CN1084376C - 燃料油组合物 - Google Patents

燃料油组合物 Download PDF

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Publication number
CN1084376C
CN1084376C CN97195776A CN97195776A CN1084376C CN 1084376 C CN1084376 C CN 1084376C CN 97195776 A CN97195776 A CN 97195776A CN 97195776 A CN97195776 A CN 97195776A CN 1084376 C CN1084376 C CN 1084376C
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fuel
alkyl
composition
oil
group
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CN1222930A (zh
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J·林
S·D·罗伯特森
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Shell Internationale Research Maatschappij BV
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Shell Internationale Research Maatschappij BV
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Abstract

燃料油组合物，其中含有主要量的燃料油和少量的添加剂，该添加剂含有至少一种溶于燃料油的烷基或烷氧基芳族化合物，其中至少1个独立地选自1-30个碳原子的烷基和烷氧基的基团连接到芳香环上，和至少1个羧基和视具体情况存在的1个或2个羟基连接到芳香环上；制备该燃料油组合物的方法；和该燃料油组合物在压燃式发动机中作为燃料以控制该发动机燃料注射系统磨损率方面的用途。

Description

燃料油组合物
本发明涉及燃料油组合物，它们的制备方法和它们在压燃式发动机中的应用。
如WO9533805(Exxon)中所述，环境问题导致了对低硫含量燃料，尤其是柴油和煤油的需求。然而，生产低硫含量燃料的精制方法也生产了具有较低粘度和在燃料中诸如多环芳烃和极性化合物之类能提供润滑性的其它组分含量较低的产物。此外，通常认为含硫化合物提供了抗磨性能，因此降低含硫化合物的比例和提供润滑性的其他组分的比例的结果是，增大了使用低硫燃料的柴油发动机中燃料泵的损坏，以及在例如凸轮盘、滚柱、转轴和主动轴中因磨损而引起的损坏。
可以预期这个问题将来会变得更加严重，其原因在于为了满足对废气排放更严格的要求，通常使用例如回转式和单元注入器系统的高压燃料泵，同时由于更广泛地要求燃料中具有较低的硫含量，因此希望这些设备比现有设备具有更严格的润滑性要求。
目前，柴油燃料中一般的硫含量为约0.25％(重量)(2500ppmw)。在欧洲最高的硫含量已经降低至0.05％(500ppmw)；瑞典的燃料等级分别为硫含量低于0.005％(50ppmw)(2级)和0.001％(10ppmw)(1级)。具有硫含量低于0.20％(重量)(2000ppmw)的燃料油可称作低硫燃料。
WO9533805(Exxon)叙述了使用冷流动改进剂以提高低硫燃料的润滑性。
WO9417160(Exxon)叙述了使用羧酸和醇的某些酯作为燃料油添加剂以降低压燃式发动机的注射系统中的磨损，在上述羧酸和醇的酯中，酸具有2-50个碳原子，醇具有1个或多个碳原子，特别是单油酸甘油酯和己二酸二异癸酯。
US5484462(Texaco)提到用作低硫柴油机燃料的市售润滑剂的二聚亚油酸(第1栏，38行)，并且它提供了用作燃料润滑性改进剂的氨烷基吗啉。
US5490864(Texaco)叙述了用作低硫柴油燃料抗磨润滑性添加剂的某些二硫代磷酸二酯-二醇。
US5482521(Mobil)描述某些采用胺形成的氮杂环产物，借助羰基化合物键合在一起。这些产物及其与羧酸反应形成的产物可以用作燃料(包括低硫柴油在内)的摩擦改性剂与润滑剂。
