CN1048520C - 燃料油组合物 - Google Patents

燃料油组合物 Download PDF

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Publication number
CN1048520C
CN1048520C CN95193503A CN95193503A CN1048520C CN 1048520 C CN1048520 C CN 1048520C CN 95193503 A CN95193503 A CN 95193503A CN 95193503 A CN95193503 A CN 95193503A CN 1048520 C CN1048520 C CN 1048520C
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composition
alkyl
acid
application
fuel
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CN1150446A (zh
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R·卡普罗逖
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ExxonMobil Chemical Patents Inc
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Exxon Chemical Patents Inc
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Abstract

在低硫燃料中加入冷流改进剂提高了低硫燃料的润滑性。

Description

燃料油组合物
本发明涉及燃料油和应用添加剂改进燃料油的特性，更特别是柴油机燃料和煤油的特性。
由于环境保护的原因，需要降低燃料中的硫含量，特别是降低柴油机燃料和煤油中的硫含量，但是生产低硫含量燃料的精炼工艺也产生低粘度和燃料中其它组分含量降低了的产品，这些组分，例如多环芳烃和极性化合物，对燃料的润滑性是起作用的。再者，一般认为含硫化合物提供了抗磨性能，并且据报道，含硫化合物的比例的降低，再加上提供润滑性的其它组分的比例的降低已经使采用低硫燃料的柴油发动机的燃料泵的故障增加，故障的产生是由于例如凸轮板，滚子，心轴和驱动轴的磨损。
这一问题在将来可能会变得更坏，因为为了满足对废气排放的更严格的要求，一般要使用高压燃料泵，包括串联的、旋转的和组合式的喷射体系，它们比现在的设备须有更严格的润滑性要求，同时燃料的低硫含量将成为更广泛的要求。
现今，柴油机燃料的典型含硫量约为0.25％(重量)。欧洲的最高含硫量已降至0.20％，还期望降至0.05％；瑞典已经使用的燃料等级是含硫量低于0.005％(2类)和0.001％(1类)的燃料，在本文中含硫量低于0.20％(重量)的燃料油组合物称之为低硫燃料。
本发明是根据冷流改进剂增进低硫燃料润滑性的观察结果为基础的。
本发明的第一方面是提供用冷流改进剂增进含硫量至多为0.2％(重量)，特别是至多0.05％(重量)的燃料油组合物的润滑性。
本发明的第二方面是提供增进了润滑性的以石油为基础的燃料油的制造方法，该方法包括原油的精炼以生产低硫含量的燃料油，然后将冷流改进剂与精炼产品混合，以提供硫含量至多为0.2％(重量)，优选至多为0.05％(重量)和使之能产生的磨痕直径在60℃以HFRR试验(如下文所定义)测定至多为500μm，诸如至多450μm、优选至多380μm、更优选至多350μm的润滑性的燃料油组合物。
有利的是，以石油为基础的燃料油是中馏分燃料油。
本发明的第三方面提供了一组合物，该组合物包括主要部分的以石油为基础的燃料油和一小部分冷流改进剂，该冷流改进剂包括带有一个或多个式＝NR13取代基的油溶性极性氮化合物(式中R13代表含8-40个碳原子的烃基，该取代基或一个或多个这种取代基可以是其阳离子的形式)，组合物的硫含量至多为0.2％(重量)。有利的硫含量至多为0.05％(重量)。
有利的是，以石油为基础的燃料(油)是中馏分燃料油。
所说的极性氮化合物可以与一乙烯-不饱和酯共聚物流动改进剂结合使用。
有利的是，使用本发明的第一方面得到的组合物和本发明第三方面的组合物都有本发明第二方面所定义的润滑性。
本文所用“冷流改进剂”一词是指相对于未处理的基础燃料能够降低车辆适用性温度的任何添加剂，其例证是降低燃料的倾点、浊点、蜡出现温度、冷滤堵塞点(下称CFPP)或燃料的低温流动试验(LTFT)温度，或是减少燃料中、特别是中馏分燃料中蜡沉降的程度。
本文的“中馏分”一词是指得自原油精炼中作为较轻的煤油或喷气(机)燃料油馏分至重燃料油馏分的燃料油。这种燃料油也包括直馏和热裂解和/或催化裂解馏分的大气压或真空馏分、裂化瓦斯油或任何比例的混合物，其例包括煤油、喷气燃料、柴油机燃料、取暖油、减粘瓦斯油、轻循环油、真空瓦斯油、轻燃料油和燃料油。这种中馏分燃料油通常的沸点范围一般在100℃至500℃(按ASTM D 86方法测定)，更特别是在150℃至400℃范围。
