CN104204077A - 用于石油开采的高强度柔性管状结构体 - Google Patents
用于石油开采的高强度柔性管状结构体 Download PDFInfo
- Publication number
- CN104204077A CN104204077A CN201380011985.1A CN201380011985A CN104204077A CN 104204077 A CN104204077 A CN 104204077A CN 201380011985 A CN201380011985 A CN 201380011985A CN 104204077 A CN104204077 A CN 104204077A
- Authority
- CN
- China
- Prior art keywords
- flexible tubular
- tubular structure
- multipolymer
- composition
- mixed thing
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
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Classifications
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- E—FIXED CONSTRUCTIONS
- E21—EARTH OR ROCK DRILLING; MINING
- E21B—EARTH OR ROCK DRILLING; OBTAINING OIL, GAS, WATER, SOLUBLE OR MELTABLE MATERIALS OR A SLURRY OF MINERALS FROM WELLS
- E21B17/00—Drilling rods or pipes; Flexible drill strings; Kellies; Drill collars; Sucker rods; Cables; Casings; Tubings
- E21B17/20—Flexible or articulated drilling pipes, e.g. flexible or articulated rods, pipes or cables
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
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- B29C48/022—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor characterised by the choice of material
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- B32B27/304—Layered products comprising a layer of synthetic resin comprising vinyl (co)polymers; comprising acrylic (co)polymers comprising vinyl halide (co)polymers, e.g. PVC, PVDC, PVF, PVDF
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- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/34—Layered products comprising a layer of synthetic resin comprising polyamides
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/10—Esters; Ether-esters
- C08K5/12—Esters; Ether-esters of cyclic polycarboxylic acids
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L27/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers
- C08L27/02—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L27/12—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
- C08L27/16—Homopolymers or copolymers or vinylidene fluoride
