CN110078964A - 一种耐磨耐高温材料的制备方法及其在石油钻采密封材料中的应用 - Google Patents
一种耐磨耐高温材料的制备方法及其在石油钻采密封材料中的应用 Download PDFInfo
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Abstract
本发明公开了一种耐磨耐高温材料的制备方法及其在石油钻采密封材料中的应用,所述耐磨耐高温材料的制备方法,包括以下步骤,制备混炼胶;将聚四氟乙烯薄膜进行表面活化处理;将混炼胶加入有机溶剂中,并加入酚醛树脂,混合搅拌均匀得胶浆;在经活化处理的聚四氟乙烯薄膜表面均匀涂抹硅烷偶联剂,得硅烷偶联剂层,在硅烷偶联剂层的表面均匀涂抹胶浆,得改性聚四氟乙烯薄膜;将改性聚四氟乙烯薄膜具有胶浆的一面包裹混炼胶,并施压成型,再经加压热硫化处理得所述耐磨耐高温材料;本发明的有益效果为:本发明所述一种耐磨耐高温材料的制备方法,制备的耐磨耐高温材料具有耐磨、抗冲击、耐高温、耐老化、耐腐蚀的性能,可应用于特殊密封领域。
Description
技术领域
本发明涉及耐磨耐高温材料技术领域,具体涉及一种耐磨耐高温材料的制备方法及其在石油钻采密材料中的应用。
背景技术
聚四氟乙烯(PTFE)材料因其具有极好的耐高温、低温性能、优异的耐化学腐蚀性、低摩擦因数等诸多优点,常常用来与其他材料组合并广泛用于生产橡胶密封件、低摩擦阻力减震件,以提高制品的使用寿命和密封性能,因此PTFE/橡胶的粘合性能成了研究的重点。
PTFE结构中碳链被氟原子完全屏蔽,因此具有非常稳定的化学特性,其饱和的氟原子赋予了PTFE极其稳定的惰性,很难与其他材料粘合,而随着工业的发展进步,在PTFE表面处理方面已有很多成熟的方法使其能够进行表面活化,例如萘纳处理液,化学填料融烧处理等。而多种类粘接剂的开发为提高PTFE的粘合强度提供了解决方案,例如无氟粘接环氧树脂类粘接剂,硅树脂粘接剂;含氟粘接偏氟乙烯类聚合物制备的溶剂型粘接剂。
虽然聚四氟乙烯与其他材料的粘接已趋于成熟,但其与橡胶热硫化粘合的报道较少,这两种材料的成型实现与否将会是两种材料能否互相取长补短的关键,也将拓展其应用领域。
发明内容
本发明的目的是提供一种耐磨耐高温材料的制备方法及其在石油钻采密封材料中的应用。
一种耐磨耐高温材料的制备方法,包括以下步骤:
(1)制备混炼胶;
(2)将聚四氟乙烯薄膜进行表面活化处理;本发明所述聚四氟乙烯薄膜活化处理的方式为:将聚四氟乙烯薄膜浸在萘钠处理液中进行活化处理;
(3)将混炼胶加入有机溶剂中,并加入酚醛树脂,混合搅拌均匀得胶浆;
(4)在经活化处理的聚四氟乙烯薄膜表面均匀涂抹硅烷偶联剂,得硅烷偶联剂层,在硅烷偶联剂层的表面均匀涂抹胶浆,得改性聚四氟乙烯薄膜;
(5)将改性聚四氟乙烯薄膜具有胶浆的一面包裹混炼胶,并施压成型,再经加压热硫化处理得所述耐磨耐高温材料。
本发明所述一种耐磨耐高温材料的制备方法,先制备混炼胶,使制得的混炼胶在耐腐蚀性、抗撕裂性和弹性性能方面,相对于生胶具有明显的提高;
因聚四氟乙烯薄膜具有很好的物理性能,抗酸抗碱、抗各种有机溶剂,几乎不溶于所有的溶剂,同时具有耐高温的特点,且摩擦系数极低,但将聚四氟乙烯薄膜与橡胶进行硫化粘合以提高使用性能的研究却比较少。本发明利用硅烷偶联剂与胶浆相结合将混炼胶粘附在聚四氟乙烯薄膜,即用聚四氟乙烯薄膜包裹混炼胶,产生一种耐磨耐高温、耐腐蚀的材料。
