CN101519585B - Shearing cross-linking sensitive plugging agent and preparation method thereof - Google Patents

Shearing cross-linking sensitive plugging agent and preparation method thereof Download PDF

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CN101519585B
CN101519585B CN 200910061384 CN200910061384A CN101519585B CN 101519585 B CN101519585 B CN 101519585B CN 200910061384 CN200910061384 CN 200910061384 CN 200910061384 A CN200910061384 A CN 200910061384A CN 101519585 B CN101519585 B CN 101519585B
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solution
linking
organic titanium
guar gum
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CN101519585A (en )
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刘莉
高丽
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荆州市弘利化工科技有限公司
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Abstract

The invention provides a shearing cross-linking sensitive plugging agent used for the drilling engineering. The plugging agent comprises the following components: 40 to 60 parts of organic titanium coThe invention provides a shearing cross-linking sensitive plugging agent used for the drilling engineering. The plugging agent comprises the following components: 40 to 60 parts of organic titanium coal-oil solution, 40 to 60 parts of modified guar gum solution and 2 to 5 parts of emulsifier, wherein the organic titanium coal-oil solution is the mixture of coal oil and organic titanium, the organial-oil solution, 40 to 60 parts of modified guar gum solution and 2 to 5 parts of emulsifier, wherein the organic titanium coal-oil solution is the mixture of coal oil and organic titanium, the organic titanium is any one of the titanate compounds, the modified guar gum solution is obtained by the graft copolymerization of acrylamide, hydroxymethyl acrylamide monomer and guar gum, and the emulsific titanium is any one of the titanate compounds, the modified guar gum solution is obtained by the graft copolymerization of acrylamide, hydroxymethyl acrylamide monomer and guar gum, and the emulsifier is fatty acid polyoxyethylene ether. The preparation method comprises the following steps: the 2 to 5 parts of the emulsifier is added to the 40 to 60 parts of the organic titanium coal-oil solutioer is fatty acid polyoxyethylene ether. The preparation method comprises the following steps: the 2 to 5 parts of the emulsifier is added to the 40 to 60 parts of the organic titanium coal-oil solution, the emulsifier and the organic titanium coal-oil solution are evenly stirred, then the 40 to 60 parts of the modified guar gum solution is added into the mixture slowly and stirred for 1 hour at thn, the emulsifier and the organic titanium coal-oil solution are evenly stirred, then the 40 to 60 parts of the modified guar gum solution is added into the mixture slowly and stirred for 1 hour at the temperature of 30 to 35 DEG C to form stable reversed emulsion through a colloid mill, and the finished product of the shearing cross-linking sensitive plugging agent is further obtained. The shearie temperature of 30 to 35 DEG C to form stable reversed emulsion through a colloid mill, and the finished product of the shearing cross-linking sensitive plugging agent is further obtained. The shearing cross-linking sensitive plugging agent is used for plugging a drilling, the cross-linking agent can be immediately mixed with macromolecule under the action of the high shearing rate of the bit porng cross-linking sensitive plugging agent is used for plugging a drilling, the cross-linking agent can be immediately mixed with macromolecule under the action of the high shearing rate of the bit port to generate cross-linking, and the gelling stemming similar to the plastic solid is formed so as to rapidly block the serious leakage layer.t to generate cross-linking, and the gelling stemming similar to the plastic solid is formed so as to rapidly block the serious leakage layer.

Description

剪切交联敏感性堵漏剂及制备方法技术领域 TECHNICAL FIELD The shear sensitivity of crosslinked plugging agent

[0001] 本发明涉及到钻井堵漏工程领域,尤其涉及到剪切交联敏感性堵漏剂及制备方法。 [0001] The present invention relates to the field of drilling plugging, particularly in relation to the shear-sensitive crosslinking agent and preparation method of plugging. 背景技术 Background technique

