CN1020632C - 燃料产物 - Google Patents
燃料产物 Download PDFInfo
- Publication number
- CN1020632C CN1020632C CN86106817A CN86106817A CN1020632C CN 1020632 C CN1020632 C CN 1020632C CN 86106817 A CN86106817 A CN 86106817A CN 86106817 A CN86106817 A CN 86106817A CN 1020632 C CN1020632 C CN 1020632C
- Authority
- CN
- China
- Prior art keywords
- fuel
- acid
- composition
- hydrocarbon
- group
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Lifetime
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- C10L10/00—Use of additives to fuels or fires for particular purposes
- C10L10/08—Use of additives to fuels or fires for particular purposes for improving lubricity; for reducing wear
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- C10L1/00—Liquid carbonaceous fuels
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Abstract
本发明描述一种内燃机燃料组合物,特别是每加仑燃料含铅少于约0.5克的内燃机燃料组合物。在指定用含铅燃料开动的发动机中,该燃料提供容许的阀座保护。另一方面本发明是要减少汽缸内形成的沉积物。
Description
本发明是关于用于内燃机的燃料组合物,特别是关于被称为无铅或低铅燃料的燃料组合物。
为了减少空气污染,从汽油中除去铅添加剂,例如四乙基铅和四甲基铅时,人们发现燃料中的铅具有若干所需要的性能。例如,人们发现铅不仅作为抗爆剂,而且还能有效地防止阀座后退磨损。在
传统的内燃汽油发动机中,通常排气阀安装在阀座上使带有轻微的族转运动。操作期间,这种族转运动传给阀杆改变阀的相对位置,并且防止阀顶部的不规则磨损。旋转运动还使得阀在每次操作时处在不同的位置, 在从汽油中除去铅添加剂时,已经发现阀座磨损急剧增加,例如,参见“Unleaded versus Leaded Fuel Results in Laboratory Engine Tests”,E.J.Fuchs,The Lubrizol Corporation,presented at the Society of Automotive Engineers National West Coast Meeting,Vancouver,British Columbia,Canada,August16-19,1971(32页)。
阀座磨损与发动机的设计,负载及速度条件,以及阀的操作温度有关。阀座磨损在高速和高负载条件下最严重,对拖拉机,高速的小汽车,船内和船外发动机等,特别是当内燃机最初设计使用含铅燃料时,观察了阀座磨损的问题。
含铅燃料一般与少量的有机卤化物一起使用,来改善发动机性能。例如,参见美国专利4,430,092,1984年2月7日出版。在1985年6月4日出版的美国专利4,521,610中讨论了使用氨基甲酸酯化合物来控制内燃机中的沉积物。
在1977年12月6日授予Gautreaux的美国再版专利29,488中公开了环戊二烯基锰化合物,该专利提出了此锰化合物在含低量铅和无铅燃料中作为抗爆添加剂,其他有用的锰化合物可在1984年3月20日出版的美国专利4,437,436中找到,在1975年4月15日出版的美国专利4,131,626中描述了用于燃料的钴化合物,在1985年5月21日出版的美国专利4,518,395中描述了燃料中的铜化合物。
1956年9月25日出版的美国专利2,764,548描述了含有包括钠、钾、钙、钠、铵和胺盐在内的各种二壬基萘磺酸盐的马达油及发动机燃料。据报导这些盐是有效的防锈剂。
1970年4月14日,出版的美国专利3,506,416中描述了加铅汽油,其中包括溶于汽油的化学式为RC(O)NHOH的异羟肟酸盐,式中R是低于30个炭原子的羟基。金属可以从Ⅰa,Ⅱa,Ⅲa,Ⅴa,Ⅰb,Ⅱb,Ⅲb,Ⅳb,Ⅴb,Ⅵb,Ⅶb,Ⅷ族和锡中选择。
1965年5月4日出版的美国专利3,182,019中描述了含有络合物的润滑油和燃料油,其中的络合物含有胶状的碱金属或碱土金属的炭酸盐。
在1976年5月11日出版的美国专利3,955,938中建议在无铅汽油组合物中使用钠抑制阀座后退,钠可以几种不同形式结合到燃料中,如可溶的或者分散在汽油中的钠衍生物或有机化合物。例如可以使用简单的有机酸钠盐,象石油磺酸钠,尽管加入钠的形式以无机酸钠盐为优先,如以胶体形式分散在油中的炭酸钠。在美国专利3,955,938中描述的引进燃料中的钠的其它形式,包括各种磺酸钠盐,饱和的和不饱和的羧酸钠盐,硫化磷炭氢化合物的钠盐,例如可通过P2S5与石油馏分,如光亮油,苯酚和烷基苯酚的钠盐反应来制备。Graham专利描述的各种可选的添加剂包括抗腐蚀剂,防锈剂,抗爆化合物,抗氧化剂,溶剂油,抗静电剂,辛烷鉴定剂,例如乙酸叔丁酯,染料,防冻剂,例如异丙醇,乙二醇,无灰分散剂,洗涤剂等等。含在燃料中的钠添加剂的量是一规定量大约为0.5-20lbs的钠每1000桶汽油(2.86克/1000升是llb/1000bbl),最好为0.5-10lbs的钠。
还建议通过加入特定的洗涤剂和分散剂来改进汽油组合物。1969年5月13日出版的美国专利3,443,918描述了向汽油中添加二或三聚亚甲基聚胺的一,二,或三链烯基琥珀酰亚胺。据报导,当燃料用于内燃机时这些添加剂对形成沉积危害最小。
1965年3月9日出版的美国专利3,172,892 1966年11月23日公开的美国专利3,219,666,1966年11月23日公开的美国专利3,272,749,1966年10月25日公开的美国专利3,281,428,以及1969年5月13日公开的美国专利3,444,170的目标均为聚链烯基琥珀酰类无灰添加剂,并且美国专利指出了其中公开的添加剂作为燃料去垢剂使用。1967年10月17日公开的美国专利3,347,645也描述了使用链烯基琥珀酰亚胺作为汽油中的分散剂,但要注意该分散剂在贮存和海运期间保进含水乳胶的形成。1972年3月14日公开的美国专利3,649,229提出了一种含适量去垢剂的燃料,其中的去垢剂是使用链烯基琥珀酰化合物加上其他反应物制备的曼尼期碱,1980年12月23日公开的美国专利4,240,803
也涉及烃燃料组合物,它包含适量的专用链烯基琥珀酰亚胺,其中链烯基从C16-18烯烃混合物中获得。
尽管已提出有机酸钠盐在汽油中,特别是在低铅或无铅汽油中是有效添加剂,但这种钠盐具有一种使水乳化进入汽油中的能力,并且出现一种不需要的某些钠盐进入水中的钠提取过程。
使用碱金属或碱土金属盐,在有些情况下导致形成沉积,从而使燃烧汽缸绝热,导致辛烷需要量增加ORI。灼热的沉积物还可能引起预燃,从而引起爆画。通过分析人们已经发现,这些沉积物具有含炭金属性能,现在已经发现可以减少这些沉积物,并且如同这里所描述的,有效地增加了盐用于保护阀座的可用性。
在说明书和权利要求书中,除专门指出外,温度采用摄氏,百分数和比率以重量计,压力以千帕(KPa)计,引入的出版物列入参考文献中。
本发明叙述一种内燃机用无铅燃料组合物,其主要部分为液态烃燃料,并含少量如下组合物:
(a),一种烃可溶的含碱金属或碱土金属的组合物和
(b),一种铅清除剂
本发明另一方面叙述一种内燃机用燃料组合物,其主要部分为液态烃燃料,并含少量如下组合物:
(a),一种烃可溶的含碱金属或碱土金属的组合物和
(b),一种烃可溶的选自以下组分的组合物:含铝组合物,含硅组合物,含钼组合物,含锂组合物,含钙组合物,含镁组合物及其混合物。
本发明也叙述一种内燃机用燃料组合物,其主要数量为液态烃燃料,并含少量如下组合物:
(a),一种烃可溶的含碱金属或碱土金属的组合物和
(b),一种烃可溶的含过渡金属的组合物。
所制备的一种适用于燃料的浓缩物含有如下组分:
(a),一种烃可溶的碱金属或碱土金属盐;
(b),选自以下组分的组合物:
(1)铅清除剂
(2)一种烃可溶的选自以下组分的组合物:含铝组合物,含硅合物,含钼组合物,含锂组合物,含钙组合物,含镁组合物及其混合物;和
(3)一种烃可溶的含过渡金属的组合物及其混合物,和
(c),一种燃料可溶的或可分散的有机稀释剂。
在这里也叙述一种减少阀座后退的方法,通过含在无铅燃料中烃可溶的含碱金属或碱土金属的组合物,其数量足以减少阀座后退,以及足够数量的清除剂化合物,能减少燃烧汽缸内的碱金属或碱土金属沉积物的形成。
本发明叙述一种内燃机用燃料组合物,更具体的说是一种每升燃料中含少于约0.5克铅的燃料组合物。该燃料组合物主要含液态烃,并含少量性能改进的如下组合物:
(A),至少一种烃可溶的含碱金属或碱土金属的组合物,和
(B),至少一种烃可溶的无灰分散剂。
当把含金属的组合物(A)和无灰分散剂(B)的混合物加到每升燃料含少于约0.5克铅的汽油中时,该处理过的燃料稳定性有改进和呈现耐水性,并且当本发明的无铅或低铅燃料用于内燃机时,明显减少了阀座后退。本发明也叙述了在内燃机中用无铅或低铅燃料减少阀座后退的方法。
发明说明书
要用于本发明的燃料组合物的燃料通常是汽油沸点范围的液态烃燃料,包括以烃为主的燃料,可用于本发明的燃料组合物中并且有上面特征沸点的燃料,也用术语“石油馏分燃料”表示。但是并不是要把该术语限制到直馏馏分。馏分燃料可以是直馏馏分燃料,催化或热裂化的(包括加氢裂化的)馏分燃料,或直馏馏分燃料,石脑油等与裂化馏分油料的混合物。用于形成本发明的燃料组合物的基础燃料可按照已知的工业方法,例如酸或苛性碱处理,加氢、溶剂精制,白土处理等进行精制。
根据要使用的类型,要用许多不同等级的汽油。在本发明中所用的汽油包括那些指定作为车用或航空用的汽油。车用汽油包括那些符合ASTM标准D-439-73并且是由不同类型的烃类包括芳烃、烯烃、烷烃、异构烷烃,环烷烃及偶而也有二烯烃的混合物组成的汽油。车用汽油的沸程通常限制在约20℃~230℃,而航空汽油的沸程较窄,通常限制在约37℃~165℃。
含碱金属或碱土金属的组合物
本发明的燃料组合物将含少量(A)至少一种烃可溶的含碱金属或碱土金属的组合物。在本发明的燃料组合物中存在这样含金属的组合物就使得燃料组合物具有所要求的防止内燃机中阀座后退或把阀座后退减到最小的能力,特别是当燃料是无铅或低铅燃料时更是如此。
虽然碱金属是较好的,最好用碱金属钠,但金属的选择似乎不是特别关键的。
