CN107906202A - 一种纤维盘根的制备方法 - Google Patents

一种纤维盘根的制备方法 Download PDF

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CN107906202A
CN107906202A CN201711118361.6A CN201711118361A CN107906202A CN 107906202 A CN107906202 A CN 107906202A CN 201711118361 A CN201711118361 A CN 201711118361A CN 107906202 A CN107906202 A CN 107906202A
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fiber
mixing
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mass ratio
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吴迪
徐珉
陈水
陈一水
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Abstract

本发明公开了一种纤维盘根的制备方法，属于密封材料技术领域。将改性芳纶纤维与盐酸混合浸泡，过滤，干燥后移入硫酸铜溶液中，混合浸泡，过滤，干燥，得1次处理改性芳纶纤维；将1次处理改性芳纶纤维与硅烷偶联剂混合浸泡，过滤，得滤饼，将滤饼与有机硅树脂混合浸泡，过滤，干燥，得2次处理改性芳纶纤维；将2次处理改性芳纶纤维与1号浸渍液混合浸泡，过滤，得预处理盘根纤维，将预处理芳纶纤维与编织机中进行编织，得纤维盘根坯料；将纤维盘根坯料与2号浸渍液混合浸泡，过滤，干燥，即得纤维盘根。本发明技术方案制备的纤维盘根具有优异的耐热性能及耐磨性能的特点。

Description

一种纤维盘根的制备方法
技术领域
本发明公开了一种纤维盘根的制备方法，属于密封材料技术领域。
背景技术
编织型密封填料即密封盘根是填料密封中应用最为广泛的，具有承载介质压力大、对介质的适应性广、成本低、安装方便等优点。在密封盘根中，聚四氟乙烯（PTFE）纤维编织密封填料具有优良的化学稳定性和自润滑性能，但缺点是热传导性差和热膨胀系数大，在一定温度和压力的工况条件下，容易产生蠕变或冷流现象，不适应高温、高压、高速的工况要求。然而，随着宇航、核电站、国防工业、石化工业的发展，当今密封问题所涉及的广度和深度已远远超越防止“跑、冒、滴、漏”的范围，诸如高温及超高温、低温及超低温、高压、高真空、高速以及强腐蚀等苛刻工况对密封填料提出了更高的要求
丁腈橡胶由于具有的良好耐油性、耐磨性和低廉的价格，在石油工业中得到了广泛应用，是井口密封盘根的主要材料。但是，分析油井常规密封盘根的材质和使用情况，发现应用过程中存在以下问题：1）这种材质具有较好的弹性，压缩回弹率大，但耐热性较差，弹性补偿性能不好，易老化，密封效果相对较差。2）在用盘根更换较为频繁，平均更换周期为1个月，严重井1～2d就需要更换，导致维护工作量和生产成本较大。3）材料表面缺陷是造成盘根磨损的重要因素。盘根的耐磨性能是由材质和表面性质所决定。
