CN1219951A - 柴油燃料和润滑油消泡剂及其使用方法 - Google Patents

柴油燃料和润滑油消泡剂及其使用方法 Download PDF

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Publication number
CN1219951A
CN1219951A CN97195053A CN97195053A CN1219951A CN 1219951 A CN1219951 A CN 1219951A CN 97195053 A CN97195053 A CN 97195053A CN 97195053 A CN97195053 A CN 97195053A CN 1219951 A CN1219951 A CN 1219951A
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Prior art keywords
modified polyorganosiloxane
organic modified
formula
propane
polymkeric substance
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CN1090229C (zh
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W·格拉伯斯基
R·豪布里希斯
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General Electric Co
Lanxess Solutions US Inc
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Witco Corp
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Abstract

本发明涉及柴油燃料和润滑油消泡剂,和原油破乳剂,以及这些药剂的使用方法。具体地说,这些消泡剂和破乳剂由共聚物组成,该共聚物有构成聚硅氧烷主链的结构,并有一个有机基团接枝到该主链上。这些结构包括通式MDxD′yD″zM的一种聚合物,式中M是O.5Si(CH3)3、D是一个OSi(CH3)2、D′是OSi(CH3)R、D″是OSi(CH3)R′、R是一个多羟基C6～C28有机基团、R′是一种苯酚衍生物或一个长链脂肪族基团或聚醚、z是0－80、x+y+z是10～200、x/z≥1且x/(y+z)是约1～约5;或者通式M′DaM′的一种聚合物,式中M′是O.5Si(CH3)2R,a是4－10,且R和D与以上定义的相同。

Description

柴油燃料和润滑油消泡剂及其使用方法
                     发明背景
1．发明领域
本发明涉及石油产品(如柴油和润滑油)消泡剂和原油破乳剂，及其使用方法。
2．相关技术描述
柴油燃料是各种烃类的混合物。这些烃类大多数是脂肪族的，但也可能有占该燃料的可多达20～25％(重量)的芳香烃存在。该混合物也会包含煤油或粗柴油。柴油燃料常用于机动车辆，而且当它注入机动车辆的燃料箱中时有产生大量泡沫的趋势。因此，理想的是减少这样的发泡，这可以通过添加一种消泡剂来实现。
石油公司用有机添加剂例如洗涤剂、鲸蜡烷改进剂、减粘剂和偶尔用香料(总称“DAP”)处理柴油燃料。每家石油公司都有它自己偏爱的DAP，各该公司典型地只用这种DAP来与它自己的燃料混合。这些有机添加剂全部必须与该消泡剂兼容。
送到各加油站的柴油燃料也可能含有一定量的分散水或溶解水，这会对以前已知的消泡剂的性能特征产生有害影响。这种水引起消泡特征衰减，而且在一些极端情况下可能使该消泡剂增强发泡而不是抑制发泡。这样的湿消泡剂也会导致增加燃料箱中的油泥沉积。
授予Adams等人的美国专利No.4,690,688公开了一种用作消泡剂的典型先有技术聚硅氧烷，其中，该聚硅氧烷是一种有聚酯侧链的共聚物，这些侧链占该共聚物的至少25％(重量)。然而，这些聚硅氧烷共聚物对湿柴油燃料不太管用，因为作为一种亲水物质，这些醚类将倾向于稳定湿燃料的发泡。此外，为了恰如其分地起作用，这些聚硅氧烷在柴油燃料中的存在水平必须高于在发动机***中的理想水平。
DE 4032006描述了通过添加一种含有带不饱和侧链的有机聚硅氧烷的泡沫抑制剂，使包括柴油在内的有机体系消泡和/或脱气的一种工艺。这种泡沫抑制剂的一个缺点是它含有高水平的硅，这会有害于发动机。此外，它可能与DAP不兼容，而且熟化得不太好。
润滑油往往包含一种烃类基料(例如矿物油)和润滑性能增强成分(例如酯类)的混合物。例如，典型的油含有高度精制的石蜡烃原料，或合成聚烯烃。在施用和使用期间(例如，在使齿轮箱或涡轮润滑时)，这样的润滑油产品有大量产生泡沫的趋势。这样的发泡，与运动机械零件截留空气的倾向相结合，会对润滑性产生有害影响，这对快速运动的机械零件会是有害的。润滑油的泡沫减少和迅速脱气是对润滑油使用的一个严格技术要求。
标准硅油可以用来防止润滑油发泡，而且在很低添加率(约10～20ppm)时就是高效消泡剂。然而，它们的使用通常导致一种所不希望的低脱气率。硅油消泡剂效率越高，脱气问题就越显著。例如，硅油典型地在通入的空气流关掉之后约10分钟内就能夹持和截留空气。
有机消泡剂(例如，目前技术上流行的聚丙烯酸酯基消泡剂)是有效的润滑油消泡剂，其浓度为约100～200ppm。然而，它们作为消泡剂的效率在浓度为约10～50ppm时是非常低的。虽然有机消泡剂提供令人满意的脱气速度，但处理速度高到所不希望的程度，甚至比硅油的处理速度高若干倍。
