CN116751619A - 一种钛合金切削加工智能润滑剂及其制备方法 - Google Patents
一种钛合金切削加工智能润滑剂及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种钛合金切削加工智能润滑剂及其制备方法,具体是用于钛合金加工过程中的聚(N‑异丙基丙烯酰胺‑co‑丙烯酸)‑二硫化钼/氧化石墨烯智能润滑剂及其制备方法,其制备步骤包括:先制备无机类富勒烯结构二硫化钼并与氧化石墨烯复合制备二硫化钼/氧化石墨烯水溶液,其次采用水相溶液聚合法制备聚(N‑异丙基丙烯酰胺‑co‑丙烯酸)复合微球,最后将聚(N‑异丙基丙烯酰胺‑co‑丙烯酸)复合微球与二硫化钼/氧化石墨烯水溶液复合制备成该智能润滑剂。本发明简单有效,所制备的智能润滑剂分散性好,能够实现基于温度和pH的智能润滑响应,用于钛合金/硬质合金摩擦副时具有较好的润滑性能,在钛合金加工等领域具有良好的应用前景。
Description
技术领域
本发明涉及机械加工润滑剂领域,具体涉及一种钛合金切削加工智能润滑剂及其制备方法,该润滑剂可以通过温度与pH响应实现智能润滑。
背景技术
钛合金具有比强度高、抗腐蚀性好以及热稳定性高等显著优势,已被广泛应用于航空航天、海洋、能源、化工和生物医疗等领域。随着社会发展,全球钛合金材料的需求与日俱增,然而,钛合金切削加工过程中存在变形系数小、切削温度高以及切削力大等问题,尤其是长时间切削过程,随摩擦温度升高,切削液降解酸化,导致常规切削液润滑性能显著降低,刀具磨损严重,严重制约钛合金加工精度与加工效率。研究表明,降低钛合金与刀具之间的摩擦系数,防止刀具过快磨损,是保障钛合金加工精度与效率的关键,因此,如何实现钛合金加工过程中的高效润滑已成为亟待解决的重要问题,尤其是在钛合金连续切削加工过程中,随温度升高及pH降低导致的润滑性能不足问题亟需解决。
纳米二硫化钼与氧化石墨烯作为常见的纳米润滑剂,在多种机械加工领域有广泛应用,然而两者的表面能较高,易发生团聚,成为影响纳米润滑剂润滑性能优势发挥的技术瓶颈。聚合物微凝胶是一类具有三维网络结构的纳米微球智能材料,对环境变化如温度等能产生显著响应行为,并且在水中具有良好的分散性,已广泛应用于药物释放、污水处理和开关阀等领域,同时在润滑领域也扮演着越来越重要的角色。为此,若将聚合物微凝胶与二硫化钼/氧化石墨烯各自的优势结合起来,则有望发展一种钛合金加工过程用的新型智能润滑剂,能根据环境变化产生智能润滑响应,然而,复合材料的结合方式、结构组成以及其制备方法等均会对其润滑性能产生难以预知的影响,迄今为止,尚未见有关这种同时实现温度与pH调控并负载纳米润滑剂的钛合金加工智能润滑剂及其制备方法的相关报道。
发明内容
本发明所要解决的技术问题是针对现有技术的不足,提供一种钛合金切削加工智能润滑剂用于钛合金切削加工过程的减摩润滑,该润滑剂能基于切削加工过程中对温度与pH响应,实现智能润滑,从而降低摩擦与磨损,改善钛合金表面质量。
本发明通过以下具体技术方案来实现:
钛合金切削加工智能润滑剂,其化学结构组成为:聚(N-异丙基丙烯酰胺-co-丙烯酸)-二硫化钼/氧化石墨烯;其中聚丙烯酸与聚N-异丙基丙烯酰胺形成三维互穿网络结构复合微球,粒径大小400-700nm,二硫化钼为无机类富勒烯结构,并与复合微球吸附在氧化石墨烯纳米片表面;聚N-异丙基丙烯酰胺与聚丙烯酸质量比为8-9:1,复合微球与氧化石墨烯、二硫化钼的质量比为1500-5000:30-50:1,二硫化钼粒径为50-80nm。
