CN102174340B - 润滑组合物所用的季铵盐清洁剂 - Google Patents

润滑组合物所用的季铵盐清洁剂 Download PDF

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CN102174340B
CN102174340B CN2011100763269A CN201110076326A CN102174340B CN 102174340 B CN102174340 B CN 102174340B CN 2011100763269 A CN2011100763269 A CN 2011100763269A CN 201110076326 A CN201110076326 A CN 201110076326A CN 102174340 B CN102174340 B CN 102174340B
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W·巴顿
M·C·戴维斯
D·J·莫尔顿
P·R·斯蒂文森
D·德福特
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Abstract

季铵盐清洁剂，其由下述的反应产物制成：(a)烃基取代的酰化剂和含有能够与上述的酰化剂缩合的氧或氮原子且另外含有叔胺基的化合物的反应；和(b)适于将叔胺基转变成季氮的季铵化剂，上述季铵盐清洁剂的用途，用于燃料组合物以减少进气阀沉积物。

Description

润滑组合物所用的季铵盐清洁剂
相关申请的引用
本申请是申请号为200680021682.8、国际申请号为PCT/US2006/022925、申请日为2006年6月13日的中国发明专利申请的分案申请。本申请主张来自申请号60/691115的优先权。
发明背景
本发明的组合物涉及季铵盐清洁剂以及将这种季铵盐清洁剂用于燃料组合物以减少进气阀沉积物和移走或清除在进气阀上现有的沉积物。
众所周知的是液态燃料含有在发动机运行过程中可以分解并形成沉积物的成分。这些沉积物可导致燃料的不完全燃烧，从而导致更高的排放和更差的燃料经济性。燃料添加剂，例如清洁剂，是众所周知的在液态燃料中用于帮助控制或最小化沉积物形成的添加剂。随着发动机动力学和机械学的持续发展，对燃料的要求也必须发展以跟上这些发动机的发展。例如，当今的发动机具有容忍度更小的喷油器系统并在更高压力下运行以提高燃料喷雾到压缩室或燃烧室里。在这些新型发动机中，防止沉积和减少沉积对优化当今发动机的运行已经成为关键。在燃料添加剂技术上的发展，例如清洁剂，已经能够让燃料跟上这些发动机的发展。因此，需要清洁剂能够提供在液态燃料中可以接受的性能以提升当今发动机的优化运行。
US5000792公开了通过将2份的多羟基羧酸与1份二亚烷基三胺反应，得到聚酯胺清洁剂。
US4171959公开了一个含有琥珀酰亚胺的季铵盐的发动机燃料组合物。季铵盐有卤化物，磺酸盐或羧酸盐的反离子。
US4338206和US4326973公开了含有琥珀酰亚胺的季铵盐的发动机燃料组合物，其中铵离子是杂环芳香族的(吡啶
Figure GDA0000146006430000021
离子)。
US4108858公开了含有添加有吡啶
Figure GDA0000146006430000022
盐、Mw为800到1400的C2到C4聚烯烃的燃料或润滑油组合物。
US5254138公开了一种含有聚烷基琥珀酸酐与多氨基羟基烷基季铵盐的反应产物的燃料组合物。
US4056531公开了含有被连接到三亚乙基二胺、Mw为350到3000的烃的季铵盐的润滑油或燃料。季铵盐的反离子选自：卤化物、磷酸盐、烷基磷酸盐、二烷基磷酸盐、硼酸盐、烷基硼酸盐、亚硝酸盐、硝酸盐、碳酸盐、碳酸氢盐、链烷酸盐以及O，O-二烷基二硫代磷酸盐。
US4248719公开了含有琥珀酰亚的季铵盐和单羧酸酯的燃料或润滑油。US4248719没有教导、建议或另外公开了低硫燃料，存在流化剂等。实施例1教导了使用有DMAPA的聚异丁烯琥珀酰亚胺作为胺。然后将琥珀酰亚胺与水杨酸盐反应。
