CN1090596A - 胶凝油组合物 - Google Patents

胶凝油组合物 Download PDF

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Publication number
CN1090596A
CN1090596A CN93120502A CN93120502A CN1090596A CN 1090596 A CN1090596 A CN 1090596A CN 93120502 A CN93120502 A CN 93120502A CN 93120502 A CN93120502 A CN 93120502A CN 1090596 A CN1090596 A CN 1090596A
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Prior art keywords
acid
described composition
oil
total amount
accounts
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CN93120502A
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CN1035885C (zh
Inventor
M·布劳尔
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Caschem Inc
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Caschem Inc
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    • G—PHYSICS
    • G02—OPTICS
    • G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B6/00—Light guides; Structural details of arrangements comprising light guides and other optical elements, e.g. couplings
    • G02B6/44—Mechanical structures for providing tensile strength and external protection for fibres, e.g. optical transmission cables
    • G02B6/4401—Optical cables
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
    • C—CHEMISTRY; METALLURGY
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    • C10M101/00—Lubricating compositions characterised by the base-material being a mineral or fatty oil
    • C10M101/02—Petroleum fractions
    • C—CHEMISTRY; METALLURGY
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    • C10M107/00—Lubricating compositions characterised by the base-material being a macromolecular compound
    • C10M107/02—Hydrocarbon polymers; Hydrocarbon polymers modified by oxidation
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    • C10M117/00—Lubricating compositions characterised by the thickener being a non-macromolecular carboxylic acid or salt thereof
