CN1201473A - 有机硅糊状物和脂膏 - Google Patents

有机硅糊状物和脂膏 Download PDF

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Publication number
CN1201473A
CN1201473A CN96198049A CN96198049A CN1201473A CN 1201473 A CN1201473 A CN 1201473A CN 96198049 A CN96198049 A CN 96198049A CN 96198049 A CN96198049 A CN 96198049A CN 1201473 A CN1201473 A CN 1201473A
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Prior art keywords
fat
carbonate
mashed prod
mashed
prod
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B·达尔伯
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Rhodia Chimie SAS
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Rhone Poulenc Chimie SA
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Publication of CN1201473A publication Critical patent/CN1201473A/zh
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Abstract

含有至少一种25℃时运动粘度至少是500mPa·s的油性二有机聚硅氧烷聚合物和至少一种碱金属或碱土金属碳酸盐,但是不含严格意义上的触变剂的有机硅糊状物和脂膏,其中所述碳酸盐的粒度为0.5μmBET比表面为5m2/g,并且以组合物总量的至少20wt%的量存在。制备方法在低温例如5—40℃下进行。

Description

有机硅糊状物和脂膏
本发明涉及尤其是在碱性，酸性和盐基质中具有流动极限和抗降解性的有机硅糊状物或脂膏、其制备方法及其特别在食品领域的用途(润滑作用，活栓润滑脂等)。
硅氧烷脂膏通常用于润滑在相对低的应力下工作的零件，例如活栓。硅氧烷糊状物也用作填充糊状物，特别是用于电路保护，或者作为减震器。
在可交联，特别是可冷交联硅氧烷弹性体组合物领域，有人建议将沉淀磷酸盐加入到这些组合物中。目的是使器皿中的该组合物在其应用之时，在固化之前具备一定的稠度，提高弹性体的机械性能。
此外，1977年12月6日提交的专利申请JP-A-52/146405公开了一种由低粘度润滑油(在实施例中在37.8℃时在大约110和220mPa·s之间)、防锈剂和碳酸钙组成的润滑脂膏，所述油可能是一种矿物油，二酯油，硅氧烷油或各种性质油的混合物。该组合物可以含有至多50％重量的碳酸钙，而且优选含20％至30％。涉及其区别特征在于油的性质的不同类型的脂膏的该文献主要涉及矿物油。该申请没有涉及应用硅氧烷油的实施例。
迄今为止，硅氧烷糊状物和脂膏一般由没有脂族不饱和度的二有机聚硅氧烷油，燃烧二氧化硅和触变体系组成，所述触变体系可以是，例如，硼酸和多醇的结合产物，聚醚，特别是聚氧亚烷基二醇，或者是一种低分子量α，ω-二羟基硅氧烷油。硅氧烷糊状物和脂膏一般通过热加工制备，包括在大约120℃将各组分混合几小时。
为了给予糊状物以良好的流变学特性以及为了避免其流变学特性随着时间的推移而变坏，高温过程是必须的，但是，在某些情况下，在再现流变学特性时会遇到困难。另外，由于触变体系的复杂性，特别是由于加热，使生产成本提高。
专利DE-A-2535304公开了向有固化剂的硅氧烷树脂中加入30-70％重量天然碳酸盐。天然碳酸钙优选是疏水性的，而且其粒度小于10μm。
专利JP-A-4307058公开了一种以硅氧烷油或树胶为基础的疏水流体，其中加入粒度大约为45μm的天然碳酸钙。
但是，这些磨细的粒度大于1μm的天然碳酸盐未赋予该组合物以流动极限。