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F16—ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
- F16L—PIPES; JOINTS OR FITTINGS FOR PIPES; SUPPORTS FOR PIPES, CABLES OR PROTECTIVE TUBING; MEANS FOR THERMAL INSULATION IN GENERAL
- F16L11/00—Hoses, i.e. flexible pipes
- F16L11/04—Hoses, i.e. flexible pipes made of rubber or flexible plastics
- F16L11/08—Hoses, i.e. flexible pipes made of rubber or flexible plastics with reinforcements embedded in the wall
- F16L11/081—Hoses, i.e. flexible pipes made of rubber or flexible plastics with reinforcements embedded in the wall comprising one or more layers of a helically wound cord or wire
- F16L11/083—Hoses, i.e. flexible pipes made of rubber or flexible plastics with reinforcements embedded in the wall comprising one or more layers of a helically wound cord or wire three or more layers
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29K—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR MOULDS, REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS
- B29K2027/00—Use of polyvinylhalogenides or derivatives thereof as moulding material
- B29K2027/12—Use of polyvinylhalogenides or derivatives thereof as moulding material containing fluorine
- B29K2027/16—PVDF, i.e. polyvinylidene fluoride
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B29K2105/00—Condition, form or state of moulded material or of the material to be shaped
- B29K2105/0005—Condition, form or state of moulded material or of the material to be shaped containing compounding ingredients
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B29K2705/00—Use of metals, their alloys or their compounds, for preformed parts, e.g. for inserts
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B29L—INDEXING SCHEME ASSOCIATED WITH SUBCLASS B29C, RELATING TO PARTICULAR ARTICLES
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- B32B2264/10—Inorganic particles
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Abstract
本发明涉及用于石油开采的柔性管状结构体，该柔性管状结构体包括至少一个增强层和至少一个含氟聚合物混配物的层，其中该含氟聚合物混配物具有包括聚偏二氟乙烯均聚物和偏二氟乙烯/氟代共聚单体共聚物和增塑剂的组合物。该共聚物中六氟丙烯共聚单体的重量比例高于25％。
Description
本发明涉及包括增强层和含氟聚合物混配物层的用于石油开采的柔性管状结构体。
预期的一个应用领域尤其是用于海上和陆上石油开采的流体输送。
术语“柔性管状结构体”指代用于石油或天然气开采的近海和陆上柔性管、海底管缆和结合了柔性管和海底管缆的功能的结构体。