US4253980和US4306070公开了含酯-内酯的季铵盐的燃料组合物。
US3778371公开了含Mw为350到3000的烃的季铵盐的润滑油或燃料；而且季氮的其余基团选自：C1到C20烷基、C2到C8羟基烷基、C2到C20烯基或环烷基。
由此，本发明促进了发动机运行优化，也就是说，提高了燃料经济性，更好的车辆操纵性，减少排放以及通过减少、最小化和控制沉积形成而需要更少的发动机维护。
发明综述
本发明另外还提供一种为内燃机提供燃料的方法，包含：
A.供给所述发动机：
i.在室温下呈液态的燃料；以及
ii.含下述的反应的产物的季铵盐：
(a)烃基取代的酰化剂和含有能够与上述的酰化剂缩合的氧或氮原子且另外含有叔胺基的化合物的反应；和
(b)适于将叔胺基转变成季氮的季铵化剂
其中季铵化剂选自：硫酸二烷基酯、苄基卤化物、烃基取代的碳酸酯；烃基环氧化物与酸的组合或其混合物。
本发明另外还提供含有季铵盐的组合物，其含有下述的反应产物：
a.烃基取代的酰化剂和含有能够与上述的酰化剂缩合的氧或氮原子且另外含有叔胺基的化合物的反应；和
b.适于将叔胺基转变成季氮的季铵化剂
其中季铵化剂选自：硫酸二烷基酯、苄基卤化物、烃基取代的碳酸酯；烃基环氧化物与酸的组合或其混合物。
发明详述
下面将经由非限制性说明对各种优选的特征和实现方案进行阐述。
发明领域
本发明涉及季铵盐，包含季铵盐的燃料组合物，以及用该燃料组合物运行内燃机的方法。本发明的组合物和方法可以最小化、减少和控制发动机中沉积的形成，这可以降低燃料消耗，促进操纵性，车辆维护，以及减少排放，从而能够优化发动机运行。
燃料
本发明的组合物可含有一种在室温下呈液态的燃料并有用于发动机提供燃料。燃料在环境条件下呈液态，例如，室温(20到30℃)。燃料可以是烃类燃料，非烃类燃料，或其混合物。烃类燃料可以是石油馏出物，从而包括由ASTM规范D4814所定义的汽油或由ASTM规范D975所定义的柴油。在本发明的一个实现方案中，燃料是汽油，而在另一个实现方案中，燃料是加铅汽油，或不加铅汽油。在本发明的另一个实现方案中，燃料是柴油。烃类燃料可以是通过气液过程所制得的烃，包括例如通过例如Fischer Tropsch过程的过程制得的烃。非烃类燃料可以是含氧组合物，通常被称作含氧物(oxygenate)，包括醇，醚，酮，羧酸酯，硝基烷，或其混合物。非烃类燃料可包括例如甲醇，乙醇，甲基叔丁基醚，甲基乙基酮，从植物和动物得到的酯交换油和/或脂肪如油菜籽甲基酯和大豆甲基酯，和硝基甲烷。烃类和非烃类燃料的混合物可包括例如汽油和甲醇和/或乙醇，柴油和乙醇，以及柴油和酯交换植物油如油菜籽甲基酯。在本发明的一个实现方案中，液态燃料是水在烃类燃料，非烃类燃料，或其混合物中的乳状液。在本发明的一些实现方案中，按重量计，燃料中的硫含量为5000ppm或更小，1000ppm或更小，300ppm或更小，200ppm或更小，30ppm或更小，或10ppm或更小。在另一个实现方案中，按重量计，燃料中的含硫量为1到100ppm。在一个实现方案中，燃料含有约0ppm到约1000ppm，约0ppm到约500ppm，约0ppm到约100ppm，约0ppm到约50ppm，约0ppm到约25ppm，约0ppm到约10ppm，或约0ppm到5ppm的碱金属，碱土金属，过渡金属或其混合物。在另一个实现方案中，燃料含有约1重量ppm到10重量ppm的碱金属，碱土金属，过渡金属或其混合物。本领域众所周知的是含有碱金属，碱土金属，过渡金属或其混合物的燃料具有更大倾向性形成沉积并因而淤塞或堵上共轨喷射器(common railinjector)。在燃料组合物中本发明的燃料是以主要量存在的，其量一般大于50重量％，而在另一个实现方案中，其量大于90重量％，大于95重量％，大于99.5重量％，或大于99.8重量％。
季铵盐
本发明的组合物含有季铵盐，其含有下述的反应的产物：(a)烃基取代的酰化剂和含有能够与上述的酰化剂缩合的氧或氮原子且另外含有叔胺基的化合物的反应；和(b)适于将叔胺基转变成季氮的季铵化剂，其中季铵化剂选自：硫酸二烷基酯、苄基卤化物、烃基取代的碳酸酯；烃基环氧化物与酸的组合或其混合物。
