CN104350135A - 胺封端和羟基端接聚醚分散剂 - Google Patents
胺封端和羟基端接聚醚分散剂 Download PDFInfo
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- CN104350135A CN104350135A CN201380029855.0A CN201380029855A CN104350135A CN 104350135 A CN104350135 A CN 104350135A CN 201380029855 A CN201380029855 A CN 201380029855A CN 104350135 A CN104350135 A CN 104350135A
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- 230000000802 nitrating effect Effects 0.000 description 1
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- 229920000642 polymer Polymers 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 230000000379 polymerizing effect Effects 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
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- UKPBXIFLSVLDPA-UHFFFAOYSA-N propylhydrazine Chemical class CCCNN UKPBXIFLSVLDPA-UHFFFAOYSA-N 0.000 description 1
- 125000004076 pyridyl group Chemical group 0.000 description 1
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- 239000011541 reaction mixture Substances 0.000 description 1
- CQRYARSYNCAZFO-UHFFFAOYSA-N salicyl alcohol Chemical compound OCC1=CC=CC=C1O CQRYARSYNCAZFO-UHFFFAOYSA-N 0.000 description 1
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- 229960001860 salicylate Drugs 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 238000004088 simulation Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000007655 standard test method Methods 0.000 description 1
- 125000000475 sulfinyl group Chemical group [*:2]S([*:1])=O 0.000 description 1
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- 239000011593 sulfur Substances 0.000 description 1
- 230000008961 swelling Effects 0.000 description 1
- 125000001302 tertiary amino group Chemical group 0.000 description 1
- 125000001544 thienyl group Chemical group 0.000 description 1
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- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
Classifications
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- 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
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Abstract
所公开的技术涉及包含聚烯烃酰化剂和胺端基或羟基端接聚醚的反应产物的分散剂组合物。另外，该技术涉及包含分散剂组合物和任选协同增效量的其它分散剂的润滑组合物，以及在发动机和发动机油中使用分散剂组合物的方法。
Description
发明背景
所公开的技术涉及包含聚烯烃酰化剂和胺封端或羟基端接聚醚的反应产物的分散剂组合物。另外，该技术涉及包含分散剂组合物和任选协同增效量的其它分散剂的润滑组合物，以及在发动机和发动机油中使用分散剂组合物的方法。
由发动机油配制剂的热应力产生的沉积物形成是增长的顾虑，当考虑设计更具燃料效率的发动机时尤其如此。效率改进措施例如通过推进更小的油箱尺寸、涡轮增压和执行汽油直喷(GDI)实现。这些效率措施赋予用于润滑发动机的发动机油配制剂更大的热应力。配制剂经历的热应力越大，配制剂形成沉积物的倾向提高，净结果是发动机效率和总寿命损失。
