CN1029786C - 一种分散剂/粘度指数改进剂的制备方法 - Google Patents

一种分散剂/粘度指数改进剂的制备方法 Download PDF

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CN1029786C
CN1029786C CN91101910A CN91101910A CN1029786C CN 1029786 C CN1029786 C CN 1029786C CN 91101910 A CN91101910 A CN 91101910A CN 91101910 A CN91101910 A CN 91101910A CN 1029786 C CN1029786 C CN 1029786C
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star polymer
reaction
carboxylic acid
acid
polymkeric substance
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CN1055758A (zh
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阿里·范佐
格哈达·雅格巴
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Shell Internationale Research Maatschappij BV
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Shell Internationale Research Maatschappij BV
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Abstract

分散剂/VI改进剂润滑油添加剂的生产是通过将一星形聚合物与-α，β-不饱和羧酸或其活性衍生物反应而生成活化的星形聚合物，然后将其与(a)至少一种具下面通式的化合物反应
RO(AO)nH
其中R是C4-20的烷基，部分A独立地是乙烯部分或丙烯部分，n是0到5，然后可视情与(b)烷基羧酸和/或(c)烷基胺或多羟基链烷反应，或与反应物(b)和反应物(c)预先生成的产物反应，随后视情用-C1～6的链烷醇酯化任一残余的酯基。

Description

本发明与改性的聚合物有关，它们在作为润滑油的添加剂时具有有用的性质。
新近的发动机对于所用的润滑剂提出了越来越高的要求。过去已有若干种不同的添加剂加入到润滑油中以改进诸如粘度指数和分散性等这些性能。加入润滑油改进粘度指数（简称VI，下同）的这样一种添加剂之一是一种双嵌段共聚物，一般构型为A-B，其中A为苯乙烯，B为氢化异戊二烯，也即如美国专利3，763，044和3，772，196中所描述的。一种极大地改进了机械切变稳定性的VI改进剂是选择性氢化的星形聚合物，公布于英国专利说明书1，575，507。使用单一一种添加剂来改进若干种润油剂的性能，可以显著地降低成本，并可避开各种不同的添加剂之间（或添加剂与基油之间）可能产生的相容性问题。不过，在设法改进一种以上的润滑剂性能时，必须注意不会导致其它性能的降低。例如，美国专利3864268中，使用氧化步骤将极性基团连接到聚合物骨架上，这就由于引入点的氧化侵蚀而降低了润滑剂的稳定剂。
美国专利4，077，893公布了无灰份的油溶性添加剂，其制备方法包括：
（a）在约150℃到约300℃之间，约1小时到约20小时时间内，将选择性氢化的星形聚合物与α，β-不饱和羧酸或酸酐或酯反应，其中所述的星形聚合物包括一个聚合（聚烯烃偶合剂）核，以及至少四个与上述的核相连的聚合物支链，其中所说的聚合物支链选自下面一组物质：
（ⅰ）共轭二烯的氢化的均聚物和氢化共聚物;
（ⅱ）共轭二烯与单链烯基芳香烃的氢化共聚物;及