该智能润滑剂按以下方法制备:
(1)取1.0-2.3g硫代乙酰胺、0.5-1.0g钼酸钠、80-160mL去离子水依次加入到带回流装置的三口烧瓶中,以300r/min搅拌并加热至79-81℃,加入7-15mL无水乙醇继续加热并搅拌,待温度为82-84℃时加入15-30mL质量浓度36-38%的浓盐酸,保温并搅拌反应10-15min,过滤反应产物并用水洗涤至中性,然后于110-120℃烘干后,在480-500℃煅烧并保温60-65min,最后对其进行研磨处理,得无机类富勒烯结构二硫化钼;
(2)将步骤(1)制备的二硫化钼配置成浓度为0.05g/L的水溶液,与浓度为2g/L的氧化石墨烯水溶液混合处理,体积比为0.75-1.25:1,以200-300r/min的速率进行磁力搅拌20-40min后超声50-60min,其中超声功率为200-400W,得二硫化钼/氧化石墨烯水溶液;
(3)取1.6-3.6gN-异丙基丙烯酰胺、0.2-0.4g丙烯酸、0.033-0.066gN,N'-亚甲基双丙烯酰胺、0.02-0.04g十二烷基硫酸钠、120-250mL去离子水依次加入到三口烧瓶中,随后通入氮气去除溶液中的氧气,以450-550r/min的速率进行磁力搅拌50-55min后开始升温,待温度为67-70℃时,将10-20mL浓度为0.0080-0.0085g/mL的过硫酸钾溶液缓慢加入到三口烧瓶中,最后在67-70℃条件下反应5-5.5h;
(4)将步骤(3)中反应后的溶液用去离子水进行透析处理,透析过程使用磁力搅拌加速透析速度,每隔8-10h更换一次去离子水,透析6-7d,得聚(N-异丙基丙烯酰胺-co-丙烯酸)复合微球;
(5)将步骤(4)制备的聚(N-异丙基丙烯酰胺-co-丙烯酸)复合微球调配浓度为1.0wt%后,与步骤(2)制备的二硫化钼/氧化石墨烯水溶液混合处理,以200-260r/min的速率进行磁力搅拌25-35min后超声1.5-2h,其中超声功率为300-400W,最后搅拌7-8h,高速离心,即得智能润滑剂;
其中,步骤(3)中N-异丙基丙烯酰胺与丙烯酸质量比为8-9:1,步骤(5)中聚(N-异丙基丙烯酰胺-co-丙烯酸)复合微球与氧化石墨烯质量比为50-100:1。
与现有技术相比,本发明的有益效果体现在:
(1)本发明采用特定的反应原料配比与制备工艺,先将无机类富勒烯结构二硫化钼分散在氧化石墨烯纳米片表面,后将聚(N-异丙基丙烯酰胺-co-丙烯酸)复合微球利用表面氢键再次吸附在氧化石墨烯纳米片表面,解决了纳米二硫化钼及氧化石墨烯的团聚问题,所得聚(N-异丙基丙烯酰胺-co-丙烯酸)-二硫化钼/氧化石墨烯智能润滑剂具有较好的水溶液分散性,稳定时间显著增加。
(2)本发明所制备的智能润滑剂粒径分布均匀且可控,能够随温度升高或pH降低,做出快速响应增强润滑性能,具备智能润滑效果。
(3)本发明所制备的智能润滑剂各组分之间具有协同润滑效果,与单一原料相比具有显著的减摩效果与表面加工质量,平均摩擦系数降幅达20%以上。
(4)本发明制备方法工艺简便,成本低,制备条件温和,能实现智能润滑剂的可控制备,易于规模化应用。
附图说明
图1为实施例1制备的智能润滑剂在不同温度下存放30d前后外观照片对比:(a)新制备,25℃,(b)新制备,35℃,(c)存放30d,25℃,(d)存放30d,35℃。
图2为实施例1制备的智能润滑剂在不同温度下存放30d前后平均粒径及分散性指数对比:(a)25℃,(b)35℃。