因此，如何改善传统盘根耐热性能及耐磨性能不佳的缺点，以获取更高综合性能的盘根，是其推广与应用，满足工业生产需求亟待解决的问题。
发明内容
本发明主要解决的技术问题是：针对传统盘根耐热性能及耐磨性能不佳的缺点，提供了一种纤维盘根的制备方法。
为了解决上述技术问题，本发明所采用的技术方案是：
（1）将金属纤维与玻璃纤维纺丝液按质量比1：3～1：5混合，得混合玻璃纤维纺丝液，将混合玻璃纤维纺丝液纺织成丝，得改性玻璃纤维；
（2）将改性玻璃纤维与芳纶纺丝液按质量比1：2～1：4混合，并加入芳纶纺丝液质量0.4～0.5倍的玻璃纤维，搅拌混合后，得改性芳纶纺丝液，将改性芳纶纺丝液纺织成丝，得改性芳纶纤维；
（3）将改性芳纶纤维与盐酸按质量比1：3～1：5混合浸泡，过滤，干燥后移入硫酸铜溶液中，混合浸泡，过滤，干燥，得1次处理改性芳纶纤维；
（4）将1次处理改性芳纶纤维与硅烷偶联剂按质量比1：8～1：10混合浸泡，过滤，得滤饼，将滤饼与有机硅树脂按质量比1：3～1：6混合浸泡，过滤，干燥，得2次处理改性芳纶纤维；
（5）将2次处理改性芳纶纤维与1号浸渍液按质量比1：5～1：6混合浸泡，过滤，得预处理盘根纤维，将预处理芳纶纤维与编织机中进行编织，得纤维盘根坯料；
（6）将纤维盘根坯料与2号浸渍液按质量比1：3～1：6混合浸泡，过滤，干燥，即得纤维盘根。
步骤（1）所述金属纤维为铁纤维，铝纤维或镍纤维中任意一种。
步骤（2）所述玻璃纤维为中碱玻璃纤维或无碱玻璃纤维中任意一种。
步骤（4）所述硅烷偶联剂为硅烷偶联剂KH-550，硅烷偶联剂KH-560或硅烷偶联剂KH-570中任意一种。
步骤（5）所述1号浸渍液的制备方法为将聚四氟乙烯与纳米二氧化钛和氯化锌按质量比5：1～5：2混合，并加入聚四氟乙烯质量0.08～0.10倍的丙酸钙，聚四氟乙烯质量0.10～0.14倍的滑石粉和聚四氟乙烯质量0.1～0.2倍的水，搅拌混合，得1号浸渍液。
步骤（6）所述2号浸渍液的制备过程为将凡士林和石蜡按质量比3：1～4：1混合，并加入凡士林质量0.2～0.4倍的卵磷脂，搅拌混合，得2号浸渍液。
本发明的有益效果是：
（1）本发明在制备纤维盘根时使用金属纤维改性的玻璃纤维，首先，改性玻璃纤维的加入可增加纤维盘根的强度，并且在盘根表面形成许多细小的触须，从而使产品的耐磨性得到提高，其次，在经过酸液浸泡后，改性玻璃纤维表面玻璃纤维被侵蚀，金属纤维显露，在浸泡于硫酸铜溶液后，可在盘根表面覆盖铜层，从而使产品的耐磨性进一步提高，并且由于铜和金属纤维导热性能优良，从而使产品的耐热性提高；
（2）本发明在制备纤维盘根时使用玻璃纤维，并将1次处理改性芳纶纤维与有机硅树脂混合浸泡，一方面，玻璃纤维在加入体系中后，可与改性玻璃纤维一起在盘根表面相处细小的触须，从而使产品的力学性能和耐磨性进一步提高，另一方面，玻璃纤维在硅烷偶联剂的作用下可与有机硅树脂结合，在干燥后，有机硅树脂可在盘根表面形成一层有机硅树脂的保护层，从而使产品的耐磨性和耐热性进一步提高。
具体实施方式