海上柔性管主要用于输送从近海沉积床提取的石油或天然气。其也可以用于输送打算注入沉积床中以提高烃产量的加压海水。
这些柔性管是由不同层的组合体形成的，各层旨在使该管耐受海底使用或安装应力。这些层尤其包括聚合物护套和由成形金属线、窄条或复合材料线卷绕而成的增强层。
柔性管状管通常从内到外包括：用于运输待输送流体的至少一个内部水密管、在该内部水密管周围的增强层和在该增强层周围的外保护护套。该内部水密管通常由聚合物材料构成，其被称作“内部水密护套”或“压力护套”。
在美国石油协会(American Petroleum Institute)(API)公布的标准文件API17J“未粘着柔性管的标准(Specification for Unbonded Flexible Pipe)”和API RP17B“柔性管的操作规程建议(Recommended Practice for FlexiblePipe)”中描述了这些柔性管。
本发明涉及的陆上柔性管主要用于油井钻探和控制，尤其是美国石油协会(American Petroleum Institute)公布的标准API 16C“节流压井系统(Chokeand Kill Systems)”中描述的节流管线和压井管线。与用于井口密封和控制的设备连接的这些安全管必须能够耐受极端的压力和温度条件，通常为1000巴和130℃。其通常具有与海上柔性管类似的结构。
本发明还涉及美国石油协会(American Petroleum Institute)公布的标准API RP15S“可缠绕的增强塑料线管的标准(Qualification of SpoolableReinforced Plastic Line Pipe)”中描述的陆上柔性管。这些陆上柔性管是本领域技术人员已知的，英语名称为“Reinforced Thermoplastic Pipe(增强热塑性管)”。其用于在压力下(通常高达150巴)输送石油和天然气。其结构与海上柔性管的类似。
海底管缆主要用于向海上设备输送流体、电力和信号，例如阀、井口装置、收集器、泵或分离器，用于供应电力和远程监控和控制该设备的执行器。用于这些应用输送的流体通常是用于液压操作的油。海底管缆也可以用于输送各种流体，该流体旨在注入主管线中以输送烃，以便于所述烃的流动，例如通过注入化学物质用于防止生成水合物的堵塞，或注入甲烷，有利于将石油带到表面(“气体提升”法)，或者用于提供该主管线的维护，例如通过注入腐蚀抑制剂。
海底管缆由一个或多个水密管和非必要的电缆和/或光纤缆的组合体构成，该组合体由该管和缆螺旋或S/Z卷绕制成，其制备方式使得该管缆是柔性的，且该组合体可以被增强层和外部保护性聚合物护套围绕。这些水密管(具有输送前述流体的作用)通常具有比该管缆的外径小得多的直径。管缆的水密管通常由单一无氧化金属管构成或者由包括被一个或多个增强层围绕的不可渗透的聚合物管的增强柔性管构成。
美国石油协会(American Petroleum Institute)公布的标准API17E“海底管缆规格(Specification for Subsea Umbilicals)”中以及标准ISO13628-5中都描述了这种类型的海底管缆。
文献US6 102 077公开了结合了海底柔性管和海底管缆的功能的柔性管状结构体。该结构体在其中心包括大直径的柔性管，用于输送烃，该中心柔性管被多个小直径的外管以螺旋或S/Z组合方式围绕在该中心柔性管周围，该外管用于与管缆中的那些类似的功能，尤其用于液压传动或注射流体。这些柔性管状结构体被本领域技术人员称作“集成海底管缆”和“集成产品束”。这些大直径的结构体通常被外部聚合物护套围绕。
文献EP0608939描述了基于含氟聚合物的聚合物组合物，用于输送含氟聚合物混配物以制备用于石油开采的柔性管状结构体。这些管状结构体包括至少一个增强层和至少一个含氟聚合物混配物的层。该组合物以重量计包括：60-80％PVDF、20-40％的VDF和另一氟代共聚单体(在共聚物中的含量为5-25％)的热塑性共聚物、和5-20％增塑剂(相对于PVDF和共聚物的总量计)。该预期的热塑性共聚物包括VDF/HFP共聚物。在实施例中公开的HFP在该共聚物中声称的含量约为10％。
然而，以这种组合物制备的管状结构体的含氟聚合物混配物并不完全令人满意。特别是在该结构体经受因海流产生的反复运动时，判断这些含氟聚合物混配物的疲劳强度不够。而且，在将这些管状结构体铺设在高深度时，其中温度较低，但通过其的流体处于较高的温度，这些管也不具有足够的使用寿命。
因此，产生的问题也是本发明所要解决的问题是提供用于石油开采的柔性管状结构体，其包括不仅具有改进的机械、热和化学性质而且在该管的使用寿命过程中性质不会改变的含氟聚合物混配物。
为此目的，本发明提出了用于石油开采的柔性管状结构体，该柔性管状结构体包括至少一个增强层和至少一个含氟聚合物混配物的层，该含氟聚合物混配物具有组合物，所述组合物在一方面包括聚偏二氟乙烯均聚物和偏二氟乙烯/氟代共聚单体共聚物和在另一方面包括增塑剂；依照本发明，该氟代共聚单体在该共聚物中的重量比例高于25％。