季铵盐的例子及其制备方法在下面的专利中有叙述，由此将其结合于此作为参考，US4253980，US3778371，US4171959，US4326973，US4338206和US5254138。
烃基取代的酰化剂
本发明的烃基取代的酰化剂是这样的反应产物，即长链烃，一般是被单不饱和羧酸反应物取代的聚烯烃，所述单不饱和羧酸反应物例如(i)α，β-单不饱和C4到C10二羧酸如富马酸，衣康酸，马来酸；(ii)(i)的衍生物如(i)的C1到C5醇衍生单-或二酯或酸酐；(iii)α，β-单不饱和C3到C10单羧酸如丙烯酸和甲基丙烯酸；或(iv)(iii)的衍生物如(iii)的C1到C5醇衍生酯，与由下式所表示的具有烯键的任何化合物的反应产物
(R1)(R2)C＝C(R6)(CH(R7)(R8))            (I)
其中R1和R2各自独自为氢或基于烃的的基团。R6，R7和R8各自独自为氢或基于烃的的基团；优选至少一个是含有至少20个碳原子的基于烃的的基团。
与单不饱和羧酸反应的烯烃聚合物可包括主要摩尔量的C2到C20，举例来说C2到C5单烯烃。这样的烯烃包括乙烯，丙烯，丁烯，异丁烯，戊烯，1-辛烯，或苯乙烯。聚合物可以是均聚物如聚异丁烯，以及两种或多种这些烯烃的共聚物如，乙烯和丙烯；丁烯和异丁烯；丙烯和异丁烯的共聚物。其他共聚物包括那些其中次要摩尔量的共聚物单体，例如，1到10摩尔％是C4到C18二烯的共聚物，例如异丁烯和丁二烯的共聚物；或乙烯，丙烯和1，4-己二烯的共聚物。
在一个实现方案中，至少一个(I)式的R是源自于聚丁烯，也就是说，C4烯烃的聚合物，包括1-丁烯，2-丁烯和异丁烯。C4聚合物可包括聚异丁烯。在另一个实现方案中，至少一个(I)式的R是源自于乙烯-α烯烃聚合物，包括乙烯-丙烯-二烯聚合物。乙烯-α烯烃共聚物和乙烯-低级烯烃-二烯三聚物在许多的专利文献中有叙述，包括欧洲专利文献EP 0279863和下面的美国专利：3598738、4026809、4032700、4137185、4156061、4320019、4357250、4658078、4668834、4937299、5324800，由于其中关于基于乙烯的聚合物的公开，将其每一个结合于此作为参考。
在另一个实现方案中，(I)式的烯键主要是由下式所表示的亚乙烯基：
Figure GDA0000146006430000061
其中R是烃基
Figure GDA0000146006430000062
其中R是烃基。
在一个实现方案中，(I)式的亚乙烯基物质可含有至少约30mol％亚乙烯基，至少约50mol％亚乙烯基，或至少约70mol％亚乙烯基。这样的物质和其制备方法在美国专利5071919、5137978、5137980、5286823、5408018、6562913、6683138、7037999和美国公布20040176552A1、20050137363和20060079652A1中有叙述，将其特别结合于此作为参考，这样的产品有市售，由BASF所提供的商品和由TexasPetroChemical LP所提供的TCP 1105TM和TPC595TM。
从单不饱和羧酸反应物与(I)式化合物的反应来制备烃基取代的酰化剂的方法在本领域是众所周知的并在下面的专利中公开：美国专利3361673和3401118，导致烯热裂解反应进行；美国专利3087436、3172892、3272746、3215707、3231587、3912764、4110349、4234435、6077909、6165235并由此将其结合于此作为参考。
在另一个实现方案中，烃基取代的酰化剂可以从由下式所表示的至少一个羧基反应物与任何含有如(I)式所表示的烯键的化合物的反应来制得：
(R3C(O)(R4)nC(O))R5      (IV)
和
其中R3、R5和R9各自独自为H或烃基，R4是二价亚烃基且n是0或1。化合物及其制备方法在美国专利5739356、5777142、5786490、5856524、6020500和6114547中公开。
