CN1102668A - 制备润滑剂组合物分散剂的方法 - Google Patents
制备润滑剂组合物分散剂的方法 Download PDFInfo
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- CN1102668A CN1102668A CN94115107A CN94115107A CN1102668A CN 1102668 A CN1102668 A CN 1102668A CN 94115107 A CN94115107 A CN 94115107A CN 94115107 A CN94115107 A CN 94115107A CN 1102668 A CN1102668 A CN 1102668A
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Abstract
由羟烷基或羟芳基化合物同胺化合物经缩和反
应,得到性能改进的供润滑剂和燃料组成用的添加剂
/分散剂。按照本发明,这种缩和物可从胺同羟基反
应物经酸催化缩和制取。
Description
本发明是关于用于润滑剂和燃料组成的高分子量含氮缩合物(Condensate)。更确切的说,本发明是关于用作润滑剂和燃料组成的添加剂和分散剂,包括显示高总碱值和含低游离胺量的分散剂。本发明的缩合物是将胺反应物与羟烷基或羟芳基反应物通过酸催化缩合制备的。
已经知道用于润滑剂和燃料组成的含氮分散剂,并在此技术中已广泛应用。例如,美国专利号3219666和3272746公开了作为润滑剂和燃料组成的各种含氮“无灰”型分散剂。
美国专利号4428849公开了将链烯基琥珀酰亚胺或硼化链烯基琥珀酰亚胺与烯化聚胺反应制备的用于柴油内燃机氧化油的分散剂。
美国专利号4234435公开了各种羧酸酰化剂,该剂可进一步与聚乙撑多胺和多元醇一类的反应物反应,以制备衍生物,用作进一步后处理的润滑剂添加剂或中间体。已发现该剂在润滑剂添加剂技术中具有其它用途。
美国专利号4477362公开了各种含氮和含氧组分,它们是将脂肪族羟基化合物至少与一叔氨基烷醇反应制备的用作润滑剂和燃料添加剂的衍生物。
美国专利号4200545描述了各种氨基酚,它们可与烃胺或酰化含氮化合物结合,所达到的组分可用于燃料和润滑剂加到2-冲程内燃机中。
美国专利号4116643公开了羧酸半酯的胺盐,它是有机酸物质和羟基胺类的反应产物,这种物质可用作烃类燃料如汽油的防锈添加剂。
上文讨论的专利都没提出本发明的高分子量含氮缩合物,即通过高分子量的聚胺反应物与羟烷基或羟芳基反应物缩合而成。
根据本发明,已发现一种新型的高分子量延长的聚胺,其粘度高于胺反应物,且聚胺缩合物的粘度,按照本发明可根据反应条件和最终产品所需的性质而变化,直至生产出固体物质。
此外,根据本发明已经发现,本发明延长的聚胺对于制备基本无游离胺的分散剂有用,并改进了润滑剂和燃料组成的性能。
另外,根据本发明已经发现,本发明的聚胺可单独用作润滑剂和燃料组成的分散剂和添加剂,或者也可与例如一种酰化剂反应,得到一种更高分子量的分散剂。
再则,根据本发明,已开发一种高产、一步反应,用以制备本发明的高分子聚胺,该反应包括:在酸催化剂存在下,至少一多胺反应物与至少一羟烷基或羟芳基反应物脱氢缩合。
除此之外,根据本发明,各种润滑剂组分,燃料组成和其它多官能流体组分,包括本发明的高分子延长的聚胺或其反应产物,也期望在本发明的范围内。
在专业人员阅读和理解本说明书后,将清楚本发明这些和其它目的。
一种新型的高分子聚胺类已令人惊奇的发现,并以下式说明:
式中R可任意为或烃基,R′为氢、烷基或NH2R″[NR″]y,其中Y的范围从1至大约6,R″为1至大约10个碳原子的链烯基,X为至少1个碳原子的链烯烃,Y代表硫、氮或氧,A为烃基,Z为1至大约10个碳原子的链烯基,1至大约10个碳原子的氧亚烷基或至少含一个氮原子的杂环,这里n为0或1,其值取决于m和q,其中q为0或1,m为1,2或3,X为1至大约10,U为大于1的整数。在优选方案中,X和A的结合必须至少含2个碳原子。在一个方案中,按照上式(Ⅰ)的多胺单元可由下式定义:
其中R,R′,A,Z,X和U按式(Ⅰ)定义,且e是1或2。上述聚(如式(Ⅰ)所举例)是从下述物质得到的:
(A)一种羟烷基或羟芳基反应物,如下式(Ⅱ)所代表:
式中R,Y,X,A,n,q和m与上述规定的相同,以及
(B)一种多胺反应物,如下式(Ⅲ)所代表:
式中R,R′,Z和X与上述规定的相同。
本文使用的术语“烃基”指的是具有与分子残留物直接连接的碳原子以及在本文范围内主要具有碳氢化合物性质的基。这种基包括如下:
(1)烃基;即脂肪族(如烷基或链烯基),脂环族(如烷基或环链烯基),芳香族,脂肪族和脂环族取代的芳香族,芳香族取代的脂肪族和脂环族基等,以及环基,其中环是通过分子另一部分完成的(这就是说,任何两个指出的取代基可一起形成脂肪基)。专业人员对这种基是了解的;
(2)取代了的烃基;即含非烃取代基的基,在本发明里,它不改变基的主要烃的性质。专业人员了解适宜的取代基;
(3)杂基;即当在本发明里主要为碳氢化合物性质时,这种基含有除存在于链中或碳原子构成的环中的碳以外的原子。专业人员对适宜的杂原子是了解的,它包括例如氮、氧和硫。
一般地说,在烃基中每10个碳原子有不大于约三个取代基或杂原子,最好不大于一个。
“以烷基为基础的基”(alkyl-based radical)、“以芳基为基础的基”(alkyl-based radical)等的名称,其意思与上述烷基和芳基等类似。
本发明化合物中的烃基最好无炔
、通常也无烯
的不饱和性,至少约有一个碳原子。这些基一般为碳氢化合物,尤其是低级碳氢化合物,词“低级”指的是含有七个碳原子以下的基。它们最好为低烷基或芳基,最佳一般为烷基。
本发明新型多胺缩合物,是通过羟烷基或羟芳基反应物与胺反应物(Ⅲ)在高温下酸催化缩合制备的。
上面式Ⅲ表示的胺反应物,其特征在于结构中存在R-N基团,其中R如上所述,是低分子量多胺。二种或二种以上胺的混合物可用于与本发明范围内的一种或一种以上的羟烷基或羟芳基反应物反应。本发明的胺反应物可含有脂肪族,环脂族,芳香族,或杂环族,包括脂肪取代的芳香族,脂肪族取代的杂环族,环脂族取代的脂肪族,环脂族取代的芳香族,环脂族取代的杂环族,芳香族取代的脂肪族,芳香族取代的环脂族,芳香族取代的杂环族,杂环取代的脂肪族,杂环族取代的脂环族,和杂环取代的芳香族基团,并且可在分子中含有不饱和部位。如果胺含有这种不饱和部位,则这种不饱和性不是炔烃,这些胺还可含有非烃取代基或基团,只要这些基团不明显干扰胺与本发明的羟烷基或羟芳基反应物反应。这种非烃取代基或基团包括低级烷氧基,较低级烷巯基,硝基,中间插入的基团象-o-和-s-(例如,在-CH2CH2-X-CH2CH2-这样的基团中,X为-o-或-s-)。
按照本发明适宜的多胺反应的包括N-氨基丙基-环己胺,NN′-二正丁基-对苯撑二胺,双-(对氨基苯基)甲烷1,4-二氨基环己烷等等。
在制备本发明的组分中,还可使用杂环多胺(Ⅲ)。本文所用的术语“杂环多胺(类)”意思是描述那些在杂环中至少含有一个氮原子作为杂原子的杂环胺。杂环胺(按照本发明)可以是饱和的,或不饱和的,以及可含有不同的取代基,如硝基,烷氧基,烷巯基,烷基,链烯基,芳基,烷代芳基或芳代烷基取代基。一般来说,取代基中碳原子总数不大于约20。杂环胺可含有不大于一个氮杂原子,最好为五元或六元杂环。
适宜的杂环多胺为氮丙啶,吖丁啶,吖戊烷,四氢化和二氢化吡啶,吡咯,吲哚,哌啶,咪唑,二氢化和四氢咪唑,哌嗪,异吲哚,嘌呤,吗啉,硫吗啉,N-氨基烷基吗啉,N-氨基烷基硫吗啉,N-氨基烷基哌嗪,N,N′-二氨基烷基哌嗪,氨杂环庚三烯,吖辛因,壬癸因,吖癸因,四氢化和二氢化和多氢化上述每种化合物的衍生物,以及二种或二种以上的这些杂环的混合物。优先选择的杂环胺是饱和的五元和六元杂环胺,在杂环中只有氮,氧和/或硫,尤其是哌啶,哌嗪,硫吗啉,吗啉,吡咯烷等等。哌啶,氨烷基取代的哌啶,哌嗪,氨基烷基取代的哌嗪,吗啉,氨烷基取代的吗啉,吡咯烷,以及氨烷基取代的吡咯烷尤其更佳。通常,在杂环的氮原子形成部分上氨烷基取代基被取代。这种杂环胺的具体例子包括氨基丙基吗啉,氨基乙基哌嗪,及N,N′-二氨基乙基哌嗪。
作为胺类,氨基磺酸及其相应于通式(Ⅳ)的衍生物也适用:
