CN107382927A - 一种润滑油性剂及其合成方法和应用 - Google Patents

一种润滑油性剂及其合成方法和应用 Download PDF

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CN107382927A
CN107382927A CN201710654454.4A CN201710654454A CN107382927A CN 107382927 A CN107382927 A CN 107382927A CN 201710654454 A CN201710654454 A CN 201710654454A CN 107382927 A CN107382927 A CN 107382927A
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余金
余宪虎
余红杰
黄峰
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Abstract

本发明提供一种润滑油性剂及其合成方法和应用，以二聚酸为核心反应物，将二聚酸的一端羧基用脂肪酸酯改性，使之能在摩擦副表面吸附，另一端羧基用聚乙二醇改性，使之具有水分散性，合成了高沸点粘稠状的脂肪酸聚合物油性剂，再将其作为润滑油性剂和磷酸酯、表面活性剂、增粘剂、缓蚀剂、100#白油、动物油、油酸、三乙醇胺、磷酸酯铵盐、二缩三乙二醇、硅酸钠、水杨酸和氢氧化钠复配形成水基拉丝润滑剂。本发明提供的能分散于水的脂肪酸聚合物油性剂，并将其用于钢丝的高速拉拔，从而保证拉拔过程不断丝、不大模，且生产合成方便。

