CN104313563A - 一种半金属配方刹车片中钢纤维改性的方法 - Google Patents

一种半金属配方刹车片中钢纤维改性的方法 Download PDF

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CN104313563A
CN104313563A CN201410467752.9A CN201410467752A CN104313563A CN 104313563 A CN104313563 A CN 104313563A CN 201410467752 A CN201410467752 A CN 201410467752A CN 104313563 A CN104313563 A CN 104313563A
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杨阳
刘伯威
匡湘铭
唐兵
涂元满
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HUNAN BOYUN AUTOMOBILE BRAKE MATERIAL CO Ltd
HUNAN BOYUN AUTOMOBILE BRAKE MATERIALS CO Ltd
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Abstract

本发明公开了一种半金属配方刹车片中钢纤维改性的方法，（1）用碳酸钠溶液浸泡进行除油，（2）稀释后的食人鱼溶液浸泡处理钢纤维，（3）偶联剂溶液处理使钢纤维表面覆盖一层膜，（4）进行热处理使膜固化，并进行打散制得表面分布均匀、厚度适宜有机膜的钢纤维。本发明成功改性钢纤维，解决了金属摩擦片热衰退性能差、使用寿命短和易生锈的问题，使用改性后的钢纤维作为金属刹车片的原料，刹车片的热衰退性能使用寿命大大提升。