因此，本发明的特性特征是使用了其中氟代共聚单体重量比例高于25％的共聚物。优选地，该氟代共聚单体选自：六氟丙烯(HFP)、全氟(甲基乙烯基)醚(PMVE)、全氟(乙基乙烯基)醚(PEVE)、全氟(丙基乙烯基)醚(PPVE)、四氟乙烯(TFE)或全氟丁基乙烯(PFBE)、一氯三氟乙烯(CTFE)、氟乙烯丙烯(FEP)或三氟乙烯。
而且，该共聚物也可以是三元聚合物。
依照优选实施方式，该氟代共聚单体是六氟丙烯。
因此，该共聚物具有赋予到含氟聚合物混配物的弹性性质，使得不仅可以提高该混配物的疲劳强度，而且可以提高低温强度。而且，由此得到的柔性管状结构体的使用寿命得以提高。
这是与文献EP0608939的主题的根本差异，在EP0608939的主题中寻求精准的组成以能够形成非弹性含氟聚合物混配物。
依照本发明的特别有利的实施方式，该偏二氟乙烯和氟代共聚单体的共聚物在该组合物中以10-35％的重量比例存在。因此，该共聚物是弹性体，其能够使该含氟聚合物混配物具有甚至更显著的弹性性质，由此使得可以制备具有甚至更进一步提高的使用寿命的柔性管状结构体。
优选地，该偏二氟乙烯和该氟代共聚单体的共聚物在该组合物中以20-35％，例如25％-35％的重量比例存在。
依照本发明的另一实施方式，该增塑剂选自癸二酸二丁酯、邻苯二甲酸二辛酯、N-正丁基磺酰胺、聚酯聚合物及其组合，例如该增塑剂是癸二酸二丁酯。对于该混配物的塑性材料，这组增塑剂展现出比其他更少的渗出。该增塑剂有利地在该组合物中以1-5％，例如2-3.5％的重量比例存在。
而且，依照本发明的特别有利的特征，该氟代共聚单体在该共聚物中的重量比例为：大于或等于26％，和/或小于或等于40％，优选小于或等于37％。这防止了该混配物在该增强层的金属元件中的热蠕变。
而且，该柔性管状结构体的含氟聚合物混配物优选在未老化状态时具有平均大于或等于50000次循环，优选大于或等于100000次循环的疲劳强度，和/或在150℃在空气中老化1个月的状态时具有平均大于或等于5000次循环，优选大于或等于8000次循环的疲劳强度。因此，该含氟聚合物混配物的疲劳强度提高了，该柔性管状结构体更长期地保持其所有性质：化学、热和机械性质。
依照本发明的另一特别有利的特征，该含氟聚合物组合物由该聚偏二氟乙烯均聚物、偏二氟乙烯和氟代共聚单体的共聚物和该增塑剂构成。因此，该聚合物组合物仅包括这些使其具有所需性质的要素。
而且，依照本发明的第一实施方式，该含氟聚合物混配物的层形成压力护套，而该增强层包括螺旋卷绕在该压力护套周围的型材。依照本发明的第二实施方式，该含氟聚合物混配物的层是由该含氟聚合物混配物的条带螺旋卷绕形成的。而且，依照该第二种变型的第一实施方式，该柔性管状结构体有利地包括两个增强层，而该含氟聚合物混配物的条带螺旋卷绕在这两个增强层之间。依照第二实施方式，其包括压力护套和位于该压力护套内部的金属骨架，而该含氟聚合物混配物的条带螺旋卷绕在该骨架和该压力护套之间。
依照本发明的变型，本发明的柔性管状结构体包括几个相邻的聚合物层，其至少一个是由具有组合物的含氟聚合物混配物的层形成的，所述组合物一方面包括聚偏二氟乙烯均聚物和偏二氟乙烯与六氟丙烯的共聚物且另一方面包括增塑剂，该六氟丙烯单体在该共聚物中的重量比例高于25％。
依照另一方面，本发明涉及用于石油开采的柔性管状结构体的制造方法，依照该类型的方法，提供组合物，所述组合物一方面包括聚偏二氟乙烯均聚物和偏二氟乙烯与氟代共聚单体的共聚物且另一方面包括增塑剂，和形成增强层和含氟聚合物混配物的层，以将该层相结合；依照本发明，提供组合物，其中该氟代共聚单体在该共聚物中的重量比例高于25％。优选地，该氟代共聚单体是六氟丙烯。
一旦参照单一附图阅读下面提供用于示例而非限制的本发明的特别实施方式的描述，本发明的其他特别的特征和优点将变得显而易见，在附图中：
-该单幅图是依照本发明的柔性结构的部分透视示意图。
该单幅图示例了一种依照本发明的柔性管状结构体。该结构是明确用于在海洋环境中运输烃的管道的结构。其从外到内包括：外防护护套10(称作外护套)、卷绕在外抗张铠甲层14周围的保持层12、以与外层14相反的方向卷绕的内抗张铠甲层16、用于取走(take)输送流体压力产生的径向应力的压力铠甲层20、用于取走径向压碎应力的内部水密聚合物护套18和内部骨架17。由于内部骨架17的存在，该管称作“粗镗(rough bore)”。
内部水密聚合物护套18或压力护套旨在用于以水密方式输送内部的烃。因此该压力护套18被压力铠甲层20围绕，该压力铠甲层20是由常用(stapled)金属形状的线短节距卷绕而成的，用于取走压力护套18的内部压力应力。该抗张铠甲层14、16以长节距卷绕，其用于取走该管经受的纵向抗张应力。
依照本发明，该柔性管状结构体包括至少一个增强层和含氟聚合物混配物的层，该混配物具有一方面包括聚偏二氟乙烯均聚物(PVDF)和偏二氟乙烯(VDF)与六氟丙烯(HFP)的共聚物且另一方面包括增塑剂的组合物，六氟丙烯单体在共聚物中的重量比例高于25％。