（ⅲ）它们的混合物;
且其中星形聚合物的至少约80%的脂族不饱和已被氢化作用所还原，同时少于20%的芳香族不饱和已被还原;和
（b）将步骤（a）的产物与一种至少有两个羟基基团的多羟基链烷在约150℃到约250℃的温度下反应。
EP-A-364058（Applicants′ref.T5277EPC）描述了改进分散剂和粘度指数（VI）性质的无灰份的、油溶性添加剂，它通过下列方法制得：
（1）最好在约100℃到约300℃之间经过约1小时到约24小时，将α，β-不饱和羧酸或其活性衍生物与一选择性氢化的星形聚合物反应，该聚合物含有一个聚乙烯基芳核和至少4个如4至25个聚合物支链，每个支链可有例如5000至150000的数均分子量，且这些支链与上述的核相联接，上述的聚合物支链选自下面一组物质：
（ⅰ）共轭二烯的氢化均聚物和氢化共聚物;
（ⅱ）共轭二烯与单链烯基芳烃的氢化共聚物;以及
（ⅲ）它们的混合物;
且其中星形聚合物的至少80%，最好是90%到98%的脂族不饱和已被氢化作用所还原，而同时少于20%的芳族不饱和已被还原;和
（2）将由此形成的活化的氢化星形聚合物与下列物反应：
（a）与一长链烷基取代的羧酸或其活性衍生物，和
（b）与一含有1至8个氮原子的C1到C18的胺，和/或一个含有至少二个羟基的多羟基链烷，进行反应;或与
（c）反应物（a）和反应物（b）的预先生成的产物，进行反应。
根据本发明提供的一种制备分散剂/VI改进剂的方法，该方法包括：
（1）将-α，β-不饱和的羧酸或其活性衍生物与一选择性氢化的星形聚合物进行反应，该聚合物包括一个聚乙烯基芳香族的核团和至少4个与该核团联接的聚合物支链，其中所述的聚合物支链选自下列一组物质：
（ⅰ）共轭二烯的氢化均聚物和氢化共聚物;
（ⅱ）共轭二烯与单链烯基芳烃的氢化共聚物;以及
（ⅲ）它们的混合物;
其中星形聚合物的至少80%的脂族不饱和已被氢化作用还原，而同时少于20%的芳族不饱和已被还原;和
（2）将这样生成的活化的星形聚合物与下列物质反应：
（a）至少一个式Ⅰ的化合物
其中R是C4-20的烷基，A独立地为亚乙基或亚丙基，n为0至10，随后视情与以下物质反应
（b）一长链烷烃取代的羧酸或其活性衍生物，和/或
（c）一含有1至8个氮原子的C1到C18的胺，和/或一具有至少二个羟基的多羟基链烷;
或与（d）即反应物（b）和反应物（c）的预先生成的产物，随后视情用C1到C6的链烷醇来酯化任何残余酸基。
上面的步骤（1）与EP-A-364058的步骤（1）基本相同。
用于制取本分散剂/VI改进剂的星形聚合物的一般生产方法包含下列的反应步骤：
（ⅰ）在离子引发剂存在的条件下在溶液中聚合一种或一种以上共轭双烯，以生成活性高聚物;
（ⅱ）将该活性高聚物与一种聚乙烯基芳香化合物，最好是二乙烯基苯反应，生成星形的聚合物;和
（ⅲ）将该星形聚合物氢化，形成氢化星形聚合物。
此制备方法在英国专利说明书1575507中有详细的描述。
在上面方法的反应步骤（ⅰ）中产生的活性高聚物是从聚乙烯基芳香核团向外伸延的各条氢化聚合物链的前体。最好每条聚合物支链都是氢化的聚异戊二烯均聚物。
在反应步骤（ⅲ）中被氢化的星形聚合物的分子量可以在比较宽的范围内变化。有可能产生峰值分子量在约25000和约1250000之间的星形聚合物。较好的分子量是从100000到500000。这些峰值分子量是用聚苯乙烯标定的凝胶渗透色谱（GPC）测定的。
在步骤（ⅲ）中，星形聚合物是用任一种适当的技术氢化的。初始的烯烃不饱和被氢化的比例，以至少80%为适用，以大约90%到大约98%为好。芳族不饱和被氢化的量，若有的话，将取决于所用的氢化条件。然而，这种被氢化的芳族不饱和 最好少于20%，更好的是少于5%。
氢化星形聚合物的分子量与未氢化的星形聚合物的分子量大致相当。
氢化作用可以如英国专利说明书1，575，507中所描述的那样进行，且较好的方法即选择性氢化方法在美国专利3，595，942中作的描述。在该方法中，氢化作用最好是在与制备聚合物相同的溶剂中进行，该反应使用了一种烷基铝与镍（或钴）的羧酸盐或醇盐反应产物的催化剂。较适用的催化剂是三烷基铝与辛酸钴生成的反应产物。