    • C10M117/02—Lubricating compositions characterised by the thickener being a non-macromolecular carboxylic acid or salt thereof having only one carboxyl group bound to an acyclic carbon atom, cycloaliphatic carbon atom or hydrogen
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    • C10M117/08—Lubricating compositions characterised by the thickener being a non-macromolecular carboxylic acid or salt thereof having only one carboxyl group bound to a carbon atom of a six-membered aromatic ring
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    • C10M135/28—Thiols; Sulfides; Polysulfides containing sulfur atoms bound to a carbon atom of a six-membered aromatic ring
    • C10M135/30—Thiols; Sulfides; Polysulfides containing sulfur atoms bound to a carbon atom of a six-membered aromatic ring containing hydroxy groups; Derivatives thereof
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01R—ELECTRICALLY-CONDUCTIVE CONNECTIONS; STRUCTURAL ASSOCIATIONS OF A PLURALITY OF MUTUALLY-INSULATED ELECTRICAL CONNECTING ELEMENTS; COUPLING DEVICES; CURRENT COLLECTORS
    • H01R13/00—Details of coupling devices of the kinds covered by groups H01R12/70 or H01R24/00 - H01R33/00
    • H01R13/46—Bases; Cases
    • H01R13/52—Dustproof, splashproof, drip-proof, waterproof, or flameproof cases
    • H01R13/5216—Dustproof, splashproof, drip-proof, waterproof, or flameproof cases characterised by the sealing material, e.g. gels or resins
    • H—ELECTRICITY
    • H02—GENERATION; CONVERSION OR DISTRIBUTION OF ELECTRIC POWER
    • H02G—INSTALLATION OF ELECTRIC CABLES OR LINES, OR OF COMBINED OPTICAL AND ELECTRIC CABLES OR LINES
    • H02G15/00—Cable fittings
    • H02G15/003—Filling materials, e.g. solid or fluid insulation
    • H—ELECTRICITY
    • H02—GENERATION; CONVERSION OR DISTRIBUTION OF ELECTRIC POWER