Description

一种半金属配方刹车片中钢纤维改性的方法
技术领域
本发明属于新材料技术领域，特别涉及一种半金属配方刹车片中钢纤维改性的方法。
背景技术
随着人们经济收入的不断提高及汽车产业的快速发展,汽车已越来越多地进入普通家庭,刹车片的销量也日益增加，客户对刹车片耐磨和使用寿命要求越来越高。钢纤维因其具有优良的力学性能，如高韧性、强度高、良好的导热性和耐热性，在半金属配方摩擦材料中作为增强组分得到广泛应用。但半金属刹车片存在一个缺点就是磨损大，这样会导致落灰严重、使用寿命短等问题。另外，钢纤维在潮湿环境下容易生锈，影响产品外观且导致锈粘结问题影响客户使用。
半金属配方摩擦材料中的钢纤维表面物理化学性质如表面晶体结构、官能团、表面能与摩擦材料中的有机粘结剂树脂存在很大差异，钢纤维与基体树脂的结合能力明显差于非金属纤维及其矿物纤维，摩擦材料中的钢纤维在摩擦磨损的高温条件下易出现纤维与基体的分离和转移，导致磨损率上升。钢纤维属金属材料与有机树脂表面属性差异很大,和树脂有机粘结剂结合力弱，尤其是刹车片中钢纤维添加量过高时, 从基体上脱落的概率大大增加, 温度较高时树脂与纤维界面之间易形成热裂纹使疲劳磨损更加显著。大量脱落的硬相钢纤维形成的磨粒又加剧了摩擦面的磨料磨损。另外, 钢纤维与灰铸铁的摩擦对偶件同属铁基材料, 在高温下二者极易发生黏着形成黏着磨损。
硅烷和钛酸酯偶联剂是一种有机-无机杂化的双官能团化合物，与亲水的钢表面和疏水的有机粘结剂都可以发生化学吸附或化学反应，形成比较牢固而耐久的分子键或化学键，在树脂和钢纤维之间起着化学桥的作用。这样就能大大提高树脂和钢纤维的结合能力。钢纤维通过进行改性后，可减少刹车片的磨损，提高使用寿命。
偶联剂在水解后能形成硅醇、钛醇,醇羟基之间可以互相反应生成一层交联的致密网状疏水膜,由于这种膜表面有能够和树脂起反应的有机官能基团,钢纤维表面覆盖硅烷或钛膜，具有一定防蚀作用。且钢纤维表面覆盖的偶联剂膜本身是疏水的，防腐效果更强，可用作有机腐蚀抑制剂，可防止钢纤维的生锈。   
发明内容
本发明的目的是提供一种半金属配方刹车片中钢纤维改性的方法，此方法原料易得，操作简单，对刹车片配方中的钢纤维进行改性，提升了刹车片的热衰退、防锈蚀和磨损性能。
为了达到以上目的，本发明采用的技术方案为：一种半金属配方刹车片中钢纤维改性的方法,其特征在于包括以下步骤：
步骤一：在反应器里加入水、Na2CO3加热搅拌溶解，得到质量分数为3%-5%的Na2CO3溶液，再将钢纤维缓慢加入Na2CO3溶液中搅拌，使钢纤维完全浸入Na2CO3溶液，保持Na2CO3溶液温度35℃-45℃左右，浸泡10min-30min，待除去钢纤维表面的油脂后把钢纤维取出、沥干；
步骤二：将步骤一中除去表面油脂的钢纤维浸入到用水稀释80-100倍的食人鱼溶液15min-25min，其中食人鱼溶液是由稀释100倍浓硫酸和稀释10倍30%双氧水质量比为3-7:1配置的，然后取出钢纤维进行沥干；
步骤三：将偶联剂、醇、水、NaH2PO4 、酒石酸钠和柠檬酸放入反应容器中混匀得到偶联剂溶液，其中，偶联剂、醇、水、NaH2PO4 、酒石酸钠和柠檬酸质量比为5-10:40-60:30-50:1-4:1-2:0.2-1，用磷酸、硫酸或醋酸将溶液调节pH至2-5，其中醇为甲醇、乙醇或异丙醇，将步骤二中得到的钢纤维放入上述偶联剂溶液中进行水解，保持水解过程中温度为 20℃～40℃；具体步骤为搅拌10min-50min，再静止1-5h；取出钢纤维沥干，再将刚纤维浸入偶联剂溶液20min-40min后取出再次沥干；
步骤四：将步骤三中得到的钢纤维放入干燥箱中采用70℃-90℃干燥1h-3h，打散结团的钢纤维。
进一步地说，所述偶联剂包括硅烷偶联剂或钛酸酯偶联剂；所述硅烷偶联剂结构通式为YSiX3,其中Y为非水解基团，包括链烃基，及末端带有Cl、NH2、SH基团，X为可水解基团，包括Cl,OMe, OEt, OC2H4OCH3, OSiMe3, 及OAc等；所述钛酸酯类偶联剂结构通式为ROO(4-n)Ti(OX-R’Y)n，其中-OX可水解的短链烷氧基、羧基。
进一步地说，步骤一中所述得到的Na2CO3溶液质量分数为4%，再将钢纤维缓慢加入Na2CO3溶液中搅拌，使钢纤维完全浸入Na2CO3溶液，保持Na2CO3溶液温度40℃左右，浸泡20min，除去钢纤维表面的油脂后把钢纤维取出、沥干。
进一步地说，步骤二中将所述步骤一中除去表面油脂的钢纤维浸入到用水稀释90倍的食人鱼溶液20min，食人鱼溶液由稀酸和稀双氧水5:1配置的，然后取出钢纤维进行沥干。
进一步地说，步骤三中所述偶联剂溶液内的偶联剂、醇、水、NaH2PO4 、酒石酸钠和柠檬酸质量比为7:55:45:3:1:0.8，用磷酸、硫酸或醋酸将溶液调节pH至4，其中醇为甲醇、乙醇或异丙醇，将步骤三中得到的钢纤维放入上述偶联剂溶液中进行水解，水解温度为 25℃，搅拌35min后，静止3h；取出钢纤维沥干，再将刚纤维浸入偶联剂溶液25min后取出再次沥干。
进一步地说，步骤四中将所述步骤三中得到的钢纤维放入干燥箱中80℃干燥2h，打散结团的钢纤维。
本发明对钢纤维表面进行处理后，偶联剂水解后形成单体和钢纤维表面羟基发生反应促成单体和钢纤维有效连接，钢纤维表面形成一层膜。偶联剂是一种有机－无机杂化的双官能团化合物，与亲水的钢表面和疏水的有机粘结剂都会发生化学吸附或化学反应，形成比较牢固而耐久的分子键或化学键，在刹车片粘结剂树脂和钢纤维之间起着化学桥的作用。
钢纤维用Na2CO3溶液进行处理后，再用稀释的食人鱼溶液处理，加入到偶联剂溶液中。其中，酸可以使钢纤维表面羟基化，偶联剂首先要进行水解。其中硅烷偶联剂水解单体可和钢纤维表面含结晶水-OH羟基Fe或氢氧化铁发生下列反应在钢纤维表面形成稳定的膜结构。而钛酸酯偶联剂处理后可在钢纤维表面覆盖钛酸类膜。
X-R-Si（OH）3+Fe（OH）3→X-R-SiO3Fe+3H2O
使用偶联剂溶液对钢纤维进行处理前,用碳酸钠溶液对钢纤维进行碱洗,可以保留钢纤维表面的碱性羟基，以便水解后偶联剂单体反应。用稀释后食人鱼溶液进行处理，可在钢纤维表面实行羟基化，大部分硅烷或钛酸酯类偶联剂在pH=4时水解速度快而聚合速度慢，因此调节pH在3-4范围。
本发明的有益效果是：（1）本发明原料易得到，且操作简单，对刹车片配方中的钢纤维进行改性，提升了刹车片的热衰退、防锈蚀和磨损性能，且通过用偶联剂处理的钢纤维制备盘片刹车片N300做台架实验，发现处理后的钢纤维制备的刹车片磨损率降低50%左右，同时通过锈粘结试验对比发现偶联剂处理对刹车片防腐蚀作用明显，在半金属刹车片中应用前景十分广阔。
（2）本发明在偶联剂溶液中增加了柠檬酸和酒石酸钠，加入这两种化学试剂可稳定偶联溶液的pH，加快偶联的反应速度。酒石酸钠是一种络合剂, 能与溶液中的Fe3+络合, 控制沉渣生成量, 延长偶联剂使用寿命，且酒石酸属于有机弱酸, 和共轭碱组成缓冲溶液, 保持溶液pH值长时间稳定在一定范围, 稳定溶液酸度，促进偶联反应更快的进行。
（3）本发明还有使用到稀释的食人鱼溶液处理钢纤维可使其表面羟基化，增加钢纤维表面的羟基，和偶联剂结合的位点增加，实验效果表明，提高了钢纤维表面单位面积偶联剂密度，以此为原材料刹车片性能更优异。
具体实施方式
下面结合实施例对本发明作进一步说明。
实施例1：
步骤一：在反应器里加入水、Na2CO3加热搅拌溶解，得到200L的质量分数为4%的Na2CO3溶液，再将50kg钢纤维缓慢加入Na2CO3溶液中搅拌，使钢纤维完全浸入Na2CO3溶液，保持Na2CO3溶液温度40℃左右，浸泡15min，待除去钢纤维表面的油脂后把钢纤维取出、沥干；
步骤二：将步骤一中除去表面油脂的钢纤维浸泡到用水稀释90倍的200L食人鱼溶液20min，食人鱼溶液是由稀释100倍浓硫酸和稀释10倍数30%双氧水质量比为4:1配置的，然后取出钢纤维进行沥干；
步骤三：将硅烷偶联剂、无水乙醇、水、NaH2PO4 、酒石酸钠和柠檬酸放入反应容器中混匀得到100kg偶联剂溶液，其中，偶联剂、醇、水、NaH2PO4 、酒石酸钠和柠檬酸质量比为5:43:48.5:2:1:0.5，用磷酸、硫酸或醋酸将溶液调节pH至4，其中醇为甲醇、乙醇或异丙醇，将步骤二中得到的钢纤维放入上述偶联剂溶液中进行水解，保持水解温度为 30℃，搅拌30min，再静止5h；取出钢纤维沥干，再将刚纤维浸入偶联剂溶液40min后取出再次沥干；
步骤四：将步骤三中得到的钢纤维放入干燥箱中采用80℃干燥2h，打散结团的钢纤维。
把改性钢纤维作为原料制备金属刹车片。
按JASO C427-1983分别对实施例1制备五菱汽车盘片N300的半金属刹车片样件进行试验及评价，实施结果见表1。看到钢纤维改性后制备N300盘片进行磨损实验磨损厚度和质量大大降低。台架实验表明钢纤维硅烷偶联剂改性后可有效改善刹车片的磨损率，延长使用寿命。
表1 未改性和改性钢纤维制盘片N300磨损实验数据对比
                                                  