氢化星形聚合物随后使用任何适宜的技术例如蒸发溶剂，以固态形式从溶剂中回收。或者，可以将一种油，例如润滑油，加入溶液中，溶剂再从如此形成的混合物中汽提出去，生成浓缩物。易于加工的浓缩物即使在溶液中的氢化星形聚合物的量超过10%重量时也可生成。合适的浓缩物含有10%到25%重量的氢化星形聚合物。
如上法所制备的选择性氢化的星形聚合物本身不具有足够的分散物性，而要按下面的说明进行改性：
1）星形聚合物首先通过与α，β-不饱和羧酸或其活性衍生物反应而被活化。此处的“其活性衍生物”指酸酐、酯等等。合适的不饱和酸与衍生物包括马来酸、马来酐、衣康酸、衣康酸二甲酯、丙烯酸、丙烯酸二酯、甲基丙烯酸、甲基丙烯酸甲酯、油酸、亚油酸、等等，而以马来酐为最好。
不饱和羧酸化合物与氢化星形聚合物在100℃至300℃，最好是130℃到250℃的温度范围内很容易进行反应。较合适的接触时间从1小时到24小时，最好是4小时到8小时。羧酸化合物与星形聚合物的二烯部分所提供的残余烯键反应，并且/或者与聚合物链上引发的游离基反应，后一反应的合适温度是从100℃到150℃。
可以用于羧酸衍生物加入步骤1）的各种溶剂一般包括烯烃一单体石油烃、芳香烃和卤代烃。较好的一种溶剂是润滑油基本组份。共聚物在溶剂中的浓度在大约1%（重量）到约20%（重量）范围内时是适用于这一转化过程的。
一般来说不饱和羧酸化合物的用量，对于与选择性氢化的星形聚合物中二烯部分所留有的所有残余双键起反应来说，是化学量过量的。较好的是，对于选择性氢化的星形聚合物中存在的每一烯烃不饱和，使用至少一摩尔的羧酸化合物，并以羧酸化合物与烯双键的当量比在1∶1到2∶1范围内为好，不过，也可使用化学量不足量的羧酸化合物。
使用或不使用催化剂或如叔丁基过氧化氢或叔丁基过苯甲酸酯等的游离基引发剂，上述反应都可进行。过量羧酸化合物典型的移去方法是通过真空蒸馏或用水蒸汽汽提。
2）从上面与不饱和羧酸反应得到的活化的氢化星形聚合物随后通过与下列物反应改性：
（a）至少一种具下面通过式的化合物：
RO（AO）nH （Ⅰ）
其中R是一个C4到C20的烷基，A独立地为亚乙基或亚丙基，n为0到10，接着视情与下列物反应：
（b）一长链烷烃取代的羧酸或其活性衍生物，最好是琥珀酸或琥珀酐或琥珀酸酯，和/或
（c）含1到8个氮原子的C1到C18的胺和/或至少含二个羟基的多羟基链烷;或（d）：反应物（b）和反应物（c）的预先生成的产物，随后视情以一个C1到C16的链烷醇酯化剩余酸基的反应。活化的星形聚合物与式Ⅰ化合物（反应物（a））之间的反应可通过将这些反应物一起加热而给予适当影响，合适的温度是在100℃到200℃，最好140℃到170℃范围之内。随后与链烷羧酸（反应物（b））的反应，和/或与烷胺或多羟基链烷（反应物（c））的反应，或与一个（a）与（b）预先生成的反应产物（反应物（d））的反应，都可通过在活化星形聚合物与反应物（a）反应时所用的同样方式给予适当影响，但反应物（b）和反应物（c）可按任意顺序加入或一起加入。不过最好是当反应物（b）和（c）使用时先加入反应物（b）。反应可在溶剂存在的条件下进行，较方便的是用与星形聚合物活化的步骤1）中所用的同一溶剂，润滑油基本组份对于过程的两个步骤都是特别合适的。如在一种惰性的环境较合适的如氮气环境一下面操作，较合乎要求。
式Ⅰ的化合物是已知的。值得重视的是n为0时，式Ⅰ的化合物是C4到C20的链烷醇，如正丁醇或C9到C15的洗涤剂作用伯醇，诸如Royal Dutch/Shell Group of companies在DOBANOL商标下出售的，如DOBANOL91，DOBANOL23，DOBANOL25，或DOBANOL45。然而，对n来说最好是在2至10的范围之内，更好的是在3到7的范围，非常合适的值是5 左右。A最好是一乙烯部分。R最好是C9到C15的烷基，更好是C9到C11的烷基。合适的此类化合物是Royal Dutch/Shell Group of companies出售的DOBANOL（商标）乙氧基酯，如DOBANOL91-2.5、DOBANOL 91-6、DOBANOL 23-6.5、DOBANOL 25-3、DOBANOL 25-7、及十分适用的DOBANOL91-5。