另外，不断限制的排放规章(总是抑制使用带有灰的沉积物控制组分(因为它们可能不可逆地毒害后处理装置))扩大了形成具有低沉积物倾向的有力配制剂的配制挑战。
通常，沉积物用具有例如大于20,000道尔顿的高分子量多胺琥珀酰亚胺分散剂抑制。尽管胺端基和羟基端接聚醚可用于发动机油配制剂中以降低白色油渣倾向，未考虑这类聚醚并入分散剂骨架中作为降低热致沉积物形成、氧化和硝化以及促进TBN保持力和密封改良的方式。
2011年2月24日公开的Barton等人的WO 2011/022317尤其教导了酸如羟基乙酸或乳酸与胺、醇和氨基醇的反应产物。教导了形成的低分子量、高极性组合物充当抗磨剂。
一系列出版物，包括2010年10月19日发行的美国专利Nos.7,816,309、2010年10月26日发行的7,820,605，2011年4月19日发行的7,928,044，Stokes等人，和2010年10月26日发行的美国专利Nos.7,820,604，2010年12月28日发行的7,858,566，2011年11月29日发行的8,067,341，RuheJr.等人，和2009年10月29日公开的U.S.2009/0270531，Ruhe，Jr.，教导了包含至少：(A)至少一种通过自由基共聚得到的共聚物和(B)至少一种胺端基醚化合物的反应产物，以及任选其它化合物的多种组合物。需要新的分散剂技术。
发明概述
发明人现在发现具有改进的性能特征的分散剂组合物。
所公开的技术提供分散剂组合物。该分散剂组合物包含聚烯烃酰化剂和羟基端接或胺端基聚醚的反应产物。
羟基端接或胺端基聚醚可选自由(i)聚乙二醇、(ii)聚丙二醇、(iii)聚氧化烯胺混合物或(iv)其一些组合组成的组。羟基端接或胺端基聚醚还可选自由如下物质组成的组：(i)三甘醇，(ii)二甘醇，(iii)250-350分子量聚乙二醇，(iv)200-350分子量聚四氢呋喃，(v)一种或多种包含衍生自氧化乙烯、氧化丙烯、氧化丁烯或其一些组合的单元的胺封端甘醇的混合物，或者(vi)其一些组合。
在一个实施方案中，分散剂组合物中的聚醚包含衍生自式I的单元：
其中：
R3可以为氢(H)、-R6OH、-R6NH2、-(C＝O)R6、-R6-N(H)C(＝O)R6，或具有1-30个碳原子的烃基，
R4可以为H，或者具有1-10个碳原子的烃基，
R5可以为具有1-6个碳原子的直链或支化烃基，
R6可以为具有1-20个碳原子的烃基，
Y可以为NR7R8、OH、-R6NH2或-R6OH，
R7和R8可独立地为H，或者具有1-50个碳原子且其中至多三分之一的碳原子可以被N取代或者被另一式I聚醚官能化的烃基，且
m可以为1-30的整数。
在另一实施方案中，提供包含分散剂组合物和具有润滑粘度的油的润滑剂组合物。在一个类似的实施方案中，润滑剂组合物可进一步包含聚(异丁烯)(PIB)琥珀酰亚胺。
在其它实施方案中，提供改进发动机中的沉积性能，或者改进发动机中的密封性能的方法，所述方法包括向发动机应用分散剂组合物或包含分散剂组合物的润滑剂组合物。
在又另外的实施方案中，提供改进发动机油中的硝化和氧化性能，和保持发动机油中的TBN的方法，所述方法包括向发动机应用分散剂组合物或包含分散剂组合物的润滑剂组合物。
在另一实施方案中，所述方法可进一步包括向发动机油应用PIB琥珀酰亚胺。
发明详述
下面通过非限定性阐述描述各个优选特征和实施方案。
本发明一方面是包含聚烯烃酰化剂和羟基端接或胺端基聚醚的反应产物的分散剂组合物。
酰化剂为可在酰化反应中提供酰基的化合物。有用的酰化剂或不饱和羧酸反应物通常为羧酸，例如单烯属不饱和C3-C28单羧酸或其酯，或者单烯属不饱和C4-C28二羧酸、其酐或酯。酰化剂的典型实例为例如马来酸、衣康酸、富马酸、肉桂酸、(甲基)丙烯酸及其反应性等价物和衍生物如酐或酯。聚烯烃酰化剂为被至少一种酰化剂官能化的聚烯烃。
聚烯烃可以为均聚物或共聚物。聚烯烃可以为例如常规聚烯烃，例如常规聚异丁烯(PIB)、高亚乙烯基PIB，和烯烃共聚物，例如乙烯-丙烯共聚物。
在一个实施方案中，聚烯烃可以为常规聚烯烃。常规聚烯烃衍生自聚合的C2-C6单烯烃。聚合物可以为均聚物、共聚物或共聚体。优选的聚烯烃为通过使用氯化铝或其它酸催化剂体系使催化裂化器的C4萃余液或者乙烯装置丁烷/丁烯料流聚合而形成的PIB。
以上述方式使用氯化铝制备的聚烯烃称为常规PIB且特征是具有表1中所示的不饱和端基，其中它们的摩尔％估算值基于聚异丁烯的摩尔数。结构如EPO 355 895所示。常规PIB以大量商品名市售，包括来自Exxon的和来自Lubrizol的3104。
表1
聚烯烃也可以为高亚乙烯基聚烯烃，例如高亚乙烯基PIB。如表1所示，高亚乙烯基PIB可表征为具有主要量，通常多于50摩尔％的α-亚乙烯基，通常称为甲基亚乙烯基，和/或β-双键异构体(分别–CH2C(CH3)＝CH2和/或–CH＝C(CH3)2)，和次要量的其它异构体，包括四取代的双键异构体。高亚乙烯基PIB通常可包含大于约50摩尔％、60摩尔％，或者70摩尔％或更大，通常约80摩尔％或更大或者90摩尔％或更大的α-亚乙烯基和/或β-双键异构体，和约1-10摩尔％的四取代双键异构体。在本发明一个实施方案中，高亚乙烯基PIB具有55摩尔％或更大的α-和/或β-亚乙烯基双键异构体含量，在其它实施方案中，具有65摩尔％，或75摩尔％，或者85摩尔％或更大的α-亚乙烯基和/或β-双键异构体含量。高亚乙烯基PIB通过使异丁烯或者含异丁烯组合物与较温和的酸性聚合催化剂如BF3聚合而制备。高亚乙烯基PIB从包括BASF和Texas Petroleum Chemicals的几个厂商市购。