式中Rd为-NHz,碱或碱土金属;Ra为一多价有机基,其价数等于X+Y;Rb和Rc每个可任意为氢,烃基及取代烃,但至少Rb或Rc之一的每个氨基磺酸分子为氢;X和Y每个为等于或大于1的整数。从式中可见,每个氨基磺酸反应物以至少一个HN或HzN-基团和至少一个-
-R基团为特征。这些磺酸可以是脂肪酸,环脂酸,或芳香族氨基磺酸,以及相应官能的磺基衍生物。尤其是氨基磺酸可以是芳香族氨基磺酸,即RaY为一多价芳香基,如苯撑,其中至少一个-
-R基团直接与芳基核碳原子相连。氨基磺酸还可以是单氨基脂磺酸,即其中X为1,Ra为多价脂肪基,如乙撑,甲代乙撑,三甲撑和2-亚甲基甲代乙撑。美国专利3029250,3367864,3926820公开了适宜用作胺反应物(Ⅲ)的氨基磺酸及其衍生物,在这里将这种公开一并作为参考。
可用作(Ⅲ)的高分子量烃基胺,一般是通过把分子量至少约400的氯化聚烯烃与氨或适当的胺反应制备而得。这种胺类在技术中为已知且作了叙述,例如在美国专利3275554和3438757中就如何制备这些胺作了公布,在此一同作为参考。
适宜用作胺反应(Ⅲ)的另一组胺是支链多亚烷基聚胺。支链多亚烷基聚胺类是多亚烷基聚胺类,其中的支链基团是平均至少含有一个氮键合的氨基链烯基团的侧链。
这些反应物可表示如下:
其中R为亚烷基,例如乙撑,甲代乙撑,丁撑和其它同系物(都是直链和支链)等等。但最好是乙撑,X,Y和Z为整数,例如X为4~24或更大,但最好为6~18,Y为1~6或更大,但最好为1~3,Y为0~6,但最好为0~1。X和Y单元可以是连续,交替,有规或无规分布。
这种聚胺反应物优选种类包括以下类型:
其中n为整数,例如1~20或更大,但最好为1~3,其中R最好为乙撑,但也可以是甲代乙撑,丁撑等等(直链或支链)。
美国专利3200106和3259578就如何制备这种聚胺作了公开,在此一并作为参考。
适宜的胺类还包括聚氧化亚烷基多胺,例如聚氧化亚烷基二胺和聚氧化亚烷基三胺,其平均分子量范围在约200~400,最好约为400~2000。所举的这些聚氯化亚烷基多胺可以下式为特征:
NH2-亚烷基-(O-亚烷基)m-NH2(ⅦA)
其中m值约为3~70,最好约为10~35。
R-[亚烷基-(O-亚烷基)n-NH2]3-6(Ⅷ)
其中n总值约为1~40,但须所有n值总和约为3~70,一般约为6~35,R为多价饱和的多达10个碳原子的烃基,其碳原子价数为3~6。亚烷基团可以是直链或支链,含有1~7个碳原子,一般为1~4。或Ⅶ和Ⅷ中的各种亚烷基团可相同或各异。
用于本发明目的的优选的多氧化亚烷基聚胺反应物包括聚氧化乙撑二胺聚氧化丙撑二胺及平均分子量为200~2000的聚氧化丙撑二胺。市售聚氧化亚烷基多胺类,例如可从Jefferson化学有限公司以商品名“Jeffamines D-230,D-400,D-1000,D-2000,T-403等”得到。
美国专利3804763和3948800对这种聚氧化亚烷基多胺反应物作了公开,在此一同作为参考。
另一类用于本发明优选胺反应物是亚烷基多胺,包括聚亚烷基多胺,这在下文详细说明。亚烷基多胺包括符合下式的那些:
H-
-(亚烷基-NR)n-R11(ⅦB)
式中n为1至大约10;每个R″可任意为氢原子、烃基或多达约30个碳原子的羟基取代烃基团,而“亚烷基”团具有1至大约10个碳原子,但优选的亚烷基是乙撑或甲代乙撑,尤以每个R″为氢的亚烷基多胺为佳,以乙撑多胺和乙撑多胺的混合物为最佳。通常n的平均值约为2~7。这种亚烷基多胺包括甲撑多胺,己撑多胺,乙撑多胺,丙撑多胺,戊撑多胺,庚撑多胺,等。也包括这种胺及有关的氨烷基取代的哌嗪的同系物。
亚烷基多胺用于制备羧基衍生物组合物,它包括乙二胺,三乙撑四胺,丙二胺,三甲撑二胺,己甲撑二胺,癸甲撑二胺,辛甲撑二胺,二(庚甲撑)三胺,三丙撑四胺,三乙撑戊胺,二(三甲撑)三胺,N-(2-氨基乙基哌嗪,1,4-双(2-氨基乙基)哌嗪等。由两种或多种上述亚烷基胺缩合得到的高级同系物,同两种或多种任何前述多胺的混合物一样,也可用作反应物(Ⅲ)。
亚乙基多胺,诸如上面提到的那些品种,基于价格和效果的原因,是特别有用的。这类多胺在题目为“二胺和高级胺”一文中有详细叙述,该文登载在“Encyclopedia of Chemical Technology”(化学工艺大全),第二版,第7卷,27~39页(Kirk & othmer,Interscienec Publishers,Division of John Wiley and Sons,1965),由于该文公开了有用的多胺,在此以供参考。这类化合物传统上是通过氯代亚烷同氨反应制取,或从哌嗪同开环剂如氨等反应制取。由此得到的亚烷基多胺的略为复杂的混合物,包括诸如哌嗪的环状缩合产物。
其它类型有用的多胺反应剂混合物是由汽提上述多胺混合物获得。在这种情况下,分子量较低的多胺和挥发性杂质从亚烷基多胺混合物中被除掉,留下的残余物常称之为“多胺底”(Polyamine bottom)。一般说来,从亚烷基多胺底中可以鉴定出不到2%(通常不到1%)材料的沸点约低于200℃的物质。乙撑多胺底对本发明十分有用,它易于取得,这种底含有不到~2%重量的二亚乙基三胺(DETA)或三亚乙基四胺(TETA)。其代表性样品产自美国得克萨斯州Freeport的DOW化学公司,它被称之为“E-100”,其比重在15.6℃为1.0168,含氮重量百分数为33.15,在40℃的粘度为121厘沲。样品的气体色谱分析结果表明,它含有~0.93%“低沸馏份端”(DETA),0.72%TETA,21.74%四乙基五胺,以及76.61%。五亚乙基六胺和高级胺(按重量计算)。这些亚烷基多胺基包括环状的缩合产物,诸如哌嗪,以及二亚乙基三胺三亚乙基四胺等的高级同系物。
本发明用的多胺反应物的优选基团包括式(Ⅱ)的多胺:
其中各R是氢或烃基,各R′分别为氢、烷基或NH2R″(NR″)y(其中各R″分别为C1-约C10亚烷基,Y是1-约6的数),各Z分别为C1-约C10亚烷基、含杂环氮的环亚烷基或C1-约C10氧亚烷基且X是1-约10的数。
如上面式(Ⅱ)所示的羟烷基的羟芳基反应物是推荐的多羟基物质,它们能同上面讨论的胺缩合,并更容易缩合成与形成环状产物不同的分子量极高的物质。含羟基的反应物可从以脂肪族、环脂族和芳族为主的基团中选取,这种基团以烷基为主的基团为宜,最好是羟乙基。这些含羟基物质还可含有别的官能团,只要它们不影响同胺的缩合反应,或对生成的高分子量聚胺缩合物性质产生有害的影响。
对含羟基反应物除了上面讨论的限制外,它们能从许多含羟基化合物中选取。可以提到的这类范围广泛的物质(但不是全部)有聚亚烷基多醇、亚烷基二醇、以及聚氧烷烯多醇,诸如聚氧乙烯多醇、聚氧丙烯多醇、聚氧丁烯多醇等。这些聚氧烷烯多醇(有时称之为聚二醇)可含有高达150个氧烷烯基团,其中的氧烷烯基含有2~8个碳原子。这种聚氧烷烯多醇一般是二元醇。也就是其分子的每个末端带一个-OH基。为了使这类醇可用作反应物,它至少需带有两个末端-OH基团。这些亚烷基二醇和聚氧烷烯二醇的单醚也是有用的反应剂。它们包括这些二醇的单芳基醚、单烷基醚、以及单芳烷基醚。这类醇可用下面的通式来表示:
其中R是芳基,如苯基、低级烷氧苯基、或低级烷代苯基;低级烷基,诸如乙基、丙基、叔丁基、戊基等;或者是芳烷基,诸如苄基、苯乙基、苯丙基、对-乙基-苯乙基等;P等于零至约150,RARB是碳原子数2~8个的低级亚烷基,又以2~4个碳原子为宜。对本发明的用途来说,聚氧化烯二醇及其上面所述的单醚被认为十分有用;这种二醇里,亚烷基是乙撑或甲代乙撑,P至少是2。
用作羟基反应物的芳基多元醇,包括多元酚和萘酚,它们是推荐使用的羟芳基化合物。这些羟基取代的芳族化合物,除了羟基取代基外,还可含有其它的取代基,诸如卤基、烷基、链烯基、烷氧基、烷基巯基、硝基等。通常芳族羟基化合物含有1~4个羟基,它们可用下列具体例子来加以说明:β-萘酚,对-硝基苯酚,α-萘酚,甲酚,间苯二酚,邻苯二酚,百里酚,丁子香酚,P,P′-二羟基联苯,氢醌,连苯三酚,间苯三酚,己基-间苯二酚,苔里酚,愈疮木酚,α-癸基-β-萘酚,庚酚同0.5克分子甲醛的缩合产物,辛酚同丙酮的缩合产物,二-(羟苯基)醚,二-(羟苯基)硫醚,二-(羟苯基)二硫醚。
用作含羟基反应物的其它具体醇类是醚醇和氨基醇,包括如氧烷烯一,氧芳烯一,氨基亚烷基一,以及氨基亚芳基取代醇,这些醇带有一个或若干个氧烷烯基,氨基亚烷基,或氨基亚芳氧基-亚芳基。其例子有溶纤剂,卡必醇,单-(庚基苯氧基亚丙基)取代的丙三醇,聚(氧苯乙烯)、氨基乙醇,二(羟乙基)胺,三(羟丙基)胺,N,N,N′,N′-四羟基三甲撑二胺等。
