CN111423920A - 一种高滴点高机械稳定性复合锂基脂及其制备工艺 - Google Patents

一种高滴点高机械稳定性复合锂基脂及其制备工艺 Download PDF

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CN111423920A
CN111423920A CN202010306042.3A CN202010306042A CN111423920A CN 111423920 A CN111423920 A CN 111423920A CN 202010306042 A CN202010306042 A CN 202010306042A CN 111423920 A CN111423920 A CN 111423920A
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mechanical stability
grease
dropping point
lithium
base oil
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艾罡
万书晓
万如月
张博雯
乔小华
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Grtf Lubechemy International Ltd
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Abstract

本发明涉及润滑脂技术领域，具体涉及一种高滴点高机械稳定性复合锂基脂及其制备工艺，其原料包括：基础油、壬二酸、12‑羟基硬脂酸、稠化剂、抗氧剂、防腐防锈剂、极压抗磨剂、粘度改进剂；所述壬二酸的纯度≧92％。与现有技术相比，本发明所提供的高滴点高机械稳定性复合锂基脂的制备方法，通过引入高纯度的壬二酸，同时改进壬二酸的添加工艺，使得皂化反应体系由固液反应方式转变为液液反应，大大提升了反应速率的同时使得反应体系的传质传热效果提高，避免局部过热，反应温度易控制，减少凝胶效应的发生，提高了整体复合反应的效率。本发明制备的复合锂基脂具有更高的滴点和优良的高温性能，具有更好的机械安定性，使用寿命长。