现在我们意外地发现，当将具有至少1个连接到其芳环上的羧基的烷基和烷氧基芳族化合物加入到燃料油中时，可提供抗磨润滑性作用。
因此，根据本发明提供燃料油组合物，该组合物含有主要量的燃料油和少量的添加剂，该添加剂含有至少一种溶于燃料油的烷基或烷氧基芳族化合物，其中该燃料油是硫含量至多为0.2％重量的中间馏分燃料油，并且其中至少1个独立地选自1-30个碳原子的烷基和烷氧基的基团连接到芳香环上，和至少1个羧基和视具体情况存在的1个或2个羟基连接到芳香环上。
燃料油可由石油或植物油来源或其混合物得到。该燃料油通常是沸程为100-500℃，例如150-400℃的中间馏分燃料油。石油得到的燃料油可含有常压馏分或减压馏分，或裂化瓦斯油或以任何比例与直馏和热裂化和/或催化裂化馏分的掺和物。燃料油包括煤油、喷气燃料、柴油燃料、取暖用油和重质燃料油。优选的燃料油是柴油，并且本发明优选的燃料油组合物是柴油燃料组合物。一般根据燃料的等级和应用，柴油燃料的初始蒸馏温度为约160℃，最终蒸馏温度为290-360℃。
燃料油，例如柴油，其自身可以是加添加剂的(含添加剂)油或不加添加剂的(无添加剂)油。如果燃料油，例如柴油是加添加剂的油，那么它将含有少量的一种或多种添加剂，例如一种或多种下列添加剂：抗静电剂、管线减阻剂、流动性改进剂(例如乙烯/乙酸乙烯酯共聚物或丙烯酸酯/马来酐共聚物)和蜡抗沉降剂(例如以商标“PARAFLOW”(例如“PARAFLOW”450；购自Paramins)，“OCTEF”(例如“OCTEF”W5000；购自Octel)和“DODIFLOW”(例如“DODIFLOW”v 3958；购自Hoechst)市售的那些试剂)。
优选硫含量至多0.05％(重量)(500ppmw)(“ppmw”是每百万重量份数)的中间馏分油如柴油。当燃料油的硫含量低于0.005％(重量)(50ppmw)或甚至低于0.001％(重量)(10ppmw)时也可得到本发明有益的组合物。
虽然烷基或烷氧基芳香族化合物的芳香环可以是单环、双环或多环，例如苯环或萘环体系，但该芳香环优选为苯环。
优选的烷基和烷氧基芳香族化合物是这样的化合物，其中每当有少于3个选自烷基和烷氧基的基团连接到芳香环上时，有至少1个选自2-30个碳原子的烷基和烷氧基的基团连接到该芳香环上。
在本发明的一个优选方面，至少1个烷基或烷氧基芳香族化合物是烷基芳香族化合物，其中至少1个C6-30烷基连接到芳香环上。
更优选的是，烷基芳香族化合物是含有1或2个6-30个碳原子的烷基的烷基苯甲酸或烷基水杨酸。
在烷基芳香族化合物中的这个或每个烷基优选是C8-22烷基，最优选是C8-18烷基。
加入到本发明燃料油组合物中的烷基或烷氧基芳香族化合物或者是已知的化合物或者可以用类似于本领域技术人员已知的用于制备已知化合物的方法制备。
优选的烷基水杨酸可以用UK专利1146925(在该专利中，烷基水杨酸是在润滑剂组合物中用作分散剂的多价金属盐制备过程的中间体)中所述的方法非常容易地制备。
基于燃料组合物的总重量，含有至少一个烷基或烷氧基芳香族化合物的添加剂的存在量优选为50-500ppmw，更优选为50-250ppmw，最优选为150-250ppmw。
在室温下在燃料油中溶解量不到50ppmw的烷基或烷氧基化合物不是本文定义的燃料油可溶性范畴(因此它们被认为是不可溶的)。
本发明燃料油组合物可用它们的制备方法制备，该方法包括将添加剂或含有添加剂的添加剂浓缩物与燃料油混合。
适合加入到燃料油组合物(优选柴油燃料组合物)中的添加剂浓缩物将包括这样的添加剂，该添加剂包括至少一种烷基或烷氧基芳香族化合物和燃料相容的稀释剂，该稀释剂可以是载油(例如矿物油)，聚醚(可以是封端的或未封端的)，非极性溶剂如甲苯、二甲苯、油漆溶剂油和Royal Dutch/Shell Group的成员公司以商标“SHELLSOL”销售的那些溶剂，和/或极性溶剂如酯和特别是醇，例如己醇，2-乙基己醇，癸醇，异十三醇和醇混合物如Royal Dutch/Shell Group的成员公司以商标“LINEVOL”，尤其是“LINEVOL”79醇销售的那些醇混合物，“LINEVOL”79醇是C7-9伯醇的混合物，或从Sidobre Sinnova，France以商标“SIPOL”可买到的C12-14醇混合物。