    • H02G—INSTALLATION OF ELECTRIC CABLES OR LINES, OR OF COMBINED OPTICAL AND ELECTRIC CABLES OR LINES
    • H02G15/00—Cable fittings
    • H02G15/08—Cable junctions
    • H02G15/10—Cable junctions protected by boxes, e.g. by distribution, connection or junction boxes
    • H02G15/117—Cable junctions protected by boxes, e.g. by distribution, connection or junction boxes for multiconductor cables
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    • C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
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    • C10M2201/102—Silicates
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    • C10M2203/1006—Petroleum or coal fractions, e.g. tars, solvents, bitumen used as base material
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Abstract

本发明一般涉及胶凝油组合物，其使用铝皂络合 物作为胶凝剂。胶凝油是由一种油成分，一种凝胶收 缩抑制剂和倾点下降剂组成。胶凝油特别适用于作 缓冲管凝胶和波导的填充剂。

Description

本发明一般涉及胶凝油填充组合物。尤其是，本发明涉及（包含铝基皂络合物的）胶凝油合成物。本发明还涉及使用这些组合物的光电缆。
越来越多地、在工业技术中使用光束用于传送数据，或用于其它通讯，从而，使用了纤维光学。由于纤维光学元件很易碎，所以一个或更多纤维光学元件被制成一束，并被插入一个保护缓冲管里，例如一种聚乙烯外套。
然而，不能允许纤维元件在缓冲管中保持松散状态。如果允许这种状态的话，那么几乎任何种类的机械振动或弯曲能导致损坏或纤维光学元件的破裂。鉴于在数据传送电缆中目前许多使用的纤维光学元件的基本长度、置换或修理纤维光学元件将是困难和昂贵的，因此，在缓冲管内，必须提供用于纤维光学元件缓冲的装置。
在对装在缓冲管中的纤维光学元件提供润滑或缓冲时，必须小心保证纤维光学元件的光学品质不降低。所以，在制成一种填充剂时，例如胶凝油用于装在缓冲管子中的纤维光学元件时，胶凝油不仅必须具有润滑和缓冲作用，而且也必须不损害纤维光学元件的光学品质。况且，该胶凝油必须不破坏缓冲管或电缆套。
对用作光学电缆的缓冲管凝胶和填充剂的胶凝油的要求，不是很容易满足的，胶凝油化合物必须在电缆所用的整个温度范围内保持稳定，其至少应该延伸在-40℃到+70℃。如果电缆处于比工作温度范围更高的温度下，而不是高到损害电缆的任何成分，那么填充剂必须是流体足以使电缆构成并完全填充以填充剂而没有使光学元件破坏或受到过应力的危险。
胶凝油也应该具有粘聚性，足以保证电缆在径向弯曲几个分米或更小，不会导致化合物的内部或表面构成空隙。同时，胶凝油应该是软的足以使这样的弯曲不使光学元件受到任何显著的应变（由于应变引起信号衰减），但是仍然能够阻挡在重力以及流体静力学压力作用下的流动。这是因为如果电缆两端的一端曝露在溢流孔中，那么流体静力学的压力同样地加到电缆上。
在已有技术中众所周知胶凝剂例如粘土和疏水性发烟硅可用来提供胶凝油组成。然而疏水性发烟硅是昂贵的，这是因为必须使用相对大量的发烟硅以提供有用的凝胶。况且，使用疏水性发烟硅，使所得的凝胶将严重地磨损。
所以，对于凝胶油组成和滑脂，要求其是具有改善的润滑性并避免基于硅的凝胶组成的磨损。