本发明用的多羟基醇反应物最好含2~10个羟基。其例子有上面提到的亚烷基二醇和聚氧烷烯二醇,诸如乙二醇、二甘醇,三甘醇,四甘醇,二丙二醇,三丙二醇,二丁二醇,三丁二醇,还有如亚烷基含2~8个碳原子的其它亚烷基二醇和聚氧烷烯二醇。
适合作反应物的最佳一类醇是碳原子数约12以下尤其是3~10个的多元醇。这类醇包括丙三醇,赤藓醇,季戊四醇,双季戊四醇,葡糖酸,甘油醛,葡萄糖,阿拉伯糖,1,7-庚二醇,2.4-庚二醇,1,2,3-己三醇,1,2,4-己三醇,1,2,5-己三醇,2,3,4-己三醇,1,2,3-丁三醇,1,2,4-丁三醇,2,2,6,6-四-(羟甲基)环己醇,1,10-癸二醇,毛地黄糖等。含羟基不少于3个、不超过5个的脂肪族醇尤其受到推荐。
考虑适合用作含羟基反应物的氨基醇,含有两个或两个以上的羟基。适用的氨基醇例子是N(-羟-低级烷基)胺和多胺,诸如二(-2-羟乙基)胺,三(-2-羟乙基)胺,N,N,N′-三-(2-羟乙基)乙二胺,N-(2-羟丙基)-5-乙酯基-2-哌啶酮,还有这些化合物同脂肪醇、尤具是低级链烷醇的醚,以及N,N-二(-3-羟丙基)甘氨酸等。另外考虑使用的氨基醇是别的多-N-羟烷基取代的亚烷基多胺,其中的亚烷基多胺已知前面所述,尤其是亚烷基含2~3个碳原子的多胺。
聚氧烷烯多醇是受推荐的一种羟基连续反应物,它含有2或3个羟基,它的分子主要是由憎水部分
和亲水部分-CH2CH2O-两类基团组成,其中Rp是碳原子数为3以下的低级烷基。制备这种多醇先是将分子式为R(OH)q的化合物同分子式为
、其末端为氧乙烯基的化合物反应(其中q等于2~3,RE是烃基),然后,将产物与氧乙烯(环氧乙烷)反应制取。RE(OH)q也可以是如三羟甲基丙烷,三羟甲基乙烷,乙二醇,三亚甲基二醇,四亚甲基二醇,三(-β-羟丙基)胺,1,4-(2-羟乙基)环己烷,三-(羟甲基)氨基甲烷,2-氨基-2-甲基-1,3-丙烷二醇,N,N,N′,N′-四(2-羟丙基)乙二胺,N,N,N′,N′-四(-2-羟乙基)乙二胺,间苯二酚,或前面提到的其它说明例之一。以上所述RE(OH)q多醇也可以单独用含羟基(Ⅱ)的反应物。
用于本发明的其它含羟基反应物是分子式如下的羟烷基,羟烷基氧烷基,以及羟芳基硫醚:
其中,f等于1或2,RF是碳原子数1~10的烷基,或烷基氧烷基,这里烷基有1~10个碳原子,又以2~4个为宜,RF还可以是碳原子数不少于6个的芳基。这类含羟基反应物,供本发明用最好选2,2′-硫二乙醇和2,2′-硫二丙醇。制备本发明多胺用的反应物的优选混合物包括这样的混合物,其中(A)是具有三个羟基的式(Ⅱ)的多元醇或具有两个或多个羟基的式(Ⅱ)的氨基醇且反应物(B)是具有两个伯氮原子的亚烷基多胺,其中亚烷基含2-约10个碳原子,反应是在高温及酸催化剂下进行的。
正如前面所述,胺反应物同羟烷基或羟芳基化合物反应需要有酸催化剂。对本发明有用的催化剂包括无机酸(单酸,二酸和多酸),诸如硫酸和磷酸;有机磷酸和有机磺酸,诸如R*P(O)(OH)2和R*SO3H,其中R*是烃基;还有H3PO4和H2SO4的碱金属部分盐,诸如NaHSO4,LiHSO4,KHSO4,NaH2PO4,LiH2PO4和KH2PO4;H3PO4和H2SO4的碱土金属部分盐,诸如CaHPO4,CaSO4和MgHPO4;此外,还有Al2O3和沸石。磷酸是优先选择的催化剂,因为它可从市场买到并易于处理。还有一些用于本发明的催化剂是在反应混合物中处理时会产生酸的物质,如亚磷酸三苯酯。
反应在高温下进行,温度取决于具体所用的反应物,其范围为60~265℃。不过,大多数反应在220~250℃范围进行。该反应既可在常压也可在减压下进行,这取决于所用的具体反应物和伴随的经济因素。用本发明方法制得的高分子量聚胺的缩聚度,只要控制在反应中不生成固体产物为限,缩聚度的控制一般采用限制缩聚剂用量的方法,即放入反应介质里的羟烷基或羟芳基反应物的用量。在某优选实例中,本发明的缩聚高分子量聚胺在室温可以浇注,其粘度范围从高于胺反应物(Ⅲ)粘度100%~6000%。在另一优选方案中,本发明的缩合的高分子量多胺的粘度为50-约1000%,高于胺反应物(Ⅲ)的粘度。在某最佳实例中,这些聚胺的粘度范围在100℃为50~200厘沲。需要指出的是,上面对本发明产物缩聚度的限制,仅是为了在润滑剂组合物里最终使用这些材料。对于其它的或有关的应用,上述缩聚反应的固体产物便能符合要求,这通过调节放入反应介质里各个反应物的相对用量来达到缩聚反应,生成高分子量固体产物。
下面的实例说明各种高分子量聚胺缩合物的典型产物的制备方法。虽然这些例子会告诉用于此行者在本发明范围内如何工作,它们并不是用作对本发明范围的限制,这种范围只是在权利要求里才予以具体规定。需要指出的是,下面的实例里,以及本说明书和权利要求,所有百分数和份数都是用来指重量百分数和重量份数,除非另外指明。
实例Ⅰ
一个500毫升四颈圆底烧瓶,装有玻璃搅拌器、温度计套管、液面下的N入口管、迪安-斯达克分水器、以及Friedrich冷凝器,并内装入
a)201克四亚乙基五胺(TEPA)。
b)151克三羟甲基氨基甲烷(THAM)的40%水溶液,以及
c)3.5克85%H3PO4将混合物经一小时加热到120℃,用N2吹扫,在一小时内再加热到130℃,然后用二小时余加热到230℃。混合物在230℃。混合物在230~240℃保持4小时,于241~250℃保持3小时。产物冷却至150℃,用硅藻土助滤剂过滤。
实例Ⅱ
一个3升四颈圆底烧瓶,装有玻璃搅拌器、温度计套管、液面下的N2入口管、迪安-斯达克分水器、以及Friedrich冷凝器,并内装入
a)1299克HPA Taft胺(amine bottom)。
b)727克三羟甲基氨基甲烷(THAM)的40%水溶液。将混合物加热到60℃,加入23克85%H3PO4。在0.6小时内加热混合物到120℃。用N2吹扫,再经1.25小时升温到150℃,经一个多小时升温到235℃。混合物在230~235℃保持5小时。然后用0.75小时升温到240℃,并在240~245℃保持5小时。产物冷却到150℃,用硅藻土助滤剂过滤。产率:84%(1221克)。
实例Ⅲ
一个3升圆底烧瓶,装有搅拌器、温度计套管、液面下的N2入口管、以及汽提冷凝器,瓶内装入363克THAM和1200克TEPA。然后在110℃加入16克H3PO4。用N以0.25英尺/小时(cfh)速度吹扫。将混合物在0.8小时内加热到220℃,并在220~225℃保持1.2小时;再用0.2小时升温到230℃,并在该温度保持4.75小时:收集得129克馏出液。混合物在242~245℃放置和保持5小时:在分水器中又收集得39克馏出液。在246~255℃再保持1.2小时:分水四里积聚得178克馏出物:NNBbpb=170。混合物在155℃用45克硅藻土助滤剂过滤。
实例Ⅳ
一个3升烧瓶,装有搅拌器、温度计套管、液面下的N2入口管以及汽提冷凝器,瓶内装入363克THAM和1200克TEPA。在100℃加入16克H3PO4。用N2以0.2cfh速度吹扫。混合物在0.4小时内升温到165℃;再用0.6小时升温到241℃。在241~243℃保持0.3小时。反应物再用0.5小时加热至250℃,并在该温度保持5.5小时:分水器里收集得288克馏出物;NNBbpb=506。用55克硅藻土助滤剂在150℃过滤。
实例Ⅴ
一个1升烧瓶,装有搅拌器、温度计套管、液面下的N2入口管以及迪安-斯达克分水器,并内装入121克THAM和400克TEPA。在60℃加入8.2克H3PO4。用N2以0.15cfh速度吹扫。反应混合物在一小时内升温到150℃,再用1.5小时升温到230℃。反应温度在230~232℃保持4.25小时:分水器里收集得17克馏出物。混合物放置并在237℃保持3.25小时:分水器里收集得38克馏出液。反应物再用0.75小时继续升温到241℃,并在241~242℃保持4.75小时:分水器里收集得到50克馏出物。后者放置并在250℃持5小时:分水器里收集共得53克馏出物:NNBbpb=96.5。用20克硅藻土助滤剂在150℃过滤。
实例Ⅵ