Description

一种润滑油性剂及其合成方法和应用
技术领域
本发明涉及润滑剂技术领域，具体是一种润滑油性剂及其合成方法和应用。
背景技术
水基拉丝润滑剂具有生物降解性好、冷却效果优良、不燃、易清洗和成本低廉等特点，已成为一种发展趋势。但现有的国内外产品润滑性能均不突出，关键原因是油性剂性能不够完善。因此，研制一种润滑性能优良的油性剂是研制绿色水基拉丝润滑剂的首要问题，也是提高水基拉丝润滑剂质量的关键之一。
油性剂具有降低摩擦的作用，常见的有矿物油、动植物油脂、高级脂肪酸、脂肪醇、脂肪胺、酰胺、脂肪酸酯以及含极性基团的高分子化合物等。作为钢丝帘线拉拔选择油性剂时，要求经过高压拉拔后产生的拉拔残留物有助于钢丝合股和有利于钢丝帘线与橡胶的粘合。
现有的油性剂都是不溶于水的有机化合物，都要通过使用大量的表面活性剂才能将其乳化分散于水中，特别是大分子的油性剂，一般乳化很困难，而且随着使用周期的延长，当润滑剂中表面活性剂消耗或HLB值的变化，这些油性剂就会从水中析出或漂浮出来，降低润滑剂的润滑性，从而造成金属加工生产困难，或断丝或增加拉丝模的增加。
发明内容
针对现有的油性剂润滑效果差，复配乳化困难，需要大量表面活性剂而带来泡沫增多不利于高速拉拔等缺点，开发出一种能分散于水的脂肪酸聚合物油性剂，并将其用于钢丝的高速拉拔，从而保证拉拔过程不断丝、不大模，且生产合成方便。
本发明提供的技术方案：一种润滑油性剂，选自下式的脂肪酸聚合物：
式中：R1为C8烷基，OR2为司盘20基、司盘40基、、司盘60基、司盘80基或单甘脂基，m＝5-25。
进一步的，所述m＝9-23。
一种润滑油性剂的合成方法，包括如下步骤：
(1)以二聚酸和脂肪酸酯为原料，再加入聚乙二醇，反应器内在氮气保护下混合升温至90℃，再加入对甲苯磺酸，120℃下保温1h，然后升温至180℃保温使之进行脱水反应，通过油水分离器分出水；
(2)将步骤(1)所得的产物减压抽滤，再蒸发浓缩得到所述的润滑油性剂。
进一步的，所述步骤(1)中二聚酸、脂肪酸酯与聚乙二醇的反应时的mol比为1:1.18:0.87。
进一步的，所述脂肪酸酯为司盘20、司盘40、司盘60、司盘80或单甘脂。
进一步的，所述聚乙二醇的数均分子量为300-2000。
进一步的，所述润滑油性剂的合成方法，包括如下步骤：
(1)分别取二聚酸280.5克、司盘80 252.8克和435克数均分子量为1000的聚乙二醇加到反应器内，在氮气保护下混合升温至90℃，加入6.7克对甲苯磺酸，120℃下保温1h，然后升温至180℃保温使之进行脱水反应，待油水分离器分出水量达到12克及以上时终止反应；
(2)将步骤(1)所得的产物减压抽滤，再蒸发浓缩得到所述的润滑油性剂。
一种润滑油性剂的应用，将所述润滑油性剂用于制备润滑剂，所述润滑剂由以下原料按照质量分数配置而成：润滑油性剂15～18％，MOA-4P磷酸酯6～9％，表面活性剂3～4％，增粘剂0.5～0.7％，B-VCI防锈剂1～3％，100号白油5～10％，动物油4～6％，油酸2～4％，三乙醇胺1～3％，磷酸酯胺盐3～5％，二缩三乙二醇1～3％，硅酸钠0.3～0.8％，水杨酸0.3～0.5％，氢氧化钠0.1～0.8％，余量为水，各组分的质量分数之和为100％。
进一步的，所述表面活性剂由吐温80和司盘80以质量比3:1的比例配置而成。
进一步的，所述增粘剂为1-羟甲基苯三唑磷酸酯乙二胺盐，以苯并三氮唑、甲醛、P2O5和乙二胺为原料通过化学合成的方式制得。
所述润滑油性剂和增粘剂在实验室通过化学合成的方式制得，其他原料均通过购买得到。
本发明的有益效果：(1)将合成的脂肪酸聚合物用作润滑油性剂，所述润滑油性剂可自乳化，减少了润滑剂中表面活性剂的用量，将其用于轮胎镀铜钢丝的高速拉拔，具有生物降解性好、润滑冷却效果优良、不燃、易清洗和成本低廉等特点。
(2)司盘80和吐温80为分子结构为多分支的表面活性剂，具有一定的界面吸附成膜的特性，容易在固液界面生成润滑膜；同时，二者分别为亲油性和亲水性表面活性剂，可以在油水界面上吸附，参与液液界面膜的形成，将两者复配形成功能效果更好的乳化剂。所述MOA-4P磷酸酯用作抗磨剂，增加润滑剂的使用寿命，三乙醇胺用于润滑油的抗腐蚀添加剂，用作防锈剂，磷酸酯胺盐用作极压剂，在高温下与金属表面形成化学润滑膜，二缩三乙二醇用作偶联剂，延缓老化，硅酸钠用作阻垢剂，水杨酸用作杀菌剂，氢氧化钠用于pH调节，将各种功能效果好的原料复配形成润滑剂，具有超级润滑、减磨、抗极压，易被微生物降解，有利于环境的保护。
附图说明
图1是本发明的润滑油性剂的化学结构式；
图2是本发明实施例一的润滑油性剂的化学结构式；
图3是本发明实施例二的润滑油性剂的化学结构式；
图4是本发明实施例三的润滑油性剂的化学结构式；
图5是本发明实施例四的润滑油性剂的化学结构式；
图6是本发明实施例四的润滑油性剂的化学结构式；
图7是本发明的润滑油性剂的化学合成反应式一，其中脂肪酸酯为司盘。
图8是本发明的润滑油性剂的化学合成反应式二，其中脂肪酸酯为单甘脂。
具体实施方式
下面结合附图和具体实施例对本发明做进一步的说明。
以下实施例中所用增粘剂为1-羟甲基苯三唑磷酸酯乙二胺盐，以苯并三氮唑、甲醛为原料先合成得到1-羟甲基苯并三氮唑，再与P2O5和乙二胺合成制得1-羟甲基苯三唑磷酸酯乙二胺盐。所述司盘80为脱水山梨醇单油酸酯，所述司盘60为脱水山梨醇单硬脂酸酯，所述司盘40为脱水山梨醇单棕榈酸酯，所述司盘20为脱水山梨醇单月桂酸酯，所述单甘脂为单硬脂酸酯。
