CN111434708B - 一种水溶性碳纳米管交联剂、钻井堵漏用改性胶塞及制备方法 - Google Patents
一种水溶性碳纳米管交联剂、钻井堵漏用改性胶塞及制备方法 Download PDFInfo
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- CN111434708B CN111434708B CN201910026782.9A CN201910026782A CN111434708B CN 111434708 B CN111434708 B CN 111434708B CN 201910026782 A CN201910026782 A CN 201910026782A CN 111434708 B CN111434708 B CN 111434708B
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Abstract
本发明公开了一种水溶性碳纳米管交联剂、钻井堵漏用改性胶塞及制备方法。所述胶塞是由包括以下组分的原料制备而得:聚丙烯酰胺0.3‑1%;丙烯酰胺10‑25%;丙烯酸钠5‑20%;抗温单体0.1‑5%;引发剂0.01‑0.5%;缓聚剂0.1‑1%;乳化剂0.1‑1%;油0.1‑3%;纤维0.5‑3%;橡胶粉0.1‑1%;水溶性碳纳米管交联剂0.1‑2%;余量为水。本发明的堵漏用改性胶塞在高温条件下的成胶时间可控,成胶后抗压能力强。可应用于钻井工程堵漏作业,能解决高温条件下的井漏问题。
Description
技术领域
本发明涉及钻井堵漏技术领域,具体是涉及一种水溶性碳纳米管交联剂、钻井堵漏用改性胶塞及制备方法。
背景技术
井漏是钻井过程中经常遇到的技术难题,井漏导致成本增加,严重制约钻井速度。为了解决井漏问题,现有的技术中主要的思路是向地层中注入堵漏材料,从而解决漏失的问题。因此,堵漏材料的好坏及选择对于堵漏是否成功至关重要。目前国内外研发出多种堵漏材料,但是对于高温地层堵漏都存在一定问题。
桥接类堵漏材料的可变形性较差,如果堵漏材料直径大于漏层孔隙尺寸,就不易进入到漏层中,而在表面形成堆积,造成堵漏效果不佳。同时桥接堵漏用的核桃壳、棉籽壳和锯末等,在井内高温、高压条件下,这些材料会慢慢变软,甚至会被烧焦,导致强度降低,造成二次漏失;吸水树脂类堵漏剂,在吸水后树脂的承压强度低,对于地层骨架应力低或承压强度要求高的地层,不能满足堵漏的需要;水泥类堵漏材料,存在以下问题,水泥在固化后容易收缩,使堵漏成功率低;水泥堵漏后的扫塞过程中,会对泥浆性能造成极大伤害,造成成本增加;环氧树脂类堵漏材料,固化时间不易控制,同时固化后太脆,易造成复漏;常规凝胶抗温性能差,例如中国专利CN106010485A提供的一种自胶结堵漏剂及堵漏方法,其中用到的引发剂为过硫酸盐,该体系适合于低温地层的堵漏。中国专利CN105504158A公开的一种在地层条件下可再交联的智能凝胶颗粒,需要造粒使用,形成的吸水树脂易碎,强度较低。因此研发可抗高温的堵漏材料迫在眉睫。
发明内容
为解决现有技术的问题,本发明提供了一种水溶性碳纳米管交联剂、钻井堵漏用改性胶塞及制备方法,本发明的堵漏用改性胶塞在高温条件下的成胶时间可控,成胶后抗压能力强。可应用于钻井工程堵漏作业,能解决高温条件下的井漏问题。