将植物基的燃料油或“生物燃料”，例如菜籽甲酯或菜油包括在内作为组合物的组分也在本发明范围之内。
HFRR或高频往复装置(High Frequency Reciprocating Rig)试验是按CEC F-06-T-94和ISO TC22/SCT/WG6N 180所述的试验。
CFPP试验在下述期刊中有所定义：“石油研究院杂志”(Journal ofthe Institute of Petroleum)，52(1966)PP173-185。
现对本发明所用的冷流改进剂做进一步的详细叙述。许多种类的流动改进剂、特别是中馏分流动改进剂都适于在本发明中使用。在这些流动改进剂中可以论及的有：
(A)乙烯-不饱和酯共聚物，更特别是除了得自乙烯的单元外还含有下式单元的共聚物：
                   -CR1R2-CHR3-式中，R1代表氢或甲基；R2代表COOR4(R4代表1-9个碳原子的烷基，为直链烷基，或如果含有3个或更多的碳原子，则是支化的烷基)或OOCR5(式中R5代表R4或H)；R3代表H或COOR4。
它们包括乙烯与烯属不饱和酯或其衍生物的共聚物。其例是乙烯与一饱和醇和不饱和羧酸形成的酯的共聚物，但最好是由不饱和醇与饱和羧酸形成的酯。乙烯-乙烯基酯共聚物是有利的；优选的是乙烯-醋酸乙烯酯、乙烯-丙酸乙烯酯、乙烯-己酸乙烯酯或乙烯-辛酸乙烯酯共聚物。共聚物最好含5-40wt％的乙烯基酯，更优选10-35wt％的乙烯基酯。可以使用两种共聚物的混合物，如US3,961,916中所述。用气相渗透压测定法测得的共聚物数均分子量最好是1,000至10,000，优选1,000至5,000。需要时，共聚物可含来自其它共聚单体的单元，例如三元共聚物、四元共聚物或更高级的共聚物，例如其它的共聚单体是异丁烯或二异丁烯单体的共聚物。
共聚物的制备可用共聚单体直接聚合，或用乙烯-不饱和酯共聚物进行酯基转移或经水解然后再酯化的方法以得到不同的乙烯-不饱和酯共聚物。例如用此方法从乙烯-醋酸乙烯酯共聚物可以制得乙烯-己酸乙烯酯和乙烯-辛酸乙烯酯共聚物。
(B)梳形聚合物。这类聚合物的含烃基的支链是聚合物主链的侧基，它们已在下述文献中讨论：“梳形聚合物。结构和性质”(Comb-LikePolymer.Structure and Properties)，N.A.Plate和V.P.Shibaev，聚合物科学杂志大分子述评(J.Poly.Sci，Macromolecular Revs.)，8，pp117-253(1974)。
一般，梳形聚合物有一个或多个长链烃基分枝，例如通常情况下是10-30个碳原子的氧烃基分枝，在聚合物主链之侧，所说的分枝是直接或间接与主链结合的。间接结合的例子包括通过中置的原子或基团的结合，这种结合包括共价和/或电价结合，诸如盐中的结合。
梳形聚合物最好是均聚物，具有含至少6个碳原子并优选至少10个碳原子的侧链；或者是共聚物，其至少25、优选至少40、更优选至少50摩尔％的单元具有含至少6个碳原子并优选至少10个碳原子的侧链。
可述及的优选梳形聚合物的实例是具有下述通式的聚合物：式中，D＝R11、COOR11、OCR11、R12COOR11或OR11，
  E＝H、CH3、D或R12，
  G＝H或D，
  J＝H、R12、R12COOR11或芳基或杂环基，
  K＝H、COOR12、OCOR12、OR12或COOH，
  L＝H、R12、COOR12、OCOR12或芳基，
  R11为≥C10烃基，
  R12为≥C1烃基或亚烃基，
m和n代表摩尔份数；m是限定的数，最好是在1.0至0.4的范围；n小于1，最好是在0至0.6的范围。R11最好是代表有10至30个碳原子的烃基，而R12最好是代表有1至30个碳原子的烃基。
如果需要或要求，梳形聚合物可含从其它单体得到的单元。
这些梳形聚合物可以是马来酐或富马酸或衣康酸与另一烯属不饱和单体例如α-烯烃(包括苯乙烯)或一不饱和酯例如醋酸乙烯酯的共聚物，或是富马酸或衣康酸的均聚物。最好使用(但非必要的)等摩尔量共聚单体，虽然摩尔比在2∶1和1∶2的范围是适合的。可与例如马来酐共聚的烯烃实例包括1-癸烯、1-十二碳烯、1-十四碳烯、1-十六碳烯和1-十八碳烯。
梳形聚合物的酸基或酸酐基团可用任何适合的技术酯化，虽然优选马来酸或富马酸至少有50％被酯化，但不是必要的，可以使用的醇的实例包括正癸-1-醇、正十二碳-1-醇、正十四碳-1-醇、正十六碳-1-醇和正十八碳-1-醇。醇的每一链也可包括一个甲基支链，例如1-甲基-十五碳-1-醇或2-甲基-十三碳-1-醇。醇可以是正构醇和单甲基支化醇的混合物。优选使用的是纯的醇而不是商品供应的醇混合物，但如果使用混合物，则R12指烷基中碳原子的平均数；如果使用在1-位或2-位上含有一支链的醇，则R12指醇的直链主链链段；