添加剂浓缩物和由其制备的燃料油组合物还可含有附加的添加剂，如无灰清净剂或分散剂，例如直链或支链烃基胺，例如烷基胺，烃基取代的瑚珀酰亚胺，例如在EP-A-147240中叙述的那些，优选聚异丁烯琥珀酸或酐与四亚乙基五胺的反应产物，其中聚异丁烯取代基的数均分子量(Mn)为500-1200，和/或在欧洲专利申请96302953.3(申请人案卷号TS 7030 EPC)中所述的烷氧基乙酸衍生物；去混浊剂，例如烷氧基化苯酚甲醛聚合物如以“NALCO”(商标)EC5462A(以前为7D07)(购自Nalco)，和“TOLAD”(商标)2683(购自Petrolite)市售的那些；防泡剂(例如以“TEGOPREN”(商标)5851，Q25907(购自DowCorning)或“RHODORSIL”(购自Rhone Poulenc)市售的聚醚改性的聚硅氧烷)；十六烷值增进剂(例如硝酸2-乙基己酯，硝酸环己酯，二叔丁基过氧化物和在US4208190，2栏，27行至3栏21行中公开的那些)；防锈剂(例如由Rhein Chemie，Mannheim，Germany以“RC 4801”销售的那些，或琥珀酸衍生物的多元醇酯，在至少一个其α碳原子上具有未取代的或取代的20-500个碳原子的脂族烃基的琥珀酸衍生物，例如聚异丁烯取代的琥珀酸的季戊四醇二酯)，除臭剂，抗磨剂；抗氧化剂(例如酚类抗氧化剂如2，6-二-叔丁基苯酚，或苯二胺如N，N’-二-仲丁基对苯二胺)；和金属钝化剂。
除非另有说明，在柴油燃料中每种附加添加剂的(活性物质)浓度优选高达1％(重量)，更优选5-1000ppmw(柴油燃料的每百万份重量份数)。在柴油燃料中清净剂或分散剂的(活性物质)浓度优选为30-1000ppmw，更优选50-600ppmw，有利的是75-300ppmw，例如95-150ppmw。
在柴油燃料中去混浊剂的(活性物质)浓度优选为1-20ppmw，更优选1-15ppmw，更加优选1-10ppmw，有利的是1-5ppmw。其他添加剂(十六烷值增进剂除外)的(活性物质)浓度均优选为0-20ppmw，更优选0-10ppmw。在柴油燃料中十六烷值增进剂的(活性物质)浓度优选为0-600ppmw，更优选0-500ppmw。如果将十六烷值增进剂加入到柴油燃料中，其常规的用量为300-500ppmw。
本发明还提供了如上定义的燃料组合物作为压燃式发动机中燃料的应用，以控制发动机的燃料注射系统，尤其是燃料注射泵和/或燃料注射器的磨损率。
本发明的后一种情况也可以表示为操作压燃式发动机的方法，该方法包括提供如上定义的燃料组合物作为发动机中的燃料，从而控制发动机燃料注射系统，尤其是燃料注射泵和/或燃料注射器的磨损率。
通过下面的说明性实施例进一步理解本发明，其中基础燃料和添加剂组分如下：
                             基础       基础        基础         基础
                             燃料1      燃料2       燃料3        燃料4密度(kg/l)在15℃(ASTM D 4052)    0.821      0.8291      0.8165       0.8165硫(ppmw)(IP 373)                 182        145         2            ＜5蒸馏，℃(ASTM D 86)IBP                              166.5      167         184.5        184.510％                             203.5      199         213          206.520％                             216        120.5       218.5        213.550％                             256.5      247.5       238          235.590％                             322.5      309.5       269.5        268.595％                             342.5      324.5       278.5        277.5FBP                              355        338.5       292          290总芳族化合物含量(％W)               20.2      22.1       5.2        3.8“烷基水杨酸A”是通过酚化、羧化和水解由C14-18烷基苯酚制备的，如UK专利1146925所述。