂层领域,章秋明等(一种自润滑型环氧树脂材料及其制备方法,中国专利,公开号CN101348600A)将润滑油胶囊、环氧树脂和固化剂混合均匀浇模,制得自润滑性环氧树脂材料。这种材料在一定程度上能够降低摩擦系数,但是润滑油胶囊不稳定,耐久性差,且材料只能现配现用,不能长期保存,应用受到限制。弗雷克曼等(自润滑涂层及制造自润滑涂层的方法,中国专利,公开号CN102471917A)报道了一种金属层构筑的涂层,其中嵌入了能够通过磨损释放的润滑剂,这种涂层的润滑效果持续长久,但是制备工艺十分复杂,而且无法用于织物、聚合物树脂等材料的涂覆。郭强等(环氧树脂固体润滑涂层材料及其制备方法,中国专利,公开号CN101717604A)公开了一种含表面修饰氧化石墨的环氧树脂固体润滑涂层及其制备方法,克服了石墨固体润滑剂在树脂溶液中分散性差的问题,但是材料的外观受到了一定的影响,应用受到一定的限制。
目前,用于关节轴承衬垫织物的含氟环氧树脂聚合物自润滑涂层尚未见报道。
发明内容
本发明目的在于提供了一种工艺简单的制备自润滑涂层的方法,首先用含氟单体和环氧氯丙烷合成了含氟环氧树脂涂料,用酸酐型固化剂固化并添加活性稀释剂,改善了含氟环氧涂料的脆性,提高涂层的表面弹塑性,且改善了普通环氧胶难以渗入织物内里而达不到固定纤维纹理的目的,因而在低摩擦自润滑的基础上综合提高了关节轴承织物的性能。且本发明所提供的含氟环氧涂层为无溶剂固化体系,符合绿色环保的要求。
所述含氟自润滑型织物涂层材料的配方如下:
含氟树脂30~70g、固化剂10~40g、活性稀释剂5~25g、硅烷偶联剂0.5~5g、硅表面活性剂0.5~3g。
所述含氟树脂结构式如下:
其中R1、R2均为—(CF2)n—,n为1~18或
R3、R4均为CF3或CF2CF3。
所涉及的含氟树脂的制备如下:
(1)将30~40g含氟单体和20~30g环氧氯丙烷加入反应容器中,搅拌溶液,升温60-70℃。
(2)用5~10gNaOH和15~20ml去离子水配成碱液,1~1.5小时加入反应容器中,温度控制依然控制在60-70℃。
(3)滴加完碱液,将反应物在70℃下回流1.5小时,体系呈现乳黄色。
(4)加入去离子水、甲苯,搅拌均匀后,静置分液,除去水层,重复几次操作除去水层分出有机相,减压下蒸馏除去溶剂甲苯和未反应的环氧氯丙烷,得淡黄色粘稠树脂。
所述固化剂为与含氟环氧树脂配合使用的酸酐类化合物等,如邻苯二甲酸酐、均苯四甲酸酐、甲基环己烯四羧酸酐、顺丁烯二酸酐等。
所述活性稀释剂为1,6-己二醇二丙烯酸酯、甲基丙烯酸-β-羟乙酯、甲苯缩水甘油醚、蓖麻油多缩水甘油醚或乙二醇二缩水甘油醚。
所述硅烷偶联剂采用通式为Y(CH2)nSiX3的硅烷偶联剂,其中,n=0~3;X为氯基、甲氧基、乙氧基、甲氧基乙氧基、乙酰氧基等,Y为氨基或环氧基。
所述硅表面活性剂为硅烷基型、硅氧烷基型、阴离子型、阳离子型或非离子型硅表面活性剂。
所述含氟自润滑型织物涂层材料的制备方法为:按照涂层组成,首先按硅烷偶联剂、固化剂先后顺序依次溶于活性稀释剂中,搅拌0.5~1小时得到均相溶液;其次,搅拌条件下分批量向溶液中加入含氟环氧树脂,搅拌1~2小时至均匀。使用时,将织物剂清洗干净后刷涂本发明所制备的涂层材料,40~60℃下用鼓风烘箱烘1~2小时,然后施加0.2~0.3Mpa的压力并升温至150~170℃保温2~3小时固化。
本发明含氟自润滑型织物涂层材料具有以下特点:
(1)针对自润滑关节轴承最常用的聚四氟乙烯织物,选择含氟环氧树脂对其进行编织纤维之间的固位,防止织物走位引起的摩擦磨损。即利用了环氧树脂良好的粘接性能,又通过含氟环氧的改性降低了涂层的摩擦系数和提高了涂层的自润滑性能。