在又另一个实现方案中，烃基取代的酰化剂可以从由(I)式与(IV)或(V)式所表示的任何化合物，在存在至少一个醛或酮的情况下进行反应来制得。适合的醛包括甲醇、乙醛、丙醛、丁醛、异丁醛、戊醛、己醛、庚醛、辛醛、苯甲醛和高级醛。其他醛，例如二醛，尤其是乙二醛，也是有用的，尽管一般优选单醛。在一个实现方案中，醛是甲醛，其可以是以俗称为福尔马林的水溶液形式来提供，但通常是以聚合态的形式使用，如多聚甲醛，其是甲醛的活性等价物或甲醛来源。其他活性等价物包括水合物或环状三聚物。适合的酮包括丙酮，丁酮，甲基乙基酮和其他酮。优选两个烃基之一是甲基。两或多个醛和/或酮的混合物也是有用的。
化合物及其制备方法在美国专利5840920、6147036和6207839中公开。
在另一个实现方案中，烃基取代的酰化剂可包括，亚甲基双酚链烷酸化合物，下式(i)的芳香化合物：
Rm-Ar-Zc                 (VI)
其中R独自为烃基，Ar是有5到约30个碳原子和可选的0到3个取代基如氨基、羟基或烷基聚氧烷基、硝基、氨基烷基、羧基或两个或多个所述可选取代基的组合的芳基，Z独自是OH，低级烷氧基，(OR10)bOR11，或O-其中R10独自为二价烃基，R11是氢或烃基且b是从1到约30的数字，c是从1到约3的数字，m是0或从1到约6的整数，条件是m不能超过相应的Ar可取代的价数，和(ii)至少一种羧基反应物，如上述的(IV)和(V)式化合物，的缩合产物。在一个实现方案中，芳基上的至少一个烃基衍生自聚丁烯。在一个实现方案中，烃基来源是上述的在存在Lewis酸催化剂如三氯化铝或三氟化硼下异丁烯聚合所得到的聚丁烯。
化合物及其制备方法在美国专利3954808、5336278、5458793、5620949、5827805和6001781中公开。
在另一个实现方案中，在任选存在酸性催化剂如有机磺酸，杂多酸和无机酸的情形下，(i)与(ii)在存在至少一种醛或酮下进行反应。用于本实现方案的醛或酮反应物与上述的那些相同。羟基芳香化合物∶羧基反应物∶醛或酮的比例可以是2∶(0.1到1.5)∶(1.9到0.5)。在一个实现方案中，该比例是2∶(0.8到1.1)∶(1.2到0.9)。进料到反应混合物的这些物质一般接近这些比例，尽管为了补偿一种成分或另一种成分的更高或更低的反应性需要修正，以便获得具有所需要的单体比例的反应产物。这样的修正对熟悉该领域的人员来说是显而易见的。尽管三种反应物能同时缩合成产物，也可以按顺序实施反应，由此首先将羟基芳香化合物与羧基反应物，随后与醛或酮反应，反之亦然。化合物及其制备方法在美国专利5620949中公开。
烃基取代的酰化剂的其他制备方法可在下面的文献中找到：美国专利5912213、5851966和5885944，由此将其结合于此作为参考。
具有氮或氧原子的化合物
本发明的组合物具有含有能够和酰化剂缩合的氧或氮原子并且具有季胺基的化合物。
在一个实现方案中，能够和酰化剂缩合并且具有季胺基的含氧或氮原子的化合物可由下式表示：
Figure GDA0000146006430000081
其中X是有约1到约4个碳原子的亚烷基；R2，R3和R4是烃基。
Figure GDA0000146006430000091
其中X是有约1到约4个碳原子的亚烷基；R3和R4是烃基。
能够和酰化剂缩合并且具有季胺基的含氧或氮的化合物的例子包括但不限于：N-甲基-1，3-二氨基丙烷、二甲基氨基丙胺、N，N-二甲基-氨基丙胺、N，N-二乙基-氨基丙胺、N，N-二甲基-氨基乙胺、乙二胺、1，2-丙二胺、1，3-丙二胺、同分异构的丁二胺、戊二胺、己二胺、庚二胺、二亚乙基三胺、二亚丙基三胺、二亚丁基三胺、三亚乙基四胺、四亚乙基五胺、五亚乙基六胺、六亚甲基四胺、和双(六亚甲基)三胺、二氨基苯、二氨基吡啶或其混合物。能够和酰化剂缩合并且具有季胺基的含氧或氮的化合物另外可包括氨基烷基取代的杂环化合物如1-(3-氨基丙基)咪唑和4-(3-氨基丙基)吗啉、1-(2-氨基乙基)哌啶、3，3-二氨基-N-甲基二丙胺、3，3-氨基双(N，N-二甲基丙胺)。另一类能够和酰化剂缩合并且具有季胺基的含氧或氮的化合物包括链烷醇胺，包括但不限于三乙醇胺、三甲醇胺、N，N-二甲基氨基丙醇、N，N-二乙基氨基丙醇、N，N-二乙基氨基丁醇、N，N，N-三(羟基乙基)胺、N，N，N-三(羟基甲基)胺。
