CN105602682A - 一种汽车制动液及其制备方法 - Google Patents

一种汽车制动液及其制备方法 Download PDF

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CN105602682A
CN105602682A CN201510954958.9A CN201510954958A CN105602682A CN 105602682 A CN105602682 A CN 105602682A CN 201510954958 A CN201510954958 A CN 201510954958A CN 105602682 A CN105602682 A CN 105602682A
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刘文军
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CHANGCHUN DELIAN CHEMICAL Co Ltd
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Abstract

本发明公开了一种汽车制动液,按照重量份的原料组成如下:二乙二醇丁醚40-60份、丙二醇15-30份、聚乙二醇单醚25-35份、硼酸5-8份、苯并三氮唑0.03-0.12份、二烷基二硫代氨基甲酸锌0.05-0.10份、抗氧剂264?0.13-0.18份、三乙醇胺0.05-0.08份、硼砂0.15-0.25份和PH调节剂1.2-2.6份。本发明还提供了汽车制动液的制备方法。本发明汽车制动液通过苯并三氮唑、二烷基二硫代氨基甲酸锌和抗氧剂264配合,能够明显的提高汽车制动液的抗氧化性能,符合GB?12981质量指标,且表现优异。该汽车制动液的高温抗气阻性、抗腐蚀性、高温稳定性、化学稳定性以及蒸发损失等均达到了HZY5的标准。