Description

一种高滴点高机械稳定性复合锂基脂及其制备工艺
技术领域
本发明涉及润滑脂技术领域，具体涉及一种高滴点高机械稳定性复合锂基脂及其制备工艺。
背景技术
润滑脂属于润滑剂的范畴，是一种稠状的油脂状半固体，主要由基础油、稠化剂以及少量的添加剂组成，用于机械轴承间的摩擦部分，起润滑和密封作用，有的也用于金属表面，起填充空隙和防锈作用。润滑脂在机械工作中，受到剪切力的作用后皂纤维会脱开或断裂，造成润滑脂稠度下降。理想的润滑脂--受剪切后润滑脂稠度变化小，从而获得较长的使用寿命。
复合锂基润滑脂由羟基脂肪酸锂皂与低分子酸(二元或三元酸)锂盐复合生成的复合皂稠化基础油并加入添加剂制备的润滑脂，具有优异的高温性能，可以用于汽车、钢铁、铁路、航空等多个领域，是一种多效、长寿命润滑脂。且在润滑脂中所占比例呈逐年上升的趋势，目前国内生产复合锂基润滑脂主要采用12-羟基硬脂酸-癸二酸体系，也有少部分采用12-羟基硬脂酸-硼酸体系。目前国内大多数复合锂基润滑脂能够做到滴点在260以上，但是在不添加结构改善剂或其它添加剂的情况下，均存在机械安定性差(十万次剪切锥入度变化值大于25)的问题。
发明内容
为了克服上述技术缺陷的不足，本发明提供了一种高滴点高机械稳定性复合锂基脂及其制备工艺。
一种高滴点高机械稳定性复合锂基脂，关键在于其原料组分按质量分数计包括：基础油72～87％、壬二酸1-5％、12-羟基硬脂酸8-10％、稠化剂2-5％、抗氧剂0.5～1％、防腐防锈剂0.5～1％、极压抗磨剂0.5～3％、粘度改进剂0.5～3％；所述壬二酸的纯度≧92％。
所述基础油为LP101M、PE1350、PAO-8、150BS、500N、900N、4010、4006中的一种或几种混合，LP101M和PE1350均为广研德孚(深圳)科技发展有限公司的产品，LP101M(CAS:15834-06-7)、PE1350(CAS:128218-61-3)，PAO-8、150BS、500N、900N、4010和4006均为市购基础油。
所述稠化剂为一水氢氧化锂、无水氢氧化钙中的一种或两种混合。
所述抗氧化剂为二苯胺、苯基-α-萘胺、N,N-二仲丁基对苯二胺中的一种或几种混合。
所述防腐防锈剂为石油磺酸钡、石油磺酸钙、磷酸三钠苯并三氮唑中的一种或几种混合。
所述极压抗磨剂为硫化异丁烯、亚磷酸二正丁酯、硫化棉籽油中的一种或几种混合；所述粘度改进剂为聚甲基丙烯酸甲酯、聚异丁烯、三元乙丙胶中的一种或几种混合。
一种高滴点高机械稳定性复合锂基脂的制备方法，关键在于包括以下步骤：
步骤一、将部分基础油投入反应釜中，升温至60.0～70.0℃，投入12-羟基硬脂酸、一水氢氧化锂和水，搅拌并继续升温；
步骤二、当升温至80～90℃，将壬二酸水溶液边搅拌边缓慢加入到反应釜中，进行皂化反应；
步骤三、升温至130～210℃进行复合反应及高温炼制；
步骤四、加入剩余基础油进行降温至80-100℃，加入抗氧剂、防腐防锈剂、极压抗磨剂和粘度改进剂，搅拌均匀，得到成品。
优选的，所述步骤一中基础油占基础油总量的40-60％，所述步骤四中基础油占基础油总量的10-20％。
优选的，所述步骤二中壬二酸水溶液温度为80-90℃。
优选的，步骤三具体为：升温至130～140℃，恒温恒压反应60-120min后，开始泄压直至压力为零，然后升温至160.0℃左右，加入部分基础油，继续升温至205～210℃，保温5～10min。
有益效果是：与现有技术相比，本发明所提供的一种高滴点高机械稳定性复合锂基脂的制备方法，通过引入高纯度的壬二酸，同时改进壬二酸的添加工艺，使反应更充分高效，有助于复合反应的进行，在制备复合锂的过程中，先将壬二酸完全溶解在水中，然后通过滴加的方式参与皂化反应，使得皂化反应体系由固液反应方式转变为液液反应，大大提升了反应速率的同时使得反应体系的传质传热效果提高，避免局部过热，反应温度易控制，减少凝胶效应的发生--形成的壬二酸锂皂的结构更加均匀规整，下一阶段复合反应中更易复合的同时形成的复合皂纤维结构也更加的均匀规整，从而提高了润滑脂的机械安定性能；另外壬二酸溶液与碱金属溶液的充分反应使得复合时有更多的壬二酸锂皂能够参与下一阶段复合反应，提高了整体复合反应的效率，减少复合反应的时间，从而降低能耗。本发明制备的复合锂基脂具有更高的滴点和优良的高温性能，具有更好的机械安定性，轴承漏失量小，使用寿命长。
具体实施方法
为使本领域技术人员更好的理解本发明的技术方案，下面结合附表和具体实施方式对本发明作详细说明。
实施例1复合锂基脂I
各原料为：28.6％150BS、50.2％4010、5％LP101M、2.6％壬二酸、7.4％12-羟基硬脂酸、2.2％一水氢氧化锂、0.8％二苯胺、0.7％石油磺酸钡、1％硫化异丁烯、1.5％聚甲基丙烯酸甲酯。
制备工艺：将占基础油总量的40％的基础油投入反应釜中，升温至60.0～70.0℃，投入12-羟基硬脂酸、一水氢氧化锂和水，搅拌并继续升温；当升温至80～90℃，将温度为80-90℃为壬二酸水溶液边搅拌边缓慢加入到反应釜中，进行皂化反应；升温至130～140℃，恒温恒压反应60-120min后，开始泄压直至压力为零，然后升温至160.0℃左右，加入占基础油总量的40％的基础油，继续升温至205～210℃，保温5～10min；加入占基础油总量的20％的基础油进行降温至80-100℃，加入二苯胺、石油磺酸钡、硫化异丁烯和聚甲基丙烯酸甲酯，搅拌均匀，得到复合锂基脂I。
实施例2复合锂基脂II
各原料为：74.0％500N、7.0％PE1350、2.2％壬二酸、8.5％12-羟基硬脂酸、2.3％一水氢氧化锂、0.5％苯基-α-萘胺、1％石油磺酸钙钡、3％亚磷酸二正丁酯、1.5％聚异丁烯。
制备工艺：将占基础油总量的60％的基础油投入反应釜中，升温至60.0～70.0℃，投入12-羟基硬脂酸、一水氢氧化锂和水，搅拌并继续升温；当升温至80～90℃，将温度为80-90℃为壬二酸水溶液边搅拌边缓慢加入到反应釜中，进行皂化反应；升温至130～140℃，恒温恒压反应60-120min后，开始泄压直至压力为零，然后升温至160.0℃左右，加入占基础油总量的30％的基础油，继续升温至205～210℃，保温5～10min；加入占基础油总量的10％的基础油进行降温至80-100℃，加入苯基-α-萘胺、石油磺酸钙钡、亚磷酸二正丁酯、聚异丁烯，搅拌均匀，得到复合锂基脂II。
实施例3复合锂基脂III
各原料为：39％PAO-8、27％150BS、6％PE1350、5％壬二酸、10％12-羟基硬脂酸、5％一水氢氧化锂、1％N,N-二仲丁基对苯二胺、1％磷酸三钠苯并三氮唑、3％硫化棉籽油、3％三元乙丙胶。
制备工艺与实施例1相同。
实施例4复合锂基脂IV
各原料为：46％4010、36％4006、5％LP101M、1％壬二酸、8％12-羟基硬脂酸、2％一水氢氧化锂、0.5％N,N-二仲丁基对苯二胺、0.5％磷酸三钠苯并三氮唑、0.5％硫化棉籽油、0.5％三元乙丙胶。
制备工艺与实施例2相同。
对比实施例5锂基脂V
各原料和制备工艺均与实施例1相同，区别在于壬二酸的纯度为70％。
对比实施例6锂基脂VI
各原料和制备工艺均与实施例1相同，区别在于用癸二酸代替壬二酸。
对比实施例7锂基脂VII
各原料与实施例1相同，区别在于用癸二酸代替壬二酸。
制备工艺为：
将占基础油总量的40％的基础油投入反应釜中，升温至80～90℃，投入12-羟基硬脂酸、一水氢氧化锂、水和癸二酸进行皂化反应；然后加入占基础油总量的40％的基础油，最高升温到210℃进行高温炼制，然后冷却到180℃，降温至100℃加入二苯胺、石油磺酸钡、硫化异丁烯和聚甲基丙烯酸甲酯，然后用均质机或循环剪切进行后处理，过滤，包装。
对各实施例制备得到的复合锂基脂I-IV及对比实施例制备得到的锂基脂V-VII进行如下性能测试：
Figure BDA0002455820690000061
从上表中可以看到，本发明制备的复合锂基脂I-V的滴点高，锥入度变化值介于12-14之间，机械安定性好，使用寿命长。
最后需要说明，上述描述仅为本发明的优选实施例，本领域的技术人员在本发明的启示下，在不违背本发明宗旨及权利要求的前提下，可以做出多种类似的表示，这样的变换均落入本发明的保护范围之内。

