CN106350180A - 一种复合硅烷润滑切削液及其制备方法 - Google Patents

一种复合硅烷润滑切削液及其制备方法 Download PDF

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CN106350180A
CN106350180A CN201610762761.XA CN201610762761A CN106350180A CN 106350180 A CN106350180 A CN 106350180A CN 201610762761 A CN201610762761 A CN 201610762761A CN 106350180 A CN106350180 A CN 106350180A
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江海涛
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Tianchang Runda Metal Antirust Auxiliary Co Ltd
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Abstract

本发明公开了一种复合硅烷润滑切削液，它是由下述重量份的原料组成的：甲苯基二苯基磷酸酯2‑3、三乙醇胺油酸皂3‑4、硫酸铜0.2‑0.3、苯乙烯10‑17、马来酸酐3‑4、过氧化苯甲酰0.1‑0.2、纳米二氧化硅5‑7、丙炔醇1‑2、氮化钠0.4‑1、氯化铝0.6‑1、硅烷偶联剂kh5600.7‑1、抗坏血酸钠0.1‑0.2、硫醇丁基锡0.8‑1、氨基三甲叉膦酸3‑4、1H，1H，2H，2H‑全氟癸基三乙氧基硅烷0.6‑1、烷基化二苯胺0.8‑1、微晶石蜡1‑2、四丁基溴化铵2‑3、硅灰石粉2‑3。本发明的纳米二氧化硅表面存在的不饱和残键和不同键合状态的羟基，使得其表面具有很高的表面活性，容易沉积到金属摩擦表面上，提高了切削液的润滑性。