因经表面活化处理的聚四氟乙烯薄膜的表面具有一定的活性,将硅烷偶联剂涂抹在其表面后,聚四氟乙烯薄膜表面的活性成分与硅烷偶联剂中的硅原子相缩合,从而使硅原子与聚四氟乙烯薄膜表面紧紧接触;
而在硅烷偶联剂的表面涂抹一层胶浆(胶浆具有很强的粘性,其由混炼胶与酚醛树脂在有机溶剂中反应制得),这样就使得聚四氟乙烯薄膜的表面具有很强的粘性,即可以将混炼胶牢固地粘附在其表面,而进行加压热硫化处理。
如果不将混炼胶粘附在聚四氟乙烯薄膜的表面,就进行加热热硫化处理,得到的产品很容易开胶,影响其使用性能。
进一步地,步骤(1)中,所述混炼胶为混炼丁腈橡胶。
进一步地,所述混炼丁腈橡胶由下述重量份的原料制成:丁腈橡胶-40 80-120份、硬脂酸0.8-1.2份、硬质炭黑8-12份、氧化锌3-7份、硫磺1-3份、2-巯基苯并噻唑0.8-1.2份。
进一步地,所述混炼丁腈橡胶的制备方法为:将丁腈橡胶-40、氧化锌、硬脂酸、硬质炭黑、2-巯基苯并噻唑、硫磺依次加入混炼机中,混炼10-15min,得混炼丁腈橡胶。
硬脂酸在橡胶的合成和加工过程中起重要的作用,硬脂酸是天然胶、合成橡胶和胶乳中广泛应用的硫化活性剂,也可用作增塑剂和软化剂,在生产合成橡胶过程中需加硬脂酸作乳化剂,在制造泡沫橡胶时,硬脂酸可作起泡剂,硬脂酸还可用作橡胶制品的脱模剂。
硬质炭黑是橡胶用炭黑的一种习惯分类方法,指在橡胶制品中以补强为主要作用的炭黑,系相对软质炭黑而言。
氧化锌主要用于橡胶或电缆工业作补强剂和活性剂,在橡胶工业中用作天然橡胶,合成橡胶及乳胶的硫化活性剂,补强剂及着色剂,能使橡胶具有良好的耐腐蚀性、抗撕裂性和弹性。
2-巯基苯并噻唑是一种化学物质,作为通用型硫化促进剂,广泛用于各种橡胶。对于天然橡胶和通常以硫磺硫化的合成胶具有硫化促进作用。但使用前需要氧化锌、脂肪酸等进行活化。
硬脂酸作为硫化活性剂,增强合成橡胶的性能,氧化锌与2-巯基苯并噻唑相互作用,使2-巯基苯并噻唑活化,促进丁腈橡胶的硫化,增强合成橡胶的耐腐蚀性、抗撕裂性和弹性,炭黑的加入对合成橡胶的性能起到增强的作用,使所生成的合成橡胶-混炼胶相对于丁腈橡胶在耐腐蚀性、抗撕裂性和弹性方面都有所提高。
进一步地,步骤(2)中,聚四氟乙烯薄膜的厚度为0.5mm以下。聚四氟乙烯薄膜一般称作“不粘涂层”或易清洁物料,这种材料具有抗酸抗碱、抗各种有机溶剂的特点,几乎不溶于所有的溶剂,同时,聚四氟乙烯薄膜具有耐高温的特点,它的摩擦系数极低。
进一步地,步骤(3)中,所述有机溶剂为苯、二甲苯或乙酸乙酯。
进一步地,步骤(3)中,所述混炼胶、酚醛树脂、有机溶剂的量比为1-1.5:3:4。将混炼胶溶解在有机溶剂中与酚醛树脂发生反应,此反应只需在常温下搅拌即可发生,混炼胶与酚醛树脂发生反应生成一种炼胶,该炼胶具有很好的粘性;所述酚醛树脂为液体酚醛树脂,可以为钡酚醛树脂。
进一步地,步骤(5)中,所述施压的压力为1.8-2.5MPa;施压维持的时间为2-3min。
进一步地,步骤(5)中,所述加压的压力为8-9MPa,在此压力下的硫化温度为145-155℃,硫化时间为10-12min。
进一步地,所述一种耐磨耐高温材料在石油钻采密封材料中的应用。
本发明的有益效果为:本发明所述一种耐磨耐高温材料的制备方法,先制备混炼胶,使制得的混炼胶在耐腐蚀性、抗撕裂性和弹性性能方面,相对于生胶具有明显的提高;因经表面活化处理的聚四氟乙烯薄膜的表面具有一定的活性,将硅烷偶联剂涂抹在其表面后,聚四氟乙烯薄膜表面的活性成分与硅烷偶联剂中的硅原子相缩合,从而使硅原子与聚四氟乙烯薄膜表面紧紧接触;