含金属钠的组合物(A)可以是碱金属或碱土金属的硫酸盐,羧酸盐,酚盐和磷酸盐。这些盐可以是中性的或是碱性的。前者含一定量的金属阳离子刚好足以中和存在于盐阴离子中的酸性基团,后者含过量的金属阳离子并常常称为超碱性盐。
这些碱性或中性盐可以是能油溶的有机含硫酸如磺酸,氨基磺酸,硫代磺酸,亚磺酸,次磺酸,偏酯磺酸,亚硫酸和硫代硫酸的盐。一般地它们是脂族或芳族磺酸盐。
这些磺酸包括单或多环芳族或环脂族化合物,这些磺酸大部分可用下面的式子表示:
R1(SO3H)r 式Ⅰ
(R2)xT(SO3H)y式Ⅱ
其中T是个芳环,例如苯,萘,蒽,菲,二苯并呋喃,噻蒽,吩噻噁,二亚苯基硫化物,吩噻嗪,苯醚,二苯硫,二苯胺,环己烷,石油萘,十氢萘,环戊烷等;R1和R2分别为脂肪基,R1至少含约15个碳原子,在R2和T中碳原子的总数至少经为15,r,x和y分别为1或大于1。
R1的具体的例子是由含油地蜡,饱和的和不饱和的石蜡和聚烯烃(包括聚合的C2,C3,C4,C5,C6等聚烯烃),含约15~7000或更多碳原子的烯烃衍生的基团。在上式中的T,R1和R2基团除了含有上面列举的那些基团,例如羟基,硫基,卤,硝基,氨基,亚硝基,硫化物,二硫化物等之外也,也可含有其他的无机或有机取代基。下标X一般是1-3,下标r+y一般为每个分子约1-4的平均值。
下面是上面Ⅰ和Ⅱ式范围之内的油溶磺酸的具体例子,而且要理解为这些例子也用来说明在本发明中这些磺酸的盐类是有用的。换句话说,对所列举的每种磺酸对它们相应的中性和碱性金属盐也是这样理解说明的。这些磺酸是石油磺酸;光亮的磺酸;由具有塞氏粘度在100°F(37.7°)约100秒至在210°F(99℃)的200秒的润滑油馏分衍生的磺酸,含油地蜡磺酸;单或多蜡取代的如苯,二苯胺,噻吩,2-氯萘等的磺酸和多磺酸;其他取代的磺酸如烷基苯磺酸(其烷基至少有8个碳原子),十六烷基酚单硫化物磺酸,联十六烷基噻蒽二磺酸,二月桂基β萘磺酸和烷芳基磺酸如十二烷基苯“塔底油料”磺酸。
后者是由苯用丙烯四聚物或异丁烯三聚物烷基化在苯环上引入1,2,3或更多个支链C12取代基的苯衍生的酸。十二烷基苯塔底油料主要是单和双十二烷基苯的混合物,可由制备家用洗涤剂作为副产品而得到。由在制备长链烷基磺酸盐(LAS)的过程中形成的烷基化塔底油料得到的类似产品在制备用于本发明的磺酸盐中也是有用的。
由制备洗涤剂的副产品与例如SO3反应生产磺酸盐是公知的技术,例如,见1969年John Wiley和Sons(纽约)出版的在Kirk-Othmer“化工技术百科全书”中的文章“磺酸盐”,第二版,19卷,第291页及其后页。
关于中性和碱性磺酸盐及它们的制备技术的其他描述可在下面的美国专利中找到:
2174110,2174506,2174508,2193824,
2197800,2202781,2212786,2213360,
2228598,2223676,2239974,2263312,
2276090,2276097,2315514,2319121,
2321022,2333568,2333788,2335259,
2337552,2347568,2366027,2374193,
2383319,3312618,3471403,3488284,3595790和3798012,其在此一并列出做为参考。也包括脂肪族磺酸,如石蜡磺酸,不饱和石蜡磺酸,羟基取代的石蜡磺酸,己丙烯磺酸,四戊烯磺酸,聚异丁烯磺酸(其中聚异丁烯含有20~7000或更多的碳原子),氯取代的石蜡磺酸,硝基石蜡磺酸等;环脂族磺酸如石油环烷磺酸,十六烷基环戊基磺酸,十二烷基环己基磺酸,双-(二-异丁基)环己基磺酸,单或多蜡取代的环己基磺酸等。
关于在这当中提到的磺酸或其盐及在后面的权利要求书中要用术语“石油磺酸”“或石油磺酸盐”,其包括所有由石油产品衍生的磺酸或其盐。一组特别有用的石油磺酸是由硫酸法制备石油白油做为副产品得到的石油磺酸(因为它们是微红棕色,所以
叫石油磺酸)。
可以由其制备本发明所用的合适的中性和碱性碱金属和碱土金属盐的羧酸包括脂肪族,环脂族和芳香族单和多元的羧酸如那些环烷酸,烷基或链烯基取代的环戊酸,相应的环己酸和相应的芳香酸。脂肪酸一般至少含8个碳原子,最好至少含12个碳原子。通常,它们的碳原子数不大于400。一般地,如果脂肪族碳链是支链,对于任何给定碳原子含量的酸都是较油溶的。环脂族和脂肪族羧酸可以是饱和的或不饱和的。具体的例子包括2-乙基己酸,2-亚麻酸,丙烯四聚物取代的马来酸,二十二烷酸,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,十四烷酸,二月桂基十氢萘羧酸,十八烷基八氢茚羧酸,十六烷酸,工业上可以得到的两种或多种羧酸的混合物如妥尔油酸,松香酸等等。
用于制备本发明的盐的一组较好的油溶的羧酸是油溶的芳香羧酸,这些酸可用下面的一般式表示:
(R*)aAr*(CXXH)m 式Ⅲ
基中R*是一个至少4个碳原子而不多于约400个脂族碳原子的脂肪烃基的基团,a是整数1~4,Ar*是一个多价的低于约14个碳原子的芳香烃环,每一个X分别是硫或氧原子,m是带有附加条件的整数1~4,其附加条件为R*和a应满足对由于式Ⅲ表示的每一个酸分子由R*基提供至少平均8个脂族碳原子。由变化的Ar*表示的芳香核的例子是由苯,萘,蒽,菲,茚,联苯等等衍生的多价芳香基。一般地,由Ar*表示的基团应是由苯或萘如亚苯基和萘衍生的多价环,例如甲基亚苯基,乙氧基亚苯基,硝基亚苯基,异丙基亚苯基,羟基亚苯基,巯基亚苯基,N,N-二乙基氨基亚苯基,氯亚苯基,二丙氧基萘,三乙基萘和其类似的三,四,五价核等等。
R*基通常是单纯的烃基,最好是烷基或链烯基这样的基因。但是,R*基可含小数取代基如苯基,环烷基(例如环己基,环戊基等)和非羟基如硝基,氨基,卤(例如:氯、溴等),低碳烷氧基,低碳烷基巯基,氧合取代基(即,=O),硫基(即,=S),断开基团如-NH-,-O-,-S-等等。使得R*基基本上保持烃特性。只要在R*基中存在的任何非碳原子总计不要超过R*基总重的约10%。就是本发明要求保持烃特性。
R*基的例子包括丁基,异丁基,戊基,辛基,壬基,十二烷基,二十二烷基,四十烷基,5-氯己基,4-乙氧基戊基,2-己烯基,环己基辛基,4-(对氯苯基)-辛基,2,3,5-三甲基庚基,2-乙基-5-甲基辛基,和由聚合的烯烃衍生的取代基,如聚氯丁烯,聚乙烯,聚丙烯,聚异丁烯,乙烯丙烯共聚物,氯化的烯烃聚合物,氧化的乙烯-丙烯共聚物等等。同样,Ar基可含非烃取代基,例如像如下的不同的取代基;低碳烷氧基,低碳烷基巯基,硝基,卤,少于4个碳原子的烷基或链烯基,羟基,巯基等等。
特别有用的羧酸基是下式的那些基因:
R* aAr*(CXXH)m(XH)p 式Ⅳ
其中,R*,X,Ar*,m和a的定义同式Ⅱ,P是整数1~4,通常是1或2。在该基团中,一种特别好的油溶类型的羧酸是下式的那些羧酸:
(R**)pha(COOH)6(OH)c 式Ⅴ
式中R**是一个含至少4~约400个碳原子的脂族烃基,Ph是苯基,a是整数1~3,b是1或2,c是0,1或2而最好是1,附加的条件是R**和a要满足在每个酸分子的脂肪烃取代基中至少含平均约十二个脂族碳原子。在这后类油溶的羧酸中,最有用的是其中每个脂肪族烃取代基含平均至少约十六个碳原子并且每个分子含1~3个取代基的脂肪烃取代的水杨酸。由这样的水杨酸制备的盐,其中脂肪烃取代基是由聚合的烯烃,特别是聚合的低碳1-单-烯烃如聚乙烯,聚丙烯,聚乙丁烯,乙烯/丙烯共聚物等等衍生的并且平均碳含量约30~400个碳原子。
相应于上面的式Ⅲ和Ⅳ的羧酸是公知的或可按现有技术的已知方法制备。由上述的式子所列举的羧酸和制备它们的中性和碱性金属盐的方法是已知的并已公开,例如在下面的美国专利中:
2197832,2197835,2252662,2252664,2714092,3410798,和3595791。
用于本发明的其他类型的中性和碱性羧酸盐是由下述一般式的链烯基琥珀酸衍生的那些盐:
R*CH(COOH)CH2COOH 式Ⅵ
其中R*的定义同上述的式Ⅲ。这些盐及其制备方
法在以下的美国专利中已公开:3271130,3567637和3632610。
具体地介绍上述磺酸,羧酸的碱性盐和任意其两种或多种的混合物的制备方法的其他专利包括美国专利2501731,2616904,2616905,2616906,2616911,2616924,2616925,2617049,2777874,3027325,3256186,3282835,3384585,3373108,3368396,3342733,3320162,3312618,3318809,3471403,3488284,3595790和3629109。
中性的和碱性的酚盐(一般叫酚盐)在本发明的组合物中也是有用的,并且是公知的技术。形成酚盐的那些酚有如下一般式:
(R*)a-(Ar*)-(OH)m 式Ⅶ
其中R*、a、Ar*和m跟上述式Ⅲ描述的意思相同并且较好。关于式Ⅲ所描述过的同样的例子也适用。
普通地可用的酚盐类是由下述一般式的酚制得的那些酚盐:
(R1)a(R4)zPh(OH) 式Ⅷ
其中a是整数1-3,b是1或2,z是0或1,Ph是苯基,或Ⅷ中的R1基本是饱和的平均有约30~400个脂肪碳原子的烃基取代基,R4选自低碳烷基,低碳烷氧基,硝基和卤基。
用于本发明的一种特殊类型的酚盐是碱性的(即过碱性的等)碱金属和碱土金属硫化的酚盐,其是通过用上述的硫化剂如硫,卤化硫或硫化物或氢硫盐硫化酚制得的。制备这些硫化的酚盐的技术在美国专利2680096,3036971和3775321中作了介绍。
其他有用的酚盐是由通过亚烷基(例如亚甲基)桥连在一起的酚制备的,它们是由单环或多环酚与醛或酮,典型地是在酸性或碱性催化剂存在下反应制备的,这些连接的酚盐及硫化的酚盐在美国专利3350038,特别是在其6~8栏中作了详细的叙述。
碱金属或碱土金属的磷酸盐在本发明的燃料组合物中也是有用的,例如:由无机磷试剂如P2S5与石油馏分如光亮油或由2~6碳原子的烯烃得到的聚烯烃反应制得的膦酸和/或硫代膦酸的正盐和碱性盐。聚烯烃的具体的例子是分子量为700~100000的聚丁烯。其他的与烯烃反应的含磷试及包括三氯化磷或三氯化硫氯化硫混合物。(例如美国专利3001981和2195517)亚磷酸盐和亚磷酰氯(例如美国专利3033890和2863834)和空气或氧与卤化磷(例如美国专利2939841)。
用在本发明的所述的磷酸和金属盐及由烯烃与硫化磷反应制备它们的其他专利包括下面的美国专利:2316078,2316079,2316080,2316081,2316082,2316085,2316088,2375315,2406575,2496508,2766206,2838484,2893959和2907713。上述专利中叙述的那些酸是作为油添加剂,在本发明的燃料组合物中是有用的。这些酸通过公知的反应可被转化为中性和碱性盐。在上文中叙述的有机含硫酸、羧酸、磷酸和酚的两种或多种中性和碱性盐的混合物可用在本发明的燃料组合物中。通常,这些中性和碱性盐将是钠、锂、镁、钙或钦盐,包括它们之中任意的两种或多种的混合物。如上所述,包括在燃料组合物中的含碱金属或碱土金属的组合物(A)的量要足以使得在燃料组合物中约含百万分之1~100的碱金属或碱土金属。当用在无铅或低铅燃料中时,在燃料中包括的含碱金属或碱土金属的组合物(A)的量要足以减少当燃料用在内燃机中时的阀座后退。
