CN116103026A - 竞争交联型高密度抗盐固化水微凝胶暂堵剂及其制备方法 - Google Patents
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Abstract
本发明提供了一种竞争交联型高密度抗盐固化水微凝胶暂堵剂及其制备方法,属于油气田钻完井工程领域。其原料包括45%~64%的磷酸盐类化合物,3.3%~4.7%的固化剂,以及2.5%~10%的交联剂,其余为水。本发明突破了柔性微凝胶(吸水树脂类材料)无法爱吸收饱和高密度盐水的瓶颈,通过多级交联解决了凝胶暂堵剂密度难以答复提升的难题。其最高密度可达1.83g/cm3,通过盐水加重可防止在高密度完井液中上浮,并且耐温180℃,暂堵后通过高温自降解或破胶液加速破胶返排,有效解决了高温高压多压力层系油气井下部射孔层段暂堵控漏的难题,应用前景广阔。
Description
技术领域
本发明涉及油气田钻完井工程领域,具体为竞争交联型高密度抗盐固化水微凝胶暂堵剂及其制备方法。
背景技术
现今油气藏开发对象逐渐向深层、超深层转移。在开发过程中井深增加,地质条件复杂多变,常伴随着众多挑战性的难题,如高温、高压、储层压力反转、“上喷下漏”等问题。针对存在异常高压储层的井,井控安全需求和低压储层压井液漏失之间的矛盾是修、完井作业面临的主要技术难点和成本增长点。按照现有理论技术,对于存在异常高压储层的井,进行井下作业时必须按照“就高不就低”的压井液密度选择原则先进行压井操作。在满足井控安全需求的同时,高密度压井液液柱会对低压储层带来较大的压差。当压差值超过储层的漏失阈值以后,高密度工作液会漏失进入储层。工作液漏失轻则增大压井液用量、增加成本,重则伤害储层、降低产量,非常严重的时候甚至会造成井控安全风险。综上所述,掌握适用于高温高压及多压力层系油气井的压井堵漏技术非常关键。
无固相完井液和修井液是目前针对高温高压油藏的新的思路,由于其不具有相应的固相,因此无论是泵送还是在地层中的运移都要优于含固相的完井液与修井液,因此是目前研究的热点。但是对于现有的无固相完井与修井液体系来讲,有的密度较低,难以适用于高压地层;有的则难以固化,作用较为单一;即使少数具有较高密度和能够固化的无固相完井液与修井液,其仍然存在耐温性不足的问题。
发明内容
为解决上述至少一种问题,本发明提出了一种竞争交联型高密度抗盐固化水微凝胶暂堵剂的制备方法。
为实现上述目标,本发明的技术方案如下:一种竞争交联型高密度抗盐固化水微凝胶暂堵剂,按质量百分数,包括45%~64%的磷酸盐类化合物,3.3%~4.7%的固化剂,以及1.4%~6.7%的交联剂,其余为水;所述磷酸盐类化合物为磷酸氢二钾、七水磷酸钾、焦磷酸钾中的一种或多种,所述固化剂为柔性微凝胶,所述交联剂为所述柔性微凝胶的交联剂;
所述柔性微凝胶的制备方法如下:取丙烯酸,并将其中和度调节至50%~70%,再依次加入丙烯酰胺、N,N'-亚甲基双丙烯酰胺、木质素硫酸镁和过硫酸钾,将其依次在50~60℃、60~70℃、70~80℃反应2~3h,反应结束后对其进行分离、提纯、干燥、造粒即得;以摩尔比计,所述丙烯酸、丙烯酰胺、N,N'-亚甲基双丙烯酰胺和过硫酸钾的比例为:1000:900~1100:0.4~0.6:3~5,且每加入1mol丙烯酸,需加入1.5~1.8g木质素磺酸镁。
