CN101128312B - 颗粒材料的石墨涂层 - Google Patents
颗粒材料的石墨涂层 Download PDFInfo
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Abstract
提供具有石墨浸渍的树脂涂层的涂层的颗粒。油田颗粒可包括井壁砾石充填沙、粒状膨润土、粉碎的黑沥青、碳酸钙、玻璃珠、矿毛绝缘纤维、碎纸、金属球、陶瓷珠、坚果壳、粉碎的橡胶、塑料珠、白云母、焙烧的石油焦和珍珠岩中的任何一种。该树脂可包括一种或更多种天然、合成的水溶性和有机树脂作为粘合剂。更具体地,该树脂可包括有机成膜树脂,例如醇酸树脂、聚氨酯和环氧树脂。或者,树脂可包括成膜的水溶性聚合物,例如淀粉、羧甲基纤维素、羟乙基纤维素和黄原胶。在进一步的替代方案中,树脂可包括树脂分散的乳液,例如胶乳或丙烯酸树脂。
Description
发明背景
本发明涉及具有石墨浸渍的涂层的颗粒,和更特别地涉及典型地加入到钻井、完井(completion)或强化采油液体等中的具有石墨浸渍的涂层的颗粒。
油井钻探、完井、强化采油(stimulation)、漏失循环液(“LC”或“LCM”)、渗流和扭矩以及阻力减小添加剂技术中,存在许多使用中的产品。当在大于~10lb/bbl的浓度下泵送到井下时,可通过降低摩擦作用,在功能上改进所有这些。
表1中列出了这些材料的实例。
表1
井壁砾石充填 沙 粒状膨润土 粉碎的黑沥青
碳酸钙 玻璃珠 矿毛绝缘纤维
碎纸 金属球 陶瓷珠
坚果壳 粉碎的橡胶 塑料珠
白云母 焙烧的石油焦 珍珠岩
因此,本发明的目的是提供具有抗摩擦涂层的各种油田颗粒。
发明概述
通过提供具有石墨浸渍的涂层的油田颗粒,将实现本发明的这一和其它目的,其中所述目的在参考下述详细说明的基础上将变得很清楚。油田颗粒可包括,但不限于表1中所述的任何颗粒。对于本发明的目的来说,术语“颗粒”包括纤维和纤维材料。
涂层可包括一种或更多种天然、合成、水溶性和有机树脂的粘合剂。更具体地,该树脂可包括有机成膜树脂,例如醇酸树脂、聚氨酯和环氧树脂。或者,粘合剂可包括成膜的水溶性聚合物,例如淀粉、羧甲基纤维素、羟乙基纤维素和黄原胶。在进一步的替代方案中,粘合剂可包括树脂分散的乳液,例如胶乳或丙烯酸类树脂。在再进一步的替代方案中,粘合剂可包括石蜡或烷属烃。
在本发明另一方面中,石墨可以是天然薄片、天然的无定形或合成石墨,其中石墨颗粒的尺寸范围为0.001微米-850微米。涂层的颗粒的尺寸范围可以是5微米-30,000微米。
发明详述
在任何表1材料上的石墨浸渍的涂层提供通常归于石墨的所有优点,亦即,低摩擦、非反应性、不污染和导电性。可利用各类石墨,例如天然薄片、天然无定形和合成石墨。然而,必需使用特定的方法形成耐用涂层。在形成涂层中最常见的问题是难以将石墨粘合到表面上,这部分是由于石墨不具有电荷,且在扁平状晶体之间存在弱的化学键这一事实导致的。相反,大多数矿物总体带负电荷,且一些矿物在同一颗粒内兼有负电荷和正电荷。因此,重要的是,涂层包括包封石墨并粘合到基底上的粘合剂,优选树脂或聚合物。因此,本发明方法的重要部分是在粘合剂内分散石墨,以便当(例如通过温度、催化剂或蒸发水和/或有机溶剂)固化时,石墨/粘合剂的混合物将在应用所要求的程度和时间下粘合到基底上。正如所示的,粘合剂可以是水溶性聚合物,水性乳液或溶剂基烃。粘合剂可包括有机成膜树脂,例如醇酸树脂、聚氨酯和环氧树脂;成膜水溶性聚合物,例如淀粉、羧甲基纤维素(CMC)、羟乙基纤维素(HEC)和黄原胶(XC聚合物);树脂分散的乳液,例如胶乳和丙烯酸类树脂;或蜡和烷属烃。