下面的具体用作说明的例子描述了用在本发明燃料组合物中的示范性的碱金属和碱土金属组合物(A)的制备情况。
实施例A-1
在637份矿物油中的1000份伯支链的一烷基苯磺酸钠(酸的分子量是522)混合物用145.7份50%的苛性钠溶液中和,并把过量的水和苛性钠除去,以这样的方法得到的含钠盐的产物含2.5%钠和3.8%硫。
实施例A-2
除了苛性钠用化学当量的Ca(OH)2代替之外,重覆实施例A-1的方法。
实施例A-3
除了苛性钠用化学当量的KOH代替之外,重覆实施例A-1的方法。
实施例A-4
906份烷基苯磺酸(具有平均分子量450,汽相渗透压测定),564份矿物油,600份甲苯,98.7份氧化镁和120份水的混合物,在78-85℃温度下,以每小时3立方英尺二氧化炭(85L/hr)的
速率吹7小时。整个碳酸饱和过程中不停地搅拌反应混合物。炭酸饱和作用后,汽提该反应混合物至105℃/20毫米汞柱(2.65千帕),并且过滤残液,滤液是具有金属比大约为3的所需高碱性磺酸镁的油溶液。
实施例A-5
制备323份矿物油,4.8份水,0.74份氯化钙,79份石灰,和128份甲醇组成的混合物,将其加热到50℃左右。向该混合物中混合添加具有平均分子量(汽相渗透压测定)为500的烷基苯基磺酸盐1000份,然后在50℃左右,以每小时约5.4lbs(40.8克/分)的速率用二氧化炭吹混合物2.5小时左右。炭酸饱和作用后,另添加102份油,混合物在55mm(7.3千帕)压力下,温度大约150-155℃时除去挥发物质。过滤残液,滤液是钙含量3.7%左右并且金属比大约为1.7的高碱性磺酸钙的所需油溶液。
清除剂
这里的第一种清除剂是能够从内燃机的汽缸内除去铅的物质。当然铅不是无铅燃料的一种组份,然而碱金属和碱金属盐酷似铅,能在电花插头和汽缸部分形成沉积物。该沉积物还含有大量与盐结合出现的含炭物质。在所要求组合物中,使用铅清除剂有减少沉积物形成的效果。
其次,本发明使用清除剂增强发动机内的燃烧。通过降低燃烧温度,使含炭沉积物燃烧脱离汽缸壁和电花插头。沉积物中无含炭物质时,盐类形成有机质的能力削弱。因此,由于燃烧炭,清除剂不给予盐附着能力,于是盐沿着排出路径从燃烧室排出。
清除剂的第三种形式是沉积物改良剂。在减少含炭沉积物或盐沉积物生长,或者减少沉积物附着在汽缸壁上,许多化合物是有效的。
这里第一类有效物质是铅清除剂,例如卤化烃。卤化烃可以是芳族或脂肪族,一般含有1至30个左右炭原子。卤化烃还可以包括其他部分,例如氧或硫,假如它们对主要的清除作用是无害的话。此外清除剂还有溶于烃的氨基甲酸酯和1,4叔二烷基苯。
卤化烃一般是短链烷基,每个清除剂分子至少含有两个卤素原子。卤素最好是氯,其次是溴。卤化烃混合物在这里也是有效的。提出的卤化烃包括1,2-二氯乙烷,1,2-二溴乙烷,三氯甲烷,三溴甲烷,二氯苯,三氯苯及其混合物。使用的1,2-二氯乙烷和1,2-二溴乙烷重量比分别为10∶1至1∶10,最好为7∶1至1∶7。另外的卤化物质包括三氯乙烯,1,1,2-三氯乙烷,四氯乙烯,1,1,2,2-四氯乙烷,五氯乙烷,六氯乙烷,1,2,4-三氯苯,1,2,4,5-四氯苯,五氯苯,三氯甲烷,三溴甲烷,四氯化炭及其混合物。
通常,卤化烃在阳离子与卤素当量比基础上与含碱金属或碱土金属的组合物一起使用,即对一摩尔钠,使用0.5摩尔1,2-二氯乙烷。对于钙盐,盐中每摩尔钙使用2/3摩尔三氯苯。
通常,阳离子与卤素的当量比可在2∶1至1∶15内变化,最好为3∶2至1∶7。
第二类清除剂(促进燃烧)是一般的过渡金属。任何一种以溶于烃形式存在的过渡金属可在这里使用。一般来说,过渡金属以羧酸盐,酚盐或磺酸盐形式存在,优选的过渡金属是锰、铈、铜、铁和钛,以锰为最佳,参见1985年3月19日公开的美国专利4,505,718。
使用的燃烧改良剂型清除剂的量,应足以减少汽缸内含炭沉积物的量。当含炭沉积物的性质随使用的燃料改变时,沉积物中碱金属和碱土金属的量通过燃料中存在的盐量来控制。因此当需要除去所有的含炭物质时,只需燃烧足够的量来阻止盐在汽缸中沉积成一层衬质。
通常,过渡金属在燃料中的浓度为5ppm至500ppm左右,最好为燃料的10ppm至300ppm左右。燃烧改良剂型清除剂具有另一优点,即不论盐是否存在于沉积物中,都能减少含炭沉积物。因而通过除去沉积物,辛烷必需量的增加减少。
第三类清除剂(沉积物改良型)能提高盐中金属的溶点。由于盐的熔点升高,盐在汽缸内保持结晶状,由于盐不能自由熔化,甚至不能在汽缸内流动,所以在汽缸壁上有少量粘滞物。盐的结晶性质使得沉积物分解,迫使离开汽缸。
这里使用的沉积物改良剂是铝、镁、钙、锂、硼、硅(一般来自聚硅氧烷型硅油)和钼的溶于烃的形式。如前所述,这里可以使用上述物质的任何一种熔于烃的形式。例如,这里可以使用1981年3月12日公开的美国专利4,266,945中获得的
钼化合物。硼化合物可以包括在1963年4月30日公开的美国专利3,087,936中描述的含分散剂的硼的形式。
这里使用的沉积物改良剂型清除剂的量要足以减少沉积物,或减少沉积物的再形成。一般来说,沉积物改良剂中的活性组分存在于组合物中,它与碱金属或碱土金属的当量比大约是20∶1至1∶5,最好是12∶1至1∶3左右。
还要强调的是,各种形式的清除剂可以混合使用。即需要用燃烧改良剂清洁堆积沉积物的发动机,或者在沉积物形成前使用有机卤化物络合盐的同时,除去沉积物。
溶于烃的无灰分散剂
本发明需要的燃料组合物还包含少量至少一种溶于烃的无灰分散剂。有效的无灰分散剂化合物一般其特征为,具有一个与高分子量的烃链连接的极性基团,该极性基团一般含有一个或多个氮、氧和磷元素。溶解的链其分子量一般比使用的金属类分子量高,但有时它们非常相似。
一般来说,本发明的燃料组合物中可使用任意一种已知的用于润滑油和燃料的无灰洗涤剂。
在本发明的一个实施例中,分散剂从含有下列基的基团中选择,
(Ⅰ)至少一个烃基取代胺,其中烃基取代物基本上是脂肪族的,并且含有至少8个炭原子。
(Ⅱ)至少一个酰化了的,具有至少10个脂肪族炭原子取代物的含氮化合物,它通过羧酸酰化剂与至少一个含有一个以上-NH-基的氨基化合物反应制的,上述酰化剂通过亚氨基,酰氨基,脒,或酰氧基铵交连与氨基化合物连接;
(Ⅲ)至少一个苯酚,醛,以及具有至少一个-NH-基团的氨基化合物的含氮缩合物;
(Ⅳ)至少一种取代羧酸的酯;
(Ⅴ)至少一种聚合分散剂;
(Ⅵ)至少一种烃取代的酚分散剂;
(Ⅶ)至少一种燃料溶于醇,酚或胺的烷氧基化衍生物。
烃基取代胺
本发明的燃料组合物中的烃基取代胺对于本领域内熟练的技术人员来说是已知的,并且几篇专利介绍了它们,这些专利是:美国专利3,275,554 3,438,757 3,454,555 3,565,864 3,755,433和3,822,209。这些专利公开了用于本发明的合适的烃基胺,它括它们的制备方法。
一般的烃基胺具有通式:
[AXN]x[-N([-UN]a[-UQ]b)]yR2c+
H1+2y+ay-c式Ⅸ
其中A是氢,从1到10左右炭原子的烃基基团,或从1到10炭原子的羟基烃基基团;X是氢,从1到10炭原子的烃基基团。或从1到10炭原子的羟基烃基基团,并且A和N可一起形成一个5至6节的环,直到12个炭原子;U是2到10个炭原子的烯基,这里不言而喻,需要任何能提供三价氮原子的烃;R2是从30到400个炭原子的脂肪族烃;Q是哌嗪结构;a是从0到10之间的整数;b是从0到1之间的整数;a+2b是从1至10之间的整数;c是从1到5之间的整数;并且是1到4范围内的平均值,等于或低于分子中氮原子数;X是从0到1之间的整数;Y是从0到1之间的整数;X+Y等于1。
在说明这个化学式时,需要知道R2和H原子是连接到通式的方括号内不饱和的氮原子价上。因此该分子式包括辅属的分子式,其中R连接到末端氮原子上和同分异构的辅属分子式,R接到非末端氮原子上。不与R2连接的氮原子可以提供一个氢原子或一个AXN取代基。
本发明中和上述分子式包括的有效烃基胺含有单胺,其通式为:
AXNR2式Ⅹ
对这种单胺作如下说明:
聚(丙烯)胺
N,N-二甲基-正-聚(乙烯/丙烯)胺
(50∶50摩尔比单体)
聚(异丁烯)胺
N,N-二(羟基乙基)-N-聚(异丁烯)胺
聚(异丁烯/1-丁烯/2-丁烯)胺
(50∶25∶25摩尔比单体)
N-(2-羟基乙基)-N-聚(异丁烯)胺
N-(2-羟基丙基)-N-聚(异丁烯)胺
N-聚(1-丁烯)-苯胺
N-聚(异丁烯)-吗啉
如上所列通式Ⅸ包括的烃基胺是聚胺,其通式为:
-N-([-UN-]a[-UQ]b)R2 c
H1+2y+ay-c式Ⅺ
对这种聚胺的说明如下:
N-聚(异丁烯)乙烯二胺
N-聚(丙烯)三亚甲基二胺
N-聚(1-丁烯)二乙烯基三胺
N′,N′-聚(异丁烯)四乙烯五胺
N,N-二甲基-N′-聚(丙烯),1,3-丙烯二胺
本发明燃料组合物中有效的羟基取代胺包括一些在上面通式Ⅸ中不包括的N-氨基吗啉。这些烃基取代的氨基烃基吗啉其通式为:
R2N(A)UM 式Ⅻ
其中R2是大约从30到400个炭的脂肪族烃基,A是氢,从1到10个炭原子的烃基或从1到10个炭原子的羟基烃基基团,U是从2到10个炭原子的烯基,M是吗淋结构。这些烃基取代的氨基烃基吗啉以及分子式Ⅹ描述的聚胺,在一般的烃基取代胺中用于制备本发明的化合物。
酰化的含氮化合物
一些酰化的,具有至少10个脂肪族炭原子取代基的含氮化合物,该含氮化合物是通过羧酸酰化剂与氨基化合物反应获得的,对于本领域的技术人员来说是已知的。在这些组合物中,酰化剂通过亚氨基,酰氨基,脒,或酰氧基铵与氨基化合物连接。10个脂肪族原子的取代基可以是在分子中羧酸酰化剂衍生部分,或在分子中氨基化合物衍生部分,然而最好是在酰化剂部分,酰化剂可以从甲酸及其酰化衍生物到具有高分子量的直到5000,10000,或20,000个炭原子的脂肪族取代基有酰化剂之间变化,氨基化合物可以从氨本身到具有30左右炭原子脂肪族取代基的胺之间改变。
本发明的组合物中,一般有效的酰化氨基化合物通过具有至少10个炭原子脂肪族取代基的酰化剂与至少存在一个-NH-基团的氮化合物反应制得。通常,酰化剂是单或多羧酸(或反应等同物)。例如取代的琥珀酸或丙酸以及氨基化合物可以是聚胺或聚胺的混合物,最典型的是乙烯聚胺混合物。胺还可以是羟基烷基取代的聚胺。这些酰化剂中的脂肪族取代基最好平均有至少约30或50,直到400个左右炭原子。
含有至少10个炭原子的以烃为主的基团是正癸基,正-十二烷基,叔丙基,正-十八烷基,油基,氯十八烷基,三-icontanyl等等。一般来说,以烃为主的取代基从单烯烃和二烯烃的均聚物或共聚物(例如,共聚物,三元共聚物)获得,其中的一或二烯烃具有2到10个炭原子,例如乙烯、丙烯、丁烯-1、异丁烯、丁二烯、异戊二烯,1-己烯,1-辛烯等等,通常这些烯烃是1-单烯烃。取代基还可以从这些均聚物或共聚物的卤化(例如氯化或溴化)类似物得到。然而取代基还可以从其他来源获得,例如单体的高分子量烯烃(例如,1-四-contene)和它们的氯化类似物以及其氢氯化类似物,脂肪族石油馏分,特别是石脂和裂解及氯化类似物,以及它们的氢氯化类似物,白油,象通过Ziegler-Natte过程(例如,聚(乙烯)润滑脂)制备的合成烯烃,以及对于本领域已知的方法通过氯化可以减少或排除取代基中的不饱和现象。