本发明的主要目的是提供新的硅氧烷糊状物和脂膏，其即使在高温下也具有随时间稳定的高的流动极限，并且其可以通过冷加工，在相对体成本、尤其是在低于先前技术硅氧烷糊状物和脂膏的成本的条件下制备。
本发明的另一个主要目的是提供这样的糊状物和脂膏，其在碱性和酸性基质中和在海水环境中具有提高的耐久性。
本发明的另一个主要目的是提供这样的糊状物和脂膏，其可以在食品领域使用而没有危害。
而且本发明的另一个目的是提供这样的糊状物和脂膏，其流动极限可以以简单和可再现的方式调节到至少等于20Pa的值，该性质可根据下文详述内容来测定。
因此，本发明的主题是一种有机硅糊状物或脂膏，其中含有至少一种25℃时运动粘度至少等于500mPa·s的油性二有机聚硅氧烷聚合物和至少一种碱金属或碱土金属碳酸盐，不存在一种严格意义上的触变剂，即先有技术纯触变性质的试剂，碳酸盐粒度(平均颗粒直径)小于或等于0.5μm，碳酸盐具有大于5m2/g的高的BET比表面，而且相对于组合物总重来说以至少20％，优选大于30％，优选30至70％的此例存在，更优选为35至45％重量。
申请人发现在本发明条件下，通过单一化合物可以代替通常的触变剂和填充剂，所述单一化合物是一种上文定义的碳酸盐，它的使用使其能在低温下工作，并且保证如此制备的糊状物和脂膏具备所需的机械性能，而且给予糊状物和脂膏随时间稳定的高的流动极限，即使在高温下也是如此。另外，本发明的一些碳酸盐完全适用于食品领域。获得这样的糊状物或脂膏的事实带来的另一个优点是呈现改善的油脂性。
根据本发明，术语低温过程被理解为是指可以在5至40℃，优选在室温下(大约20至25℃)进行的过程。
油性聚合物优选具有800和30000mPa·s之间的运动粘度，更优选900和15000mPa·s之间的运动粘度。
本发明的碳酸盐优选具有小于或等于0.1μm，更优选0.01和0.1μm之间的平均粒径或粒度，并且优选具有10至70m2/g，优选15至30m2/g的BET比表面。
优选碱土金属碳酸盐，优选碳酸钙。
作为适合实施本发明的商售产品，可以提到的是沉淀碳酸盐。
根据本发明，碳酸盐被理解为是指工业中使用的碳酸盐，是含有一定量水合残余水份，一般含有大约0.1至0.5％水合水的碳酸盐。
在本发明应用中，油的粘度是25℃时的牛顿运动粘度，是使用Brookfield粘度计根据1982年5月AF NOR NF T76102标准测定的。
BET比表面是根据相应于1987年11月AFNOR NFT 45007标准的《美国化学学会会刊》(The Journal of American ChemicalSociety)，Vol.80，第309页(1938)中描述的Brunauer-Emmet-Teller方法来测定的。
在特别优选的方法中，已知为了提高碳酸盐在疏水基质中的分散性，特别是用脂肪族羧酸，例如硬脂酸来处理本发明的碳酸盐。
已经有益地发现，对于给定的粒度和给定的比表面，流动极限随着碳酸盐的量而增大，因此本领域技术人员容易获得设想应用的组合物或所需流动极限的组合物，并且可以获得非常高的流动极限。对于一种给定的碳酸盐也可以变化油性聚合物的粘度。
本发明糊状物基本组成的油性二有机聚硅氧烷聚合物总的来说对应于下面的分子式：
R3Si(OSiR2)nOSiR3其中符号R可以相同或不同，代表没有脂族不饱和度，且具有不多于10个碳原子的烃基，符号n代表能够导致上述粘度的任何数。
除终端部分外，这些线性聚合物因此而基本上由式R2SiO单元顺序组成；但是不排除特别是以不大于1％R2SiO部分的比例存在的少量其它部分，例如式SiO2或RSiO1.5部分。
符号R所代表的烃基选自
-具有1至8个碳原子的烷基，例如甲基，乙基，丙基，丁基，戊基，己基和2-乙基己基，
-具有6至10个碳原子的一个苯环的芳香基团，例如苯基，甲苯基，二甲苯基，乙基苯基，异丙苯基和丁基苯基。
但是对于每个聚合物分子来说，优选所有烃基R的至少45％，更优选至少80％是甲基。其中大多数是通过硅氧烷生产商工业生产的。
作为可以使用的聚合物的范例，可以提到的是下式所代表的那些化合物：
(CH3)3SiO[Si(CH3)2O]n1Si(CH3)3
(CH3)3SiO[Si(CH3)2O]n2[Si(C6H5)(CH3)O]n3Si(CH3)3
(CH3)3SiO[Si(CH3)2O]n4[Si(C6H5)2O]n5Si(CH3)3其中
选择n1至n5，使具有上文所定义的粘度。更精确地说，n1，n2+n3+n4+n5在200和1000之间。
