CN1079410C - 添加剂组合物、油品组合物、添加剂浓缩物及用途 - Google Patents

添加剂组合物、油品组合物、添加剂浓缩物及用途 Download PDF

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CN1079410C
CN1079410C CN93107713A CN93107713A CN1079410C CN 1079410 C CN1079410 C CN 1079410C CN 93107713 A CN93107713 A CN 93107713A CN 93107713 A CN93107713 A CN 93107713A CN 1079410 C CN1079410 C CN 1079410C
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composition
oil
ester
polymkeric substance
structural unit
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CN1081691A (zh
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R·J·布罗德
B·W·戴维斯
T·伊布拉海姆
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ExxonMobil Chemical Patents Inc
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ExxonMobil Chemical Patents Inc
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Abstract

含有两种或两种以上有不同酯含量的乙烯一不饱和酯共聚物的组合物可改进各种燃料油品的低温性质。

Description

添加剂组合物、油品组合物、添加剂浓缩物及用途
本发明涉及油品组合物，主要是燃料油品组合物，特别是对低温下生成蜡敏感的燃料油品组合物，以及涉及用于这样的燃料油品组合物的添加剂组合物。
取暖用油和其他石油镏分油燃料，如柴油燃料都含有在低温下以大结晶蜡沉淀的烷烃，因此生成使燃料失去流动能力的凝胶结构。燃料仍能流动的最低温度称为倾点。
当燃料的温度下降並接近倾点时，通过管道和泵输送燃料出现困难。而且，在高于倾点的温度下，蜡晶体有堵塞燃料管道、筛网和过滤器的倾向。这些问题在本技术领域已充分认识到，並提出了各种添加剂，它们中有许多正在工业应用，用于降低燃料油品的倾点。同样，还提出了其他一些添加剂，它们正在工业上用于减小生成的蜡晶体的尺寸和改变生成的蜡晶体的形状。较小尺寸的晶体是所希望的，因为它们更不容易堵塞过滤器；某些添加剂可防止蜡呈小片状体结晶出来，使蜡以针状结构结晶出来，生成的针状体比小片状体更容易通过过滤器。添加剂还有使生成的晶体以悬浮的形式保留在燃料中的作用，得到较少的沉淀也有助于防止堵塞。用乙烯-醋酸乙烯酯或乙烯-丙酸乙烯酯共聚物(EVAC或EVPC)基流动改进剂可有效地改变蜡晶体(如用冷过堵塞点(CFPP)和其他操作性能试验以及模拟和现场性能测定表明的那样)。
在欧州专利EP-A-45342中公开了一种低温流动性改进剂，它以2-乙基己酸、丙烯酸和邻苯二甲酸酯化改性的EVAC为基础。
在德文杂志“科学与技术”第42卷第6期第238页(1989)中，M.Ratsch和M.Gebauer描述了包括正己酸酯化的EVAC在内的低温流动性改进剂。
在美国专利3961916中，描述了中间镏分油流动性改进剂，它含有防止蜡生长剂和成核剂，前者宜为有较高酯含量的较低分子量乙烯-乙烯酯共聚物，后者宜为有较低酯含量的较高分子量乙烯-乙烯酯共聚物，两种酯最好都是但不必须是醋酸乙烯酯。
在德国专利DE-AS-2407158中，描述了中间镏分油流动性改进剂，它含有低分子量乙烯-乙烯基酯和乙烯-丙烯酸酯共聚物，两者都含有至少40％(摩尔)酯组分。
本发明提供一种有效地改进油品低温流动性的油品(特别是燃料油品)添加剂，它以含有至少两种不同的乙烯与不饱和酯共聚物的组合物或含有乙烯与至少两种不同类型不饱和酯衍生的单元的共聚物的组合物为基础，是一种其优越性超过以前提出的组合物的有效的低温流动性改进剂。