在本说明书及其权利要求中使用的术语“以烃为主的”表示一个基团,该基团有一炭原子与分子余留部分直接相连,并在整个发明内主要具有烃性质。因此,以烃为主的基团每十个炭原子可以含有一个无烃基团,假如这种非烃基团基本上不改变基团主要的烃特性。本领域的技术人员已知的这些基团有,例如包括羟基,卤素(尤其是氯和氟),烷氧基,烷基硫基,烷基次硫酸基等等。然而通常以烃为主的取代基是纯烃基,并且不含这种非烃基。
以烃为主的取代基基本上是饱和的,也就是说,对于每10个炭-炭单键含有不超过一个炭-炭不饱和键。通常,每50个炭-炭键含有不超过一个炭-炭非芳族不饱和键。
以烃为主的取代基性质上基本是脂肪族的,也就是说,取代基中每10个炭原子含有不超过一个六个或更少炭原子的非脂肪族单体(环烷基,环烯基或芳族的)基团。然而通常对每50个炭原子,取代基含有不超过一个这种非脂肪族基团,并且在许多情形,它们根本不含这种非脂肪族基团,也就是说,一般的取代基纯是脂肪族的。一般说来,这些纯脂肪族取代基是烷基或烯基基团。
含有平均数30个以上的碳原子的基本饱和的以烃为主的取代基举例如下:
大约35到70个炭原子的聚(乙烯/丙烯)基团的混合物。
大约35至70个炭原子的氧化或机械降解的
聚(乙烯/丙烯)基团的混合物
大约80至150个炭原子的聚(丙烯/1-己烯)基团的混合物
具有平均数50至75个炭原子的聚(异丁烯)基团的混合物
取代基的优先来源是在路易斯酸催化剂,如三氯化铝或三氟化硼存在下,通过聚合含35-75重量-%丁烯和30-60重量-%异丁烯的C4精制流获得的聚-(异丁烯)。
这些聚丁烯主要含有(大于80%的总重复单元)异丁烯构型重复单元;
-C(CH2)2CH2-
在制造这些酰化化合物中有效的氨基化合物举例如下:
(1)聚亚烷基聚胺,其通式为:
(R3)2N[U-N(R3)]nR3式Ⅷ
其中每个R3可以任意为氢原子,烃基基团或含有大约直到30个炭原子的羟基取代烃基基团,但须至少有一个R3是氢原子,n是1至10之间所有的数,u是一个C1-18烯基;(2)包括羟基烷基取代聚胺的杂环取代聚胺,其中聚胺如上描述,杂环取代基例如,哌嗪,咪唑啉,嘧啶,吗啉等等,以及(3)芳族聚胺,其通式为:
Ar(NR3 2)y 式ⅩⅣ
其中Ar是6到20个左右炭原子的芳核,每个R3如上定义,Y是2至8左右。聚亚烷基聚胺(1)的具体例子是乙烯二胺,四(乙烯)五胺,三-(三亚甲基)四胺,1,2-丙烯二胺等等。羟基烷基取代聚胺的具体例子含有N-(2-羟基乙基)乙烯二胺,N,N′-双-(2-羟基乙基)乙烯二胺,N-(3-羟基丁基)四亚甲基二胺等等。杂环取代聚胺(2)的具体例子是;N-2-氨基乙基哌嗪,N-2和N-3氨基丙基吗啉,N-3(二甲基氨基)丙基哌嗪,2-庚基-3-(2-氨基丙基)咪唑啉,1,4-双(2-氨基乙基)哌嗪,1-(2-羟基乙基)哌嗪,以及2-十七烷基-1-(2-羟基乙基)-咪唑啉等等。芳族聚胺(3)的具体例子是各种同分异构的亚苯基二胺,各种同分异构的萘二胺等等。
许多专利介绍了有效的酰化氮化合物,这些专利包括美国专利3,172,892 3,219,666 3,272,746 3,310,492 3,341,542 3,444,170 3,455,831 3,455,832 3,576,743 3,630,904 3,632,511 3,804,763和4,234,435。一般这类酰化含氮化合物是通过聚(异丁烯)-取代的琥珀酐酰化剂(例如,酐,酸,酯等等),其中聚(异丁烯)取代基具有大约50到100个炭原子,与每个乙烯聚胺具有3到7个左右的氨基氮原子的乙烯聚胺和大约1至6个乙烯氯化物的混合物反应得到。由于这种酰化氨基化合物的广泛公开,在这里不必对它们的性质和制备方法进一步讨论。上面提到的美国专利公开了酰化氨基化合物及它们的制备方法。
另一种属于这类的酰化氮化合物是通过以前描述的烯烃胺与以前描述的取代琥珀酸或酐以及具有2至22个炭原子的脂族单羧酸反应制得的。在这些形式的酰化氮化合物中,琥珀酸与单一羧酸的摩尔比是在1∶0.1至1∶1的范围。一般的单一羧酸是甲酸,乙酸,十二烷酸,丁酸,油酸,硬脂酸,称为异硬脂酸的硬脂酸同分异构体的工业混合物,甲苯酸等等。在美国专利3,216,936和3,250,715中充分描述了这些物质。
在制造本发明燃料中另一种有效的酰化氮化合物是大约20-30个炭原子的脂肪单羧酸与前描述的烯烃胺反应的产物。这些烯烃胺一般是乙烯,丙烯或含有2-8个氨基基团的三亚甲基聚胺及其混合物。脂族单羧酸一般是含有12-30个炭原子的直链或支链脂肪羧酸的混合物。广泛使用的酰化氮化合物是通过以前描述的烯烃聚胺与具有5至30左右摩尔百分数直链酸的脂肪酸和大约70至95左右摩尔百分数支链脂肪酸的混合物反应获得。能买到的混合物,在贸易中作为异硬脂酸广为人知。这些混合物是作为副产品从美国专利2,812,342和3,260,671中描述的不饱和脂肪酸的二聚化作用制得。
支链脂肪酸还包括那些支链性质上不是烷基的脂肪酸,例如苯基和环己基硬脂酸和氯硬脂酸。支链脂肪族羧酸/亚烷基聚胺产物已在本领域内广泛地被描述过,参见例子,美国专利,3,110,673 3,251,853 3,326,801 3,337,459 3,405,064 3,429,674 3,468,693 3,857,791。这些专利用于公开脂肪酸/聚胺缩合物在润滑油配制中的应用。
苯酚,醛,和氨基化合物的含氮缩合物本发明燃料组合物中的有效分散剂苯酚/醛/
氨基化合物的缩合物包括通常称为曼尼期的缩合物。一般可通过至少一种活性氢化合物与至少一种醛或产生醛的物质(一般是甲醛母体),以及至少一个氨基或至少含一个=NH基团的聚氨基化合物同时或连续反应来获得,其中的活性氢化合物例如烃取代的苯酚(例如,烷基苯酚,其中烷基至少有平均数大约为12至400个炭原子,最好是30至400个左右炭原子),具有至少一个与芳炭键合的氢原子。氨基化合物包括伯胺或仲胺,它们具有1至30个炭原子的烃基或1至30个左右灰原子的羟基取代的烃取代基。另一种典型的氨基化合物是聚胺,在讨论酰化的含氮化合物期间已作过介绍。
典型的单胺包括甲基乙基胺,甲基十八烷基胺,苯胺,二乙基胺,二乙醇胺,二丙其胺等等。下列美国专利包括用于制造本发明的组合物中的广泛公开的曼尼期缩合物:
美国专利
2,459,112 3,413,347
2,962,442 3,442,808 3,558,743 2,984,550
3,448,047 3,586,629 3,036,003 3,454,497
3,591,598 3,166,516 3,459,661 3,600,372
3,236,770 3,461,172 3,634,515 3,355,270
3,493,520 3,649,229 3,368,972 3,539,633
3,697,574
从含硫反应物得到的缩合物还可用于本发明的燃料组合物中。在美国专利3,368,9,72,3,649,229,3,600,372,3,649,659和3,741,896中对这种含硫缩合物作了描述。这些专利还公开了含硫曼尼期缩合物。通常在制造本发明的组合物中使用的缩合物是从带有大约6至400个炭原子,特别是30至250个左右炭原子烷基取代基的苯酚制得。这些典型的缩合物是从甲醛或C2-7脂族醛,以及用于制造(B)(ⅱ)描述的酰化的含氮化合物的氨基化合物来制得。
这些优先的缩合物是通过大约1摩尔苯酚化合物与大约1至2摩尔醛以及大约1至5当量氨基化合物(氨基化合物的当量是其分子量除以存在的=NH基团数)反应制得的。缩合物进行反应的条件通过上述提到的专利已为本领域的技术人员所知。因此,这些专利由于公开了反应条件也列入参考文献。
用于本发明燃料的特别优先的含氮缩合物产物通过1974年3月15日公开的,现已放弃的美国流水号451,644中公开的2步方法制得。简言之,这些含氮缩合物是通过(1)至少一个羟基芳族化合物与低脂族C1-7醛或其可逆聚合物,在碱试剂,例如碱金属的氢氧化物存在下,温度为直到150℃左右时反应制得,其中的羟基芳族化合物含一个具有至少30个炭原子和直到大约400个炭原子的脂肪族为主的取代基或环脂族为主的取代基;(2)中和的中间产物与至少一种化合物反应,这种化合物含有一个具有至少一个-NH-基团的氨基基团。
特别是,这些2步缩合物是从(a)带有含大约30至250个炭原子烃基取代基的苯酚,上述取代基来源于丙烯,1-丁烯,2-丁烯,或异丁烯的聚合物,以及(b)甲醛,或其可逆聚合物,(例如三噁烷多聚甲醛)或其作用等同物(例如,羧甲基),以及(c)烯烃聚胺,例如具有2到10个氮原子之间的乙烯聚胺来获得。在上提到的美国流水号451,644中可以找到这些优选缩合物的进一步细节,由于它公开了2步缩合物,故在这里列入参考文献中。
取代羧酸酯
在本发明中,用作洗涤剂/分散剂的酯是取代羧酸的衍生物,其中取代物实际上是脂肪族物质,至少含有约30(最好是约50到750个脂肪族原子的饱和烃基类。在此所说的术语“烃基类”是表示这样的一类:即其一炭原子直接连接到分子的其他部分,并且在本发明中具有突出的烃类特性。这样的类包括如下几种:1)烃类:即脂肪族类,芳香族和脂环族取代的脂肪族类等等,这些类别是本专业领域技术人员所已知的。
2)取代烃类:即含有非烃取代物的类,该取代物在本发明中改变该类主要的烃类特性。那些本专业领域技术人员知道相应的取代物:例如,卤族,硝基,羟基,烷氧基,烷酯基和烷硫基。
3)杂类:即在本发明的范围内当其主要是烃特征时,该类所含的原子不同于链或环上的炭,而该链或环是由炭原子构成的。适合的杂原子对那些本专业领域的技术人员来说是清楚的,例如,它包括氮,氧,硫。
通常,在此烃基类中,每10个炭原子存在的取代物或杂原子不多于3个,最好不多于1个。
已取代的羧酸(和它的衍生物包括酯,胺和酰亚胺)一般是用不饱和酸或它的衍生物如酐、酯、胺或酰亚胺与所需要的烃基类的原料进行烷基化反应来制备。适合的不饱和酸和它的衍生物包括丙烯酸,异丁烯酸,顺丁烯二酸,顺丁烯二酸酐,反式丁烯二酸,亚甲基丁二酸,亚甲基丁二酸酐,甲基顺丁烯二酸,甲基顺丁烯二酸酐,甲基反丁烯二酸,戊烯二酸,(E)-氯代丁烯二酸,丙烯二甲酸,丁烯酸,甲基丁烯酸,2,4-己二烯酸,3-己烯酸,10-壬烯二酸和2-戊烯-1,3,5-三羧酸。特别适合的有不饱和二羧酸和它们的衍生物,尤其是顺丁烯二酸,反式丁烯二酸和顺式丁烯二酸酐。
适合的烷基化剂包括可聚烯烃单体的均聚物和共聚物,和它们的含有极性取代物的衍生物,该可聚烯烃单体含有2到10个,一般包含2到6个炭原子。该聚合物事实上是饱和的(如,它们含有不大于约5%的烯烃键)并且是脂肪族的(如,它们含有至少80%,最好至少95%,按从脂肪族单烯烃得到的单元重量计算)。用于生产该聚合物的单体有:乙烯,丙烯,1-丁烯,2-丁烯,异丁烯,1-辛烯和1-癸烯。一些不饱和单元可有下列烯烃生成:共轭二烯烃如,1,3-丁二烯和异戊二烯;非共轭二烯烃如,1,4-己二烯,1,4-环己二烯,5-亚乙基-2-降冰片烯和1,6-辛二烯,三烯如,1-异亚丙基-3a,4,7a-四氢茚,1-异亚丙基-二环戊二烯和2-(2-亚甲基-4-甲基-3-戊烯基)[2,2,1]二环-5-庚烯。