本发明使获得具有大于20Pa的流动极限的糊状物或脂膏成为可能，并且该极限可以超过500Pa这样高的值，并且可以以可再现的方式进行。本发明也使完成上述其它目的成为可能。
根据最终的应用，本发明糊状物或脂膏也可以混入其它常用无机填充物或其它添加剂。
本发明还涉及一种制备糊状物和脂膏的方法，其中糊状物和脂膏在低温，优选在5和40℃之间的温度下使用，根据本发明的一个优选实施方案，搅拌下向硅油中逐渐加入碳酸盐和/或在室温下进行混合，尤其是混合几小时，然后视具体情况而定将混合物在真空下脱气。
更一般性地来说，本发明还涉及本发明碳酸盐加入到硅氧烷糊状物或脂膏中的用途，特别是在食品应用、使糊状物或脂膏具有流动极限方面的用途，所述碳酸盐以上述量存在。
对于食品应用，必须使用法律所规定的允许用于食品的油和碳酸盐。关于油，它们尤其是完全甲基化的。
本发明将以非限制性本发明例举的实施方案更详细地加以说明，例举的实施方案会阐明本发明其它特征和优点。
糊状物中碳酸钙的量在20％和40％重量比之间变化。对包含三甲基甲硅烷基终端部分的聚二甲基硅氧烷油的不同粘度进行了试验：粘度在1000和10000mPa·s之间。所有试验都是在不加入触变剂或燃烧硅石的条件下进行的。每次都得到了其流动极限随沉淀磷酸盐的量的增加而增加的脂膏状白色糊状物。
在平行试验中，用具有大约2m2/g BET比表面和5μm平均粒径的磨细的天然碳酸钙进行了试验，当天然碳酸盐含量达40％重量时，该糊状物没有流动极限。
实施例1
制备有沉淀碳酸盐的糊状物：
向叶片式混合器(Meili)中加入2190g 25℃时粘度为10000mPa·s，带有三甲基甲硅烷基终端基团的聚二甲基硅氧烷硅油，并逐渐加入939g沉淀碳酸钙(购自Rhone-Poulenc的CalofortS；平均直径0.07μm BET表面积为23m2/g)。在室温下(22℃)混合2小时，直到获得均匀的白色糊状物为止。该糊状物在真空(30mmHg，3990Pa)下脱气5分钟。这样制得含有30％(重量)沉淀碳酸盐的白色糊状物。
用相同方法制备含有20％和40％CalofortS的糊状物。
用购自Omya的BLR3磨细的天然碳酸盐(平均直径5μm，BET表面为2m2/g)代替CalofortS，在相同条件下(仍然用相同的油)也制备了一种糊状物。该糊状物含有40％BLR3碳酸盐。
糊状物性能分析：
测定流动极限：
根据厂商在“使用5.0版软件对于流变仪的Carri-med CSL范围的操作说明”中的规定，用锥体/平面几何学，锥体直径为2cm，角为1°，在25℃下，使用Carri-med CS 100固化应变流变仪(Carri-med公司出售)进行测定。
根据下面的Carri-med说明，根据Cass-on模型用测定值计算极限。
以Pa为单位的流动极限(Casson)
含有20％CalofortS的糊状物   57
含有30％CalofortS的糊状物   300
含有40％Calofort S的糊状物  1000
含有40％BLR3的糊状物  0.1
发现流动极限随着沉淀碳酸盐的量的增加而增大。另一方面，含有BLR 3天然碳酸盐的糊状物没有流动极限。
流变学随温度的变化：
在-10℃和+60℃之间研究本发明糊状物流动极限的变化；含有40％CalofortS的糊状物的流变学在试验温度范围内不变化。
本发明糊状物在高温下的稳定性：
在通风箱中以每24小时25℃的速度使糊状物由100℃升至200℃。直至升至150℃为止未发现性能(表观，稠度)发生变化。在175℃时，发现表面表观有所变化，但是稠度没有变化。在200℃保持24小时后，变化与在175℃时发现的相同；另一方面，在200℃保持100小时后，记录到表面严重硬化，糊状物中心增稠。
实施例2：
用沉淀碳酸盐，用实施例1中粘度是1000mPa·s的油制备脂膏：
向叶片式混合器(Meili)中加入硅油并逐渐加入沉淀碳酸钙(购自Rhone-Poulenc的CalofortS)。混合3小时，直到获得均匀的白色糊状物。该糊状物在真空(30mmHg)下脱气5分钟，这样制得含有35％Calofort S的脂膏。
该脂膏在25℃下具有160Pa Casson流动极限。
这种新的脂膏可以用于润滑饮用水旋塞。
根据本发明使用的沉淀碳酸盐能够实现本发明提出的各种目的。
不用说，为了调节各种应用的流动极限，如果需要，本领域技术人员能用实施例中的数据和结果进行简单的常规试验。