这些梳形聚合物可以特别是富马酸酯或衣康酸酯的聚合物和共聚物，例如EP-A-153176、-153177和-225688以及WO91/16407中所述的聚合物和共聚物。
特别优选的富马酸酯梳形聚合物是富马酸烷基酯与醋酸乙烯基酯的共聚物，其中烷基有12-20个碳原子，更特别的是聚合物中的烷基有14个碳原子或者其中烷基是C14/C16烷基的混合物，是用例如等摩尔量的富马酸和醋酸乙烯酯的混合物进行溶液共聚合制得的，然后将得到的共聚物与醇或混合醇(最好是直链醇)进行反应。当使用混合醇时，最好是用1∶1(重量)的正构C14和C16醇的混合物。而且可以有利地使用C14酯和C14/C16混合酯的混合物。这种混合物中的C14与C14/C16比最好是在1∶1至4∶1、优选2∶1至7∶2、最优选约3∶1(重量)的范围。特别优选的梳形聚合物是那些数均分子量(以气相渗透压测定法测定)为1,000至100,000、更特别是1,000至30,000的聚合物。
其它适合的梳形聚合物是α-烯烃与酯化的苯乙烯-马来酐共聚物以及酯化的苯乙烯-富马酸共聚物的聚合物和共聚物。本发明可以使用两种或多种梳形聚合物的混合物，并且如上已指出，这种使用可以是有利的。梳形聚合物的其它实例是烃聚合物，例如乙烯和至少一种α-烯烃的共聚物，α-烯烃最好具有至多20个碳原子，其例是正癸-1-烯和正十二碳-1-烯，这种共聚物优选的数均分子量至少为30,000(以GPC测定)。烃共聚物可用本技术领域中的已知方法，例如用齐格勒(Ziegler)型催化剂来制备。
(C)极性氮化合物
这类化合物如上述本发明的组合物方面中所指出，是带有一个或多个、优选两个或更多的式＝NR13取代基的油溶性极性氮化合物，式中R13代表含8-40个碳原子的烃基，该取代基或一个或多个这种取代基可以是其阳离子形式。R13最好代表一含12至24个碳原子的脂肪烃基，油溶性极性氮化合物一般在燃料中作为蜡晶生长抑制剂。
烃基最好是线性或微线性的，即它可有一短(1-4碳原子)的烃支链。取代基是氨基时，它可带有多于一个的可以相同、也可以不相同的所说的烃基。
“烃基”一词是指有一碳原子直接连接到分子的其余部分并具有烃或主要是烃的性质的基团，其实例包括烃基，包括脂族的(例如烷基或链烯基)、脂环的(例如环烷基或环烯基)、芳族的、和脂环取代的芳族的、和芳族取代的脂族的和脂环基团。脂族基团最好是饱和的。这些基团可含非烃取代基，只要它们的存在不会改变基团的占优势的烃性质。非烃取代基的例子包括酮基、卤素、羟基、硝基、氰基、烷氧基和酰基。如果烃基是取代烃基，则优选单取代烃基。
取代的烃基的实例包括2-羟乙基、3-羟丙基、4-羟丁基、2-酮丙基、乙氧基乙基和丙氧基丙基。这些基团也可以是在其链中或由碳原子另外组成的环中含有非碳的原子。适合的杂原子包括例如氮、硫和(优选的)氧。
更特别的是，氨基或亚氨基或每一氨基或亚氨基取代基是通过诸如-CO-、-CO2 (-)、-SO3 (-)或亚烃基的中间连接基团结合到其一部分上的。连接基团是阴离子基团情况下，取代基是阳离子基团的一部分，如胺盐基团的情况。
当极性氮化合物带有多于一个的氨基或亚氨基取代基时，则每一取代基的连接基团可以是相同的或不相同的。
适合的氨基取代物是长链C12-C40、优选C12-C24烷基的伯、仲、叔和季氨基取代基。
优选的氨基取代基是二烷基氨基取代基，如上已指出，它可以是其胺盐的形式；叔胺和季胺只能形成胺盐，所说的烷基可以是相同的或不相同的。
氨基取代基的实例包括十二烷基氨基、十四烷基氨基、可可氨基和氢化牛脂氨基。仲氨基取代基的实例包括双十八烷基氨基和甲基二十二烷基氨基。混合的氨基取代基是可以存在的，诸如由天然存在的胺得到的氨基取代基。优选的氨基取代基是氢化牛脂仲氨基取代基，它的烷基衍生自氢化牛油脂肪，通常是由大约4％(重量)C14、31％(重量)C16和59％(重量)C18正构烷基组成的。
适合的亚氨基取代基是长链C12-C40、优选C12-C24烷基取代基。
所说的一部分可以是单体(环状或非环状)或聚合物。当它是非环状时，它可由一环状前体诸如酸酐或螺二内酯得到。
环状体系可包括碳环、杂环或稠合多环系列，或是两个或多个这样的环系列互相结合并且其中的环系列可以相同或不同的体系。当有两个或多个这样的环系列时，取代基可以在相同的或不同的系列上，优选在同一系列上。环系列或各环系列最好是芳香环，优选苯环。最优选的环状体系是单苯环，其取代基最好是在邻位或间位上，苯环还可以进一步被取代。
环系列的环原子最好是碳原子，但可包括例如一个或多个环N、S或O原子，此时的化合物即成为杂环化合物。
多环系列的实例包括：
(a)稠合苯结构，诸如萘、蒽、菲和芘；
(b)无苯环或非所有的环都是苯环的稠合环结构，诸如菌、茚、氢化茚、芴和二苯并呋喃；
(c)“头-头”结合的环，诸如联苯；
(d)杂环化合物，诸如喹啉、吲哚、2：3二氢吲哚、苯并呋喃、香豆素、异香豆素、苯并噻吩、咔唑和吩噻嗪；
(e)非芳环或部分饱和环系，诸如十氢萘、α-蒎烯、小豆蔻烯和冰片烯；
(f)三维结构，诸如降冰片烯、双环庚烷(即降冰片烷)、双环辛烷和双环辛烯。