本发明一般涉及胶凝油组合物。胶凝油是由烃油、凝胶收缩抑制剂、铝皂络合物，以及任选的抗氧化剂和倾点下降剂组成。胶凝油特别适用作缓冲管凝胶，以及波导的填充剂。
按照本发明给出了特别适用作缓冲管凝胶和波导的填充剂的胶凝油合成物。胶凝油合成物包括一种油成分例如烃油，一种或更多的凝胶收缩抑制剂，以及一种铝皂铬合物。胶凝油可以有选择地包括抗氧化剂和倾点下降剂。该油成分可以是一种矿物油，最好是一种食品级矿物油，一种环烷油，一种石蜡油，或一种聚α-烯烃油中的至少一种。该胶凝油组合物包括40-90%，最好50-75%的油成分，5-50%最好25-45%的凝胶收缩抑止剂，以及4-15%，最好6到8%的脂肪酸和芳香酸的铝皂络合物。用于制造铝皂络合物的脂肪酸能包括硬脂酸、油酸、肉豆蔻酸、癸酸，和棕榈酸中的至少一种酸。有用的凝胶收缩抑制剂包括嵌段共聚物例如橡胶混合物和小于10个碳原子聚合成油并且有芳香含量少于6%的烃。有用的橡胶混合物包括丁基橡胶、乙丙橡胶、乙丙二聚物橡胶、氯化橡胶、和热塑料橡胶嵌段共聚物。最好，嵌段共聚物和聚合油的混合物，用作凝胶收缩抑制剂。选定的抗氧化剂的含量，按重量比可在0.1-2%。最好，抗氧化剂包括一种含有硫键的位阻酚化合物。
本发明的胶凝组合物具有改善的润滑性和比竞争产品硅基小的磨损性。况且，本发明的胶凝油能达到和基于硅石配方相同的粘滞度，而且还具有意想不到的更低的胶凝剂量。
特别是用作缓冲管凝胶的凝胶组合物，含有20-90%的油例如矿物油，和5-50%的凝胶收缩抑制剂，在此，矿物油对于凝胶收缩抑制剂的重量比是7∶3-1∶1，在铝皂络合物中，脂肪酸对于芳香酸的克分子量比是1∶1左右，而在铝皂铬合物中，铝对（脂肪酸+芳香酸）的克分子量比是1∶2左右。
本发明的胶凝油组合物，除了对于光波用作填充剂和缓冲管凝胶剂之外，还可对于无线电通讯器件例如接线板，用作密封剂和在钢模脱开组合物中用作润滑剂。
简短地概述本发明，参照以下说明书和非限定的实例，现在将详细地描述本发明。除非另有说明外，所有百分比是以重量比，而所有温度是以摄氏度。
一般来说，本发明胶凝油组合物含有一种油成分，一种铝皂络合物，一种凝胶收缩抑制剂，和选定量的倾点下降剂与抗氧化剂。油成分可以是40-90%左右，最好50-75%按照组合物重量比，凝胶收缩抑制剂可以是5-50%，最好是25-45%;铝皂络合物可以是4-15%左右，最好是5-9%，最佳是组合物的6-8%。选定的倾点下降剂可以是0.5-10%左右，最好是1-3%，而选定的抗氧化剂可以是0.1-2%，最好是组合物的0.5-1.5%。
一般来说，通过在油成分存在的情况下就地形成一种铝皂络合物，来生产本发明的胶凝油。油成分含有一种或更多的凝胶收缩抑制剂，以及选定抗氧化剂和倾点下降剂。
胶凝油组合物的油成分可以是烃油例如矿物油，一种十个碳原子或更少的α-烯烃聚合成的一种油，一种环烷油或一种石腊油。最好，油成分是一种矿物油，最佳是一种食品级矿物油。尤其是有用的烃油具有一个苯胺点220°F以上，一个闪点至少350°F，最好是500°F，一个粘滞度在65-600赛波特通用秒数（“SUS”）在100°F下，最好530SUS，以及一个平均分子量至少300，最好大于400。
为了上述公开的目的，下列术语具有下列含意：
（a）“石腊矿物油”意思是一种具有通过美国检测材料学会（ASTM）D2501-67步骤中指定的步骤所测定的粘度-比重常数在0.78和0.85之间，且含有65%的石膜碳原子的一个最小值，和重量5%的芳香碳原子的一个最大值的矿物油。
（b）“环烷矿物油”意思是一种具有通过美国检测材料学会D2501-67步骤中指定的步骤所测定的粘度-比重常数在0.78和0.85之间，且含有35%环烷碳原子的一个最小值，和5%的芳香碳原子的一个最大值的矿物油。
用在本发明的胶凝油中的矿物油，一般包括但不限制在变压器油、锭子油、绝缘电缆油和机械油。有用的环烷油包括但不限制在Drakeol  35，可从Pennreco公司买到，Telura油例如Telura  309和可从Exxon买到的滨海淡油。有用的石腊油包括但不限制在Pale  100，和Telura油例如Telura  607，所有这些可从Exxon买到。
按照本发明，很容易调节铝皂络合物作为有效的胶凝剂用于各种各样的油。典型地，通过取决于油成分苯胺点的脂肪酸和芳香酸成分的控制，来改变铝皂络合物的组合物。皂络合物配方可能的变化包括：芳香酸对脂肪酸克分子浓度比，脂肪酸碳链长度，和全部酸（脂肪酸和芳香酸）对铝的克分子浓度比。脂肪酸对于芳香酸克分子量比，一般是从1.4∶0.6到0.6∶1.4左右，并且最好是1∶1。全部酸∶铝的比值是1.8∶1-2.2∶1左右，最好是1.9∶1到2.1∶1，并且最佳是2∶1。