无论是常规还是高亚乙烯基，聚烯烃的数均分子量(Mn)范围可以为约300-10,000或者甚至至多50,000。然而，例如，PIB的优选范围可以为约300-5,000的Mn，最优选的上限Mn可以为约Mn300-2,500，或者300-1,500。一般而言，聚烯烃可由包含约2至约16，或者约2至约8，或者约2至约6个碳原子的可聚合单体制备。通常，可聚合单体包含丙烯、异丁烯、1-丁烯、异戊二烯、1,3-丁二烯或其混合物中的一种或多种。
聚烯烃还可以为至少两种不同烯烃的共聚物，也称为烯烃共聚物(OCP)。这些共聚物优选为具有2至约28个碳原子的α-烯烃的共聚物，优选乙烯与至少一种具有3至约28个碳原子，通常具有式CH2＝CHR1的α-烯烃的共聚物，其中R1为包含1-26个碳原子的直链或支链烷基。α-烯烃的实例包括单烯烃，例如丙烯、1-丁烯、异丁烯、1-戊烯、1-己烯、1-庚烯、1-辛烯、1-壬烯、1-癸烯等。优选，上式中的R1可以为具有1-8个碳原子的烷基，更优选可以为具有1-2个碳原子的烷基。优选，烯烃聚合物为乙烯-丙烯共聚物。
如果烯烃共聚物包含乙烯，则乙烯含量优选为20-80重量％，更优选30-70重量％。当丙烯和/或1-丁烯用作与乙烯的共聚单体时，这类共聚物的乙烯含量最优选为45-65％，但可存在较高或较低的乙烯含量。
OCP的Mn范围通常可以为至多150,000或更高，例如1,000或5,000至150,000或者至120,000或100,000，例如10,000-50,000，尤其是10,000-15,000(例如约12,000)或30,000-50,000(例如约40,000)。在一个实施方案中，OCP可具有大于5,000，例如大于5000至150,000的Mn。还预期上述分子量极限的其它组合。
聚烯烃酰化剂可通过使聚烯烃和酰化剂在热方法或氯方法中反应而制备。热方法和氯方法的讨论可在例如2005年2月10日公开的Eveland等人的WO 2005/012468的第[0013]-[0017]段中找到。如WO’468公开中所讨论的，关于涉及聚烯烃酰化剂的信息，必须进一步参考美国专利Nos.6,165,235；4,152,499和5,275,747。
每种方法中反应物的量可以为约0.5摩尔，通常约0.6摩尔酰化剂每摩尔聚烯烃至3摩尔酰化剂每摩尔聚烯烃。在一个实施方案中，可使用约0.8摩尔酰化剂每摩尔聚烯烃至约1.2摩尔酰化剂每摩尔聚烯烃，甚至更通常约0.95摩尔酰化剂每摩尔聚烯烃至约1.05摩尔酰化剂每摩尔聚烯烃。在另一实施方案中，使用多于1.5摩尔酰化剂，优选约1.6-3摩尔酰化剂每摩尔聚烯烃。在该实施方案中，优选使用约1.8至约2.5摩尔酰化剂每摩尔聚烯烃，更优选约1.9至约2.1摩尔酰化剂每摩尔聚烯烃。
在其中聚烯烃为高亚乙烯基聚烯烃的该实施方案中，聚烯烃可具有平均约1.0-2.0个酰化剂结构部分每聚合物。例如，聚烯烃酰化剂可以为高亚乙烯基聚(异丁烯)琥珀酸酐(PIBSA)，其中衍生出PIBSA的PIB包含至少50摩尔％甲基亚乙烯基封端分子。
为产生本发明第一方面的分散剂组合物，可使聚烯烃酰化剂与羟基端接或胺端基聚醚反应。在一个实施方案中，聚烯烃酰化剂可以与羟基端接或胺端基聚醚以基于聚烯烃酰化剂/羟基端接或胺端基聚醚的摩尔数为约4:1-1:4，或者约2:1-1:2，或者甚至1.1:1-1:1.1的比反应。
在一个实施方案中，聚醚可具有约100-1500的Mn，在另一实施方案中，聚醚可具有约200-1200，或者300-1000的Mn。在某些实施方案中，聚醚可具有约600-900的Mn。
根据本发明一个方面的聚醚可通过通常已知的路线制备，或者作为市售化合物购得。
在本发明一个实施方案中，羟基端接和胺端基聚醚可包含衍生自式I的单元：
其中：
R3可以为氢(H)、-R6OH、-R6NH2、-(C＝O)R6、-R6-N(H)C(＝O)R6，或者具有1-30个碳原子，或者1-20，或者1-10个碳原子，在一些实施方案中，1-6，或者1-4，或者1或2个碳原子的烃基，优选R3可以为H或甲基，
R4可以为H，或者具有1-10个碳原子，或者1-8，或者1-6个碳原子的烃基，优选R4可以为H或甲基，即单碳烃基，
R5可以为具有1-6个碳原子，或者1-4，或者1或2个碳原子的直链或支化亚烃基，优选R5可以为亚甲基，
R6可以为具有1-20个碳原子，或者1-10个碳原子，在一些实施方案中，1-6，或者1-4，或者1或2个碳原子的亚烃基，优选R6可以为CH2CH(CH3)，
Y可以为NR7R8或OH，在某些实施方案中，Y可以为R6NH2或R6OH，优选Y可以为NH2或OH，
R7和R8可独立地为H，或者具有1-50个碳原子且其中至多三分之一的碳原子被N取代或者被另外的式I聚醚官能化的烃基，且
m可以为1-30，或者2-20，或者3-10，更优选3-7的整数。
如本文所用，术语“烃基取代基”或者“烃基”或“亚烃基”以其本领域技术人员熟知的常用意义使用。具体而言，它指具有直接连接在分子其余部分上的碳原子且主要具有烃性质的基团。烃基的实例包括：
烃取代基，即脂族(例如链烷基或链烯基)、脂环族(例如环烷基、环烯基)取代基，和芳族-、脂族-和脂环族取代的芳族取代基，以及其中环通过该分子的另一部分完成(例如两个取代基一起形成环)的环状取代基；
取代的烃取代基，即含有在本发明上下文中不改变取代基的主要烃性质的非烃基团(例如卤素(尤其是氯和氟)、羟基、烷氧基、巯基、烷基巯基、硝基、亚硝基和亚硫酰基(sulfoxy))的取代基；