Description

一种复合硅烷润滑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，尤其涉及一种复合硅烷润滑切削液及其制备方法。
背景技术
纳米二氧化硅因具有呈三维网状结构，稳定性、补强性及增稠性优越，价格便宜，易制取等特点，广泛运用于切削液中，以提高切削液的承载与防腐能力，纳米二氧化硅的比表面积大，比表面能高，在切削液中容易发生团聚而形成二次粒子，导致增强增韧的性能降低，同时其表面的羟基还强化了此种现象。因此，改善纳米二氧化硅在切削液中的分散性是亟待解决的问题；
增强纳米二氧化硅在有机涂层中的分散性可以采用物理共混、化学接枝等方法。有的借助原位自由基聚合在纳米二氧化硅表面接枝PS和PSMA，制得了双亲性纳米二氧化硅，有的利用二甲基二氯硅烷干法工艺制备了分散性较好的纳米二氧化硅，有的通过聚乙二醇和癸二酸在纳米二氧化硅表面进行缩聚反应，改善了纳米二氧化硅的分散性，有的利用“点击”化学与RAFT及ATRP聚合相结合的方法在粒子表面接枝聚丙烯酰胺和聚苯乙烯，改善了粒子的分散性，目前的研究发现，表面接枝聚合物是改善纳米二氧化硅分散性最有效的方法，但研究中多见发生接枝反应的功能基只位于分子链的一端，对于分子链上含有多个功能基的报道很少；
本发明中首先制备分子链上含有多个炔基的苯乙烯-马来酸酐共聚物，然后改性纳米二氧化硅使其表面引入多个叠氮基，最后利用简单、高效的“点击”化学法在粒子表面接枝聚合物。聚合物分子链有多个点接枝到粒子表面，使得分子链“趴伏”在粒子表面，从而在不需要引入大量聚合物链的条件下实现对粒子的包覆，得到接枝密度高、分散性好的纳米二氧化硅，增强其在切削液中的分散性；
研究表明，纳米微粒作为切削液中的润滑添加剂使用时，可以起到特殊的减摩、抗磨和极压作用，有的合成了油酸修饰二氧化钛纳米微粒，也具有很好的摩擦性能，而单分散纳米二氧化硅粒度可控性好、分布范围窄、分散性好、无毒无味，因此将其运用于切削液中来提高其抗磨性能，是目前研究的一个重点。
发明内容
本发明目的就是为了弥补已有技术的缺陷，提供一种复合硅烷润滑切削液及其制备方法。
本发明是通过以下技术方案实现的：
一种复合硅烷润滑切削液，它是由下述重量份的原料组成的：
甲苯基二苯基磷酸酯2-3、三乙醇胺油酸皂3-4、硫酸铜0.2-0.3、苯乙烯10-17、马来酸酐3-4、过氧化苯甲酰0.1-0.2、纳米二氧化硅5-7、丙炔醇1-2、氮化钠0.4-1、氯化铝0.6-1、硅烷偶联剂kh5600.7-1、抗坏血酸钠0.1-0.2、硫醇丁基锡0.8-1、氨基三甲叉膦酸3-4、1H，1H，2H，2H-全氟癸基三乙氧基硅烷0.6-1、烷基化二苯胺0.8-1、微晶石蜡1-2、四丁基溴化铵2-3、硅灰石粉2-3。
一种所述的复合硅烷润滑切削液的制备方法，包括以下步骤：
(1)将上述硅灰石粉在760-800℃下煅烧1-2小时，冷却至常温，与上述马来酸酐混合，加入到混合料重量10-14倍的去离子水中，加入烷基化二苯胺，在70-76℃下保温搅拌20-30分钟，过滤，将沉淀在50-60℃下真空干燥1-2小时，得酸酐石粉；
(2)将上述苯乙烯、过氧化苯甲酰混合，加入到混合料重量17-20倍的二甲基甲酰胺中，通入氮气，加入上述酸酐石粉、硫醇丁基锡，在70-80℃下保温搅拌4-5小时，出料，将产物加入到无水乙醇中，搅拌均匀，过滤，真空干燥，得酸酐共聚物；
(3)将上述酸酐共聚物、丙炔醇混合，加入到混合料重量10-12倍的四氢呋喃中，搅拌均匀，升高温度为76-80℃，保温搅拌30-40分钟，减压蒸馏除去液体，真空干燥，得预处理共聚物；
(4)将上述三乙醇胺油酸皂加入到其重量3-4倍的无水乙醇中，送入到80-90℃的水浴中，保温搅拌10-20分钟，出料，加入上述预处理共聚物，搅拌至常温，过滤，将沉淀常温干燥，得改性预处理共聚物；
(5)将上述四丁基溴化铵、纳米二氧化硅混合，加入到混合料重量50-60倍的无水乙醇中，超声100-120分钟，加入上述硅烷偶联剂kh560，在87-90℃下保温搅拌20-24小时，抽滤，将沉淀真空干燥，得硅烷改性二氧化硅；
(6)将上述微晶石蜡加入到其重量6-10倍的无水乙醇中，送入110-120℃的油浴中，保温搅拌20-30分钟，出料，加入1H，1H，2H，2H-全氟癸基三乙氧基硅烷，搅拌至常温，得硅烷醇液；
(7)取上述硅烷改性二氧化硅，加入到其重量30-40倍的二甲基甲酰胺中，超声100-110分钟，加入上述氮化钠、氯化铝，在30-35℃下保温搅拌20-25小时，抽滤，将沉淀水洗3-4次，真空干燥，得叠氮化二氧化硅；