首先，本发明提供一种组合物，它含有：
(i)一种油溶性乙烯共聚物，除由乙烯衍生的结构单元外，还有7.5～35％(摩尔)化学式为-CH2-CRR1(I)的结构单元和
(ii)一种油溶性乙烯共聚物，除由乙烯衍生的结构单元外，还有至多10％(摩尔)化学式为-CH2-CRR2(II)的结构单元，其中每一R各自独立地代表H或CH3，每一R1和R2各自独立地代表化学式为COOR3或OOCR4的基团，其中R3和R4各自独立地代表一个烃基，附加条件为R1和R2不同时为乙酸酯基，聚合物(i)中的结构单元I比聚合物(ii)中的结构单元II至少多2％(摩尔)。
本说明书中所用的术语“烃基”指有直接连接在分子其余部分的碳原子的，有烃类特征或主要有烃类特征的基团。其中，可提到的烃基包括脂肪族基团(如烷基或链烯基)、脂环族基团(如环烷基或环链烯基)、芳香族基团、脂族和脂环族取代的芳香族基团，以及芳香族取代的脂肪族和脂环族基团。脂肪族基团优选的是饱和基团。这些基团可含有非烃取代基，只要它们的存在不改变所述基团的主要烃类特征。例子包括酮基、卤素、羟基、硝基、氰基、烷氧基和酰基。如果烃基是被取代的，优选的是单取代基。取代的烃基的例子包括2-羟乙基、3-羟丙基、4-羟丁基、2-酮丙基、乙氧乙基和丙氧丙基。这些基团在原由碳原子构成的链或环中也可(或者)含有除碳原子以外的其他原子。例如，适用的杂原子包括氮、硫和优选的是氧。有益的是，烃基含有至多30个(优选至多15个，更优选至多10个，最优选至多8个)碳原子。
优选的R代表H。
优选的是，R3和R4每一个独立地代表链烯基或如上所述优选的是烷基，它最好是直链的。如果烷基或链烯基是支链的，例如在2-乙基己基中，那么α碳原子最好是亚甲基的一部分。烷基或链烯基含有至多30个碳原子，优选的是1(在链烯基情况下为2)至14个碳原子，更优选的是4～10个碳原子。作为烷基或链烯基的例子，可提到的是丙基、正丁基、异丁基和下列基团的异构体，最好是其直链异构体，如戊基、己基、庚基、辛基、壬基、癸基、十一烷基、十二烷基、十三烷基、十四烷基、十五烷基、十六烷基、十七烷基、十八烷基、十九烷基和二十烷基，以及它们对应的链烯基，优选的是末位链烯基。当R1和1或R2为化学式OOCR4时，R4最优选的是代表戊基，如上所述优选的是正戊基。
作为环烷基、烷芳基和芳基，可提到的例子是环己基、苄基和苯基。
共聚物也可含有除上面提到的化学式以外的其他化学式的结构单元，例如化学式-CH2-CRR5-(III)的结构单元或化学式-CCH3(CH2R6)-CHR7-(IV)的结构单元，其中R5代表-OH，R6和R7各自独立地代表氢或有至多4个碳原子的烷基，结构单元IV优选的是由异丁烯、2-甲基-丁-2-烯或2-甲基戊-2-烯衍生得到。
化学式I或II的结构单元可为末端结构单元，但优选的是中间结构单元。优选的是，化学式I的结构单元相当于聚合物(i)的10～25(优选的是10～20，更优选的是11～16)％(摩尔)。优选的是，化学式II的结构单元相当于聚合物(ii)的至多7.5(优选的是0.3～7.5，更优选的是3.5～7.0)％(摩尔)。
共聚物(i)的数均分子量(如用凝胶渗透色谱法测定的)以至多14000为好，更好的是至多10000，最好是1400～7000，优选的是2000～5500，最优选的是约4000。对于聚合物(ii)来说，数均分子量至多为20000，优选的是至多15000，更优选的是1200～10000，最优选的是3000～10000。优选的数均分子量在某种程度上取决于R3和R4中碳原子的数目，碳原子数目越高，在上述范围内优选的分子量越高。聚合物(ii)的数均分子量比聚合物(i)至少高500，优选的是至少高1000为好。
R1或R2代表OOCR4的聚合物是优选的，更优选的是R1和R2都代表OOCR4。
在相同的添加剂组合物中，使用两种或两种以上聚合物(i)和/或两种或两种以上聚合物(ii)均包括在本发明的范围内。使用有两种或两种以上不同的I型和II型结构单元的聚合物(i)或(ii)也在本发明的范围内。聚合物(i)中的结构单元I可与聚合物(ii)中的结构单元II相同或不同，如上所述只要它们不同时含有乙酸酯基。
