CN106350155A - 一种纳米微乳化切削液及其制备方法 - Google Patents

一种纳米微乳化切削液及其制备方法 Download PDF

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CN106350155A
CN106350155A CN201610763462.8A CN201610763462A CN106350155A CN 106350155 A CN106350155 A CN 106350155A CN 201610763462 A CN201610763462 A CN 201610763462A CN 106350155 A CN106350155 A CN 106350155A
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江海涛
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Tianchang Runda Metal Antirust Auxiliary Co Ltd
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Abstract

本发明公开了一种纳米微乳化切削液，它是由下述重量份的原料组成的：氧化聚乙烯蜡2‑3、乙二胺四乙酸二钠锌1‑2、二甲氨基丙胺0.3‑1、硅酸钾钠1‑2、磷酸三乙酸胺2‑4、溴代十六烷0.4‑1、四丁基溴化铵0.3‑1、氢氧化铜6‑7、10‑15%的甲酸水溶液20‑30、碳纳米管4‑5、甲基硅油50‑60、十二烷基磺酸钠3‑4、水适量、十二烷基硫醇3‑4、纳米硅灰石粉2‑3、十二烷基三甲基氯化铵0.7‑1、棕榈酸钙2‑3、硬脂酸1‑3。本发明将酯化后的碳纳米管与甲酸铜混合球磨后，通过热解，Cu2+会吸附于碳纳米管表面，在碳纳米管表面生成纳米铜颗粒。