该柔性管状结构体的压力护套可以与其他聚合物层相邻，该其他聚合物层可以由非必要地具有填料的聚合物(例如聚酰胺(PA)、聚乙烯(PE)或聚偏二氟乙烯(PVDF))制成。
依照变型，该含氟聚合物混配物的层形成该中间保护护套。因此，本发明的柔性管状结构体的含氟聚合物混配物的层不是内部水密护套而是该结构体的另一护套，例如中间护套或牺牲护套。牺牲护套是位于水密护套之下的护套，且其在制造过程中和/或该柔性管状结构体的使用操作过程中保护该水密护套的完整性。
依照本发明的优选实施方式，柔性管状结构体的压力护套18是含氟聚合物混配物的层，该混配物具有一方面包括聚偏二氟乙烯均聚物(PVDF)和偏二氟乙烯(VDF)与六氟丙烯(HFP)的共聚物且另一方面包括增塑剂的组合物，六氟丙烯单体在共聚物中的重量比例高于25％。
依照标准ISO1133(230℃,12.5kg)，本发明的内容中使用的PVDF聚合物优选具有小于或等于15g/10min，有利地小于或等于10g/10min的热熔融流动指数，以确保良好的机械强度性质。
本发明的内容中使用的VDF/HFP共聚物优选是弹性体，其在专用技术公布(Special Technical Publication)No.184中由ASTM定义为在室温时能够拉伸到其初始长度的两倍且一旦释放能快速再次返回其最初长度±10％内的材料。
VDF/HFP共聚物是由VDF单体和HFP单体共聚得到的。发现该VDF/HFP共聚物在低HFP含量时是热塑性的，在高HFP含量时是弹性体的。在本发明的内容中，HFP单体的重量含量或比例高于25％。
依照某些实施方式中，HFP单体的重量比例大于或等于26％或27％或28％或29％或30％或31％或32％或33％或34％或35％或36％或37％或38％或39％。
依照某些实施方式，HFP单体的重量比例小于或等于40％或39％或38％或37％或36％或35％或34％或33％或32％或31％或30％或29％或28％或27％或26％。
HFP在共聚物中的重量比例优选是由核磁共振法测定的。我们尤其可以使用以下19F NMR方法。
将共聚物样品溶解在直径为5mm的NMR管中。将包含大于10wt％HFP的共聚物的样品在55℃溶解在丙酮-d6中。将一定量的共聚物(约10mg)放入管中，添加溶剂以充满该管的5.5cm(约0.75ml溶剂)。使用加热块将样品加热到所需的温度。将样品加热至少一个小时直至该固体溶解，凝胶消失。将该管倒置以核实不存在凝胶。
在溶剂丙酮-d6的情况中在55℃操作的Bruker DMX或Varian Mercury300型光谱仪上获得光谱，并依照“Composition and sequence distribution ofvinylidene fluoride copolymer and terpolymer fluoroelastomers.Determinationby19F NMR spectroscopy and correlation with some properties”.M.Pianca等,Polymer,1987,Vol.28,224-230中描述的方法进行分析。通过测定CF3和CF的积分并将其进行比较以核实其事实上是否为3:1的比例而验证测量的精确性。
优选地，用于制备旨在形成该柔性管状结构体的含氟聚合物混配物的组合物的共聚物基本上不含均聚物。
该共聚物可以通过上面引用的M.Pianca等的文章中描述的方法制备。
本发明意义上的增塑剂是Wiley & Sons(1989)出版的著作Encyclopediaof Polymer Science and Engineering第568-569页和第588-593页中定义的化合物。其可以是单体的或聚合的。我们尤其可以提及癸二酸二丁酯、邻苯二甲酸二辛酯、N-正丁基磺酰胺、聚酯聚合物及其组合物。适合的聚酯聚合物尤其是由己二酸、壬二酸或癸二酸和二醇得到的那些，以及它们的组合，分子量优选大于或等于1500，更优选大于或等于1800，优选小于或等于5000，更特别地小于或等于2500。分子量过高的增塑剂将会得到抗冲强度过低的组合物。
癸二酸二丁酯是特别有利的增塑剂。
增塑剂的存在有利于制备该组合物或其处理，用于制备该柔性管状结构体的含氟聚合物混配物的层。其还提高了该含氟聚合物混配物的抗冲强度。
除PVDF、共聚物和增塑剂之外，该含氟聚合物混配物的组成可以包括各种添加剂和/或填料和/或导电颗粒和/或无机或有机颜料或染料。
在可能的填料中，我们可以非穷尽地提及云母、氧化铝、滑石、炭黑、玻璃纤维、大分子化合物和碳酸钙，以及选自由Fe2O3、PbO、ZnO、NiO、CoO、CdO、CuO、SnO2、MoO3、Fe3O4、Ag2O、CrO2、CrO3、Cr2O3、TiO、TiO2和Ti2O3构成的组的金属氧化物填料、选自CaO、Ca(OH)2和MgO的碱金属和碱土金属氧化物。
在其他可能的添加剂中，我们可以非穷尽地提及紫外稳定剂(优选非型试剂)、防火产品、热稳定剂和制备助剂(优选除聚烯烃和尤其基于乙烯的聚合物之外)。
在其存在时，除PVDF、共聚物和增塑剂之外的上述化合物以至多20％，优选至多15％，或至多10％，或至多7％，或至多5％，或至多3％，或至多2％，或至多1％的量存在(以相对于总组合物的重量比例计)。