本发明还提供一种含有所述添加剂组合物的油品，以及一种添加剂的浓缩物，该浓缩物由本发明的添加剂组合物与油品或可与油品混溶的溶剂混合而成。本发明还提出用所述添加剂组合物改进油品的低温性能。所述的油品可为原油，也就是直接从钻井得到的、炼制前的石油，本发明的组合物适合用作它们的流动改进剂。
所述的油品可为润滑油，润滑油可为动物油、植物油或矿物油，例如从石脑油或锭子油到SAE30级、40级或50级润滑油的石油馏分、蓖麻油、鱼油或氧化的矿物油。视油品的用途而定，这样的油品可含数种添加剂，例如粘度指数改进剂(如乙丙共聚物)、琥珀酸基分散剂、含金属的清净添加剂和二烷基二硫代磷酸锌抗磨添加齐。本发明的组合物适用于在润滑油中作流动性改进剂、降凝剂或脱蜡助剂。
所述的油品可为燃料油品，特别是中间馏分燃料油品。这样的馏份燃料油品的沸点一般为110～500℃，例如150～400℃。所述的燃料油品可含常压馏分油或减压馏分油，或裂化瓦斯油或由直馏的和热裂化和或催化裂化馏分油按任何比例的调合油。最通用的石油馏分燃料是煤油、喷气燃料、柴油、取暖用油和重质燃料油。取暖用油可为直馏常压馏分油或含有少量(例如至多35％(重量))减压瓦斯油或裂化瓦斯油或这两种油。上面提到的低温流动性问题最常发生在柴油和取暖用油。本发明也可用于植物基燃料油品，例如菜籽油。
添加剂在环境温度下应最好在油中是可溶的，并可达每单位重油品至少1000PPm的程度。但是，在接近油品浊点时至少有一部分添加剂可从溶液中析出来，起到改变生成的蜡晶体的作用。
在本发明的组合物中，用每100个亚甲基单元的甲基数目表示的聚合物线性度(如用质子核磁共振谱测定的)最好为1～15。
所述的共聚物可用本专业技术已知的方法制备，例如自由基引发的溶液聚合法，或很容易在高压釜或管式反应器中进行的高压聚合法。
另一方面，共聚物可用乙烯-醋酸乙烯酯或乙烯-丙酸乙烯酯，或乙烯-(甲基)丙烯酸甲酯或乙烯-(甲基)丙烯酸乙酯共聚物的皂化和再酯化法制备。
制备共聚物的另一方法是转移酯化法，若进入的酸或醇比要脱除的酸或醇不易挥发的话。
如果希望，所有的或基本上所有的现存的酯基可被水解並完全被所希望的链取代基所代替。另一方面，可只有一定比例的酯被水解，以致生成的聚合物含有例如乙酸酯侧链和更长的链。
含有结构单元I和结构单元II的聚合物，二者的重量比宜为10∶1～1∶10，优选的是10∶1～1∶3，更优选的是7∶1～1∶1
添加剂组合物和油品组合物还可含有其他改进低温性质和/或其他性质的添加剂，它们中的许多正在本技术领域应用或在文献中已知的。
例如，组合物也可含有另外的乙烯-乙烯酯(特别是醋酸酯)共聚物，特别是数均分子量至多为14000、乙烯基酯含量7.5～35％(摩尔)的乙烯-乙烯酯共聚物。
所述的添加剂组合物还可含有梳状聚合物。这样的聚合物在N.A.Plate和V.P.Shibaev在“聚合物科学杂志、大分子评述”第8卷第117～253页(1974)上“梳状聚合物、结构和性质”一文中讨论。
优选的是，梳状聚合物是均聚物或共聚物。该均聚物含有或共聚物的至少25(优选的是至少40，更优选的是至少50)％(摩尔)的单元含有至少6(优选的是至少10)个原子的侧链。
作为优选硫状聚合物的例子，可提到下列通式
其中D为R11、COOR11、OCOR11、R12CODR11或OR11，E为H、CH3、D或R12，G为H或D，J为H、R12、R12COOR11或芳基或杂环基，K为H、COOR12、OCOR12、OR12或COOH，L为H、R12、COOR12、OCOR12、COOH或芳基，R11为至少C10烃基，R12为至少C1烃基，m和n代表摩尔比，m为1.0～0.4，n为0～0.4。R11优选的是代表有10～30个碳原子的烃基，而R12优选的是代表有1～30个碳原子的烃基。
如果希望或需要的话，梳状聚合物可含有由其他单体衍生的结构单元。包括两种或两种以上不同的硫状共聚物亦在本发明的范围内。
这些梳状聚合物可为马来酸酐或富马酸和其他乙烯属不饱和单体(如α-烯烃)或不饱和酯(如醋酸乙烯酯)的共聚物。虽然摩尔比在2∶1至1∶2范围内是适合的，但使用等摩尔量共聚单体是优选的，但不是必要的。
可与例如马来酸酐共聚的烯烃包括1-癸烯、1-十二碳烯、1-十四碳烯、1-十六碳烯和1-十八碳烯。
共聚物可用任何适用的技术酯化，虽然马来酸酐或富马酸至少50％被酯化是优选的，但不是必要的。