最优先选用的聚合物类是那些含有端烯烃的,如丙烯,1-丁烯,异丁烯和1-己烯。在该类中尤其可取的是主要含有异丁烯的聚丁烯。其次优先选用的聚合物类是乙烯的三元共聚物,C3-8α-单烯烃和选自含有非共轭二烯烃(它是特别优先选用的)和三烯烃的聚烯。这些作为例子的三元共聚物是由E.I dupont de Nemours & Company制备的“ortholeum2052”。这些三元共聚物含有约48%(摩尔)的乙烯类,48%(摩尔)丙烯类和4%(摩尔)1,4-己二烯类,并且具有比浓对数粘度1.35(在30℃温度下,10毫升四氯化炭中含8.2克聚合物)。
取代羧酸和其衍生物的制备方法在现有技术中是已知的,不需要详细说明。参考文献已给出,例如,美国专利3,272,746 3,522,179和4,234,435在此已列入参考文献中。聚合物与不饱和酸或其衍生物的摩尔比可以等于,大于或小于1,取决于所需产品的类型。
酯是上述那些含有羟基化合物的琥珀酸,该羟基化合物可以是脂肪族化合物,如一羟基和多羟基醇,或芳香族化合物如苯酚和萘酚。芳香族羟基化合物,由该化合物可以制得本发明的酯,可用下面的具体实施说明:酚,β-萘酚,α-萘酚,甲酚,间苯二酚,邻苯二酚,P,P′二羟基二苯基,二-氯酚,2,4-二丁基酚,丙烯四聚物取代酚,双十二烷基酚,4,4′-亚甲基双酚,α-癸基-β-萘酚,聚异丁烯(分子量为1000)-取代酚,含有0.5摩尔甲醛的庚基酚缩合产品,带有丙酮的辛基酚缩合产物,二(羟基苯基)氧化物,二(羟基苯基)硫化物,二(羟基苯基)二硫化物,和4-环己酚。较佳的是酚和烷基化酚,该酚具有直至3个烷基取代基,每个烷基取代基可含有100或更多的炭原子。
醇,由它可以生产酯,最好是含有直至约40个脂肪族炭原子。它们可以是一羟基醇,如甲醇,乙醇,异辛醇,十二醇,环己醇,环戊醇,二十二醇,三十六醇,新戊醇,己丁醇,苄醇,β-苯基乙醇,2-甲基环己醇,β-氯乙醇,乙二醇的一甲基醚,乙二醇的-丁基醚,二乙二醇的-丙基醚,三乙二醇的单十二烷基醚,乙二醇的单油酸酯,二乙二醇的单硬脂酸酯,仲戊醇,叔丁醇,5-溴十二醇,硝基十八醇和甘油的二油酸酯。多羟基醇最好含有2到约10个羟基。如下面列举的化合物:乙二醇,二乙二醇,三乙二醇,四乙二醇,二丙二醇,三丙二醇,二丁二醇,三丁二醇和其他的烷二醇,其中亚烷基含有2到约8个炭原子。其他有用的多羟基醇包括:甘油,甘油的单油酸酯,甘油的一硬脂酸,甘油的一甲基醚,季戊四醇,9,10-二羟基硬脂酸,9,10-二羟基硬脂酸的甲基酯,1,2-丁二醇,2,3-己二醇,2,4-己二醇,Penacel,1,2,3,4-丁四醇,阿糖醇,山梨醇,甘露糖醇,1,2-环己二醇,二甲苯乙二醇。炭水化合物如:糖淀粉,纤维素等等可以生产本发明的酯。炭水化合物还可列举如下:葡萄糖,果糖,蔗糖,鼠李糖,甘露糖,甘油醛和半
乳糖。
特别优选的多羟基醇类是那些含有至少三个羟基的醇,其中有些醇已经与含有约8到约30个炭原子的一元羧酸进行了酯化反应,如:辛酸,油酸,硬脂酸,亚油酸,十二烷酸,或妥尔油酸。这样部分酯化的多羟基醇的例子有山梨醇的单油酸酯,山梨醇的二硬脂酸酯,甘油的单油酸酯,甘油的单硬脂酸酯,1,2,3,4-丁四醇的二-十二酸酯。
酯也可由不饱和醇生成,如:烯丙醇,肉桂醇,炔丙醇,1-环己烯-3-醇,油醇。还有另外的一些醇也可以生成本发明的酯,这些醇包括醚醇和氨基醇,该醚醇和氨基醇包括氧化烯-,氧化芳-,氨基-烃基-,和氨基-亚芳基-取代的醇,该醇含有一个或多个氧化烯,氨基-亚烃基或氨基-亚芳基氧化芳基。这些化合物的例子如下:山梨醇,苯氧基乙醇,庚基苯基-(氧化丙类)6-H,辛基-(氧乙烯)30-H,芳基-(氧化辛烯)2-H,单(庚基苯基-氧化丙烯)30-H,芳基-(氧化辛烯)2-H,单(庚基苯基-氧化丙烯)取代的甘油,多(氧化苯乙烯),氨基乙醇,3-氨基乙基戊醇,二(羟基乙基)胺,对-氨基酚,三(羟基丙基)胺,N-羟基乙基乙撑二胺,N,N,N′N′-四羟基-三亚甲基二胺等等。对大部分来说,较佳的是具有直至约150个氧化烯基的醚醇,其中亚烃基含有1到约8个炭原子。
酯可以是琥珀酸的二酯或酸性酯,即:部分酯化的多羟基醇或酚,即:含有游离醇或酚的羟基酯。上述酯的混合物同样可以考虑包括在本发明的范围之内。
酯可由多种方法中的任一个来制备,方法是较佳的,因为它是方便的,并且常带来了酯的优良特性,该方法包括适当的醇或酚与一实质上是烃取代的琥珀酸酐反应。酯化反应通常在高于约100℃的温度下,最好在150℃到300℃温度下进行。
作为副产品生成的水可在酯化反应进行时通过蒸馏除去。在酯化反应中,可使用一种溶剂以便于混合和控制温度。也容易从反应混合物中除去水。有效的溶剂包括二甲苯,甲苯,二甲基醚,氯苯和矿物油。
上述方法的改进包括用相应的琥珀酸代替被取代的琥珀酸酐。但是,琥珀酸在温度高于约100℃时,容易发生脱水反应,并因此转化成它们的酸酐,然后这些酸酐与醇反应物进行酯化反应。在这方面,琥珀酸在本过程中似乎是与它们的酸酐大体上等效。
琥珀反应物与所用的羟基反应物的相对比例大多是取决于所需产品的类型和存在于羟基反应物分子中的羟基数。例如琥珀酸半酯的形成,即两个酸基中只有1个被酯化,每摩尔已取代的琥珀酸反应物就需要1摩尔单羟基醇,反之,要生成琥珀酸的二酯,则每摩尔的酸就需2摩尔的醇。另一方面,1摩尔六羟基醇可与同样多的6摩尔琥珀酸化合生成酯,在生成的酯中,六羟基醇中的每个羟基与琥珀酸的二酸基中的一个发生酯化反应。这样所用的琥珀酸与多羟基醇的最大比例可由存在于羟基反应物分子中的羟基数来确定。为了本发明的应用发现琥珀酸反应物与羟基反应物等摩尔量反应所得到的酯具有优良的特性,因此是较佳的。
在某些情况,在催化剂存在下,进行酯化反应是有利的,如硫酸,吡啶氢氯化物,氢氯酸,苯磺酸,对-甲苯磺酸,磷酸或一些其它已知的酯化反应催化剂。反应中催化剂的量可以仅为0.01%(按反应混合物的重量计算),通常为约0.1%到约0.5%。
本发明的酯也可通过已取代的琥珀酸或酸酐与环氧化物或环氧化物与水的混合物反应而得到。这个反应类似于酸或酐与乙二醇的反应。例如,产品可通过已取代的琥珀酸与一摩尔的环氧乙烷反应来制备。同样地,产品可通过已取代的琥珀酸与2摩尔的环氧乙烷反应来制备。通常,可用于这种反应的其它环氧化物有:例如,1,2-环氧丙烷,氧化苯乙烯,氧化1,2-丁烯,氧化2,3-丁烯,氯甲代氧丙环,氧化环己烯,氧化1,2-辛烯,环氧化的大豆油,9,10-桥氧-硬脂酸的甲基酯和丁二烯单环氧化物。环氧化物多半是烯氧化物,在烯氧化物中,亚烷基含有2到8个炭原子,或者是环氧化的脂肪酸酯,其中,脂肪酸基含有直到约30个炭原子,酯基是从含有直至约8个炭原子的低醇得到的。代替琥珀酸或酸酐,一种内酯酰化物或已取代的琥珀酸卤化物,可用在上述举例说明的方法中制备本发明的酯,该酰基卤可以是酰二溴,酰二氯,酰基氯和酰基溴。已取代的琥珀酸和酸酐可用下列方法制备,例如:顺丁烯二酸酐与高
分子量的烯烃或卤代烃反应,该卤代烃可用前面所述的烯烃聚合物的卤化而得到。本反应仅是在约100℃到250℃的最佳温度下加热反应产物。由这个反应得到的产品是烯基琥珀酸酐。这个烯基可加氢成为烷基。这个酐可用水或蒸汤水解成为相应的酸。用于制备琥珀酸或酸酐的另一个方法包括衣康酸或酸酐与烯烃或氯化烃反应,反应温度通常在约100℃到250℃范围内。琥珀酸卤化物可用酸或其酸酐与卤化剂如三溴化磷,五氯化磷或亚硫酰二氯反应来制备。制备琥珀化合物的这些和其他方法在现有技术中是已知的,在此无需进一步详细说明。
制备用于本发明燃料的酯,还有其他的有效方法,例如,酯可用下列反应得到,如用顺丁烯二酸或酸酐与如上述的醇反应生成顺丁烯二酸的单或二酯,然后该酯与烯烃或如上所述的氯化烃反应。也可用下面的反应得到酯,首先酰化衣康酸或酸酐,然后将这个酯的中间体与烯烃或氯化烃在类似于上文所述的那些条件下反应。
聚合的分散剂
已提出大量不同类型的聚合的分散剂,在润滑油的配制中很有效。在本发明的燃料组合物中,这种聚合的分散剂也是有效的。通常这类添加剂被述之为具有分散性的粘度指数改进剂,像在润滑油配制中一样有效。聚合的分散剂通常是具有长炭链和含有“极性”化合物的聚合物或共聚物,极性化合物具有分散性。含有的极性基团有:胺,酰胺,亚胺,亚酰胺,羟基,醚等。例如,聚合的分散剂可以是异丁烯酸酯或含有附加极性团的丙烯酸酯的共聚物,含有极性基团的乙烯丙烯共聚物,乙烯基乙酸酯反式丁烯二酸酯共聚物。
许多这种聚合的分散剂在现有技术中已经介绍过,所以没有必要详细列出各种不同类别。下面是叙述聚合的分散剂的专利例子。美国专利4,402,844介绍了含氮共聚物,是用Lithiated加氢的共轭的二烯乙烯芳基共聚物与已取代的氨基内酰胺反应来制备的。美国专利3,356,763介绍了一种制备二烯烃块状共聚物的方法,该二烯烃如1,3-丁二烯和乙烯基芳烃如乙烯基苯乙烯。美国专利3,891,721介绍了苯乙烯-丁二烯-2-乙烯基吡啶的块状聚合物。
许多聚合的分散剂可通过将极性单体接到聚烯烃主链上来制备。例如,美国专利3,687,849和3,687,905叙述了用顺丁烯二酸酐作为接枝单体接到聚烯烃主链上。顺丁烯二酸或酸酐特别适合于作接枝单体,因为这种单体相对来说是廉价的,并提供了一种经济的方法,该方法是通过顺丁烯二酸或酸酐的羧基与如氮化合物或羟基化合物进一步反应,将分散剂氮化合物加入到聚合物中。美国专利4,160,739叙述了接枝共聚物,该接枝共聚物是由含顺丁烯二酸或酸酐的单体体系与至少另一个不同的单体接枝而得到,该不同单体可立即加成,并且是可共聚的,然后被接枝的单体系与聚胺进行后反应。与顺丁烯二酸或酸酐可共聚的单体是任何α1β-单烯酸不饱和单体,该单体可充分的溶解在反应介质中,并且容易与顺丁烯二酸或酸酐反应,以便使大量的顺丁烯二酸或酸酐能加入到接枝聚合产物中。因此,适合的单体包括酯,胺和丙烯酸与异丁烯酸的腈,和含有非游离酸类的单体。杂环单体夹杂到接枝共聚物中的过程述之如下:第一步,内烯酸或异丁烯酸的烷基酯以单独或与苯乙烯化合的形式接枝聚合到主链共聚物上,形成第一接枝聚合物,该主链共聚物是加氢了的,苯乙烯和含有4到6个炭原子的共轭二烯的块状共聚物。第二步,可聚合的杂环单体以单独的或与疏水乙烯酯化合的形式共聚到第一接枝共聚物上。形成第二接枝共聚物。
叙述有效的接枝共聚物作为本发明燃料分散剂的其他专利有:美国专利3,243,481,3,475,514,3,723,575,4,026,167,4,085,055,4,181,618和4,476,283。
另一类在本发明燃料组合物中的有效的聚合的分散剂是所谓的“星形”高聚物和均聚物。例如该聚合物在美国专利4,346,193,4,141,847,4,358,565,4,409,120和4,077,893中叙述过。以上所有有关聚合的分散剂的专利作为合适的聚合分散剂专利公开了。这些聚合的分散剂可用于本发明的燃料中。
烃取代的酚分散剂