图3为实施例1制备的智能润滑剂的透射电镜图(a)与结构示意图(b)。
图4为实施例1制备的智能润滑剂粒径随温度与pH变化的曲线图。
图5为实施例1制备的智能润滑剂的摩擦系数对比图。
具体实施方式
下面结合具体实施例,对本发明进一步阐述。实施例仅用于说明本发明而不用于限制本发明的范围。
实施例1
(1)取1.0g硫代乙酰胺、0.5g钼酸钠、80mL去离子水依次加入到带回流装置的三口烧瓶中,以300r/min搅拌并加热至80℃,加入7.5mL无水乙醇继续加热并搅拌,待温度为82℃时加入15mL质量浓度36-38%的浓盐酸,保温并搅拌反应15min,过滤反应产物并用水洗涤至中性,然后于110℃烘干后,在480℃煅烧并保温60min,最后对其进行研磨处理,得无机类富勒烯结构二硫化钼;
(2)将步骤(1)制备的二硫化钼配置成浓度为0.05g/L的水溶液,与浓度为2g/L的氧化石墨烯水溶液混合处理,体积比为1:1,以260r/min的速率进行磁力搅拌20min后超声60min,其中超声功率为300W,得二硫化钼/氧化石墨烯水溶液;
(3)取1.7gN-异丙基丙烯酰胺、0.2g丙烯酸、0.033gN,N'-亚甲基双丙烯酰胺、0.02g十二烷基硫酸钠、120mL去离子水依次加入到三口烧瓶中,随后通入氮气去除溶液中的氧气,以500r/min的速率进行磁力搅拌50min后开始升温,待温度为70℃时,将10mL浓度为0.0083g/mL的过硫酸钾溶液缓慢加入到三口烧瓶中,最后在70℃条件下反应5h;
(4)将步骤(3)中反应后的溶液用去离子水进行透析处理,透析过程使用磁力搅拌加速透析速度,每隔8h更换一次去离子水,透析7d,得聚(N-异丙基丙烯酰胺-co-丙烯酸)复合微球;
(5)将步骤(4)制备的聚(N-异丙基丙烯酰胺-co-丙烯酸)复合微球调配浓度为1.0wt%后,与步骤(2)制备的二硫化钼/氧化石墨烯水溶液混合处理,聚(N-异丙基丙烯酰胺-co-丙烯酸)复合微球与氧化石墨烯质量比为50:1,以200r/min的速率进行磁力搅拌30min后超声2h,其中超声功率为400W,最后搅拌8h,高速离心,即得智能润滑剂。
为了测试本发明的智能润滑性能,采用球-盘往复式摩擦试验机,摩擦副材料为TC4盘、YG8球,摩擦实验参数为:载荷15N,单次行程5mm,往复运动频率5Hz,实验时间10min,温度为25、30、32、35℃,pH为3、5、7、9,浓度为0.25、0.5、0.75、1.0wt%。
从图1、图2可以看出,实施例1所制备的聚(N-异丙基丙烯酰胺-co-丙烯酸)-二硫化钼/氧化石墨烯智能润滑剂分散稳定性时间长达30d,具有明显的温敏响应特性,长时间存放后粒径与分散指数略微增加,未对智能润滑剂产生明显影响。
从图3可以看出,实施例1所制备的二硫化钼与聚(N-异丙基丙烯酰胺-co-丙烯酸)复合微球共同吸附在氧化石墨烯纳米片表面,且分散性能较好,未出现明显团聚。
从图4可以看出,实施例1所制备的聚(N-异丙基丙烯酰胺-co-丙烯酸)-二硫化钼/氧化石墨烯智能润滑剂同时对温度与pH敏感,随着温度的升高粒径逐渐减小,在32℃附近降幅速率最大,随着pH的升高粒径逐渐增大,呈线性增大的趋势。
从图5可以看出,实施例1所制备的聚(N-异丙基丙烯酰胺-co-丙烯酸)-二硫化钼/氧化石墨烯智能润滑剂各组分具有协同润滑效果,与单一原料相比具有更低的摩擦系数,钛合金润滑性能显著改善。
以摩擦系数为响应指标,选取温度25、30、32、35℃,浓度0.25、0.5、0.75、1.0wt%与pH3、pH5、pH7、pH9进行三因素四水平正交实验探索温度、浓度与pH对智能润滑剂润滑性能的影响,将极差分析结果如表1所示。