依照本发明的柔性管状结构体的另一实施方式，获得该含氟聚合物混配物的组合物基本上由PVDF、共聚物或增塑剂构成，或甚至仅由PVDF、共聚物和增塑剂构成。
该组合物中共聚物的重量含量为10-35％，尤其20-35％，优选25-35％。
依照某些实施方式，共聚物在该组合物中的重量含量大于或等于11％或12％或13％或14％或15％或16％或17％或18％或19％或20％或21％或22％或23％或24％或25％或26％或27％或28％或29％或30％或31％或32％或33％或34％。
依照某些实施方式，共聚物在该组合物中的重量含量小于或等于34％或33％或32％或31％或30％或29％或28％或27％或26％或25％或24％或23％或22％或21％或20％或19％或18％或17％或16％或15％或14％或13％或12％或11％。
增塑剂在该柔性管状结构体的含氟聚合物混配物的层的最终组合物中的重量含量优选为1-5％，特别地为2-3.5％。过量的增塑剂通过增塑剂的渗出导致该组合物不期望的体积变化。
由文献WO2010/026356中描述的疲劳试验测定依照前述组合物得到的柔性管状结构体的含氟聚合物混配物。其由以下构成：测定聚合物组合物的给定样本的断裂循环数(指定NCR)，即在该样本发生断裂后的循环数。NCR值越高，疲劳试验的结果越好。
为了进行疲劳试验，从挤出管的厚度上切下轴对称的试验样本，切口弯曲半径为4mm，最小半径为2mm。这些试验样本被认为代表了该管的局部几何形状。使用伺服液压控制的测力计(例如MTS810型)进行切割。夹具间距为10mm。用具有1Hz频率的正弦信号使试验样本经过1.4mm的最大伸长量，最小伸长量与最大伸长量之比为0.21，这相当于最小伸长量为0.3mm。试验结果(NCR)是在10个试验样本上得到的结果的平均值。
为进行热蠕变试验，依照标准ISO527(1A型试验样本，试验速度为50mm/min)对该聚合物组合物的未经老化的样本进行抗张试验，在试验之前将这些试验样本在130℃的试验温度调节20分钟。这些试验样本的阈应力(threshold stress)相当于试验样本在应力中承受的最大公称应力。该应力越高，该聚合物组合物的蠕变强度越好。
实施例
由以下化合物制备组合物：
–400：PVDF双峰均聚物，Arkema销售。
–氟代共聚物A：VDF-HFP共聚物(35wt％HFP)，在230℃和100s–1具有3200Pa.s的熔融粘度；
–氟代共聚物B：VDF-HFP共聚物(25wt％HFP)，在230℃和100s–1具有1800Pa.s的熔融粘度；
–2750：VDF-HFP共聚物(15wt％HFP)，在230℃和100s–1具有2250Pa.s的熔融粘度，由Arkema销售。
–DBS：癸二酸二丁酯(增塑剂)。
试验了五种组合物，配方1和四种用于对比的配方2-5。测定了依照这些组合物得到的混配物的性质，尤其是疲劳强度(依照上述NCR试验，对经老化和未经老化的样品都测定)和蠕变强度(依照上述试验)。结果呈现在下面提供的表中。““ND”表示未进行相应测量。
能够看到配方1提供了异常好的疲劳强度结果。蠕变强度也是优良的。其他试验(测定延展性-易碎性转变温度)也证实该含氟聚合物混配物具有优良的性能。
实施例1和2的对比显示共聚物A的选择可以在新的和经老化的状态得到更好的结果。
在150℃老化30天，PVDF基质或该氟代共聚物没有物化改变：老化对该组分的分子量或该基质的结晶性没有影响，无论我们考虑的是结晶程度还是晶体形态。由老化造成的构成实施例1和2的材料的唯一变化是在150℃在空气中保持30天之后损失了增塑剂。因此，在实施例1和2中在新的和经老化的状态的结果比较显示增塑剂的存在对疲劳强度性质的有益作用(新状态和老化状态的对比)。
在比较实施例5和2时，能够看到在老化状态时没有增塑剂的配方5具有比配方2更低的强度。在两种情况中(经老化的实施例2和新状态的实施例5)，该材料不(或不再)具有增塑剂。而且，其配方在所用共聚物的比例和性质方面是相同的。然而，新状态的实施例5中的性质明显低于老化状态的实施例2中的性质：这种差别由以下事实解释的：在实施例5的情况中，观察到存在挤出缺陷和微裂缝，而在配方2的情况中其并不存在(其在初始状态中包含增塑剂)，而这些微裂缝的存在大大影响了该材料的疲劳强度。事实上，本领域技术人员了解材料(无论是何种材料)的疲劳强度非常依赖于该材料中存在缺陷的程度。应当注意到在任何其他包含增塑剂的配方中都没有观察到这种类型的缺陷或微裂缝：因此，这清楚地证实了增塑剂对疲劳强度的另一实质的有利作用，即可以挤出具有良好性质且没有缺陷的厚部件(厚度至少3mm)。
实施例1和3的比较显示了使用足够高含量的A型共聚物的优点，因为配方3中的含量明显不足。
最后，实施例1和2与实施例4的比较显示了使用包括足够高含量的共聚单体以提供疲劳性质的显著改进的氟代共聚物的优点。因此，在配方4中，尽管共聚单体的含量与实施例1和2中接近，且该配方包含增塑剂，其仍具有较低的疲劳强度。
表