实施例一
(1)分别取二聚酸280.5克、司盘80 252.8克和435克的数均分子量为1000的聚乙二醇加到反应器内，在氮气保护下混合升温至90℃，加入6.7克对甲苯磺酸，120℃下保温1h，然后升温至180℃保温使之进行脱水反应，待油水分离器分出水量达到12克及以上时终止反应；
(2)将步骤(1)所得的产物减压抽滤，再蒸发浓缩得到所述的润滑油性剂；所得润滑油性剂的化学结构式如图2所示。
将制备得到的润滑油性剂和增粘剂用于制备润滑剂，所述润滑剂由以下原料按照质量分数配置而成：润滑油性剂16％，MOA-4P磷酸酯7％，表面活性剂3.2％，抗氧增粘剂0.55％，B-VCI防锈剂1.5％，100号白油7％，动物油4.5％，油酸2.5％，三乙醇胺1.5％，磷酸酯胺盐4％，二缩三乙二醇1％，硅酸钠0.6％，水杨酸0.3％，氢氧化钠0.1％，余量为水，各组分的质量分数之和为100％。
实施例二
分别取二聚酸280.5克、司盘20 204.4克和130.5克的数均分子量为300的聚乙二醇加到反应器内，在氮气保护下混合升温至90℃，加入6.7克对甲苯磺酸，120℃下保温1h，然后升温至180℃保温使之进行脱水反应，待油水分离器分出水量达到12克及以上时终止反应；将所得的产物减压抽滤，再蒸发浓缩得到所述的润滑油性剂；所得润滑油性剂的化学结构式如图3所示。
将制备得到的润滑油性剂，用于制备润滑剂，所述润滑剂由以下原料按照质量分数配置而成：润滑油性剂18％，MOA-4P磷酸酯9％，表面活性剂4％，增粘剂0.7％，B-VCI防锈剂3％，100号白油10％，动物油6％，油酸4％，三乙醇胺3％，磷酸酯胺盐5％，二缩三乙二醇3％，硅酸钠0.8％，水杨酸0.5％，氢氧化钠0.8％，余量为水，各组分的质量分数之和为100％。
实施例三
分别取二聚酸280.5克、司盘40 237.6克和174克的数均分子量为400的聚乙二醇加到反应器内，在氮气保护下混合升温至90℃，加入6.7克对甲苯磺酸，120℃下保温1h，然后升温至180℃保温使之进行脱水反应，待油水分离器分出水量达到12克及以上时终止反应；将所得的产物减压抽滤，再蒸发浓缩得到所述的润滑油性剂；所得润滑油性剂的化学结构式如图4所示。
将制备得到的润滑油性剂，用于制备润滑剂，所述润滑剂由以下原料按照质量分数配置而成：润滑油性剂16％，MOA-4P磷酸酯7％，表面活性剂3.3％，增粘剂0.55％，B-VCI防锈剂1.5％，100号白油6％，动物油4.5％，油酸2.5％，三乙醇胺1.5％，磷酸酯胺盐3.5％，二缩三乙二醇1.8％，硅酸钠0.5％，水杨酸0.34％，氢氧化钠0.3％，余量为水，各组分的质量分数之和为100％。
实施例四
分别取二聚酸280.5克、司盘60 254克和267克的数均分子量为600的聚乙二醇加到反应器内，在氮气保护下混合升温至90℃，加入6.7克对甲苯磺酸，120℃下保温1h，然后升温至180℃保温使之进行脱水反应，待油水分离器分出水量达到12克及以上时终止反应；将所得的产物减压抽滤，再蒸发浓缩得到所述的润滑油性剂；所得润滑油性剂的化学结构式如图5所示。
将制备得到的润滑油性剂，用于制备润滑剂，所述润滑剂由以下原料按照质量分数配置而成：润滑油性剂17％，MOA-4P磷酸酯8％，表面活性剂3.5％，增粘剂0.6％，B-VCI防锈剂2％，100号白油8％，动物油5％，油酸3％，三乙醇胺2％，磷酸酯胺盐4％，二缩三乙二醇2％，硅酸钠0.6％，水杨酸0.4％，氢氧化钠0.5％，余量为水，各组分的质量分数之和为100％。
实施例五
分别取二聚酸280.5克、单硬脂酸酯211.6克和522克的数均分子量为1500的聚乙二醇加到反应器内，在氮气保护下混合升温至90℃，加入6.7克对甲苯磺酸，120℃下保温1h，然后升温至180℃保温使之进行脱水反应，待油水分离器分出水量达到12克及以上时终止反应；将所得的产物减压抽滤，再蒸发浓缩得到所述的润滑油性剂；所得润滑油性剂的化学结构式如图6所示。
将制备得到的润滑油性剂，用于制备润滑剂，所述润滑剂由以下原料按照质量分数配置而成：润滑油性剂16.5％，MOA-4P磷酸酯7.5％，表面活性剂3.8％，增粘剂0.65％，B-VCI防锈剂2.5％，100号白油9％，动物油5.5％，油酸3.5％，三乙醇胺2.5％，磷酸酯胺盐4.5％，二缩三乙二醇2.5％，硅酸钠0.7％，水杨酸0.45％，氢氧化钠0.7％，余量为水，各组分的质量分数之和为100％。
将本发明制得的润滑剂进行防腐蚀试验，与购买得到的ADMUV2润滑液和VSV77R润滑液进行对比，试验结果如表1所示，结果表明，本发明制得的润滑剂相对于对照例具有更好的防腐蚀效果。
表1防腐蚀试验结果
将本发明制得的润滑剂用于钢丝帘线拉拔，与购买得到的ADMU V2润滑液和VSV77R润滑液进行对比，试验结果如表2所示，本发明的拉拔速度达到15-16m/s，粘合力达到1750N，本发明制得的润滑剂具有生物降解性好、润滑冷却效果优良、不燃、易清洗和成本低廉等特点。
表2工业生产应用
以上所述仅为本发明的具体实施方案的详细描述，并不以此限制本发明，凡在本发明的设计思路上所作的任何修改、等同替换和改进等，均应包含在本发明的保护范围之内。

