CN106398839A - 一种树脂基润滑切削液及其制备方法 - Google Patents
一种树脂基润滑切削液及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种树脂基润滑切削液,它是由下述重量份的原料组成的:硬脂酸铝2‑3、三乙醇胺0.6‑2、双咪唑烷基脲0.6‑1、烃基丁二酸2‑3、聚乙烯醇缩丁醛1‑2、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、苯骈三氮唑1‑2、醇酸树脂4‑5、聚氧丙烯甘油醚2‑3、硼酸三丁酯1‑2、正硅酸乙酯3‑4。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
技术领域
本发明涉及切削液技术领域,尤其涉及一种树脂基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,提供一种树脂基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:
一种树脂基润滑切削液,它是由下述重量份的原料组成的:
硬脂酸铝2-3、三乙醇胺0.6-2、双咪唑烷基脲0.6-1、烃基丁二酸2-3、聚乙烯醇缩丁醛1-2、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、苯骈三氮唑1-2、醇酸树脂4-5、聚氧丙烯甘油醚2-3、硼酸三丁酯1-2、正硅酸乙酯3-4。
一种所述的树脂基润滑切削液的制备方法,包括以下步骤:
(1)将上述正硅酸乙酯加入到其重量57-60倍的去离子水中,搅拌均匀,加入三乙醇胺,升高温度为50-60℃,保温搅拌10-14分钟,加入浓度为20-25%的氨水,调节pH为10-12,升高温度为70-80℃,继续保温搅拌30-40分钟,加入上述聚氧丙烯甘油醚,搅拌至常温,得硅胶分散液;
(2)将上述苯乙烯、马来酸酐、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,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、硬脂酸铝混合,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)将上述纳米二氧化硅加入到其重量50-60倍的无水乙醇中,加入上述苯骈三氮唑,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;
(5)取上述双咪唑烷基脲,加入到其重量16-20倍的无水乙醇中,搅拌均匀,加入醇酸树脂,送入87-90℃的水浴中,保温搅拌30-49分钟,出料,与上述预处理共聚物混合,搅拌至常温,过滤,常温干燥,得树脂改性共聚物;
(6)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;
(7)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;
(8)取上述叠氮化二氧化硅,与树脂改性共聚物混合,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,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;
(9)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;本发明加入的醇酸树脂可以有效的改善填料在切削液中的分散性,提高成品的稳定性。
具体实施方式
一种树脂基润滑切削液,它是由下述重量份的原料组成的:
硬脂酸铝2、三乙醇胺0.6、双咪唑烷基脲0.6、烃基丁二酸2、聚乙烯醇缩丁醛1、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、苯骈三氮唑1、醇酸树脂4、聚氧丙烯甘油醚2、硼酸三丁酯1、正硅酸乙酯3。
一种所述的树脂基润滑切削液的制备方法,包括以下步骤:
(1)将上述正硅酸乙酯加入到其重量57倍的去离子水中,搅拌均匀,加入三乙醇胺,升高温度为50℃,保温搅拌10分钟,加入浓度为20%的氨水,调节pH为10,升高温度为70℃,继续保温搅拌30分钟,加入上述聚氧丙烯甘油醚,搅拌至常温,得硅胶分散液;
(2)将上述苯乙烯、马来酸酐、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,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、硬脂酸铝混合,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)将上述纳米二氧化硅加入到其重量50倍的无水乙醇中,加入上述苯骈三氮唑,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;
(5)取上述双咪唑烷基脲,加入到其重量16倍的无水乙醇中,搅拌均匀,加入醇酸树脂,送入87℃的水浴中,保温搅拌30分钟,出料,与上述预处理共聚物混合,搅拌至常温,过滤,常温干燥,得树脂改性共聚物;
(6)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;
(7)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;
(8)取上述叠氮化二氧化硅,与树脂改性共聚物混合,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,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;
(9)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)
1.一种树脂基润滑切削液,其特征在于,它是由下述重量份的原料组成的:
硬脂酸铝2-3、三乙醇胺0.6-2、双咪唑烷基脲0.6-1、烃基丁二酸2-3、聚乙烯醇缩丁醛1-2、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、苯骈三氮唑1-2、醇酸树脂4-5、聚氧丙烯甘油醚2-3、硼酸三丁酯1-2、正硅酸乙酯3-4。
2.一种如权利要求1所述的树脂基润滑切削液的制备方法,其特征在于,包括以下步骤:
(1)将上述正硅酸乙酯加入到其重量57-60倍的去离子水中,搅拌均匀,加入三乙醇胺,升高温度为50-60℃,保温搅拌10-14分钟,加入浓度为20-25%的氨水,调节pH为10-12,升高温度为70-80℃,继续保温搅拌30-40分钟,加入上述聚氧丙烯甘油醚,搅拌至常温,得硅胶分散液;
(2)将上述苯乙烯、马来酸酐、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,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、硬脂酸铝混合,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)将上述纳米二氧化硅加入到其重量50-60倍的无水乙醇中,加入上述苯骈三氮唑,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;
(5)取上述双咪唑烷基脲,加入到其重量16-20倍的无水乙醇中,搅拌均匀,加入醇酸树脂,送入87-90℃的水浴中,保温搅拌30-49分钟,出料,与上述预处理共聚物混合,搅拌至常温,过滤,常温干燥,得树脂改性共聚物;
(6)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;
(7)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;
(8)取上述叠氮化二氧化硅,与树脂改性共聚物混合,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,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;
(9)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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