CN111718773A - 一种聚脲稠化剂及其所得的润滑脂和润滑脂的制备方法 - Google Patents

一种聚脲稠化剂及其所得的润滑脂和润滑脂的制备方法 Download PDF

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CN111718773A
CN111718773A CN202010684643.8A CN202010684643A CN111718773A CN 111718773 A CN111718773 A CN 111718773A CN 202010684643 A CN202010684643 A CN 202010684643A CN 111718773 A CN111718773 A CN 111718773A
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polyurea
thickening agent
lubricating grease
base oil
oil
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王晓波
徐状
王卓群
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Qingdao Center Of Resource Chemistry & New Materials (qingdao Research Development Center Lanzhou Institute Of Chemical Physics Chinese Academy Of Sciences)
Lanzhou Institute of Chemical Physics LICP of CAS
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Abstract

本发明提供一种聚脲稠化剂及其所得的润滑脂和润滑脂的制备方法，涉及润滑材料技术领域。该聚脲基润滑脂包括如下重量百分比的组分：基础油69.2～89.8％，聚脲稠化剂10～25％，抗氧剂0‑5％，防锈剂0.2～0.8％，所述聚脲稠化剂采用二苯基甲烷‑4,4’‑二异氰酸酯和2‑氨基‑6‑甲氧基苯并噻唑或混合胺合成，所述混合胺为2‑氨基‑6‑甲氧基苯并噻唑和结构式为R‑NH2的混合物，其中，R为碳原子数为8‑22的烷基或环烷基。本发明制备的聚脲润滑脂采用新型具有极压性能的聚脲稠化剂，与现有的聚脲润滑脂技术相比，不用添加极压剂，且具有良好的极压性能，减少添加剂的种类和用量，能够广泛应用于轴承润滑领域。