在本发明中,磷酸盐类化合物的作用有二:第一,能够增加整个体系的密度,最高可达1.8g/cm3;第二,能够作为柔性微凝胶的交联剂,由于磷酸盐中具有较多的氧原子,其能够与胺基形成N-H···O氢键,同时,磷酸基团通过磷酸化被引入到柔性微凝胶的聚电解质分子链中形成三维离子网络。磷酸盐和交联剂一起,共同促进柔性微凝胶的固化。
同时,本发明的体系,由于同时设置有柔性微凝胶、磷酸盐类化合物和交联剂,在三者的协同作用下,能够应用于较高温度的环境,最高使用温度可达180℃,且在该温度条件下,成胶时间在1.5~3h,凝胶强度可达H~I范围。相对于现有技术,其具有较好的效果。
本发明的一种实施方式在于,所述交联剂为乌洛托品、聚乙烯亚胺中的至少一种。
本发明的一种实施方式在于,所述柔性微凝胶的分离、提纯、干燥、造粒步骤具体为:将反应产物取出并切片,后用无水乙醇浸泡至少8h,取出产物,将其置于真空干燥箱中干燥,对其进行粉碎、过筛,选取60~100目的颗粒即得。
本发明的另一个目的是公开一种竞争交联型高密度抗盐固化水微凝胶暂堵剂的制备方法,该方法包括以下步骤:取磷酸盐类化合物,将其加入水中溶解;加入柔性微凝胶,搅拌10~30min,加入交联剂溶液搅拌均匀即可。
有益效果:本发明的竞争交联型高密度抗盐固化水微凝胶暂堵剂,其具有较高的密度,可控制在1.5~1.8g/cm3范围内,同时,还具有较好的耐温性能,能够达到160~180℃,且最终的凝胶强度可达H~I范围,说明本发明具有较好的耐温性能;同时成胶后具有较高的强度,对不同缝宽压井液漏失后可通过形变延缓漏失,具有动态暂堵承压性能,暂堵后通过破胶液渗透多孔结构可实现高温下快速破胶降解,能够适用于一些高温高压油气藏。
附图说明
图1为磷酸盐溶液密度-质量分数关系曲线。
表1为不同密度抗盐固化水微凝胶体系固化与强度性能(根据凝胶强度规范(Sydansk,R.D.and Argabright,P.A.1987.Conformance Improvement in aSubterranean Hydrocarbon-Bearing Formation Using a Polymer Gel.US PatentNo.4,683,949.),A-E定义为未固化,F-I定义为固化)。
图2为竞争交联型高密度抗盐固化水微凝胶暂堵剂的承压和漏失结果。(a)4.0mm缝宽的压力曲线。(b)4.0mm缝宽的漏失曲线。(c)2.5mm缝宽的压力曲线。(d)2.5mm缝宽的漏失曲线。
具体实施方式
下面将结合实例对本发明的具体实施方式进行清楚、完整地描述,显然,所描述的实例仅仅是本发明一部分实施例,而不是全部的实施例。
下面结合实施例对本发明作进一步描述:
下述实施例中,若未特别说明,所述的操作为本领域常规操作。
下述实施例中,若未特别说明,所采用的原料均能通过常规商业途径获得。
实施例1
柔性微凝胶的制备:取72g丙烯酸加水使其溶解,随后滴加66ml的氢氧化钠溶液,该氢氧化钠溶液的浓度为9mol/L,再依次加入71g丙烯酰胺、0.077gN,N'-亚甲基双丙烯酰胺、1.6g木质素硫酸镁和1.08g过硫酸钾,加水使得溶液体积为660ml,将其依次在50~60℃、60~70℃、70~80℃反应2~3h,反应结束后,将反应产物取出并进行切片,将切片后的产物用无水乙醇浸泡10h,然后取出产物,将其置于真空干燥箱中,在50℃条件下干燥,随后对其进行粉碎、过筛,取60~100目的颗粒即可。