将制动器和制动盘实车状态下装配，将间隙调整到调整到设计状态0.2~0.4mm，全部浸入水中2 min. 取出后在制动器拉臂输入端施加1000N的拉力，保持96h后，用扭矩仪检测盘片与制动盘的脱开力矩。进行锈粘结试验。脱开力矩越小，表明刹车片耐锈蚀能力越强。测试得到钢纤维进行处理压制刹车片脱开力矩7N·m,钢纤维未经处理压制盘片脱开力矩为46N·m。通过刹车片锈粘结试验表明钢纤维用硅烷偶联剂进行处理后，对钢纤维能起有效的防腐蚀作用。
实施例2：
步骤一：在反应器里加入水、Na2CO3加热搅拌溶解，得到200L的质量分数为4%的Na2CO3溶液，再将50kg钢纤维缓慢加入Na2CO3溶液中搅拌，使钢纤维完全浸入Na2CO3溶液，保持Na2CO3溶液温度40℃左右，浸泡15min，待除去钢纤维表面的油脂后把钢纤维取出、沥干；
步骤二：将步骤一中除去表面油脂的钢纤维浸泡到用水稀释90倍的200L食人鱼溶液20min，食人鱼溶液是由稀释100倍浓硫酸和稀释10倍数30%双氧水质量比为4:1配置的，然后取出钢纤维进行沥干；
步骤三：将硅烷偶联剂、无水乙醇、水、NaH2PO4 、酒石酸钠和柠檬酸放入反应容器中混匀得到100kg偶联剂溶液，其中，偶联剂、醇、水、NaH2PO4 、酒石酸钠和柠檬酸质量比为5:50.5:41:2:1:0.5，用磷酸、硫酸或醋酸将溶液调节pH至4，其中醇为甲醇、乙醇或异丙醇，将步骤二中得到的钢纤维放入上述偶联剂溶液中进行水解，保持水解温度为 30℃，搅拌10min，再静止5h；取出钢纤维沥干，再将刚纤维浸入偶联剂溶液40min后取出再次沥干；
步骤四：将步骤三中得到的钢纤维放入干燥箱中采用80℃干燥2h，打散结团的钢纤维。
改性钢纤维作为原料制备半金属刹车片。同样磨损率减少达到50%。
表2  实施例2改性钢纤维制N300磨损实验数据
 