在测试这些当前消泡剂时，让一股强空气流在预定时间内通入油内，并测定这样的泡沫油密度随时间的变化。所形成泡沫的密度比新鲜无气油的密度低得多。脱气起快，意味着诸如10分钟后油的密度越高。因此，对于一种密度为0.872的油来说，由于空气搅入泡沫中的缘故，初始泡沫密度是0.810；10分钟后它又达到其未处理油的原来数值，而用10ppm硅油或200ppm有机消泡剂处理的油10分钟后的密度分别为0.832和0.844。
一般不说，在石油工业中，在油从炼油厂中装运之前，它必须通过一个破乳过程，从而使所不希望的水从原油中分离、除去。目前，破乳是用数量约100ppm的一种有机破乳剂例如TROS公司生产的TROS6002X进行的。这种有机破乳剂通常溶解在一种芳香族化合物中，然后添加到原油中进行破乳。破乳剂的数量取决于原油类型和原油中水的数量。
                     发明概要
因此，本发明的目的包括针对以上所述技术上的问题的消泡剂开发。
在一种实施方案中，本发明期待一类可以用来减少柴油和润滑油等石油产品的发泡的有机硅氧烷共聚物。这些共聚物有构成聚硅氧烷主链而且有一种有机基团接枝到主链上的结构。因此，本专利中，共聚物这一术语旨在涵盖有机改性的聚硅氧烷。具体地说，这些消泡剂可以包含一种通式MDxD′yD″zM的聚合物，式中M是O0.5Si(CH3)3；D是一个OSi(CH3)2；D′是OSi(CH3)R，其中R是一个多羟基(即含有至少2个羟基)C6～C28有机基团、其分子量较好在约134与约644之间，而且是完全饱和的；D″是OSi(CH3)R′；其中R′是一种苯酚衍生物或一个长链(C10-C20)脂肪族基团或聚醚；z是0～80、x+y+z是10～200(且较好的是20～160)；x/z≥1；且x/(y+z)是约2.0～约10.0(且较好的是约3.0～约6.0)。这种聚合物应当以足以减少石油产品发泡的数量(即有效量)存在，较好的是以约1.0～约5.0ppm存在，这导致Si水平为约0.22～约1.10ppm。
除以上通式外，这些消泡剂还可以包含一种通式M′DaM′的聚合物，式中M′是O0.5Si(CH3)2R，R和D的定义同上，且a是4～10(且较好的是5～8)。这种聚合物应当以足以减少石油产品发泡的数量存在，且较好的是以约4ppm存在。这些消泡剂可以包含要么通式MDxD′yD″zM要么通式M′DaM′各自单独的聚合物，也可以包含两者的混合物。
在一种相关的实施方案中，本发明涉及减少石油产品发泡的方法。这些方法包括向石油产品(例如柴油燃料和润滑油)中添加一种组合物，其中以能有效减少石油产品发泡的数量(如以上所述)包含通式MDxD′yD″zM(如以上所述)和/或通式M′DaM′(如以上所述)的聚合物。
本发明的一个进一步目的是提供能证实有可接受高脱气速度的润滑油消泡剂。因此，在另一种实施方案中，本发明期待一类可用来使润滑油消泡的有机硅氧烷共聚物。这些共聚物可以包含通式MDxD′yD″zM(如以上所述)和/或通式M′DaM′(如以上所述)的一种聚合物，而且其存在量应当足以进行润滑油消泡，较好的是低于100ppm，更好的是20～50ppm。这些消泡剂可以包含要么通式MDxD′yD″zM要么通式M′DaM′各自单独的聚合物，也可以包含两者的混合物。
在一种相关实施方案中，本发明涉及润滑油消泡方法。这些方法包括向润滑油中添加一种组合物，其中，以足以进行润滑油消泡的数量，较好的是20～50ppm，含有通式MDxD′yD″zM(如以上所述)或通式M′DaM′(如以上所述)的一种聚合物。
本发明的一个进一步目的是开发针对以上所述技术上的问题的原油破乳剂。因此，在另一种实施方案中，本发明期待一类可以用来使原油破乳的有机硅氧烷共聚物。这些共聚物可以包含通式MDxD′yD″zM(如以上所述)和/或通式M′DaM′(如以上所述)的一种聚合物，而且其存在量应当足以进行原油破乳，较好的是约5ppm。这些乳化剂可以包含要么通式MDxD′yD″zM要么通式M′DaM′各自单独的聚合物，也可以包含两者的混合物。
在一个相关实施方案中，本发明涉及原油破乳方法。这些方法包括向原油中添加一种组合物，其中，以足以进行原油破乳的数量，较好的是约5ppm，含有通式MDxD′yD″zM(如以上所述)或通式M′DaM′(如以上所述)的一种聚合物。
本发明的共聚物中很多本身是新型化合物，不管它们作为柴油燃料或润滑油的消泡剂稳定性如何。在R基团是一种烷氧基化烯丙基山梨糖醇衍生物、一种烷氧基化季戊四醇衍生物、一种烷氧基化或非烷氧基化三甲基丙烷衍生物的情况下，尤其如此。
                 本发明的详细描述
本发明的共聚物组合物包括以上所述R的低分子量有机残基。这些有机侧链的羟基产生高极性。在一些特定的情况下，含有两个或多个羟基的分子的极性可以通过使一个多羟基基团转化成相应的缩醛或缩酮来调节(即减少)。
这里所描述的共聚物考虑到柴油燃料中的低处理率，这对应于燃料中非常低的硅水平(例如，低达0.5ppm)。因此，人们可以期待当前使用的消泡剂所产生的问题的完全消除或实质性减少。此外，本发明的共聚物在有水分散或溶解的柴油中显示高稳定性。
本发明的这些优点之所以成为可能，是由于低分子量、緻密、高极性有机基团共接枝到硅氧烷主链上。这些有机基团的取代，令人惊讶地提高了该共聚物的消泡能力，因为它提高了消泡效率而且有助于保持该共聚物在有水分散或溶解的柴油燃料中的性能特征，而且因为它使得在低硅浓度时就能完全消除泡沫。
此外，本发明提供一种在100ppm或更低、较好50ppm或更低的浓度就有效的、全新的润滑油消泡剂结构。
此外，本发明还提供一种全新的原油破乳剂结构，它与以前已知的破乳剂相比的优异之处在于它在非常低的数量例如10ppm时就有效，而以前已知的破乳剂只有当以约100ppm的数量存在时才有效。
