CN115418261B - 一种含聚合物的光纤防腐润滑脂及其制备方法 - Google Patents

一种含聚合物的光纤防腐润滑脂及其制备方法 Download PDF

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CN115418261B
CN115418261B CN202211167015.8A CN202211167015A CN115418261B CN 115418261 B CN115418261 B CN 115418261B CN 202211167015 A CN202211167015 A CN 202211167015A CN 115418261 B CN115418261 B CN 115418261B
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罗海棠
谢龙
凡明锦
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Baoji University of Arts and Sciences
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Abstract

本发明公开了一种含聚合物的光纤防腐润滑脂及其制备方法,属于润滑脂技术领域。所述润滑脂由下述重量份数的组分组成:合成基础油70‑85份;气相二氧化硅5‑15份,聚合物3‑10份;抗磨剂1‑5份,防锈剂0.5‑2份,抗氧剂0.5‑2份;经分散、高温膨化、调和等工艺制备成一种高滴点长寿命的光纤防腐润滑脂。本发明简化了加工工艺;制备过程绿色化;所得润滑脂的使用温度范围宽,适用温度‑50‑300℃;并且具有优异的抗磨、抗水、防锈性能,降低设备使用时造成的断裂、腐蚀等风险,显著延长了光纤的使用寿命。

Description

一种含聚合物的光纤防腐润滑脂及其制备方法
技术领域
本发明属于润滑脂技术领域,具体而言,涉及一种含聚合物的光纤防腐润滑脂及其制备方法。
背景技术
随着现代工业的迅速发展,工业生产部门对润滑脂的耐高温、极压、抗磨、抗水、防护、轴承寿命等多方面的性能都提出了日益严格的要求。目前润滑脂发展的总趋势是多效能、高滴点,以适应现代机械部件的润滑要求。
光纤是由一根根的玻璃或纤维制作而成的纤维线,用于传送光信号。用几层保护层包裹着一束光纤,外面再用胶皮保护,就形成了光缆。光缆都非常长,需要弯曲盘起来以便运输。然而,纤芯是玻璃制作,质地脆,容易断裂。玻璃丝断裂的主要原因是在弯曲的时候,玻璃丝受到了应力。因此,只要能减轻玻璃丝的应力,就可以大幅度降低玻璃丝断裂的可能性。光纤润滑脂是一种在光纤光缆中使用的专用润滑脂,可以减少玻璃丝的应力,保护光纤不被折断。
目前,现有的光纤润滑脂在运行过程中接触电阻和温升较大,产品的抗磨性能差,产品的使用寿命较短。另外,现有的光纤润滑脂的高、低温性能较差,在高温时易氧化、结碳,而在低温时不流动,不能起到很好的润滑作用。除此之外,光缆的防腐性能和耐磨损性能差,导致在户外进行长时间的使用时会使光缆出现腐蚀和磨损,造成光缆内部的光纤损坏,从而影响传输效果。
发明内容
鉴于现有技术存在的问题,本发明的目的在于提供一种含聚合物的光纤防腐润滑脂,其具有优异的抗磨、抗水、防锈性能,可降低运输或使用时造成的光纤断裂、腐蚀等风险,显著延长光纤的使用寿命,可应用于各类光纤的润滑与防腐。