可使用的醇的例子包括正癸-1-醇、正十二-1-醇、正十四-1-醇、正十六-1-醇和正十八-1-醇。醇也可包括每一主链至多有一个甲基侧链的醇，例如1-甲基十五-1-醇、2-甲基-十三-1-醇。醇可为正构醇和单甲基支链醇的混合物。优选的是使用纯醇而不是使用商购的混合醇，但如果使用混合醇，R12指烷基的平均碳原子数；如果使用在1或2位有分支的醇，R12指醇的直链主链部分。
这些梳状聚合物特别可为富马酸酯或衣康酸酯聚合物和共聚物，如在欧州专利153176、153177和225688和世界专利91/16407中描述的。
特别优选的富马酸酯梳状聚合物是富马酸烷基酯和醋酸乙烯酯的共聚物，其中烷基有12～20个碳原子。更特别优选的聚合物中烷基有14个碳原子或为C14/C16烷基的混合物它们例如用等摩尔富马酸和醋酸乙烯酯混合物溶液聚合，生成的共聚物再与醇或混合醇(优选的是直链醇)反应制得。当使用混合醇时，优选的是重量比为1∶1的正构C14和C16醇的混合物。而且，使用C14酯和C14/C16混合酯的混合物是有益的。在这样的混合物中，C14与C14/C16的重量比宜为1∶1至4∶1，优选的是2∶1至7∶2，更优选的是约3∶1。
其他适用的硫状聚合物是α-烯烃的聚合物和共聚物和苯乙烯和马来酸酐的酯化共聚物，以及苯乙烯和富马酸的酯化共聚物；如上所述按照本发明可使用两种或多种梳状聚合物的混合物，这样使用可能是有利的。
所述的添加剂组合物也可含极性含氮化合物，如在美国专利4211534中描述的，特别是邻苯二甲酸酐与2摩尔氢化牛脂胺的酰胺-胺盐，或邻磺基苯甲酸酐相应的酰胺-胺盐。
本发明的添加剂组合物也可含乙烯和至少一种α-烯的共聚物，其数均分子量至少为30000。α-烯烃至多宜有20个碳原子。这样的α-烯烃的例子是丙烯、1-丁烯、异丁烯、正辛烯-1、异辛烯-1、正癸烯-1和正十二烯-1。共聚物也可含少量(如至多10％(重量))其他可共聚的单体，例如，除α-烯烃以外的烯烃和非共轭二烯。优选的共聚物是乙烯-丙烯共聚物。包括两种或两种以上这类不同的乙烯-α-烯烃共聚物是在本发明的范围内。
如上所述，乙烯-α-烯烃共聚物的数均分子量为至少30000(用凝胶渗透色谱(GPC)相对聚苯乙烯标准样测定的)，宜为至少60000，优选的是至少80000。就其作用而言，分子量没有上限，但当分子量超过约150000时，由于粘度增加使混合困难，因此优选的分子量范围是60000和80000至120000。
共聚物的乙烯含量为50～80％(摩尔)。尤其是乙烯含量为57～80％是有益的。优选的是58～73％，更优选的是62～71％，最优选的是65～70％。
优选的乙烯-α-烯烃共聚物是乙烯含量为62～71％(摩尔)，数均分子量为60000～120000的乙烯-丙烯共聚物，特别优选的共聚物是乙烯含量为62～71％(摩尔)数均分子量为80000～100000的乙烯-丙烯共聚物。
所述的共聚物可用本技术领域已知的任何方法制备，例如用齐格勒型催化剂。聚合物应基本上是无定形的，因为高度结晶的聚合物在低温下在燃料油品中是相对不溶的。
所述的添加剂组合物也可含另外的乙烯-α-烯烃共聚物，其数均分子至多7500，宜为1000～6000，优选的是2000～5000，用气相渗透压测定法测定。适用的α-烯烃如上面给出的或苯乙烯，其中丙烯又是优选的。虽然可以使用至多86％(摩尔)乙烯的乙烯-丙烯共聚物，但乙烯含量宜为60～77％(摩尔)。
所述的组合物也可含聚(乙二醇)酯，优选的是链上含有18～22个碳原子的脂肪酸的聚(乙二醇)酯，特别是所处理的燃料不合作为蜡结晶成核剂的高级烷烃时。
另外，所述的添加剂组合物和燃料油品组合物可含有其他用途的添加剂，如减少颗粒物排放或抑制贮存过程中变色和生成沉淀物的添加剂。
本发明的燃料油品组合物宜含有本发明的添加剂，即上述的组分(i)和(ii)，按燃料重量计，其总量为0.0005～1％，宜为0.001～0.1％，优选的是0.04～0.06％。
以下实施例用来说明本发明，其中所有份数和百分数都用重量表示，数均分子量用凝胶渗透色谱法测定。
实施例A
将10公斤(3.33摩尔)含有35％(重量)醋酸乙烯酯的乙烯-醋酸乙烯酯共聚物(数均分子量3000、支链度4CH3/100CH2)装入有冷凝器的烧瓶中，並在氮气覆盖下搅拌加热到60℃。将216克(4摩尔)在1.5升正丁醇中的甲醇钠细心地加到聚合物中，随后再加入4升正丁醇。溶液从无色变成橙黄色，温度下降到46℃。然后将混合物加热到90℃，颜色变到深红色，在搅拌下在这一温度保持2小时。