作为已知技术，通过将有机-铝氧基化合物与一种脂肪酸和一种芳香酸起反应生成铝皂络合物。在油的存在下，可以就地形成皂，或可以进行并加到油成分上。最好通过在高苯胺点矿物油存在下，尤其是矿物油例如Drakeol  500可从Pennreco买到，将一克分子量的硬脂酸，一克分子量的苯甲酸，和三-铝三-醇盐起反应，在油成分存在下就地生成铝皂络合物。
许多种脂肪酸可以使用来构成使用在本发明的铝皂络合物。一般来说，这些酸来源于动物，或来自蔬菜成分或来自海中生命。能用来提供有用的铝皂络合物的脂肪酸，包括但不限制在具有链长度C8到C22的脂肪酸。最好，脂肪酸链长度是C12到C22，最佳是C14-C18。列举了有用的脂肪酸，但并不限于此，例如硬脂酸、肉豆蔻酸、癸酸、油酸和棕榈酸以及这些酸的混合物。橡胶用硬脂酸和简单动物脂肪酸，未氢化的，也可以使用。
在用于形成铝皂络合物的脂肪酸中，未饱合量也可以变化。典型地，依据磺值测量的未饱合度是0.5，但是它能多到10到12。
用于生成铝皂络合物的铝成分、典型地是以醇盐形式提供的，最好是异丙氧化物或其三聚物。可以提供铝成分其它有效的来源象氧化铝酰化产物例如氧铝辛酸盐，和铝醇盐螯合物例如酮缩醇碱（可从Chattem化学药品公司买到）。
在本发明中用作胶凝剂的铝皂络合物，可用于与碱金属皂和碱土金属皂混合，例如Na、Ca、Li、Ba、Sr、Zn、Pb、Cd、K和类似金属。附加增稠剂和胶凝剂可以与铝皂络合物结合。有用的增稠剂和胶凝剂包括：皂土、硅和菲斯拉塞奈（phythlocyanine）;聚脲例如具有2到20脲键和分子量100到5000的那些;氨基酸类型油胶凝剂例如N-月桂酰-L-谷氨酸-α、β-二n丁酰胺;纤维素衍生物例如纤维素的季铵盐和糊精的脂肪酸酯及其类似物。
作为胶凝剂可以使用铝皂络合物的量，在宽广的重量百分比范围上变化。然而，如果铝皂络合物的量是过剩，那么生成的胶凝油的粘滞度和流动点可能变得过高。
用在胶凝油中的凝胶收缩抑制剂，可以是合成烃油或嵌段共聚物，及其混合物，最好是混合物。作为凝胶收缩抑制剂，低分子量合成油尤其理想。可用的合成油包括但不限于α-烯烃低聚物，C2-C9链烯烃例如聚丁烯、聚异戊二烯、聚己烯、聚庚烯、聚辛烯、聚壬烯及其类似物。最佳的凝胶收缩抑制剂是聚丁烯。
用作凝胶抑制剂聚合物的例子包括：乙丙橡胶，苯乙烯-丁二烯橡胶共聚物，苯乙烯-乙丙橡胶共聚物，苯乙烯-乙烯/丁烯-苯乙烯嵌段共聚物，苯乙烯-异戊二烯-苯乙烯嵌段共聚物，以及，最好是，苯乙烯-乙烯/丙烯嵌段共聚物。最好，嵌段共聚物含量，按组合物的重量计算，在0.5-10%。
在最佳嵌段共聚物中，能有益地在本发明中用作凝胶收缩抑制剂是苯乙烯橡胶嵌段共聚物。典型的嵌段共聚物是线性嵌段共聚物例如具有苯乙烯-橡胶和苯乙烯-橡胶-苯乙烯的那些，化学式（苯乙烯-橡胶）n的径向嵌段共聚物，其中n典型地是3-4。在这些共聚物中，有用的橡胶包括但不限于：异戊二烯、丁二烯、乙烯/丙烯，及其混合物。这些共聚物典型地具有一个苯乙烯∶橡胶的比率是在近似1∶9-1∶1之间。尤其是最佳嵌段共聚物是苯乙烯-乙烯/丙烯嵌段共聚物具有一个苯乙烯∶橡胶的比率是在0.37∶0.63左右，非增塑的，比重0.93左右，断裂强度（ASTM  D-412）300磅/吋，可从壳牌化学公司买到，Kraton  G  1701是商品名称。
用在本发明胶凝油中的倾点下降剂包括可从乙基有限公司买到的Hitek  672。倾点下降剂可构成约胶凝油重量的0.1-2%。而用在胶凝油的抗氧化剂包括位阻酚的化合物其具有硫键。能使用抗氧化剂的量是在胶凝油重量的0.1-2%。这些成分的比百分数随着胶凝油预期应用的不同可以变化。
如上所述，铝皂铬合物的组合物能在广泛的范围内提供胶凝剂，其能和许多种油组合物一起使用，比基于硅胶凝剂的已有技术可能的更多。例如，通过改变用于生成铝皂络合物的脂肪酸链长度，能使铝皂络合物达到胶凝油范围内的比粘度。通过减少用于生成铝皂络合物的脂肪酸链长度，能实质上减少胶凝油的粘滞度。