极性氮化合物的实例叙述如下：
(i)一元或多元羧酸(例如具有1-4个羧酸基)的胺盐和/或酰胺。其制备方法可用例如至少1摩尔份的烃基取代胺与1摩尔份的酸或其酐反应。
当形成酰胺时，其连接基团是-CO-；当形成胺盐时，其连接基团是-CO2 (-)。
该部分可以是环或非环，环部分的实例是其中的酸为环己烷-1，2-二羧酸、环己烷-1，2-二羧酸、环戊烷-1，2-二羧酸和萘二羧酸。一般这样的酸在环的部分有5-13个碳原子。优选的这种环酸是苯二羧酸，诸如邻苯二羧酸、间苯二羧酸和对苯二羧酸，以及苯四羧酸，诸如1，2，4，5-苯四酸。邻苯二羧酸是优先选择的。含这一部分的极性氮化合物叙述于US-A-4,211,534和EP-A-272,889中。
非环部分的实例是其中的酸是长链烷基或亚烷基取代的二羧酸，诸如琥珀酸，例如US-A-4,147,520中所述。
非环部分的其它实例是其中的酸是一含氮的酸，诸如乙二胺四乙酸和次氮基乙酸，如DE-A-3,916,366(相当于CA-A-2,017,126)(BASF)中所述。
进一步的实例是二烷基螺二内酯与胺反应得到的部分，如EP-A-413,279(Hoechst)中所述。
(ii)EP-A-0,261,957叙述的本发明的极性氮化合物的通式如下：
Figure C9519350300131
式中，-Y-R2是SO3 (-)(+)NR3R2，-SO3 (-)(+)HNR2 3R2，-SO3 (-)(+)H2NR3R2，-SO3 (-)(+)H3NR2，-SO2NR3R2或-SO3R2；-X-R1是-Y-R2或-CONR3R1，-CO2 (-)(+)NR3 3R1，-CO2 (-)(+)HNR2 3R1，-R4-COOR1，-NR3COR1，-R4OR1，-R4OCOR1，-R4，R1，-N(COR3)R1或Z(-)(+)NR3 3R1；-Z(-)是SO3 (-)或-CO2 (-)；R1和R2是主链至少含10个碳原子的烷基、烷氧基烷基或多烷氧基烷基；R3是烃基，各R3可以相同或不同；R4是C1-C5亚烷基或不存在；以及在式中碳-碳(C-C)键是a)烯属不饱和键(当A和B是烷基、链烯基或取代烃基时)，或是b)环结构的一部分，环结构可以是芳族的、多核芳族或环-脂族的。X-R1和Y-R2之间最好至少含3个烷基、烷氧基烷基或多烷氧基烷基。
可以使用多组分添加剂体系，添加剂的比率决定于需要处理的燃料。
iii)EP-A-0,316,108所述的(a)、(b)、(c)或(d)的胺盐或二胺盐；(a)磺基琥珀酸，(b)磺基琥珀酸酯或二酯，(c)磺基琥珀酸酰胺或二酰胺，(d)磺基琥珀酸酯-酰胺。
iv)WO9,304,148所述的由一环体系组成或包括一环体系的化合物，在环体系上至少带有两个通式(1)的取代基
                   -A-NR1R2    (1)式中A是一脂肪烃基，它可被一个或多个杂原子任选地隔断，而且是直链或有支链的；R1和R2是相同或不同的并分别是一可以被一个或多个杂原子任选地隔断的含有9-40个碳原子的烃基。取代基是相同或不同的，并且化合物还可以是其盐的形式。
A最好具有1-20个碳原子，优选亚甲基或多亚甲基。
在本发明(式1)中构成R1和R2的各烃基可以是例如烷基或亚烷基或单烷氧基烷基或多烷氧基烷基。每一烃基优选是直链烷基。每一烃基的碳原子数最好是16-40，更优选16-24。
再者，环体系仅用两个通式(1)的取代基取代并且A是亚甲基是优先选择的。
此类化合物的盐的实例是乙酸盐或盐酸盐。
该化合物可以方便地用还原相应的酰胺的方法来制取，酰胺可将一仲胺与适合的酰基氯反应制备，WO9,407,842叙述了此类中的其它化合物(曼尼期碱)。
(v)长链伯胺或仲胺与含羧酸的聚合物的缩合产物
具体实例包括诸如在GB-A-2,121,807、FR-A-2,592,387和DE-A-3,941,561中叙述的聚合物；和在诸如US-A-4,639,256中叙述的telemer酸的酯和烷醇胺；以及US-A-4,631,071中叙述的含支化羧酸酯的胺、环氧化物和一元羧酸聚酯的反应产物。
EP-0,283,292叙述了含酰胺的聚合物；EP-0,343,981叙述了含胺盐的聚合物。
须注意，极性氮化合物可含有其它的官能团，诸如酯官能团。
(D)烃聚合物
适合的烃聚合物实例是具有下述通式的聚合物
Figure C9519350300151
式中T＝H或R21，其中
R21＝C1-C40烃基；
U＝H、T或芳基；
v和w代表摩尔份数，v是在1.0-0.0范围内，w是在0.0-1.0范围。
烃聚合物的制取可以直接从单烯属不饱和单体或间接地用多不饱和单体(例如异戊二烯和丁二烯)得到的聚合物进行氢化。
烃聚合物的实例公开于WO91/11488中。
优选的共聚物是数均分子量至少为30,000的乙烯-α-烯烃共聚物。α-烯最好是至多28个碳原子。这种烯烃的实例是丙烯、1-丁烯、异丁烯、正辛烯-1、异辛烯-1、正癸烯-1、正十二碳烯-1、共聚物也可含少量的，例如可达10％(重量)的其它可共聚单体，例如除α-烯烃外的烯烃和非共轭二烯。优选的共聚物是乙烯-丙烯共聚物。