为实现上述技术目的,本发明人结合市场上使用的润滑脂产品以及润滑脂的使用工况条件,针对光纤独特的润滑方式并通过大量试验探索和研究,最终在制备润滑脂时选用气相二氧化硅作为稠化剂,并加入一些性能优良的聚合物和特殊结构的抗氧剂和抗磨剂,从而增强其胶体结构的稳定性、成膜能力和润滑性能,延长设备的使用寿命,节约能源,以致提高国内外润滑脂水平。
具体地,本发明的目的是通过如下技术方案实现的:一种光纤防腐润滑脂,由下述重量份数的组分制备而成:
所述的聚合物选自如下的一种或两种以上:聚异丁烯、聚丙烯、乙丙胶、聚甲基丙烯酸甲酯、氯磺化聚乙烯、环氧树脂;所述的聚合物优选为聚丙烯、氯磺化聚乙烯橡胶和环氧树脂。
进一步优选地,如上所述的光纤防腐润滑脂,其中的基础油为合成基础油聚α烯烃;所述的聚α烯烃可以是不同粘度等级的PAO,具体选自如下的一种或两种以上:PAO10、PAO25、PAO40、PAO100、PAO150、PAO300。
进一步优选地,如上所述的光纤防腐润滑脂,其中的气相二氧化硅作为无机稠化剂,其为白色疏松粉末,粒径为20~200nm,比表面积为200-503m2/g,其制备方法如下:
1)将体积分数95-98%的乙醇水溶液采用浓氨水调pH=9-10,升温至50-60℃,搅拌均匀;
2)将体积分数15-18%的正硅酸乙酯乙醇溶液按照1:(1.8-2.5)的体积比加入步骤1)配制的溶液中,在50-60℃下恒温反应6-7h,得到硅溶胶溶液;
3)加入50-70%体积的去离子水,搅拌,再滴加盐酸溶液,中和至中性,静置;
4)8500-9500r/min离心,乙醇洗涤,在40-50℃下真空干燥,得到气相二氧化硅白色粉末。
进一步优选地,如上所述的光纤防腐润滑脂,其中的抗磨剂选自如下的一种或两种以上:硫代磷酸锌盐、硫代氨基甲酸钼盐、硫代磷酸酯铵盐、硼酸盐、硼酸酯、噻二唑或噻二唑衍生物。
再进一步优选地,如上所述的光纤防腐润滑脂,其中的硫代磷酸锌盐是硫磷双辛基碱性锌盐T203;所述的硫代氨基甲酸钼盐是二异辛基二硫代氨基甲酸钼;所述的硫代磷酸酯铵盐为T307;所述的硼酸盐为T361;所述的噻二唑衍生物为噻二唑二聚体。
进一步优选地,如上所述的光纤防腐润滑脂,其中的防锈剂选自如下的一种或两种以上:磺酸盐类、羧酸,酸酐及其皂类、环烷酸锌、单油酸酯、羊毛脂、噻二唑类、苯并三氮唑类。
再进一步优选地,如上所述的光纤防腐润滑脂,其中的磺酸盐类为磺酸钡;所述的羧酸,酸酐及其皂类为十二烯基丁二酸酐。
进一步优选地,如上所述的光纤防腐润滑脂,其中的抗氧剂选自如下的一种或两种以上:二芳基仲胺、N-苯基苯胺、烷基二苯胺、对苯二胺、苯酚,2,4-二叔丁基苯酚,2,6-二叔丁基苯酚。
另外,本发明还提供了一种上述光纤防腐润滑脂的制备方法,该方法包括如下步骤:
(1)将基础油在搅拌下加热至70-80℃,加入气相二氧化硅,继续搅拌直至混匀;
(2)升温至90~100℃进行膨化,膨化时间为60~90min;
(3)膨化结束后用三辊研磨机研磨,然后保持在80~100℃的温度下,加入聚合物、抗磨剂、防锈剂和抗氧剂,搅拌后进行均质处理,得到光纤防腐润滑脂。
进一步优选地,如上所述光纤防腐润滑脂的制备方法,其步骤(3)研磨后保持在80~90℃的温度下,加入聚合物、抗磨剂、防锈剂和抗氧剂。
与现有技术比,本发明提供了一种光纤用防腐润滑脂,采用合成基础油、稠化剂气相二氧化硅,调配各类功能添加剂,经过分散、稠化、膨化、调和等工艺制备,其优异性能表述如下:
(1)基础油是合成基础油PAO,其高低温性能优良;稠化剂为气相二氧化硅,其耐高温性能、抗水性能优良;所制备的润滑脂的使用温度范围宽,适用温度-50-300℃。既耐高温又具有耐低温性能。
(2)制备过程绿色化和简单化,本发明不使用易挥发性物质,避免了环境污染和对操作人员的伤害,整个过程绿色环保;同时,制备过程简单可靠,只需升温与降温,不需要皂化。
(3)气相二氧化硅润滑脂的防锈性能非常好,再加入一些抗磨、抗氧化、防锈添加剂,其抗磨性能进一步升级,能显著延长光纤的使用寿命,从而降低使用成本。
附图说明
图1:气相二氧化硅的SEM图。
图2:不同聚合物对防腐润滑脂的高温黏附性能影响。
具体实施方式
下面结合具体实施例对本发明进行详细说明。以下实施例将有助于本领域的技术人员进一步理解本发明,但不以任何形式限制本发明。应当指出的是,对本领域的普通技术人员来说,在不脱离本发明构思的前提下,还可以做出若干变形和改进。这些都属于本发明的保护范围。
需要的说明的是,以下实施例中采用的气相二氧化硅,其为白色疏松粉末,粒径20~200nm,比表面积为300-503m2/g,SEM图如图1所示。其制备步骤为:
1)依次在反应釜中加入220mL无水乙醇、15.6mL浓氨水(质量浓度为25%)、3.2mL去离子水;
2)升温至50-60℃,搅拌均匀;
3)往以上釜中加入以下混合溶液:20mL正硅酸乙酯溶于100mL乙醇;
4)在以上温度下恒温反应6-7h,得到硅溶胶溶液;
5)加入200mL去离子水,搅拌,再滴加适量的盐酸溶液,中和至中性,静置;
6)高速离心(转速为9000r/min),乙醇洗涤,在40-50℃下真空干燥,得到气相二氧化硅白色粉末。
实施例1
一种光纤防腐润滑脂,通过以下步骤制备所得:
S1、按重量份称取:PAO4082份、气相二氧化硅9份、聚丙烯5份、硫磷双辛基碱性锌盐T2032份、磺酸钡1份、N-苯基苯胺1份;
S2、将PAO40作为基础油;
S3、将82份的PAO40基础油投入反应釜中,搅拌加热至70~80℃,投入9份的气相二氧化硅,搅拌均匀;
S4、升温至90~100℃膨化,膨化时间为60~90min;
S5、膨化结束后进行三辊研磨机进行研磨,即制得润滑脂半成品;
S6、按GB5017-85试验方法测定润滑脂的1/4锥入度,采用GB270方法测定润滑脂滴点,采用GB3142-82四球机试验方法测定润滑脂的PB值和PD值;测试合格后进行后续步骤;
S7、把测试合格的润滑脂半成品保持在80~90℃,加入聚合物、抗磨剂、防锈剂和抗氧剂,搅拌后进行均质处理,既得光纤用防腐润滑脂。其各项典型理化指标测定结果见表1。
实施例2
一种光纤防腐润滑脂,按重量份计:其配方组成为:PAO10083份、气相二氧化硅11份、乙丙胶3份、噻二唑二聚体1份、十二烯基丁二酸酐1份、N-苯基苯胺1份。制备工艺同实施例1。
实施例3
一种光纤防腐润滑脂,按重量份计:其配方组成为:PAO25与PAO150(质量比为1:2)84份、气相二氧化硅10份、环氧树脂3份、噻二唑二聚体1份、环烷酸锌1份、烷基二苯胺1份。制备工艺同实施例1。
实施例4
一种光纤防腐润滑脂,按重量份计:其配方组成为:PAO10083份、气相二氧化硅10份、乙丙胶3份、硫磷双辛基碱性锌盐T2032份、十二烯基丁二酸酐1份、N-苯基苯胺1份。制备工艺同实施例1。
实施例5
一种光纤防腐润滑脂,按重量份计:其配方组成为:PAO10与PAO150(质量比为1:3)82份、气相二氧化硅11份、氯磺化聚乙烯3份、噻二唑二聚体1份、磺酸钡1.5份、烷基二苯胺0.5份。制备工艺同实施例1。