(2)使用了活性稀释剂,涂层材料能够有效浸渍纤维,且固化剂使用是酸酐和活性稀释剂体系,提高弹塑性,能有效将应力分散而提高了轴承的承载能力。
(3)采用可参与反应的活性稀释剂取代传统的挥发性溶剂,符合绿色环保的理念。
附图说明
图1为实施例1中含氟树脂的核磁谱图。
图2为实施例1中含氟树脂的红外谱图。
具体实施方式
下面结合实施例对本发明作进一步详细的描述。
实施例1
顺丁烯二酸酐35g、活性稀释剂(669)15g、氨丙基三乙氧基硅烷偶联剂0.5g、硅表面活性剂SH-2000.5g超声分散均匀1小时,继续分10次加入60g含氟树脂,在低速分散机中搅拌分散1小时得到自润滑涂层。将待涂刷织物用丙酮清洗干净,使用本发明涂层进行薄层刷涂,置于鼓风烘箱中50℃烘1小时,取出施加0.2Mpa的压力并升温(程序升温,2小时内)至160℃固化2小时。固化完成后测得摩擦系数为0.032,比磨损率为2.8±0.7(×10-6mm3/Nm)。
所涉及的含氟树脂的制备如下:
(1)将30g1,1-双(4-羟基苯基)-1-苯基-2,2,2-三氟乙烷和28g环氧氯丙烷加入加入带有搅拌棒及控温装置的三口烧瓶中,搅拌溶液,升温65℃。
(2)取6gNaOH和17ml去离子水配成碱液,1.5小时内加入反应容器中,温度控制依然控制在65℃。
(3)滴加完碱液,将反应物在70℃下回流1.5小时,体系呈现乳黄色。
(4)加入27ml去离子水、54ml甲苯,搅拌均匀后,静置分液,除去水层,重复几次操作除去水层分出有机相,减压下蒸馏除去溶剂甲苯和未反应的环氧氯丙烷,得淡黄色粘稠含氟树脂。
实施例2
顺丁烯二酸酐30g、活性稀释剂66920g、氨丙基三乙氧基硅烷偶联剂1g、硅表面活性剂SH-2000.5ml超声分散均匀1小时,继续分10次加入60g含氟树脂,在低速分散机中搅拌分散1小时得到自润滑涂层。将待涂刷织物用丙酮清洗干净,使用本发明涂层进行薄层刷涂,置于鼓风烘箱中50℃烘1小时,取出施加0.2Mpa的压力并升温(程序升温,2小时内)至160℃固化2小时。固化完成后测得摩擦系数为0.036,比磨损率为2.7±0.7(×10-6mm3/Nm)。
所涉及的含氟树脂的制备如下:
(1)将35g1,1-双(4-羟基苯基)-1-(3-三氟甲基苯基)-2,2,2-三氟乙烷和26g环氧氯丙烷加入加入带有搅拌棒及控温装置的三口烧瓶中,搅拌溶液,升温65℃。
(2)取7gNaOH和15ml去离子水配成碱液,1.5小时内加入反应容器中,温度控制依然控制在65℃。
(3)滴加完碱液,将反应物在70℃下回流1.5小时,体系呈现乳黄色。
(4)加入27ml去离子水、54ml甲苯,搅拌均匀后,静置分液,除去水层,重复几次操作除去水层分出有机相,减压下蒸馏除去溶剂甲苯和未反应的环氧氯丙烷,得淡黄色粘稠含氟树脂。
实施例3
顺丁烯二酸酐35g、活性稀释剂66920g、氨丙基三乙氧基硅烷偶联剂1g、硅表面活性剂SH-2001g超声分散均匀1小时,继续分10次加入65g含氟树脂,在低速分散机中搅拌分散1小时得到自润滑涂层。将待涂刷织物用丙酮清洗干净,使用本发明涂层进行薄层刷涂,置于鼓风烘箱中50℃烘1小时,取出施加0.2Mpa的压力并升温(程序升温,2小时内)至160℃固化2小时。固化完成后测得摩擦系数为0.035,比磨损率为2.9±0.7(×10-6mm3/Nm)。
所涉及的含氟树脂的制备如下:
(1)将30g2,2-二(羟基苯基)-,1,1,3.3,3-六氟丙烷和26g环氧氯丙烷加入加入带有搅拌棒及控温装置的三口烧瓶中,搅拌溶液,升温65℃。