(8)将上述抗坏血酸钠、硫酸铜混合，加入到混合料重量18-20倍的去离子水中，搅拌均匀；
(9)将上述叠氮化二氧化硅、改性预处理共聚物混合，加入到混合料重量30-40倍的二甲基甲酰胺中，通入氮气，加入上述抗坏血酸钠、硫酸铜的混合水溶液，在80-85℃下保温搅拌20-25小时，加入上述硅烷醇液，搅拌均匀，抽滤，将沉淀用去离子水、二甲基甲酰胺各洗涤4-5次，真空干燥，得叠氮化二氧化硅接枝共聚物；
(10)将上述叠氮化二氧化硅接枝共聚物与剩余各原料混合，加入到混合料重量10-14倍的去离子水中，500-1000转/分搅拌分散30-40分钟，即得所述切削液。
本发明的优点是：本发明首先利用普通自由基聚合的方式制备苯乙烯及马来酸酐共聚物，再与丙炔醇反应，在分子链上引入多个炔基，然后利用硅烷偶联剂改性纳米二氧化硅，之后与叠氮化钠反应，在纳米二氧化硅粒子表面引入多个叠氮基团，最后将带有多个炔基的分子链通过“点击”化学接枝到纳米二氧化硅表面，可以较迅速地与粒子表面周围的叠氮基反应，从而起到反应自加速的作用，使得分子链“趴伏”在粒子表面，从而在不需要引入大量聚合物链的条件下实现对粒子的包覆，阻碍了纳米粒子的团聚，得到接枝密度高、分散性好的纳米二氧化硅，增强其在切削液中的分散性，本发明的纳米二氧化硅分子状态呈三维链状结构，表面存在的不饱和残键和不同键合状态的羟基，使得其表面具有很高的表面活性，容易沉积到金属摩擦表面上，在摩擦接触面形成均匀的二氧化硅纳米沉积膜，提高了切削液的润滑性；本发明加入了1H，1H，2H，2H全氟癸基三乙氧基硅烷、硅烷偶联剂，可以有效的提高成品切削液的润滑性和分散性。
具体实施方式
一种复合硅烷润滑切削液，它是由下述重量份的原料组成的：
甲苯基二苯基磷酸酯2、三乙醇胺油酸皂3、硫酸铜0.2、苯乙烯10、马来酸酐3、过氧化苯甲酰0.1、纳米二氧化硅5、丙炔醇1、氮化钠0.4、氯化铝0.6、硅烷偶联剂kh5600.7、抗坏血酸钠0.1、硫醇丁基锡0.8、氨基三甲叉膦酸3、1H，1H，2H，2H全氟癸基三乙氧基硅烷0.6、烷基化二苯胺0.8、微晶石蜡1、四丁基溴化铵2、硅灰石粉2。
一种所述的复合硅烷润滑切削液的制备方法，包括以下步骤：
(1)将上述硅灰石粉在760℃下煅烧1小时，冷却至常温，与上述马来酸酐混合，加入到混合料重量10倍的去离子水中，加入烷基化二苯胺，在70℃下保温搅拌20分钟，过滤，将沉淀在50℃下真空干燥1小时，得酸酐石粉；
(2)将上述苯乙烯、过氧化苯甲酰混合，加入到混合料重量17倍的二甲基甲酰胺中，通入氮气，加入上述酸酐石粉、硫醇丁基锡，在70℃下保温搅拌4小时，出料，将产物加入到无水乙醇中，搅拌均匀，过滤，真空干燥，得酸酐共聚物；
(3)将上述酸酐共聚物、丙炔醇混合，加入到混合料重量10倍的四氢呋喃中，搅拌均匀，升高温度为76℃，保温搅拌30分钟，减压蒸馏除去液体，真空干燥，得预处理共聚物；
(4)将上述三乙醇胺油酸皂加入到其重量3倍的无水乙醇中，送入到80℃的水浴中，保温搅拌10分钟，出料，加入上述预处理共聚物，搅拌至常温，过滤，将沉淀常温干燥，得改性预处理共聚物；
(5)将上述四丁基溴化铵、纳米二氧化硅混合，加入到混合料重量50倍的无水乙醇中，超声100分钟，加入上述硅烷偶联剂kh560，在87℃下保温搅拌20小时，抽滤，将沉淀真空干燥，得硅烷改性二氧化硅；
(6)将上述微晶石蜡加入到其重量6倍的无水乙醇中，送入110℃的油浴中，保温搅拌20分钟，出料，加入1H，1H，2H，2H全氟癸基三乙氧基硅烷，搅拌至常温，得硅烷醇液；
(7)取上述硅烷改性二氧化硅，加入到其重量30倍的二甲基甲酰胺中，超声100分钟，加入上述氮化钠、氯化铝，在30℃下保温搅拌20小时，抽滤，将沉淀水洗3次，真空干燥，得叠氮化二氧化硅；
(8)将上述抗坏血酸钠、硫酸铜混合，加入到混合料重量18倍的去离子水中，搅拌均匀；
(9)将上述叠氮化二氧化硅、改性预处理共聚物混合，加入到混合料重量30倍的二甲基甲酰胺中，通入氮气，加入上述抗坏血酸钠、硫酸铜的混合水溶液，在80℃下保温搅拌20小时，加入上述硅烷醇液，搅拌均匀，抽滤，将沉淀用去离子水、二甲基甲酰胺各洗涤4次，真空干燥，得叠氮化二氧化硅接枝共聚物；
(10)将上述叠氮化二氧化硅接枝共聚物与剩余各原料混合，加入到混合料重量10倍的去离子水中，500转/分搅拌分散30分钟，即得所述切削液。
性能测试：