将金属纤维与玻璃纤维纺丝液按质量比1：3～1：5混合，于温度为700～850℃，转速为250～350r/min的条件下，搅拌混合30～40min后，得混合玻璃纤维纺丝液，将混合玻璃纤维纺丝液纺织成丝，得改性玻璃纤维；将改性玻璃纤维与芳纶纺丝液按质量比1：2～1：4混合于反应釜中，并向反应釜中加入芳纶纺丝液质量0.4～0.5倍的玻璃纤维，于温度为580～650℃，转速为240～300r/min的条件下搅拌混合70～80min后，得改性芳纶纺丝液，将改性芳纶纺丝液纺织成丝，得改性芳纶纤维；将改性芳纶纤维与浓度为2～4mol/L的盐酸按质量比1：3～1：5混合浸泡45～70min后，过滤，得滤渣，将滤渣移入干燥箱，于温度为70～90℃的条件下，恒温干燥15～30min后，将干燥后的改性芳纶纤维浸没质量分数15～20%的硫酸铜溶液中，于温度为30～45℃混合浸泡30～45min后，过滤，得1次预处理改性芳纶纤维，将1次预处理改性芳纶纤维于温度为75～85℃的条件下干燥20～30min后，得1次处理改性芳纶纤维；将1次处理改性芳纶纤维与硅烷偶联剂按质量比1：8～1：10混合，于温度为55～75℃的条件下浸泡3～4h后，过滤，得滤饼，将滤饼与有机硅树脂按质量比1：3～1：6混合，于温度为45～55℃的条件下浸泡100～150min后，过滤，得2次预处理改性芳纶纤维，将2次预处理改性芳纶纤维于温度为200～220℃的条件下，干燥25～45min后，得2次处理改性芳纶纤维；将2次处理改性芳纶纤维与1号浸渍液按质量比1：5～1：6混合，并于温度为55～75℃的条件下浸泡3～4h后，过滤，得预处理盘根纤维，将预处理盘根纤维移入编织机中进行编织，得纤维盘根坯料；将纤维盘根坯料与2号浸渍液按质量比1：3～1：6混合，于温度为80～90℃的条件下浸泡35～70min后，过滤，得预处理纤维盘根，将预处理纤维盘根移入干燥箱，于温度为35～45℃的条件下，干燥20～40min，即得纤维盘根。所述金属纤维为铁纤维，铝纤维或镍纤维中任意一种。所述硅烷偶联剂为硅烷偶联剂KH-550，硅烷偶联剂KH-560或硅烷偶联剂KH-570中任意一种。所述1号浸渍液的制备方法为将聚四氟乙烯与纳米二氧化钛和氯化锌按质量比5：1～5：2混合，并加入聚四氟乙烯质量0.08～0.10倍的丙酸钙，聚四氟乙烯质量0.10～0.14倍的滑石粉和聚四氟乙烯质量0.1～0.2倍的水，搅拌混合，得1号浸渍液。所述2号浸渍液的制备过程为将凡士林和石蜡按质量比3：1～4：1混合，并加入凡士林质量0.2～0.4倍的卵磷脂，搅拌混合，得2号浸渍液。
实例1
将金属纤维与玻璃纤维纺丝液按质量比1：5混合，于温度为850℃，转速为350r/min的条件下，搅拌混合40min后，得混合玻璃纤维纺丝液，将混合玻璃纤维纺丝液纺织成丝，得改性玻璃纤维；将改性玻璃纤维与芳纶纺丝液按质量比1：4混合于反应釜中，并向反应釜中加入芳纶纺丝液质量0.5倍的玻璃纤维，于温度为650℃，转速为300r/min的条件下搅拌混合80min后，得改性芳纶纺丝液，将改性芳纶纺丝液纺织成丝，得改性芳纶纤维；将改性芳纶纤维与浓度为4mol/L的盐酸按质量比1：5混合浸泡70min后，过滤，得滤渣，将滤渣移入干燥箱，于温度为90℃的条件下，恒温干燥30min后，将干燥后的改性芳纶纤维浸没质量分数20%的硫酸铜溶液中，于温度为45℃混合浸泡45min后，过滤，得1次预处理改性芳纶纤维，将1次预处理改性芳纶纤维于温度为85℃的条件下干燥30min后，得1次处理改性芳纶纤维；将1次处理改性芳纶纤维与硅烷偶联剂按质量比1：10混合，于温度为75℃的条件下浸泡4h后，过滤，得滤饼，将滤饼与有机硅树脂按质量比1：6混合，于温度为55℃的条件下浸泡150min