杂取代基，即在本发明上下文中，在具有主要烃性质的同时在由碳原子组成的环或链中含有不同于碳的取代基，包括取代基如吡啶基、呋喃基、噻吩基和咪唑基。杂原子包括硫、氧和氮。一般而言，对于每10个碳原子，在烃基中存在不多于2，优选不多于1个非烃取代基；作为选择，烃基中不存在非烃取代基。
在某些实施方案中，式I的聚醚可以为具有约600-1200Mn的胺端基聚醚，其中Y为NH2。在这类实施方案中，R3可优选为例如甲基或CH2CH(CH3)NH2。类似地，R4可优选为H或甲基，且优选R5可以为亚甲基。优选的m值可以为3-22，或者10-20。在胺端基聚醚的某些实施方案中，m可以为约3或4，或者约10-13，优选10或12至13，在其它实施方案中，约18-22，优选18至19或22。
在某些其它实施方案中，聚醚可以为具有约100-600Mn的羟基端接聚醚，其中Y为OH。在这类实施方案中，R3可以为例如H或甲基，更优选H。类似地，R4优选为H且R5优选为亚甲基。优选的m值可以为2-13，或者5-10。在羟基端接聚醚的某些实施方案中，m可以为2或3，或者约6-7或7，或者约13。
在一个实施方案中，当R4为烷基时，R5为线性烷基，优选亚甲基。同样，在一些实施方案中，当R5为支化烷基时，R4为H。
应当理解上式包括的聚醚可具有与式I重复单元不同的端基。端基例如可取决于聚醚的引发方法而轻微改变。然而，端基本身包括在式I中。因此，本文预期的聚醚可包括式I的重复单元和式I变体的组合。例如，如在式中，直接如下：
其中Y为OH。显然，嵌段1和嵌段2包括在式I中。在嵌段1中，R5为支化烷基，且R4为H，而在嵌段2中，R5为亚甲基且R4为甲基，使得该式为式I变体的组合。
在另一实例中，式I可包括直接如下的嵌段聚醚：
其中与式I相比，R5为亚甲基，R4为甲基或H，Y优选为NH2，且mx、my和mz表示各自的嵌段。
典型的具有1-20个碳原子的烃基，即R6可包括芳基，脂族、脂环族、线性或支化烃基。在一个实施方案中，R6可由下式表示：
其中x可以为1-10个碳原子。
典型的具有1-50个碳原子且其中至多三分之一的碳原子可被N取代的式I烃基可包括例如具有至少4个芳族基团、至少一个NH2官能团和至少2个仲或叔氨基的胺，其例如由下式表示：
其中各变量独立地：
R’可以为H或R5，
U可以为脂族、脂环族或芳族基团，条件是当U为脂族时，脂族基团可以为包含1-5，或者1-2个碳原子的线性或支化亚烷基；且
w可以为1-10，或者1-4，或者1-2(通常1)。
如前述式中所示烃基的其它实例可如2011年12月15日公开的Gieselman等人的美国公开#2011/0306528的第[0030]-[0038]段所述找到。
典型的具有1-50个碳原子且其中至多三分之一的碳原子可被N取代的式I烃基还可包括例如氨基丙胺或乙氧基化氨基丙胺，例如具有以下通式的来自AkzoNobel的DuomeenTM系列。
根据式I聚醚，具有1-50个碳原子且其中至多三分之一的碳原子可被N取代的烃基还可被另外的式I聚醚官能化。该官能化可例如通过使基础烃基与氧化物如氧化乙烯在升高的温度和压力下反应而实现。该官能化的实例可在下式的化合物中见到：
其中m各自单独地可以为0、1、2、3或4且其中m1+m2+m3+m4+m5+m6可以为4-24，或者6-22或8-20，在某些实施方案中，m1+m2+m3+m4+m5+m6的总和可以为10或20。
被另外的式I聚醚官能化的聚醚的另一实例可在下式的化合物中见到：
其中m各自单独地可以为0、1、2、3、4或5且其中m1+m2+m3可以为2-15，或者3-12，或者4-10，在某些实施方案中，m1+m2+m3的总和可以为3，或者10，或者15。
又一实例可以在下式中见到：
其中m各自单独地可以为0、1、2、3、4或5，且其中m1+m2+m3可以为2-10，或者3-9，或者4-8，在某些实施方案中，其中m1+m2+m3之和可以为5或6。
聚烯烃酰化剂和胺端基聚醚或羟基端接聚醚可在高温下反应以形成分散剂组合物。通常，聚烯烃酰化剂和羟基端接聚醚的反应可能需要酸催化剂以实现更大的转化率。在一些实施方案中，在与聚烯烃酰化剂反应产生分散剂组合物以前，可使羟基端接聚醚或胺端基聚醚与酸或酐如邻氨基苯甲酸或靛红酸酐反应。
分散剂组合物还可与胺反应，优选胺可以为多胺，优选脂族多胺。胺可以为脂族多胺，例如亚乙基多胺(即多亚乙基多胺)、亚丙基多胺、亚丁基多胺或者其两种或更多种的混合物。脂族多胺可以为亚乙基多胺。脂族多胺可选自乙二胺、二亚乙基三胺、三亚乙基四胺、四亚乙基五胺、五亚乙基六胺、多胺釜残，或者其两种或更多种的混合物。可测量分散剂组合物的酸值并可使足量的多胺与分散剂组合物反应以中和分散剂组合物中的任何残余酸。
在本发明另一方面，所述分散剂组合物可并入具有具有润滑粘度的油和任选其它性能添加剂的润滑剂组合物中。
在一个实施方案中，本文所述分散剂组合物可以以润滑组合物的0.01-20重量％，或者0.05-10重量％，或者0.08-5重量％，或者0.1-3重量％，或者甚至0.3-2重量％加入具有润滑粘度的油中。
具有润滑粘度的油可包括例如天然和合成油，衍生自加氢裂化、氢化或加氢精制的油，未精炼、精炼和再精炼油及其混合物。具有润滑粘度的油也可如American Petroleum Institute(API)Base Oil InterchangeabilityGuidelines中所述定义。
可用于本发明中的各种油的更全面详述可在2011年12月15日公开的Gieselman等人的美国公开#2011/0306528的第[0104]-[0111]段中找到。
润滑剂组合物可以为浓缩物和/或完全配制润滑剂的形式。如果本发明聚合物为浓缩物的形式(其可以与其它油结合以完全或部分地形成最终润滑剂)，则聚合物与具有润滑粘度的油和/或与稀释油之比包括1:99-99:1重量计，或80:20-10:90重量计的范围。