Claims (19)

1.含有至少一种在25℃下运动粘度至少等于500mPa·s的油性二有机聚硅氧烷聚合物和至少一种碱金属或碱土金属碳酸盐，其中不存在严格意义上的触变剂的有机硅糊状物或脂膏，所述碳酸盐的粒度小于或等于0.5μm，其BET比表面大于5m2/g，并以相对于组合物总量的至少20％重量的比例存在。
2.权利要求1的糊状物或脂膏，其特征在于碳酸盐以大于相对于组合物总量的30％重量的比例存在。
3.权利要求1的糊状物或脂膏，其特征在于碳酸盐以相对于组合物总量的30至70％重量存在。
4.权利要求3的糊状物或脂膏，其特征在于碳酸盐以相对于组合物总量的35至45％重量存在。
5.权利要求1至4中任一项的糊状物或脂膏，其特征在于所述油性聚合物具有800和30000mPa·s之间的运动粘度。
6.权利要求5的糊状物或脂膏，其特征在于所述油性聚合物具有900和15000mPa·s之间的运动粘度。
7.权利要求1至6中任一项的糊状物或脂膏，其特征在于碳酸盐的粒度小于或等于0.1μm。
8.权利要求7的糊状物或脂膏，其特征在于碳酸盐的粒度为0.01～0.1μm。
9.权利要求1至8中任一项的糊状物或脂膏，其特征在于碳酸盐的BET此表面为10至70m2/g。
10.权利要求9的糊状物或脂膏，其特征在于碳酸盐的BET比表面为15至30m2/g。
11.权利要求1至10中任一项的糊状物或脂膏，其特征在于碳酸盐是一种碱土金属碳酸盐。
12.权利要求11的糊状物或脂膏，其特征在于碱土金属碳酸盐是碳酸钙。
13.权利要求1至12中任一项的糊状物或脂膏，其特征在于碳酸盐是沉淀碳酸盐。
14.权利要求1至13中任一项的糊状物或脂膏，其特征在于碳酸盐经过硬脂酸处理。
15.权利要求1至14中任一项的糊状物或脂膏，其特征在于油性二有机聚硅氧烷聚合物对应于通式
R3Si(OSiR2)nOSiR3其中符号R可以相同或不同，代表没有脂族不饱和度且具有不多于10个碳原子的烃基，符号n代表能够产生至少等于500mPa·s粘度的任何数。
16.权利要求15的糊状物或脂膏，其特征在于符号R全部代表甲基。
17.权利要求1至16中任一项的糊状物或脂膏，其特征在于具有大于20Pa的流动极限。
18.权利要求1至17中任一项的有机硅糊状物或脂膏的制备方法，其特征在于使用低温糊状物或脂膏。
19.权利要求18的制备方法，其特征在于在5和40℃之间使用糊状物或脂膏。
CN96198049A 1995-10-31 1996-10-30 有机硅糊状物和脂膏 Pending CN1201473A (zh)

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CN103772991A (zh) * 2012-10-23 2014-05-07 信越化学工业株式会社 硅酮组合物以及润滑脂

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CN103772991A (zh) * 2012-10-23 2014-05-07 信越化学工业株式会社 硅酮组合物以及润滑脂
CN103772991B (zh) * 2012-10-23 2017-04-12 信越化学工业株式会社 硅酮组合物以及润滑脂
CN103087551A (zh) * 2013-02-04 2013-05-08 道奇威（成都）科技有限公司 一种提高塑料用碳酸钙疏水性和耐温性的表面改性方法

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