本发明的目的之一是提供一种水溶性碳纳米管交联剂。
所述水溶性碳纳米管交联剂是由包括以下步骤的方法制备的:
步骤S1,碳纳米管溶解于浓硫酸和浓硝酸中,超声30-60min后80-120℃加热2-5h,冷却后用去离子水稀释,微孔滤膜过滤并水洗至中性,真空干燥后得到酸化碳纳米管;
步骤S2,将步骤S1中合成的酸化碳纳米管,氯化亚砜以及有机溶剂混合,50-70℃氮气保护下回流24-48h后冷却,减压蒸馏除去未反应的氯化亚砜后,真空干燥得到酰氯化碳纳米管;
步骤S3,将步骤S2中合成的酰氯化碳纳米管溶解在二甲基甲酰胺中,搅拌升温至40-55℃,取有机胺与烷基酚聚氧乙烯醚混合,加入二氯甲烷溶解,后将40-55℃的酰氯化碳纳米管溶液滴加到有机胺与烷基酚聚氧乙烯醚的混合溶液中,后体系升温到90-120℃反应36-48h,氮气保护;冷却后减压蒸馏除去有机胺并用丙酮清洗,产物真空干燥得到氨基/烷基酚聚氧乙烯醚基改性碳纳米管;
步骤S4,往步骤S3的改性碳纳米管中加入二氯甲烷配制成溶液,在0-5℃、通入氮气的条件下,加入丙烯酰氯,反应20-48h,冷却,减压蒸馏,洗涤、干燥,减压蒸馏得到水溶性碳纳米管交联剂。
其中,优选:
步骤S1中,浓硝酸和浓硫酸体积比1:3;
碳纳米管与浓硝酸和浓硫酸的用量比为1g:(400-2500ml)。
步骤S2中,酸化碳纳米管,氯化亚砜以及有机溶剂的用量比为1g:(100-1500ml):(500-2000ml)。
所述有机溶剂为N,N’-二甲基苯甲酰、丙酮、二甲苯、二甲基甲酰胺或甲苯。
步骤S3中,酰氯化碳纳米管与二甲基甲酰胺的用量比为1g:(400-2000ml);
有机胺、烷基酚聚氧乙烯醚、二氯甲烷的体积比范围是1:(0.5~2):(5-40);
酰氯化碳纳米管与烷基酚聚氧乙烯醚的用量范围是1g:(50-130ml)。
所述有机胺为乙二胺、二乙烯三胺、丙二胺、三乙烯四胺或己二胺。
步骤S4中,改性碳纳米管与二氯甲烷的用量比为1g:(500-2500ml);改性碳纳米管与丙烯酰氯的用量比为1g:(1-2mol)。
本发明的目的之二是提供一种采用所述水溶性碳纳米管交联剂的钻井堵漏用改性胶塞。
所述胶塞是由包括以下组分的原料制备而得:
其中,
所述聚丙烯酰胺分子量为800-3000万;
所述抗温单体为甲基丙烯酰氧乙基三甲基氯化铵、二甲基二烯丙基氯化铵、2-丙烯酰胺-2甲基丙磺酸钠、苯乙烯基磺酸钠或乙烯基磺酸钠中的一种或组合;
所述引发剂为过氧化二叔丁基、异丙苯过氧化氢或2,5-二甲基-2,5二叔丁基过氧化己烷中的一种或组合;
所述缓聚剂可采用本领域常规的缓聚剂,本发明中可优选对苯二酚、对苯醌、酚噻嗪、氯化亚铜中的一种或组合;
所述乳化剂可采用本领域常规的乳化剂,本发明可优选OP-10、OP-15、十二烷基硫酸钠、十二烷基苯磺酸钠、NP-10、NP-15、T-20、T-60、S-80、S-85中的一种或组合;
所述油为白油、柴油、煤油或植物油;
所述纤维为聚丙烯纤维、聚氨酯纤维或聚丙烯腈纤维,纤维长度为1-5mm,直径范围15-30微米;
所述的橡胶粉颗粒直径范围1-2mm。
本发明的目的之三是提供一种钻井堵漏用改性胶塞的制备方法。
包括:
所述组分按所述用量采用胶束聚合制得所述钻井堵漏用改性胶塞
本发明具体可采用以下技术方案:
本发明是以碳纳米管为起始剂,对碳纳米管进行酸化、酰氯化、胺化/酯化、取代,制备含有可聚合双键的水溶性碳纳米管交联剂;以水为分散性介质、水溶性碳纳米管为交联剂,聚丙烯酰胺为增稠剂,加入丙烯酰胺、丙烯酸钠、抗温单体、引发剂、缓聚剂、乳化剂、油、纤维、橡胶粉,采用胶束聚合得到钻井堵漏用的胶塞。
所述的聚丙烯酰胺分子量为800-3000万。
所述的抗温单体为甲基丙烯酰氧乙基三甲基氯化铵、二甲基二烯丙基氯化铵、2-丙烯酰胺-2甲基丙磺酸钠、苯乙烯基磺酸钠或乙烯基磺酸钠。
所述的引发剂为过氧化二叔丁基、异丙苯过氧化氢或2,5-二甲基-2,5二叔丁基过氧化己烷。
所述的缓聚剂为对苯二酚、对苯醌、酚噻嗪或氯化亚铜。
所述的乳化剂为OP-10、OP-15、十二烷基硫酸钠、十二烷基苯磺酸钠、NP-10、NP-15、T-20、T-60、S-80或S-85。
所述的油为白油、柴油、煤油或植物油。
所述的纤维为聚丙烯纤维、聚氨酯纤维和聚丙烯腈纤维,长度为1-5mm,直径15-30微米。
所述的橡胶粉颗粒直径1-2mm。
所述胶塞的制备配方为:
发明的效果
1、本发明首先合成抗温的改性碳纳米管为交联剂,改性后的碳纳米管表面接枝多个可反应的不饱和双键。跟以N,N-亚甲基双丙烯酰胺为交联剂的凝胶相比,本发明中的改性碳纳米管交联剂的交联点多,形成立体空间网络结构,比前者密集,宏观上表现为凝胶强度高。
2、本发明的原理是以聚丙烯酰胺为增稠悬浮剂,以丙烯酰胺、丙烯酸盐、抗温单体为主体,改性碳纳米管为交联剂,在引发剂条件下发生聚合形成高强度的立体网络凝胶。在体系中引入韧性极好的碳纳米管可以大幅度提升凝胶的强度。
3、本发明的堵漏凝胶中加入的橡胶颗粒以及纤维材料可以增强凝胶的抗压能力与抗撕裂能力。
4、在高温150℃条件下成胶时间可控制在4-11h,成胶后承压强度大于12Mpa;
5、在150℃条件下老化4个月,胶塞强度基本上不变。
6、本发明的改性胶塞抗冲刷能力强,注水冲刷50PV后,封堵率保持在90%以上。
附图说明
图1为实施例1制备的胶塞在温度130℃、压力105Mpa条件下的成胶结果;
图2为实施例3制备的胶塞在温度150℃、压力85Mpa条件下的成胶结果。
图2中,1-温度;2-压力;3-稠度。
具体实施方式
下面结合实施例,进一步说明本发明
实施例中所用原料均为市售;
实施例1
第一步:水溶性碳纳米管交联剂的制备
步骤S1,称取800mg碳纳米管放于烧杯中,用500ml浓硫酸和浓硝酸(硝酸硫酸体积比1:3)将其溶解,然后超声30min后80℃加热3h,冷却后用去离子水稀释,微孔滤膜过滤并水洗至中性,真空干燥后得到酸化碳纳米管。
步骤S2,将步骤S1中合成的酸化碳纳米管750mg,250ml氯化亚砜以及700ml二甲苯导入到三口烧瓶中,50℃氮气保护下回流24h后冷却。减压蒸馏除去大部分未反应的氯化亚砜后,真空干燥得到酰氯化碳纳米管。
步骤S3,将步骤S2中合成的酰氯化碳纳米管600mg溶解在300ml二甲基甲酰胺中,搅拌升温至50℃,取40ml乙二胺与30ml烷基酚聚氧乙烯醚混合,加入250ml二氯甲烷溶解,后将50℃的酰氯化碳纳米管溶液滴加到有机胺与烷基酚聚氧乙烯醚的混合溶液中,后体系升温到120℃反应48h,氮气保护。冷却后减压蒸馏除去乙二胺并用丙酮清洗,产物真空干燥得到氨基/烷基酚聚氧乙烯醚基改性碳纳米管。