如上已指出，乙烯-α-烯烃共聚物的数均分子量最好是至少30,000，相对于聚苯乙烯标准物以凝胶渗透色谱法(GPC)测定，有利的是至少60,000，并优选至少80,000。在功能上分子量无上限，但当分子量高于约150,000时，由于增高的粘度使混合产生困难，优选的分子量范围是从60,000和80,000至120,000。
共聚物的乙烯摩尔含量在50-85％之间是有利的，更有利的乙烯含量是在57-80％的范围内；优选的范围是58-73％，更优选62-71％，最优选65-70％。
优选的乙烯-α-烯烃共聚物是乙烯摩尔含量为62-71％、数均分子量范围为60,000-120,000的乙烯-丙烯共聚物。特别优选的共聚物是乙烯摩尔含量为62-71％、分子量为80,000-100,000的乙烯-丙烯共聚物。
共聚物的制备可用本技术领域中任何的已知方法，例如用齐格勒型催化剂。聚合物应是基本上无定型的，因为高度结晶的聚合物在低温时是相对不溶于燃料油的。
其它适合的烃聚合物包括低分子量的乙烯-α-烯烃共聚物，其数均分子量至多为7,500是有利的，有利的范围是1,000-6,000，优选2,000-5,000，以气相渗透压测定法测定。适合的α-烯烃是上述的α-烯烃或苯乙烯，丙烯仍然是优选的。乙烯的摩尔含量为60-77％是有利的，虽然对乙烯-丙烯共聚物来说采用达86％摩尔的乙烯是有利的。
(E)线型化合物，例如聚氧化亚烷基化合物
这类化合物包括这样的化合物，其中至少一个有10-30个碳原子的基本上是线型的烷基通过一任选的可以是支化的连接基团连结到一非聚合物残基诸如有机残基上，以提供至少一个线型原子链，该链包括所说烷基的碳原子和一个或多个非终端氧、硫和/或氮原子。连接基团可以是聚合的。
“基本上是线型”意指烷基最好是直链，但可以使用诸如以单个甲基分枝形式的小程度支化的直链烷基。
当线型链可包括多于一个所说烷基的碳原子时，该化合物最好至少有两个所说的烷基。当化合物至少有三个所说的烷基时，可有多于一个的这种线型链，这些链可重叠。线型链或多个链可在化合物的任意两个这种烷基之间提供一部分连接基团。
氧原子或多个氧原子(如果存在的话)最好是直接置于链中的碳原子之间，并且可以被提供于连接基团(如果存在的话)之中以单-或多-氧化亚烷基的形式存在，所说的氧化亚烷基最好有2-4个碳原子，其例是氧化亚乙基和氧化亚丙基。
如已指出，链或多个链中包括了碳、氧、硫和/或氮原子。
化合物可以是酯，其烷基连接到化合物的其余部分，如-O-CO正构烷基或-CO-O正构烷基。前者是烷基来源于酸，化合物的其余部分来源于多元醇；后者是烷基来源于醇，化合物的其余部分来源于多元酸。化合物也可以是烷基连结于化合物的其余部分的醚，如-O-正构烷基。化合物可同时是酯和醚，或者可含不同的酯基。
实例包括聚氧化亚烷基酯、醚、酯/醚和它们的混合物，特别是那些含有至少一个、优选至少两个C10-C30线型烷基和分子量达5000、优选2,000-5,000的聚氧化亚烷基二醇基的化合物，所说聚氧化亚烷基二醇中的亚烷基含1-4个碳原子，如EP-A-61,895和US4,491,455中所述。
可以使用的优选的酯、醚、酯/醚可包括这样的化合物，其中一个或多个式-OR25基(诸如2，3或4个基)是结合在残基E上的，E可代表例如A(亚烷基)q，其中A代表C或N或不存在，q代表1-4的整数，亚烷基具有1-4个碳原子，A(亚烷基)q是例如N(CH2CH2)3、C(CH2)4、或(CH2)2；R25可独立地为
(a)正构烷基
(b)正构烷基-CO-
(c)正构烷基-OCO-(CH2)n-
(d)正构烷基-OCO-(CH2)nCO-n是例如1-34，烷基是线型的并含10-30个碳原子。例如它们可用式R23OBOR24代表，R23和R24的定义如上述R25，B代表二醇的聚亚烷基链段，其中的亚烷基具有1-4个碳原子，例如基本上是线型的聚氧化亚甲基、聚氧化亚乙基或聚氧化三亚甲基的部分，具有低级烷基侧链的某种程度的支化(诸如聚氧化亚丙基二醇中)是可以容许的，但优选的二醇应基本上是线型的。
适合的二醇一般基本上是线型聚乙二醇(PEG)和聚丙二醇(PPG)，其分子量约为100-5,000，优选约200-2,000。酯类是优选的，并且含10-30个碳原子的脂肪酸用于与二醇反应以形成酯添加剂，使用C18-C24脂肪酸是优选的，特别是山萮酸。酯类也可以用聚乙氧化的脂肪酸或聚乙氧化的醇经酯化来制备。
当石油基组分是窄沸点馏分，当少量的单醚和单酯(它们常在制造过程中形成)也可能存在时，聚氧化亚烷基二酯、二醚、醚/酯和它们的混合物是适合作为添加剂的，优选的是二酯。存在主要量的二烷基化合物对于活性是重要的。特别是聚乙二醇、聚丙二醇或聚乙二醇/聚丙二醇混合物的硬脂酸或山萮酸二酯是优先选择的。
这一总类的其它化合物的实例有在日本专利公开No2-51477和3-34790和EP-A-117,108和EP-A-326,356中叙述的化合物，及在诸如EP-A-356,256中叙述的环状酯化的乙氧基化物。