季铵化剂
本发明的组合物含有适于将季胺基转化成季氮的季铵化剂，其中季铵化剂选自：硫酸二烷基酯、苄基卤化物、烃基取代的碳酸酯；烃基环氧化物与酸的组合或其混合物。
在一个实现方案中，季铵化剂可包括卤化物，例如氯化物、碘化物或溴化物；氢氧化物；磺酸酯；烷基硫酸酯，如硫酸二甲酯；磺内酯；磷酸酯；磷酸C1-12烷基酯；磷酸二C1-C12烷基酯；硼酸酯；硼酸C1-12烷基酯；亚硝酸酯；硝酸酯；碳酸酯；碳酸氢酯；链烷酸酯；O，O-二-C1-12烷基二硫代磷酸酯；或其混合物。
在一个实现方案中，季铵化剂可衍生自硫酸二烷基酯如硫酸二甲酯，N-氧化物，磺内酯如丙烷和丁烷磺内酯；烷基，酰基或芳基烷基卤化物如甲基和乙基氯化物、溴化物或碘化物或苄基氯，以及烃基(或烷基)取代的碳酸酯。如果酰基卤化物是苄基氯，芳环可进一步被烷基或亚烷基取代。
烃基取代的碳酸酯的烃基(或烷基)每一个基团可含1到50、1到20、1到10或1到5个碳原子。在一个实现方案中，烃基取代的碳酸酯含有两个相同或不相同的烃基。适宜的烃基取代的碳酸酯的例子包括二甲基或二乙基碳酸酯。
在另一个实现方案中，季铵化剂可以是如下式所示的烃基环氧化物与酸的组合：
其中R1、R2、R3和R4可以独自为H或C1-50烃基。
烃基环氧化物的例子可包括氧化苯乙烯，环氧乙烷，环氧丙烷，环氧丁烷，氧化均二苯代乙烯和C2-50环氧化物。
润滑粘度的油
本发明的组合物可含有润滑粘度的油。润滑粘度的油包括润滑粘度的天然或合成油，得自氢化裂解、加氢、加氢精制的油，未精炼、精炼、再精炼的油，或其混合物。在一个实现方案中，润滑粘度的油是分散剂和/或其他性能添加剂的载液。
天然油包括动物油、植物油、矿物油或其混合物。合成油包括烃类油、基于硅的油、含磷的酸的液态酯。合成油可通过Fischer-Tropsch反应来制备，一般是加氢异构化的Fischer-Tropsch烃或蜡。
润滑粘度的油也可以按在American Petroleum Institute(API)BaseOil Interchangeability Guideline中所规定的进行定义。在一个实现方案中，润滑粘度的油包括API Group I，II，III，IV，V或其混合物，而在另一个实现方案中，API Group I，II，III或其混合物。
杂项
组合物任选含有一种或多种其他性能添加剂。其他性能添加剂包括金属钝化剂，清洁剂，分散剂，粘度改性剂，摩擦改性剂，分散剂粘度改性剂，极压剂，抗磨损剂(antiwear agent)，抗氧化剂，腐蚀抑制剂，抑泡剂，破乳剂，倾点下降剂，密封溶胀剂，蜡控制聚合物，防垢剂(scaleinhibitor)，气体-水合物抑制剂(gas-hydrate inhibitor)及其混合物。
基于不含油基础上，额外性能添加剂化合物的合计总量在0重量％到25重量％或0.01重量％到20重量％的组合物。虽然可以存在一种或多种其他性能添加剂，通常对于其他性能添加剂各自以不同的量存在。
在一个实现方案中，组合物可以为处于浓缩状态的量。如果本发明呈浓缩物(其可以与另外的油混合，全部或部分地形成最终的润滑剂和/或液态燃料)，在润滑粘度的油和/或液态燃料中，本发明添加剂和/或其他另外的性能添加剂对稀释油的比例在80∶20到10∶90(重量)的范围里。
抗氧化剂包括二硫代氨基甲酸钼，硫化的烯烃，受阻酚，联苯胺；清洁剂包括碱金属、碱土金属和过渡金属与一种或多种酚盐、硫化的酚盐、磺酸盐、羧酸、磷酸、单和/或二硫代磷酸、水杨甙、水杨酸烷基酯、salixarate形成的中性或高碱性，牛顿或非牛顿，碱性盐。分散剂包括N-取代的长链亚烷基琥珀酰亚胺以及其后处理变体，后处理的分散剂包括那些与脲、硫脲、二巯基噻二唑、二硫化碳、醛、酮、羧酸、烃取代的琥珀酸酐、腈、环氧化物、硼化合物，以及磷化合物反应的分散剂。
