CN1215154C - 低粘度官能液组合物 - Google Patents

低粘度官能液组合物 Download PDF

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Publication number
CN1215154C
CN1215154C CNB018201881A CN01820188A CN1215154C CN 1215154 C CN1215154 C CN 1215154C CN B018201881 A CNB018201881 A CN B018201881A CN 01820188 A CN01820188 A CN 01820188A CN 1215154 C CN1215154 C CN 1215154C
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composition
gross weight
amount
alkoxyl group
acid ester
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CN1479779A (zh
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T·T·香农
B·T·基恩
J·L·汉森
P·L·克罗森
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Union Carbide Chemicals and Plastics Technology LLC
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Union Carbide Chemicals and Plastics Technology LLC
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Abstract

低粘度官能液组合物，尤其用作防锁制动***中的制动液，其含有硼酸酯成分，烷氧基乙二醇成分和含有腐蚀抑制剂的添加剂包。

Description

低粘度官能液组合物
本发明涉及低粘度官能液，其在多种应用中有用，尤其用作新的防锁制动***的制动液，该***需要满足低温下良好操作的较低粘度液体。
基于硼酸酯的官能液组合物在本领域是已知的。为了用作DOT 4或DOT 5.1制动液，这些硼酸酯基组合物必须满足严格的物理特性和性能要求，尤其是最小干平衡回流沸点(ERBP)、最小湿平衡沸点(WERBP)和最大低温(-40℃)粘度，同时维持足够的抗腐蚀性和稳定性，并满足其它物理特性要求如pH值、储备碱度、橡胶膨润等等。按照联邦机动车标准(Federal Motor Vehicle Standards)116中所定义的，最小ERBP、最小WERBP和最大粘度要求在下述表1中给出：
表1
                DOT 4               DOT 5.1
ERBP℃          230                 260
WERBP℃         155                 180
-40℃粘度cSt    1800(18cm2/s)      900(9cm2/s)
最新开发的装置如电子的或自动的防锁制动***已经产生了对高性能制动液的需求，所需要的高性能制动液需要具有比表1中规定的甚至更好的物理和性能特性。具体而言，存在对于具有低温粘度的高性能制动液的强烈需求，所述低温粘度显著低于表1中规定的那些，同时满足或超过最小ERBP和WERBP温度要求。正在探索具有低温粘度的高性能制动液用于这些最新开发的制动***中，所述低温粘度对于DOT 5.1液而言低于700厘沲(7.0cm2/s)，对于DOT 4液而言低于500厘沲(5.0cm2/s)。
配制具有低温粘度的硼酸酯基制动液的能力已经证明是工业上的一个难度很大的挑战，所述低温粘度对于DOT 4液来说低于700(7.0cm2/s)厘沲和甚至更低，同时可以维持足够高的ERBP和WERBP温度。制动液中必需存在充足的硼酸酯，以提供期望的高ERBP和WERBP温度。然而，液体组合物中硼酸酯的量过高往往会提高低温粘度，使其超出可接受水平。此外，许多传统的制动液添加剂如链烷醇胺腐蚀抑制剂往往会提高液体的低温粘度，尤其在需要维持液体pH稳定性的水平。因此具有非常低粘度的制动液组合物仍然在寻找中。