对比例1:12-羟基硬脂酸锂皂代替气相二氧化硅作为稠化剂
一种光纤防腐润滑脂,通过以下步骤制备所得:
S1、按重量份称取:PAO4082份、12-羟基硬脂酸锂皂9份、聚丙烯5份、硫磷双辛基碱性锌盐T2032份、磺酸钡1份、N-苯基苯胺1份;
S2、将PAO40作为基础油;
S3、将82份的PAO40基础油投入反应釜中,搅拌加热至70~80℃,投入9份的12-羟基硬脂酸锂皂,搅拌均匀;
S4、升温至180~200℃膨化,膨化时间为30~60min;
S5、膨化结束后进行三辊研磨机进行研磨,即制得润滑脂半成品;
S6、按GB5017-85试验方法测定润滑脂的1/4锥入度,采用GB270方法测定润滑脂滴点,采用GB3142-82四球机试验方法测定润滑脂的PB值和PD值;测试合格后进行后续步骤;
S7、把测试合格的润滑脂半成品保持在80~90℃,加入聚合物、抗磨剂、防锈剂和抗氧剂,搅拌后进行均质处理,既得光纤用防腐润滑脂。其各项典型理化指标测定结果见表1。
对比例2:150BS代替PAO作为基础油
一种光纤防腐润滑脂,通过以下步骤制备所得:
S1、按重量份称取:150BS82份、气相二氧化硅9份、聚丙烯5份、硫磷双辛基碱性锌盐T2032份、磺酸钡1份、N-苯基苯胺1份;
S2、将150BS作为基础油;
S3、将82份的150BS基础油投入反应釜中,搅拌加热至70~80℃,投入9份的气相二氧化硅,搅拌均匀;
S4、升温至90~100℃膨化,膨化时间为60~90min;
S5、膨化结束后进行三辊研磨机进行研磨,即制得润滑脂半成品;
S6、按GB5017-85试验方法测定润滑脂的1/4锥入度,采用GB270方法测定润滑脂滴点,采用GB3142-82四球机试验方法测定润滑脂的PB值和PD值;测试合格后进行后续步骤;
S7、把测试合格的润滑脂半成品保持在80~90℃,加入聚合物、抗磨剂、防锈剂和抗氧剂,搅拌后进行均质处理,既得光纤用防腐润滑脂。其各项典型理化指标测定结果见表1。
对比例3:聚合物选用聚氯乙烯
一种光纤防腐润滑脂,通过以下步骤制备所得:
S1、按重量份称取:PAO4082份、气相二氧化硅9份、聚氯乙烯5份、硫磷双辛基碱性锌盐T2032份、磺酸钡1份、N-苯基苯胺1份;
S2、将PAO40作为基础油;
S3、将82份的PAO40基础油投入反应釜中,搅拌加热至70~80℃,投入9份的气相二氧化硅,搅拌均匀;
S4、升温至90~100℃膨化,膨化时间为60~90min;
S5、膨化结束后进行三辊研磨机进行研磨,即制得润滑脂半成品;
S6、按GB5017-85试验方法测定润滑脂的1/4锥入度,采用GB270方法测定润滑脂滴点,采用GB3142-82四球机试验方法测定润滑脂的PB值和PD值;测试合格后进行后续步骤;
S7、把测试合格的润滑脂半成品保持在80~90℃,加入聚合物、抗磨剂、防锈剂和抗氧剂,搅拌后进行均质处理,既得光纤用防腐润滑脂。其各项典型理化指标测定结果见表1。
实施例1-5和对比例1-3的性能测试数据见表1:
表1 实施例的性能测试数据
本发明中基础油的性能对脂的高低温性能影响较大,所以选择了高低温性能优良的合成基础油PAO,制备的润滑脂的使用温度范围宽,适用温度-50-300℃。另外,本发明制备过程绿色化,具有优异的抗剪切性能及防锈性和抗水性能,显著延长光纤的使用寿命,从而降低使用成本。