锈粘结试验测试得到例2方法钢纤维进行处理制得样品脱开力矩6N·m,钢纤维未经处理压制盘片脱开力矩为46N·m。同例1，处理后防锈作用有很大改善。
实施例3：
步骤一：在反应器里加入水、Na2CO3加热搅拌溶解，得到200L的质量分数为3%的Na2CO3溶液，再将50kg钢纤维缓慢加入Na2CO3溶液中搅拌，使钢纤维完全浸入Na2CO3溶液，保持Na2CO3溶液温度35℃左右，浸泡10min，待除去钢纤维表面的油脂后把钢纤维取出、沥干；
步骤二：将步骤一中除去表面油脂的钢纤维浸泡到用水稀释80倍的200L食人鱼溶液15min，食人鱼溶液是由稀释100倍浓硫酸和稀释10倍数30%双氧水质量比为3:1配置的，然后取出钢纤维进行沥干；
步骤三：将硅烷偶联剂、乙醇、甲醇、水、NaH2PO4 、酒石酸钠和柠檬酸放入反应容器中混匀得到100kg偶联剂溶液，其中，硅烷偶联剂、乙醇、甲醇、水、NaH2PO4 、酒石酸钠和柠檬酸质量比为5:30:13:48.5:2:1:0.5，用磷酸、硫酸或醋酸将溶液调节pH至2，其中醇为30份无水乙醇、13份无水甲醇，将步骤二中得到的钢纤维放入上述偶联剂溶液中进行水解，保持水解温度为 20℃，搅拌10min，再静止2h；取出钢纤维沥干，再将刚纤维浸入偶联剂溶液20min后取出再次沥干；
步骤四：将步骤三中得到的钢纤维放入干燥箱中采用70℃干燥1h，打散结团的钢纤维。
实施例4：
步骤一：在反应器里加入水、Na2CO3加热搅拌溶解，得到质量分数为5%的Na2CO3溶液，再将钢纤维缓慢加入Na2CO3溶液中搅拌，使钢纤维完全浸入Na2CO3溶液，保持Na2CO3溶液温度45℃左右，浸泡30min，待除去钢纤维表面的油脂后把钢纤维取出、沥干；
步骤二：将步骤一中除去表面油脂的钢纤维浸泡到用水稀释100倍的200L食人鱼溶液25min，食人鱼溶液是由稀释100倍浓硫酸和稀释10倍数30%双氧水质量比为7:1配置的，然后取出钢纤维进行沥干；
步骤三：将钛酸酯偶联剂、醇、水、NaH2PO4 、酒石酸钠和柠檬酸放入反应容器中混匀得到偶联剂溶液，其中，钛酸酯偶联剂、醇、水、NaH2PO4 、酒石酸钠和柠檬酸质量比为10:50:50:4:2:1，用磷酸、硫酸或醋酸将溶液调节pH至5，其中醇为甲醇、乙醇或异丙醇，将步骤二中得到的钢纤维放入上述偶联剂溶液中进行水解，保持水解温度为 40℃，搅拌50min，再静止5h；取出钢纤维沥干，再将刚纤维浸入偶联剂溶液40min后取出再次沥干；
步骤四：将步骤三中得到的钢纤维放入干燥箱中采用90℃干燥3h，打散结团的钢纤维。