步骤S4,往步骤S3的改性碳纳米管500mg中加入二氯甲烷300ml配制成溶液,在5℃、通入氮气的条件下,加入1mol的丙烯酰氯,反应24h,冷却,减压蒸馏,洗涤、干燥,减压蒸馏得到水溶性碳纳米管交联剂。
第二步:水溶性碳纳米管改性胶塞的制备
称取0.5g分子量为1000万的聚丙烯酰胺、14g丙烯酰胺、9g丙烯酸钠、2-丙烯酰胺-2甲基丙磺酸钠3g、0.2g引发剂异丙苯过氧化氢、0.18g缓聚剂对苯醌、0.4g乳化剂OP-15、1.8g白油、3g长度为3.5mm,直径范围15微米聚丙烯纤维、0.15g直径为1mm橡胶粉、0.8g水溶性碳纳米管交联剂,加入到水中至体系总重为100g.充分乳化得到胶塞体系T-1;将体系中的水溶性碳纳米管交联剂换成等量的未改性碳纳米管,其它组份不变,乳化得到体系N-1;将两体系放置在室温条件下,观察体系的稳定性。结果表明,N-1乳液2h左右有分层现象,而T-1乳液12h未见分层。对比表明水溶性碳纳米管有较好的溶解性,在后期固化体系中会均匀分散在体系中。
将T-1乳液倒入到高温高压稠化仪中。为了真实模拟井下条件,设定固化温度为130℃,固化压力105Mpa,得到的实验结果如图1所示,成胶时间为6.25h。
研究T-1凝胶的承压强度、老化后的性能及抗冲刷强度。
测定方法:利用岩心渗透率评价仪进行测定。将配制好的本堵漏剂,倒入装有模拟裂缝的岩心中(岩心长8cm、直径2.54cm,岩心中间挖出2cm宽裂缝),将填充堵漏剂的岩心两端密封放置于高温(130℃)烘箱中养护12h,之后将岩心冷却后放入岩心渗透率评价仪岩心夹持器中,加围压25MPa,开启平流泵,模拟现场堵漏憋挤工况,驱替清水,记录驱替泵压及出口端液体体积的变化,计算承压强度。结果表明T-1体系的承压强度为12MPa,继续注水冲刷,注水50PV时,封堵率可达91.8%;将凝胶体系注入到岩心后两端密封,放置在130℃条件下老化4个月,后测定凝胶的承压强度。结果表明,T-1体系老化4个月的承压强度为11.4MPa。
以上结果表明水溶性碳纳米管改性胶塞的承压强度高、抗冲刷性能强、抗老化性能好。
实施例2
第一步:水溶性碳纳米管交联剂的制备
步骤S1,称取1g碳纳米管放于烧杯中,用2200ml浓硫酸和浓硝酸(硝酸硫酸体积比1:3)将其溶解,然后超声50min后100℃加热5h,冷却后用去离子水稀释,微孔滤膜过滤并水洗至中性,真空干燥后得到酸化碳纳米管。
步骤S2,将步骤S1中合成的酸化碳纳米管500mg,650ml氯化亚砜以及300ml二甲基甲酰胺导入到三口烧瓶中,70℃氮气保护下回流24h后冷却。减压蒸馏除去大部分未反应的氯化亚砜后,真空干燥得到酰氯化碳纳米管。
步骤S3,将步骤S2中合成的酰氯化碳纳米管450mg溶解在450ml二甲基甲酰胺中,搅拌升温至50℃,取40ml己二胺与50ml烷基酚聚氧乙烯醚混合,加入800ml二氯甲烷溶解,后将50℃的酰氯化碳纳米管溶液滴加到有机胺与烷基酚聚氧乙烯醚的混合溶液中,后体系升温到120℃反应48h,氮气保护。冷却后减压蒸馏除去己二胺并用丙酮清洗,产物真空干燥得到氨基/烷基酚聚氧乙烯醚基改性碳纳米管。
步骤S4,往步骤S3的改性碳纳米管400mg中加入1000ml二氯甲烷配制成溶液,在3℃、通入氮气的条件下,加入0.4mol的丙烯酰氯,反应48h,冷却,减压蒸馏,洗涤、干燥,减压蒸馏得到水溶性碳纳米管交联剂。