用于本发明燃料组合物中的烃取代酚分散剂有烃取代的酚化合物,其中烃取代物具有分子量足以使酚化合物溶于燃料。通常,烃取代物实际上是饱和的,至少含有约30个炭原子的烃基类。该酚化合物通常由下列分子式表示:
(R)a-Ar-(OH)b分子式ⅩⅤ
其中R实际上是含有平均为30到约400个脂肪族炭原子的饱和烃基取代物,a和B分别为1,2或3。Ar为芳族的一部分,如苯核,萘核或联苯核。由上面通过分子式ⅩⅤ表示的酚盐可任意合有其他取代物如低烷基类,低烷氧基,硝基,氨基和卤素。任意取代物的最好例子是硝基和氨基类。
分子式ⅩⅤ中实际上饱和的烃基类R含有直至约750个脂肪族碳原子,尽管它一般含最大平均值约为400个炭原子。在某些情况下,R含量小值约50个炭原子。如上所述,在芳族的一部分Ar中,对于每个芳核,该酚化合物可含有一个以上的R基。
通常烃基类R是由单或二烯烃的均聚物或互聚物(如共聚物,三聚物)制得的,该单或二烯烃含有2到10个炭原子,如乙烯,丙烯,丁烯-1,异丁烯,丁二烯,异戊间二烯,1-己烯,1-辛烯等。特别的是,这些烯烃是1-单烯烃。该R可由该均聚物或互聚物的卤化(如,氯化或溴化)类似物制得。可是该R类可由下列其他的原料得到,例如,单体高分子量的烯烃(如,1-四十烯)和它的氯化类似物和氢氯化类似物,脂肪族石油馏份,特别是石腊和它的裂化,氯化类似物和氢氯化类似物,甘油,如由Ziegler-Natta过程制备的含成烯烃(如聚(乙烯)润滑脂)和其他本专业领域技术人员所知道的原料。在R类中任何不饱和部分可在下面叙述的硝化步骤之前,按照现有技术已知的方法,经过加氢反应得到减少或除去。
下面是饱和的烃基R类的特殊例子:
四十烷基
五十一烷基
含有约35到70个炭原子的聚(乙烯/丙烯)类的混合物
含有约35到70个炭原子的氧化或机械降解的聚(乙烯/丙烯)类的混合物
含有约80到150个炭原子的聚(丙烯/1-己烯)类的混合物
含有20到32个炭原子之间的聚(异丁烯)类混合物
含有平均数为50到75个炭原子的聚(异丁烯)类混合物
较佳的R类原料是聚(异丁烯),该聚(异丁烯)可由含35%到75%(重量)的丁烯和30%到60%(重量)的异丁烯的C4炼油流出物在路易斯酸催化剂如三氯化铝或三氟化硼存在下通过聚合反应得到。这些聚丁烯主要含有(大于总重复单元的80%)如下结构重复单元的异丁烯。
-C(CH3)2CH2-
把烃基类R连接到本发明的氨基酚的芳族的一部分Ar上的方法可由本专业领域技术人员所已知的一些方法来完成。
在一个较佳的实例中,用于本发明燃料中的酚分散剂是由分子式ⅩⅤ表示的烃取代的硝基酚,分子式ⅩⅤ中的任意取代物是一个或多个硝基。通过硝化适合的酚可方便地制备硝基酚。典型的硝基酚可通过硝化烷基酚制成,该烷基酚含有一至少30个,最好约50个炭原子的烷基。用于制备本发明燃料中烃取代硝基酚的一些方法,已在美国专利4,347,148中介绍过。
在另一个较佳的实例中,用于本发明中的烃取代分散剂是如分子式ⅩⅤ表示的烃取代氨基酚,分子式ⅩⅤ中的任意取代物是一个或多个氨基。氨基酚可以容易的通过硝化适合的如上所述的羟基芳族化合物,然后还原硝基成氨基而制备出来。典型地,有效的氨基酚可通过硝化和还原烷基酚而生成,该烷基酚含有至少约30,最好约50个炭原子的烷基或烯基。在本发明中,作为分散剂使用的大量的烃取代氨基酚的制备方法在美国专利4,320,021中作过介绍。
可溶于燃料的烷氧基化了的醇,酚或胺的衍生物
可溶于燃料的醇,酚或胺的烷氧基化衍生物也可作为分散剂用在本发明的燃料组合物中。只要衍生物是能溶于燃料的。这种衍生物的各种繁多品种就能得到利用。最好是,这种衍生物除能溶于燃料外,应当是不溶于水的。因此,在一个较佳实施例中,作为分散剂溶于燃料中的烷氧基化的衍生物具有的特征是,有1到约13的亲水亲油平衡值。
本专业领域技术人员知道,烷氧基化的衍生物的燃料可溶性和水不溶性的特征,可通过醇或酚和胺的选择,特别是烷氧基反应物的选择,和通过烷氧基反应物与醇,酚和胺反应的数量选择得到控制。因此用于制备烷氧基衍生物的醇是以烃为基的醇,而胺是烃取代的胺,例如,上述的作为分散剂
(B)(ⅰ)的烃取代胺。酚可以是苯酚或烃取代酚,烃取代物可含有至少一个炭原子。
烷氧基化衍生物通过醇,酚或胺与环氧化物或环氧化物与水的混合物反应而获得。例如,该衍生物可通过醇,酚或胺与等摩尔量的或过剩的环氧乙烷反应而制备出来。其它的能与醇,酚或胺反应的环氧化物包括,例如,环氧丙烷,氧化苯乙烯,氧化1,2-丁烯,氧化2,3-丁烯,氰甲代氧丙环,氧化环己烯,氧化1,2-辛烯等。最好的环氧化物是氧化烯,在该氧化烯中,亚烷基含有约2到8个炭原子。如上所述,所希望的并且较佳的是,与醇,酚或胺反应的氧化烯的量不足以使衍生生物溶于水。
下面是可以市售得到的氧化烯衍生物的例子,该衍生物在本发明的燃料组合物中,可用作分散剂:Ethomeen S/12,伯脂肪胺的叔胺环氧乙烷缩合产品(亲水亲油平衡值,4.15,Armak Industries)Plurfac A-24,由巴登苯胺烧矸厂Wgandotte Industries得到的氧乙烯化的直链醇(亲水亲油平衡值5,0)等。对那些熟悉现有技术的人来说,其他适合的可溶于燃料的醇,酚和胺的烷氧基化的衍生物已是显而易见的。
下列的具体实施例说明了用于本发明燃料组合物中的典型分散剂的制备方法。
实施例B-1
将下列由三种化合物组成的混合物加热到回流,
这三种化合物是:1500份分子量为950,(含氯5.6%)的氯化聚(异丁烯);285份含有在化学计量中相当于四亚乙基五胺的平均组份的亚烷基聚胺和1200份苯。然后,在整4小时内,将该混合物的温度慢慢地增加到170℃,同时苯被除去。已冷却的混合物用同等体积的己烷和无水乙醇(1∶1)的混合物稀释,加热混合物到回流,然后,将1/3体积的10%含水碳酸钠加到该混合物中。搅拌后,冷却混合物,并进行相分离。得到的有机相用水洗涤,汽提,就得到了所需要的含有4.5%(重量)氮的聚异丁烯基聚胺。
实施例B-2
将下列由三种化合物组成的混合物加热到150℃,同时除去了水/甲苯共沸物,这三种化合物是:140份的甲苯,400份皂化值为109的聚异丁烯基的琥珀酸酐(由分子量约为850的聚(异丁烯)制备,汽相渗透压测定法)和63.3份含有在化学计量上相当于四亚乙基五胺的平均组份的亚乙基胺。然后该反应混合物在减压下加热到150℃,直到甲苯不再蒸馏出,剩下的酰化了的聚胺含有4.7%(重量)的氮。
实施例B-3
在整2个小时内,将6820份异硬脂酸加入到在110-150℃温度下加热的1133份工业用二亚乙基三胺中。该混合物在150℃温度下保持1小时,然后再加热,在1小时内使温度达到180℃,最后该混合物在0.5小时内加热到205℃,在整个加热过程中,将氮气吹入混合物中,以除去易挥发组份。该混合物在205-230℃温度下保持总共11.5小时,然后在230℃/20托(2.65千帕)下汽提,得到的剩余物为所需要的含6.2%(重量)氮的酰化聚胺。
实施例B-4
在1小时内,将22份37%的甲醛(相当于8份醛)的水溶液逐滴加入到一混合物中,该混合物含有50份聚丙基取代的酚(其分子量约为900,汽相渗透压测压法),500份矿物油(一种溶剂精制石腊油,在100°F粘度为100赛氏通用粘度秒)和130份9.5%的含水二甲基胺溶液(相当于12份胺)。在上面加入过程中,反应温度慢慢地增加到100℃,然后,在那个温度下保持3小时,同时将氮气吹入混合物中。将100份甲苯和50份混合的丁醇加入到冷却的反应混合物中。有机相用水洗涤三次直到对石蕊试低显中性,过滤有机相,在200℃/5-10(0.66-1.33千帕)托下汽提,剩余物是含0.45%(重量)氮的以油状溶液存在的最终产物。
实施例B-5
有一混合物是在90℃下制备的,该混合物含有140份矿物油,174份皂化值为105的聚(异丁烯)取代的琥珀酸酐(分子量为1000)和23份异硬酯酸。在1.3小时内,在80°-100℃下,将17.6份具有总组份相当于四亚乙基五胺的聚亚烷基胺的混合物加入到这个混合物中。反应是放热的,在225℃,氮气以每小时5磅(2.27公斤)的流速吹入混合物中,吹3小时,随后得到47份含水馏份。混合物在225℃干燥1小时,冷却到
100℃,过滤得到所需要的以油状溶液形式存在的最终产物。
实施例B-6
烃取代的琥珀酸酐可由下面的方法制备,即氯化分子量为1000的聚异丁烯,使氯的含量为4.5%,然后在150℃-220℃下加热氯化聚异丁烯具有摩尔比为1.2的顺丁烯二酸酐,如此得到的琥珀酸酐的酸值为130,含有874克(1摩尔)的琥珀酸酐和104克(1摩尔)的新戊二醇的混合物在240°-250℃/30毫米(4千帕)下混合12小时,残余物是一个酯的混合物,该酯是由酯化乙二醇的一个和两个羟基而得到的,该残余物的皂化值为101,醇的羟基含量为0.2%(重量)。
实施例B-7
实施例B-2中的烃取代琥珀酸酐的二甲基酯的制备方法如下:在50°-65℃下加热含有2185克酸酐,480克甲醇和1000毫升甲苯的混合物,同时用氯化氢鼓泡通过反应混合物,鼓泡3小时。然后,在60-65℃下,加热混合物2小时,再溶解在苯中,用水洗涤,干燥,过滤。在150℃/60毫米(8千帕)下加热滤液,除去挥发物组份。残余物确定为二甲基酯。实施例B-8
羧酸酯的制备如下:在1.5小时内,温度保持在115°-125℃,将3240份高分子量的羧酸(由氯化聚异丁烯和丙烯酸以1∶1的当量比反应制得,并且具有平均分子量为982)慢慢地加入到含有200份山梨酸和100份稀释剂油的混合物中,然后加入400份附加稀释剂油,该混合物在约195°-205℃下保持16小时,同时向混合物中吹入氮气。然后,加入另外的755份油,混合物冷却到140℃,过滤。滤液是所需要的酯的油状溶液。
实施例B-9
有一酯的制备如下:加热658份平均分子量为1018的羧酸(通过氯化聚异丁烯和丙烯酸反应而制备)和22份季戊四醇,同时温度在180°-205℃下保持18小时,在此期间,吹氮气通过混合物。然后过滤混合物,所得滤液为所需要的酯。
实施例B-10
将含有408份季戊四醇和1100份油的混合物加热到120℃,然后,慢慢地加入2946份已预热到120℃的实施例B-9的酸,225份二甲苯和95份二甘醇二甲基醚。所得混合物在195-205℃下加热,在氮气氛下和回流条件下进行11小时,在140℃22毫米汞柱(2.92千帕)压力下,汽提,过滤,滤液含有所需要的酯。稀释该酯,使油的总含量为40%。
如上所述,本发明的燃料组份含有大量的液态烃燃料和少量的下列化合物:
(A)至少一个含有可溶于烃的含碱金属或碱土金属的如上所述的组合物和
(B)如前所述的清除剂。
本发明与燃料组合物特别有关,该燃料组份是无铅或低铅汽油。为了本说明书和权利要求的应用,术语:“无铅”是表示无铅化合物,如有意加入到燃料中的四乙铅或四甲基铅。术语“低铅”是表示每加仑燃料含有小于约0.5克铅。本发明对于每加仑燃料含有小到0.1克铅的低铅燃料组合物(0.0264克/升)特别有效。