在胶凝油的组成中特别是用作缓冲管凝胶和用作电缆填充剂，通过由铝的化合物例如氧化铝酰化产物，铝醇盐螯合物和铝醇盐或其三聚物，给出的一克分子量的铝，与一定分子量的硬脂酸和一克分子的苯甲酸，在油成分的存在下起反应，最好就地形成铝皂络合物。一种高苯胺点油，最好是食品级的矿物油用来提供缓冲管凝胶。在电缆填充组合物中，使用了具有一种芳香含量0-11%，一种环烷含量31-46%，和一种石腊含量51-65%的油。还可包括一种凝胶收缩抑制剂，和选定量的倾点下降剂与抗氧化剂。
适合用于制造电缆填充剂油的例子包括但不限于Puremore  ＃WOT  14，聚-XH51，和聚X-M51P，所有这些可从Burmah-Castrol  Plc买到，如Edelex  27可从英国壳牌公司买到。用于提供电缆填充剂的铝皂络合物，可以是4-30%的胶凝油组合物。铝皂络合物具有一个铝对全部酸的克分子量比是1∶2.1-1∶1.9，和一个脂肪酸对芳香酸的比是1.3∶0.7-0.7∶1.3，最好是0.9∶1.1-1.1∶0.9。凝胶收缩抑制剂可以是一种或多于一种的合成弹性体例如苯乙烯-丁二烯嵌段共聚物，和一种组合油例如聚丁烯。最好，用作缓冲管凝胶的油成分具有粘滞度，在25℃，至少150cps。最好，在重量比为6∶4下，使用矿物油和聚丁烯。
以54-56%矿物油（食品级）的油成分，例如可从Pennreco买到的Drakeol  500，6-7%铝皂络合物，34到36%的一种聚丁烯凝胶收缩抑制剂例如可从Soltex公司买到的Soltex  PB32，或可从Amoco公司买到的AmocoH-300，还有1%的抗氧化剂例如可从Ciba  Geigy买到的Irganox  1035，和1到2%的一种凝胶收缩抑制剂例如可从壳牌石油公司买到的Kraton  G-1701，与2%的倾点下降剂来组成特别用于缓冲管凝胶应用的胶凝油组合物。用在缓冲管胶凝油组成的铝皂络合物，最好具有脂肪酸对芳香酸的比是1∶1，和全部酸（脂肪+芳香）对铝的比是2∶1。有用的芳香酸包括苯甲酸，p-甲苯甲酸，O-甲苯甲酸，2-氯苯甲酸，α-萘甲酸，β-萘甲酸，9苯蒽甲酸，3-苯蒽甲酸，蒽醌-α-羧酸，蒽醌-β-羟酸和脱氢枞酸。
例1.将259.95克Drakeol  500，173.3克聚丁烯32和10克Kraton  G1701装入树脂制长颈瓶中，该长颈瓶装备有一个加热罩，一个搅拌器，一个滴液漏斗，一个氮气入口和一个气体出口管。使氮气进入长颈瓶中并且添加了22.74克硬脂酸（酸值205.60）。搅拌生成的混合物，同时加热到温度为100℃。一滴滴地将9克三-铝-三-异丙氧化物（12.5%Al）滴入。加入10克的苯甲酸，温度增加到124℃，而且一滴滴地再添加三-铝-三-异丙氧化物的附加9克。在49分钟内，温度进一步增加到190℃。该温度保持8分钟，同时在氮气下进行搅拌。在17分钟周期内，将混合物冷却到130℃。添加了5克Irganox  1035（可从Ciba-Geigy买到）抗氧化剂和1克的Hitek  672倾点下降剂。生成的混合物冷却到室温过夜以产生一种胶凝物。
例2.除了不使用Kraton  G1701之外，执行例1的其它步骤。
例3.除了不使用聚丁烯之外，执行例1的其它步骤。
例4.除了聚丁烯和Kraton  G1701两种都不使用之外，执行例1的其它步骤。
例5.将254.43克Drakeol  500油，169.62克聚丁烯32，10克的Kraton  G1701，7.59克酸值205.60的硬酯酸，和42.38克的Kolate  6054（5.3%铝），可从Phone-Poulenc买到，装入树脂制长颈瓶中，该长颈瓶的装备如同例1.。加入氮气并且温度上升到100℃。加入苯甲酸9.99克同时温度上升到125℃并保持20分钟。此后，在49分钟的周期内温度上升到190℃。温度保持8分钟同时在氮气下搅拌。然后，在17分钟周期内将混合物冷却到130℃。然后，加入1克的Hitek672倾点下降剂，5克的Irganox  1035。生成的混合物冷却到室温过夜以生成一种胶凝物。
例6.将258.81克的Drakeol  500，172.54克聚丁烯-32和10克的Kraton  G1701装入树脂制长颈瓶中，装备如同例1。将氮气加入长颈瓶中并加入21.26克肉豆寇酸（酸值＝246.50）。搅拌生成的混合物同时加热到温度100℃。一滴滴地加入10.09克三-铝-三-异丙氧化物（12.5%Al）。加入11.22克的苯甲酸，温度增加到124℃，同时，一滴滴地再加入三-铝-三-异丙氧化物的附加的10.09克。在49分钟之内，温度进一步增加到190℃。温度保持8分钟同时在氮气下进行搅拌。在17分钟之内，混合物冷却到130℃。添加5克的Irganox  1035和1克Hitek  672。生成的混合物冷却过夜以生成胶凝物。