一个500毫升烧瓶,装有搅拌器、温度计套管、液面下N2入口管、通往迪安-斯达克分水器,瓶内装入201克TEPA,468克甘油。在80℃加入2.3克H3PO4。用N2以0.35cfh的速度吹扫。混合物在2小时内加热到220℃;用1小时升温到240℃;1.5小时到245℃,再1小时到255℃。反应温度保持在255~252℃2小时:从分水器收集到12克馏出物。使混合物放置,并在255~262℃保持7小时;在分水器中收集得34克馏出物。再将混合物温度保持在255~260℃一个多小时。在分水器里共收集到36克馏出物:NNBbph=435。在130℃用23克硅藻土助滤剂过滤。
实例Ⅶ
一个500毫升烧瓶,装有搅拌器、温度计套管、液面下N2入口管、迪安-斯达克分水器,瓶内装入201克TEPA,45克六元甘油。在85℃加入3.5克H3PO4。用N2以0.35cfh的速度吹扫。混合物经0.7小时升温到245℃,并在245~260℃保持1.75小时:在分水器中收集得10g馏出液。使混合物放置并在260~270℃保持7.5小时:在分水器里共收集得27克馏出物:NNBbph=645。在125℃用20克硅藻土助滤剂过滤。
高缩合的聚胺继续反应生成分散剂
本发明的高分子量缩合聚胺,虽然本身就可用作润滑剂、燃料的添加剂和分散剂。一般说来,能用来同本发明的聚胺继续反应的物质,都为专于此行者所熟悉,它们在许多书、论文和专利中均有叙述。下文提到的许多参考资料,涉及到到分散剂的具体类型,由于它们公开的技术适合于这里讨论的内容,当然将其列入本说明书,以供参考。
羧酸或酚类反应物
可以用来同上述聚胺反应生产较高分子量的分散剂,藉以提供本发明用途的反应物,首先要提到的是羧酸。它可以制成适合本发明用途的中性和碱式盐,所用的羧酸包括脂肪族、环脂族、以及芳族单羧酸和多元羧酸,诸如环烷酸,烷基或链烯基取代的环戊酸,烷基或链烯基取代的环己酸,烷基或链烯基取代的芳香族羧酸。所用脂肪酸一般至少含八个碳原子,最好多于12个。通常,碳原子数不超过约400个。一般说来,如果脂族碳链带有支链,与任何给定同样碳原子数相比,其油溶性更好。所用环脂族和脂族羧酸可以是饱和酸,也可以是不饱和酸。具体例子包括2-乙基己酸,亚麻酸,丙烯四聚体取代的马来酸,水愈酸,异硬脂酸,壬酸,癸酸,棕榈油酸,亚油酸,月桂酸,油酸,蓖麻油酸,十一烷酸,二辛基环戊烷羧酸,肉豆蔻酸,二月桂基十氢萘羧酸,硬脂酰-八氢茚羧酸,棕榈酸,市售的二种或几种羧酸如妥尔油酸,品红酸等的混合物。
用于本发明的盐类制备,优先选使用的一类油溶性羧酸基团是油溶性芳香族羧酸。其通式表示如下:
其中R*是以脂肪族烃为主的基团,它至少含有四个碳原子,但不超过400个脂肪族碳原子,a是1~4的整数,Ar*是碳原子数约14以下的多元芳烃环,每个X可以是硫或氧原子,m是1~4的整数,但是,此时R*和a必须使每个以XⅢ表示的酸分子中,由R*基团提供的脂肪族碳原子至少平均占8个。由可变的Ar*表示的芳香环例子,是从苯,萘,蒽,菲,茚,萄,联苯等派生得到的多元芳基。一般说来,用Ar*表示的基团是由苯或萘派生达到的多元环,如亚苯基,亚萘基,诸如甲基亚苯基,乙氧基亚苯基,硝基亚苯基,异丙基亚苯基,羧基亚苯基,巯基亚苯基,N,N-二乙基-氨基亚苯基,氯代亚苯基,二丙氧基亚萘基,三乙基亚萘基,以及其类似的三元、四元、五元环等。
R*基团通常仅是烃基,宜采用诸如烷基或链烯基等基团。不过,R*基可以含有少量取代基,如苯基,环烷基(如环己基,环戊基等),只要R*基团上保持烃的特性,它还可以含有非烃基团,如硝基,氨基,卤素(如氯,溴等),低级烷氧基,低级烷基巯基,桥氧基(即=O),硫代基(即=S),中间插入的基团如-NH-,-O-,-S-等。为了本发明的用途,R*中的非碳原子所占R*基团的总重量只要不超过约10%,便能保留其烃的特性。
R*基团的例子包括丁基,异丁基,戊基,辛基,壬基,十二烷基,廿二烷基,四十烷基,5-氯己基,4-乙氧基戊基,4-己烯基,3-环己基辛基,4-(对-氯苯基)辛基,2,3,5-三甲基庚基,4-乙基-5-甲基辛基,以及由聚合的烯烃得到的取代基,诸如聚氯丁二烯,聚乙烯,聚丙烯,聚异丁烯,乙-丙共聚物,氯化烯烃聚合物,氧化乙-丙共聚物等。Ar*基团同样地也可以含有非烃取代基,这些种类不同的取代基例如低级的烷氧基,低级的烷基巯基,硝基,卤基,碳原子数少于4的烷基或链烯基,羟基,巯基等。
特别有用的一类羧酸,其分子式如下:
其中,R*,X,Ar*,m和a与XⅢ规定的相同,P是1~4的整数,通常是1或2。这类羧酸里,尤其受推荐的一类油溶性羧酸,
其中,R**是含有至少4个至约400个碳原子的脂肪族烃基,a是1~3的整数,b是1或2,c是0,1或2,最好是1,但是,R**和a必须使每个酸分子的脂肪烃取代基平均至少含约12个脂族碳原子。在后一类油溶性羧酸基团中,尤其有用的是脂肪烃取代的水杨酸,其中,每个脂肪烃取代基平均至少含约16个碳原子,而每个分子中含有1~3个取代基。由这类水杨酸制成盐,水杨酸里的脂肪烃取代基,来自聚合的烯烃,尤其是聚合的低级1-单烯烃,诸如聚乙烯,聚丙烯,聚异丁烯,乙-丙共聚物等,取代基平均含有约30~400个碳原子。
上述分子式为XⅢ-XⅤ的羧酸是十分有名的,它们可以按照这方面大家知道的方法制取。这类羧酸以及制备它们的中性和碱式金属盐的方法也是为人熟知的,并开发在如美国专利2,197,832;2197835;2,252,662;2,252,664;2,174,092;3,410,798以及3,595,791。
另一类用于本发明的中性和碱式羧酸盐,来自丁二酸链烯酯,其通式如下:
其中,R*的规定与前面式XⅢ相同。美国专利3,271,130;3,567,637和3,632,510对这类盐和制备它们的方法有所叙述,借此供这方面参考。所需的R*基的例子是多亚烷基,其特征在于Mn值为150-约5000,且Mw/Mn值约为1.5-约4.0。
具体叙述从上文所说的磺酸、羧酸及其两种或多种这些酸的混合物制成碱式盐方法的其它专利,包括美国专利2,501,731;2,616,904;2,616,905;2,616,906;2,616,911;2,616,924;2,616,925;2,617,049;2,777,874;3,027,325;3,256,186;3,282,835;3,384,585;3,373,108;3,365,396;3,342,733;3,320,162;3,312,618;3,318,809;3,471,403;3,488,284;3,595,790以及3,629,109。由于这些专利公开了这方面现有的技术条件以及具体适用的碱式金属盐,因此,把它们公开的技术包括到本说明书里。酚类的中性和碱式盐(一般称之为酚盐),在本发明的组成中也是有用的,这些酚盐为专于此行者所熟知。生产这些酚盐的酚类,其通式如下:
R*,a,Ar,X和m与上文式XⅢ所述的意义和选择方法相同。也适用对式XⅢ所述的同样实例。
常用的一类酚盐是由通式如下的酚类制得:
其中,a是1~3的整数,b是1或2的整数,z是零或1,式XⅢ的R′是基本上以饱和烃为主的取代基,平均含有30至约400个脂肪族碳族原子,R选自低级烷基、低级烷氧基、硝基以及卤素这些基团所组成。
用于本发明的特定一类酚盐,是碱性的(即高碱性等)ⅡA族金属硫化酚盐,它们是用上文所述的酚,经硫化剂如硫、卤化硫、硫化物或氢硫化盐化制成。美国专利2,680,096;3,036,971和3,775,321谈到了制备这些硫化酚盐的方法,对于它们在这方面的公开,在此以供参考。
酚类经亚烷基(如亚甲基)桥键合成制成的另一种酚盐也是合用的。它们是用单环或多环酚类,一般在某种酸性或碱性催化剂存在下,与醛或酮反应制成。美国专利到3,350,038,特别是其中6~8栏,对这类键合酚盐和硫化酚盐均有详细叙述,对于该专利在这方面的公开,在此以供参考。
当然,在本发明的组合物中,上文所述的羧酸类以及酚类的中性和碱式盐,也可用它们二种以上的混合物,包括任何这些二种以上盐的混合物。
上述反应产物形成通式如下的添加剂/分散剂物质:
[(QTt)vJj]
其中Q表示上述羧酸或酚反应物中的非活性部分;T表示其中的活性部分,可以是酰基,酸基,氧亚烷基,亚芳基或亚氨基;J表示上述高分子量聚胺的缩聚部分;这与上述定义的相同;t和j为至少是1的任意整数。
上述分散剂一般按合成本发明的高分子量聚胺相同的方法制取。换句话说,它们是用至少一种本发明的高分子量聚胺同至少一种上文所述的反应物,在高温下通过酸催化缩合反应制取。前面所述的催化剂也适用于这个反应。这些分散剂一般具有总碱值约45-约90,特别是约55-约80。