虽然,本发明的燃料组合物中最好不含有多余的大量过剩的金属组份,但是在本发明的燃料组合物中,含有烃可溶的碱金属或碱土金属的组合物(A)的量可在一个很大的范围内变化。燃料中所含有的这个量应足以改善需要的性能,例如,当该燃料在不是为使用无铅汽油设计的内燃机中燃烧时,减少阀座后退的磨损。例如,为加铅燃料设计的老内燃机,其构造不带有特殊的淬火阀座。因此燃料中所含有金属组合物的量,将部分的取决于燃料中铅的含量。对无铅燃料,需要大量的金属组合物以提供所需要的减低阀座后退磨损。当按照本发明处理低铅燃料时,通常需要较少量的含金属的组份。
总之,当本发明的燃料组合物用在内燃机中时,该燃料所含的组合物(A)的量,将足以减小阀座退回的磨损。通常,每升燃料中含有小于约0.2克,最好小于0.1克的碱金属或碱土金属化合物。虽然,每百万份燃料中含有10到60份的碱金属或碱土金属的量似乎是适用于大多数情况,但是,在另一个实例中,在本发明的燃料组合物中,每百万份的燃料约含有1到约100份的碱金属或碱土金属。含碱金属或碱土金属的燃料组合物与清除剂的重量比,一般为约5∶1到约1∶25,最好为约3∶1到约1∶15。
可选择地存在于本发明的燃料组合物中的可溶
于烃的无灰分散剂的用量,也可有一个很大的变化范围,并且该用量部分地取决于含金属组合物的用量(A),该含金属组合物与无灰分散剂的用量比范围从约4∶0.1到1∶4。包含在一定的燃料组合物中的无灰分散剂的用量,可由本专业领域技术人员很容易地决定,显然,包含在燃烧中的分散剂的用量不应太高,以致受到有害杂质的影响,如当内燃机冷却时,在内燃机部件上会有沉积物形成。通常,把燃料制备成每百万份重量的燃料就含有50-500份,最好是80-400份重量的分散剂。
本发明的燃料组合物的制备,或是通过把各种单独组分加到液体烃燃料中,或是加入一种浓缩物,该制备好的浓缩物含有各种纯的或存在于烃稀释剂如矿物油中的组份。最好是该稀释剂的闪点处在产品在内燃机内容易燃烧的温度范围内。当制备一种浓缩物时,包含在浓缩物中的各组份的相对数量与所需的燃料组合物的相对数量基本上是一致的。所得产品具有高度的水稳定性,如无机阳离子与水接触时,不会被明显地从产品中浸出。
下面的实施例按照本发明说明了浓缩物和燃料组合物。
实施例1(浓缩物) 重量份数
实施例A-1的中性磺酸钠 200
实施例B-1的分散剂 75
矿物油 75
实施例2(浓缩物)
实施例A-1的中性钠盐 100
实施例B-5的分散剂 25
矿物油 25
实施例3(浓缩物)
实施例A-1的中性磺酸钠 168
实施例B-5的分散剂 42
重油 40
矿物油
实施例4(浓缩物)
实施例A-1的中性磺酸钠 336
实施例B-5的分散剂 84
重油 80
实施例5(浓缩物)
每1000桶无铅汽油燃料用500磅实施例2的浓缩物处理。
实施例6
利用吲哚烯清净燃料使内燃机稳定,发动机稳定后,输入实施例1的添加剂1000PTB。二烷基苯磺酸镁也以每2个钠原子中就有1个镁原子的比例存在于燃料中。通过使用碱金属和碱土金属盐的混合物保持阀门的安全。
除了本发明的添加剂外,其他通用的燃料添加剂的使用也已仔细考虑过。因此,该燃料组合物也可以含有表面点燃抑制剂,染料,胶质抑制剂,氧化抑制剂等等。
本发明一般地针对于燃料组合物,但特别是针对于含有一种金属或碱土金属组合物,一种无灰分散剂和净化剂的低铅或无铅汽油组合物。本发明的燃料组合物也可用来降低从排气口中排出的烃,使燃烧室得到改善和使阀洁净,减少活塞上的积炭,减少汽化器狭口的沉积物,降低曲柄箱内和阀盖的淤渣和积炭。
实施例7
把250PTB(0.72克/升)实施例3的浓缩物加入吲哚烯中(燃料标准参考文献)。该燃料也含有0.1克/加仑(0.026克/升)铅如四乙基铅。发动机运行170小时后没有观察到辛烷需要量(ORT)明显增加。在没有实施例2的浓缩物时,利用燃料和铅的混合物使发动机何持原来的稳定108小时。
上述实验的目的是为了表明实施例3的添加浓缩物,以适于保护排气口阀座的比例加到低铅燃料中时,不会过分增加发动机的辛烷需要量。
实施例8
起始辛烷需要量为84的发动机加注吲哚烯,并且运行了144小时。运行到144小时为了使发动机稳定辛烷需要量增加5个单位。在144小时的时候标明燃料已被换成含有实施例3浓缩物250PTB的吲哚烯。发动机总运行时间数为252小时,而且观察到辛烷需要量又增加了2个单位。
这个实施例表明了一台发动机靠含铅燃料运行的稳定效果,该含铅燃料在稳定过程中含有一种无铅燃料。在没有任何净化剂的情况下浓缩物的气门安全效果也能获得。当浓缩物(实施例3)对ORI的影响最小时,由于发动机运行了开头的144小时后的稳定效果,对于某些发动机来说,多半是不合格的。因此在这个实施例中考虑到有必要减少总ORI。
实施例9
一台发动机像实施例8中的一样稳定了144小时。该实例中使用的燃料也是吲哚烯纯。发动机稳定后,加入250PTB实施例3的添加浓缩物。稳定后的燃料含有一种作为净化剂的二溴化乙烯和二氯化乙烯混合物。所用的二溴化乙烯的含量用摩尔比率表示是每2个钠原子就有来自二溴化乙烯(EDB)的1个溴原子。氯化乙烯(EDC)的含量为每1分子钠就有来自于(EDC)的一分子氯。
发动机运行240小时后没有观察到ORI增加。该实施例表明,当使用了净化剂即实施例3的添加浓缩物ORI不会进一步增加。
实施例10
一台发动机依靠吲哚烯纯燃料稳定运行了110小时。然后使用实施例4的一种阀处理剂1000PTB(百万分之32钠)重新起动发动机。燃料也含有二溴化乙烯和二氯化乙烯,其溴和氯与钠之比与实施例9一样。
该实施例表明,增加添加浓缩物含量对保护气门是有利的。在320小时的时候,ORI的升高与110小时稳定期是相等的。
实施例11
一种吲哚烯纯试样用于稳定一台内燃机145小时。在145小时的时候,把1000PTB(百万分之32钠)实施例4的浓缩物加入燃料中,然后继续试验。145小时稳定期后,作为曼尼期卤咸的有百万分之15铜还存在于燃料中。该内燃机的试验继续到350小时。
拆开内燃机发现内燃机内有沉积物形成。在350小时整个过程中,内燃机内形成一些沉积物,没有缺口或枝状沉积物迹象。没有枝状沉积物说明燃料没有受到反常的预热作用。对阀座的保护令人满意。
实施例12
一台内燃机靠吲哚烯纯运行,并稳定了210小时。运行到210小时时,1000PTB实施例4中的浓缩物加入到燃料中。铈也以其辛酸盐的形式存在于燃料中,其辛酸盐含百万分之55的铈。该产物能减少阀座的后退磨损。观察到的ORI增值在运行210到396小时之间比开头的稳定期低。
实施例13
该实施例使用一台靠吲哚烯纯燃料稳定了96小时的内燃机。运行到96小时时,调配燃料使其含有1000PTB实施例4的浓缩物,锰也以羧酸盐的形式存在于燃料的混合物中。锰含量是百万分之15。
该实施例表明利用锰对减少内燃机内离子一含炭沉积物的形成是有利的。ORI增值在96小时(开头稳定期间)的试验结束的240小时之间仅仅稍大于开头试验期。对阀座的保护也是合格的。
实施例14
一种吲哚烯纯燃料被稳定96小时。96小时后,在燃料中加注1000PTB实施例4的添加浓缩物。然后重新起动内燃机,使实验进行到时间总数为310小时。
该实验表明在没有任何类型净化剂的情况下,在整个过程中(稳定+后添加)其ORI增值大于含有燃烧改进剂(净化剂)或通用的铅净化剂那些实施的ORI增值。该实施例中对阀座的保护是合格的。
实施例15
一种吲哚烯纯燃料试样用于稳定一台内燃机。内燃机稳定后,在燃料中加入1000PTB实施例4的浓缩物。燃料中另外一种成分是铝,以三异丙基铝和2-乙基己基醇化合的加和物的形式存在(摩尔比率分别为1∶2)。Ethomeen G1-12也存在于燃料中,它与异丙醇的摩尔比率是1∶1。浓缩物里每摩尔的钠,就要使用1摩尔铝。然后用浓缩物和燃料中的铝物料重新稳定内燃机。然后拆开内燃机,对沉积物的形成分级。对阀座后退的防护令人满意,沉积物的形成是可允许的。
实施例16
一种吲哚烯纯燃料用于稳定内燃机140小时。发动机运行到140小时时,处理燃料使其含有100PTB实施例4的浓缩物,该浓缩物通过把硼充分溶合到分散剂中而得到改进。阀座磨损的保护合格,而且汽缸中没有过多的沉积物形成。
实施例17
象上述实施例一样,有一种吲哚烯纯燃料物源,使内燃机稳定120小时。记录120小时稳定期的ORI值。然后在燃料中加入1000PTB实施例4的浓缩物和以其羧酸盐形式存在的铁。燃料中铁的浓度是百万分之15。稳定后ORI增值仅仅稍大于开头稳定期间的增值。
实施例18
有一种与上述实施例一样的吲哚烯纯燃料试样。利用该燃料使一台内燃机稳定以得到初始ORI增值。用250PTB(百万分之8的钠)实施例3的浓缩物处理燃料。该燃料也用具有实施例9给予的氯与钠比例的二氯化乙烯处理。该内燃机可重新稳定,并确定ORI值。该ORI值是合格的,阀座的保护令人满意。
实施例19
有一种与前面实施例一样的燃料。初始稳定期间确定ORI需要量,然后改变燃料供给,配入以硅酮流体形式存在的硅。硅以每2摩尔钠中有一摩尔硅的比率加到燃料中。
在试验期终点,重新确定ORI值,观察内燃机的阀座磨损。阀座磨损和ORI增值是合格的。
实施例20
有一种与前面的实施例一样的吲哚烯纯燃料。试验内燃机直到获得ORI值稳定。稳定后燃料改变成含有250PTB实施例3的添加剂。除了实施例3的添加剂外,该燃料还含有锂,以1比1摩为基础,每1份钠就有1份锂。锂以其烷基苯磺酸盐的形式加入到配料中。
重新起动内燃机,并再次达到ORI值稳定。以后,拆开内燃机检查阀座的磨损情况。该产品在ORI值和阀座磨损两方面是合格的。
实施例21
有一种吲哚烯纯燃料试样,使内燃机的ORI值稳定。这时改善燃料使其含有250PTB实施例3的浓缩物。进一步改善燃料使其含钛,钛以其异丙氧化物和C9-11醇与2,4-戊醇二酮混合物的形式存在,三者的摩尔比率是1∶1∶1。钛与钠的比率为1∶1。
用改性燃料重新起动内燃机,使其ORI值再次稳定。试验结束时测量ORI值和磨损结果是合格的。
实施例22
与前面的实施例一样,一种吲哚烯纯燃料用于内燃机中,稳定后,燃料中加入250PTB实施例4的浓缩物。燃料中也含有百万分之15的钛。钛以其异丙氧化物(A)的形式存在,带有2,4戊二酮(B)和十一烷基醇与壬基醇混合物(C),摩尔比率A∶B∶C是1∶1∶1。
用改性燃料重新起动内燃机,使其再次获得ORI值稳定。试验结束时测量ORI值,拆开内燃机检查沉积物和阀座磨损情况。所得ORI值和磨损结果合格。
实施例23
有一种如实施例20中的燃料。使内燃机稳定,改性燃料使其含有百万分之15的钼,钼以二钼酸铵的二甲苯溶液,并带有表面活性剂Eethomeen0-12的形式存在。钼组合物含11.9%重量钼。该燃料也含有1000PTB实施例4的浓缩物。观察得到的ORI值和阀门磨损,结果合格。
Claims (14)
1、一种内燃机燃料组合物,其中含有数量居多的液态烃燃料和少量当该燃料用于内燃机时足以减少阀座后退的下述组分,
(A).至少一种烃溶的含碱金属或碱土金属的组合物,
(B).至少一种烃溶的无灰散剂,每升燃料含铅少于0.5克,每升燃料含碱金属或碱土金属少于0.2克,组分(A)和(B)之比值为从约4∶0.1至约1∶4,组合物(A)是硫酸,磷酸羧酸或酚的一种碱金属或碱土金属的盐,其中(A)是一种中性或碱性的有机磺酸盐。
2、按照权利要求1的燃料组合物,其中燃料为无铅汽油。
3、按照权利要求2的无铅组合物,其中(A)为烃基琥珀酸的碱金属盐。
4、按照权利要求2、3或1的无铅组合物,其中(A)为钾盐。