现有技术公开了降低硼酸酯基制动液的粘度同时维持足够高的ERBP和WERBP温度的多种努力。例如，美国专利4,371,448公开了一种硼酸酯基制动液，其含有一种显著量的必需成分双(乙二醇单烷基醚)。EP 0 750 033和EP 0 617 116公开了通过用一种络合物或化合物的混合物取代传统的腐蚀抑制剂来降低硼酸酯基制动液粘度的尝试。所有这些努力涉及将络合物和昂贵的成分加入制动液，然而却没有达到申请人的目标，即将硼酸酯基制动液的低温粘度降至低于700厘沲(7.0cm2/s)以满足DOT 5.1规格和低于500厘沲(5.0cm2/s)以满足DOT 4规格。
根据本发明，申请人已经发现了一些组合物的独特组合，其具有足够高的ERBP和WERBP温度以满足或超过DOT 4和5.1液体的要求，和对于DOT 4和5.1液体来说低于700厘沲(7.0cm2/s)的低温粘度(-40℃)，优选对于DOT 4液体低于500厘沲(5.0cm2/s)。本发明的新颖的官能液组合物是用易于获得且便宜的成分制备的，该组合物包括一种特殊限定的硼酸酯成分，一种特殊限定的烷氧基乙二醇成分和许多普通的添加剂包中的一种。
本发明的新颖的低粘度官能液包括
(a)以总组合物的重量计，35-70wt％具有下式的烷氧基乙二醇硼酸酯成分，
[RO(CH2CH2O)n]3-B
其中R是甲基、乙基、丙基或丁基，或其混合物，n基本上为2-4，其中以硼酸酯成分的总重量计，n＝3的硼酸酯大于90wt％，
(b)以组合物的总重量计，25-65wt％具有以下分子式的烷氧基乙二醇成分
RO(CH2CH2O)nH
其中R是具有1-8个碳原子的烷基或其混合物，n基本上为2-4，其中以烷氧基乙二醇成分的总重量计，n＝2的烷氧基乙二醇的存在量为1-88wt％，其中以烷氧基乙二醇成分的总重量计，n＝4的烷氧基乙二醇的存在量为0-20wt％，和
(c)以组合物的总重量计，0.3-10wt％的添加剂包，其含有下述的一种或多种：腐蚀抑制剂、消泡剂、pH稳定剂和抗氧化剂，
其中，其中以组合物的总重量计，n＝2的成分(a)和(b)的总存在量为1-45wt％，其中以组合物的总重量计，n＝4的成分(a)和(b)的总存在量为0-10wt％。
当n＝3的成分(a)大于90wt％，n＝2的成分(b)12-88wt％，n＝4的成分(b)0-10wt％，n＝2的成分(a)和(b)总量为8-45wt％且n＝4的成分(a)和(b)总量为0-6wt％时，所获得的本发明的液体组合物具有至少240℃的ERBP，至少165℃的WERBP和低于500厘沲(5.0cm2/s)的低温粘度。
当n＝3的成分(a)大于95wt％，n＝2的成分(b)从1-12wt％且n＝4的成分(b)为0-20wt％，n＝2的成分(a)和(b)总量为1-8wt％且n＝4的成分(a)和(b)总量为0-10wt％时，所获得的本发明的液体组合物具有至少260℃的ERBP，至少180℃的WERBP和低于700厘沲(7.0cm2/s)的低温度粘度。
在成分(a)中，n＝3的烷氧基乙二醇硼酸酯成分的存在量优选为95wt％或更高，更优选为96wt％或更高。在成分(a)中，n＝2的烷氧基乙二醇硼酸酯成分的存在量优选为0.5wt％或更高，更优选为1.0wt％或更高。在成分(a)中，R优选是甲基、乙基或其混合物，最优选是甲基。
在成分(b)中，n＝2的乙二醇醚的存在量优选为1wt％或更高，更优选为2wt％或更高。
优选在成分(b)中，n＝2的乙二醇醚的存在量少于65wt％，更优选为40wt％或更低。在成分(b)中，n＝4的乙二醇醚的存在量为0.5wt％或更高，更优选为1wt％或更高。在成分(b)中，n＝4的乙二醇醚的存在量优选为12wt％或更低，更优选为10wt％或更低。在成分(a)和(b)中，n＝2的硼酸酯和乙二醇醚的存在量为0.5wt％或更高，更优选为1wt％或更高，最优选为2wt％或更高。在成分(a)和(b)中，n＝2的硼酸酯和乙二醇醚的存在量优选为45wt％或更低，更优选为35wt％或更低，最优选为25wt％或更低。在成分(a)和(b)中，n＝4的硼酸酯和乙二醇醚的存在量优选为0.5wt％或更高。在成分(a)和(b)中，n＝4的硼酸酯和乙二醇醚的存在量为8wt％或更低，更优选为7wt％或更低。
本发明的官能液组合物的成分(a)是用以下分子式表示的烷氧基乙二醇硼酸酯
[RO(CH2CH2O)n]3-B