Description

一种汽车制动液及其制备方法
技术领域
本发明涉及精细化工汽车化学品领域,具体是一种汽车制动液及其制备方法。
背景技术
汽车制动液是汽车液压式制动系统中用来传递制动能量的功能性液体,其性能及质量状况直接关系到车辆的行驶安全。自从20世纪30年代初汽车开始使用制动液以来,汽车制动液可以按照其生产原料的不同分为三种类型:蓖麻油-醇型、矿物油型和合成型制动液。蓖麻油-醇型、矿物油型制动液因其沸点低,凝固点高逐渐被淘汰,合成型制动液被广泛使用。
合成型制动液又分为硅油型、醇醚型和硼酸酯型。随着汽车工业的发展和人们对安全越来越高度的重视,ABS防抱死制动装置在制动系统中得到广泛的应用,必须研发具有高的干湿沸点和低的低温运动粘度的高级制动液,以更好地适应ABS防抱死刹车系统。此外,由于硼酸酯型制动液具备优异的高低温性能、高性价比以及与醇醚型制动液较好的相容性,特别适用一些高性能车辆和在极端温度环境下的应用,如大型工程机械车辆、赛车、南极考察、高温热带地区等。
国家对汽车制动液的质量有严格的要求(GB+12981-2003),其主要涉及到制动液的高温抗气阻性、低温流动性、对橡胶的溶胀性、抗金属腐蚀性、抗氧化性、稳定性等。标准中DOT4要求ERBP不小于230℃,WERBP不小于155℃,-40℃时运动粘度不大于1800。目前,国内汽车配件市场中出售的汽车制动液大部分是不合格产品,其主要的问题是对制动系统腐蚀严重、对橡胶有溶胀性、质量蒸发损失不达标,从而导致汽车制动存在不安全隐患、维修频繁、维修费增加等;另外其高温抗气阻性和低温流动性不能满足要求,而受到气候条件及季节的限制。随着硼酸酯合成技术的不断完善,汽车制动液高温性能和低温性能得到了大的改进,但仍存在对制动系统的腐蚀、抗氧化性差不达标等问题。
发明内容
本发明的目的在于提供一种汽车制动液及其制备方法,以解决上述背景技术中提出的问题。
为实现上述目的,本发明提供如下技术方案:
一种汽车制动液,按照重量份的原料组成如下:二乙二醇丁醚40-60份、丙二醇15-30份、聚乙二醇单醚25-35份、硼酸5-8份、苯并三氮唑0.03-0.12份、二烷基二硫代氨基甲酸锌0.05-0.10份、抗氧剂2640.13-0.18份、三乙醇胺0.05-0.08份、硼砂0.15-0.25份和PH调节剂1.2-2.6份。
作为本发明进一步的方案:按照重量份的原料组成如下:二乙二醇丁醚45-55份、丙二醇20-25份、聚乙二醇单醚28-32份、硼酸6-8份、苯并三氮唑0.05-0.10份、二烷基二硫代氨基甲酸锌0.06-0.08份、抗氧剂2640.15-0.17份、三乙醇胺0.06-0.07份、硼砂0.18-0.23份和PH调节剂1.4-2.3份。
作为本发明再进一步的方案:按照重量份的原料组成如下:二乙二醇丁醚50份、丙二醇23份、聚乙二醇单醚30份、硼酸7份、苯并三氮唑0.08份、二烷基二硫代氨基甲酸锌0.07份、抗氧剂2640.16份、三乙醇胺0.07份、硼砂0.21份和PH调节剂1.6份。
作为本发明再进一步的方案:所述聚乙二醇单醚的化学式为HO(CH2CH2O)nCmH2m+1,式中n=2~4,m=1~4,CmH2m+1为直链或支链烷基。
作为本发明再进一步的方案:所述PH调节剂为丁基二乙醇胺。
所述汽车制动液的制备方法,步骤如下:
1)称取二乙二醇丁醚、丙二醇、聚乙二醇单醚和硼酸,加入至反应釜内,开启真空泵,使反应釜内的压力控制在0.005-0.018MPa,在85-90℃下搅拌保温1-2h,抽出反应生成的水,继续升温至125-138℃,并搅拌反应0.5-1h,测试水分含量,若水分含量大于0.1%,则加热真空脱水,直至水分含量小于0.1%,获得基础溶液;
2)经基础溶液降温至50-70℃,称取并加入硼酸、苯并三氮唑、二烷基二硫代氨基甲酸锌、抗氧剂264、三乙醇胺和硼砂,搅拌1-2h后,获得第一溶液;
3)将第一溶液冷却至室温,加入PH调节剂调节PH至7-9,获得第二溶液;
4)将第二溶液过滤,获得该汽车制动液。
与现有技术相比,本发明的有益效果是:1、本发明汽车制动液通过苯并三氮唑、二烷基二硫代氨基甲酸锌和抗氧剂264配合,能够明显的提高汽车制动液的抗氧化性能,在抗氧化性试验中,铸铁的质量变化为0.01-0.06mg/cm2,铝的质量变化为0.00-0.02mg/cm2,符合GB12981质量指标,且表现优异。2、本发明汽车制动液的高温抗气阻性、抗腐蚀性、高温稳定性、化学稳定性以及蒸发损失等均达到了HZY5的标准。
具体实施方式
下面结合具体实施方式对本发明的技术方案作进一步详细地说明。
聚乙二醇单醚的化学式为HO(CH2CH2O)nCmH2m+1,式中n=2~4,m=1~4,CmH2m+1为直链或支链烷基。
实施例1
一种汽车制动液,按照重量份的原料组成如下:二乙二醇丁醚40份、丙二醇15份、聚乙二醇单醚25份、硼酸5份、苯并三氮唑0.03份、二烷基二硫代氨基甲酸锌0.05份、抗氧剂2640.13份、三乙醇胺0.05份、硼砂0.15份和丁基二乙醇胺1.2份。
本实施例中所述汽车制动液的制备方法,步骤如下:
1)称取二乙二醇丁醚、丙二醇、聚乙二醇单醚和硼酸,加入至反应釜内,开启真空泵,使反应釜内的压力控制在0.005MPa,在85℃下搅拌保温1h,抽出反应生成的水,继续升温至125℃,并搅拌反应0.5h,测试水分含量,若水分含量大于0.1%,则加热真空脱水,直至水分含量小于0.1%,获得基础溶液;
2)经基础溶液降温至50℃,称取并加入硼酸、苯并三氮唑、二烷基二硫代氨基甲酸锌、抗氧剂264、三乙醇胺和硼砂,搅拌1h后,获得第一溶液;
3)将第一溶液冷却至室温,加入丁基二乙醇胺调节PH至7,获得第二溶液;
4)将第二溶液过滤,获得该汽车制动液。
实施例2