5、按照权利要求2、3或1的无铅组合物,其中(A)为钠盐。
6、按照权利要求1的燃料组合物,其中(A)是一种碱金属或碱土金属的磺酸盐,该磺酸由式R1(SD3H)r或(R2)XT(SD3H)y表示,其中R1和R2分别是脂族基,R1至少含约15个碳原子,R1和T中的碳原子总数至少约是15,T是一个芳烃核,x、r和y都是至少为1。
7、按照权利要求1的燃料组合物,其中分散剂(B)选自下述化合物:
(Ⅰ).一种烃基取代的胺,其中该烃基取代基本上是脂族基并至少含8个碳原子,
(Ⅱ).一种酰化了的含氮化合物,该化合物有一个至少10个脂族碳原子的取代基,它是由羧酸酰化剂与至少一个含至少一个-NH-基的氨基化合物反应制得的,所说的酰化剂是通过一个亚氨基,酰氨基,或酸基铵键连到所说的氨基化合物上,
(Ⅲ).一种酚,醛和至少有一个-NH-基的氨基化合物的含氮缩合物,
(Ⅳ).一种取代羧酸的酯,
(Ⅴ).一种聚合的分散剂,
(Ⅵ).一种烃取代的酚分散剂,和
(Ⅶ).一种燃料溶的烷氧基化的醇,酚或胺的衍生物。
8、按照权利要求1的燃料组合物,其中分散剂(B)是至少一种酰化了的含氮化合物,该化合物有一个至少约10个脂族碳原子的取代基,是由一种羧酸酰化剂与至少一种含至少一个-NH-基的氨基化合物反应制得的,所说的酰化剂通过一个亚氨基,酰氨基,或酸基铵键连到所说的氨基化合物上。
9、按照权利要求1的燃料组合物,其中分散剂(B)是至少一种取代羧酸的酯。
10、按照权利要求7的燃料组合物,其中酰化了的含氮的化合物(B)是由羧酸酰化剂与至少一种含至少一个-NH-基的氨基化合物反应剂得的,所说的酰化剂通过一个亚氨基,酰氨基,或酸基氨键连到所说的氨基化合物上。
11、按照权利要求10的燃料组合物,其中氨基化合物是一种有一般式为
R3-N(-U-N)n-R3
R3R3
的亚烷基聚胺,其中U是一个约1~18个碳原子的亚烷基,每一个R2分别是氢原子,烃基或含有直至约30个碳原子的羟基取代的烃基,但须至少一个R3是氢原子,n是1~大约10。
12、按照权利要求11的燃料组合物,其中亚烷基聚胺是至少2~大约8个氨基的乙烯,丙烯或三亚甲基聚胺,或这些聚胺的混合物。
13、按照权利要求11的燃料组合物,其中羧酸酰化剂是单或多羧酸,或与其相当的反应物,该羧酸含一个至少约30个碳原子的脂肪烃基取代基。
14、按照权利要求7的燃料组合物,其中(B)是一种在链烯其中含至少约30个脂族碳原子的烯基琥珀酰亚胺。
Applications Claiming Priority (4)
Application Number | Priority Date | Filing Date | Title |
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US06/766,615 US4659338A (en) | 1985-08-16 | 1985-08-16 | Fuel compositions for lessening valve seat recession |
US766,615 | 1985-08-16 | ||
US06/863,623 US4690687A (en) | 1985-08-16 | 1986-05-14 | Fuel products comprising a lead scavenger |
US863,623 | 1986-05-14 |
Publications (2)
Publication Number | Publication Date |
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CN86106817A CN86106817A (zh) | 1987-05-27 |
CN1020632C true CN1020632C (zh) | 1993-05-12 |
Family
ID=27117773
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Application Number | Title | Priority Date | Filing Date |
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CN86106817A Expired - Lifetime CN1020632C (zh) | 1985-08-16 | 1986-08-15 | 燃料产物 |
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US (1) | US4690687A (zh) |
EP (2) | EP0423744B2 (zh) |
JP (1) | JPH0788514B2 (zh) |
CN (1) | CN1020632C (zh) |
AR (1) | AR243589A1 (zh) |
AT (3) | ATE77828T1 (zh) |
AU (2) | AU591394B2 (zh) |
BR (1) | BR8606850A (zh) |
CA (1) | CA1303853C (zh) |
DE (4) | DE233250T1 (zh) |
DK (2) | DK170216B2 (zh) |
ES (1) | ES2001515A6 (zh) |
FI (2) | FI871661A0 (zh) |
HK (1) | HK36993A (zh) |
IL (1) | IL79599A (zh) |
MX (1) | MX164983B (zh) |
NO (1) | NO174814C (zh) |
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-
1986
- 1986-05-14 US US06/863,623 patent/US4690687A/en not_active Expired - Lifetime
- 1986-07-31 AT AT86905065T patent/ATE77828T1/de not_active IP Right Cessation
- 1986-07-31 DE DE198686905065T patent/DE233250T1/de active Pending
- 1986-07-31 DE DE3685877T patent/DE3685877T3/de not_active Expired - Fee Related
- 1986-07-31 DE DE3650239T patent/DE3650239T3/de not_active Expired - Lifetime
- 1986-07-31 DE DE3650634T patent/DE3650634T2/de not_active Expired - Lifetime
- 1986-07-31 AT AT90119864T patent/ATE118528T1/de not_active IP Right Cessation
- 1986-07-31 AT AT93202642T patent/ATE154068T1/de not_active IP Right Cessation
- 1986-07-31 EP EP90119864A patent/EP0423744B2/en not_active Expired - Lifetime
- 1986-07-31 BR BR8606850A patent/BR8606850A/pt not_active IP Right Cessation
- 1986-07-31 EP EP86905065A patent/EP0233250B2/en not_active Expired - Lifetime
- 1986-07-31 AU AU61929/86A patent/AU591394B2/en not_active Ceased
- 1986-07-31 JP JP61504335A patent/JPH0788514B2/ja not_active Expired - Fee Related
- 1986-07-31 WO PCT/US1986/001592 patent/WO1987001126A1/en active IP Right Grant
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- 1986-08-11 CA CA000515694A patent/CA1303853C/en not_active Expired - Fee Related
- 1986-08-11 AR AR86304864A patent/AR243589A1/es active
- 1986-08-14 ES ES8601105A patent/ES2001515A6/es not_active Expired
- 1986-08-15 MX MX3457A patent/MX164983B/es unknown
- 1986-08-15 CN CN86106817A patent/CN1020632C/zh not_active Expired - Lifetime
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1987
- 1987-04-13 NO NO19871551A patent/NO174814C/no not_active IP Right Cessation
- 1987-04-14 DK DK198701925A patent/DK170216B2/da not_active IP Right Cessation
- 1987-04-15 FI FI871661A patent/FI871661A0/fi not_active Application Discontinuation
- 1987-04-16 FI FI871707A patent/FI871707A0/fi not_active Application Discontinuation
- 1987-12-14 AU AU82530/87A patent/AU600058B2/en not_active Ceased
-
1993
- 1993-02-12 SG SG159/93A patent/SG15993G/en unknown
- 1993-04-15 HK HK369/93A patent/HK36993A/xx not_active IP Right Cessation
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1995
- 1995-06-12 DK DK066695A patent/DK66695A/da unknown
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