例7.将267.30克Drakeol  500，178.20克聚丁烯-32，和5克Kraton  G1701装入树脂制长颈瓶中，装备如同例1.将氮气加入长颈瓶中并加入19.49克硬酯酸（酸值＝205.60）。搅拌生成的混合物并加热到温度100℃。一滴滴地加入7.72克三-铝-三-异丙氧化物（12.5%Al）。加入8.58克苯甲酸，温度增加到124℃，并且再一滴滴地加入三-铝-三-异丙氧化物的一个附加的7.72克。在49分钟内，温度进一步增加到190℃。温度保持8分钟，同时在氮气下搅拌。在17分钟内，混合物冷却到130℃。加入5克的Irganox  1035和1克Hitek  672。生成的混合物冷却过夜以生成胶凝物。
通过这些例子构成的凝胶组成的性质，摘要在下表Ⅰ中：
Figure 931205026_IMG1
在以上表Ⅰ中表示了改变铝皂络合物的脂肪酸成分对胶凝油粘滞度的影响。在表Ⅰ中，脂肪酸∶苯甲酸的克分子量比率是1而全部酸对铝克分子量比率是2。油成分对于聚丁烯凝胶收缩抑制剂的比率是6∶4。
如表Ⅰ所示，意想不到的是，在例6与例1和5相比时，由于增加皂含量和/或增加凝胶收缩抑制剂，脂肪酸链长度的减少控制了发生更高粘滞度的趋势。例6还表明了予料不到的发现：链长度的少量减少而惊人地减小凝胶油的屈服点和张弛时间。
在以上例子中，在一种Brookfield锥体和板粘度计DV-Ⅱ型上，按照操作规程粘度计在剪切速率20/秒下工作，来测定粘滞度。通过在1赫芝频率下测量存储模量（G′）作为在Bohlin  VOR电流计上应力的函数，来予算屈服点（G′）。从G′对应力的值，通过已有技术的方法计算了临界应力（如果超过该应力，G′就减少）。通过将小于临界应力的应力的G′平均值乘以临界应力，来予算屈服点。
通过在应力小于以上定义的临界应力下，测量凝胶在Bohlin VOR电流计上的应力张弛，来测定张弛时间。在这些测试中，频率是1赫芝。当测试期间，存储模量G′作为时间的函数被监视了。张弛时间是G′达到值：（ (G′初始)/(e) ）的时间。
纸凝胶收缩测试描述如下：
材料
1.5毫升注射器
2.11厘米直径，型号1过滤纸
3.硼硅酸耐热表面玻璃（12厘米直径）
4.600毫升硼硅酸耐热玻璃烧杯
5.实验室刮刀
6.分析天秤
7.镊子
8.剪刀
9.定到65℃的强制通风炉
步骤
1.用刮刀将滑脂化合物装入注射器中，慢慢地压柱塞以消除空气泡。
2.切割1英吋×1英吋滤纸方块;称重（WT1）并记录（到0.0001克）。
3.慢慢地将注射器的1毫升化合物加到过滤纸方块上形成圆形的斑点。（围绕着该边缘留一些地方以让斑点散布）。称量这个“样品方块”并记录这个值作为WT2。
4.称量一个11厘米直径的过滤纸圆片（WT3），并把它放在表面玻璃上。将“样品方块”放在过滤纸中央并用600毫升烧杯盖上。
5.让样品不受到打扰、在室温下放16小时。
6.称量样品方块（WT2A）和大过滤纸圆片（WT3A）
7.把样品方块放回到烧杯下，并把整个组件放入炉中，24小时不受到干扰。
8.从炉中移出并在大理石表面上冷却5分钟。称量样品方块（WT2B）和过滤纸圆片（WT3B）。注意颜色的变化。
9.抛弃样品方块和过滤纸。
10.当处理样品方块和过滤纸圆片时，只用镊子。注意保持湿度并且使所有外部颗粒远离样品方块。
计算
1.初始重量二（WT2）-（WT1）
2.重量损失＝（WT2）-（WT2A或WT2B）
3.%重量损失＝重量损失×100/初始重量
4.过滤纸重量增量＝（WT3A或WT3B）-（WT3）
5.挥发重量
a.（重量损失）-（过滤纸重量增量）如果＞0或
b.O，如果（重量损失）-（过滤纸重量增量）≤0
6.%挥发重量＝挥发重量×100/初始重量
7.%非挥发的分离物＝%重量损失-%挥发重量
在室温放16小时之后，计算重量的变化使用“A”值。在65℃附加24小时之后，测定重量的变化使用“B”值。
测量误差
由于反复处理样品，因此应该预期到某些误差存在，特别是在计算在室温下挥发重量损失时更是如此。所有的重量应该记录精确到0.0001克。应该报告所有计算的结果精确到整数。每个被测定的化合物，应该同时测试至少三个样品。然后，可以平均结果的百分比值以测定%重量损失和%非挥发分离物。