[0002] 井漏是油田钻井过程中普遍存在而又十分严重的问题,它不仅影响钻井速度,而且会造成巨大的经济损失。 [0002] lost circulation during drilling oil is widespread and very serious problem, which not only affects the drilling speed, but will also cause huge economic losses. 目前国内外普遍采用的堵漏方法主要是桥塞堵漏,由于井下漏层性质(如裂缝宽度)难以准确判断,堵剂颗粒粒径与漏层裂缝宽度不匹配,往往易造成堵漏效果不佳和堵漏后发生重复性漏失。 Currently widely used at home and abroad plugging method is mainly bridge plug plugging, because the underground drain layer properties (e.g., crack width) is difficult to accurately determine, blocking agent particle size and crack does not match the width of the drain layer, the effect is not often easy to cause plugging repeatability and good leakage occurred after plugging. 同时,桥塞堵漏在堵漏实施过程中需要起下钻,从而影响钻井作业效率。 Meanwhile, the bridge plug in the plugging requires tripping embodiment plugging process, thereby affecting the efficiency of drilling operations. 近年来,从国外堵漏材料的研究与应用状况看,化学堵漏剂发展较快。 In recent years, the research and application status abroad plugging material point of view, the rapid development of chemical blocking agent. 由于石油开发速度的加快,钻井面临着更加复杂多变的漏失地层,需要进一步研制开发新型的堵漏剂,以适应和满足封堵不同类型漏层的需要,以及优质快速钻井的要求。 Due to accelerate the speed of development of oil drilling faced with a more complex formations leakage, the need for further research and development of new sealing agent, in order to adapt and meet the needs of different types of blocking the drain layer, and the requirements of high-quality fast drilling. 发明内容 SUMMARY

[0003] 本发明的目的是提供一种在钻头水眼高剪切速率的作用下可发生交联而形成凝胶堵塞物的堵漏剂及制备方法。 [0003] The object of the present invention is to provide a method for preparing a gel plug plugging agent to form a crosslinked under the action of the water hole drill high shear rates.

[0004] 为实现上述目的,本发明的技术方案为: [0004] To achieve the above object, the technical solution of the present invention is:

[0005] 剪切交联敏感性堵漏剂由如下重量份组分构成: [0005] Shear-sensitive sealing crosslinking agent component consists of the following parts by weight:

[0006] 有机钛煤油溶液40〜60份 [0006] kerosene solution 40~60 parts organotitanium

[0007] 改性瓜尔胶水溶液40〜60份 40~60 parts [0007] The modified guar solution

[0008] 乳化剂 2〜5份 [0008] 2 ~ 5 parts emulsifier

[0009] 其中:有机钛煤油溶液为煤油与有机钛的混合物,有机钛浓度(质量百分比)为0. 1〜1.0%,改性瓜尔胶水溶液是由丙烯酰胺、羟甲基丙烯酰胺单体与瓜尔胶接枝共聚而得,乳化剂为脂肪酸聚氧乙烯醚。 [0009] wherein: organic titanium solution is a mixture of kerosene and kerosene with an organic titanium, organic titanium concentration (percent by mass) was 0.5 1~1.0%, modified guar solution is an acrylamide, methylol acrylamide monomers and obtained by graft copolymerization of guar gum, emulsifier polyoxyethylene fatty acid ethers.

[0010] 有机钛为钛酸酯化合物:如正钛酸四异丙基酯、正钛酸双乳酸双异丙基酯、正钛酸双三乙醇胺双异丙基脂中的任意一种。 [0010] The organic titanium compound is a titanate: tetra-n, such as isopropyl acrylate, n-titanate, bis bis acid isopropyl ester, bis any one of triethanolamine titanate, bis n-isopropyl grease in.

[0011] 改性瓜尔胶水溶液的接枝共聚过程为:用100份冷水将0. 5〜1. 5份瓜尔胶分散、 溶解,通氮气lh,加入0. 001〜0. 01份硫酸铈铵溶液,搅拌10分钟后,加入0. 1〜0. 3份丙烯酰胺、0. 1〜0. 3份羟甲基丙烯酰胺单体,在氮气保护下继续搅拌反应2小时。 [0011] The graft copolymerization process modified guar solution is: 0.5 with 100 parts of cold water and 5 parts guar gum 5~1 dispersed, dissolved, LH nitrogen, was added 0.5 parts of sulfuric acid 01 001~0. cerium hydroxide solution. after stirring for 10 minutes, 0.5 1~0 3 parts of acrylamide, 0. 1~0. 3 parts of monomers methylol acrylamide, with stirring under nitrogen the reaction was continued for 2 hours.

[0012] 脂肪酸聚氧乙烯醚是由碳链长度为C12〜C18的饱和或不饱和脂肪酸和环氧乙烷的加成产物,脂肪酸和环氧乙烷的摩尔比例为1 : 3〜15。 [0012] polyoxyethylene fatty acid is a carbon chain length of saturated or unsaturated fatty acids and ethylene oxide addition products C12~C18, the molar ratio of fatty acids and ethylene oxide is 1: 3~15.