有效地使用选自一个或多个概括于上的不同类型的两种或多种流动改进剂是在本发明的范围之内。
流动改进剂的有利使用比例是在0.001-1％，例如0.01-1％，有利的是0.05-0.5％，优选0.075-0.25％(重量)，以燃料重为基础计算。
流动改进剂也可以与一种或多种其它本技术领域中已知的助添加剂结合使用，例如下述的添加剂：洗涤剂、抗氧化剂、腐蚀抑制剂、去浊雾剂、破乳剂、抗泡剂、十六烷值增进剂、助溶剂、包装相容剂和其它已知的润滑性添加剂。
实施例
下面以实施例对本发明进行说明。
在实施例中，HFRR试验在下列的条件下进行，磨耗自始至终是在60℃下测定的。
    负荷                   2N
    行程                   1mm(0.5mm振幅)
    频率                   50Hz
    温度                   60℃
    冶金                   BALL ANSI 52 100(淬火轴承
                           工具钢)645HV30
                           FLAT ANSI 52 100(轴承工具
                           钢)180 HV30
    时间                   75分钟
试验完后测定磨耗。
测试了燃料I、II和III中的各种添加剂。
燃料I是瑞典商品供应的一级柴油机燃料。燃料特性如下：
    比重             0.8088
    硫               0.001重量％
    馏分，℃   IBP   186
               10％  203
               50％  225
               95％  273
净燃料的HFRR试验结果如下：
         磨耗，μm
               701(两次试验平均值)
燃料II的特性如下：
    比重             0.8184
    硫               0.03重量％
    馏分，℃   IBP   156
               10％  192
               20％    202
               50％    233
               90％    303
               95％    326
               FBP     355
净燃料的HFRR试验结果如下：
          磨耗，μm
          575(两次试验平均值)
燃料III的特性如下：
    比重             0.8204
    硫               0.03重量％
    馏分，℃   IBP   161
               10％  197
               20％  208
               50％  239
               90％  301
               95％  314
               FBP   336
净燃料的HFRR试验结果为585μm(两次试验平均值)。
在编号的实施例中使用了各种不同的添加剂，其结果和处理率(基于燃料重量的以ppm表示的活性组分重量)示于表中。
                    所用的添加剂
实施例1
极性氮化合物2-N’，N’-二烷基酰氨基苯甲酸的N，N-二烷基铵盐(1摩尔邻苯二甲酸酐与2摩尔二(氢化牛脂)胺的反应产物)。
实施例2
BASF商品供应的冷流改进剂“Keroflux 3243”，相信含有乙二胺四乙酸与二(氢化牛脂)胺(摩尔比1∶4)的反应产物与乙烯-丙酸乙烯酯共聚物的混合物。
实施例3
Hoechst商品供应的冷流改进剂“Dodiflow V/4237”，相信含有链烯基螺二内酯与1摩尔二(氢化牛脂)胺和1摩尔(氢化牛脂)胺的反应产物。
实施例4
乙烯-乙酸乙烯酯共聚物，其乙酸乙烯酯含量为13.5％，Mn为5000(凝胶渗透色谱法测定)。
实施例5
乙烯-乙酸乙烯酯共聚物，其乙酸乙烯酯含量为36.5重量％，Mn3000(GPC)。
实施例6
乙烯-乙酸乙烯酯共聚物，乙酸乙烯酯含量29重量％，Mn 3400(GPC)。
实施例7
乙烯-乙酸乙烯酯共聚物，乙酸乙烯酯含量28重量％，Mn 18000(GPC)。
实施例8
实施例4/5添加剂混合物(1∶3重量/重量)。
实施例9
乙烯-丙酸乙烯酯共聚物，38重量％丙酸乙烯酯，Mn约5200(GPC)。
实施例10
富马酸十二烷酯-乙酸乙烯酯(摩尔比1∶1)梳形聚合物。
实施例11
衣康酸十六烷酯梳形聚合物。
实施例12
衣康酸十四烷酯梳形聚合物。
实施例13
富马酸十二烷酯-苯乙烯(摩尔比1∶1)梳形聚合物。
实施例14
乙二胺四乙酸与二(氢化牛脂)胺(摩尔比1∶4)的反应产物。