然后反应混合物在104℃、370mmHg下加热，蒸出大约4升乙酸丁酯。在90℃下将剩余的粘稠聚合物倒入含有100升水和5升丙酮的酸化溶剂(有150毫升36％(重量)的盐酸溶液)中。将溶液搅拌3小时，在PH值6下将固体放置过夜。沥干后，聚合物通过细筛布过滤，並在70℃下干燥。
将20克生成的聚合物(数均分子量3300、NMR测定85％水解)溶于100毫升甲苯和10毫升吡啶的无水混合物中。滴加溶于100毫升甲苯中的30毫升十二烷酰氯，反应混合物在室温下搅拌1小时。过滤出生成的固体，真空下除去溶剂，得到粘稠聚合物。在真空中120℃下进一步干燥除去挥发物，得到21克聚合物，其中R1代表化学式为-OOCR4的基团，R4代表正十一烷基。产量21克，数均分子量5000。
实施例B
重复实施例A的第二部分，但是用十四烷酰氯酯化50克己皂化的聚合物得到一个聚合物，其中R1代表-OOCR3，R3代表正十三烷基。产量40克，数均分子量5000。
实施例C
重复实施例A的第二部分，但是用己酰氯酯化，生成的聚合物的数均分子量为3700，其中OOCR4中R4代表正戊基。
实施例D
重复实施例A第一部分的步骤，用47.5克甲醇钠和共250克正丁醇皂化450克乙烯-醋酸乙烯酯共聚物，共聚物有13.5％(重量)醋酸乙烯酯、数均分子量5000、支化度6CH3/100CH2。
将50克生成的聚合物(数均分子量4000、93％水解)溶于含有375毫升甲苯和8毫升吡啶的无水溶剂混合物中。滴加14毫升在250毫升甲苯中的己酰氯，生成的混合物在室温下搅拌5小时。过滤出固体，並在真空中除去溶剂得到粘稠聚合物，它在120℃、真空中进一步干燥，得到38克聚合物(数均分子量4000)，其中R2代表-OOCR4，R4代表正戊基。
实施例E
重复实施例A第一部分的步骤，用19.3克甲醇钠和90克正丁醇皂化100克含有29％(重量)醋酸乙烯酯的乙烯-醋酸乙烯酯共聚物(数均分子量3300、支化度4CH3/100CH2。产量74克，数均分子量3000，93％水解。
将20克生成的皂化的聚合物在室温下溶于含有150毫升甲苯和6毫升吡啶的无水溶剂中。滴加入10毫升溶于100毫升甲苯中的己酰氯，反应混合物在室温下搅拌5小时。如实施例A所述干燥产物，生成20克类似的聚合物。
实施例F
重复实施例A的步骤，但用正庚酰氯再酯化己皂化产物。
实施例G
重复实施例A的步骤，但用正辛酰氯再酯化己皂化的产物。
实施例H
将636克环己烷、148.5克丁酸乙烯酯和足够的乙烯装入3立升搅拌的高压釜中，使压力在124℃下达到97巴(9.7帕)。将18克过辛酸叔丁酯溶于85毫升环己烷中量入高压气，再加351克丁酸乙烯酯和乙烯，使上述压力维持75分钟。浸湿10分钟后，用二甲苯冲洗反应容器。蒸发溶剂后，回收992克乙烯-丁酸乙烯酯共聚物，丁酸乙烯酯含量36％，数均分子量2400。
实施例J
在1200巴、220℃下，在高压釜中聚合含醋酸乙烯酯、异丁烯和乙烯的混合物与500ppm过辛酸叔丁酯。
回收得到乙烯/醋酸乙烯酯/异丁烯三元聚合物，醋酸乙烯酯含量13.5％(重量)，异丁烯含量7.8％(重量)，9.3CH3/100CH2(NMR测定)，数均分子量5450。
实施例K
将100克乙烯-醋酸乙烯酯共聚物(醋酸乙烯酯含量36％(重量)、数均分子量3300、分支度4CH3/100CH2)倒入装有搅拌器、热电偶(连接到加热控制器上)、氮气入口和蒸镏用冷凝器的烧瓶中，並加热到60℃。加入66.46克(摩尔当量)辛酸甲酯和2.268甲醇钠(0.1摩尔当量，作为催化剂)，将混合物加热到80℃。15分钟后，将反应混合物加热到120℃，並保持在这一温度下，无色的镏出物收集在冷凝器烧瓶中。隔一定时间取聚合物样品，用比较1240厘米-1(醋酸酯基)和1170厘米-1(辛酸酯)处的红外光谱峰高度的方法跟踪酯基转移反应的进程。3.5小时后，79％的醋酸酯基被取代，並回收11克镏出物。反应在120℃下再继续5小时，此时92％的醋酸酯基已发生酯基转移。在120℃下再经过4小时后，得到18.2克镏出物。产量122克，酯基转移94％。数均分子量4250。
以下的燃料用于下列实施例中描述的试验：