而在硅烷偶联剂的表面涂抹一层胶浆(胶浆具有很强的粘性,其由混炼胶与酚醛树脂在有机溶剂中反应制得),这样就使得聚四氟乙烯薄膜的表面具有很强的粘性,即可以将混炼胶牢固地粘附在其表面,而进行加压热硫化处理得一种耐磨、抗冲击、耐高温、耐老化、耐腐蚀,化学性质稳定的材料,这种材料可应用于特殊密封领域。
本发明所述一种耐磨耐高温材料的制备方法,制备方法比较简单,容易实现,可以进行大规模的生产。
具体实施方式
实施例一
一种耐磨耐高温材料的制备方法,包括以下步骤:
(1)制备混炼胶;
(2)将聚四氟乙烯薄膜进行表面活化处理;
(3)将混炼胶加入有机溶剂中,并加入酚醛树脂,混合搅拌均匀得胶浆;
(4)在经活化处理的聚四氟乙烯薄膜表面均匀涂抹硅烷偶联剂,得硅烷偶联剂层,在硅烷偶联剂层的表面均匀涂抹胶浆,得改性聚四氟乙烯薄膜;
(5)将改性聚四氟乙烯薄膜具有胶浆的一面包裹混炼胶,并施压成型,再经加压热硫化处理得所述耐磨耐高温材料。
所述耐磨耐高温材料可以应用到石油钻采密封材料中。
实施例二
一种耐磨耐高温材料的制备方法,包括以下步骤:
(1)制备混炼丁腈橡胶;所述混炼丁腈橡胶由下述重量份的原料制成:丁腈橡胶-40 80kg、硬脂酸0.8kg、硬质炭黑8kg、氧化锌3kg、硫磺1kg、2-巯基苯并噻唑0.8kg;其制备方法为:将丁腈橡胶-40、氧化锌、硬脂酸、硬质炭黑、2-巯基苯并噻唑、硫磺依次加入混炼机中,混炼10min,得混炼丁腈橡胶;丁腈橡胶-40在氧化锌、硬脂酸、硬质炭黑、2-巯基苯并噻唑、硫磺的作用下进行改性得到一种耐腐蚀性、抗撕裂性和弹性都有所提高的混炼胶-混炼丁腈橡胶;
(2)将厚度为0.5mm以下的的聚四氟乙烯薄膜进行表面活化处理;
(3)将混炼胶加入有机溶剂苯中,并加入酚醛树脂,所述混炼胶、酚醛树脂、有机溶剂的量比为1:3:4,混合搅拌均匀得胶浆;
(4)在经活化处理的聚四氟乙烯薄膜表面均匀涂抹硅烷偶联剂,得硅烷偶联剂层,在硅烷偶联剂层的表面均匀涂抹胶浆,得改性聚四氟乙烯薄膜;
(5)将改性聚四氟乙烯薄膜具有胶浆的一面包裹混炼胶,并用1.8MPa的压力施压成型,并保持压力2min,再经8MPa的压力加压,并在此压力下进行温度为145℃,时间为10min的热硫化处理得所述耐磨耐高温材料。
所述耐磨耐高温材料可以应用到石油钻采密封材料中。
实施例三
一种耐磨耐高温材料的制备方法,包括以下步骤:
(1)制备混炼丁腈橡胶;所述混炼丁腈橡胶由下述重量份的原料制成:丁腈橡胶-40 100kg、硬脂酸1kg、硬质炭黑10kg、氧化锌5kg、硫磺2kg、2-巯基苯并噻唑1kg;其制备方法为:将丁腈橡胶-40、氧化锌、硬脂酸、硬质炭黑、2-巯基苯并噻唑、硫磺依次加入混炼机中,混炼12min,得混炼丁腈橡胶;丁腈橡胶-40在氧化锌、硬脂酸、硬质炭黑、2-巯基苯并噻唑、硫磺的作用下进行改性得到一种耐腐蚀性、抗撕裂性和弹性都有所提高的混炼胶-混炼丁腈橡胶;
(2)将厚度为0.5mm以下的的聚四氟乙烯薄膜进行表面活化处理;
(3)将混炼胶加入有机溶剂二甲苯中,并加入酚醛树脂,所述混炼胶、酚醛树脂、有机溶剂的量比为1.2:3:4,混合搅拌均匀得胶浆;
(4)在经活化处理的聚四氟乙烯薄膜表面均匀涂抹硅烷偶联剂,得硅烷偶联剂层,在硅烷偶联剂层的表面均匀涂抹胶浆,得改性聚四氟乙烯薄膜;