组合物还可任选包含其它性能添加剂。其它性能添加剂可包含以下至少一种：金属减活剂、分散剂、粘度改进剂、摩擦改进剂、抗磨剂、腐蚀抑制剂、分散剂粘度改进剂、特压剂、抗磨剂、抗氧化剂、抑泡剂、反乳化剂、倾点下降剂、密封溶胀剂及其混合物。通常，完全配制润滑油包含这些性能添加剂中的一种或多种。
润滑剂组合物任选进一步包含已知的中性或过碱性清净剂。合适的清净剂基质包括酚盐、含硫酚盐、磺酸盐、salixarate、水杨酸盐、羧酸、含磷酸、单-和/或二硫代磷酸、烷基苯酚、硫偶联的烷基苯酚化合物或水杨苷。各种过碱性清净剂及其制备方法更详细地描述于大量专利公开中，包括WO2004/096957及其中引用的参考文献。在一个实施方案中，润滑剂组合物可包含磺酸钙过碱性清净剂，或者磺酸钠或磺酸镁过碱性清净剂。在另一实施方案中，润滑剂组合物可包含苯酚钙清净剂。在又一实施方案中，润滑剂组合物可包含磺酸钙与如下至少一种的组合：苯酚钙、磺酸钠或磺酸镁过碱性清净剂。
清净剂可以以0-10重量％，或者0.1-8重量％，或者1-4重量％，或者大于4至8重量％存在。特别地，其它分散剂可与分散剂组合物一起用于润滑剂组合物中。
过碱性清净剂通常通过总碱值(TBN)表征。TBN为中和所有过碱性材料的碱性所需强酸的量，表示为氢氧化钾(mg KOH/g试样)。由于过碱性清净剂通常以包含一定量的稀释油如40-50％油的形式提供，该清净剂的实际TBN值会取决于存在的该稀释油的量，而不管过碱性材料的“固有”碱性。就本发明而言，过碱性清净剂的TBN应基于无油再计算。用于本技术中的清净剂通常可具有100-800，在一个实施方案中，150-750，在另一实施方案中，400-700的TBN(基于无油)。如果使用多种清净剂，则清净剂组分的总TBN(即所有具体清净剂一起的平均值)通常在以上范围内，对含金属清净剂组分的TBN的所需贡献是各单独清净剂的贡献总和。
包括油在内的组合物的总TBN得自各个组分如分散剂、清净剂和其它碱性材料的TBN贡献。在一些实施方案中，总TBN为至少4或至少6，或者有时甚至至少8。含金属清净剂提供的TBN的量为至少1，或者至少2，或者至少4，或者至少6，且含金属清净剂的量通常为适于提供该TBN水平的量。在某些实施方案中，含金属清净剂的实际量可以为0.2-5重量％或0.3-3％，或者0.5-2％或0.9-1.5重量％。技术人员会认识到如果含金属清净剂以0.2重量％使用且它贡献给配制剂至少2TBN，则该清净剂本身必须具有至少1000的TBN(量和TBN值基于无油表示)。
在一个实施方案中，分散剂组合物可包含其它分散剂。分散剂通常称为无灰分散剂，因为在混入润滑油组合物中以前，它们不包含成灰金属，且它们在加入润滑剂和聚合分散剂中以前通常不贡献任何成灰金属。无灰型分散剂的特征是连接在较高分子量烃链上的极性基团。典型的无灰分散剂包括N-取代的长链烯基琥珀酰亚胺。N-取代的长链烯基琥珀酰亚胺的实例包括PIB取代基的数均分子量为350-5000，或者500-3000的PIB琥珀酰亚胺。琥珀酰亚胺分散剂及其制备公开于例如美国专利4,234,435中。琥珀酰亚胺分散剂通常为由多胺，通常多亚乙基多胺，或芳族多胺如氨基二苯胺(ADPA)形成的酰亚胺。
在一个实施方案中，润滑剂组合物可进一步包含PIB琥珀酸酐和胺，优选多胺，优选脂族多胺，例如亚乙基多胺(即多亚乙基多胺)、亚丙基多胺、亚丁基多胺或者其两种或更多种的混合物的反应产物。脂族多胺可以为亚乙基多胺。脂族多胺可选自乙二胺、二亚乙基三胺、三亚乙基四胺、四亚乙基五胺、五亚乙基六胺、多胺釜残或者其两种或更多种的混合物。
在一个实施方案中，润滑剂组合物进一步包含至少一种衍生自数均分子量为350-5000，或者500-3000的PIB的PIB琥珀酰亚胺分散剂。PIB琥珀酰亚胺可单独或与其它分散剂组合使用。
另一类无灰分散剂为曼尼希碱。曼尼希分散剂为烷基苯酚与醛(尤其是甲醛)和胺(尤其是聚亚烷基多胺)的反应产物。烷基通常包含至少30个碳原子。
也可将分散剂通过常规方法通过与多种试剂中的任一种反应而后处理。其中，这些为硼、脲、硫脲、二巯基噻二唑、二硫化碳、醛、酮、羧酸、烃取代的琥珀酸酐、马来酸酐、腈、环氧化物、磷化合物和/或金属化合物。
分散剂可以以润滑组合物的0-20重量％，或者0.1-15重量％，或者0.1-10重量％，或者1-6重量％，或者7-12重量％存在。
在一个实施方案中，任选性能添加剂的总结合量占润滑组合物的0或0.01重量％至50重量％，在另一实施方案中，0或0.01至40重量％，在另一实施方案中，0或0.01至30重量％，在另一实施方案中，0.05或者0.1或0.5至20重量％。在一个实施方案中，存在的其它性能添加剂化合物的总结合量基于无油为组合物的0-25重量％或0.01-20重量％。尽管可存在一种或多种其它性能添加剂，其它性能添加剂通常以彼此不同的量存在。
工业应用
润滑组合物可用于内燃机中。内燃机可具有或不具有废气循环系统。
在一个实施方案中，内燃机可以为以柴油为燃料的发动机(通常为重型柴油机)、以汽油为燃料的发动机、以天然气为燃料的发动机或以混合汽油/醇为燃料的发动机。在一个实施方案中，内燃机可以为以柴油为燃料的发动机，在另一实施方案中为以汽油为燃料的发动机。在一个实施方案中，发动机可以为火花点火发动机，在一个实施方案中，为压缩机。
内燃机可以为2冲程或4冲程发动机。合适的内燃机包括船用柴油机、航空用活塞式发动机、低载荷柴油机以及汽车和筒塞发动机。