(2)取6gNaOH和15ml去离子水配成碱液,1.5小时内加入反应容器中,温度控制依然控制在65℃。
(3)滴加完碱液,将反应物在70℃下回流1.5小时,体系呈现乳黄色。
(4)加入27ml去离子水、54ml甲苯,搅拌均匀后,静置分液,除去水层,重复几次操作除去水层分出有机相,减压下蒸馏除去溶剂甲苯和未反应的环氧氯丙烷,得淡黄色粘稠含氟树脂。
实施例4
顺丁烯二酸酐30g、活性稀释剂66915g、氨丙基三乙氧基硅烷偶联剂1g、硅表面活性剂SH-2000.5g超声分散均匀1小时,继续分10次加入50g含氟树脂,在低速分散机中搅拌分散1小时得到自润滑涂层。将待涂刷织物用丙酮清洗干净,使用本发明涂层进行薄层刷涂,置于鼓风烘箱中50℃烘1小时,取出施加0.2Mpa的压力并升温(程序升温,2小时内)至160℃固化2小时。固化完成后测得摩擦系数为0.034,比磨损率为2.9±0.7(×10-6mm3/Nm)。
所涉及的双酚AF型环氧树脂的制备同实施例3。
Claims (7)
1.一种含氟自润滑型织物涂层材料,其特征在于所述织物涂层材料的配方如下:
含氟树脂30~70g、固化剂10~40g、活性稀释剂5~25g、硅烷偶联剂0.5~5g、硅表面活性剂0.5~3g;
所述含氟树脂结构式如下:
其中R1、R2均为—(CF2)n—,n为1~18或
R3、R4均为CF3或CF2CF3。
2.根据权利要求1所述的一种含氟自润滑型织物涂层材料,其特征在于所述含氟树脂的制备方法如下:
(1)将30~40g含氟单体和20~30g环氧氯丙烷加入反应容器中,搅拌溶液,升温60-70℃;
(2)用5~10gNaOH和15~20g水配成碱液,1~1.5小时加入反应容器中,温度控制依然控制在60-70℃;
(3)滴加完碱液,将反应物在70℃下回流1.5小时,体系呈现乳黄色;
(4)加入去离子水、甲苯,搅拌均匀后,静置分液,除去水层,重复几次操作除去水层分出有机相,减压下蒸馏除去溶剂甲苯和未反应的环氧氯丙烷,得淡黄色粘稠树脂。
3.根据权利要求2所述的一种含氟自润滑型织物涂层材料,其特征在于所述固化剂为与含氟环氧树脂配合使用的酸酐类化合物,为邻苯二甲酸酐、均苯四甲酸酐、甲基环己烯四羧酸酐、顺丁烯二酸酐的一种。
4.根据权利要求3所述的一种含氟自润滑型织物涂层材料,其特征在于所述活性稀释剂为1,6-己二醇二丙烯酸酯、甲基丙烯酸-β-羟乙酯、甲苯缩水甘油醚、蓖麻油多缩水甘油醚或乙二醇二缩水甘油醚。
5.根据权利要求4所述的一种含氟自润滑型织物涂层材料,其特征在于所述硅烷偶联剂采用通式为Y(CH2)nSiX3的硅烷偶联剂,其中,n=0~3;X为氯基、甲氧基、乙氧基、甲氧基乙氧基、乙酰氧基,Y为氨基或环氧基。
6.根据权利要求5所述的一种含氟自润滑型织物涂层材料,其特征在于所述硅表面活性剂为硅烷基型、硅氧烷基型、阴离子型、阳离子型或非离子型硅表面活性剂。
7.根据权利1至6之一所述的一种含氟自润滑型织物涂层材料的制备方法,其特征在于按照所述涂层组成,按硅烷偶联剂、固化剂先后顺序依次溶于活性稀释剂中,搅拌0.5~1小时得到均相溶液;其次,搅拌条件下分批量向溶液中加入含氟环氧树脂,搅拌1~2小时至均匀;使用时,将织物清洗干净后刷涂涂层材料,40~60℃下用鼓风烘箱烘1~2小时,然后施加0.2~0.3MPa的压力并升温至150~170℃保温2~3小时固化。
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