[0013] 本发明的积极效果是: [0013] The positive effect of the invention is:

[0014] 1、可适合不同宽度裂缝地层和渗漏地层堵漏; [0014] 1, different widths may be suitable for formation fracture formation and plugging leaks;

[0015] 2、堵漏作业过程中无需起下钻; [0015] 2, during plugging operations without tripping;

[0016] 3、堵漏剂在地面上不发生交联,可泵送通过任何井下工具,仅在通过钻头水眼产生高强度剪切后才能引发胶凝;[0017] 4、与各种钻井液都可以匹配。 [0016] 3, not crosslinked sealing agent on the ground, can be pumped by any downhole tool, can be triggered gelling only after generation of high intensity shear the water hole by the drill bit; [0017] 4, and various drilling liquid can match. 具体实施方式 Detailed ways

[0018] 下面通过实施例对本发明做进一步的说明: [0018] The following examples further illustrate the present invention:

[0019] (1)有机钛煤油溶液的制备 Preparing an organic titanium kerosene solution [0019] (1)

[0020] 有机钛作为交联剂,能将含有〜OH高分子链相互联结形成一种体型结构,有机钛为钛酸酯化合物如:正钛酸四异丙基酯、正钛酸双乳酸双异丙基酯、正钛酸双三乙醇胺双异丙基酯中的任意一种,将有机钛与煤油混合形成有机钛煤油溶液,有机钛交联剂在煤油中的浓度(质量百分比)为0. 1〜1.0%。 [0020] Organic titanium as a crosslinking agent, a polymer chain can contain ~OH linked to each other to form a body structure, an organic titanium compound such as titanate: tetra-n-isopropyl ester, n-titanate acid bis-bis isopropyl acrylate, n-isopropyl titanate, bis any one ester bis triethanolamine, organic titanium kerosene kerosene are mixed to form a solution of an organic titanium, titanium concentration of the organic crosslinking agent in kerosene (mass percentage) 0 . 1~1.0%.

[0021] (2)改性瓜尔胶水溶液的制备 Preparing an aqueous solution of modified guar [0021] (2)

[0022] 改性瓜尔胶作为稠化剂,是由丙烯酰胺、羟甲基丙烯酰胺单体与瓜尔胶接枝共聚得到,其接枝共聚过程为:用100份冷水将0. 5〜1. 5份瓜尔胶分散、溶解,通氮气1小时, 加入0. 001〜0. 01份硫酸铈铵溶液,搅拌10分钟后,加入0. 1〜0. 3份丙烯酰胺、0. 1〜 0. 3份羟甲基丙烯酰胺单体,在氮气保护下继续搅拌反应2小时。 [0022] The modified guar as a thickening agent is obtained by the copolymerization of acrylamide, methylol acrylamide monomer grafted guar gum, which is a graft copolymerization process: 100 parts of cold water with 0. -5 to 1.5 parts of guar gum dispersed, dissolved, through nitrogen for 1 hour, 0.5 001~0. 01 parts by ceric ammonium sulfate solution, stirred for 10 minutes, a solution of 0.5 1~0 3 parts of acrylamide, 0.1 ~ 0.3 parts methylol acrylamide monomers, stirring was continued for 2 hours under nitrogen.

[0023] (3)乳化剂的制备 Preparation of [0023] (3) an emulsifier

[0024] 脂肪酸聚氧乙烯醚由碳链长度为C12〜C18的饱和或不饱和脂肪酸与环氧乙烷的加成产物,其中脂肪酸和环氧乙烷的摩尔比例为1 : 3〜15。 [0024] polyoxyethylene fatty acid having a carbon chain length of saturated or unsaturated fatty acids and ethylene oxide addition products of C12~C18, wherein the molar ratio of the fatty acid and ethylene oxide is 1: 3~15.