Description

一种纳米微乳化切削液及其制备方法
技术领域
本发明涉及切削液技术领域，尤其涉及一种纳米微乳化切削液及其制备方法。
背景技术
由于纳米微粒具有很多常规固体所不具备的性能，比如低熔点、高延展性、易扩散等，使它的硬度、韧性！抗剪切度等也可能发生改变，这意味着通常情况下不能作为润滑材料的固体颗粒，当处于纳米级别时有可能具有润滑性能，并且很可能具有一些不同于传统添加剂的边界润滑机理；其次纳米润滑油添加剂取代传统的S、P、Cl等有机化合物极压抗磨添加剂，可望解决S、P、Cl对基体金属造成的腐蚀和带来的环境问题；但是将纳米粒子应用于切削液中起减摩抗磨作用，也需要解决一些难题；
由于纳米粒子比表面积大！表面能高，所以在溶剂中，尤其是在润滑油这种非水介质中，极易团聚，假如纳米粒子在润滑油中团聚成大的颗粒，就像油中有杂质一样反而会降低润滑油的性能"同时，纳米粒子的分散性和稳定性是两个密切相关而又相互独立的因素，分散性好，稳定性不一定好，另外，切削液一般使用在高温、高压工作环境下，切削液中本身处于悬浮状态的胶体纳米粒子在这样的工作环境下极易破坏其稳定性，从而发生团聚和聚沉，最终使纳米粒子失去抗磨性能；
纳米铜粉作为油性切削液的添加剂可以有效的提高切削液的摩擦性能，但是纳米铜粉在切削液基础油中的稳定性还有待于改善，所以，本研发明通过对碳纳米管的表面改性，制备出碳纳米管/纳米铜复合切削液添加剂，以期在改善其在切削液中分散稳定性的同时，达到提高切削液摩擦性能的目的。
发明内容
本发明目的就是为了弥补已有技术的缺陷，提供一种纳米微乳化切削液及其制备方法。
本发明是通过以下技术方案实现的：
一种纳米微乳化切削液，它是由下述重量份的原料组成的：
氧化聚乙烯蜡2-3、乙二胺四乙酸二钠锌1-2、二甲氨基丙胺0.3-1、硅酸钾钠1-2、磷酸三乙酸胺2-4、溴代十六烷0.4-1、四丁基溴化铵0.3-1、氢氧化铜6-7、10-15％的甲酸水溶液20-30、碳纳米管4-5、甲基硅油50-60、十二烷基磺酸钠3-4、水适量、十二烷基硫醇3-4、纳米硅灰石粉2-3、十二烷基三甲基氯化铵0.7-1、棕榈酸钙2-3、硬脂酸1-3。
一种所述的纳米微乳化切削液的制备方法，包括以下步骤：
(1)将上述氢氧化铜加入到其重量20-35倍的去离子水中，搅拌条件下滴加上述10-15％的甲酸水溶液，滴加完毕后升高温度为80-85℃，保温搅拌至水干，得甲酸化纳米铜；
(2)将上述硅酸钾钠加入到其重量10-14倍的去离子水中，搅拌均匀，升高温度为67-70℃，保温搅拌6-9分钟，加入上述乙二胺四乙酸二钠锌，搅拌至常温，与上述碳纳米管混合，搅拌均匀，加入到质量比为3-4:1的硫酸、硝酸的混合溶液中，所述的硫酸的浓度为96-98％、硝酸的浓度为65-70％，送入117-120℃的恒温油浴中，保温搅拌100-120分钟，出料冷却，抽滤，将沉淀水洗4-5次，在70-80℃下真空干燥20-26小时，得纯化碳纳米管；
(3)将上述棕榈酸钙、氧化聚乙烯蜡混合，加入到混合料重量7-10倍的无水乙醇中，搅拌均匀，加入磷酸三乙酸胺，升高温度为60-80℃，保温搅拌4-7分钟，加入上述纯化碳纳米管，搅拌至常温，过滤，将沉淀水洗3-4次，常温干燥，得改性纯化碳纳米管；
(4)将上述改性纯化碳纳米管加入到其重量80-100倍的、0.2-1mol/l的氢氧化钠溶液中，超声20-30分钟，加入上述溴代十六烷、四丁基溴化铵，继续超声17-20分钟，送入80-85℃的水浴中，保温搅拌7-9小时，出料，滴加氯仿，至沉淀不再改变，静置分层，取下层溶液，加入其重量10-15％的无水乙醇，搅拌均匀后抽滤，将沉淀置于100-105℃的真空干燥箱中干燥完全，得酯化碳纳米管；
(5)将上述十二烷基三甲基氯化铵加入到其重量10-13倍的去离子水中，搅拌均匀，加入纳米硅灰石粉，升高温度为70-76℃，保温搅拌20-30分钟，加入上述二甲氨基丙胺，搅拌至常温，过滤，将沉淀水洗3-4次，在50-60℃下真空干燥1-2小时，得改性硅灰石粉；
(6)将上述酯化碳纳米管、甲酸化纳米铜、改性硅灰石粉混合，加入到上述甲基硅油中，球磨10-13小时，送入190-200℃的油浴中，保温搅拌27-30分钟，出料冷却，得极压抗磨助剂；