    燃料     1       2     3      4      5      6     7       8      9     10     11
浊点，℃     -5     -6    -5     -3     -6     -7    -12     -3     -4     +8     -3比重       0.838  0.847  0.842  0.842  0.845  0.834  0.850  0.846  0.830  0.866冷滤点，℃   -6     -8    -6     -3     -7     -8    -12     -4     -7     +3     -4
初馏点，℃   153    154    142    180   185    111    150    174    124    241    168终馏点，℃   354    361    360    364   364    357    360    369    357    372    37190-20℃   105     80    102     82    78    126     74    110    118     67    127终馏点-90℃   24     31     32     26    35     31     36     26     31     19     41
蜡含量，     2.4    3.4    3.1    3.1   2.9    2.3    2.3    2.0    3.1    3.0    1.5在浊点以下10℃
上表中的冷过滤堵塞点(CFPP)用“石油学会杂志”第52卷第173页(1966)描述的方法测定。
实施例1
在本实施例中，86％(重量)实施例C的产物和14％(重量)实施例D的产物的掺合物(下面称为掺合物CD)按不同的添加量用于各种燃料中。所得到的CFPP下降与最初的聚合物(下面称为EVA掺合物)在相同用量下达到的CFPP下降进行了比较。
  燃料号          1    2    3    4    5    6    7     8     9    10
  用量，ppm     300  300  100  200  200  100   50   100   100   400用掺合物CD时    9    6   11    9   16    8   10    16    10    14冷滤点下降℃用EVA掺合物     7    3    8    4   11    4   12    11     7    14时冷滤点下降℃
从实验结果可以看出，在所试验的10种燃料中有8种，乙烯-己酸乙烯酯聚合物的掺合物得到比市售乙烯-醋酸乙烯酯聚合物更好的结果。
实施例2
掺合物CD本身与等量乙烯/醋酸乙烯酯共聚物(29％醋酸乙烯酯、数均分子量3300、下面称为EVA29)再掺合，得到的掺合物下面称为CD/EVA，测定各种燃料中CFPP下降。与只使用EVA29和只使用掺合物CD得到的CFPP降进行了比较。
    燃料号1      2      3      4
    总用量          300    300    100    200冷滤点下降，℃掺合物：CD                9      6     11      9EVA29             9      3      8      3CD/EVA29         10     10     13      9
实验结果表明，在许多种燃料中，本发明的组合物与市售低温流动性添加剂相比有进一步改进。
实施例3和4
在这些实施例中，测定了成核剂和防止蜡生长剂的组合对2号燃料油CFPP的影响。
使用实施例D的产物和用相同的乙烯-醋酸乙烯酯共聚物与丁酰氯再酯化得到的相应产物；将实施例D的聚合物本身，称为D6，将其丁酸酯称为D4。还使用实施例C的产物(称为C6)和用丁酰氯再酯化得到的相应产物(称为C4)。在实施例3中，使用按重量比1∶3的D6和C4的混合物，而在实施例4中，使用等量D4和C6的混合物，在每一情况中在2号燃料油中总用量为100ppm，2号燃料油的冷滤点(CFPP)为-4℃。在每一情况中冷滤点都下降到-18℃。