共聚物的结构
对于消泡剂来说，本发明的这一类有机硅氧烷共聚物的特征在于组合了高摩尔分数的D单元，和存在着低分子量、緻密、高极性的有机基团。本发明的这些有利性能可以通过仔细选择以上所述的通式MDxD′yD″zM和/或通式M′DaM′的硅氧烷主链来实现。尽管这里专门提到了线型结构，但本发明也期待T结构和Q结构。
改变这种聚硅氧烷的分子量一般不会改变该聚合物性能，但确切地说，x+y+z的上限决定于操作非常粘的硅烷的技术能力，而分子量下限决定于这样一个事实：在尺寸较小的共聚物中；改性基团的分布可能造成一些共聚物没有改性基团，在这种情况下所得到的材料有一部分可能成为要么是惰性的要么可能增强发泡的非改性硅油。本发明偏爱x+y+z之和介于约10至约200之间，但熟悉本门技术的人员会明白，生产能力的改善会允许在这个范围之外使用共聚物。
本发明的聚硅氧烷共聚物组合物的物理性能决定于硅氧烷链的尺寸、不同于甲基的有机基团的取代度和取代聚硅氧烷中原甲基基团的有机残基的性质(极性)等变量。
本发明期待的有机基团(R)主要是脂肪族低分子量二醇。这个有机基团的分子量较好的是约134～约644，更好的是约134～约400。此外，该有机基团是完全饱和的。在接枝之前，该有机基团R带有一个不饱和端子，例如一个烯丙基、甲基烯丙基或乙烯基。例如，该端子可以是一个烯丙基、一个甲基烯丙基或一个乙烯基。当该有机基团被硅氢化到硅氧烷主链上时，这个不饱和端子就变成饱和的。因此，所得到的硅氧烷共聚物没有任何不饱和。
在聚硅氧烷上接枝的有机基团可以用溶解度参数来描述，该参数是一个热力学尺度而且是内聚力的指示。溶解度参数可以从已知数据表计算。人们普遍公认的是，某一种化合物的溶解度参数值越高，对应于该化合物的极性就越高。然而，高极性不一定意味着一种物质将有高亲水性，即使反过来是真的：高亲水性物质有高极性。因此，烷基苯酚衍生物(例如丁子香酚)有高极性但不溶于水。
以下表1提供若干溶解度参数。
                   表1三(羟甲基)丙烷一烯丙基醚               25.3乙氧基化季戊四醇烯丙基醚               25.3丙氧基化季戊四醇烯丙基醚               23.6三(异丙醇)胺烯丙基醚                   20.3甘油一烯丙基醚                         27.1
较好的溶解度参数范围为23～35。
为了比较，烯丙醇上7摩尔甲基封端环氧乙烷加成物的溶解度参数为18.2，而环氧乙烷的溶解度参数为19.2。
该有机基团预期为脂肪族多羟基基团、其烷氧基化衍生物或者也可以是在甲醛与多羟基物的反应中得到的环状缩醛(甲缩醛)。较好的是，R基团的前体是三(羟甲基)丙烷一烯丙基醚。然而，该R基团的前体可以是乙氧基化的季戊四醇烯丙基醚、丙氧基化的季戊四醇烯丙基醚、三(异丙醇)胺烯丙基醚，或烯丙基丙烷-1,3-二醇。通过多羟基化合物与甲醛的反应，可以使二醇转化成对应的环状甲缩醛，而所得到的环状烯烃可以接枝到硅氧烷主链上。适合于用作R基团的化合物可购自诸如瑞典的Perstorp AB公司。
如同熟悉本门技术的人员会明白的那样，该R基团应当选择得使所得到的有机硅氧烷共聚物在柴油和水中都不可溶。因此，R基团的选择必须根据硅氧烷主链的尺寸来平衡，以达到所希望的亲水/疏水平衡。
例如，通过改变有机硅氧烷的总尺寸，即x+y+z，硅氧烷基团的比值，即x/(y+z)，和接枝基团R的性质，人们可以设计一种适用于特定燃料等级、特定发动机***和特定使用条件的共聚物。x/(y+z)比值定义由给定的一组接枝基团构成的共聚物的亲水性能，而且可以按照要使用该共聚物的燃料的含水量来调整。
例如，本发明期待的一个小R基团是烯丙基丙烷-1,3-二醇，而一个大R基团是乙氧基化的烯丙基山梨糖醇。本发明的有机硅氧烷中很多本身是新型化合物，在R基团是乙氧基化的烯丙基山梨糖醇的情况下尤其如此。
一个特别好的R基团是三(羟甲基)丙烷一烯丙基醚(TMPMAE)。可用于本发明的其它R基团包括乙氧基化的季戊四醇烯丙基醚、丙氧基化的季戊四醇烯丙基醚、三(异丙醇)胺烯丙基醚、和烯丙基丙烷-1,3-二醇。TMPMAE及其衍生物，对于相同的硅氧烷主链来说，比聚醚衍生物提供更多的表面活性，尽管事实上TMPMAE有更高的极性。相信这是由于TMPMAE的紧凑分子结构的缘故。
例如，在消泡剂和原油破乳剂两者的一种较好组合物中，x是100，y是24,z是0，且R是TMPMAE。类似地，在另一种较好的组合物中，R是TMPMAE，且a是约7.0。这些较好组合物的独特结构之所以特别有利，就在于在不同类型的表面上该组合物的吸附得到加强。此外，一些矿物表面例如膨润土，及其它表面例如织物、纸张和混凝土，可通过这些组合物的吸附而成为疏水的。这种较好组合物在玻璃板上的吸附导致玻璃表面能的实质性降低。事实上，估计该玻璃的表面张力从约72达因/cm下降到约30达因/cm。本发明的组合物的如此高表面活性可以解释它们在消泡和破乳方面的效率。然而，本发明的硅氧烷的极低浓度使得不容易进行作用机制细节的调研。与固体表面上的吸附有关的观测可以认为是平行于在燃料或原油中发生的而且与界面上个别分子间相互作用有关的现象的。
该共聚物的制造
消泡剂和破乳剂的制造方法在本技术中是已知的。例如，美国专利No.3,794,693公开了如何制作共聚物组合物。
在制造过程中，往往有利的是添加一种溶剂，以确保在整个反应过程中反应物能充分混合。用于这些目的溶剂包括DPG(二聚丙二醇)、甲苯和任何有适当溶解度特征的其它溶剂，例如2-乙基己醇、异丙醇，各种芳香族溶解例如Solwesso 150，脂肪族酯醇例如Texanol(2,2,4-三甲基-1,3-戊二醇-异丁酸酯)，异佛尔酮，这些的混合物等。利用本发明的共聚物，不一定要除去溶剂才能使该共聚物有效地作为消泡剂。然而，为了安全运输起见，也可以脱除甲苯、异丙醇等挥发性溶剂。非挥发性溶剂或高闪点溶剂(如DPG和乙基己醇)不会引起同样的安全问题，没有必要将其脱除。