在一个方案中,可通过以下方法制备润滑剂和燃料组合物用的高分子量添加剂/分散剂,即使(A)和(B)反应,其中
(A)是烃基取代的羧酸或其至少含约34个碳原子的衍生物,
(B)至少一种由式(Ⅰ)和式(Ⅱ)的羟烷基或羟芳基化合物衍生的多胺反应物:
这里各R分别是氢或烃基,Y代表S,N或O;A和X各分别代表亚烷基;n是0,1或2(取决于m和q,q是0或1,m是1,2或3),
这里各R是氢或烃基,各R′分别是氢、烷基或NH2R″(NR″)y(其中各R″分别是C1-约C10亚烷基且Y是C1-约C6之间一个数,各Z分别是C1-约C10亚烷基、含氮杂环的环亚烷基或C1-约C10氧亚烷基且X是1-约10之间的一个数。
按照上述方法制得的添加剂分散剂具有约3-约90的总碱值,在一实施方案中,可以为约55-约85。
按照上述方法制得的添加剂分散剂(总碱值为3-约90)的一个方案是至少一种取代的琥珀酸或由取代基和琥珀酸基构成的其衍生物,其中取代基是由多亚烷基得到的,所述多亚烷基的特征在于Mn值为1300-约5000且Mw/Mn值为1.5-约40,其中所述多胺是由选自甘油、三羟甲基丙烷、三羟甲基乙烷和三(羟甲基)氨基甲烷的羟烷基或羟基化合物和选自三亚乙基四胺、二亚乙基三胺、四亚乙基五胺、五亚乙基六胺及其混合物的胺化合物衍生的。
特别是,Q可以是由多亚烷基取代的琥珀酸或其衍生物衍生的,其中所述多亚烷基取代基的特征在于Mn值为150-约5000且Mw/Mn为约1.5-约4.0。
下面提供的实施例,是用来说明从本发明聚胺同上述反应物反应制得的各种分散剂。此外,需要强调的是,这些实例只是供说明的用途,并不是用来限制本发明的范围,这种范围仅在权利要求中予以澄清。
实例A
一个12升四颈圆底烧瓶,装有搅拌器、温度计套管、液面下N2入口管、迪安-斯达克分水器以及Friedrich冷凝器,瓶内装入(a)460克TEPA/THAM(5N∶1.50H)聚胺,H3PO4催化剂,(b)2500克2C稀释油。将混合物加热到105℃,从滴液漏斗在1.5小时内加入3360克聚异丁烯(分子量1000)取代的丁二酸酐(皂化值100)。用N2慢慢吹扫。混合物升温到160℃,并保持5.0小时。用硅藻土助滤剂在150℃过滤混合物,得到最终产物。产率:96%(5991克),40%2C稀释油。产物分析:%N=2.31/2.42;游离胺=0;TBN(776)=49.1。
实例B
一个12升四颈圆底烧瓶,装有搅拌器、温度计套管、液面下N2入口管、迪安-斯达克分水器、以及Friedrich冷凝器,瓶内装入(a)605克HPA Taft胺/THAM(SN∶1.20H)聚胺,H3PO4催化剂,(b)3262克2C稀释油。将混合物加热到110℃,从滴液漏斗在0.7小时内加入4300克聚异丁烯(分子量1000)取代的丁二酸酐(皂化值100)。用N慢慢吹扫。混合物在一小时内升温到160℃,并在160~162℃保持5小时。用硅藻土助滤剂在150℃过滤混合物,得到最终产物。产率:96%(8155克),40%2C稀释油。产品分析:%N=2.28/2.19;TBN(776)=46.5;TAN(744)=7.7。
实例C
一个1升烧瓶,装有搅拌器、温度计套管、以及回流冷凝器,瓶内装入39克实例Ⅳ的反应产物以及75克甲醇。将混合物在40℃加热和搅拌成透明溶液。在40℃往混合物中加入2C稀释油。接着在62~50℃用0.8小时加入218克聚异丁烯(分子量1000)取代的丁二酸酐(皂化值100,溶于110克甲苯的溶液)。混合物在50~65℃保持1小时。然后用1.5小时汽提至110℃,用1小时提至120℃,再用0.8小时多点汽提到160℃。通N2以0.15cfh的速度慢慢吹扫,并在160℃保持6小时,随后用25克硅藻土助滤剂在150℃过滤。
实例D
一个1升烧瓶,装有搅拌器、温度计套管、液面下的N2入口管、以及迪安-斯达克分水器,瓶内装入64.6克实例Ⅰ的产物以及168稀释油。在110℃~135℃用0.1小时加进110克聚丙烯(分子量168)取代的丁二酸酐(皂化值420)。用N2以0.15cfh的速度慢慢吹扫。混合物在130℃~130℃保持0.2小时。然后将它在0.8小时内升温到165℃,并在165℃保持4.5小时。混合物放置后加入56克VcomLB625。用25克硅藻土助滤剂在145℃过滤混合物。
实例E
一个1升烧瓶,装有搅拌器、温度计套管、漏粉斗、以及迪安-斯达克分水器,瓶内装入44.3克实例Ⅵ的产物和2Cdil油。在105℃用0.7小时将336克聚异丁烯(分子量1000)取代的丁二酸酐(皂化值100)加入混合物中。用N2以0.35cfh的速度慢慢吹扫。混合物在1小时内升温到160℃,并在160℃~162℃保持5.5小时。用30克硅藻土助滤剂在150℃过滤混合物。
实例F
一个1升烧瓶,装有搅拌器、温度计套管、液面下的N2入口管、以及迪安-斯达克分水器,瓶内装入50.3克实例Ⅶ的产物和2C稀释油。在110℃用0.9小时将336克聚异丁烯(分子量1000)取代的丁二酸酐(皂化值100)加入混合物中。用N2以0.35cfh的速度慢慢吹扫。混合物在0.6小时内升温到160℃,并在160℃~163℃保持5.5小时。用22克硅藻土助滤剂在150℃过滤混合物。
实例G
一个1升烧瓶,装有搅拌器、温度计套管、回流冷凝器、瓶内装入224克聚异丁烯(分子量1000)取代苯酚在72℃用0.15小时向混合物加入13.2克(CH2O)x、正丁醇、1.6克NaOH溶液。混合物于72℃保持5小时(4.5小时后溶液变透明)。然后向混合物中加入25克HCl溶液,使溶液呈中性。再用0.1小时加入13.9克1074~27181。混合物在1.2小时内升温到110℃(开始逸出馏出液)。接着混合物用0.4小时升温到120℃,再用0.6小时多升温到158℃。混合物在158~160℃保持0.8小时。使它放置并在160℃保持5小时。然后将它在160℃,30mm下汽提。用22克DD1600在150℃过滤。便制成过滤后的产物。
上述实例具体说明了高TBN(45~50)分散剂,其中游离胺含量特别低(<0.1),并采用本发明高分子量缩合聚胺制成的品种,其引擎(发动机)测试特性,要优于用一般的胺如胺底(Amine bottom)、四亚乙基胺等制成的品种。此外,从这些产物得到了热稳定性更好、TBN高达77、40%溶液的分散剂。不过,对发动机特性有改进作用的低TBN分散剂,也可以按本发明方法制取。
本发明的上述组合物,可以用作基于不同润滑粘度油的各种各样润滑剂,这些油包括天然和合成的润滑剂油及其混合物。这类润滑剂有供火花点火和压缩点火内燃机的曲轴箱润滑油,它们可用于汽车和拖拉机发动机,二冲程循环发动机,航空活塞发动机,航海和铁路柴油发动机等。也可用于气体发动机,固定式电力发动机以及透平机等。将本发明的组合物混入自动传动流体,传动轴润滑剂,齿轮润滑剂,金属加2润滑剂,液压流体和其它润滑油,以及润滑脂组分,也能见到好处。
天然油包括动物油和植物油(如蓖麻油,猪油),液态石油润滑剂,用加氢精制,溶剂精或酸洗等方法加工过的石腊、石脑(及其混合物)。矿物润滑油。从煤或页岩得来的润滑粘度油在是合用的基油。
合成润滑油包括烃油和卤代烃油,诸如合的和共聚的烯烃(如聚丁烯,聚丙烯,丙烯-异丁烯共聚物,氯化聚丁烯,聚(1-己烯),聚(1-辛烯),聚(1-癸烯));烷基苯(如十二烷基苯,十四烷基苯,二壬基苯,二(2-乙基己基)苯;聚苯(如联苯,三联苯,烷基化多酚);烷基化联苯醚,烷基化联苯硫醚,以及它们的衍生物,同型物,同系物。
烯化氧聚合物和共聚物,以及它们的衍生物,其末端羟基己由酯化、醚化等反应进行了改性,它们组成另一类大家知道的合成润滑油。其例子有从环氧乙烷或环氧丙烷聚合制得的聚氧化烯聚合物,这些聚合物的烷基和芳基醚(如平均分子量为1000的聚异丙二醇甲醚,分子量为500-1000的聚乙二醇苯醚,分子量为1000~1500的聚丙二醇二乙醚);它们的单羧酸和多羧酸酯,如醋酸酯,C3-C8的混合脂肪酸酯,以及CB含氧酸的四甘醇二酯。
另一类合用的合成润滑油,包括二羧酸与各种醇生成的酯,所用酸如邻苯二甲酸,丁二酸,烷基丁二酸,链烯基丁二酸,马来酸,壬二酸,辛二酸,癸二酸,富马酸,己二酸,亚油酸二聚体,丙二酸,烷基丙二酸,链烯基丙二酸;所用醇如丁醇,己醇,十二烷醇,2-乙基己醇,乙二醇,二甘醇单醚,丙二醇。这些酯的具体例子有己二酸二丁酯,癸二酸二(2-乙基己酯),富马酸二-正己酯,癸二酸二辛酯,壬二酸二异辛酯,壬二酸二异癸酯,邻苯二甲酸二辛酯,邻苯二甲酸二癸酯,癸二酸二-二十烷基酯,亚油酸二聚体的双2-乙基己酯,该二聚体的混合酯,以及由1克分子癸二酸同2克分子四甘醇、2克分子2-乙基己酸反应得到的混合酯。