Claims (6)

1.一种半金属配方刹车片中钢纤维改性的方法,其特征在于包括以下步骤：
步骤一：在反应器里加入水、Na2CO3加热搅拌溶解，得到质量分数为3%-5%的Na2CO3溶液，再将钢纤维缓慢加入Na2CO3溶液中搅拌，使钢纤维完全浸入Na2CO3溶液，保持Na2CO3溶液温度35℃-45℃左右，浸泡10min-30min，待除去钢纤维表面的油脂后把钢纤维取出、沥干；
步骤二：将步骤一中除去表面油脂的钢纤维浸入到用水稀释80-100倍的食人鱼溶液15min-25min，其中食人鱼溶液是由稀释100倍浓硫酸和稀释10倍30%双氧水质量比为3-7:1配置的，然后取出钢纤维进行沥干；
步骤三：将偶联剂、醇、水、NaH2PO4 、酒石酸钠和柠檬酸放入反应容器中混匀得到偶联剂溶液，其中，偶联剂、醇、水、NaH2PO4 、酒石酸钠和柠檬酸质量比为5-10:40-60:30-50:1-4:1-2:0.2-1，用磷酸、硫酸或醋酸将溶液调节pH至2-5，其中醇为甲醇、乙醇或异丙醇，将步骤二中得到的钢纤维放入上述偶联剂溶液中进行水解，保持水解过程中温度为 20℃～40℃；具体步骤为搅拌10min-50min，再静止1-5h；取出钢纤维沥干，再将刚纤维浸入偶联剂溶液20min-40min后取出再次沥干；
步骤四：将步骤三中得到的钢纤维放入干燥箱中采用70℃-90℃干燥1h-3h，打散结团的钢纤维。
2.根据权利要求1一种半金属配方刹车片中钢纤维改性的方法,其特征在于，所述偶联剂包括硅烷偶联剂或钛酸酯偶联剂；所述硅烷偶联剂结构通式为YSiX3,其中Y为非水解基团，包括链烃基，及末端带有Cl、NH2、SH基团，X为可水解基团，包括Cl,OMe, OEt, OC2H4OCH3, OSiMe3, 及OAc等；所述钛酸酯类偶联剂结构通式为ROO(4-n)Ti(OX-R’Y)n，其中-OX可水解的短链烷氧基、羧基。
3.根据权利要求1或2所述的任意一种半金属配方刹车片中钢纤维改性的方法,其特征在于，步骤一中所述得到的Na2CO3溶液质量分数为4%，再将钢纤维缓慢加入Na2CO3溶液中搅拌，使钢纤维完全浸入Na2CO3溶液，保持Na2CO3溶液温度40℃左右，浸泡20min，除去钢纤维表面的油脂后把钢纤维取出、沥干。
4.根据权利要求1或2所述的任意一种半金属配方刹车片中钢纤维改性的方法,其特征在于，步骤二中将所述步骤一中除去表面油脂的钢纤维浸入到用水稀释90倍的食人鱼溶液20min，食人鱼溶液由稀释100倍浓硫酸和稀释10倍30%双氧水质量比5:1配置，然后取出钢纤维进行沥干。
5.根据权利要求1或2所述的任意一种半金属配方刹车片中钢纤维改性的方法,其特征在于，步骤三中所述偶联剂溶液内的偶联剂、醇、水、NaH2PO4 、酒石酸钠和柠檬酸质量比为7:55:45:3:1:0.8，用磷酸、硫酸或醋酸将溶液调节pH至4，其中醇为甲醇、乙醇或异丙醇，将步骤三中得到的钢纤维放入上述偶联剂溶液中进行水解，水解温度为 25℃，搅拌35min后，静止3h；取出钢纤维沥干，再将刚纤维浸入偶联剂溶液25min后取出再次沥干。
6.根据权利要求1或2所述的任意一种半金属配方刹车片中钢纤维改性的方法,其特征在于，步骤四中将所述步骤三中得到的钢纤维放入干燥箱中80℃干燥2h，打散结团的钢纤维。
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