本发明的组合物中有一些(例如较好的组合物)是疏水的，当引进水中时将作为白色凝胶沉淀出来。
该共聚物的使用
对于消泡剂来说，改性聚硅氧烷典型地是与DAP(有市售)掺合的，并在炼油厂添加到石油产品中。对于破乳剂来说，聚硅氧烷共聚物被溶解在一种芳香族化合物中，然后添加到原油中。
本发明的聚硅氧烷共聚物应当以约5ppm添加到柴油中。较好的是，使用最小量的聚硅氧烷共聚物，较好的添加范围是2ppm～4ppm。本发明的聚硅氧烷应当以约10ppm～约50ppm添加到原油中，以提供原油与水含量的充分分离。
该共聚物的特征
溶解度模式、分子量分布和表面张力降低是可用来评价本发明组合物的物理性能。
表2揭示从MD100D*24M硅烷(D*=HSiOCH3)和作为唯一取代基的TMPMAE制作的本发明的有机硅氧烷之一的溶解度模式。
                       表2从MD100D*24M和TMPMAE制成的有机硅氧烷的溶解度模式溶剂             MD100D′24M的浓度：
            1％   5％   10％  20％  50％柴油            No    No    No    No    No2-乙基己醇      Yes   Yes   Yes   Yes   Yes二甲苯          No    No    No    No    YesSolvesso 100    No    No    No    No    YesSolvesso 150    No    No    No    No    Yes碳酸丙二醇酯    No    No    No    No    NoVammar D 10N    No    No    No    No    NoYes=在环境条件下溶于溶剂中No=在环境条件下不溶于溶剂中
以下说明性实例和比较例更详细地描述本发明。然而，它们无意限制本说明书和权利要求的范围。
                      实例
有机硅氧烷实例
实例1
每克含有2.5×10-3摩尔活泼氢的平衡物MD100D*24M(D*=HSiOCH3)与占总加料量50％的TMPMAE和二聚丙二醇掺合。采用30％摩尔过量的烯丙基键。反应用15ppm以氯铂酸溶液形式添加的铂催化。产生15度放热，反应在45分钟内完成。
此产物以相当于1.1ppm硅的浓度用作柴油燃料消泡剂。记录消泡性能。实际上没有泡沫形成。
实例2
每克含有2.5毫摩尔活泼氢的平衡物MD44D*11M与TMPMAE和二聚丙二醇掺合，反应在70℃用15ppm铂触发。在几分钟内展现约15度放热，反应在不到45分钟内完成。
此产物以1.1ppm硅的浓度施用于柴油燃料中时显示出优异的性能特征，因为初始泡沫体积减少到约20％，消泡时间是空白(标准)的约10％。
实例3
每克含有2.5毫摩尔活泼氢的平衡物MD100D*24M与TMPMAE和由七摩尔环氧乙烷组成并以甲基封端的聚醚(60/40摩尔比)以及作为反应溶剂的DPG掺合。反应在70℃用15ppm铂触发。在几分钟内就展现出约15度的放热，反应在不到45分钟内完成。
反应产物作为一种消泡剂应用于在法国市场上可以买到的柴油之一中。此产物显示出与实例1类似的消泡特征。这两种产物以0.5ppm Si的浓度施用时都能消除实际上所有泡沫，因为泡沫体积低于5％，消泡时间是1～4秒。
实例4
每克含有2.5毫摩尔活泼氢的平衡物MD100D*24M与TMPMAE和由七摩尔环氧乙烷组成并以甲基封端的聚醚(50/50摩尔比)以及作为反应溶剂的2-乙基己醇掺合。反应在70℃用15ppm铂触发。在几分钟内就展现出约15度的放热，反应在不到45分钟内完成。
反应产物作为一种消泡剂应用于法国市场上可以买到的柴油之一。此产物显示出与实例1类似的消泡特征。这两种产物以0.5ppm Si的浓度施用时都能消除实际上所有泡沫，因为泡沫体积低于5％，消泡时间是1～4秒。
比较例(DE 4032006)
实例2中所述的平衡物用二噁烷稀释，添加足够量的丁-2-炔-1,4-二醇。反应用德国专利(DE 4032006-A)中所述的催化剂催化。需要约40小时和过量催化剂与丁炔二醇才能使反应完成。
在柴油中以高出约40％的硅浓度达到了与实例1同样的性能。
在所有制备中，都采用30％摩尔过量的不饱和键。
柴油消泡性能
柴油消泡剂的性能是根据向量筒注入100毫升燃料所得到的泡沫体积或者在量筒中出现清晰燃料表面所需要的时间来评价的。消泡时间往往表示为空白、未处理燃料样品所需时间的百分率。在这种情况下，数值越低，表明泡沫塌陷越快，且消泡剂效率越高。
引进燃料中的硅的数量应当尽可能低，但通常是消泡剂的效率随燃料中硅量增加而增加。柴油燃料很经常用DAP添加剂处理，这些添加剂是为了改善发动机性能而引进燃料中的。因此，重要的是，施用的消泡剂在DAP的存在下应当保持其性能特征。
表3记录了与用脂肪族二醇(包括TMPMAE、烯丙基甘油、二醇的环状衍生物)作为唯一接枝基团制成的本发明组合物的几个实例和用丁-2-炔-1,4-二醇的比较例有关的数据。也包括一个用聚醚作为接枝基团的实例，所有有机硅氧烷都用反应溶剂稀释，是按照以上实例1～3中所述的程序制备的，而且以10ppm处理率施用，而不管该分子中的硅含量如何。
                         表3