用100ppm乙烯-醋酸乙烯酯共聚物(29％醋酸乙烯酯、数均分子量3300)其冷滤点仅下降到-14℃，而用乙烯-丙酸乙烯酯共聚物(丙酸乙烯酯含量38％、数均分子量5200)，冷滤点仅下降到-4℃。
实施例5和6
这些实施例说明本发明的两种组合物对11号燃料冷滤点的影响。
使用乙烯-醋酸乙烯酯共聚物(醋酸乙烯酯13.5％、数均分子量5000)作为成核剂，即低酯含量聚合物。在实施例5中使用实施例H中的产物作为防止蜡生长剂，即高酯含量聚合物。在实施例6中，使用通过实施例A第1部分描述的方法皂化，並用该实施例描述的相同方法(但用丁酰氯)再酯化制备的产物。
在这两个实施例中，使用25ppm乙烯/醋酸乙烯酯共聚物成核剂，而每次使用的防止蜡生长剂为75ppm。
      实施例      冷滤点，℃
      5              -17
      6              -21
实施例7和8
在这些实施例中，在11号燃料中使用实施例J的产物作为成核剂。在实施例7中，防止蜡生长剂是实施例H的产物，而在实施例8中，使用与实施例6相同的防止蜡生长剂。在实施例7和8中，成核剂的用量都为25ppm，防止蜡生长剂的用量都为75ppm。
         实施例    冷滤点，℃
          7             -17
          8             -18

Claims (28)

1.一种添加剂组合物，含有：
(i)一种油溶性乙烯共聚物，它除了有由乙烯衍生物的结构单元外，还有7.5-35％(摩尔)的下式(I)的结构单元；
-CH2-CRR1-    (I)
(ii)一种油溶性乙烯共聚物，它除了有由乙烯衍生的结构单元外，还有至多10％(摩尔)的下式(II)的结构单元，
-CH2-CRR2-    (II)其中R各自独立代表H或CH3，R1和R2各自独立代表式COOR3和OOCR4的基团，其中R3和R4各自独立地代表烃基，附加条件是R1和R2不同时为乙酸酯基，聚合物(i)中结构单元I的量至少比聚合物(ii)中的结构单元II多2％(摩尔)，其中该组合物也含乙烯-乙烯基酯共聚物。
2.按照权利要求1的组合物，其中R3和R4都代表至少有4个碳原子的直链烷基。
3.按照权利要求1或2的组合物，其中R3和R4有至多30个碳原子。
4.按照权利要求1或2的组合物，其中R1和R2都代表-OOCR4。
5.按照权利要求1的组合物，其中R代表H。
6.按照权利要求1的组合物，其中R1和R2都代表式OOCR4的基团，其中R4代表有5-13个碳原子的烷基。
7.按照权利要求1的组合物，其中聚合物组分(i)的数均分子量至多为14000。
8.按照权利要求8的组合物，其中数均分子量为2000-5500。
9.按照权利要求1的组合物，其中聚合物组分(ii)的数均分子量至多为20000。
10.按照权利要求9的组合物，其中数均分子量为3000-10000。
11.按照权利要求1的组合物，其中式I的结构单元相当于聚合物(i)的11-16％(摩尔)，而式II的结构单元相当于聚合物(ii)的3.5-7.0％(摩尔)。
12.按照权利要求1的组合物，其中至少一种聚合物是由乙烯-不饱和酯共聚物的皂化和再酯化制得的。
13.按照权利要求1的组合物，其中R1和R2都代表-OOCR4，而聚合物是由乙烯-乙酸乙烯酯共聚物的皂化和再酯化制得的。
14.按照权利要求1的组合物，其中乙烯-乙烯基酯共聚物是乙烯-乙酸乙烯基酯共聚物。
15.按照权利要求14的组合物，其中乙烯-乙酸乙烯酯共聚物含7.5-35％(摩尔)乙酸酯单元。
16.按照权利要求1的组合物，它还含有一个下式的梳状聚合物
Figure C9310771300031
其中D为R11、COOR11、OCOR、R12COOR11或OR11，
E为H、CH3、D或R12，
G为H或D，
J为H、R12、R12COOR11或芳基或杂环基，
K为H、COOR12、OCOR12、OR12或COOH，
L为H、R12、COOR12、COOH或芳基，
R11为大于或等于10个碳原子的烃基，
R12为大于或等于1个碳原子的烃基，
m和n代表摩尔比，m在1.0-0.4范围内，n在0-0.6范围内。
17.按照权利要求16的组合物，其中梳状聚合物是乙酸乙烯酯和富马酸酯的共聚物。