喷洒或共混基底与刚刚充足的粘合剂和石墨对于涂布小的颗粒来说作用良好。优选的方法是合适尺寸的混合器或共混器,其中空气或热量可加速制造质量均匀涂层的时间。与用一层厚的涂层通常获得的相比,两层或三层薄的涂层得到较好质量的涂层。
在颗粒,和在特别参考此处的实施例3的情况下,工序牵涉添加已知量的Slip Plate No.3(石墨和树脂的预混配方,获自Superior Graphite Co.of Chicago,Illinois)到已知重量的坚果壳(或其它基底)中,混合直到触摸起来干燥,然后添加更多的配制的石墨和粘合剂。反复这一路线,直到施加所需量的涂层。根据相对于起始的重量增加来计算石墨/粘合剂的用量。
相反的工序,亦即添加坚果壳(或任何其它物质)到已知量的粘合剂中也作用良好。当树脂渗流到基底内并开始聚合时,添加石墨。然而,这一方法增加另一步骤,因为必需除去没有固定到基底上的过量石墨。
可用各种粘合剂涂布表1所述的基底,且涂层的颗粒的尺寸范围可以是约+20微米到-6.3毫米。涂层的厚度可从约3mil(0.076mm)变化到待涂层的颗粒直径的三倍。相对于基底,石墨的重量百分数(wt%)可从小于1wt%变化到97wt%,和更优选约5wt%-95wt%。
可用含有30wt%石墨的环氧树脂涂布陶瓷珠。或者,可用分散在去离子水内的高支链淀粉和NaCMC的水溶性混合物涂布陶瓷珠,其中与更加常见的直链淀粉相比,支链糖苷提供对陶瓷珠更强的粘合性。淀粉之后紧跟着添加小量的Na-CMC和戊二醛作为杀虫剂以供稳定储存。
CMC是阴离子的。水合胶体将吸收在任何电正性的位点上,而与其组成无关。这将增加所需粘合剂的“韧度”,从而在除去游离水(例如,加热到135℉)之后,石墨保持在珠粒的表面上。
可用小于1-约50wt%的石墨处理材料。处理剂可以是部分涂层或者它可以是最多约15mil(38.1mm)厚的石墨膜。在一些应用中,已发现有用的是在树脂或聚合物粘合剂内分散石墨以供极其长期地用于水或油中,或者可配制它用于临时应用,其中含有石墨的粘合剂溶解在它将输送到井下的流体内,从而从高性能的粒状固体中释放石墨。在此情况下,石墨可以多达97wt%。然而,使用石墨处理过的颗粒不是引入石墨的唯一方法,而是为了改进它将与之缔合的基础材料的性能。
套管钻进(drill-in)和完井流体添加剂
目前的完井流体技术常常利用筛分的碳酸钙颗粒降低在付费区域内的流体损失,当使用高纯度、高密度盐水,例如溴化锌/钙或甲酸铈/钾完井时。
使用碳酸钙颗粒的一个问题是,当用盐水将颗粒泵送到钻井内时,由于彼此碰撞的颗粒质量导致泵送摩擦增加。石油公司意识到这一问题需要改进。在任何情况下,在采用石墨涂层的颗粒情况下,尤其在数千英尺长的水平钻探的油井内,将实现泵送效率的显著增加。
涂布碳酸钙将降低摩擦系数从约0.3到0.08,和在未涂层的颗粒上,碳酸钙颗粒的石墨涂层对流变学不具有可测量的影响。碳酸钙100%可溶于15%氢氟酸与盐酸的混合酸内。筛分碳酸钙的尺寸,在生产区域内堵住孔隙的入口,并可在大于或等于10-25lb/bbl的浓度下使用。当允许油井流动时,石墨涂层的材料将通过进入生产钻具组内的所产生的油强制流出孔隙。然而,具有石墨的临时薄涂层的碳酸钙一旦合适地位于生产岩层内,则仍可用酸溶解。由于石墨的表面亲油,因此石墨涂层的碳酸钙可比未涂层的矿物更加容易流出孔隙。
在一些套管钻进和完井中,亲水聚合物,例如XC-聚合物(或黄原胶)、淀粉或羟乙基纤维素(统称为WSP(水溶性聚合物))可与碳酸钙一起使用,得到小于1ml/30min的非常低API的流体损失。
可通过改变粘合剂的类型和组成来控制石墨涂层的寿命。对于小于或等于约1小时的短期寿命来说,可使用由淀粉和羟乙基纤维素制造的水溶性粘合剂。对于数小时的涂层寿命来说,用可渗流的膜制造的粘合剂,例如丙烯酸乳液可最好地起作用。对于耐水性高的长期涂层来说,可优选石墨填充的环氧基涂层。在每一情况下,由于一下两个原因,涂层的石墨含量导致岩层损坏的几率最小:1)石墨具有极其微细的粒度(<10微米),和2)每一颗粒的石墨重量百分数可下降到微量污染物的水平。
