CN107760407A - 一种水基润滑剂用复酯的制备方法 - Google Patents
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M105/00—Lubricating compositions characterised by the base-material being a non-macromolecular organic compound
- C10M105/08—Lubricating compositions characterised by the base-material being a non-macromolecular organic compound containing oxygen
- C10M105/32—Esters
- C10M105/42—Complex esters, i.e. compounds containing at least three esterified carboxyl groups and derived from the combination of at least three different types of the following five types of compound: monohydroxy compounds, polyhydroxy compounds, monocarboxylic acids, polycarboxylic acids and hydroxy carboxylic acids
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- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M129/00—Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing oxygen
- C10M129/86—Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing oxygen having a carbon chain of 30 or more atoms
- C10M129/95—Esters
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
- C10M2207/28—Esters
- C10M2207/30—Complex esters, i.e. compounds containing at leasst three esterified carboxyl groups and derived from the combination of at least three different types of the following five types of compounds: monohydroxyl compounds, polyhydroxy xompounds, monocarboxylic acids, polycarboxylic acids or hydroxy carboxylic acids
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- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
- C10M2207/28—Esters
- C10M2207/30—Complex esters, i.e. compounds containing at leasst three esterified carboxyl groups and derived from the combination of at least three different types of the following five types of compounds: monohydroxyl compounds, polyhydroxy xompounds, monocarboxylic acids, polycarboxylic acids or hydroxy carboxylic acids
- C10M2207/301—Complex esters, i.e. compounds containing at leasst three esterified carboxyl groups and derived from the combination of at least three different types of the following five types of compounds: monohydroxyl compounds, polyhydroxy xompounds, monocarboxylic acids, polycarboxylic acids or hydroxy carboxylic acids used as base material
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Abstract
本发明涉及一种水基润滑剂用复酯的制备方法，其包括以下制备步骤：取以下原料备用：季戊四醇，濮阳华鹏宇化工科技有限公司；辛二酸，常州康隆化工有限公司；本发明所述方法制备的水基润滑剂用复酯具有良好的极压抗磨性，能够加强钢帘线与橡胶的粘合作用。
Description
技术领域
本发明涉及一种水基润滑剂用复酯的制备方法。
背景技术