一种汽车制动液,按照重量份的原料组成如下:二乙二醇丁醚60份、丙二醇30份、聚乙二醇单醚35份、硼酸8份、苯并三氮唑0.12份、二烷基二硫代氨基甲酸锌0.10份、抗氧剂2640.18份、三乙醇胺0.08份、硼砂0.25份和丁基二乙醇胺2.6份。
本实施例中所述汽车制动液的制备方法,步骤如下:
1)称取二乙二醇丁醚、丙二醇、聚乙二醇单醚和硼酸,加入至反应釜内,开启真空泵,使反应釜内的压力控制在0.018MPa,在90℃下搅拌保温2h,抽出反应生成的水,继续升温至138℃,并搅拌反应1h,测试水分含量,若水分含量大于0.1%,则加热真空脱水,直至水分含量小于0.1%,获得基础溶液;
2)经基础溶液降温至70℃,称取并加入硼酸、苯并三氮唑、二烷基二硫代氨基甲酸锌、抗氧剂264、三乙醇胺和硼砂,搅拌2h后,获得第一溶液;
3)将第一溶液冷却至室温,加入丁基二乙醇胺调节PH至9,获得第二溶液;
4)将第二溶液过滤,获得该汽车制动液。
实施例3
一种汽车制动液,按照重量份的原料组成如下:二乙二醇丁醚50份、丙二醇23份、聚乙二醇单醚30份、硼酸7份、苯并三氮唑0.08份、二烷基二硫代氨基甲酸锌0.07份、抗氧剂2640.16份、三乙醇胺0.07份、硼砂0.21份和丁基二乙醇胺1.6份。
本实施例中所述汽车制动液的制备方法,步骤如下:
1)称取二乙二醇丁醚、丙二醇、聚乙二醇单醚和硼酸,加入至反应釜内,开启真空泵,使反应釜内的压力控制在0.01MPa,在88℃下搅拌保温1.5h,抽出反应生成的水,继续升温至130℃,并搅拌反应1h,测试水分含量,若水分含量大于0.1%,则加热真空脱水,直至水分含量小于0.1%,获得基础溶液;
2)经基础溶液降温至60℃,称取并加入硼酸、苯并三氮唑、二烷基二硫代氨基甲酸锌、抗氧剂264、三乙醇胺和硼砂,搅拌1.5h后,获得第一溶液;
3)将第一溶液冷却至室温,加入丁基二乙醇胺调节PH至8,获得第二溶液;
4)将第二溶液过滤,获得该汽车制动液。
实施例4
一种汽车制动液,按照重量份的原料组成如下:二乙二醇丁醚60份、丙二醇15份、聚乙二醇单醚20份、硼酸8份、苯并三氮唑0.06份、二烷基二硫代氨基甲酸锌0.10份、抗氧剂2640.14份、三乙醇胺0.06份、硼砂0.25份和丁基二乙醇胺1.4份。
本实施例中所述汽车制动液的制备方法,步骤如下:
1)称取二乙二醇丁醚、丙二醇、聚乙二醇单醚和硼酸,加入至反应釜内,开启真空泵,使反应釜内的压力控制在0.013MPa,在86℃下搅拌保温1h,抽出反应生成的水,继续升温至128℃,并搅拌反应0.5h,测试水分含量,若水分含量大于0.1%,则加热真空脱水,直至水分含量小于0.1%,获得基础溶液;
2)经基础溶液降温至70℃,称取并加入硼酸、苯并三氮唑、二烷基二硫代氨基甲酸锌、抗氧剂264、三乙醇胺和硼砂,搅拌1.5h后,获得第一溶液;
3)将第一溶液冷却至室温,加入丁基二乙醇胺调节PH至7,获得第二溶液;
4)将第二溶液过滤,获得该汽车制动液。
实施例5
一种汽车制动液,按照重量份的原料组成如下:二乙二醇丁醚47份、丙二醇19份、聚乙二醇单醚26份、硼酸8份、苯并三氮唑0.12份、二烷基二硫代氨基甲酸锌0.05-0.10份、抗氧剂2640.18份、三乙醇胺0.05份、硼砂0.2份和丁基二乙醇胺1.6份。
本实施例中所述汽车制动液的制备方法,步骤如下:
1)称取二乙二醇丁醚、丙二醇、聚乙二醇单醚和硼酸,加入至反应釜内,开启真空泵,使反应釜内的压力控制在0.012MPa,在85-90℃下搅拌保温1h,抽出反应生成的水,继续升温至128℃,并搅拌反应0.5h,测试水分含量,若水分含量大于0.1%,则加热真空脱水,直至水分含量小于0.1%,获得基础溶液;
2)经基础溶液降温至55℃,称取并加入硼酸、苯并三氮唑、二烷基二硫代氨基甲酸锌、抗氧剂264、三乙醇胺和硼砂,搅拌1h后,获得第一溶液;
3)将第一溶液冷却至室温,加入丁基二乙醇胺调节PH至8,获得第二溶液;
4)将第二溶液过滤,获得该汽车制动液。
对比例1
请参阅实施例3,与实施例3相比,不含苯并三氮唑、二烷基二硫代氨基甲酸锌和抗氧剂264,其他与实施例3相同。
对比例2
请参阅实施例3,与实施例3相比,不含苯并三氮唑和二烷基二硫代氨基甲酸锌,其他与实施例3相同。
对比例3
请参阅实施例3,与实施例3相比,不含抗氧剂264,其他与实施例3相同。
性能实验
对实施例1-5和对比例1-3按照GB12981进行抗氧化性试验,实验结果如表1所示。
表1抗氧化性试验结果
从表1可以看出,本发明汽车制动液的抗氧化性试验中,铸铁的质量变化为0.01-0.06mg/cm2,铝的质量变化为0.00-0.02mg/cm2,符合GB12981质量指标,且表现优异。
将实施例3与对比例1-3的试验结果进行对比,对比例1中不含苯并三氮唑、二烷基二硫代氨基甲酸锌和抗氧剂264,其抗氧化性达不到GB12981质量指标,对比例2中仅含有抗氧剂264,对比例3中仅含有苯并三氮唑和二烷基二硫代氨基甲酸锌,对比例2和对比例3的抗氧化性虽然达到了GB12981质量指标,但表现一般,实施例3中同时含苯并三氮唑、二烷基二硫代氨基甲酸锌和抗氧剂264,其抗氧化性达到了GB12981质量指标,且表现优异。因此可以看出,苯并三氮唑、二烷基二硫代氨基甲酸锌和抗氧剂264配合,能够明显的提高汽车制动液的抗氧化性能。
抽取本发明实施例3的汽车制动液的样品,按照GB12981进行其他性能检测,检测结果如表2所示。
表2GB12981性能检测结果
本发明汽车制动液的样品达到HZY5标准,性能优异。
上面对本发明的较佳实施方式作了详细说明,但是本发明并不限于上述实施方式,在本领域的普通技术人员所具备的知识范围内,还可以在不脱离本发明宗旨的前提下作出各种变化。