抗磨损剂包括化合物如金属硫代磷酸盐，尤其是二烷基二硫代磷酸锌；磷酸酯或其盐；亚磷酸盐；以及含磷羧酸酯、醚和酰胺。抗磨剂(antiscuffingagent)包括有机硫化物和多硫化物，如二硫甲基苯，二硫二(氯甲基苯)，二丁基四硫，二叔丁基多硫化物，二叔丁基硫，硫化Diels-Alder加成物或烷基亚磺酰基N，N-二烷基二硫代氨基甲酸酯。极压(EP)剂包括氯化蜡，有机硫化物和多硫化物，如二硫甲基苯，二-(氯苄基)二硫，二丁基四硫，硫化的油酸甲酯，硫化的烷基苯酚，硫化的二戊烯，硫化的萜烯，以及硫化的Diels-Alder加成物；磷硫化烃类，金属硫代氨基甲酸盐，如二辛基二硫代氨基甲酸锌和庚基苯酚二酸钡。
摩擦改性剂包括脂肪胺、酯如硼酸处理的甘油酯，甘油的部分酯如甘油单油酸酯，脂肪亚磷酸酯，脂肪酸酰胺，脂肪环氧化物，硼酸处理脂肪环氧化物，烷氧基化脂肪胺，硼酸处理烷氧基化脂肪胺，脂肪酸的金属盐，脂肪咪唑啉，羧酸与聚亚烷基多胺的缩合物，烷基磷酸的胺盐。粘度改性剂包括氢化苯乙烯-丁二烯共聚物，乙烯-丙烯聚合物，聚异丁烯，氢化苯乙烯-异戊二烯聚合物，氢化异戊二烯聚合物，聚甲基丙烯酸的酯，聚丙烯酸酯，聚烷基苯乙烯，烯基芳基共轭二烯共聚物，聚烯烃，聚甲基丙烯酸烷基酯和马来酸酐-苯乙烯共聚物的酯。分散剂粘度改性剂(通常被称作DVM)包括官能化聚烯烃，例如，已经用马来酸酐和胺的反应产物进行官能化的乙烯-丙烯共聚物，或与胺反应了的苯乙烯-马来酸酐共聚物。
腐蚀抑制剂包括辛胺辛烷酸酯，十二烯基琥珀酸或酸酐和脂肪酸如油酸与多胺的缩合物。金属钝化剂包括苯并三唑，1，2，4-三唑，苯并咪唑，2-烷基二硫代苯并咪唑或2-烷基二硫代苯并噻唑的衍生物。抑泡剂包括丙烯酸乙酯和2-乙基己基丙烯酸酯以及任选的醋酸乙烯酯的共聚物。破乳剂包括聚乙二醇，聚氧化乙烯，聚氧化丙烯和(环氧乙烷-环氧丙烷)聚合物；倾点下降剂包括马来酸酐-苯乙烯的酯，聚甲基丙烯酸酯，聚丙烯酸酯或聚丙烯酰胺。密封溶胀剂包括Exxon Necton-37TM(FN 1380)和ExxonMineral Seal Oil。
工业应用
在一个实现方案中，本发明是有用于内燃机的液态燃料。内燃机包括火花点火和压缩点火发动机；2冲程或4冲程循环；经过直接喷射、间接喷射、进气口喷射(port injection)和汽化器供给液态燃料；共轨和机组喷射器系统(unit injector system)；轻型(例如客车)和重型(例如商用卡车)发动机；用烃和非烃燃料和其混合物提供燃料的发动机。发动机可以是合并了这样的部件的组合排气装置的一部分；EGR系统；后处理包括三元催化剂，氧化催化剂，NOx吸附剂和催化剂，任选使用燃料携带催化剂的催化或非催化颗粒捕集器；可控气门正时；以及喷射正时和速率形态调整(rate shaping)。
对于在此所用到的，术语“烃基取代基”或“烃基”是使用其通常的含义，对本领域技术人员来说是众所周知的。具体来说，指碳原子直接连接到分子的其余部分且烃特性占优的基团。烃基的例子包括：烃取代基，也就是说，脂肪族(例如烷基或烯基)、脂环族(例如环烷基，环烯基)取代基，和芳香-，脂肪-，和脂环-取代的芳香取代基，以及环状取代基，其中环是通过分子的另一部分完成的(例如，两个取代基一起形成环)；被取代的烃取代基，也就是，含有在本发明的上下文中没有改变烃特性占优的非烃基的取代基(例如，卤素(尤其是氯和氟)，羟基，烷氧基，巯基，烷基巯基，硝基，亚硝基，和亚硫酰(sulfoxy)基)；杂取代基，也就是在本发明的上下文中，在若非如此由碳原子构成的环或链中含有非碳同时烃特性占优的取代基。杂原子包括硫、氧、氮，并包括取代基如吡啶基、呋喃基、噻吩基和咪唑基。一般在烃基中每10个碳原子中存在不超过2个，优选不超过1个非烃取代基；典型的是在烃基中没有非烃取代基。
已知上述一些物质在最后的配方中可相互作用，因此最后配方中的成分可以不同于那些开始所添加的。例如，金属离子(例如清洁剂中的)可迁移到其他分子的其他酸性或阴离子的位置。由此所形成的产物，包括在使用本发明的组合物到其预计的用途上所形成的产品，可能并非那么容易说明。然而，所有这样的修改和反应产物都被包含在本发明的范围里；本发明还包含通过将上述的成分混合所制得的组合物。
实施例