实施例15
次氮基乙酸与二(氢化牛脂)胺(摩尔比1∶3)的反应产物。
实施例16
1摩尔链烯基螺二内酯与1摩尔二(氢化牛脂)胺和1摩尔(氢化牛脂)胺的反应产物。
                   结果
                  (燃料I)
实施例       处理率(ppm)      磨耗(μm)
  1            1334             254
  2            1000             246
  3            920              313
  4            452              328
  5            1456             301
  6            1200             486
  7            500              274
  8            904              290
  9            1000             471
  10           800              226
  11           1760             192
  12           1760             240
  13           980              311
净燃料                          701
结果显示，所有的流动改进剂都提高了润滑性(磨耗测定减小)，富马酸十二烷酯-乙酸乙烯酯梳形共聚物甚致在低处理率情况下是最突出的。
                    燃料II
    实施例和(处理率，ppm)      磨耗(μm)(i)    1(60)                          480
                   4(450)           535
     1(60)；       4(495)           340  (ii)         1(60)                          480
                       9(750)             565
           1(60)；     9(700)             305(iii)        1(60)                          480
                       2(165)             420
           1(60)；     2(165)             300(iv)         1(60)                          480
                       2(150)     495
           1(60)；     2(150)     315净燃料                                        575
结果显示，所有的流动改进剂均提高了润滑性，并且某些流动改进剂的组合对改进润滑性起着协同作用(磨耗测定减小)。
                       燃料III
实施例和(处理率，ppm)             磨耗(μm)
        14(300)                       340
        15(300)                       380
        16(300)                       405
        1(300)                        385
        1(144)；4(36)                 385
           净燃料                     585
结果显示，受试的极性氮化合物提高了润滑性，并且少量实施例4的乙烯-乙酸乙烯酯提高了实施例1的极性氮化合物的润滑性。

Claims (47)

1.使用包含带有一个或多个式＝NR13取代基的油溶性极性氮化合物与乙烯-不饱和酯共聚物流动改进剂结合的冷流改进剂以提高硫含量至多为0.05％(重量)的燃料油组合物的润滑性，以便组合物的润滑性是使产生的磨痕直径至多为450μm，在60℃用HFRR试验测定，在上式中R13代表含8-40个碳原子的烃基，该取代基可以是其阳离子的形式。
2.权利要求1的应用，其中R13代表含12-24个碳原子的脂肪族烃基。
3.权利要求2的应用，其中烃基是直链烷基。
4.权利要求1的应用，其中＝NR13是式-NR13R14，式中R14代表氢或R13，以R13和R14可以相同或不相同为条件。
5.权利要求1的应用，其中极性氮化合物是蜡晶体生长抑制剂。
6.权利要求1的应用，其中取代基是氨基。