依照配方1的组合物是形成用于石油开采的柔性管状结构体的含氟聚合物混配物层的最佳候选者。
本发明还涉及依照本发明的柔性管状结构体的制备方法。为此目的，依照第一实施方式，使用具有一个进料螺杆的挤出机，其在一端具有进料料斗，另一端具有注射喷嘴，该注射喷嘴与十字头相连，管线能够通过该十字头。作为单幅图中示例的柔性管状管的举例，前述管线相当于该骨架。将其从十字头的上游供给到下游。由配方1得到的组合物处于颗粒的形式状态，将其放入进料料斗中。然后将其加热并在进料螺杆内软化，使其聚集并形成该软化组合物的单一相，将其向十字头进料，其设计为在该骨架之上及周围形成该软化组合物的圆筒层。
然后在该十字头进一步的下游，将涂覆有该软化组合物的圆筒层的骨架在空气中或经过水浴进行冷却。由此得到由具有依照配方1的组合物的结构特征的含氟聚合物混配物制成的压力护套。然后，通过公知的制备步骤，首先将压力铠甲层卷绕，由成型的线或窄条以短节距螺线形式的线圈形成，然后卷绕长节距抗张铠甲层。
由此，制备了用于输送烃的海上或陆上柔性管，其能够在操作中耐受高温高压，通常高达1000巴和130℃。
PVDF均聚物(有时仅用于压力护套)具有良好的高温行为，但在低温时具有低延展性的缺点。现在，在该管的制造和安装过程中，该压力护套必须在低温时(冬季霜冻、安装在寒冷区域中等)可以弯曲而不会受到损害。这就是单独的PVDF均聚物并不是最适合制备柔性管的压力护套的原因。
所述柔性管状管主要是“未粘合”类型的柔性管。然而，依照本发明的柔性管状结构体还包括“粘合”类型的管。
依照另一实施方式，通过由依照配方1的组合物挤出形成纵向窄条。在用于各种功能(尤其是在其插入增强层、抗张层或压力层之间时对磨损和摩擦的防护)的柔性管中使用这些含氟聚合物混配物的窄条。其还用于热绝缘或用于保护对温度和侵蚀性化学物质敏感的组合体，例如将其以接合线匝卷绕时，特别是在骨架和压力护套之间如此。
依照配方1的组合物有利地用于在标准ISO13628-5中定义的海底管缆中。这些管缆包括至少一个增强层和至少一个含氟聚合物混配物的层，且通常包括管束，且尤其包括：压力护套、压力管、柔性管中的外护套或窄条、电缆或光纤缆中的护套或窄条、内部或外部加衬的金属管、用于填充在管缆的组合体之间的杆、或“填料”、围绕在管和缆的组合体全部或一部分的周围的中间或外部护套或窄条。
依照另一方面，本发明涉及用于石油开采的管状结构体，该管状结构体包括至少一个衬里和至少一个含氟聚合物混配物的层，该含氟聚合物混配物具有一方面包括聚偏二氟乙烯均聚物和偏二氟乙烯与氟代共聚单体的共聚物且另一方面包括增塑剂的组合物。氟代共聚单体在该共聚物中的总量比例高于25％。
因此，本发明涉及海上使用的所谓“刚性”的管状管。其是申请人的专利申请WO03/062691中描述的那些类型的。其包括金属管，在该金属内部有聚合物层，其尤其具有保护该金属管不被腐蚀的功能。这些管状管意图通过本领域技术人员公知的安装方法(例如J铺设、S铺设或称作“卷绕铺设(reeledlay)”的铺设技术)安装在海中。这最后述及的技术由以下构成：将陆上制备的“刚性”管状管卷绕在管线铺设船的机动轮上，在将其输送到安装地点之前使其塑性变形，其中然后将其退绕并伸直，安装在油田处。
缩略语
在说明书和下文给出的权利要求书中使用以下缩略语：
VDF：偏二氟乙烯
PVDF：聚偏二氟乙烯
HFP：六氟丙烯
PMVE：全氟(甲基乙烯基)醚
PEVE：全氟(乙基乙烯基)醚
PPVE：全氟(丙基乙烯基)醚
PFBE：全氟丁基乙烯
TFE：四氟乙烯
CTFE：一氯三氟乙烯
FEP：氟乙烯丙烯
NCR：在疲劳试验中测定的平均破裂循环数
Claims (16)
1.用于石油开采的柔性管状结构体，该柔性管状结构体包括至少一个增强层和至少一个含氟聚合物混配物的层，其中该含氟聚合物混配物具有组合物，所述组合物在一方面包括聚偏二氟乙烯均聚物和偏二氟乙烯/氟代共聚单体共聚物和在另一方面包括增塑剂；
其特征在于该共聚物中氟代共聚单体的重量比例高于25％。
2.权利要求1的柔性管状结构体，其特征在于该氟代共聚单体是六氟丙烯。
3.权利要求1或2的柔性管状结构体，其特征在于该偏二氟乙烯和氟代共聚单体的共聚物在该组合物中以10-35％的重量比例存在。
4.权利要求3的柔性管状结构体，其特征在于该偏二氟乙烯和氟代共聚单体的共聚物在该组合物中以20-35％，优选25-35％的重量比例存在。
5.权利要求1-4中任一项的柔性管状结构体，其特征在于该增塑剂选自癸二酸二丁酯、邻苯二甲酸二辛酯、N-正丁基磺酰胺、聚酯聚合物及其组合物，且优选为癸二酸二丁酯。
6.权利要求1-5中任一项的柔性管状结构体，其特征在于该增塑剂在该组合物中以1-5％，优选2-3.5％的重量比例存在。
7.权利要求1-6中任一项的柔性管状结构体，其特征在于该氟代共聚单体在该共聚物中的重量比例大于或等于26％和/或小于或等于40％，优选小于或等于37％。
8.权利要求1-7中任一项的柔性管状结构体，其特征在于该共聚物是弹性体。
9.权利要求1-8中任一项的柔性管状结构体，其特征在于该含氟聚合物混配物在未老化状态时平均具有大于或等于50000次循环，优选大于或等于100000次循环的疲劳强度，和/或在150℃在空气中老化1个月的状态时平均具有大于或等于5000次循环，优选大于或等于8000次循环的疲劳强度。