不同结构的柴油消泡剂的性能，全部以10ppm测试(产品用反应溶剂稀)硅氧烷主链    接枝的烯烃            参照              相对泡沫塌陷时间(％)无            无                    空白              100MD100D*24M   聚醚/丁子香酚         SAG TP-325,       24
                                市售MD100D*24M   TMPMAE                  A               2MD100D*24M   TMPMAE/聚醚             B               4
          (60/40 mol)MD102D*18M   TMPMAE                  C               1MD44D*11M    烯丙基甘油甲缩醛        D               94MD44D*11M    TMPMAE的甲缩醛          E               88MD44D*11M    烯丙醇上加成了七摩尔    F               46
          环氧乙烷的聚醚MD44D*11M    丁-2-炔-1,4-二醇        G               2MD44D*11M    烯丙基甘油              H               2MD44D*11M    TMPMAE                  I               6MD48D*12M    TMPMAE                  J               16MD42D*7M     TMPMAE                  K               13
所使用的燃料是从壳牌公司得到的，是一种会大量发泡的柴油，100毫升液体会产生约217毫升泡沫，消泡时间约60秒。对于有聚醚和环状甲缩醛取代的硅氧烷来说，记录到性能的大幅度丧失。对于相同摩尔分数的D单元来说，用一种环状甲缩醛代替二醇会使硅氧烷的总体极性大大降低。使用一种从7摩尔环氧乙烷制成的无封端聚醚，使D单元的摩尔分数从约80％减少到50％。如表3中所示，使用封端的聚醚代替未封端的聚醚导致同样的普通性能。
处理率调整到相同硅含量时，改变了消泡剂的效率顺序。SAG TP-325(即，最先进的商用柴油燃料消泡剂；WITCO OrganoSilicone公司制)用来作为10ppm处理率的参照，这对应于向燃料中引进0.90ppm硅。使用来自壳牌公司的同种柴油，全部以0.90ppm硅施用的不同消泡剂的结果列于表4中。
                         表4燃料中0.90ppm硅的柴油消泡剂的性能
    参照 泡沫体积(毫升) 相对塌陷时间％ 塌陷时间(秒)
    空白     217     66
    TP-325     150     24     16
    A     113     15     10
    G     123     20     13
    H     105     3     2
    I     110     8     5
(参照物A、G、H和I与表3中相同)。
显而易见，含有残留不饱和的材料G的工作性能不如用已饱和烯烃制成的消泡剂。结构G、H和I全都用相同的硅氧烷主链制成。
也可以证实，含有残留不饱和的有机硅氧烷对DAP组分更敏感，在老化期间，它的性能将迅速下降。
表5显示TMPMAE衍生物的柴油消泡剂的结构和性能，用泡沫体积表示。当泡沫体积值等于或小于105毫升(即，约100毫升～约105毫升燃料)时，这是实际上基本上不产生泡沫的指示。反之，超过105毫升的泡沫体积表明有机硅氧烷消泡剂的消泡特征不能令人满意。消泡剂的稳定性能，在所配制的燃料可能要贮存若干周后才使用的情况下，是特别重要的。实例G和G型是有残留不饱和的有机硅氧烷，而且对应于以上比较例的描述。对于G型衍生物，看到了这种性能的损失。这种性能降级因DAP的存在而得到加强。
对于要么未被处理要么含有某种DAP的各种燃料，实测了以下表5中所列的泡沫体积。没有考察等于或小于105毫升的泡沫体积的塌陷时间，因为对于这些数值来说基本上没有发泡。
                         表5
100％用TMPMAE取代的柴油消泡剂的结构与性能，用泡沫体积表示参照    柴油类型    DAP    燃料中的    第0天体积    第17天体积    第42天体积
                ppm    Si,ppm       (毫升)       (毫升)        (毫升)TP-325    D1        200    0.45           130         130             +A         D1        200    0.22           105          +              +A         D1        200    0.55           105          +              +B         D1        200    0.50           105          +              +G型       D1        200    1.00           102          110            +B         D2        无     0.50           105          130(*)        160(**)G型       D2        无     0.50           