可以用作合成润滑油的酯,还包括由C5-C12的单羧酸同多元醇反应得到的酯,这些多元醇如新戊基二醇,三羟甲基丙烷,季戊四醇,双季戊四醇,以及三季戊四醇。
基于硅的润滑油,如聚烷基一,聚芳基一,聚氧氧基一,或聚芳氧基-硅烷油,以及硅酸酯油,组成了另一类有用的合成润滑剂;它们包括硅酸四乙酯,硅酸四异丙酯,硅酸四-(2-乙基己酯),硅酸四-(4-甲基-2-乙基己酯),硅酸四-(对-叔丁基苯基酯),六-(4-甲基-2-戊氧基)二硅氧烷,聚甲基硅氧烷,以及聚甲基苯基硅氧烷。其它合成润滑油包括含磷酸的液态酯(如磷酸三甲苯酯,磷酸三辛酯,癸基膦酸二乙酯),以及聚合的四氢呋喃。
未经精制的、精制的、再精制的油,都可用作本发明的润滑剂。未精制的油直接得自天然或合成来源,不需作另外的纯化处理。例如,由页岩干馏直接得到的页岩油,由蒸馏直接得到的石油润滑剂,或直接从酯化方法得到后不再作另外处理便使用的酯油,这些都属未精制油。而精制油除了另行经过一步或几步纯化处理,以改进其某种或若干性能以外,其余均同未精制油相似。油的纯化方法很多,诸如蒸馏,溶剂萃取,酸或碱萃取,过滤,渗透,它们都是专于此行者所熟悉的方法。再精制油的制取方法,同如今已经使用得到精制油的方法相类似。这种再精制油也被称作再生油或再加工油,它们常采用一些方法再作处理,以除去失去效能的添加剂和油的裂解产物。
本发明的润滑剂,通常含有适量可改善润滑性的某种或几种本发明组合物,即足以保证它具有改善了的去垢剂/分散剂和/或粘度指数性能。其正常使用量约为润滑组合物总重量的0.05%至大约20%,最好约为0.1~10%。该用量没有把溶剂/稀释剂介质计算在内。在润滑剂组成物于十分严酷的条件下使用时,如用于航海柴油发动机,本发明的金属盐用量,可高达润滑剂组合物总重量的约30%或以上。
本发明还打算与本发明的组合物结合,使用其它的添加剂。这些添加包括产生灰份和无灰份两种类型的去垢剂和分散剂,缓蚀剂,抗氧化剂,倾点下降剂,耐特压添加剂,抗磨添加剂,色泽稳定剂,以及消泡剂。
很多上述的耐特压添加剂和缓蚀剂、抗氧剂,也可用作抗磨剂。二烷基偶磷二硫羟酸锌是大家知道的一个例子。
倾点下降剂是一种特别有用的添加剂类型,它常常包括在这里所叙述的润滑油里。在油基的组合物里使用这种倾点下降剂可以改善它们的低温性能,这种方法在该技艺里颇为有名。其实例可参见由CV.Smalheer和R.Kennedy Smith所著的“润滑添加剂”第8页(美国Ohio州Cleveland,Lezius-Hiles出版公司,1967年出版)。
合用的倾点下降剂例子有聚甲基丙烯酸酯,聚丙烯酸酯,聚丙烯酰胺,卤代石蜡同芳香族化合物的缩合产物,羧酸乙烯酯聚合物,富马酸二烷酯的三聚物,脂肪酸的乙烯酯,以及烷基乙烯醚。美国专利2,387,501;2,015,748;2,655,479;1,815,022;2,191,498;2,666,746;2,721,877;2,721,878以及3,250,715,叙述了可供本发明用途的倾点下降剂的制备方法,以及它们的效用,在此作为参考。
消泡剂可用来减少或防止组合物形成稳定的泡沫。典型的消泡剂包括聚硅氧烷或有机聚合物。Henry T.Kerner所著的“泡沫控制剂”(No.yes Data出版公司1976年出版)第125~162页,谈到了其它的消泡剂组合物。
本发明的组合物可以直接加入燃料或润滑剂中。不过,它们最好选用基本惰性的普通液体有机稀释剂稀释,诸如矿物油,石脑油,苯,甲苯,或二甲苯,以形成添加剂提浓液。这些提浓液通常含有约10~80%重量的本发明组合物,以及20~90%重量的惰性稀释剂。提浓液还可含有某种或若干种本技艺里大家所知道的或上述的其它添加剂。
本发明的燃料组合物,其主要成分是一般的液体燃料,通常用的是烃类石油馏出液燃料,诸如由美国材料试验学会(ASTM)技术标准D396限定的柴油机燃料或燃料油,以及D439规定的马达汽油。非烃类物质,诸如醇,醚,有机硝基化合物等(如甲醇,乙醇,乙醚,甲乙醚,硝基甲烷),含这类非烃物的液体燃料组成,一般也在本发明范围之内。而由一种或几种烃类燃料用一种或几种非烃物质组成的混合物,这类液体燃料也可供考虑使用。混合燃料的例子有汽油同乙醇,柴油同乙醚的混合物。汽油是特别受到推荐的燃料,它是烃类的混合物,其ASTM馏程从10%馏出量的60℃左右到90%馏出量的205℃。
一般说来,含有适量本发明的燃料添加剂的燃料组成,能足以使它的某种或若干种性质得到改善,诸如防锈性,分散性等;通常,其用量按燃料组成体积计算,约为0.005~0.5%,又以约0.01~0.1%为宜。
除了本发明的燃料添加剂组成以外,燃料组成还可含有为专于此行者十分熟悉的其它添加剂。它们包括抗震剂如四烷基铅;铅清除剂,如卤代烷(如二氯乙烷,二溴乙烷);沉积预防剂或改良剂,如磷酸三芳酯,染料,十六烷值改进剂;抗氧剂,如2,6-二叔丁基-4-甲基苯酚;防锈剂,如烷基化丁二酸和酐;抑菌剂;胶质抑制剂,金属碱活剂,破乳剂;上部汽缸润滑剂;以及防冻剂。
本发明的燃料添加剂组合物,可以直接加入燃料,也可先用基本惰性的一般液体有机稀释剂稀释,诸如石脑油、苯、甲苯、二甲苯或上述的一般液体燃料,形成添加剂提浓。这些提浓液通常含有约20~90%重量的本发明组合物,还可含有一种或几种上述的或本技艺所熟知的其它常用添加剂。
本发明的燃料添加剂组合物,能以低于上述添加剂用量的提浓液形式提供使用,然后将它同本发明组合物的补加量和大家熟悉的其它添加剂一起,直接加入燃料;也可以在加入燃料之前,再用添加剂稀释,使添加剂用量达到所要求用量。
Claims (7)
1、一种制备润滑剂组合物分散剂的方法,它包括:在升温及(C)存在下使(A)和(B)反应,其中(A)为至少一种选自至少含35个碳原子的烃基取代的羧酸,
(B)为至少一种多胺,该多胺是由下述(1)和(2)衍生的,
(1)至少一种下式(Ⅱ)表示的化合物:
其中R为氢或烃基,Y代表S,N或O;A和X相互无关,分别代表亚烷基;n(取决于m和q)是0或1,q是0或1,m是2或3,
(2)至少一种下式(Ⅲ)表示的多胺,
其中各R是氢或烃基,R1是氢,烷基,或NHR″(NR″)y-其中各R″分别是C1-C10亚烷基,y是1-6之间的一个数,各Z分别是C1-C10亚烷基,C1-C10氧亚烷或至少含有一个氮原子的杂环,x是1-10之间的一个数,
(C)是一种酸催化剂。
2、按照权利要求1所述的方法,其中烃基取代的羧酸或其衍生物是至少一种聚亚烷基取代的琥珀酸或其衍生物,该聚亚烷基的特征在于Mn值为1300-5000,Mn/Mn值为1.5-4.0且其中至少一种多胺反应物是由选自甘油,三羟甲基丙烷,三羟甲基乙烷和三(羟甲基)氨基甲烷的羟烷基或羟芳基化合物和 选自三亚乙基四胺,二亚乙基三胺,四亚乙基五胺,五亚乙基六胺及其混合物的胺反应物衍生的。
3、按照权利要求2所述的方法,其中所述分散剂的总碱值为55-85。
4、按照权利要求1,2或3所述的方法,其中(B)是由三(羟甲基)氨基甲烷衍生的。
5、按照权利要求1所述的方法,其中多胺组合物在室温下是可倾倒的,所述多胺组合物于100℃的粘度至少高于反应物(B)的粘度100%。
6、按照权利要求5所述的方法,其中多胺组合物于100℃的粘度为50-200cst。
7、按照权利要求1所述的方法,其中酸催化剂是磷酸,有机膦酸,H3PO4的碱金属或碱土金属部分盐或亚磷酸三苯酯。
Priority Applications (23)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
IN178/DEL/86A IN172191B (zh) | 1985-03-14 | 1986-02-28 | |
CA000502964A CA1274526A (en) | 1985-03-14 | 1986-02-28 | High molecular weight nitrogen-containing condensates and fuels and lubricants containing same |