实施例1
将Slip Plate No.3喷洒在各种颗粒上,同时在塑料碗内涡动内容物并辊压,以产生实验室规模的样品。也可以采用团状物混合器,将涂料施加到陶瓷、玻璃或塑料球和各种尺寸的碳酸钙颗粒上,其用量范围为痕量的石墨到约15mil(38.1mil)的涂层。基于平均粒度d50,根据重量增加和涂层厚度来计算涂层厚度。例如,平均粒度为710微米的陶瓷球的表面积为0.0158cm2。一个颗粒的重量为0.000497g(认为陶瓷proppant的比重为2.65)。因此,根据涂布之前和之后样品的重量,人们可大致估计涂层的厚度。在涂布工艺过程中,不存在形成永久聚集体的证据。明显地喷涂和辊压辊筒直到溶剂释放将会防止形成聚集体,即颗粒之间的粘合强度弱,于是聚集体破碎成吸引人的单独的涂布颗粒。
实施例2
用含有33wt%石墨的水性丙烯酸粘合剂涂布250g碳酸钙(~50微米)。在于10000rpm下搅拌20分钟之后,石墨涂层的碳酸钙~90%溶解在15HCl内。使用聚氨酯、乙烯乙酸乙烯酯和聚乙酸乙烯酯作为粘合剂,采用手动混合制备涂层的碳酸钙和陶瓷珠的额外样品。相对于涂层的颗粒,粘合剂优选5-10wt%,和相对于涂层的颗粒,石墨为5-15wt%,和优选7.3-12.5wt%。
用于漏失循环液控制和扭矩与阻力减小的石墨涂层的基底
在油田中强烈地认为,人们在运转管道、粘结或调节泥浆的同时,一定不具有漏失循环液。多年来使用筛分的坚果壳,以降低或防止漏失循环液。它们典型地由核桃壳制制成,但黑色胡桃壳因其强度较高,因此是优选的。过去30年来坚果壳成为优选的LC对照材料,这是因为坚果壳成本低,且作为渗流损失和漏失循环液材料也非常好。
用于漏失循环液的在油田中使用的坚果壳以三种粒度范围获得:
表2
回弹率% -30目 -60目
粗糙度,% 全部 16 52 18
中等 全部 12 28 10
微细 全部 11 85 28
对于表2的目的来说,通过用16g干燥材料(在这一情况下,为坚果壳)填充压缩的试验模具,在液压机内压缩该材料,直到表针读数为0,和测量并记录模具的高度,从而测定回弹率。压缩该材料到10,000psi,并再次测量高度。释放压力,并从压机中取出模具且使之膨胀,直到观察到不再膨胀。测量模具的高度。最终的高度减去在10,000psi下的高度除以在10,000psi下的高度乘以100即为回弹率%。
实施例3
用Slip Plate #3和用2ES-NT(一种环氧树脂粘合剂)涂布微细的坚果壳样品。这两种粘合剂含有约30wt%的石墨。石墨涂层的坚果壳容易在淡水、盐水、柴油和醇中润湿。基于在10×放大下肉眼观察颗粒表面,用2ES-NT涂层的坚果壳在水中搅拌24小时之后保持完整。在范围为5-23wt%的石墨涂层浓度下,在10,000psi下,石墨涂层的坚果壳(微细)的回弹率试验表明回弹率的轻微改进(2-4个点)。回弹材料是从压缩状态往回膨胀的材料。与回弹性固体相比,在高压下压缩坚果壳表明(通过弯曲和压平)它们的行为更象弹性固体。该工艺看起来是涂布所有三种尺寸的坚果壳的良好工艺。
石墨涂层的玻璃、塑料和陶瓷珠
理论表明,LCM的共混物是改进损耗回收(lost return)问题的最好方式,这是因为以下两个机理:(1)在损耗区域内形成强的格子状结构和(2)材料本身的机械和物理性能。
水性钻井流体的钻杆柱扭矩典型地具有0.22-0.27的摩擦因子系数。这些数值在水平孔隙内变得更加重要。另外,不合固体的套管钻进和完井流体典型地显示出高的摩擦因子。石墨涂层的颗粒,具体地涂层的珠粒将降低套钻的磨耗和可能地钻杆柱的弯曲度,同时推动油管,且在孔隙底部旋转钻头。