10.权利要求1-9中任一项的柔性管状结构体，其特征在于该含氟聚合物组合物由该聚偏二氟乙烯均聚物、该偏二氟乙烯和氟代共聚单体的共聚物和该增塑剂组成。
11.权利要求1-10中任一项的柔性管状结构体，其特征在于该含氟聚合物混配物的层形成压力护套，而该增强层包括螺旋卷绕在该压力护套周围的型材。
12.权利要求1-10中任一项的柔性管状结构体，其特征在于该含氟聚合物混配物的层形成中间防护护套。
13.权利要求1-10中任一项的柔性管状结构体，其特征在于该含氟聚合物混配物的层是由该含氟聚合物混配物的条带螺旋卷绕形成的。
14.权利要求13的柔性管状结构体，其特征在于其包括两个增强层，而该含氟聚合物混配物的条带螺旋卷绕在这两个增强层之间。
15.权利要求13的柔性管状结构体，其特征在于其包括压力护套和位于该压力护套内部的金属骨架，其中该含氟聚合物混配物的条带螺旋卷绕在该骨架和该压力护套之间。
16.用于石油开采的柔性管状结构体的制造方法，依照该类型的方法，提供组合物，所述组合物一方面包括聚偏二氟乙烯均聚物和偏二氟乙烯与氟代共聚单体的共聚物且另一方面包括增塑剂，和形成增强层和含氟聚合物混配物的层，以将该层相结合；
其特征在于提供组合物，其中该氟代共聚单体在该共聚物中的重量比例高于25％。
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| EP (1) | EP2820083B1 (zh) |
| CN (1) | CN104204077B (zh) |
| AU (1) | AU2013224775B2 (zh) |
| BR (1) | BR112014021252B1 (zh) |
| DK (1) | DK2820083T3 (zh) |
| FR (1) | FR2987667B1 (zh) |
| MY (1) | MY169264A (zh) |
| WO (1) | WO2013128110A1 (zh) |
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- 2013-02-26 BR BR112014021252-0A patent/BR112014021252B1/pt active IP Right Grant
- 2013-02-26 DK DK13712851.8T patent/DK2820083T3/en active
- 2013-02-26 EP EP13712851.8A patent/EP2820083B1/fr active Active
- 2013-02-26 US US14/381,256 patent/US11199057B2/en active Active
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107906270A (zh) * | 2017-10-24 | 2018-04-13 | 佛山科学技术学院 | 一种云母粉、石墨烯复合柔性管 |
| CN107906270B (zh) * | 2017-10-24 | 2020-08-11 | 佛山科学技术学院 | 一种云母粉、石墨烯复合柔性管 |
| CN111886436A (zh) * | 2017-12-22 | 2020-11-03 | 泰克尼普N电力公司 | 用于形成管道的管状加强件的机器和相关方法 |
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Also Published As
| Publication number | Publication date |
|---|---|
| US20150041118A1 (en) | 2015-02-12 |
| FR2987667B1 (fr) | 2014-03-07 |
| EP2820083B1 (fr) | 2018-10-24 |
| FR2987667A1 (fr) | 2013-09-06 |
| WO2013128110A1 (fr) | 2013-09-06 |
| EP2820083A1 (fr) | 2015-01-07 |
| CN104204077B (zh) | 2017-06-23 |
| US11199057B2 (en) | 2021-12-14 |
| AU2013224775B2 (en) | 2016-09-22 |
| AU2013224775A1 (en) | 2014-09-18 |
| BR112014021252B1 (pt) | 2020-12-22 |
| MY169264A (en) | 2019-03-20 |
| DK2820083T3 (en) | 2019-02-18 |
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