INDE017886 IN180407B (zh) | 1985-03-14 | 1986-02-28 | |
IL78032A IL78032A (en) | 1985-03-14 | 1986-03-04 | High molecular weight nitrogen-containing condensates and fuels and lubricants containing same |
AR86303312A AR242406A1 (es) | 1985-03-14 | 1986-03-07 | Poliamida de elevado peso molecular,un dispersante para composiciones lubricantes, procedimiento para su preparacion y del dispersante,composiciones y lubricantes y concentrados. |
AU55480/86A AU597248B2 (en) | 1985-03-14 | 1986-03-10 | High molecular weight nitrogen-containing condensates and fuels and lubricants containing same |
EP86902147A EP0215103B1 (en) | 1985-03-14 | 1986-03-10 | High molecular weight nitrogen-containing condensates and fuels and lubricants containing same |
PCT/US1986/000490 WO1986005501A1 (en) | 1985-03-14 | 1986-03-10 | High molecular weight nitrogen-containing condensates and fuels and lubricants containing same |
DE3650201T DE3650201T2 (de) | 1985-03-14 | 1986-03-10 | Hochmolekular stickstoffhaltige kondensate und diese enthaltender treibstoff und schmiermittel. |
BR8606545A BR8606545A (pt) | 1985-03-14 | 1986-03-10 | Processo para preparar uma poliamina e uma composicao poliamina de alto peso molecular,processo para preparar um dispersante basico,composicao de lubrificante,concentrado para formular composicoes lubrificantes e composicao combustivel |
AT86902147T ATE117002T1 (de) | 1985-03-14 | 1986-03-10 | Hochmolekular stickstoffhaltige kondensate und diese enthaltender treibstoff und schmiermittel. |
JP61501623A JP2542374B2 (ja) | 1985-03-14 | 1986-03-10 | 高分子量含窒素縮合物及びこれを含む燃料及び潤滑油 |
ES552862A ES8705498A1 (es) | 1985-03-14 | 1986-03-10 | Un procedimiento para la preparacion de una composicion de poliaminas de elevado peso molecular. |
ZA861874A ZA861874B (en) | 1985-03-14 | 1986-03-13 | High molecular weight nitrogen-containing condensates and fuels and lubricants containing same |
CN86102498A CN1020635C (zh) | 1985-03-14 | 1986-03-13 | 一种制备高分子量多胺组合物的方法 |
MX001855A MX174384B (es) | 1985-03-14 | 1986-03-13 | Condensados de alto peso molecular que contienen nitrogeno y los combustibles y lubricantes que los contienen |
NO86864512A NO168655C (no) | 1985-03-14 | 1986-11-12 | Polyamin, fremgangsmaate for fremstilling av et kondensasjonsprodukt inneholdene et slikt polyamin samt dets anvendelse i smoeremidler og brennstoffer |
DK542886A DK542886A (da) | 1985-03-14 | 1986-11-13 | Hoejmolekylaere nitrogenholdige kondensater og braendstoffer og smoeremidler, der indeholder saadanne kondensater |
FI864622A FI93467C (fi) | 1985-03-14 | 1986-11-13 | Suurimolekyylipainoisia, typpeä sisältäviä kondensaatiotuotteita sekä niitä sisältäviä poltto- ja voiteluaineita |
ES557200A ES8801686A1 (es) | 1985-03-14 | 1986-11-14 | Un procedimiento para la preparacion de composiciones de poliaminas de elevado peso molecular. |
CN94115107A CN1102668A (zh) | 1985-03-14 | 1994-09-10 | 制备润滑剂组合物分散剂的方法 |
JP6228407A JP2781730B2 (ja) | 1985-03-14 | 1994-09-22 | 潤滑油又は燃料組成物用分散剤 |
HK103795A HK103795A (en) | 1985-03-14 | 1995-06-29 | High molecular weight nitrogen-containing condensates and fuels and lubricants containing same |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US71179985A | 1985-03-14 | 1985-03-14 | |
CN94115107A CN1102668A (zh) | 1985-03-14 | 1994-09-10 | 制备润滑剂组合物分散剂的方法 |
Related Parent Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN92112541A Division CN1028874C (zh) | 1985-03-14 | 1992-10-31 | 润滑剂组合物及其制备方法和应用 |
Publications (1)
Publication Number | Publication Date |
---|---|
CN1102668A true CN1102668A (zh) | 1995-05-17 |
Family
ID=36930252