105          177(*)        183(**)I         D3        无     0.90           110          120            127G         D3        无     0.90           120          140            173G型       D3        无     0.90           105          208            205I         D4        1000   0.90           105          110            140G         D4        1000   0.90           167          190            190G型      D4         1000   0.90           110          160            180
+=无数据可用；(*)=15天；(**)=32天；
(参照A、B、G和I与表3中相同)。柴油D1中的实例是要显示新结构的效率与硅含量的关系。
表6显示TMPMAE衍生物的分子量分类，表7显示其性能分类(其中，数值越低表明消泡效率越高)。表6和7也描述聚硅氧烷的总尺寸，D/D′比值，和产品活性(稀释度)。
                        表6(TMPMAE)按分子量分类
    硅氧烷 总D+D′(M′)  D/D′(M′)     合成N° ％活性    性能1)
    M′D2M′     2     1     RH 368-202     80     95％
    M′D3M′     3     1.5     MG 261     80     99％
    M′D4M′     4     2     RH 368-248     75     72％
    M′D5M′     5     2.5     MG 289     80     58％
    M′D8M′     6     3     MG 292     80     94％
    M′D7M′     7     3.5     MG 295     80     47％
    M′D10M′     10     5     PH 368-288     50     89％
    MD8D*2M     10     4     RH 17122-4     50     62％
    M′D15M′     15     7.5     RH 368-289     50     96％
    M′D20M′     20     10     RH 368-290     50     100％
    MD′16D*4M     20     4     RH 17122-5     50     18％
    MD24D*6M     30     4     RH 17122-6     50     12％
    MD42D*7M     49     6     RH 368-214     50     13％
    MD44D*11M     55     4     RH 368-260     50     6％
    MD48D*12M     60     4     RH 368-203     50     16％
    MD102D*18M     120     5.7     RH 368-212     50     1％
    MD100D*24M     124     4.2     RH 368-170     50     2％
注：1)性能用相对塌陷时间衡量。
                         表7按性能分类
    硅氧烷 总D+D′  D/D′(M′)     合成N° ％活性   性能1)
    M′D20M′     20     10     RH 368-290     50     100％
    M′D3M′     3     1.5     MG 261     80     99％
    M′D15M′     15     7.5     RH 368-289     50     96％
    M′D2M′     2     1     RH 368-248     80     95％
    M′D6M′     6     3     MG 292     80     94％
    M′D10M′     10     6     RH 368-288     50     89％
    M′D4M′     4     2     RH 368-202     75     72％
    MD8D*2M     10     4     RH 17122-4     50     62％
    M′D5M′     5     2.5     MG 289     80     58％
    M′D7M′     7     3.5     MG 295     80     47％
    MD16D*4M     20     4     RH 17122-5     50     16％
    MD48D*12M     60     4     RH 368-203     50     16％
    MD42D*7M     49     6     RH 368-214     50     13％