其中R是甲基、乙基、丙基或丁基，或其混合物，n基本上为2-4，其中以硼酸酯成分的总重量计，n＝3的硼酸酯大于90wt％，硼酸酯及其制备方法在本技术领域是已知的。用于本发明的官能液组合物中的硼酸酯可以通过硼酸与合适的烷氧基乙二醇成分反应制备，其中所述烷氧基乙二醇通常是含有至少90wt％，优选95wt％的烷氧基三甘醇种类的烷氧基乙二醇的选择性混合物。
有用的硼酸酯的实例包括那些含有如下成分的硼酸酯：甲氧基三甘醇硼酸酯、乙基三甘醇硼酸酯、丁基三甘醇硼酸酯及其混合物。当制备DOT 4液体时，用含有大于90％甲氧基三甘醇硼酸酯的硼酸酯成分已经获得了特别好的结果，当制备DOT 5.1液体时，用含有大于95％甲氧基三甘醇硼酸酯的硼酸酯成分已经获得了特别好的结果。以组合物的总重量计，成分(a)在官能液组合物中的存在量通常为35-70wt％。
以组合物的总重量计，本发明的官能液组合物的成分(b)包括25-65wt％具有下式的烷氧基乙二醇，
RO(CH2CH2O)nH
其中R是具有1-8个碳原子的烷基或其混合物，n基本上为2-4，其中以烷氧基二醇成分的总重量计，n＝2的烷氧基乙二醇的存在量为1-88wt％，其中以乙二醇成分的总重量计，n＝4的烷氧基乙二醇的存在量为0-20wt％。有用的烷氧基乙二醇的实例包括甲氧基三甘醇、甲氧基二甘醇、甲氧基四甘醇、乙氧基三甘醇、乙氧基二甘醇、乙氧基四甘醇、丙氧基三甘醇、丁氧基三甘醇、丁氧基二甘醇、丁氧基四甘醇、戊氧基二甘醇、戊氧基三甘醇、2-乙基己基二甘醇及其混合物。用含有甲氧基三甘醇、甲氧基二甘醇、乙氧基三甘醇、丁氧基二甘醇、丁氧基三甘醇、己氧基二甘醇及其混合物的烷氧基乙二醇已经获得了特别好的结果。
申请人已经发现其中烷氧基含有1-5个碳原子的烷氧基二甘醇在降低官能液组合物的粘度中有用。然而，当这样的低级烷氧基二甘醇在本发明的DOT 4液体中的存在量超过45％或者在本发明的DOT 5.1液体中的存在量超过8％时，ERBP和WERBP可能被降低到不可接受的水平。也就是说，其中烷氧基基团含有5-8个碳原子的高级烷氧基二甘醇在官能液组合物中以高达10％或更高的量存在是允许的，而不会严重地对ERBP或WERBP产生不利影响。当这些高级烷氧基二甘醇以这些水平存在时，已经发现它们可以提供有利的橡胶膨润特性。
以组合物的总重量计，本发明的官能液组合物的成分(c)包括0.3-10wt％的含有腐蚀抑制剂的添加剂包。在本技术领域已知的多种传统添加剂可以被有利地用于本发明的官能液组合物。其包括，例如腐蚀抑制剂、稳定剂如pH稳定剂和抗氧化剂。
选择有效的腐蚀抑制剂在配制本发明的官能液组合物中尤其重要。许多传统腐蚀抑制剂如链烷醇胺或烷基胺和其它有机胺可以增加硼酸酯基官能液的低温粘度，这导致使用更多的络合物和昂贵的添加剂，如EP 0 750 033和EP 0 617 116中所公开的。申请人的官能液组合物的一个优点是，能够使用传统的腐蚀抑制剂如链烷醇胺且仍然可以获得比迄今为止已知的更低的粘度。另一个优点是，在期望获得改进的稳定性或抗腐蚀性同时维持可接受的低粘度的场合，能够使用增加量的传统抑制剂和添加剂。
可以用于本发明的官能液组合物中的传统腐蚀抑制剂种类的实例包括：脂肪酸如月桂酸、棕榈酸、硬脂酸或油酸，磷或磷酸与脂族醇形成的酯，亚磷酸酯如磷酸三乙酯、磷酸二甲酯、磷酸异丙酯、亚磷酸丁酯、亚磷酸三苯酯和亚磷酸二异丙酯，含有杂环氮的化合物如苯并***或其衍生物，以及这些化合物与1，2，4***及其衍生物的混合物(参见美国专利6,974,992)。其它用作腐蚀抑制剂的胺化合物包括，烷基胺如二正丁胺和二正戊胺、环己胺及其盐。在本发明的官能液组合物中用作腐蚀抑制剂尤其有用的胺化合物包括链烷醇胺，优选那些含有1-3个链烷醇基团且每一个链烷醇基团含有1-6个碳原子的链烷醇胺。有用的链烷醇胺的实例包括单甲醇胺、二甲醇胺和三甲醇胺，单乙醇胺、二乙醇胺和三乙醇胺，单丙醇胺、二丙醇胺和三丙醇胺，单异丙醇胺、二异丙醇胺和三异丙醇胺。使用了易于获得且便宜的二异丙醇胺的本发明的官能液组合物已经获得了良好的结果。
以组合物的总重量计，在本发明的官能液组合物中所用的腐蚀抑制剂的使用量的范围为0.3-10wt％，优选为1-3wt％。
除了一种或多种腐蚀抑制剂，本发明的官能液组合物也可以有利地含有用于增强官能液组合物性能的其它添加剂化合物，如消泡剂、pH稳定剂和抗氧化剂，所有这些对于熟练配方设计师是已知的。以官能液组合物的总重量计，这些与腐蚀抑制剂组合的其它添加剂的存在量通常为0.3-10wt％，。
应该预料到，其它材料可以被配制到本发明的官能液中，只要注意不会将ERBP或WERBP温度降低至低于可接受水平，或者将低温粘度增加到高于可接受水平。例如，以液体的总重量计，本发明的官能液可以包括0-20wt％的稀释剂或滑润剂如，例如聚环氧乙烷、聚环氧丙烷、聚(环氧烷)二烷氧基乙二醇或硼酸盐共酯。