起始的烷基苯酚是通过在3％(重量)(基于烯烃)酸活化蒙脱石催化剂存在下在190℃和0.4巴(4×104Pa)压力下苯酚与烯烃(摩尔比为5∶1)反应由烯烃混合物(C14∶C16∶C18重量比为1∶2∶1)制备的，过量的苯酚通过蒸馏除去。最终产物C14-18烷基水杨酸含有71.5％(摩尔)单烷基水杨酸、17.2％(摩尔)单烷基苯酚和4.7％(摩尔)二烷基苯酚，余量是少量的4-羟基间苯二甲酸、二烷基水杨酸、2-羟基间苯二甲酸和烷基苯基醚。“载体B”是使用C12-15醇作为引发剂制备的聚氧化丙二醇半醚(单醚)，其Mn在1200-1500范围，在40℃根据ASTM D 445的运动粘度在72-82mm2/s范围，可从Royal Dutch/Shell集团的成员公司以商品名“SAP 949”得到。“油 C”是纯净和光亮溶剂精制的基础油，其在100℃的粘度为4.4-4.9mm2/s，倾点为-18℃，闪点为204℃，可从Royal Dutch/Shell集团的成员公司以商品名“HVI 60”得到。“防锈剂D”是四丙烯基琥珀酸的羟基丙酯(四丙烯基琥珀酸的丙烷-1，2-二醇半酯)(参看UK专利1306233的实施例IV)。“Dehazer E”是由Nalco以“NALCO”EC5462A(以前为7D07)(商标)得到的烷氧基化苯酚甲醛聚合物去混浊剂。“防泡剂F”是由 Goldchmidt AG以“TEGOPREN 5851”(商标)得到的聚醚改性的硅氧烷。“溶剂  G”是从Royal Dutch/Shell集团的成员公司以“LINEVOL79”(商标)得到的C7-9伯醇的掺和物。“溶剂 H”是沸程为205-207℃、平均分子量为156的芳香烃溶剂(74％芳族化合物)，可从Royal Dutch/Shell集团的成员公司以“SHELLSOL R”(商标)得到。“分散剂 I”是聚异丁烯瑚珀酰亚胺的27％(重量)溶液，该瑚珀酰亚胺是这样制备的：数均分子量(Mn)为950的聚异丁烯与马来酐反应生成琥珀酸化率(每个聚异丁烯链的琥珀酸酐部分的比例)为1.05∶1的聚异丁烯琥珀酸酐产物，接着酐产物与四亚乙基五胺(TEPA)以琥珀酸基：TEPA为1.5∶1的摩尔比反应。为了便于处理，通过加入“SHELLSOL R”(商标)溶剂将在“HVI 60”基础油中含有47％(重量)活性组分的聚异丁烯瑚珀酰亚胺溶液稀释至活性组分的含量为27％(重量)。实施例I
用下述方法制备添加剂浓缩物：在室温下(20℃)将69克在二甲苯(24克)中的烷基水杨酸A(45克)溶液、16克油C和15克载体B在旋转混合器上的250毫升密封玻璃瓶中混合1小时，得到100克混合好的添加剂浓缩物I。实施例II
通过将0.3319克防锈剂D，0.3325克去混浊剂E，0.6791克防泡剂F，6.6739克溶剂G，12.8809克溶剂H，32.44克分散剂I和33.66克硝酸2-乙基己酯(十六烷值增进剂)混合制备共添加剂混合物。
然后在250毫升玻璃烧杯中将1.0498克得到的共添加剂混合物与0.1620克实施例I的添加剂浓缩物混合，得到添加剂浓缩物II。
当使用添加剂浓缩物II制备调配柴油燃料时，将50毫升基础燃料1加入到上述添加剂浓缩物II样品中，在倒入1升涂漆的罐中之前充分搅拌得到的混合物。然后用另外50毫升基础燃料1清洗玻璃烧杯并倒入该罐中。通过加入基础燃料1使调配燃料的总重量高达801克。将该罐摇动2分钟得到含有1500ppmw添加剂浓缩物II的均匀的调配柴油燃料。实施例III
使用类似于实施例I的方法，通过混合45克烷基水杨酸A、24克溶剂H，16克油C和15克载体B得到添加剂浓缩物III来制备添加剂浓缩物。实施例IV
类似于实施例III，通过将45克烷基水杨酸A与39克溶剂A和16克油C混合得到添加剂浓缩物IV来制备添加剂浓缩物。燃料试验实施例
通过将定量的添加剂浓缩物I，III和IV加入到各种基础燃料1，2和3中制备调配柴油燃料。用高频往复试验台(HFRR)试验，根据CECF-06-T-94的方法，只是所用的燃料量为2毫升、流体温度为60℃，测定得到的燃料的润滑性能。
试验的调配柴油燃料的详细情况和试验结果列于下表1：
                                    表1