(7)将上述极压抗磨助剂与十二烷基磺酸钠混合，加入到混合料重量1.3-2倍的去离子水中，搅拌均匀，加入剩余各原料，700-800转/分搅拌20-30分钟，即得。
本发明的优点是：本发明通过先对碳纳米管纯化，使之接入羧基，然后通过取代反应在酯基上接入长链烷烃分子，正是碳纳米管表面的长链烷烃提供的空间位阻作用增强了碳纳米管/纳米铜复合微粒在甲基硅油中的分散稳定性；经羧基化再酯化的碳纳米管表面含有大量缺陷、自由基、含氧官能团等，表面吸附作用增强，将酯化后的碳纳米管与甲酸铜混合球磨后，通过热解，Cu2+会吸附于碳纳米管表面，在碳纳米管表面生成纳米铜颗粒，加之酯化碳纳米管长链烷烃的空间位阻作用，从而形成分散稳定的碳纳米管/纳米铜极压抗磨助剂；
由于纳米铜粉具有较大的比表面积、表面能和活性，当高活性的纳米铜添加剂添加到甲基硅油后，纳米铜颗粒在摩擦过程中与磨损表面相碰撞时，所产生的机械能大部分将转化为热能，纳米铜颗粒吸热后会团聚成很小的小团体，多个具有一定能量的小团体最终将在磨损表面上形成一定厚度的保护膜，降低了磨损表面的剪切应力和摩擦系数，此外，纳米铜颗粒对磨损表面的凹凸起到一定的填补和修复的作用，相当于传统的磨屑起到的作用，而纳米铜颗粒更小，这种作用效果也更加明显，所以，含有适量纳米铜粉的甲基硅油样品的极压性能可显著提高；另外，由于碳纳米管具有超强超韧性能，并且在受力时可通过出现五边形和七边形对来释放应力，所以碳纳米管在润滑液中滚动，碳纳米管起到了承载的作用，减少摩擦副的界面直接接触，提高了切削液的的润滑性能；
本发明加入的纳米硅灰石粉等，可以有效的提高成品切削液的柔韧性好强度。
具体实施方式
一种纳米微乳化切削液，它是由下述重量份的原料组成的：
氧化聚乙烯蜡2、乙二胺四乙酸二钠锌1、二甲氨基丙胺0.3、硅酸钾钠1、磷酸三乙酸胺2、溴代十六烷0.4、四丁基溴化铵0.3、氢氧化铜6、10％的甲酸水溶液20、碳纳米管4、甲基硅油50、十二烷基磺酸钠3、水适量、十二烷基硫醇3、纳米硅灰石粉2、十二烷基三甲基氯化铵0.7、棕榈酸钙2、硬脂酸1。
一种所述的纳米微乳化切削液的制备方法，包括以下步骤：
(1)将上述氢氧化铜加入到其重量20倍的去离子水中，搅拌条件下滴加上述10％的甲酸水溶液，滴加完毕后升高温度为80℃，保温搅拌至水干，得甲酸化纳米铜；
(2)将上述硅酸钾钠加入到其重量10倍的去离子水中，搅拌均匀，升高温度为67℃，保温搅拌6分钟，加入上述乙二胺四乙酸二钠锌，搅拌至常温，与上述碳纳米管混合，搅拌均匀，加入到质量比为3:1的硫酸、硝酸的混合溶液中，所述的硫酸的浓度为96％、硝酸的浓度为65％，送入117℃的恒温油浴中，保温搅拌100分钟，出料冷却，抽滤，将沉淀水洗4次，在70℃下真空干燥20小时，得纯化碳纳米管；
(3)将上述棕榈酸钙、氧化聚乙烯蜡混合，加入到混合料重量7倍的无水乙醇中，搅拌均匀，加入磷酸三乙酸胺，升高温度为60℃，保温搅拌4分钟，加入上述纯化碳纳米管，搅拌至常温，过滤，将沉淀水洗3次，常温干燥，得改性纯化碳纳米管；
(4)将上述改性纯化碳纳米管加入到其重量80倍的、0.2mol/l的氢氧化钠溶液中，超声20分钟，加入上述溴代十六烷、四丁基溴化铵，继续超声17分钟，送入80℃的水浴中，保温搅拌7小时，出料，滴加氯仿，至沉淀不再改变，静置分层，取下层溶液，加入其重量10％的无水乙醇，搅拌均匀后抽滤，将沉淀置于100℃的真空干燥箱中干燥完全，得酯化碳纳米管；
(5)将上述十二烷基三甲基氯化铵加入到其重量10倍的去离子水中，搅拌均匀，加入纳米硅灰石粉，升高温度为70℃，保温搅拌20分钟，加入上述二甲氨基丙胺，搅拌至常温，过滤，将沉淀水洗3次，在50℃下真空干燥1小时，得改性硅灰石粉；
(6)将上述酯化碳纳米管、甲酸化纳米铜、改性硅灰石粉混合，加入到上述甲基硅油中，球磨10小时，送入190℃的油浴中，保温搅拌27分钟，出料冷却，得极压抗磨助剂；
(7)将上述极压抗磨助剂与十二烷基磺酸钠混合，加入到混合料重量1.3倍的去离子水中，搅拌均匀，加入剩余各原料，700转/分搅拌20分钟，即得。
性能测试：