Claims (6)

1.一种汽车制动液,其特征在于,按照重量份的原料组成如下:二乙二醇丁醚40-60份、丙二醇15-30份、聚乙二醇单醚25-35份、硼酸5-8份、苯并三氮唑0.03-0.12份、二烷基二硫代氨基甲酸锌0.05-0.10份、抗氧剂2640.13-0.18份、三乙醇胺0.05-0.08份、硼砂0.15-0.25份和PH调节剂1.2-2.6份。
2.根据权利要求1所述的汽车制动液,其特征在于,按照重量份的原料组成如下:二乙二醇丁醚45-55份、丙二醇20-25份、聚乙二醇单醚28-32份、硼酸6-8份、苯并三氮唑0.05-0.10份、二烷基二硫代氨基甲酸锌0.06-0.08份、抗氧剂2640.15-0.17份、三乙醇胺0.06-0.07份、硼砂0.18-0.23份和PH调节剂1.4-2.3份。
3.根据权利要求2所述的汽车制动液,其特征在于,按照重量份的原料组成如下:二乙二醇丁醚50份、丙二醇23份、聚乙二醇单醚30份、硼酸7份、苯并三氮唑0.08份、二烷基二硫代氨基甲酸锌0.07份、抗氧剂2640.16份、三乙醇胺0.07份、硼砂0.21份和PH调节剂1.6份。
4.根据权利要求1或2或3所述的汽车制动液,其特征在于,所述聚乙二醇单醚的化学式为HO(CH2CH2O)nCmH2m+1,式中n=2~4,m=1~4,CmH2m+1为直链或支链烷基。
5.根据权利要求4所述的汽车制动液,其特征在于,所述PH调节剂为丁基二乙醇胺。
6.一种如权利要求1-5任一所述的汽车制动液的制备方法,其特征在于,步骤如下:
1)称取二乙二醇丁醚、丙二醇、聚乙二醇单醚和硼酸,加入至反应釜内,开启真空泵,使反应釜内的压力控制在0.005-0.018MPa,在85-90℃下搅拌保温1-2h,抽出反应生成的水,继续升温至125-138℃,并搅拌反应0.5-1h,测试水分含量,若水分含量大于0.1%,则加热真空脱水,直至水分含量小于0.1%,获得基础溶液;
2)经基础溶液降温至50-70℃,称取并加入硼酸、苯并三氮唑、二烷基二硫代氨基甲酸锌、抗氧剂264、三乙醇胺和硼砂,搅拌1-2h后,获得第一溶液;
3)将第一溶液冷却至室温,加入PH调节剂调节PH至7-9,获得第二溶液;
4)将第二溶液过滤,获得该汽车制动液。
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