实施例4
从Swarco America Inc.of Columbia,Tennessee处获得三种尺寸:粗糙、中等和微细的玻璃珠。用以下所示的石墨wt%涂布7种样品。玻璃、塑料和陶瓷珠的其它制造者提供类似的选择且类似地用石墨涂布。
表3
用以干燥为基础,浓度为2.5、4.5、9.5、22.5(wt%)的Slip Plate No.3涂布5种200g中等尺寸的Swarco玻璃珠样品。石墨涂层的玻璃、塑料或陶瓷的珠粒的优点是,该珠粒因最佳的强度以及扭矩和阻力减小以窄的粒度范围获得。
数种珠粒聚集成用石墨涂层的单一的大颗粒不应当是问题,这是因为石墨与石墨的表面具有弱的结合力。石墨沿着{0001}平面非常软。因此,珠粒的聚集不是严重的问题,条件是优化粘合剂与石墨之比和涂布方法。事实上,各种粒度的球形珠的混合物可用作漏失循环液材料,条件是计算最佳的堆积密度。
使用获自Superior Graphite Co.的薄片石墨,等级8624(90wt%通过200目),涂布70目的陶瓷珠。将薄片石墨缓慢地倾倒在含有淀粉分散体的玻璃瓶内。用刮刀混合之后。紧跟着用1/2HP,3个刀片的螺旋桨混合器相当高速地混合,直到珠粒充分地用石墨涂布,且大多解聚集。200g一批的坯料倾倒在包肉纸上并使之在135℉下干燥。
在铸造工业中使用陶瓷珠作为合成砂,作为强化采油的压力支撑剂和在钻井流体中用作扭矩和阻力减小剂。在钻井流体中使用陶瓷珠的主要问题是其磨蚀。以上所述的石墨涂层解决了该问题。
渗流损失减小的石墨涂层的珍珠岩
实施例5
在12lb/gal海水PHPA泥浆内,与相等重量的筛分的回弹性石墨颗粒,等级9019(一种获自Superior Graphite Co.的公知的LCM产品)相比,采用30lb/bbl珍珠岩涂层的石墨的渗流损失结果优良。在珍珠岩涂层的石墨样品和由筛分的回弹性石墨颗粒制成的LCM之间在密封性能上不存在可检测的差别。
赋予具有石墨涂层的珍珠岩的另一性能是它从泥浆和水中清除油。可设计油涂层的石墨涂布颗粒,飘浮到表面上以供容易地除去。
因此,公开了具有抗摩擦涂层的油田颗粒。尽管用一些具体的实施方案描述了本发明,但不打算限制至此。例如,可有利地根据本发明涂布除了在表1中具体地所述的那些以外的油田颗粒。此外,尽管本发明涂层的颗粒在油田中可具有特定的功效,但也可考虑其它应用领域,例如冶金。因此,通过下述权利要求来定义本发明。
Claims (16)
1.一种具有石墨浸渍的涂层的油田颗粒,其中该油田颗粒选自井壁砾石充填沙、粒状膨润土、粉碎的黑沥青、碳酸钙、玻璃珠、矿毛绝缘纤维、碎纸、金属球、陶瓷珠、坚果壳、粉碎的橡胶、塑料珠、白云母、焙烧的石油焦和珍珠岩,其中涂层包括粘合剂。
2.权利要求1的油田颗粒,其中涂层包括天然和合成树脂中的一种或更多种粘合剂。
3.权利要求2的油田颗粒,其中粘合剂为水溶性树脂粘合剂。
4.权利要求2的油田颗粒,其中粘合剂为有机树脂粘合剂。
5.权利要求1或2的油田颗粒,其中石墨选自天然鳞片、合成和无定形石墨。
6.权利要求5的油田颗粒,其中石墨的尺寸范围为0.001微米-850微米。
7.权利要求1的油田颗粒,其中油田颗粒的尺寸范围为5微米至30,000微米。
8.权利要求1的涂层的油田颗粒,其中涂层包括有机成膜树脂。
9.权利要求8的油田颗粒,其中有机成膜树脂是醇酸树脂、聚氨酯和环氧树脂中的一种或更多种。
10.权利要求1的油田颗粒,其中涂层包括成膜的水溶性聚合物。
11.权利要求10的油田颗粒,其中成膜的水溶性聚合物是淀粉、羧甲基纤维素、羟乙基纤维素和黄原胶聚合物中的一种或更多种。
12.权利要求1的油田颗粒,其中涂层包括树脂分散的乳液。