通过下面所提出的特别有利的实现方案的实施例进一步说明本发明。所提供的实施例是用来阐明本发明，而不是意图来进行限制。
在如在CEC F-23-01中所述的发动机喷嘴污脏试验中对清洁剂进行评估。发动机喷嘴污脏试验的结果被突出在表1和2中。
在这个试验中所用的清洁剂包括：市售的1000Mn二甲基氨基丙胺的聚异丁烯琥珀酰亚胺(对比实施例1)，市售的1000Mn四亚乙基五胺的聚异丁烯琥珀酰亚胺(对比实施例2)和如下述的本发明的4个实验清洁剂(实施例1-4)。
制备实施例A：
制备实施例A是从琥珀酸酐(从21425克)1000Mn聚异丁烯制得和稀释油-pilot 900(3781克)的混合物开始制备的，在氮气氛围下，搅拌加热到110℃。在45分钟里缓慢加入二甲基氨基丙胺(DMAPA，2314克)，保持物料温度低于115℃。将反应温度提高到150℃并维持3小时。所得到的化合物是DMAPA琥珀酰亚胺。
实施例1
在氮气氛围下，将制备实施例A的反应产物，氧化苯乙烯(12.5克)，醋酸(6.25克)和甲醇(43.4克)搅拌加热至回流(～80℃)5小时。通过蒸馏(30℃，-1巴)提纯反应并得到水白色馏出物。所得到的化合物是氧化苯乙烯季铵盐。
实施例2
将准备实施例A的反应产物(373.4克)搅拌加热到90℃。将硫酸二甲酯(25.35克)装入反应罐并继续在氮覆盖下搅拌，放热将物料温度提高到～100℃。在冷却回来和倾析之前反应维持在100℃下3个小时。所得到的化合物是二甲基硫酸酯季铵盐。
实施例3
在氮气氛围下将制备实施例A的反应产物(1735.2克)搅拌加热到90℃。逐滴加入苄基氯(115.4克)，保持反应温度在90℃。在90℃的温度下反应5小时。所得到的化合物是苄基氯季铵盐。
实施例4
将制备实施例A的反应产物(152.6克)，碳酸二甲酯(31克)和甲醇(26.9克)装入一个压力容器中。对容器进行加压试验以检验泄漏情况并用氮气吹扫两次。然后将容器加压到～19psi并将物料搅拌(～210rpm)加热到90℃。在加热到140℃之前物料维持在90℃下1小时并维持在140℃24小时。在冷却回环境温度后，在倾析产物之前释放残压。通过蒸馏(100℃，-0.5巴)提纯反应，将游离态的碳酸二甲酯和甲醇除去。所得到的化合物是碳酸二甲酯季铵盐。
备注：对于对比实施例1和2，活性化学品伴随有惰性稀释油，活性化学品对稀释油的比例为85∶15(重量)。
备注：对于实施例1-4，活性化学品伴随有惰性稀释油，活性化学品对稀释油的比例为50∶50(重量)。
表1：CEC F-23-01喷射器沉积试验结果
 清洁剂   活性物加入率(ppm)   残留流量百分比(％)
 无＊   0.0   11.0
 实施例1   17.5   73.2
 实施例1   17.5   46.4
 实施例2   17.5   31.0
 实施例2   17.5   24
 实施例3   17.5   33.7
 实施例4   15   27.1
备注：＊没有添加基础燃料(在燃料中不存在清洁剂)
表2：CEC F-23-01喷射器沉积试验结果
 清洁剂   活性物加入率(ppm)   残留流量百分比(％)
 对比实施例2   51   79
 对比实施例2   51   63
 实施例2   50   100
 实施例2   50   98
 对比实施例2   38.25   34
 对比实施例2   38.25   32.4
 对比实施例2   38.25   30
 实施例2   38.5   76
 实施例4   38.5   41
 实施例4   38.5   72
 实施例4   38.5   84
 对比实施例1   38.25   84.0
 实施例1   35.0   99.6
 实施例1   35.0   84.8
试验结果显示使用本发明的季铵盐清洁剂(实施例1、2、3和4)的配方相对于使用未被添加的燃料和/或市售清洁剂的配方(对比实施例1和
2)表现出相当或较高的流动性能以及更少的平均喷射器污脏。