[0025] (4)剪切交联敏感性堵漏剂的制备 Preparation shear sensitivity sealing crosslinking agent [0025] (4)

[0026] 用量筒取300mL煤油倒入烧杯中,加入1. Og正钛酸四异丙基酯,搅拌溶解,然后加入IOg油酸聚氧乙烯醚,搅拌溶解。 [0026] extracted with 300mL graduated cylinder kerosene poured into a beaker, added 1. Og n-tetraisopropyl titanate, stirred and dissolved, followed by the addition of oleic acid IOg polyoxyethylene ethers, stirred and dissolved. 在三颈反应瓶中用200!^冷水将2.(^瓜尔胶分散、溶解,通氮气1小时,加入0. 003g硫酸铈铵溶液,搅拌10分钟后,加入0. 2g丙烯酰胺、0. Ig 羟甲基丙烯酰胺单体,在氮气保护下继续搅拌反应2小时。在搅拌条件下,将三颈反应瓶中的改性瓜尔胶水溶液慢慢加入到含有油酸聚氧乙烯醚乳化剂的煤油溶液中,形成堵漏剂产PΡΠ O Three-necked reaction flask with 200! ^ 2 cold water. (^ Guar gum dispersed, dissolved, through nitrogen for 1 hour, 0. 003g ammonium cerium sulfate solution, stirred for 10 minutes, a solution of 0. 2g of acrylamide, 0 . an Ig methylol acrylamide monomers, reaction was continued for 2 hours with stirring under nitrogen. under stirring, three-necked reaction flask modified guar gum was added slowly to the aqueous solution containing emulsified vinyl oleate polyoxyethylene ethers solution in kerosene to form a sealing agent produced PΡΠ O

[0027] 实例检验结果: [0027] Examples of test results:

[0028] 在250mL水中加入7. 5gNa0H,搅拌溶解,加入250g上述堵漏剂,在10000r/min的条件下搅拌15分钟,然后测定放置不同时间下凝胶强度,结果见1。 [0028] in 250mL of water was added 7. 5gNa0H, stirred to dissolve, was added 250g sealing agent described above, was stirred at 10000r / min for 15 minutes, then the gel strength was measured at different time place, results are 1.

[0029] 表1放置不同时间下的凝胶强度 [0029] Table 1 is placed on the gel strength at different times

[0030] [0030]

Figure CN101519585BD00041

[0031] 由表1可知,堵漏剂在碱性环境下高速剪切后,30分钟后开始有凝胶强度形成, 120〜180分钟后形成较稳定的凝胶强度。 [0031], the high speed shearing sealing agent 30 minutes after the start of the gel strength formed from Table 1 in an alkaline environment to form a stable gel strength 120~180 minutes.

Claims (2)