13.权利要求12的油田颗粒,其中树脂分散的乳液是胶乳或丙烯酸树脂中的一种或更多种。
14.权利要求1的油田颗粒,其中涂层包括蜡。
15.权利要求1的油田颗粒,其中涂层包括烷属烃。
16.权利要求1的油田颗粒,其中涂层的粒径的筛目尺寸为+20微米(635目)至-6.3毫米(1/4目)。
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- 2006-02-24 CA CA2594932A patent/CA2594932C/en not_active Expired - Fee Related
- 2006-02-24 GE GEAP200610286A patent/GEP20115214B/en unknown
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- 2006-02-24 UA UAA200710445A patent/UA92339C2/ru unknown
- 2006-02-24 WO PCT/US2006/006460 patent/WO2006093805A2/en active Application Filing
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2007
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Patent Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
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US6734147B2 (en) * | 1995-06-07 | 2004-05-11 | Lcc County Mosquito Control | Lubricant compositions and methods |
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CA2594932C (en) | 2011-05-17 |
RU2393197C2 (ru) | 2010-06-27 |
US7666469B2 (en) | 2010-02-23 |
EG25244A (en) | 2011-11-20 |
US7402338B2 (en) | 2008-07-22 |
UA92339C2 (ru) | 2010-10-25 |
BRPI0607830A2 (pt) | 2009-10-06 |
NO20074847L (no) | 2007-09-24 |
US20080248308A1 (en) | 2008-10-09 |
EP1858694A4 (en) | 2012-04-04 |
JP2008538122A (ja) | 2008-10-09 |
CA2594932A1 (en) | 2006-09-08 |
WO2006093805A3 (en) | 2007-10-04 |
GEP20115214B (en) | 2011-05-25 |
WO2006093805A2 (en) | 2006-09-08 |
CN101128312A (zh) | 2008-02-20 |
US20070054121A1 (en) | 2007-03-08 |
EP1858694A2 (en) | 2007-11-28 |
RU2007134851A (ru) | 2009-03-27 |
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