在高速直接喷射试验中进一步评估清洁剂。高速直接喷射试验叙述如下。将含有1ppm的锌加上各种清洁剂的柴油加进一个2.0L高速直接喷射(HSDI)Ford Puma发动机中。发动机最初在2000转/分钟下运转5分钟(发动机预热期)。开始的发动机预热期之后，在表3所列出的条件下，发动机以六(6)功率曲线周期(power curve iteration)运行。在完成第六功率曲线周期后，在表4所列出的条件下发动机进入稳定期。稳定期结束后，在表3所列出的条件下，发动机以另一个六(6)功率曲线周期运行。在功率曲线周期的第9阶段(stage)过程中测量发动机的输出功率。将最后一功率曲线周期过程(第12功率周期)中在这个第9阶段的功率与第一功率曲线周期过程中在第9阶段的功率相比较，计算出最终的功率损失百分比。发动机功率损失百分比越小，清洁剂在减少或最小化功率损失上就越有效。试验结果汇总在表5中。
在这个试验中所用到的清洁剂包括：市售的1000Mn二甲基氨基丙胺的聚异丁烯琥珀酰亚胺(对比实施例1)，市售的1000Mn四亚乙基五胺的聚异丁烯琥珀酰亚胺(对比实施例2)和如上所述的3种本发明的实验性清洁剂(实施例1、2和4)。
表3功率曲线周期
Figure GDA0000146006430000181
备注：两个阶段之间的变化(ramp)时间是27秒，除了从第11阶段返回到第1阶段之外，是30秒。这些变化时间不包含在阶段时间里(即时间安排的总持续时间为(11＊5分钟阶段)+(10＊27秒改变)+(1＊30秒改变)，得到总循环时间为60分钟)。
表4.稳定运行
表5：高速直接喷射试验结果
 清洁剂   活性剂量率(ppm)   在17小时的功率损失％
 没有   0.0   9.13
 没有   0.0   9.71
 实施例1   17.5   1.85
 实施例2   17.5   3.15
 实施例4   15   9.95
 对比实施例1   38.25   8.35
 对比实施例1   38.25   6.48
 对比实施例2   38.25   5.30
备注：＊未被添加柴油基础燃料(在燃料中不存在清洁剂)
试验结果显示，使用本发明的季铵盐清洁剂(实施例1、2和4)的配方与使用未被添加的燃料和/或市售清洁剂的配方(对比实施例1和2)相比，产生相当或更小的功率损失。
将上面所提及的每一个文献结合于此作为参考。除了在实施例中，或另外明确指出之外，所有在本说明书中载明的物质的量，反应条件，分子量，碳原子数等，应被理解成通过“大约”修饰。除非另外指出，在此被提及的每个化学品或组合物应被认为是商品级物质，其可含有异构体，副产物，衍生物和其他通常会存在于商品级中的那些物质。然而，所展现的每一种化学成分的数值不包含任何溶剂或稀释油，其通常会存在于工业物质中，除非另外指出。应该明白，在此所陈列的高和低的量，范围和比例界限可以独自组合。类似的，对于本发明的每个特征的范围和数值可以和任何其他特征的范围和数值一起使用。如在此所用的，表述“基本上由.......组成”允许包含不在本质上影响到研究中的组合物的基本和新的特性的物质。

Claims (6)

1.含有润滑粘度的油和季铵盐的组合物，其含有下述的反应产物：
a.烃基取代的酰化剂和含有能够与上述的酰化剂缩合的氧或氮原子且另外含有叔胺基的化合物的反应；和
b.适于将叔胺基转变成季氮的季铵化剂
其中季铵化剂选自由硫酸二烷基酯、烃基取代的碳酸酯；烃基环氧化物与酸的组合或其混合物组成的组。
2.权利要求1的组合物，其中烃基取代的酰化剂是聚异丁烯琥珀酸酐。
3.权利要求1的组合物，其中化合物(a)是N-甲基-1，3-二氨基丙烷。
4.权利要求1的组合物，另外含有在室温下呈液态的燃料。
5.权利要求1的组合物，另外含有选自下述的成分：金属钝化剂、不同于权利要求1的那些的清洁剂、分散剂、粘度改性剂、摩擦改性剂、分散剂粘度改性剂、极压剂、抗磨剂、抗氧化剂、腐蚀抑制剂、抑泡剂、破乳剂、倾点下降剂、密封溶胀剂、蜡控制聚合物、防垢剂、气体-水合物抑制剂及其混合物。
6.权利要求5的组合物，其中成分是含金属的高碱性清洁剂、二烷基二硫代磷酸锌或其混合物。
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