在步骤1）的活化星形聚合物产物中，式Ⅰ化合物与羧酸部分的摩尔比，最好在0.1∶1到2∶1的范围之内。这样当α，β-不饱和羧酸或其活性衍生物，如所希望的那样，是马来酐时，式Ⅰ化合物在活化的星形聚合物中与马来酐基团的摩尔比数就最好是0.2∶1到4∶1，更好一些是0.5∶1到2∶1。在随后与反应物（b）、（c）、和（d）都没有反应的情况下，分子式Ⅰ的化合物与马来酸基团的较好的摩尔比数是0.5∶1到4∶1，更好的是1∶1到2∶1。
长链烷烃取代的羧酸/衍生物（反应物（b））最好这样获得即用-α，β-不饱和羧酸或其活性衍生物与一聚烯烃，较合适的是与一具有2到16个碳原子，更好是具有2到6个碳原子的一种或多种烯烃单体的均聚物或共聚物反应。该种共聚物包括无规的、嵌段的和组成递变共聚物。合适的单体包括乙烯、丙烯、丁烯、异丁烯、戊烯、辛烯，也包括二烯属如丁二烯和异戊二烯。如果用二烯作为单体，所得的聚合物最好氢化到至少90%饱和，更好的是彻底氢化所有的不饱和键。最好的是使用衍生自聚异丁烯的聚烯烃取代基。
聚烯烃取代基的数均分子量宜不大于5000，因为5000以上的分子量会损害最终产物的分散能力，特别是在曲轴箱的润滑剂中。为减少风险，数均分子量最好是从700到3000。数均分子量（Mn）很容易用蒸汽压渗透压力测定法或用聚合物校准后的凝胶渗透色谱法测定，正如本领域中的技术人员所推崇的那样。重均分子量（Mw）也可用凝胶渗透色谱来测定。指示分子量分布宽度的一个量度，商Mw/Mn，宜有从1.5到4.0的值。
与聚烯烃反应的不饱和酸可以是前面所列举作为适于使氢化星形聚合物活化的任一酸，尤其好的是马来酸或马来酐。在马来酸/酐的情况下，聚烯烃向不饱和键合上的加成给出一个聚烯烃取代的琥珀酸衍生物。
每个聚烯烃部分的平均不饱和羧酸基团数正常是在0.5到1.5的范围。这意味着某些聚烯烃部分联接着一个以上的琥珀酸基团。较好的是，每聚烯烃部分的琥珀酸基团平均数在0.9到1.1范围之内。
聚烯烃取代的羧酸可以按照已建立的方法，从一具有所要求的分子量的链烯烃和适量的不饱和羧酸或活性衍生物来制取。所以，聚烯烃例如聚异丁烯，就可以是与马来酐及以混合物通过的氯气相混合，产出盐酸和聚烯烃取代的琥珀酐，如同在如GB-A-949，981中所描述的那样。制备聚烯烃取代的琥珀酐的另一方法在US-A-3，172，892中有描述，根据这种方法一个卤代的，特别是氯代的聚烯烃，与马来酐发生反应。
从例如GB-A-1，483，729中，可知如何通过聚烯烃与马来酐的热反应来制备烃代的琥珀酐，这个方法可以与GB-A-949，981中的方法结合，如同GB-A-1，440，219和GB-A-1，543，627中说明的那样。用这种方式制得的产物包括这些化合物，其中的聚烯烃链与琥珀酸基团的一个或所有二个α碳原子均相联接。
本发明中所用的C1到C18的胺可以是分支的或无支链的、饱和的、脂族的、伯胺或仲胺、含1到8个氮原子，最好是单胺或二胺，如乙胺、丁胺、仲丁胺、二乙胺、3-二甲胺基丙胺、等等，但也包含高级多胺如亚烷基多胺，其中成对的氮原子被含2到4个碳原子的亚烷基相连接，因此，有如下分子式的多胺
NH2（CH2）n-[NH（CH2）n]m-NH2
也包括在内，其中n为2到4，m为0到6。这类多胺的例子包括四亚乙基五胺、三亚丙基四胺、三亚乙基四胺、二亚乙基三胺、N-氨烷基哌嗪、如N-（2-氨乙基）哌嗪、N，N′-二（2-氨乙基）哌嗪、等等。较好提二亚乙基三胺、三亚乙基四胺或四亚乙基五胺，以及相应的商品混合物如Polyamine    H和Polyamine500。