随着国家对环保要求的提高及人们环保意识的加强，金属加工领域对切屑液或润滑剂的环保性能提出了更高的要求。钢丝帘线（俗称钢帘线）是超洁净钢的代表产品和钢铁企业线材生产水平的标志性产品，也是强度最高的商用钢。在钢帘线的拉拔生产过程中需使用水基润滑剂，除对其冷却、清洗等基本性能提出要求外，还对其极压抗磨性、提高钢丝与橡胶的粘合力等方面提出了更高的要求。合成酯具有热氧化稳定性好、生物降解性好、毒性极小等特点，极易与金属表面发生物理与化学吸附，形成紧密的边界润滑层，非常有利于高速钢丝拉拔。合成酯的分子结构可人为设计，从分子官能团方面来看：所设计的分子中需含有疏水性基团赋予其油溶性，并含有亲水性基团使其具有水溶性，同时含有反应性基团赋予其极压抗磨性；从分子结构方面来看：三羟甲基丙烷油酸酯具有良好的热稳定性，生物降解率高，可用作化纤油剂的润滑剂和润滑油的基础组分。
设计的合成酯除具有良好的润滑性外，还需要考虑各种基团与金属表面的吸附能力以及对橡胶的溶解能力，以促进钢帘线与橡胶的粘合。复酯相对于多元醇酯，引入的二元酸分子结构增加了极性功能团的数量，增强了其在钢丝摩擦表面的吸附能力，使钢丝表面形成的润滑膜具有更好的极压抗磨性能。水基润滑剂的生物降解性是评价其生态效应最主要的指标。合成酯的酯基是亲水基团，为微生物攻击酯分子提供了活化点，其生物降解能力约为70-100%，水体危害等级为0，即对水体无污染。基于分子结构设计，作者选用季戊四醇、辛二酸、油酸，按两步法进行缩聚酯化反应制备复酯Ｐ，对其制备条件进行研究，通过红外光谱、凝胶渗透色谱表征其结构，并以复酯为主体制备水基润滑剂，对其摩擦学性能进行评价，以促进国产环境友好型水基润滑剂的推广应用。
发明内容
基于上述原因，本发明提出一种水基润滑剂用复酯的制备方法。
本发明所述一种水基润滑剂用复酯的制备方法，包括以下制备步骤：
（1）取以下原料备用：季戊四醇，濮阳华鹏宇化工科技有限公司；辛二酸，常州康隆化工有限公司；油酸，晋州同济油脂化工厂；金属粉末，北京蒙泰有研技术开发中心；二甲苯，武汉恒诚化工有限公司；所用试剂均为化学纯；
（2）在装有温度计、搅拌器、分水器和球形冷凝管的500毫升四口烧瓶中，按物质的量比1:2加入辛二酸、季戊四醇，按酸醇总质量的0.5%加入催化剂金属粉末，加热升温；
（3）待物料大部分熔化后，启动搅拌，加入用量为分水器容积110%的二甲苯，继续加热升温；当温度升至136-140摄氏度时，开始出现回流；
（4）调节控温装置控制反应温度在158-162℃；待分水器中液体分层后，及时分离出下层的水，直至分水器中不再有水析出，即得到低聚物中间体；
（5）延续上述实验，通入干燥的氮气赶走反应体系中空气，按油酸与辛二酸物质的量比3:1加入油，加热升温；
（6）当温度升至164-168℃时，开始出现回；调节控温装置控制反应温度为183-187℃，同时使用温棉包裹四口烧瓶；
（7）待分水器中液体分层后，及时分离出下层的水，直至分水器中没有水析出；
（8）打开真空泵切换成减压状态，停止加热，搅拌降温过程中将携水剂二甲苯全部抽出；
（9）冷却至50-60℃后，停止搅拌和通氮气；
（10）静置0.5小时后，即得到棕色半透明液体产物。
本发明所述方法制备的水基润滑剂用复酯具有良好的极压抗磨性，能够加强钢帘线与橡胶的粘合作用。
具体实施方式
实施例1。
本发明所述一种水基润滑剂用复酯的制备方法，包括以下制备步骤：
（1）取以下原料备用：季戊四醇，濮阳华鹏宇化工科技有限公司；辛二酸，常州康隆化工有限公司；油酸，晋州同济油脂化工厂；金属粉末，北京蒙泰有研技术开发中心；二甲苯，武汉恒诚化工有限公司；所用试剂均为化学纯；
（2）在装有温度计、搅拌器、分水器和球形冷凝管的500毫升四口烧瓶中，按物质的量比1:2加入辛二酸、季戊四醇，按酸醇总质量的0.5%加入催化剂金属粉末，加热升温；
（3）待物料大部分熔化后，启动搅拌，加入用量为分水器容积110%的二甲苯，继续加热升温；当温度升至136-140摄氏度时，开始出现回流；
（4）调节控温装置控制反应温度在158-162℃；待分水器中液体分层后，及时分离出下层的水，直至分水器中不再有水析出，即得到低聚物中间体；
（5）延续上述实验，通入干燥的氮气赶走反应体系中空气，按油酸与辛二酸物质的量比3:1加入油，加热升温；
（6）当温度升至164-168℃时，开始出现回；调节控温装置控制反应温度为183-187℃，同时使用温棉包裹四口烧瓶；
（7）待分水器中液体分层后，及时分离出下层的水，直至分水器中没有水析出；
（8）打开真空泵切换成减压状态，停止加热，搅拌降温过程中将携水剂二甲苯全部抽出；
（9）冷却至50-60℃后，停止搅拌和通氮气；
（10）静置0.5小时后，即得到棕色半透明液体产物。
Claims (1)
1.一种水基润滑剂用复酯的制备方法，其特征在于包括以下制备步骤：
（1）取以下原料备用：季戊四醇，濮阳华鹏宇化工科技有限公司；辛二酸，常州康隆化工有限公司；油酸，晋州同济油脂化工厂；金属粉末，北京蒙泰有研技术开发中心；二甲苯，武汉恒诚化工有限公司；所用试剂均为化学纯；
（2）在装有温度计、搅拌器、分水器和球形冷凝管的500毫升四口烧瓶中，按物质的量比1:2加入辛二酸、季戊四醇，按酸醇总质量的0.5%加入催化剂金属粉末，加热升温；
（3）待物料大部分熔化后，启动搅拌，加入用量为分水器容积110%的二甲苯，继续加热升温；当温度升至136-140摄氏度时，开始出现回流；
（4）调节控温装置控制反应温度在158-162℃；待分水器中液体分层后，及时分离出下层的水，直至分水器中不再有水析出，即得到低聚物中间体；
（5）延续上述实验，通入干燥的氮气赶走反应体系中空气，按油酸与辛二酸物质的量比3:1加入油，加热升温；
（6）当温度升至164-168℃时，开始出现回；调节控温装置控制反应温度为183-187℃，同时使用温棉包裹四口烧瓶；
（7）待分水器中液体分层后，及时分离出下层的水，直至分水器中没有水析出；
（8）打开真空泵切换成减压状态，停止加热，搅拌降温过程中将携水剂二甲苯全部抽出；
（9）冷却至50-60℃后，停止搅拌和通氮气；
（10）静置0.5小时后，即得到棕色半透明液体产物。
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Application publication date: 20180306 |