(5)将改性聚四氟乙烯薄膜具有胶浆的一面包裹混炼胶,并用2MPa的压力施压成型,并保持压力2min,再经8MPa的压力加压,并在此压力下进行温度为150℃,时间为11min的热硫化处理得所述耐磨耐高温材料。
所述耐磨耐高温材料可以应用到石油钻采密封材料中。
实施例四
一种耐磨耐高温材料的制备方法,包括以下步骤:
(1)制备混炼丁腈橡胶;所述混炼丁腈橡胶由下述重量份的原料制成:丁腈橡胶-40 120kg、硬脂酸1.2kg、硬质炭黑12kg、氧化锌7kg、硫磺3kg、2-巯基苯并噻唑1.2kg;其制备方法为:将丁腈橡胶-40、氧化锌、硬脂酸、硬质炭黑、2-巯基苯并噻唑、硫磺依次加入混炼机中,混炼15min,得混炼丁腈橡胶;丁腈橡胶-40在氧化锌、硬脂酸、硬质炭黑、2-巯基苯并噻唑、硫磺的作用下进行改性得到一种耐腐蚀性、抗撕裂性和弹性都有所提高的混炼胶-混炼丁腈橡胶;
(2)将厚度为0.5mm以下的的聚四氟乙烯薄膜进行表面活化处理;
(3)将混炼胶加入有机溶剂乙酸乙酯中,并加入酚醛树脂,所述混炼胶、酚醛树脂、有机溶剂的量比为1.5:3:4,混合搅拌均匀得胶浆;
(4)在经活化处理的聚四氟乙烯薄膜表面均匀涂抹硅烷偶联剂,得硅烷偶联剂层,在硅烷偶联剂层的表面均匀涂抹胶浆,得改性聚四氟乙烯薄膜;
(5)将改性聚四氟乙烯薄膜具有胶浆的一面包裹混炼胶,并用2.5MPa的压力施压成型,并保持压力3min,再经9MPa的压力加压,并在此压力下进行温度为155℃,时间为12min的热硫化处理得所述耐磨耐高温材料。
所述耐磨耐高温材料可以应用到石油钻采密封材料中。
对比例一
一种耐磨耐高温材料的制备方法,包括以下步骤:
(1)制备混炼丁腈橡胶;所述混炼丁腈橡胶由下述重量份的原料制成:丁腈橡胶-40 100kg、硬脂酸1kg、硬质炭黑10kg、氧化锌5kg、硫磺2kg、2-巯基苯并噻唑1kg;其制备方法为:将丁腈橡胶-40、氧化锌、硬脂酸、硬质炭黑、2-巯基苯并噻唑、硫磺依次加入混炼机中,混炼12min,得混炼丁腈橡胶;丁腈橡胶-40在氧化锌、硬脂酸、硬质炭黑、2-巯基苯并噻唑、硫磺的作用下进行改性得到一种耐腐蚀性、抗撕裂性和弹性都有所提高的混炼胶-混炼丁腈橡胶;
(2)将聚四氟乙烯薄膜包裹混炼胶,并用2MPa的压力施压成型,并保持压力2min,再经8MPa的压力加压,并在此压力下进行温度为150℃,时间为11min的热硫化处理得所述耐磨耐高温材料。
对比例二
制备混炼丁腈橡胶;所述混炼丁腈橡胶由下述重量份的原料制成:丁腈橡胶-40120kg、硬脂酸1.2kg、硬质炭黑12kg、氧化锌7kg、硫磺3kg、2-巯基苯并噻唑1.2kg;其制备方法为:将丁腈橡胶-40、氧化锌、硬脂酸、硬质炭黑、2-巯基苯并噻唑、硫磺依次加入混炼机中,混炼15min,得混炼丁腈橡胶;丁腈橡胶-40在氧化锌、硬脂酸、硬质炭黑、2-巯基苯并噻唑、硫磺的作用下进行改性得到一种耐腐蚀性、抗撕裂性和弹性都有所提高的混炼胶-混炼丁腈橡胶。
本发明制备的耐磨耐高温材料与对比例一所述耐磨耐高温材料,在耐磨性能方面的对比研究,结果如表1所示:
表1
从表1可以看出,本发明所述耐磨耐高温材料在耐磨性能方面远远优越于对比例一所述耐磨耐高温材料。本发明所述耐磨耐高温材料采用胶浆作为粘结剂,将混炼胶与经改性处理的聚四氟乙烯薄膜粘结在一起再施压、热硫化处理,而对比文件1直接将混炼胶与聚四氟乙烯薄膜施压、热硫化处理得耐磨耐高温材料,可见:经胶浆粘结后,所得耐磨耐高温材料的性能得到很大程度的提高。
本发明制备的耐磨耐高温材料与对比例一所述耐磨耐高温材料,在耐老化性能方面的对比研究,结果如表2所示:
表2
从表2可以看出,本发明所述耐磨耐高温材料在耐老化性能方面远远优越于对比例一所述耐磨耐高温材料。本发明所述耐磨耐高温材料采用胶浆作为粘结剂,将混炼胶与经改性处理的聚四氟乙烯薄膜粘结在一起再施压、热硫化处理,而对比文件1直接将混炼胶与聚四氟乙烯薄膜施压、热硫化处理得耐磨耐高温材料,可见:经胶浆粘结后,所得耐磨耐高温材料的耐老化性能得到很大程度的提高。
本发明制备的耐磨耐高温材料与对比例二所述耐磨耐高温材料,在耐高温性能方面的对比研究,结果如表3所示
表3
从表3可以看出:本发明所述一种耐磨耐高温材料在耐高温性能方面明显优越于对比例二所述耐磨耐高温材料。本发明所述一种耐磨耐高温材料,使用改性的聚四氟乙烯薄膜包裹混炼胶经加压、热硫化处理得到;而对比例二所述耐磨耐高温材料由混炼胶制成。包裹改性聚四氟乙烯膜的混炼胶在疲劳试验时需要破坏粘合界面后,出现的弯折裂口才能扩散直至龟裂,而没有这种粘合的改性聚四氟乙烯的混炼胶出现裂口及扩散更容易。
本发明不局限于上述最佳实施方式,任何人在本发明的启示下都可得出其他各种形式的产品,但不论在其细节上作任何变化,凡是具有与本申请相同或相近似的技术方案,均落在本发明的保护范围之内。
Claims (10)
1.一种耐磨耐高温材料的制备方法,其特征在于,包括以下步骤
(1)制备混炼胶;
(2)将聚四氟乙烯薄膜进行表面活化处理;
(3)将混炼胶加入有机溶剂中,并加入酚醛树脂,混合搅拌均匀得胶浆;
(4)在经活化处理的聚四氟乙烯薄膜表面均匀涂抹硅烷偶联剂,得硅烷偶联剂层,在硅烷偶联剂层的表面均匀涂抹胶浆,得改性聚四氟乙烯薄膜;
(5)将改性聚四氟乙烯薄膜具有胶浆的一面包裹混炼胶,并施压成型,再经加压热硫化处理得所述耐磨耐高温材料。
2.根据权利要求1所述一种耐磨耐高温材料的制备方法,其特征在于,步骤(1)中,所述混炼胶为混炼丁腈橡胶。
3.根据权利要求2所述一种耐磨耐高温材料的制备方法,其特征在于,所述混炼丁腈橡胶由下述重量份的原料制成:丁腈橡胶-40 80-120份、硬脂酸0.8-1.2份、硬质炭黑8-12份、氧化锌3-7份、硫磺1-3份、2-巯基苯并噻唑0.8-1.2份。
4.根据权利要求3所述一种耐磨耐高温材料的制备方法,其特征在于,所述混炼丁腈橡胶的制备方法为:将丁腈橡胶-40、氧化锌、硬脂酸、硬质炭黑、2-巯基苯并噻唑、硫磺依次加入混炼机中,混炼10-15min,得混炼丁腈橡胶。
5.根据权利要求1所述一种耐磨耐高温材料的制备方法,其特征在于,步骤(2)中,聚四氟乙烯薄膜的厚度为0.5mm以下。
6.根据权利要求1所述一种耐磨耐高温材料的制备方法,其特征在于,步骤(3)中,所述有机溶剂为苯、二甲苯或乙酸乙酯。
7.根据权利要求1所述一种耐磨耐高温材料的制备方法,其特征在于,步骤(3)中,所述混炼胶、酚醛树脂、有机溶剂的量比为1-1.5:3:4。
8.根据权利要求1所述一种耐磨耐高温材料的制备方法,其特征在于,步骤(5)中,所述施压的压力为1.8-2.5MPa;施压维持的时间为2-3min。
9.根据权利要求1所述一种耐磨耐高温材料的制备方法,其特征在于,步骤(5)中,所述加压的压力为8-9MPa,在此压力下的硫化温度为145-155℃,硫化时间为10-12min。
10.权利要求1-9所述一种耐磨耐高温材料在石油钻采密封材料中的应用。
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