也应该预料到，本发明的教导可以被应用于配制的其它液体，以获得较低粘度，如美国专利4,371,448，EP 0 750 033和EP 0 617 116中所公开的，以进一步降低粘度，同时维持可接受的最小ERBP和WERBP温度。
实施例
下述实施例说明了本发明的官能液组合物及其一些优选的实施方案，这些实施例不意在限定本发明。
在下述实施例中用于制备官能液的纯甲氧基三甘醇硼酸酯(MTGBE)是用上述在成分(a)的讨论中所示分子式表示的一种高度选择性的酯，含有98wt％n＝3的种类和2wt％n＝2的种类。用于配制下述实施例的官能液的MTGBE是作为甲氧基三甘醇中的87wt％的纯硼酸酯溶液引入的。
下述在实施例中用于配制官能液的硼酸酯和多种其它成分进行如下鉴定：
化合物               化学名称               [n＝2/3/4/5](a)
MTGBE                甲氧基三甘醇硼酸酯     (2/98/0/0)
MTG                  甲氧基三甘醇           (2/98/0/0)
MPG                  甲氧基聚(乙二醇)       (2/38/56/4)
EDG                  乙氧基二甘醇           (100/0/0/0)
ETG                  乙氧基三甘醇           (1/93/6/0)
BDG                  丁氧基二甘醇           (100/0/0/0)
BTG1                 丁氧基三甘醇           (3/91/6/0)
BTG2                 丁氧基三甘醇           (1/78/17/4)
BTG3                 丁氧基三甘醇           (2/71/24/3)
BPG                  丁氧基聚(乙二醇)       (0/30/65/0)
HxDG                 己氧基二甘醇           (100/0/0/0)
HPG                  己氧基聚(乙二醇)       (100/70/2/0)
MDG                  甲氧基二甘醇           (100/0/0/0)
DIPLA                二异丙醇胺
(a)每一烷氧基乙二醇中存在的各种种类的重量百分比
ERBP、WERBP和-40℃粘度是用Department of TransportationFMVSS 116中描述的试验方法确定的。
下述表中给出的数字涉及每一成分的存在量，是以按液体组合物总重量计的重量百分比给出。涉及乙二醇醚中存在的n＝2和n＝4种类的存在量的数字是以按所存在的乙二醇醚的总重量计的重量百分比给出。涉及总液体组合物中存在的n＝2和n＝4种类的存在量的数字是以按液体组合物的总重量计的重量百分比给出。
实施例1-5
配制5种具有表2所述的组合物的官能液。这些实施例说明本发明的官能液组合物满足DOT 4制动液的ERBP和WERBP最小温度要求，同时具有低于700厘沲(7.0cm2/s)的-40℃粘度。实施例1和2显示了具有低于500厘沲(5.0cm2/s)的低温粘度的液体组合物。
表2
成分             实施例1    实施例2    实施例3    实施例4    实施例5
MTGBE            50         42         50         56         52
MTG              8          19         24         15         18
MPG              5.4                              4
BDG              24                               10         13
BTG1                        25
BTG2                                   24                    15
BTG3                                              13