表1摩擦实验结果极差分析表
表中k1,k2,k3,k4分别表示温度、pH中水平数为1、2、3、4所对应的摩擦系数之和,K1,K2,K3,K4分别表示各因素中水平数所对应的摩擦系数的平均值,R表示每列中该水平的极差,R值越大表明所考察的因素中对考察指标的影响越大。表1中的数据表明温度、浓度与pH对智能润滑剂的润滑性能均有较大影响,可通过调控润滑剂的温度与pH实现智能润滑。
Claims (2)
1.一种钛合金切削加工智能润滑剂,其特征在于,化学结构组成为:聚(N-异丙基丙烯酰胺-co-丙烯酸)-二硫化钼/氧化石墨烯;其中聚丙烯酸与聚N-异丙基丙烯酰胺形成三维互穿网络结构复合微球,粒径大小400-700nm,二硫化钼为无机类富勒烯结构,并与复合微球吸附在氧化石墨烯纳米片表面;聚N-异丙基丙烯酰胺与聚丙烯酸质量比为8-9:1,复合微球与氧化石墨烯、二硫化钼的质量比为1500-5000:30-50:1,二硫化钼粒径为50-80nm。
2.一种权利要求1所述智能润滑剂的制备方法,其特征在于,包括以下步骤:
(1)取1.0-2.5g硫代乙酰胺、0.5-1.1g钼酸钠、60-160mL去离子水依次加入到带回流装置的三口烧瓶中,以300r/min搅拌并加热至78-82℃,加入7-20mL无水乙醇继续加热并搅拌,待温度为81-84℃时加入13-30mL质量浓度36-38%的浓盐酸,保温并搅拌反应10-15min,过滤反应产物并用水洗涤至中性,然后于100-120℃烘干后,在480-500℃煅烧并保温60-70min,最后对其进行研磨处理,得无机类富勒烯结构二硫化钼;
(2)将步骤(1)制备的二硫化钼配置成浓度为0.05g/L的水溶液,与浓度为2g/L的氧化石墨烯水溶液混合处理,体积比为0.75-1.25:1,以200-300r/min的速率进行磁力搅拌20-50min后超声40-70min,其中超声功率为200-400W,得二硫化钼/氧化石墨烯水溶液;
(3)取1.6-4.5gN-异丙基丙烯酰胺、0.2-0.5g丙烯酸、0.033-0.07g N,N'-亚甲基双丙烯酰胺、0.02-0.05g十二烷基硫酸钠、100-250mL去离子水依次加入到三口烧瓶中,随后通入氮气去除溶液中的氧气,以450-600r/min的速率进行磁力搅拌50-60min后开始升温,待温度为65-70℃时,将10-20mL浓度为0.0080-0.0085g/mL的过硫酸钾溶液缓慢加入到三口烧瓶中,最后在65-70℃条件下反应5-6h;
(4)将步骤(3)中反应后的溶液用去离子水进行透析处理,透析过程使用磁力搅拌加速透析速度,每隔8-12h更换一次去离子水,透析5-7d,得聚(N-异丙基丙烯酰胺-co-丙烯酸)复合微球;
(5)将步骤(4)制备的聚(N-异丙基丙烯酰胺-co-丙烯酸)复合微球调配浓度为1.0wt%后,与步骤(2)制备的二硫化钼/氧化石墨烯水溶液混合处理,以200-300r/min的速率进行磁力搅拌20-40min后超声1.5-2h,其中超声功率为200-400W,最后搅拌6-8h,高速离心,即得智能润滑剂;
其中,步骤(3)中N-异丙基丙烯酰胺与丙烯酸质量比为8-9:1,步骤(5)中聚(N-异丙基丙烯酰胺-co-丙烯酸)复合微球与氧化石墨烯质量比为50-100:1。
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