Description

一种聚脲稠化剂及其所得的润滑脂和润滑脂的制备方法
技术领域
本发明涉及轴承润滑材料技术领域，特别的涉及具有极压性能脲基稠化剂，包含该聚脲稠化剂的润滑脂及其制备方法。
背景技术
聚脲润滑脂，由于稠化剂体系中不含金属阳离子，避免对基础油及其稠化剂体系的催化氧化作用，所以具有优良的抗氧化性能，被应用于航空、冶金和汽车等高温润滑工况，被认为是未来最具有发展潜力的润滑脂。但是，聚脲润滑脂的润滑性能较差，且对润滑添加剂的适应性较差，极大的限制了其更广泛的应用。
目前，改善聚脲润滑脂的润滑性能一般有两种方法，即添加具有润滑性能的添加剂法和制备复合型的聚脲润滑脂。添加润滑添加剂是最常用的一种方法，通过添加含有S、P元素的极压剂或固体添加剂改善其润滑性能，专利CN 106147941A和CN 103289787A通过添加二烷基二硫代磷酸锌、硫化烯烃、二硫化钨等添加剂改善了聚脲润滑脂的极压性能，但是，为获得较好的极压性能需要通过开展大量添加剂种类和复配方案的研究。通过制备复合型的聚脲润滑脂也可改善其极压性能，专利US3846315(A)中提供了一种在聚脲润滑脂中通过引入碱金属羧酸化合物制备复合聚脲润滑脂的方法，改善了聚脲润滑脂的极压性能，但制备工艺复杂。
发明内容
本发明提供一种制备工艺简单的聚脲稠化剂、包含聚脲稠化剂的润滑脂及其制备方法，解决了现有技术中改善聚脲润滑脂润滑性能工艺复杂，需要进行大量添加剂种类和复配方法研究的技术问题。
本发明是这样实现的：
一种聚脲稠化剂，该聚脲稠化剂是由二苯基甲烷-4,4’-二异氰酸酯和2-氨基-6-甲氧基苯并噻唑或混合胺合成，所述混合胺为2-氨基-6-甲氧基苯并噻唑和结构式为R-NH2的混合物，其中，R为碳原子数为8-22的烷基或环烷基。
作为一种优选的实施方案，所述聚聚脲稠化剂的化学式为化学结构式Ⅰ，或化学结构式Ⅰ、Ⅱ和Ⅲ的混合物，所述化学结构式Ⅰ、Ⅱ和Ⅲ如下。
含有聚脲稠化剂的聚脲润滑脂，包括以下重量百分比的组分：基
Figure BDA0002587101130000021
础油69.2～89.8％，聚脲稠化剂10～25％，抗氧剂0～5％，防锈剂0.2～0.8％。
作为一种优选的实施方案，合成酯类基础油或混合油，所述混合油为合成酯类基础油与矿物油、聚α烯烃、烷基萘、植物油中的一种或几种混合，所述基础油40℃的运动粘度为20～500mm2/s。
作为一种优选的实施方案，所述抗氧剂添加量为1～2.5％。
作为一种优选的实施方案，所述抗氧剂为烷基二苯胺、N-苯基α-萘胺、二辛基二苯胺中的一种或几种。
作为一种优选的实施方案，所述防锈剂的添加量为0.3～0.6％。
作为一种优选的实施方案，所述防锈剂为石油磺酸钡、石油磺酸钠、二壬基萘磺酸钡、环烷酸锌、脂肪酸胺、苯并三氮唑中的一种或几种。
聚脲润滑脂的制备方法，包括如下步骤：
1)将部分基础油和2-氨基-6-甲氧基苯并噻唑或混合胺加入反应釜中，升温至95～105℃搅拌30min，在溶解釜中加入部分基础油和二苯基甲烷-4,4’-二异氰酸酯，升温至80℃搅拌30min，然后将溶解釜中的混合物加入到反应釜中，升温到80～140℃，反应时间30～120min；
(2)升温至160～220℃，炼化时间20～120min，降温冷却至70℃，加入余下的基础油，及抗氧剂和防锈剂，均质、过滤和脱气处理后即得成品。
作为一种优选的实施方案，所述步骤(1)中的反应温度为85-135℃，反应时间40～90min；所述步骤(2)中的炼化温度为170-210℃，炼化时间30～100min。
本发明的有益效果：本发明采用具有极压性能的聚脲稠化剂制备聚脲润滑脂，所制备的聚脲润滑脂无需添加极压剂，具有良好的极压性能，减少聚脲润滑脂添加剂的种类和使用量，且制备工艺简单。
具体实施方式
下面将结合本发明实施例，对本发明的技术方案进行清楚、完整地描述，显然，所描述的实施例仅是本发明一部分实施例，而不是全部的实施例。基于本发明中的实施例，本领域普通技术人员在没有作出创造性劳动前提下所获得的所有其他实施例，都属于本发明保护的范围。
实施例1
在5L的反应釜中加入1490g季戊四醇酯类油和301.02g 2-氨基-6-甲氧基苯并噻唑，开启搅拌并升温至95℃，保温搅拌30min；在5L的溶解釜中加入1000g季戊四醇酯类油和229.88二苯基甲烷-4,4’-二异氰酸酯，开启搅拌升温至80℃，保温搅拌30min；然后将溶解釜中的混合物加入到反应釜中，升温至100℃，保温反应120min，再升温至160℃，炼化120min；冷却降温至70℃，添加抗氧剂烷基二苯胺30g，防锈剂石油磺酸钡9g，均质、过滤、脱气后得到最终产品约3kg。
其中，所述季戊四醇酯类油40℃的运动粘度为20～500mm2/s。
实施例2
在5L的反应釜中加入894g季戊四醇酯类油、298g菜籽油和298g烷基萘-15，182.86g 2-氨基-6-甲氧基苯并噻唑和136.72g的十八胺，开启搅拌并升温至100℃，保温搅拌30min；在5L的溶解釜中加入600g季戊四醇酯酯类油、200g菜籽油、200g烷基萘-15和209.74g二苯基甲烷-4,4’-二异氰酸酯，开启搅拌升温至80℃，保温搅拌30min；然后将溶解釜中的混合物加入到反应釜中，升温至110℃，保温反应60min，再升温至170℃，炼化100min；冷却降温至70℃，添加抗氧剂N-苯基α-萘胺45g，防锈剂二壬基萘磺酸钡15g，均质、过滤、脱气后得到最终产品约3kg。
其中，所述季戊四醇酯类油、菜籽油与烷基萘-1540℃的运动粘度为20～500mm2/s。
实施例3
在5L的反应釜中加入1043g季戊四醇酯类油、298g基础油MVI500和149g的聚α烯烃(PAO10)，235.60g 2-氨基-6-甲氧基苯并噻唑和56.31g的辛胺，开启搅拌并升温至100℃，保温搅拌30min；在5L的溶解釜中加入700g季戊四醇酯酯类油、200g基础油MVI500、100g的聚α烯烃(PAO10)和239.90g二苯基甲烷-4,4’-二异氰酸酯，开启搅拌升温至80℃，保温搅拌30min；然后将溶解釜中的混合物加入到反应釜中，升温至115℃，保温反应50min，再升温至210℃，炼化30min；冷却降温至70℃，添加抗氧剂二辛基二苯胺25g和N-苯基α-萘胺20g，防锈剂苯并三氮唑9g和，均质、过滤、脱气后得到最终产品约3kg。
其中，所述季戊四醇酯类油、基础油MVI500和PAO1040℃的运动粘度为20～500mm2/s。
实施例4
在5L的反应釜中加入894g季戊四醇酯类油、447g菜籽油和149g的基础油120BS，243.10g 2-氨基-6-甲氧基苯并噻唑和41.87g的苯胺，开启搅拌并升温至105℃，保温搅拌30min；在5L的溶解釜中加入600g季戊四醇酯类油、300g菜籽油、100g的基础油120BS和247.53g二苯基甲烷-4,4’-二异氰酸酯，开启搅拌升温至80℃，保温搅拌30min；然后将溶解釜中的混合物加入到反应釜中，升温至140℃，保温反应30min，再升温至220℃，炼化20min；冷却降温至70℃，添加抗氧剂二辛基二苯胺75g，防锈剂苯并三氮唑9g和环烷酸锌12g，均质、过滤、脱气后得到最终产品约3kg。
其中，所述季戊四醇酯类油、基础油120BS与菜籽油40℃的运动粘度为20～500mm2/s。
Figure BDA0002587101130000051
实施例1中的聚脲稠化剂的化学结构式为化学结构式Ⅰ，实施例2-4中的聚脲稠化剂为化学结构式Ⅰ、Ⅱ和Ⅲ的混合物，化学结构式Ⅰ、Ⅱ和Ⅲ如下。
对本发明四个实施例所得的聚脲润滑脂进行性能测试，理化性能参见表1。
表1实施例1-4所得聚脲润滑脂的测试数据
测试项目 实施例1 实施例2 实施例3 实施例4 对比样品 测试方法
锥入度/0.1mm) 298 320 331 312 285 GB/T269
滴点/℃ 326 312 296 316 302 GB/T3498
钢网分油/％ 0.26 0.38 0.48 0.32 0.20 SH/T0324
P<sub>B</sub>(四球法)/N 696 490 549 618 274 SH/T0202
P<sub>D</sub>(四球法)/N 1569 1098 1236 1236 785 SH/T0202
注：对比样品是采用化学结构式Ⅲ的聚脲稠化剂制备的润滑脂。
由表1可见，本发明提供的聚脲润滑脂具有良好的极压性能。
以上所述仅为本发明的较佳实施例而已，并不用以限制本发明，凡在本发明的精神和原则之内，所作的任何修改、等同替换、改进等，均应包含在本发明的保护范围之内。