7.权利要求6的应用，其中氨基取代基是C12-40烷基伯，仲，叔或季氨基取代基。
8.权利要求1的应用，其中极性氮化合物是单或多羧酸的胺盐和/或酰胺。
9.权利要求8的应用，其中酸部分是环状的。
10.权利要求8的应用，其中羧酸是苯二羧酸或苯四羧酸。
11.权利要求8的应用，其中酸部分是非环状的。
12.权利要求11的应用，其中酸部分是长链烷基或亚烷基取代的二羧酸。
13.权利要求11的应用，其中酸部分是含氮酸。
14.权利要求13的应用，其中酸是乙二胺四乙酸或次氮基乙酸。
15.权利要求14的应用，其中极性氮化合物是乙二胺四乙酸与二(氢化牛脂)胺以摩尔比1∶4的反应产物。
16.权利要求1的应用，其中冷流改进剂包括两种或多种所说的极性氮化合物。
17.权利要求1的应用，其中共聚物是一除得自乙烯的单元外还含有式-CR1R2-CHR3-单元的共聚物，-CR1R2-CHR3-中的R1代表氢或甲基，R2代表COOR4，其中R4代表1-9个碳原子的烷基，为直链烷基，或当含3个或更多个的碳原子，则是支化的烷基；或R2代表OOCR5，R5代表R4或H，以及R3代表H或COOR4。
18.权利要求1的应用，其中乙烯-不饱和酯共聚物是乙烯-乙烯酯共聚物。
19.权利要求18的应用，其中共聚物是乙烯/乙酸乙烯酯，乙烯/丙酸乙烯酯，乙烯/己酸乙烯酯或乙烯/辛酸乙烯酯共聚物。
20.权利要求1的应用，其中使用两种共聚物的混合物。
21.权利要求1的应用，其中基于燃料重量计，存在0.001-1％(重量)的冷流改进剂。
22.前述任一项权利要求的应用，其中燃料油是中馏分燃料油。
23.权利要求1-21的应用，其中润滑性是使产生的磨痕直径至多为380μm，在60℃用HFRR试验测定。
24.一种制造有增强的润滑性的石油基燃料油的方法，该方法包括精炼原油以生产低硫含量的燃料油，然后将包括一带有一个或多个式＝NR13取代基的油溶性极性氮化合物和乙烯-不饱和酯共聚物冷流改进剂结合的流动改进剂与精炼产品混合以提供一种燃料油组合物，式中R13代表含8-40个碳原子的烃基，该取代基可以是其阳离子的形式，该组合物的硫含量至多为0.05％(重量)，并具有使磨痕直径至多为450μm的润滑性，在60℃用HFRR试验测定。
25.一种组合物，该组合物包括主要部分的石油基燃料油和少部分包括一带有一个或多个式＝NR13取代基的油溶性极性氮化合物与乙烯-不饱和酯共聚物流动改进剂结合的冷流改进剂，式中R13代表含8-40个碳原子的烃基，该取代基或一个或多个该取代基可以是其阳离子的形式；组合物的硫含量至多为0.05％(重量)，润滑性是使产生的磨痕直径至多为450μm，在60℃用HFRR试验测定。
26.权利要求25的组合物，其中R13代表含12-24个碳原子的脂肪族烃基。
27.权利要求26的组合物，其中烃基是直链烷基。
28.权利要求25的组合物，其中＝NR13是式-NR13R14，式中R14代表氢或R13，以R23和R14可以相同或不相同为条件。
29.权利要求25的组合物，其中极性氮化合物是蜡晶体生长抑制剂。
30.权利要求25的组合物，其中取代基是氨基。
31.权利要求30的组合物，其中氨基取代基是C12-40烷基伯，仲，叔或季氨基取代基.
32.权利要求25的组合物，其中极性氮化合物是单或多羧酸的胺盐和/或酰胺。
33.权利要求32的组合物，其中酸部分是环状的。
34.权利要求32的组合物，其中羧酸是苯二羧酸或苯四羧酸。
35.权利要求32的组合物，其中酸部分是非环状的。
36.权利要求35的组合物，其中酸部分是长链烷基或亚烷基取代的二羧酸。
37.权利要求35的组合物，其中酸部分是含氮酸。
38.权利要求37的组合物，其中酸是乙二胺四乙酸或次氮基乙酸。
39.权利要求38的组合物，其中极性氮化合物是乙二胺四乙酸与二(氢化牛脂)胺以摩尔比1∶4的反应产物。
40.权利要求25的组合物，其中冷流改进剂包括两种或多种所说的极性氮化合物。
41.权利要求25的组合物，其中乙烯-不饱和酯共聚物是一除得自乙烯的单元外还含有式-CR1R2-CHR3-单元的共聚物，-CR1R2-CHR3-中的R1代表氢或甲基，R2代表COOR4，其中R4代表1-9个碳原子的烷基，为直链烷基，或当含3个或更多个的碳原子，则是支化的烷基，或R2代表OOCR5，R5代表R4或H，以及R3代表H或COOR4。
42.权利要求25的组合物，其中乙烯-不饱和酯共聚物是乙烯-乙烯酯共聚物。
43.权利要求42的组合物，其中共聚物是乙烯/乙酸乙烯酯，乙烯/丙酸乙烯酯，乙烯/己酸乙烯酯或乙烯/辛酸乙烯酯共聚物。
44.权利要求25的组合物，其中使用两种共聚物的混合物。
45.权利要求25的组合物，其中基于燃料重量计，存在0.001-1％(重量)的冷流改进剂。
46.权利要求25-45任一项的组合物，其中燃料油是中馏分燃料油。
47.权利要求25-45任一项的组合物，其中润滑性是使产生的磨痕直径至多为380μm，在60℃用HFRR试验测定。
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