Claims (2)

1.一种复合硅烷润滑切削液，其特征在于，它是由下述重量份的原料组成的：
甲苯基二苯基磷酸酯2-3、三乙醇胺油酸皂3-4、硫酸铜0.2-0.3、苯乙烯10-17、马来酸酐3-4、过氧化苯甲酰0.1-0.2、纳米二氧化硅5-7、丙炔醇1-2、氮化钠0.4-1、氯化铝0.6-1、硅烷偶联剂kh5600.7-1、抗坏血酸钠0.1-0.2、硫醇丁基锡0.8-1、氨基三甲叉膦酸3-4、1H，1H，2H，2H-全氟癸基三乙氧基硅烷0.6-1、烷基化二苯胺0.8-1、微晶石蜡1-2、四丁基溴化铵2-3、硅灰石粉2-3。
2.一种如权利要求1所述的复合硅烷润滑切削液的制备方法，其特征在于，包括以下步骤：
（1）将上述硅灰石粉在760-800℃下煅烧1-2小时，冷却至常温，与上述马来酸酐混合，加入到混合料重量10-14倍的去离子水中，加入烷基化二苯胺，在70-76℃下保温搅拌20-30分钟，过滤，将沉淀在50-60℃下真空干燥1-2小时，得酸酐石粉；
（2）将上述苯乙烯、过氧化苯甲酰混合，加入到混合料重量17-20倍的二甲基甲酰胺中，通入氮气，加入上述酸酐石粉、硫醇丁基锡，在70-80℃下保温搅拌4-5小时，出料，将产物加入到无水乙醇中，搅拌均匀，过滤，真空干燥，得酸酐共聚物；
（3）将上述酸酐共聚物、丙炔醇混合，加入到混合料重量10-12倍的四氢呋喃中，搅拌均匀，升高温度为76-80℃，保温搅拌30-40分钟，减压蒸馏除去液体，真空干燥，得预处理共聚物；
（4）将上述三乙醇胺油酸皂加入到其重量3-4倍的无水乙醇中，送入到80-90℃的水浴中，保温搅拌10-20分钟，出料，加入上述预处理共聚物，搅拌至常温，过滤，将沉淀常温干燥，得改性预处理共聚物；
（5）将上述四丁基溴化铵、纳米二氧化硅混合，加入到混合料重量50-60倍的无水乙醇中，超声100-120分钟，加入上述硅烷偶联剂kh560，在87-90℃下保温搅拌20-24小时，抽滤，将沉淀真空干燥，得硅烷改性二氧化硅；
（6）将上述微晶石蜡加入到其重量6-10倍的无水乙醇中，送入110-120℃的油浴中，保温搅拌20-30分钟，出料，加入1H，1H，2H，2H-全氟癸基三乙氧基硅烷，搅拌至常温，得硅烷醇液；
（7）取上述硅烷改性二氧化硅，加入到其重量30-40倍的二甲基甲酰胺中，超声100-110分钟，加入上述氮化钠、氯化铝，在30-35℃下保温搅拌20-25小时，抽滤，将沉淀水洗3-4次，真空干燥，得叠氮化二氧化硅；
（8）将上述抗坏血酸钠、硫酸铜混合，加入到混合料重量18-20倍的去离子水中，搅拌均匀；
（9）将上述叠氮化二氧化硅、改性预处理共聚物混合，加入到混合料重量30-40倍的二甲基甲酰胺中，通入氮气，加入上述抗坏血酸钠、硫酸铜的混合水溶液，在80-85℃下保温搅拌20-25小时，加入上述硅烷醇液，搅拌均匀，抽滤，将沉淀用去离子水、二甲基甲酰胺各洗涤4-5次，真空干燥，得叠氮化二氧化硅接枝共聚物；
（10）将上述叠氮化二氧化硅接枝共聚物与剩余各原料混合，加入到混合料重量10-14倍的去离子水中，500-1000转/分搅拌分散30-40分钟，即得所述切削液。
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