Claims (2)

1.一种纳米微乳化切削液，其特征在于，它是由下述重量份的原料组成的：
氧化聚乙烯蜡2-3、乙二胺四乙酸二钠锌1-2、二甲氨基丙胺0.3-1、硅酸钾钠1-2、磷酸三乙酸胺2-4、溴代十六烷0.4-1、四丁基溴化铵0.3-1、氢氧化铜6-7、10-15%的甲酸水溶液20-30、碳纳米管4-5、甲基硅油50-60、十二烷基磺酸钠3-4、水适量、十二烷基硫醇3-4、纳米硅灰石粉2-3、十二烷基三甲基氯化铵0.7-1、棕榈酸钙2-3、硬脂酸1-3。
2.一种如权利要求1所述的纳米微乳化切削液的制备方法，其特征在于，包括以下步骤：
（1）将上述氢氧化铜加入到其重量20-35倍的去离子水中，搅拌条件下滴加上述10-15%的甲酸水溶液，滴加完毕后升高温度为80-85℃，保温搅拌至水干，得甲酸化纳米铜；
（2）将上述硅酸钾钠加入到其重量10-14倍的去离子水中，搅拌均匀，升高温度为67-70℃，保温搅拌6-9分钟，加入上述乙二胺四乙酸二钠锌，搅拌至常温，与上述碳纳米管混合，搅拌均匀，加入到质量比为3-4:1的硫酸、硝酸的混合溶液中，所述的硫酸的浓度为96-98%、硝酸的浓度为65-70%，送入117-120℃的恒温油浴中，保温搅拌100-120分钟，出料冷却，抽滤，将沉淀水洗4-5次，在70-80℃下真空干燥20-26小时，得纯化碳纳米管；
（3）将上述棕榈酸钙、氧化聚乙烯蜡混合，加入到混合料重量7-10倍的无水乙醇中，搅拌均匀，加入磷酸三乙酸胺，升高温度为60-80℃，保温搅拌4-7分钟，加入上述纯化碳纳米管，搅拌至常温，过滤，将沉淀水洗3-4次，常温干燥，得改性纯化碳纳米管；
（4）将上述改性纯化碳纳米管加入到其重量80-100倍的、0.2-1mol/l的氢氧化钠溶液中，超声20-30分钟，加入上述溴代十六烷、四丁基溴化铵，继续超声17-20分钟，送入80-85℃的水浴中，保温搅拌7-9小时，出料，滴加氯仿，至沉淀不再改变，静置分层，取下层溶液，加入其重量10-15%的无水乙醇，搅拌均匀后抽滤，将沉淀置于100-105℃的真空干燥箱中干燥完全，得酯化碳纳米管；
（5）将上述十二烷基三甲基氯化铵加入到其重量10-13倍的去离子水中，搅拌均匀，加入纳米硅灰石粉，升高温度为70-76℃，保温搅拌20-30分钟，加入上述二甲氨基丙胺，搅拌至常温，过滤，将沉淀水洗3-4次，在50-60℃下真空干燥1-2小时，得改性硅灰石粉；
（6）将上述酯化碳纳米管、甲酸化纳米铜、改性硅灰石粉混合，加入到上述甲基硅油中，球磨10-13小时，送入190-200℃的油浴中，保温搅拌27-30分钟，出料冷却，得极压抗磨助剂；
（7）将上述极压抗磨助剂与十二烷基磺酸钠混合，加入到混合料重量1.3-2倍的去离子水中，搅拌均匀，加入剩余各原料，700-800转/分搅拌20-30分钟，即得。
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