Claims (10)

1.一种润滑油性剂，其特征在于：选自下式的脂肪酸聚合物：
式中：R1为C8烷基，OR2为司盘20基、司盘40基、、司盘60基、司盘80基或单甘脂基中的任意一种，m＝5-25。
2.根据权利要求1所述的润滑油性剂，其特征在于：所述m＝9-23。
3.制备如权利要求1所述的润滑油性剂的合成方法，其特征在于包括如下步骤：
(1)以二聚酸和脂肪酸酯为原料，再加聚乙二醇进入反应器内，在氮气保护下混合升温至90℃，再加入对甲苯磺酸，120℃下保温1h，然后升温至180℃保温使之进行脱水反应，通过油水分离器分出水；
(2)将步骤(1)所得的产物减压抽滤，再蒸发浓缩得到所述的润滑油性剂。
4.根据权利要求3所述的润滑油性剂的合成方法，其特征在于：所述步骤(1)中二聚酸、脂肪酸酯与聚乙二醇的反应时的mol比为1:1.18:0.87。
5.根据权利要求3或4所述的润滑油性剂的合成方法，其特征在于：所述脂肪酸酯为司盘20、司盘40、司盘60、司盘80和单甘脂中的任意一种。
6.根据权利要求3所述的润滑油性剂的合成方法，其特征在于：所述聚乙二醇的数均分子量为300-2000。
7.根据权利要求3所述润滑油性剂的合成方法，其特征在于包括如下步骤：
(1)分别取二聚酸280.5克、司盘80 252.8克和435克的数均分子量为1000的聚乙二醇加到反应器内，在氮气保护下混合升温至90℃，加入6.7克对甲苯磺酸，120℃下保温1h，然后升温至180℃保温使之进行脱水反应，待油水分离器分出水量达到12克及以上时终止反应；
(2)将步骤(1)所得的产物减压抽滤，再蒸发浓缩得到所述的润滑油性剂。
8.根据权利要求1-3任一项所述的润滑油性剂的应用，其特征在于：将所述润滑油性剂用于制备润滑剂，所述润滑剂由以下原料按照质量分数配置而成：润滑油性剂15～18％，MOA-4P磷酸酯6～9％，表面活性剂3～4％，增粘剂0.5～0.7％，B-VCI防锈剂1～3％，100号白油5～10％，动物油4～6％，油酸2～4％，三乙醇胺1～3％，磷酸酯胺盐3～5％，二缩三乙二醇1～3％，硅酸钠0.3～0.8％，水杨酸0.3～0.5％，氢氧化钠0.1～0.8％，余量为水，各组分的质量分数之和为100％。
9.根据权利要求8所述的润滑油性剂的应用，其特征在于：所述表面活性剂由吐温80和司盘80以质量比3:1的比例配置而成。
10.根据权利要求8所述的润滑油性剂的应用，其特征在于：所述增粘剂为1-羟甲基苯三唑磷酸酯乙二胺盐，以苯并三氮唑、甲醛、P2O5和乙二胺为原料通过化学合成的方式制得。
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