以上对本发明的具体实施例进行了描述。需要理解的是,本发明并不局限于上述特定实施方式,本领域技术人员可以在权利要求的范围内做出各种变化或修改,这并不影响本发明的实质内容。在不冲突的情况下,本申请的实施例和实施例中的特征可以任意相互组合。

Claims (8)

1.一种光纤防腐润滑脂,其特征在于,由下述重量份数的组分制备而成:
基础油 70-85份;
气相二氧化硅 5-15份;
聚合物 3-10份;
抗磨剂 1-5份;
防锈剂 0.5-2份;
抗氧剂 0.5-2份;
所述的聚合物选自如下的一种:聚丙烯、氯磺化聚乙烯橡胶和环氧树脂;
所述的基础油选自如下的一种或两种以上:PAO10、PAO25、PAO40、PAO100、PAO150、PAO300;
所述的气相二氧化硅的制备方法如下:
1)将体积分数95-98%的乙醇水溶液采用浓氨水调pH=9-10,升温至50-60℃,搅拌均匀;
2)将体积分数15-18%的正硅酸乙酯乙醇溶液按照1:(1.8-2.5)的体积比加入步骤1)配制的溶液中,在50-60℃下恒温反应6-7h,得到硅溶胶溶液;
3)加入50-70%体积的去离子水,搅拌,再滴加盐酸溶液,中和至中性,静置;
4)8500-9500 r/min离心,乙醇洗涤,在40-50℃下真空干燥,得到气相二氧化硅白色粉末;
所述光纤防腐润滑脂的制备方法包括如下步骤:
(1)将基础油在搅拌下加热至 70-80℃,加入气相二氧化硅,继续搅拌直至混匀;
(2)升温至90~100℃进行膨化,膨化时间为60~90min;
(3)膨化结束后用三辊研磨机研磨,然后保持在80~100℃的温度下,加入聚合物、抗磨剂、防锈剂和抗氧剂,搅拌后进行均质处理,得到光纤防腐润滑脂。
2.根据权利要求1所述的光纤防腐润滑脂,其特征在于,所述的抗磨剂选自如下的一种或两种以上:硫代磷酸锌盐、硫代氨基甲酸钼盐、硫代磷酸酯铵盐、硼酸盐、硼酸酯、噻二唑或噻二唑衍生物。
3.根据权利要求2所述的光纤防腐润滑脂,其特征在于,所述的硫代磷酸锌盐是硫磷双辛基碱性锌盐T203;所述的硫代氨基甲酸钼盐是二异辛基二硫代氨基甲酸钼;所述的硫代磷酸酯铵盐为T307;所述的硼酸盐为T361;所述的噻二唑衍生物为噻二唑二聚体。
4.根据权利要求1所述的光纤防腐润滑脂,其特征在于,所述的防锈剂选自如下的一种或两种以上:磺酸盐类、羧酸,酸酐及其皂类、环烷酸锌、单油酸酯、羊毛脂、噻二唑类、苯并三氮唑类。
5.根据权利要求4所述的光纤防腐润滑脂,其特征在于,所述的磺酸盐类为磺酸钡;所述的羧酸,酸酐及其皂类为十二烯基丁二酸酐。
6.根据权利要求1所述的光纤防腐润滑脂,其特征在于,所述的抗氧剂选自如下的一种或两种以上:二芳基仲胺、N-苯基苯胺、烷基二苯胺、对苯二胺、苯酚,2,4-二叔丁基苯酚,2,6-二叔丁基苯酚。
7.一种根据权利要求1-6任一项所述光纤防腐润滑脂的制备方法,其特征在于,该方法包括如下步骤:
(1)将基础油在搅拌下加热至 70-80℃,加入气相二氧化硅,继续搅拌直至混匀;
(2)升温至90~100℃进行膨化,膨化时间为60~90min;
(3)膨化结束后用三辊研磨机研磨,然后保持在80~100℃的温度下,加入聚合物、抗磨剂、防锈剂和抗氧剂,搅拌后进行均质处理,得到光纤防腐润滑脂。
8.根据权利要求7所述光纤防腐润滑脂的制备方法,其特征在于,步骤(3)研磨后保持在80~90℃的温度下,加入聚合物、抗磨剂、防锈剂和抗氧剂。
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