18.按照权利要求17的组合物，其中酯基是有12-20个碳原子的烷基。
19.按照权利要求18的组合物，其中酯基由有14个碳原子的醇或有14和16个碳原子的醇的混合物衍生得到。
20.按照权利要求1的组合物，它含有两种或两种以上不同的梳状聚合物的混合物。
21.按照权利要求20的组合物，其中混合物含有
(i)富马酸C14酯-乙酸乙烯酯共聚物和
(ii)富马酸C14/C16酯-乙酸乙烯酯共聚物。
22.按照权利要求1的组合物，它还含有极性含氮化合物。
23.一种含有如权利要求1的添加剂组合物的燃料或润滑油组合物。
24.按照权利要求23的组合物，它含有按油品重量计总量为0.005-1％的添加剂组合物。
25.按照权利要求24的组合物，它含有按油品重量计总量为0.001-1％的添加剂组合物。
26.按照权利要求25的组合物，它含有按油品重量计总量为0.004-0.06％的添加剂组合物。
27.一种含有在油中或在与油混溶的溶剂中的权利要求1定义的添加剂组合物的添加剂浓缩剂。
28.权利要求1的添加剂组合物在改进油品的低温性质中的应用。
CN93107713A 1992-06-30 1993-06-29 添加剂组合物、油品组合物、添加剂浓缩物及用途 Expired - Lifetime CN1079410C (zh)

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DE4042206A1 (de) * 1990-12-29 1992-07-02 Hoechst Ag Terpolymerisate des ethylens, ihre herstellung und ihre verwendung als additive fuer mineraloeldestillate
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GB9213909D0 (en) * 1992-06-30 1992-08-12 Exxon Chemical Patents Inc Oil additives and compositions

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ATE247704T1 (de) 2003-09-15
EP0739971A3 (en) 1997-02-19
EP0741181A2 (en) 1996-11-06
ATE149199T1 (de) 1997-03-15
JPH07508776A (ja) 1995-09-28
AU4561093A (en) 1994-01-24
EP0648258B1 (en) 1997-02-26
CA2137140C (en) 2004-10-05
ATE256723T1 (de) 2004-01-15
EP0741181B1 (en) 2003-12-17
CN1081691A (zh) 1994-02-09
WO1994000386A1 (en) 1994-01-06
GB9213904D0 (en) 1992-08-12
DE69333368D1 (de) 2004-01-29
US5554200A (en) 1996-09-10
DE69333156D1 (de) 2003-09-25
DE69333156T2 (de) 2004-06-09
CA2137140A1 (en) 1994-01-06
KR950702231A (ko) 1995-06-19
RU95109161A (ru) 1996-12-10
JP3372253B2 (ja) 2003-01-27
DE69308304T2 (de) 1997-06-05
EP0739971A2 (en) 1996-10-30
EP0741181A3 (en) 1997-02-19
KR100295920B1 (ko) 2001-10-24
EP0648258A1 (en) 1995-04-19
DE69333368T2 (de) 2004-10-07
DE69308304D1 (de) 1997-04-03
EP0739971B1 (en) 2003-08-20

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