用于内燃机的润滑剂组合物可适于任何发动机润滑剂而不管硫、磷或硫酸盐灰(ASTM D-874)含量。发动机油润滑剂的硫含量可以为1重量％或更少，或者0.8重量％或更少，或者0.5重量％或更少，或者0.3重量％或更少。在一个实施方案中，硫含量可以为0.001-0.5重量％，或者0.01-0.3重量％。磷含量可以为0.2重量％或更少，或者0.1重量％或更少，或者0.085重量％或更少，或者甚至0.06重量％或更少、0.055重量％或更少，或者0.05重量％或更少。在一个实施方案中，磷含量可以为100-1000ppm，或者325-700ppm。总硫酸盐灰含量可以为2重量％或更少，或者1.5重量％或更少，或者1.1重量％或更少，或者1重量％或更少，或者0.8重量％或更少，或者0.5重量％或更少。在一个实施方案中，硫酸盐灰含量可以为0.05-0.9重量％，或者0.1重量％至0.2重量％至0.45重量％。
在一个实施方案中，润滑组合物为发动机油，其中润滑组合物的特征是具有如下的至少一项：(i)0.5重量％或更少的硫含量，(ii)0.1重量％或更少的磷含量，和(iii)1.5重量％或更少的硫酸盐灰含量。
分散剂组合物和包含分散剂组合物的润滑组合物可用于通过将分散剂组合物或包含分散剂组合物的润滑组合物应用于发动机而改进发动机的沉积性能和密封性能中的一种的方法中。
分散剂组合物和包含分散剂组合物的润滑组合物也可用于通过向发动机油应用分散剂组合物或包含分散剂组合物的润滑组合物而改进硝化和氧化性能和保持发动机油的TBN的方法中。另外量的PIB琥珀酰亚胺，例如PIB琥珀酸酐和胺，优选脂族胺，优选脂族多胺如聚乙烯胺(PEPA)的反应产物可用于该方法中。
除非另有说明，所述各个化学组分的量表示为排除了通常可存在于商业材料中的任何溶剂或稀释油，即基于活性化学品。然而，除非另有说明，本文提及的各个化学品或组合物应当理解为可含有异构体、副产物、衍生物和通常应当理解存在于商品级中的其它这类材料的商品级材料。
已知一些上述材料在最终配制剂中可能相互作用，使得最终配制剂的各组分可能与起初加入的那些不同。例如，金属离子(例如清净剂的)可迁移至其它分子的其它酸性或阴离子部位。由此形成的产品，包括经以其意欲用途使用本发明组合物而形成的产品可能不容易描述。然而，所有这类改进和反应产物均包括在本发明的范围内；本发明包括通过将上述各组分混合而制备的组合物。
除非另外说明，本文包括的所有百分数值、浓度和/或比基于重量提供。
实施例
试样1-9–胺端基聚醚(Y＝NH2)
将烧瓶中装入聚烯烃酰化剂。对于试样1-4，聚烯烃酰化剂中的聚烯烃为乙烯丙烯共聚物，对于试样5-9，聚烯烃为聚(异丁烯)。根据需要还加入油，并将反应混合物加热。在下面加入商业胺端基聚醚并提高混合物的温度。对于试样7和8，商业胺端基聚醚首先与靛红酸酐反应。反应产物为浅褐色的清澈稠液体。
| 1 | 2 | 3 | 4 | 5 | 6 | 7 | 8 | 9 | |
| Mn1 | 600 | 900 | 1000 | 600 | 600 | 220 | 220(前体) | 220(前体) | 600 |
| Y2 | -NH2 | -NH2 | -NH2 | -NH2 | -NH2 | -NH2 | ABA | ABA | -NH2 |
| “R3”3 | Me | 2-APr | Me | 2-APr | 2-APr | 2-APr | ABA | ABA | 2-APr |
| “R4” | H/Me4 | H/Me | H/Me | H/Me | H/Me | H/Me | H/Me | H/Me | H/Me |
| “R5” | -CH2- | -CH2- | -CH2- | -CH2- | -CH2- | -CH2- | -CH2- | -CH2- | -CH2- |
| “m” | 10 | 18-19 | 22 | 12-13 | 12-13 | 3-4 | 3-4 | 3-4 | 12-13 |
| CO:N5 | 2:1 | 2:1 | 2:1 | 2:1 | 1:0.6 | 1:0.4 | 1:0.5 | 1:0.5 | 2:1 |
| ％油 | 46 | 80 | 50 | 80 | 0 | 0 | 40 | 50 | 0 |
| TBN | 0.55 | 0.11 | 0.67 | 3.23 | 8.05 | 9.37 | 3.06 | 3.13 | 2.17 |
| TAN | 2.87 | 2.25 | 3.02 | 0.69 | 4.15 | 3.4 | 4.47 | 3.38 | 6.66 |
| ％收率 | 98 | 99 | 98 | 98 | 97 | 97 | 94 | 93 | 98 |
1.具有报告的Mn的商业胺端基聚醚
2.ABA表示-NH-C(O)-芳基-NH2(即氨基苯甲酰胺)
3.Me＝甲基；2-APr表示–CH2CH(CH3)NH2(即2-氨基丙基)
4.H/Me表示两种化学物种(即氧化乙烯/氧化丙烯(EO/PO))的混合物
5.CO:N的摩尔比
试样10-12–PEG酯(Y＝OH)
将烧瓶中装入PIBSA并加热。以两份加入具有300Mn的聚乙二醇；一份不具有酸催化剂；一份具有酸催化剂。最终反应产物为深褐色稠液体。
| 10 | 11 | 12 | |
| PEG“R3” | H | H | H |
| PEG“R4” | H | H | H |
| PEG“R5” | 亚甲基 | 亚甲基 | 亚甲基 |
| PEG“m” | 6-7 | 6-7 | 6-7 |
| 摩尔比CO:OH:催化剂 | 1CO:1.25OH:0.04H+ | 1CO:1OH:0.04H+ | 1CO:1.25OH:0.04H+ |
| TAN | 3.03 | ||
| ％收率 | 97 | 98 | 98 |
试样13-17–其它PAG酯(Y＝OH)