后，过滤，得2次预处理改性芳纶纤维，将2次预处理改性芳纶纤维于温度为220℃的条件下，干燥45min后，得2次处理改性芳纶纤维；将2次处理改性芳纶纤维与1号浸渍液按质量比1：6混合，并于温度75℃的条件下浸泡4h后，过滤，得预处理盘根纤维，将预处理盘根纤维移入编织机中进行编织，得纤维盘根坯料；将纤维盘根坯料与2号浸渍液按质量比1：6混合，于温度为90℃的条件下浸泡70min后，过滤，得预处理纤维盘根，将预处理纤维盘根移入干燥箱，于温度为45℃的条件下，干燥40min，即得纤维盘根。所述金属纤维为铁纤维。所述硅烷偶联剂为硅烷偶联剂KH-550。所述1号浸渍液的制备方法为将聚四氟乙烯与纳米二氧化钛和氯化锌按质量比5：2混合，并加入聚四氟乙烯质量0.10倍的丙酸钙，聚四氟乙烯质量0.14倍的滑石粉和聚四氟乙烯质量0.2倍的水，搅拌混合，得1号浸渍液。所述2号浸渍液的制备过程为将凡士林和石蜡按质量比4：1混合，并加入凡士林质0.4倍的卵磷脂，搅拌混合，得2号浸渍液。
实例2
将玻璃纤维与芳纶纺丝液按质量比1：5混合于反应釜中，于温度为650℃，转速为300r/min的条件下搅拌混合80min后，得改性芳纶纺丝液，将改性芳纶纺丝液纺织成丝，得改性芳纶纤维；将改性芳纶纤维与浓度为4mol/L的盐酸按质量比1：5混合浸泡70min后，过滤，得滤渣，将滤渣移入干燥箱，于温度为90℃的条件下，恒温干燥30min后，将干燥后的改性芳纶纤维浸没质量分数20%的硫酸铜溶液中，于温度为45℃混合浸泡45min后，过滤，得1次预处理改性芳纶纤维，将1次预处理改性芳纶纤维于温度为85℃的条件下干燥30min后，得1次处理改性芳纶纤维；将1次处理改性芳纶纤维与硅烷偶联剂按质量比1：10混合，于温度为75℃的条件下浸泡4h后，过滤，得滤饼，将滤饼与有机硅树脂按质量比1：6混合，于温度为55℃的条件下浸泡150min后，过滤，得2次预处理改性芳纶纤维，将2次预处理改性芳纶纤维于温度为220℃的条件下，干燥45min后，得2次处理改性芳纶纤维；将2次处理改性芳纶纤维与1号浸渍液按质量比1：6混合，并于温度75℃的条件下浸泡4h后，过滤，得预处理盘根纤维，将预处理盘根纤维移入编织机中进行编织，得纤维盘根坯料；将纤维盘根坯料与2号浸渍液按质量比1：6混合，于温度为90℃的条件下浸泡70min后，过滤，得预处理纤维盘根，将预处理纤维盘根移入干燥箱，于温度为45℃的条件下，干燥40min，即得纤维盘根。所述金属纤维为铁纤维。所述硅烷偶联剂为硅烷偶联剂KH-550。所述1号浸渍液的制备方法为将聚四氟乙烯与纳米二氧化钛和氯化锌按质量比5：2混合，并加入聚四氟乙烯质量0.10倍的丙酸钙，聚四氟乙烯质量0.14倍的滑石粉和聚四氟乙烯质量0.2倍的水，搅拌混合，得1号浸渍液。所述2号浸渍液的制备过程为将凡士林和石蜡按质量比4：1混合，并加入凡士林质0.4倍的卵磷脂，搅拌混合，得2号浸渍液。
实例3