第二步:水溶性碳纳米管改性胶塞的制备
称取0.4g分子量为2000万的聚丙烯酰胺、18g丙烯酰胺、10g丙烯酸钠、苯乙烯基磺酸3.5g、0.2g引发剂异丙苯过氧化氢、0.85g缓聚剂对苯醌、0.9g乳化剂NP-15、2g煤油、1.5g长度为4mm,直径范围20微米聚氨酯纤维、0.15g直径为1.5mm橡胶粉、0.9g水溶性碳纳米管交联剂,加入到水中至体系总重为100g,充分乳化得到胶塞体系T-2;将体系中的水溶性碳纳米管交联剂换成等量的N,N’-亚甲基双丙烯酰胺,其它组份不变,乳化得到体系N-2;将体系倒入到高温高压稠化仪中。分别测定两个体系在140℃,100Mpa条件下的成胶性能、测定两个体系的承压强度、老化后的承压强度及抗冲刷性能。结果如表1所示。以上结果表明以改性纳米二氧化硅为交联剂的凝胶比N,N-亚甲基双丙烯酰胺为交联剂的凝胶承压强度大。
表1 T-2体系与N-2体系成胶性能对比
实施例3
第一步:水溶性碳纳米管交联剂的制备
步骤S1,称取1g碳纳米管放于烧杯中,用1000ml浓硫酸和浓硝酸(硝酸硫酸体积比1:3)将其溶解,然后超声60min后100℃加热5h,冷却后用去离子水稀释,微孔滤膜过滤并水洗至中性,真空干燥后得到酸化碳纳米管。
步骤S2,将步骤S1中合成的酸化碳纳米管700mg,200ml氯化亚砜以及1100ml甲苯导入到三口烧瓶中,70℃氮气保护下回流48h后冷却。减压蒸馏除去大部分未反应的氯化亚砜后,真空干燥得到酰氯化碳纳米管。
步骤S3,将步骤S2中合成的酰氯化碳纳米管650mg溶解在1050ml二甲基甲酰胺中,搅拌升温至50℃,取40ml二乙烯三胺与80ml烷基酚聚氧乙烯醚混合,加入1300ml二氯甲烷溶解,后将50℃的酰氯化碳纳米管溶液滴加到有机胺与烷基酚聚氧乙烯醚的混合溶液中,后体系升温到120℃反应48h,氮气保护。冷却后减压蒸馏除去二乙烯三胺并用丙酮清洗,产物真空干燥得到氨基/烷基酚聚氧乙烯醚基改性碳纳米管。
步骤S4,往步骤S3的改性碳纳米管600mg中加入二氯甲烷730ml配制成溶液,在5℃、通入氮气的条件下,加入0.9mol的丙烯酰氯,反应36h,冷却,减压蒸馏,洗涤、干燥,减压蒸馏得到水溶性碳纳米管交联剂。
第二步:水溶性碳纳米管改性胶塞的制备
称取0.3g分子量为2500万的聚丙烯酰胺、23g丙烯酰胺、15g丙烯酸钠、二甲基二烯丙基氯化铵3g、0.25g引发剂2,5-二甲基-2,5二叔丁基过氧化己烷、0.49g缓聚剂酚噻嗪、0.14g乳化剂OP-15、1.5g柴油、0.5g长度为5mm,直径范围25微米聚丙烯腈纤维、0.95g直径为2mm橡胶粉、1.5g水溶性碳纳米管交联剂,加入到水中至体系总重为100g.,充分乳化得到胶塞体系,将该体系倒入到高温高压稠化仪中。为了真实模拟井下条件,设定固化温度为150℃,固化压力85Mpa。结果如图2所示,成胶时间为4.25h,成胶后承压强度为14.2Mpa,注水50PV时,封堵率可达94.5%;将凝胶体系注入到岩心后两端密封,放置在150℃条件下老化4个月,凝胶承压强度基本不变。
Claims (10)
1.一种水溶性碳纳米管交联剂,其特征在于:
所述水溶性碳纳米管交联剂是由包括以下步骤的方法制备的:
步骤S1,碳纳米管溶解于浓硫酸和浓硝酸中,超声30-60min后80-120℃加热2-5h,冷却后用去离子水稀释,微孔滤膜过滤并水洗至中性,真空干燥后得到酸化碳纳米管;
步骤S2,将步骤S1中合成的酸化碳纳米管,氯化亚砜以及有机溶剂混合,50-70℃氮气保护下回流24-48h后冷却,减压蒸馏除去未反应的氯化亚砜后,真空干燥得到酰氯化碳纳米管;
步骤S3,将步骤S2中合成的酰氯化碳纳米管溶解在二甲基甲酰胺中,搅拌升温至40-55℃,取有机胺与烷基酚聚氧乙烯醚混合,加入二氯甲烷溶解,后将40-55℃的酰氯化碳纳米管溶液滴加到有机胺与烷基酚聚氧乙烯醚的混合溶液中,后体系升温到90-120℃反应36-48h,氮气保护;冷却后减压蒸馏除去有机胺并用丙酮清洗,产物真空干燥得到氨基/烷基酚聚氧乙烯醚基改性碳纳米管;
步骤S4,往步骤S3的改性碳纳米管中加入二氯甲烷配制成溶液,在0-5℃、通入氮气的条件下,加入丙烯酰氯,反应20-48h,冷却,减压蒸馏,洗涤、干燥,减压蒸馏得到水溶性碳纳米管交联剂。
2.如权利要求1所述的水溶性碳纳米管交联剂,其特征在于:
步骤S1中,浓硝酸和浓硫酸体积比1:3;
碳纳米管与浓硝酸和浓硫酸的用量比为1g:400-2500ml。
3.如权利要求1所述的水溶性碳纳米管交联剂,其特征在于:
步骤S2中,酸化碳纳米管,氯化亚砜以及有机溶剂的用量比为1g:(100-1500ml):(500-2000ml);
所述有机溶剂为N,N’-二甲基苯甲酰、丙酮、二甲苯、二甲基甲酰胺或甲苯。
4.如权利要求1所述的水溶性碳纳米管交联剂,其特征在于:
步骤S3中,酰氯化碳纳米管与二甲基甲酰胺的用量比为1g:(400-2000ml);
有机胺、烷基酚聚氧乙烯醚、二氯甲烷的体积比范围是1:(0.5~2):(5-40);
酰氯化碳纳米管与烷基酚聚氧乙烯醚的用量范围是1g:(50-130ml);
所述有机胺为乙二胺、二乙烯三胺、丙二胺、三乙烯四胺或己二胺。
5.如权利要求1所述的水溶性碳纳米管交联剂,其特征在于:
步骤S4中,改性碳纳米管与二氯甲烷的用量比为1g:(500-2500ml);改性碳纳米管与丙烯酰氯的用量比为1g:(1-2mol)。
8.如权利要求6所述的钻井堵漏用改性胶塞,其特征在于:
所述聚丙烯酰胺分子量为800-3000万;
所述抗温单体为甲基丙烯酰氧乙基三甲基氯化铵、二甲基二烯丙基氯化铵、2-丙烯酰胺-2甲基丙磺酸钠、苯乙烯基磺酸钠或乙烯基磺酸钠中的一种或组合;
所述引发剂为过氧化二叔丁基、异丙苯过氧化氢或2,5-二甲基-2,5二叔丁基过氧化己烷中的一种或组合。
9.如权利要求6所述的钻井堵漏用改性胶塞,其特征在于:
所述缓聚剂为对苯二酚、对苯醌、酚噻嗪、氯化亚铜中的一种或组合;
所述乳化剂为OP-10、OP-15、十二烷基硫酸钠、十二烷基苯磺酸钠、NP-10、NP-15、T-20、T-60、S-80、S-85中的一种或组合;
所述油为白油、柴油、煤油或植物油;
所述纤维为聚丙烯纤维、聚氨酯纤维或聚丙烯腈纤维,纤维长度为1-5mm,直径范围15-30微米;
所述橡胶粉颗粒直径范围1-2mm。
10.一种如权利要求6~9之一所述的钻井堵漏用改性胶塞的制备方法,其特征在于所述方法包括:
所述组分按所述用量加入到水中搅拌、乳化,制得所述钻井堵漏用改性胶塞。
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