Claims (10)

1.一种高滴点高机械稳定性复合锂基脂，其特征在于其原料组分按质量分数计包括：基础油72～87％、壬二酸1-5％、12-羟基硬脂酸8-10％、稠化剂2-5％、抗氧剂0.5～1％、防腐防锈剂0.5～1％、极压抗磨剂0.5～3％、粘度改进剂0.5～3％；所述壬二酸的纯度≧92％。
2.根据权利要求1所述一种高滴点高机械稳定性复合锂基脂，其特征在于：所述基础油为LP101M、PE1350、PAO-8、150BS、500N、900N、4010、4006中的一种或几种混合。
3.根据权利要求1所述一种高滴点高机械稳定性复合锂基脂，其特征在于：所述稠化剂为一水氢氧化锂、无水氢氧化钙中的一种或两种混合。
4.根据权利要求1所述一种高滴点高机械稳定性复合锂基脂，其特征在于：所述抗氧化剂为二苯胺、苯基-α-萘胺、N,N-二仲丁基对苯二胺中的一种或几种混合。
5.根据权利要求1所述一种高滴点高机械稳定性复合锂基脂，其特征在于：所述防腐防锈剂为石油磺酸钡、石油磺酸钙、磷酸三钠苯并三氮唑中的一种或几种混合。
6.根据权利要求1所述一种高滴点高机械稳定性复合锂基脂，其特征在于：所述极压抗磨剂为硫化异丁烯、亚磷酸二正丁酯、硫化棉籽油中的一种或几种混合；所述粘度改进剂为聚甲基丙烯酸甲酯、聚异丁烯、三元乙丙胶中的一种或几种混合。
7.一种高滴点高机械稳定性复合锂基脂的制备方法，其特征在于包括以下步骤：
步骤一、将部分基础油投入反应釜中，升温至60.0～70.0℃，投入12-羟基硬脂酸、一水氢氧化锂和水，搅拌并继续升温；
步骤二、当升温至80～90℃，将壬二酸水溶液边搅拌边缓慢加入到反应釜中，进行皂化反应；
步骤三、升温至130～210℃进行复合反应及高温炼制；
步骤四、加入剩余基础油进行降温至80-100℃，加入抗氧剂、防腐防锈剂、极压抗磨剂和粘度改进剂，搅拌均匀，得到成品。
8.根据权利要求8所述的一种高滴点高机械稳定性复合锂基脂的制备方法，其特征在于：所述步骤一中基础油占基础油总量的40-60％，所述步骤四中基础油占基础油总量的10-20％。
9.根据权利要求8所述的一种高滴点高机械稳定性复合锂基脂的制备方法，其特征在于：所述步骤二中壬二酸水溶液温度为80-90℃。
10.根据权利要求8所述的一种高滴点高机械稳定性复合锂基脂的制备方法，其特征在于步骤三具体为：升温至130～140℃，恒温恒压反应60-120min后，开始泄压直至压力为零，然后升温至160.0℃左右，加入部分基础油，继续升温至205～210℃，保温5～10min。
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