    MD24D*6M     30     4     RH 17122-6     50     12％
    MD44D*11M     55     4     RH 368-260     50     6％
    MD100D*24M     124     4.2     RH 368-170     50     2％
    MD102D*18M     120     5.7     RH 368-212     50     1％
注：1)在壳牌柴油中以10ppm和20℃测试的(相对塌陷时间)，性能是用相对塌陷时间
 衡量的。原油破乳性能
用来自Trecate油田(意大利北部)的原油进行了几个实验。把水的浓度调整到20％，并搅拌原油以形成乳液。记录分离水体积随时间的变化。参照物是来自TROS公司的一种有机破乳剂。
数字列于表8中。
                          表8
                   Trcate原油分离速率
样品
               5分钟   10分钟  15分钟   30分钟   60分钟  120分钟10ppm TROS 6002X    0        0       5        5        5       5100ppm TROS 6002X   40       41      41       41       42      4210ppm RH 265        0        0       5        25       35      37MD100D′24M         25       33      35       38       38      4010ppm RH 273        0        5       25       30       35      3710ppm RH 275        0        0       0        0        5       10MD42D*7M           0        0       0        0        0       0
RH265=MD44D*11M+由7摩尔环氧乙烷组成并以烯丙基和甲基封端的聚醚
MD100D′24M=以上有机硅氧烷实例中的实例1
RH273=MD44D*11M+TMPMAE(如以上有机硅氧炕实例中的实例2)
RH275=MD44D*11M+一种从TMPMAE和甲醛制成的环状甲缩醛
MD42D′7M=MD42D*7M+TMPMAE
TROS 6002X=有机破乳剂。
所有数值均以分离水的毫米数报告，而这平行于体积。全分离对应于约42mm读数。除RH-265和RH-275外，所采用的结构均用TMPMAE制成，并在本报告的以上各表中描述。
RH-265是用MD44D*11M和聚醚制成的，而且提供很常见的柴油消泡剂性能。用TMPMAE甲缩醛制成的RH-275的低有效性是显著的，而且平行于柴油消泡剂的结果。显然，较长的硅氧烷链(有机硅氧烷实例中实例1与实例2比较而言)能加速分离。如同熟悉本门技术的人员会了解的，由于原油的多种多样，因而应当避免任何一概而论。
所列的硅氧烷在10ppm浓度时优于有机破乳剂，但即使在最好的情况下(有机硅氧烷实例中的实例1)，它们的性能也不如以100ppm施用的TROS参照物。MD100D′24M浓度提高到25ppm时并没有加速分离。
润滑油性能
用一流石油公司之一所供应的一种典型润滑油进行了几个实验。该测试包括：在5分钟期间使分散的空气以200毫升/分钟的速率通过200毫升油，记录油/气的体积，并在第二部分测定期间把空气流量率固定在100毫升/分钟，此时记录泡沫的衰减。
新鲜油和用已知工业参照消泡剂(市售品，商品名“ELF”)处理过的油作为对照组进行试验。数字列于表9中。
表9消泡剂            浓度      初始泡沫    1分钟     2分钟     3分钟
                        体积        后体积    后体积    后体积
                        毫升        毫升      毫升      毫升无                无        400         260       220       205对照              200       200实例Ⅰ            50        200实例A             50        200实例A             20        200
完全消泡是在非常低的有机硅氧烷浓度时达到的，而且与纯的二甲基硅氧烷比较，脱气时间有实质性缩短。在初始泡沫体积为200毫升的情况下，这表明基本上无泡沫存在。20ppm时的脱气对应于以200ppm施用有机参照物情况下的密度(0.844)。因此，本发明的化合物以与硅油消泡剂可比的低处理率提供与有机消泡剂可比的脱气速度。
虽然已经详细地并参照其具体实施方案说明了本发明，但对于有本门技术一般技能的人员来说显而易见的是，在不背离其精神和范围的情况下可以对它做各种变化和修饰。
以上提到的所有参考文献的全文都列为本说明书的参考文献。

Claims (33)

1．一种适合于用作消泡剂或原油破乳剂的有机改性聚硅氧烷，包括通式MDxD′yD″zM的一种聚合物，
其中M是O.5Si(CH3)3，
D是OSi(CH3)2，
D′是OSi(CH3)R，且R是一个完全饱和的多羟基C6～C28有机基团，
D″是OSi(CH3)R′，式中R′是一种苯酚衍生物或一个长链脂肪族基团或聚醚，
z是0～80，
x+y+z是10～200，