用于形成醌的多羟基链烷是含有至少两个，最好含有至少4个羟基的多羟基链烷，如三羟基链烷，例子有1，2-亚乙基二醇、丙二醇、聚亚甲基二醇类、三羟丁烷、戊烷、己烷、庚烷、辛烷、壬烷、十二烷等等，还有四羟基链烷、五羟基链烷、 六羟基链烷，以及糖醇如赤藓醇、季戊四醇、丁糖醇、戊五醇、己糖醇、甘露糖醇、山梨醇、葡萄糖等，诸如此类。特别好的醇类是季戊四醇和甘露糖醇。尤其好的是季戊四醇。
胺或多羟基化合物相对于羧酸化合物的余量一将所用的式Ⅰ休化合物的量计入后-的摩尔比典型地是在约0.1∶1到约2∶1之间，较好的是在约0.25∶1到约2∶1之间，最好的是在约0.5∶1。酰亚胺形成过程或酯化作用过程中典型的条件是在约150℃到250℃，经过约1小时到20小时。
在反应步骤2）中，反应在无氧条件下进行要好得多。常使用氮气覆盖来达到这个目的。在无氧条件下进行反应的原因是如果添加剂生成过程中有氧气存在的话，得到的添加剂会对氧化更不稳定。
在使用胺或多羟基化合物，且使用的是过量的情况下，除去过量物会更好些。这样做的办法之一是通过真空蒸馏将三氯苯溶剂换成润滑油基本组份，然后加入与油溶液同体积的庚烷。再加入等体积甲醇并混合。静置后发生分层（分为两层）;一层主要含有洗涤溶剂和未反应的胺或多羟基化合物，另一层主要含有油、庚烷和添加剂产物。将洗涤层分离以后，产物层中存在的挥发成分可用蒸馏的技术除去。另外，过量的胺或多羟基化合物可在真空下除去，或用水蒸汽汽提除去。
在所有的剩余酸基都要被C1～6的烷醇酯化的情况下，可通过已知的方式影响酯化过程，如加入烷醇和一适当的酸如对甲苯磺酸，在高温如回流温度下进行。适宜的C1～6的烷醇可以是例如甲醇、乙醇、正丙醇、异丙醇，或更好的是正丁醇。
本发明的分散剂VI改进剂可将粘度改性与氧化稳定性、机械切变稳定性和分散性的改进有效地结合起来。特别是，含有这种VI改进剂/分散剂的润滑油同时具有很好的增稠性能和高温下的切变稳定性，在低温下也有很好的粘度特性。与先有的VI改进剂相比，本发明的VI改进剂/分散剂只需要较少的量，就可得到所要求的增稠性能。进一步说，VI改进剂/分散剂还可具有出色的将氧化切变稳定性、永久切变稳定性和“瞬时切变丧失”结合一体的性质。瞬时切变丧失指的是来源于聚合物的VI改进剂的非牛顿特性的，高剪切应力条件下的瞬时粘度丧失。更进一步说，本发明聚合物添加剂的分散能力是极好的。
本发明的反应产物可以加入到润滑油组合物如汽车曲轴箱的油中，加入的浓度为约0.1-约15%（重量），最好在约0.1-3%（重量）（以组合物总重量为基）。如需要的话用碱如氢氧化钠或最好是氢氧化钙进行后处理以中和不需要的残余酸性。本发明的添加剂可添加的润滑油不仅包括矿物润滑油，也包括合成油。合成烃类润滑油也可使用，同样还有非烃类合成油，包括二元酸酯，例如二（2-乙基）己基癸二酸酯、碳酸酯、磷酸酯、卤代烃、聚硅氧烷、聚乙二醇、乙二醇酯如四亚乙基乙二醇的C含氧酸酯等等。当用于汽油或燃料油如柴油机燃料、2号燃料油等等时，一般则使用约0.001-0.5%（重量）（以组合物总重量为基）的反应产物。为便于加工起见，也可在有或没有其他种添加剂存在的条件下，制备这样的浓缩物，它含有溶于大量的烃类稀释液中的少部分的上述反应产物如15-45%（重量）和85-55%（重量）的矿物润滑油。
在上述组合物或浓缩物中，其他适当的添加剂也可存在，这包括染料、倾注点下降剂、抗磨添加剂如磷酸三（甲苯酯）、3到8个碳原子的二烷基二硫代磷酸锌，抗氧化剂如苯基-α-萘胺、硫代叔辛基苯酚、双-苯酚如4，4′-亚甲基双（3，6-二叔丁基苯酚），粘度指数改进剂如乙烯-高级烯烃共聚物、聚甲基丙烯酸酯、聚异丁烯、烷基富马酸乙烯基乙酸酯共聚物、及此类物质以及其他的无灰分散剂或去垢剂如高碱性的磺酸盐。
本发明将用下列实施例作进一步的说明，实施例的给出仅限于解释的目的，并不意味着将发明限于所公布的特定反应物和特定用量上。
实施例1
（a）在温度为133℃和叔丁基过苯甲酸酯作为游离基引发剂存在下，并于N2气氛下（50ppmO2），一种由SHELLVIS200（商标）星形聚合物和XHVI-6油（13.8%m/m）组成的浓缩物与马来酐（MALA）（用量为星形聚合物的2%m/m）在搅拌下反应18小时。游离基引发剂以50%m/m油溶液的形式烃41分钟投料（泵入）。