将烧瓶中装入PIBSA和PAG并加热。对于试样17，将烧瓶中装入官能化乙烯丙烯共聚物。加入酸催化剂。最终反应产物为深褐色稠液体。
试样18–用胺封端的PAG酯(Y＝OH)
将烧瓶中装入试样13并加热。测量试样13的酸值并加入足量多胺以中和试样中的任何残余酸。最终反应产物为非常稠的清澈褐色液体。
| 18 | |
| 摩尔比 | (1CO:1N) |
| TAN | 3.55 |
| TBN | 0.0 |
| ％收率 | 97 |
试样19–用硼酸封端的PAG酯(Y＝OH)
将烧瓶中装入试样10和硼酸并加热。加入油。最终反应产物为非常稠的清澈褐色液体。
| 19 | |
| 摩尔比 | (1OH:2BOA) |
| TAN | 6.95 |
| TBN | - |
| ％收率 | 96(14％油) |
实施例1–具有PIB琥珀酰亚胺的客车配制剂试验
在下文所示客车发动机油配制剂中测试试样的沉积和密封性能。
沉积性能可根据如ASTM D6335所示热氧化发动机油模拟试验(TEOST 33)测量。TEOST 33试验结果显示发动机油在高温下运行以后的mg沉积物。较低的TEOST 33试验结果是优选的。同样，性能可根据Komatsu热管沉积物筛选试验(KHT)测量，其提供0-10规模的性能评价，其中0为重沉积物，10为无沉积物。
密封性能可根据Mercedes-Benz供应说明(MB DBL 6674)测量。MB试验涉及将氟碳弹性体(fluorocarbon elastomer)浸入包含350mL待评估试样的烧杯中并将它加热至150℃168小时。测量处理以后试样的拉伸强度(T/S)和破坏伸长(R/E)的变化。较接近零的结果表示较好的密封相容性。
下文中第一个表显示来自置换配制剂中4.9活性物质重量％PIB琥珀酰亚胺中的全部或一部分的结果。第二个表显示当在配制剂中预处理(top-treating)实施例以实现7.9重量％总分散剂活性物质时的结果。
*重复程
实施例2-具有PIB琥珀酰亚胺的客车配制剂试验
在下文所示另一客车发动机油配制剂中测试试样的沉积性能。
| 成分 | 活性物质重量％ |
| 油 | 余量 |
| 粘度改进剂 | 0.621 |
| 倾点下降剂 | 0.115 |
| 抗氧化剂 | 1.45 |
| 磺酸钙清净剂 | 0.7424 |
| 磺酸钠清净剂 | 0.1725 |
| 抗磨剂 | 0.7892 |
| 消泡剂 | 0.00125 |
| 摩擦改进剂 | 0.1 |
| 氧化抑制剂 | 0.048 |
| 腐蚀抑制剂 | 0.05 |
| PIB琥珀酰亚胺 | 2.1 |
将PIB琥珀酰亚胺分散剂用另外2.0活性物质重量％PIB琥珀酰亚胺预处理并与配制剂本身以及用2.0活性物质重量％实施例12预处理的配制剂对比。结果显示于下表中。
实施例3–柴油配制剂1试验
在以下柴油发动机油配制剂中测试试样的沉积和密封性能以及硝化和氧化性能和TBN保持力。
| 成分 | 活性物质重量％ |
| 油 | 余量 |
| 倾点下降剂 | 0.08 |
| 粘度改进剂 | 0.65 |
| 分散剂VM | 0.50 |
| 腐蚀抑制剂 | 0.02 |
| 抗氧化剂 | 1.7 |
| 磺酸钙清净剂 | 0.78 |
| 磺酸镁清净剂 | 0.714 |
| 苯酚清净剂 | 0.5 |
| 其它分散剂 | 2.38 |
| 抗磨剂 | 1 |
| 消泡剂 | 0.01 |
| PIB琥珀酰亚胺 | 2.0 |
对于沉积性能，还通过成漆板焦化试验评估配制剂。成漆板焦化涉及将在105℃下4小时的试验油喷洒在保持在325℃的铝板上。所得沉积物的数字成像提供0-100规模的通用额定值，其中较高的额定值表示较好的性能。
氧化和硝化试验评估润滑剂的氧化和硝化抗性。润滑油的各组分氧化会导致存在的C＝O官能的量提高，而润滑油的各组分硝化会导致结构RONO2表示的各种含氮产物提高。将硝酸和环烷酸铁混入润滑剂中，50cc/min的NOx在145℃浴中清洗试样22小时。试验结束时通过FTIR评估试样的％C＝O提高(1665-1820cm-1下的峰面积)和RONO2(1629+/-20cm-1下的峰面积)。在硝化和氧化期间也可通过对比试验开始(SOT)与试验结束(EOT)时的TBN而测量TBN保持力。
在PIB琥珀酰亚胺分散剂的全部活性置换、部分置换和预处理下在配制剂中评估试样12。结果显示于下表中。
实施例4-柴油配制剂2试验
在下文所示另一柴油发动机油配制剂中测试试样。
| 成分 | 活性物质重量％ |
| 油 | 余量 |
| 倾点下降剂 | 0.08 |
| 粘度改进剂 | 0.65 |
| 分散剂VM | 0.67 |
| 腐蚀抑制剂 | 0.02 |
| 抗氧化剂 | 1.24 |
| 磺酸钙清净剂 | 0.90 |
| 苯酚钙清净剂 | 0.81 |
| 其它分散剂 | 0.092 |
| 抗磨剂 | 1.0 |
| 消泡剂 | 0.01 |
| PIB琥珀酰亚胺 | 4.1 |
在配制剂中在PIB琥珀酰亚胺分散剂的部分活性置换下评估试样7和8。结果显示于下表中，包括根据MTU沉积试验mtv5040，所述标准试验方法(DIN 51535)的另一沉积测量。
实施例5–Sequence IIIG试验
在Sequence IIIG发动机试验中测试各试样。Sequence IIIG试验使用1996General Motors 3800cc系列II水冷4行程V-6汽油机作为试验设备。Sequence IIIG试验发动机为顶置式阀设计(OHV)并使用进气阀和出气阀的借助滑动随动装置中的推杆和液压式气门挺杆操作的单凸轮轴。使用无铅汽油，发动机运行10分钟初始油流平程序(oil leveling procedure)，其后15分钟缓慢提升至速度和荷载条件。发动机然后以125bhp、3,600rpm和150℃油温操作100小时，其中以20小时间隔中断以检查油位。