本发明制造的胶凝油，特别适用作填充剂以及缓冲管胶凝剂。此外，这些化合物能够用作密封剂或缸封剂在其上引入湿气或水分的电或其它水灵敏的构件。这些组合物还能代替已有技术的软聚氨基甲酸乙酯高弹体用于许多应用场合。例如，可将本发明的组合物引入电连结器的接线板检测口，为的是在接线板口上构成防湿汽密封。况且通过用一个探针贯穿凝胶能得到通向检测口的电的入口。对于这些化合物其它相关的使用，对于本领域的普通技术人员来讲将是清楚的。

Claims (26)

1、一种胶凝油组合物，其特征在于：由大约40-90%的油成分，大约5-50%的凝胶收缩抑制剂，以及大约4-15%的铝皂络合物组成。
2、按照权利要求1所述的组合物，其特征在于：所说的油成分占总量的约50-75%。
3、按照权利要求2所述的组合物，其特征在于：所说的凝胶收缩抑制剂占总量的约25-45%。
4、按照权利要求3所述的组合物，其特征在于：所说的铝皂络合物占总量的约6-8%。
5、按照权利要求1所述的组合物：其特征在于：油成分是一种矿物油，一种环烷油，一种石腊油或一种聚α-烯烃油中的至少一种。
6、按照权利要求1所述的组合物，其特征在于：铝皂络合物是由一种脂肪酸铝盐和一种芳香酸铝盐组成。
7、按照权利要求1所述的组合物，其特征在于：凝胶收缩抑制剂是聚丁烯，一种嵌段共聚物或其混合物。
8、按照权利要求2所述的组合物。其特征在于：所说油成分是一种矿物油并且凝胶收缩抑制剂是一种聚丁烯。
9、按照权利要求1所述的组合物，其特征在于：油成分是一种矿物油，而凝胶收缩抑制剂更是一种嵌段共聚物。
10、按照权利要求9所述的组合物，其特征在于：嵌段共聚物是一种橡胶混合物而且按合成物的重量占总量的0.5-10%。
11、按照权利要求10所述的组合物，其特征在于：橡胶混合物至少是丁基橡胶、乙丙橡胶、乙丙二聚物橡胶，氯化橡胶，或一种热塑料橡胶嵌段共聚物中的一种。
12、按照权利要求9所述的组合物，其特征在于：所述的凝胶收缩抑制剂是一种苯乙烯-乙烯/丙烯嵌段共聚物，其具有苯乙烯∶橡胶的比率是约0.37∶0.63。
13、按照权利要求1所述的组合物，其特征在于：更包括至少一种倾点下降剂，占重量的约0.1到10%之间，和一种抗氧化剂按重量占总量的约0.1到2%之间。
14、按照权利要求13所述的组合物，其特征在于：抗氧化剂包括含有硫键的位阻酚化合物。
15、按照权利要求6所述的组合物，其特征在于：所说的脂肪酸至少是硬脂酸、癸酸、油酸、肉豆蔻酸和棕榈酸中的一种酸。
16、按照权利要求15所述的组合物，其特征在于：所说的芳香酸至少是苯甲酸，p-甲苯甲酸，0-甲苯甲酸，2-氯苯甲酸，α-萘甲酸，β-萘甲酸，9-苯蒽甲酸，3-苯蒽甲酸，蒽醌-α-羧酸，蒽醌-β-羧酸和脱氢枞酸中的一种酸。
17、按照权利要求16所述的组合物，其特征在于：所说的聚α烯烃具有小于10个碳原子。
18、按照权利要求1所述的组合物，其特征在于：油成分具有芳香含量小于6%。
19、一种缓冲管凝胶组合物，其特征在于：由约20-90%的一种油成分，约5-50%的一种凝胶收缩抑制剂，和约4-30%的铝皂络合物组成，其中油成分和凝胶收缩抑制剂的重量比是约7∶3-1∶1。
20、按照权利要求19所述的组合物，其特征在于：油成分占总量的约50-75%，凝胶收缩抑制剂占总量的约25-45%，和铝皂络合物占总量的约6-8%。
21、按照权利要求19所述的组合物，其特征在于：铝皂络合物占总量的约6-7%，所说的油占总量的约54-56%，和所说的凝胶收缩抑制剂占总量的约34-36%。
22、按照权利要求19所述的组合物，其特征在于：所述的凝胶收缩抑制剂是聚丁烯，一种嵌段共聚物或其混合物。
23、按照权利要求22所述的组合物，其特征在于：铝皂络合物具有脂肪酸对于芳香酸的比率是约1∶1。
24、按照权利要求23所述的组合物，其特征在于：铝皂络合物具有全部酸对铝的比率是约2。
25、按照权利要求24所述的组合物，其特征在于：所述的矿物油是食品级矿物油。
26、按照权利要求19所述的组合物，其特征在于：更包括至少一种倾点下降剂占总量的约0.5到10%之间，和一种抗氧化剂按重量占总量的约0.1到2%之间。
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