  燃料实施例  基础燃料  添加剂浓缩物(AC) 燃料中AC的浓度(ppmw)   燃料中烷基水杨酸A的浓度(ppmw)  平均磨损伤痕直径(微米，m×10-6)
  对比A1234567对比B89101112对比C131415     111111112222223333     -IIIIIIIIV-IIIIIIIIIIIIIV-IIIIIIIII     -1101702253354451500225-110170225335225-170340510     -507510015020090100-5075100150100-75150230     597472429415396398483378610518461440390434660539391383
从表1的结果可以容易地看出，通过磨损减少可以证实，即使在低浓度烷基水杨酸A和低处理量的情况下也可以出人意料的方式提高润滑性。其它燃料试验实施例
将定量的一些不同的烷基芳族化合物加到基础燃料1至浓度为100ppmw来制备另外的柴油燃料。如上述燃料试验实施例所述方法测试所得燃料的润滑特性，所不同的是采用了结构相似但却属于不同种类的试验台(这是考虑到相对于上述对比A，基础燃料试验对比D在磨损伤痕方面具有小的不明显的差异)。
所用的烷基芳族化合物如下：实施例16-4-辛基苯甲酸实施例17-4-正丁基苯甲酸实施例18-4-十二烷氧基苯甲酸对比E     -3-十五烷基苯酚对比F     -十二烷基苯酚，从Adibis以商品名“ADX 100”得到。对比G     -C14-18烷基苯酚，上述原料烷基水杨酸A的烷基苯酚。
结果列于下表2：
                      表2
燃料实施例 平均磨损伤痕直径(微米，m×10-6)
对比D(无添加剂)实施例16实施例17实施例18对比E对比F对比G     565308250319562559559
使用基础燃料4(对比H)和200ppmw浓度的2，4，6-三甲基苯甲酸(实施例19)和4-乙基苯甲酸(实施例20)进行与表2的那些燃料直接等同的试验。结果列于下表3：
                       表3
燃料实施例 平均磨损伤痕直径(微米，m×10-6)
对比H(无添加剂)实施例19实施例20     622387352
从表2和3可容易地看出，含有烷基或烷氧基苯甲酸(4-辛基苯甲酸，4-正丁基苯甲酸，4-十二烷氧基苯甲酸，2，4，6-三甲基苯甲酸和4-乙基苯甲酸)的燃料的润滑性以出人意料的方式得到提高，而在烷基苯酚的任何情况下没有发现积极的作用。
2，3-二甲基苯甲酸，2，4-二甲基苯甲酸和3，4-二甲基苯甲酸在燃料油，尤其是基础燃料4中的浓度为50ppmw下测定各自的溶解性，发现在室温下(20℃)是不溶的。因此这些二甲基苯甲酸不是燃料油溶性的烷基芳族化合物。

Claims (10)

1.一种燃料油组合物，其中含有主要量的燃料油和少量的添加剂，该添加剂含有至少一种溶于燃料油的烷基或烷氧基芳族化合物，其中该燃料油是硫含量至多为0.2％重量的中间馏分燃料油，并且其中至少1个独立地选自C1-30烷基和烷氧基的基团连接到芳环上，和至少1个羧基和视具体情况存在的1个或2个羟基连接到该芳环上。
2.权利要求1的组合物，其中所述燃料油是硫含量至多为0.05％重量的中间馏分燃料油。
3.权利要求1的组合物，其中每当有少于3个选自烷基和烷氧基的基团连接到芳环上时，有至少1个选自C2-30烷基和烷氧基的基团连接到该芳环上。
4.权利要求1-3中任一项的组合物，其中所述至少一个烷基或烷氧基芳族化合物是其中至少一个C6-30烷基连接到芳环上的烷基芳族化合物。
5.权利要求4的组合物，其中在所述烷基或烷氧基芳族化合物中，所述芳环是苯环。
6.权利要求5的组合物，其中所述烷基芳族化合物是含有1或2个C6-30烷基的烷基苯甲酸或烷基水杨酸。
7.权利要求6的组合物，其中该烷基或每个烷基是C8-22烷基。
8.权利要求1的组合物，其中以燃料组合物的总重量为基准计，所述添加剂的存在量在50-500ppmw范围内。
9.权利要求1-8中任一项的燃料油组合物的制备方法，其中包括使添加剂或含有添加剂的添加剂浓缩物与燃料油混合。
10.权利要求1-8中任一项的燃料油组合物在压燃式发动机中作为燃料在控制发动机燃料注射系统磨损率方面的用途。
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