1.由C3/C6醇的混合物制备的二烷基二硫代磷酸锌(ZDDP)
2.二芳基胺和受阻酚型抗氧化剂的组合
3.其它添加剂包括低含量的硫化烯烃、摩擦改进剂和抑泡剂
4.由2000Mn PIB制备的常规聚异丁烯(PIB)衍生的琥珀酰亚胺分散剂
将以上提及的各个文件通过引用并入本发明。任何文件的提及不是容许该文件以任何权限取得现有技术的资格或构成技术人员的常识。除实施例中外，或如果另外明确指出，该说明书中描述材料的量、反应条件、分子量、碳原子数等的所有数量应当理解为通过措辞“约”修饰。应当理解本文所述量、范围和比的上限和下限可独立地组合。类似地，本发明各个元素的范围和量可与任何其它元素的范围或量一起使用。如本文所用，表述“基本由…组成”允许包括不本质上影响所考虑的组合物的基本特征和新特征的物质。
Claims (22)
1.包含聚烯烃酰化剂和羟基端接或胺端基聚醚的反应产物的分散剂组合物。
2.根据权利要求1的分散剂组合物，其中羟基端接或胺端基聚醚选自由(i)聚乙二醇、(ii)聚丙二醇、(iii)聚氧化烯胺混合物或(iv)其一些组合组成的组。
3.根据权利要求1的分散剂组合物，其中羟基端接或胺端基聚醚选自由如下物质组成的组：(i)三甘醇，(ii)二甘醇，(iii)250-350分子量聚乙二醇，(iv)200-350分子量聚四氢呋喃，(v)一种或多种包含衍生自氧化乙烯、氧化丙烯、氧化丁烯或其一些组合的单元的胺端基甘醇的混合物，或者(vi)其一些组合。
4.根据权利要求1的分散剂组合物，其中聚醚包含衍生自式I的单元：
式I
其中：
R3为氢(H)、-R6OH、-R6NH2、-(C＝O)R6、-R6-N(H)C(＝O)R6，或具有1-30个碳原子的烃基，
R4为H，或者具有1-10个碳原子的烃基，
R5为具有1-6个碳原子的直链或支化烃基，
R6为具有1-20个碳原子的烃基，
Y为NR7R8、OH、-R6NH2或-R6OH，
R7和R8独立地为H，或者具有1-50个碳原子且其中至多三分之一的碳原子可以被N取代或者被另一式I聚醚官能化的烃基，且
m为1-30的整数。
5.根据权利要求1的分散剂组合物，其中聚烯烃酰化剂为选自聚异丁烯或烯烃共聚物的聚烯烃与选自单烯属不饱和C3-C28单羧酸或其酯，或者单烯属不饱和C4-C28二羧酸、酐或其酯的反应产物。
6.根据权利要求5的分散剂组合物，其中反应不是自由基引发的。
7.根据权利要求5的分散剂组合物，其中羧酸为马来酸、衣康酸、富马酸、及其酐或酯。
8.根据权利要求5的分散剂组合物，其中聚烯烃具有约1000-15,000的数均分子量。
9.根据前述权利要求中任一项的分散剂组合物，其中聚醚具有约100-1500的数均分子量。
10.根据前述权利要求中任一项的分散剂组合物，其中聚醚为约600-1200数均分子量的胺端基聚醚，且其中R3为甲基或CH2CH(CH3)NH2，R4为H或甲基，R5为亚甲基，Y为NH2，且m为3-22。
11.根据前述权利要求中任一项的分散剂组合物，其中聚醚为约100-600数均分子量的羟基端接聚醚，且其中R3为H或甲基，R4为H，R5为亚甲基，Y为OH，且m为2-13。
12.根据权利要求9的分散剂组合物，其中聚醚为式II的羟基端接聚醚，其中m各自单独地为0、1、2、3或4。
式II
13.根据权利要求9的分散剂组合物，其中聚醚为式III的羟基端接聚醚，
式III
其中m各自单独地为0、1、2、3、4或5。
14.根据权利要求9的分散剂组合物，其中聚醚为下式的羟基端接聚醚：
其中m各自单独地为0、1、2、3、4或5。
15.根据前述权利要求中任一项的分散剂组合物，其中反应产物进一步包含多亚乙基多胺。
16.包含根据前述权利要求中任一项的分散剂组合物和具有润滑粘度的油的润滑剂组合物。
17.根据权利要求16的润滑剂组合物，其进一步包含PIB琥珀酰亚胺。
18.改进发动机中的沉积性能的方法，其包括向发动机应用权利要求16或17的组合物。
19.改进发动机油中的硝化和氧化性能的方法，其包括向发动机应用权利要求16或17的组合物。
20.改进发动机中的密封性能的方法，其包括向发动机应用如权利要求16或17中所主张的组合物。
21.保持发动机油中的TBN的方法，其包括向发动机油应用如权利要求1-14中任一项所主张的分散剂组合物。
22.根据权利要求21的方法，其进一步包括向发动机油应用PIB琥珀酰亚胺。
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| EP1760138A2 (en) * | 2005-08-31 | 2007-03-07 | Chevron Oronite Company LLC | A lubricating oil additive composition and method of making the same |
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| US20170183602A1 (en) | 2017-06-29 |
| US20130274160A1 (en) | 2013-10-17 |
| US9624452B2 (en) | 2017-04-18 |
| CN104350135B (zh) | 2016-11-23 |
| EP2836576A1 (en) | 2015-02-18 |
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