  1. 1. 一种用于钻井堵漏的剪切交联敏感性堵漏剂,其特征在于,剪切交联敏感性堵漏剂由下列重量份组份构成:其中:有机钛煤油溶液为煤油与有机钛的混合物,有机钛为钛酸酯化合物:是正钛酸四异丙基酯、正钛酸双乳酸双异丙基酯、正钛酸双三乙醇胺双异丙基酯中的任意一种,有机钛在煤油中的浓度质量百分比为0. 1〜1. 0% ;改性瓜尔胶水溶液是由丙烯酰胺、羟甲基丙烯酰胺单体与瓜尔胶接枝共聚而得,改性瓜尔胶水溶液的接枝共聚过程为:用100份冷水将0. 5〜1. 5份瓜尔胶分散、溶解,通氮气1小时,加入0. 001〜0. 01份硫酸铈铵溶液,搅拌10分钟后,加入0. 1〜0. 3份丙烯酰胺、0. 1〜0. 3份羟甲基丙烯酰胺单体,在氮气保护下继续搅拌反应2小时;乳化剂为脂肪酸聚氧乙烯醚,脂肪酸聚氧乙烯醚是由碳链长度为C12〜Cw的饱和或不饱和脂肪酸与环氧乙烷的加 1. A shear sensitivity crosslinked plugging sealing agent for drilling, characterized in that the shear-sensitive sealing crosslinking agent consists of the following parts by weight Group: wherein: organic titanium kerosene and kerosene solution mixture of organic titanium, organic titanate as titanium compound: n is tetraisopropyl titanate, bis ortho-titanic acid bis isopropyl acrylate, n-bis triethanolamine titanate, bis any isopropyl ester of one, organotitanium mass concentration in kerosene 0. 0% 1~1; modified guar gum solution is an acrylamide, methylol acrylamide monomers and obtained by graft copolymerization of guar gum, modified guar graft copolymerization of guar gum aqueous solution: 0.5 with 100 parts of cold water and 5 parts guar gum 5~1 dispersed, dissolved, through nitrogen for 1 hour, 0.5 parts of 01 001~0 ammonium cerium sulfate solution, stirring. after 10 minutes, added 0.5 1~0 3 parts of acrylamide, 3 parts of 1~0 0 methylol acrylamide monomers, stirring continued under nitrogen for 2 hours;... emulsifier is a polyoxyethylene fatty ether , polyoxyethylene ethers of fatty acids by C12~Cw carbon chain length of saturated or unsaturated fatty acids with ethylene oxide plus 产物,脂肪酸和环氧乙烷的摩尔比例为1 : 3-15 ;剪切交联敏感性堵漏剂的制备方法为:将2〜5份乳化剂脂肪酸聚氧乙烯醚加入到40〜60份有机钛煤油溶液中,搅拌均勻,然后在200r/min的搅拌下,缓慢加入40〜 60份改性瓜尔胶水溶液,在30〜35°C时搅拌1小时,最后经胶体磨形成稳定的反相乳化液,即得到剪切交联敏感性堵漏剂成品。 The product, the molar ratio of fatty acids and ethylene oxide is 1: 3-15; Preparation shear sensitivity sealing a crosslinking agent to: 2 ~ 5 parts of polyoxyethylene fatty acid emulsifier were added to the parts of 40~60 organotitanium kerosene solution, stir, and then stirring at 200r / min, and slowly added 60 parts of 40~ modified guar solution was stirred at 30~35 ° C 1 hour and finally through a colloid mill to form a stable trans emulsion phase, i.e. cleavable crosslink to give the finished sealing agent sensitivity.
  2. 2.根据权利要求1所述的剪切交联敏感性堵漏剂的制备方法,其特征在于:将2〜5 份乳化剂脂肪酸聚氧乙烯醚加入到40〜60份有机钛煤油溶液中,搅拌均勻,然后在200r/ min的搅拌下,缓慢加入40〜60份改性瓜尔胶水溶液,在30〜35°C时搅拌1小时,最后经胶体磨形成稳定的反相乳化液,即得到剪切交联敏感性堵漏剂成品。 2. Preparation method of crosslinking a shear sensitive sealing agent according to claim, characterized in that: 2 ~ 5 parts of polyoxyethylene fatty acid emulsifier were added to the organic parts of 40~60 kerosene solution of titanium, stir, then stirred at 200r / min, the parts of 40~60 was slowly added an aqueous solution of modified guar, stirred at 30~35 ° C 1 hour and finally through a colloid mill to form a stable inverse emulsion, i.e., to give shear sensitivity crosslinking finished sealing agent. 有机钛煤油溶液改性瓜尔胶水溶液乳化剂40〜60份40〜60份2〜5份 Kerosene solution of organic titanium modified guar parts 40~60 40~60 parts emulsifier solution 2 ~ 5 parts
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CN101705082B (en) 2009-11-20 2012-07-04 中国石油大学(华东) Formulated fracturing fluid of micro emulsion gel
CN102559162B (en) * 2010-12-08 2014-11-26 中国石油天然气股份有限公司 Leakage-proof type temporary blockage additive for low-pressure thin oil well
CN102911649B (en) * 2011-08-05 2015-09-23 中国石油天然气股份有限公司 High strength degradation from the packer material and method
CN105219365B (en) * 2015-09-11 2017-11-24 中石化石油工程技术服务有限公司 The sealing deep cross-linked polymer gel and preparation method
CN106277989A (en) * 2016-08-17 2017-01-04 张静 Preparation method of anti-permeation plugging agent
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JP2001152155A (en) 1999-11-26 2001-06-05 Nippon Polyurethane Ind Co Ltd Grouting chemical liquid composition for stabilization of ground and artificial building, and the like, and method for stabilizing and reinforcing water sealing using the same
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CN1047686A (en) 1990-04-06 1990-12-12 渤海石油公司钻井公司 High temp.-resisting temporary stopping agent in drilling well
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US20060229213A1 (en) 2005-04-07 2006-10-12 Halliburton Energy Services, Inc. Fluids comprising zirconium isopropylamine crosslinking agents and associated methods
CN101314713A (en) 2008-05-08 2008-12-03 伊向艺;卢 渊;管保山 Controllable-viscosity acid liquor system for carbonatite container horizon acid fracturing

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