将金属纤维与玻璃纤维纺丝液按质量比1：5混合，于温度为850℃，转速为350r/min的条件下，搅拌混合40min后，得混合玻璃纤维纺丝液，将混合玻璃纤维纺丝液纺织成丝，得改性玻璃纤维；将改性玻璃纤维与芳纶纺丝液按质量比1：4混合于反应釜中，并向反应釜中加入芳纶纺丝液质量0.5倍的玻璃纤维，于温度为650℃，转速为300r/min的条件下搅拌混合80min后，得改性芳纶纺丝液，将改性芳纶纺丝液纺织成丝，得改性芳纶纤维；将改性芳纶纤维与浓度为4mol/L的盐酸按质量比1：5混合浸泡70min后，过滤，得滤渣，将滤渣移入干燥箱，于温度为90℃的条件下，恒温干燥30min后，得1次处理改性芳纶纤维；将1次处理改性芳纶纤维与硅烷偶联剂按质量比1：10混合，于温度为75℃的条件下浸泡4h后，过滤，得滤饼，将滤饼与有机硅树脂按质量比1：6混合，于温度为55℃的条件下浸泡150min后，过滤，得2次预处理改性芳纶纤维，将2次预处理改性芳纶纤维于温度为220℃的条件下，干燥45min后，得2次处理改性芳纶纤维；将2次处理改性芳纶纤维与1号浸渍液按质量比1：6混合，并于温度75℃的条件下浸泡4h后，过滤，得预处理盘根纤维，将预处理盘根纤维移入编织机中进行编织，得纤维盘根坯料；将纤维盘根坯料与2号浸渍液按质量比1：6混合，于温度为90℃的条件下浸泡70min后，过滤，得预处理纤维盘根，将预处理纤维盘根移入干燥箱，于温度为45℃的条件下，干燥40min，即得纤维盘根。所述金属纤维为铁纤维。所述硅烷偶联剂为硅烷偶联剂KH-550。所述1号浸渍液的制备方法为将聚四氟乙烯与纳米二氧化钛和氯化锌按质量比5：2混合，并加入聚四氟乙烯质量0.10倍的丙酸钙，聚四氟乙烯质量0.14倍的滑石粉和聚四氟乙烯质量0.2倍的水，搅拌混合，得1号浸渍液。所述2号浸渍液的制备过程为将凡士林和石蜡按质量比4：1混合，并加入凡士林质0.4倍的卵磷脂，搅拌混合，得2号浸渍液。
实例4
将金属纤维与玻璃纤维纺丝液按质量比1：5混合，于温度为850℃，转速为350r/min的条件下，搅拌混合40min后，得混合玻璃纤维纺丝液，将混合玻璃纤维纺丝液纺织成丝，得改性玻璃纤维；将改性玻璃纤维与芳纶纺丝液按质量比1：4混合于反应釜中，并向反应釜中加入芳纶纺丝液质量0.5倍的玻璃纤维，于温度为650℃，转速为300r/min的条件下搅拌混合80min后，得改性芳纶纺丝液，将改性芳纶纺丝液纺织成丝，得改性芳纶纤维；将改性芳纶纤维与浓度为4mol/L的盐酸按质量比1：5混合浸泡70min后，过滤，得滤渣，将滤渣移入干燥箱，于温度为90℃的条件下，恒温干燥30min后，将干燥后的改性芳纶纤维浸没质量分数20%的硫酸铜溶液中，于温度为45℃混合浸泡45min后，过滤，得1次预处理改性芳纶纤维，将1次预处理改性芳纶纤维于温度为85℃的条件下干燥30min后，得1次处理改性芳纶纤维；将1次处理改性芳纶纤维与硅烷偶联剂按质量比1：10混合，于温度为75℃的条件下浸泡4h后，过滤，得滤饼，得2次预处理改性芳纶纤维，将2次预处理改性芳纶纤维于温度为220℃的条件下，干燥45min后，得2次处理改性芳纶纤维；将2次处理改性芳纶纤维与1号浸渍液按质量比1：6混合，并于温度75℃的条件下浸泡4h后，过滤，得预处理盘根纤维，将预处理盘根纤维移入编织机中进行编织，得纤维盘根坯料；将纤维盘根坯料与2号浸渍液按质量比1：6混合，于温度为90℃的条件下浸泡70min后，过滤，得预处理纤维盘根，将预处理纤维盘根移入干燥箱，于温度为45℃的条件下，干燥40min，即得纤维盘根。所述金属纤维为铁纤维。所述硅烷偶联剂为硅烷偶联剂KH-550。所述1号浸渍液的制备方法为将聚四氟乙烯与纳米二氧化钛和氯化锌按质量比5：2混合，并加入聚四氟乙烯质量0.10倍的丙酸钙，聚四氟乙烯质量0.14倍的滑石粉和聚四氟乙烯质量0.2倍的水，搅拌混合，得1号浸渍液。所述2号浸渍液的制备过程为将凡士林和石蜡按质量比4：1混合，并加入凡士林质0.4倍的卵磷脂，搅拌混合，得2号浸渍液。