x/z≥1，
而x/(y+z)是约2.0～约10.0；
或者通式M′DaM′的一种聚合物，
式中M′是O.5Si(CH3)2R，且R是一种分子量为约134～约644而且除末端不饱和外已完全饱和的多羟基C6～C28有机基团，
D是一个OSi(CH3)2，
且a是4～10；
或者通式MDxD′yD″zM与通式M′DaM′的混合物。
2．按照权利要求1的有机改性聚硅氧烷，其中R是从三(羟甲基)丙烷一烯丙基醚、三(羟甲基)丙烷一烯丙基醚、乙氧基化季戊四醇烯丙基醚甲缩醛、丙氧基化季戊四醇烯丙基醚、三(异丙醇)胺烯丙基醚、烯丙基丙烷-1,3-二醇、烷氧基化烯丙基山梨糖醇、烷氧基化季戊四醇、烷氧基化三甲基丙烷或非烷氧基化三甲基丙烷衍生的。
3．按照权利要求2的有机改性聚硅氧烷，其中R是从三(羟甲基)丙烷一烯丙基醚衍生的。
4．按照权利要求1的有机改性聚硅氧烷，其中R′是一种有10～20个碳原子的长链脂肪族基团。
5．按照权利要求1的有机改性聚硅氧烷，其中x+y+z在20～160的范围内。
6．按照权利要求1的有机改性聚硅氧烷，其中x/(y+z)在约3.0～6.0范围内。
7．按照权利要求1的有机改性聚硅氧烷，其中a在5～8的范围内。
8．按照权利要求1的有机改性聚硅氧烷，其中x是100,y是24，且R是从三(羟甲基)丙烷一烯丙基醚衍生的。
9．按照权利要求1的有机改性聚硅氧烷，其中R是从三(羟甲基)丙烷一烯丙基醚衍生的，且a是7。
10．按照权利要求1的有机改性聚硅氧烷，进一步包含柴油燃料，其中通式MDxD′yD″zM的聚合物是以约1～约5ppm存在的。
11．按照权利要求1的有机改性聚硅氧烷，进一步包含柴油燃料，其中通式M′DaM′的聚合物是以约4ppm存在的。
12．按照权利要求1的有机改性聚硅氧烷，进一步包含润滑油，其中该聚合物是以低于约100ppm存在的。
13．按照权利要求1的有机改性聚硅氧烷，进一步包含润滑油，其中该聚合物是以低于约50ppm存在的。
14．按照权利要求1的有机改性聚硅氧烷，进一步包含原油，其中该聚合物是以约10ppm存在的。
15．按照权利要求1的有机改性聚硅氧烷，进一步包含原油，其中该聚合物是以约5ppm存在的。
16．按照权利要求1的有机改性聚硅氧炕，进一步包含溶剂。
17．按照权利要求15的有机改性聚硅氧烷，其中该溶剂是从下列组成的一组中选择的：二聚丙二醇、甲苯、2-乙基己醇、异丙醇、脂肪族酯醇类、异佛尔酮、二甲苯，及其混合物。
18．按照权利要求1的有机改性聚硅氧烷，进一步包含DAP。
19．一种有机改性聚硅氧烷，包括通式MDxD′yD″zM的一种聚合物，其中M是O.5Si(CH3)3，
D是OSi(CH3)2，
D′是OSi(CH3)R，且R是从烷氧基化烯丙基山梨糖醇、烷氧基化季戊四醇、烷氧基化三甲基丙烷或非烷氧基化三甲基丙烷衍生的，
D″是OSi(CH3)R′，式中R′是一种苯酚衍生物或一个长链脂肪族基团或聚醚，
z是0～80，
x+y+z是10～200，
x/z≥1，
而x/(y+z)是约2.0～约10.0；
或者通式M′DaM′的一种聚合物，
式中M′是O.5Si(CH3)2R，且R是从下列一组中选择的：烷氧基化烯丙基山梨糖醇，烷氧基化季戊四醇，烷氧基化三甲基丙烷，和非烷氧基化三甲基丙烷，
D是OSi(CH3)2，
且a是4～10；
或者通式MDxD′yD″zM与通式M′DaM′的混合物。
20．一种减少柴油燃料或润滑油发泡的方法，包括向柴油燃料或润滑油中添加足够量的权利要求1的有机改性聚硅氧烷。
21．按照权利要求20的方法，其中x是100,y是24，且R是从三(羟甲基)丙烷一烯丙基醚衍生的。
22．按照权利要求20的方法，其中R是从三(羟甲基)丙烷一烯丙基醚衍生的，且a是7。
23．按照权利要求20的方法，其中，包含通式MDxD′yD″zM的聚合物的有机改性聚硅氧烷是以约1～约5ppm的数量存在于柴油燃料中的。
24．按照权利要求20的方法，其中，包含通式M′DaM′的聚合物的有机改性聚硅氧烷是以约4ppm的数量存在于柴油燃料中的。
25．按照权利要求20的方法，其中，有机改性聚硅氧烷是以低于约100ppm的数量存在于润滑油中的。
26．按照权利要求20的方法，其中，有机改性聚硅氧烷是以约20～约50ppm的数量存在于润滑油中的。
27．一种原油破乳方法，包括向原油中添加足够量的权利要求1的有机改性聚硅氧烷。
28．按照权利要求27的方法，其中x是100,y是24，且R是从三(羟甲基)丙烷一烯丙基醚衍生的。
29．按照权利要求27的方法，其中R是从三(羟甲基)丙烷一烯丙基醚衍生的，且a是7。
30．按照权利要求27的方法，其中有机改性聚硅氧烷是以约10ppm的数量存在于原油中的。
31．按照权利要求27的方法，其中有机改性聚硅氧烷是以约5ppm的数量存在于原油中的。
32．按照权利要求20或权利要求26的方法，进一步包括溶剂的添加。
33．按照权利要求32的方法，其中溶剂是从下列一组中选择的：二聚丙二醇、甲苯、2-乙基己醇、异丙醇、脂肪族酯醇类、异佛尔酮、二甲苯，及其混合物。
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US6001140A (en) 1999-12-14
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CA2258708C (en) 2007-02-20
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AU2425797A (en) 1997-10-29
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