克    %m/m
输入    SHELLVIS    340.94    13.66
200
MALA    6.82    0.27（＝2%m/m，
以星形聚合物
计算）
Trigonox    C    9.210.37（＝2%m
（商标）    /m的叔丁基过苯甲
（＝75%的    酸酯，以星状聚合物
叔丁基过苯甲酸酯）计算）
XHVI-油    2138.87    85.70
总计    2495.84    100.0
“SHELLVIS    200”是一种星形聚合物，其支链分子量为35000，并按英国专利1，575，570的方法与二乙烯基苯偶联的氢化聚异丙烯。
反应混合物随后在110℃和高真空（0.06mmHg，8Pa）下汽提以除去残余的未反应的马来酐。
由此获得的VI改进剂浓缩物中的马来酐含量是通过用甲醇钠溶于甲醇的0.1mol/l溶液进行滴定测定的，指示剂酚酞。高真空汽提后反应产物中MALA的含量为：0.015mmol/g产物。假定100%接枝时，MALA的理论含量应为0.028mmol/g，所以接枝率是54%。
（b）从上面步骤（a）的汽提产物取1505.9克（含接枝的MALA量22.1mmol）在氮气下与C9～11的链烷醇乙氧基化物的掺合物，其中掺合物的平均相对分子量为380，并且每摩尔DOBANOL91-5（商标）的乙氧基化物，（Royal Dutch/Shell Group of companies出售）含有5摩尔的环氧乙烷，通过加热搅拌混合物使反应在150℃下进行1小时，然后在170℃下进行3小时。所得出的产物（浓缩物，产物A）据滴定含有13.6%W的星形聚合物和0.014mmol/g的酸。
1.7%W产物A加于HVI160油中的掺合物，在100℃时，粘度是15.8mm2/s（ASTMD445）。HVI60油是一种明亮、纯净的高粘度指数的基油，其粘度在100℃为4.4到4.9mm2/s（ASTMD445），最低闪点200℃（ASTMD92）。
实施例2
取实施例1（a）的汽提产物1567.0g（接枝MATA含量23.0mmol）按实施例1（b）的方式与17.5g（46.1mmol）的DOBANOL91-5（商标）乙氧基化物反应。所得的产物据滴定含有0.0125mmol/g的酸。为将酯化进行完全，将14.1g（190.5mmol）的正丁醇、3.6g对甲苯磺酸和1l甲苯加入（所得混合物酸含量0.009mmol/g），所得混合物在回流温度下加热22小时。混合物的酸含量减低到0.004mmol/g。混合物随后以20g氢氧化钙在室温（20℃）下处理1小时，过滤，在100℃下在真空中蒸发，给出一含有13.6%W星形聚合物的产物（浓缩物，产物B），它据滴定结果是无酸的。
加于HVI60油的1.7%W产物的掺合物在100℃时的粘度是14.9%mm/s（ASTMD445）。
实施例3
取实施例1（a）的汽提产物1700g（接枝的MALA含量25.5mmol）与4.84g（12.8mmol）的DOBANOL91-5（商标）乙氧基化物，在氮气下通过加热搅拌混合物进行反应，加热温度150℃，时间2小时。冷却到室温（20℃）之后，加入聚异丁烯取代的琥珀酐（简称PIBMALA）（39.2g，含38.22mmol的琥珀酐基团）。加入二亚乙基三胺（简称DETA）（2.76g，2.90ml，26.78mmol），同时在氮气下在150℃加热58分钟，然后在180℃加热3，小时，在加热的最后一小时期间内，将氮气通过反应混合物，以除去挥发性的物质。所得产物（浓缩物，产物c）据滴定含有13.3%W星形聚合物，0.010mmol/g碱性氮和0.008mmol/g酸。
加于HVI160油的1.7%W产物C的掺合物在100℃下的粘度为19.33mm/s（ASTMD445）。
实施例4