HxDG                        8
HPG                         4
MDG              10.6
DIPLA            2          2          2          2          2
n＝2/n＝4含量
n＝2乙二醇醚中   71         17         2          25         29
n＝4乙二醇醚中   6          4          8          12         5
n＝2总液体中     37         11         2          12         15
n＝4总液体中     3          2          4          6          3
测定实施例1-5的液体组合物的ERBP、WERBP和-40℃粘度，结果在表3中给出。
表3
特性             实施例1      实施例2      实施例3      实施例4      实施例5
ERBP℃           242          264          267          263          261
WERBP℃          170          173          179          179          169
-40℃粘度.CSt    368          496          611          600          535
             (3.68cm2/s) (4.96cm2/s) (6.11cm2/s) (6.00cm2/s) (5.35cm2/s)
从表3可以看出，实施例1和2的液体组合物满足DOT 4液体的最小ERBP和WERBP温度要求，且低温粘度低于优选的最大值500厘沲(5.0cm2/s)。
实施例6-9
配制4种具有表4所述的组合物的官能液。实施例6，7和8说明本发明的官能液组合物满足DOT 5.1制动液的ERBP和WERBP最小温度要求，同时具有低于700厘沲(7.0cm2/s)的-40℃粘度。实施例9显示了不满足这一粘度要求的液体组合物。
表4
成分               实施例6      实施例7      实施例8      实施例9
MTGBE              50           52           61           50
MTG                18.6         13           30.5         8
MPG                5.4                                    16
ETG                             15           2.5
BPG                                                       24
BTG1                            10           2
BTG2               24
HxDG                            4            2
HPG                             4
DIPLA              2            2            2            2
n＝2/n＝4含量
n＝2乙二醇醚中     2            11           7            1
n＝4乙二醇醚中     15           5            1            51
n＝2总液体中       2            6            4            2
n＝4总液体中       8            2            ＜1          27
测定实施例6-9的液体组合物的ERBP、WERBP和-40℃粘度，结果在表5中给出。
表5
特性             实施例6      实施例7      实施例8      实施例9
ERBP℃           268          265          265          270