Family Applications (2)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN86102498A Expired - Fee Related CN1020635C (zh) | 1985-03-14 | 1986-03-13 | 一种制备高分子量多胺组合物的方法 |
CN94115107A Pending CN1102668A (zh) | 1985-03-14 | 1994-09-10 | 制备润滑剂组合物分散剂的方法 |
Family Applications Before (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN86102498A Expired - Fee Related CN1020635C (zh) | 1985-03-14 | 1986-03-13 | 一种制备高分子量多胺组合物的方法 |
Country Status (19)
Country | Link |
---|---|
EP (1) | EP0215103B1 (zh) |
JP (2) | JP2542374B2 (zh) |
CN (2) | CN1020635C (zh) |
AR (1) | AR242406A1 (zh) |
AT (1) | ATE117002T1 (zh) |
AU (1) | AU597248B2 (zh) |
BR (1) | BR8606545A (zh) |
CA (1) | CA1274526A (zh) |
DE (1) | DE3650201T2 (zh) |
DK (1) | DK542886A (zh) |
ES (2) | ES8705498A1 (zh) |
FI (1) | FI93467C (zh) |
HK (1) | HK103795A (zh) |
IL (1) | IL78032A (zh) |
IN (2) | IN172191B (zh) |
MX (1) | MX174384B (zh) |
NO (1) | NO168655C (zh) |
WO (1) | WO1986005501A1 (zh) |
ZA (1) | ZA861874B (zh) |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
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CN100577750C (zh) * | 2003-07-18 | 2010-01-06 | 鲁布里佐尔公司 | 组合物 |
CN103958567A (zh) * | 2011-11-25 | 2014-07-30 | 巴斯夫欧洲公司 | 烷氧基化聚亚烷基多胺 |
CN103958566A (zh) * | 2011-11-25 | 2014-07-30 | 巴斯夫欧洲公司 | 通过均相催化醇胺化提高聚亚烷基多胺的摩尔质量 |
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GB9421282D0 (en) * | 1994-10-21 | 1994-12-07 | Exxon Chemical Patents Inc | Additives and oleaginous compositions |
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-
1986
- 1986-02-28 IN IN178/DEL/86A patent/IN172191B/en unknown
- 1986-02-28 CA CA000502964A patent/CA1274526A/en not_active Expired - Lifetime
- 1986-02-28 IN INDE017886 patent/IN180407B/en unknown
- 1986-03-04 IL IL78032A patent/IL78032A/xx not_active IP Right Cessation
- 1986-03-07 AR AR86303312A patent/AR242406A1/es active
- 1986-03-10 ES ES552862A patent/ES8705498A1/es not_active Expired
- 1986-03-10 BR BR8606545A patent/BR8606545A/pt not_active IP Right Cessation
- 1986-03-10 WO PCT/US1986/000490 patent/WO1986005501A1/en active IP Right Grant
- 1986-03-10 EP EP86902147A patent/EP0215103B1/en not_active Expired - Lifetime
- 1986-03-10 AU AU55480/86A patent/AU597248B2/en not_active Ceased
- 1986-03-10 JP JP61501623A patent/JP2542374B2/ja not_active Expired - Fee Related
- 1986-03-10 DE DE3650201T patent/DE3650201T2/de not_active Expired - Lifetime
- 1986-03-10 AT AT86902147T patent/ATE117002T1/de not_active IP Right Cessation
- 1986-03-13 MX MX001855A patent/MX174384B/es unknown
- 1986-03-13 ZA ZA861874A patent/ZA861874B/xx unknown
- 1986-03-13 CN CN86102498A patent/CN1020635C/zh not_active Expired - Fee Related
- 1986-11-12 NO NO86864512A patent/NO168655C/no unknown
- 1986-11-13 DK DK542886A patent/DK542886A/da not_active Application Discontinuation
- 1986-11-13 FI FI864622A patent/FI93467C/fi not_active IP Right Cessation
- 1986-11-14 ES ES557200A patent/ES8801686A1/es not_active Expired
-
1994
- 1994-09-10 CN CN94115107A patent/CN1102668A/zh active Pending
- 1994-09-22 JP JP6228407A patent/JP2781730B2/ja not_active Expired - Fee Related
-
1995
- 1995-06-29 HK HK103795A patent/HK103795A/xx not_active IP Right Cessation
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN100577750C (zh) * | 2003-07-18 | 2010-01-06 | 鲁布里佐尔公司 | 组合物 |
CN103958567A (zh) * | 2011-11-25 | 2014-07-30 | 巴斯夫欧洲公司 | 烷氧基化聚亚烷基多胺 |
CN103958566A (zh) * | 2011-11-25 | 2014-07-30 | 巴斯夫欧洲公司 | 通过均相催化醇胺化提高聚亚烷基多胺的摩尔质量 |
CN103958567B (zh) * | 2011-11-25 | 2016-10-12 | 巴斯夫欧洲公司 | 烷氧基化聚亚烷基多胺 |
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