遵循实施例3的步骤，但将二乙胺换成季戊四醇（3.47g，25.5mmol），且未反应的季戊四醇从粘性的反应终产物中除去的方法是用与反应终产物同体积的二甲苯将其稀释，100℃下过滤，并在真空下蒸发二甲苯。所得的产物（浓缩物，产物D），据滴定，含有13.3%W的星状聚合物和0.024mmol/g的酸。
加于HVI60油的1.7%W产物D的掺合物在100℃时的粘度为28.3mm/s（ASTMD445）。
实施例5
产物A、B、C、D的样品及市场出售的VI改进剂SHELLVIS200与含有6%W/W的添加剂组合物润滑油SAE10W/40掺合，该添加剂组 合物含有高碱性水杨酸盐去垢剂、琥珀酸亚胺无灰分散剂、锌基质抗磨添加剂和聚甲基丙烯酸酯倾注点下降剂。所得的油随后按照VE序列评估（见“Sequence    VE    test    Procedure”，7th    draft    dated    19th    May，1988ASTM    Monitoring    Center，44005th    Avenue    Pittsburgh，USA）。
结果在下面的表Ⅰ中给出：
表1
VE试验参数
样品%    平均引擎油淤    平均引擎积炭    平均凸轮凹角磨损
样品    W/W    （AES）    （AEV）    （ACLW）（μm）
SHELLVJS200    9.50    5.4    4.3    34.3
SHELLVIS200    7.64    4.5    5.0    8.0
产物A    7.48    6.3    4.3    14.0
产物B    8.10    6.7    4.1    21.6
产物C    7.52    6.3    4.3    18.0
产物D    4.89    5.6    5.0    88.1
SG超过界限    9（最小）    5.0（最小）    127（最小）

Claims (8)

1、一种分散剂/Ⅵ改进剂的制备方法，该方法包括：
1)将-α，β-不饱和羧酸或其活性衍生物与一选择性氢化的星形聚合物反应，该星形聚合物含有一聚乙烯基芳核和至少4个与所述的核相连的聚合物支链，其中所述的聚合物支链选自下列一组物质；
i)共轭二烯的氢化均聚物和氢化共聚物；
ii)共轭二烯和单链烯基芳烃的氢化共聚物；及
iii)它们的混合物；
且其中星形聚合物的脂族不饱和的至少80%已被氢化作用还原，而少于20%的芳族不饱和被还原。
和
2)将上述形成的活化了的星形聚合物与下列物反应；
(a)至少一种具下面通式的化合物：
其中R是C4-20的烷基，A独立地是亚乙基或亚丙基，n是0至5，随后视情与下列反应：
(b)一长链烷烃取代的羟酸或其活性衍生物，和/或(C)一个含1到8个氮原子的C1到C8的胺和/或一个至少具有两个羟基的多羟基链烷；或(d)反应物(b)和反应物(c)预先生成的产物，随后视情用-C1-6的链烷醇酯化任何残余酸基。
2、如权利要求1中所述的方法，其中聚合物支链的数目在4至25之间，且聚乙烯基芳香化合物是二乙烯基苯。
3、按照权利要求1或2所述的方法，其中在星形聚合物中，每一聚合物支链的数均分子量在5000和150000之间，和氢化星形聚合物的峰值分子量在25000和1250000之间。
4、按照权利要求1或2所述的方法，其中星形聚合物与羧酸或其活性衍生物在130℃至250℃的温度范围内反应。
5、按照权利要求1或2所述的方法，其中式Ⅰ的R是C9-15的烷基。
6、按照权利要求1或2所述的方法，其中式Ⅰ的n为3到7。
7、按照权利要求1或2所述的方法，其中的α，β-不饱和羧酸或其活性衍生物是马来酐。
8、按权利要求7所述的方法，其中式Ⅰ的化合物与活化的星形聚合物中的马来酐基团的摩尔比为0.2∶1至4∶1。
CN91101910A 1990-03-30 1991-03-28 一种分散剂/粘度指数改进剂的制备方法 Expired - Fee Related CN1029786C (zh)

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