WERBP℃          181          184          186          180
-40℃粘度.CSt    686          552          681          851
             (6.86cm2/s) (5.52cm2/s) (6.81cm2/s) (8.51cm2/s)
从表5可以看出，实施例6，7和8的液体组合物满足DOT 5.1液体的最小ERBP和WERBP温度要求，同时满足700厘沲(7.0cm2/s)的最大低温粘度目标。实施例9没有满足这一低温粘度目标。
选择实施例1，6和7的液体组合物用于测试抗腐蚀性和橡胶膨润性，使用Department of Transportation FMVSS 116中所描述的方法。橡胶膨润性试验是于170℃进行72小时。结果在表6中给出。
表6
腐蚀                 实施例1      实施例6        实施例7
锡，mg/cm2          0.02         0.00           0.02
钢铁，mg/cm2       -0.01        -0.01          -0.02
铝，mg/cm2         -0.01        -0.01           0.02
铸铁，mg/cm2       -0.02         0.06          -0.08
黄铜，mg/cm2       -0.12        -0.07           0.03
紫铜，mg/cm2       -0.10        -0.09           0.01
锌，mg/cm2          0.00         0.08           0.11
杯子底部直径，mm     0.299        0.306          0.064
硬度降低，IRHD 6.0                3.0            1.3
橡胶膨润
底部直径，mm         1.4          1.1            0.7
硬度降低，IRHD 9.5                10.5           5.7

Claims (8)

1.一种官能液组合物，其包括
(a)以总组合物的重量计，35-70wt％具有以下分子式的烷氧基乙二醇硼酸酯，
[RO(CH2CH2O)n]3-B
其中R是甲基、乙基、丙基或丁基，或其混合物，n为2-4，其中以硼酸酯成分的总重量计，n＝3的大于90wt％，
(b)以组合物的总重量计，25-65wt％具有以下分子式的烷氧基乙二醇成分，
RO(CH2CH2O)nH
其中R是具有1-8个碳原子的烷基或其混合物，n为2-4，其中以烷氧基乙二醇成分的总重量计，n＝2的烷氧基乙二醇的存在量为1-88wt％，其中以烷氧基乙二醇成分的总重量计，n＝4的烷氧基乙二醇的存在量为0-20wt％，和
(c)以组合物的总重量计，0.3-10wt％的下述的一种或多种：腐蚀抑制剂、消泡剂、pH稳定剂和抗氧化剂，
其中，以组合物的总重量计，n＝2的成分(a)和(b)的总存在量为1-45wt％，以组合物的总重量计，n＝4的成分(a)和(b)的总存在量为0-10wt％。
2.如权利要求1所述的组合物，其中成分(a)中n＝3的大于90wt％，成分(b)中n＝2的为12-88wt％且成分(b)中n＝4的为0-10wt％，n＝2的成分(a)和(b)总量为8-45wt％且n＝4的成分(a)和(b)总量为0-6wt％。
3.如权利要求1所述的组合物，其中成分(a)中n＝3的大于95wt％，成分(b)中n＝2的为1-12wt％且n＝4的为0-20wt％，n＝2的成分(a)和(b)总量为1-8wt％且n＝4的成分(a)和(b)总量为0-10wt％。
4.如权利要求1所述的组合物，其中以组合物的总重量计，所述成分(a)的存在量为35-55wt％，成分(b)的存在量为40-65wt％。
5.如权利要求1所述的组合物，其中以组合物的总重量计，所述成分(a)的存在量为45-70wt％，成分(b)的存在量为25-50wt％。
6.如权利要求1所述的组合物，其中以组合物的总重量计，所述成分(b)含有至少1wt％的己氧基二甘醇。
7.一种制动液，其包括根据权利要求1所述的组合物。
8.一种用于电子的或自动的防锁制动***的包括权利要求1所述组合物的制动液。
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