Claims (10)

1.一种聚脲稠化剂，其特征在于，该聚脲稠化剂是由二苯基甲烷-4,4’-二异氰酸酯和2-氨基-6-甲氧基苯并噻唑或混合胺合成，所述混合胺为2-氨基-6-甲氧基苯并噻唑和结构式为R-NH2的混合物，其中，R为碳原子数为8-22的烷基或环烷基。
2.根据权利要求1所述的一种聚脲稠化剂，其特征在于，所述聚聚脲稠化剂的化学式为Ⅰ，或化学结构式Ⅰ、Ⅱ和Ⅲ的混合物，所述化学结构式Ⅰ、Ⅱ和Ⅲ如下。
Figure FDA0002587101120000011
3.含有权利要求1所述的聚脲稠化剂的聚脲润滑脂，其特征在于，包括以下重量百分比的组分：基础油69.2～89.8％，聚脲稠化剂10～25％，抗氧剂0～5％，防锈剂0.2～0.8％。
4.根据权利要求3所述的聚脲润滑脂，其特征在于，所述基础油为合成酯类基础油或混合油，所述混合油为合成酯类基础油与矿物油、聚α烯烃、烷基萘、植物油中的一种或几种混合，所述基础油40℃的运动粘度为20～500mm2/s。
5.根据权利要求3所述的聚脲润滑脂，其特征在于，所述抗氧剂添加量为1～2.5％。
6.根据权利要求5所述的聚脲润滑脂，其特征在于，所述抗氧剂为烷基二苯胺、N-苯基α-萘胺、二辛基二苯胺中的一种或几种。
7.根据权利要求3所述的聚脲润滑脂，其特征在于，所述防锈剂的添加量为0.3～0.6％。
8.根据权利要求7所述的聚脲润滑脂，其特征在于，所述防锈剂为石油磺酸钡、石油磺酸钠、二壬基萘磺酸钡、环烷酸锌、脂肪酸胺、苯并三氮唑中的一种或几种。
9.如权利要求3-8任意一项所述的聚脲润滑脂的制备方法，其特征在于，包括如下步骤：
(1)将部分基础油和2-氨基-6-甲氧基苯并噻唑或混合胺加入反应釜中，升温至95～105℃搅拌30min，在溶解釜中加入部分基础油和二苯基甲烷-4,4’-二异氰酸酯，升温至80℃搅拌30min，然后将溶解釜中的混合物加入到反应釜中，升温到80～140℃，反应时间30～120min；
(2)升温至160～220℃，炼化时间20～120min，降温冷却至70℃，加入余下的基础油，及抗氧剂和防锈剂，均质、过滤和脱气处理后即得成品。
10.根据权利要求9所述的制备方法，其特征在于，所述步骤(1)中的反应温度为85-135℃，反应时间40～90min；所述步骤(2)中的炼化温度为170-210℃，炼化时间30～100min。
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