对比例：廊坊某密封材料有限公司生产的盘根。
将实例1至4所得的纤维盘根及对比例产品进行性能检测，具体检测方法如下：
1.耐热性能：在500℃空气气氛下恒温加热1h；采用德国NETZSCH4型热分析仪分析试件的失重量，并计算失重率，升温速率均为10℃/min；
2.耐磨性能：干摩擦试验，试验用轴承钢球（增大接触压力），试验载荷30N，往复频率4Hz，时间为3600s。
具体检测结果如表1所示：
表1
检测项目 实例1 实例2 实例3 实例4 对比例
失重率/% 1.538 2.474 2.953 2.792 5.642
磨耗量/mg 0.54 1.63 2.03 1.96 5.3
由表1检测结果可知，本发明技术方案制备的纤维盘根具有优异的耐热性能及耐磨性能的特点，在盘根行业的发展中具有广阔的前景。

Claims (6)

1.一种纤维盘根的制备方法，其特征在于具体制备步骤为：
（1）将金属纤维与玻璃纤维纺丝液按质量比1：3～1：5混合，得混合玻璃纤维纺丝液，将混合玻璃纤维纺丝液纺织成丝，得改性玻璃纤维；
（2）将改性玻璃纤维与芳纶纺丝液按质量比1：2～1：4混合，并加入芳纶纺丝液质量0.4～0.5倍的玻璃纤维，搅拌混合后，得改性芳纶纺丝液，将改性芳纶纺丝液纺织成丝，得改性芳纶纤维；
（3）将改性芳纶纤维与盐酸按质量比1：3～1：5混合浸泡，过滤，干燥后移入硫酸铜溶液中，混合浸泡，过滤，干燥，得1次处理改性芳纶纤维；
（4）将1次处理改性芳纶纤维与硅烷偶联剂按质量比1：8～1：10混合浸泡，过滤，得滤饼，将滤饼与有机硅树脂按质量比1：3～1：6混合浸泡，过滤，干燥，得2次处理改性芳纶纤维；
（5）将2次处理改性芳纶纤维与1号浸渍液按质量比1：5～1：6混合浸泡，过滤，得预处理盘根纤维，将预处理芳纶纤维与编织机中进行编织，得纤维盘根坯料；
（6）将纤维盘根坯料与2号浸渍液按质量比1：3～1：6混合浸泡，过滤，干燥，即得纤维盘根。
2.根据权利要求1所述的一种纤维盘根的制备方法，其特征在于：步骤（1）所述金属纤维为铁纤维，铝纤维或镍纤维中任意一种。
3.根据权利要求1所述的一种纤维盘根的制备方法，其特征在于：步骤（2）所述玻璃纤维为中碱玻璃纤维或无碱玻璃纤维中任意一种。
4.根据权利要求1所述的一种纤维盘根的制备方法，其特征在于：步骤（4）所述硅烷偶联剂为硅烷偶联剂KH-550，硅烷偶联剂KH-560或硅烷偶联剂KH-570中任意一种。
5.根据权利要求1所述的一种纤维盘根的制备方法，其特征在于：步骤（5）所述1号浸渍液的制备方法为将聚四氟乙烯与纳米二氧化钛和氯化锌按质量比5：1～5：2混合，并加入聚四氟乙烯质量0.08～0.10倍的丙酸钙，聚四氟乙烯质量0.10～0.14倍的滑石粉和聚四氟乙烯质量0.1～0.2倍的水，搅拌混合，得1号浸渍液。
6.根据权利要求1所述的一种纤维盘根的制备方法，其特征在于：步骤（6）所述2号浸渍液的制备过程为将凡士林和石蜡按质量比3：1～4：1混合，并加入凡士林质量0.2～0.4倍的卵磷脂，搅拌混合，得2号浸渍液。
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