竞争交联型高密度抗盐固化水微凝胶暂堵剂的制备:取65g磷酸盐类化合物加入水中并溶解,后加入4g柔性微凝胶并搅拌30min,最后加入5g的乌洛托品搅拌均匀并加入水使得整个溶液重量为100g并搅拌均匀即得;其中,磷酸盐类化合物由质量比为3:3:55的磷酸氢二钾、七水磷酸钾和焦磷酸钾组成,最终溶液密度可达1.8g/cm3。
实施例2
柔性微凝胶的制备方法和实施例1相同。
竞争交联型高密度抗盐固化水微凝胶暂堵剂的制备:取51g焦磷酸钾加入水中并溶解,后加入7g柔性微凝胶并搅拌30min;取1.5g聚乙烯亚胺粘稠液,缓慢加入7.5g聚乙烯亚胺稀溶液搅拌均匀并加入水使得整个溶液重量为100g并搅拌均匀即得,最终溶液密度可达1.6g/cm3。
为了进一步说明本发明实施例的效果,下面对其进行性能测试。
实施例3
柔性微凝胶的制备方法和实施例1相同。
按照图1制备不同密度焦磷酸钾溶液,按照表1不同密度盐溶液对应的浓度范围加入柔性微凝胶,搅拌30min后,再加入0~6.7%的聚乙烯亚胺溶液,制备1.1~1.8g/cm3的不同密度体系样品,密封后在180℃下老化24h后,采用目测代码法评价体系固化及强度性能。结果如表1所示。
表1不同密度抗盐固化水微凝胶体系固化与强度性能
从表1可以看出,对于含柔性微凝胶的磷酸盐溶液,在没有交联剂的情况下,任何密度的体系在180℃老化24小时后都不会固化,在相同条件下,1.1~1.4g/cm3密度范围内体系中添加2.5%~10%交联剂同样不能固化,强度代码在C~D范围。相比之下,在1.5~1.8g/cm3的体系加入交联剂后固化,强度代码在H~I范围。结果表明,抗盐固化水微凝胶暂堵剂在1.5~1.8g/cm3密度范围具有高强度,这是由于交联剂-磷酸盐与柔性微凝胶竞争交连的结果。
事实上,由于专利篇幅的限制,表2中仅表示出了柔性微凝胶浓度为4.0%时的固化情况,但是经过发明人的大量实验发现,当柔性微凝胶浓度为3.3%~4.7%、体系密度为1.5~1.8g/cm3的范围内时,最终都能够固化。
实施例4
柔性微凝胶及竞争交联型高密度抗盐固化水微凝胶暂堵剂的制备方法和实施例2相同。
将上述竞争交联型高密度抗盐固化水微凝胶暂堵剂对4.0mm和2.5mm缝宽岩心开展承压评价,实验结果如图2所示。在缝宽为4.0mm时,体系最大压力为0.29MPa,随后开始下降,但压力一直保持在0.2MPa以上。随着漏失量的增加,压力波动逐渐减小,压力主要维持在0.07~0.16MPa范围内,平均漏失约为7.82g/min。对于2.5mm的缝宽,体系在0.56MPa的压力下开始突破。相应的承压梯度为2.33MPa/m。虽然有漏失,但前30分钟压力基本在0.3MPa以上,之后压力继续波动下降。压力主要维持在0.04~0.39MPa范围内,平均漏失约为6.63g/min。与4mm的宽度相比,体系具有更高的承载力和更低的损耗。
表2归纳了传统凝胶暂堵剂的承压与防漏失性能。当常规聚合物凝胶在井筒中承受压力时,当压井液漏失后,凝胶很快就会失去承压能力。在短时间内,凝胶的压力大大降低,几乎无法恢复。相比之下,竞争交联型高密度抗盐固化水微凝胶暂堵剂在压井液损失后仍具有一定的承载力,且承载力在一定范围内稳定,说明其具有良好的动态暂堵和承压性能,这是其与传统凝胶在暂堵承压方面的最大区别。
表2本发明凝胶封堵剂和现有技术中的凝胶封堵剂的封堵情况
以上所述,仅是本发明的较佳实施例而已,并非对本发明作任何形式上的限制,虽然本发明已以较佳实施例揭露如上,然而并非用以限定本发明,任何熟悉本专业的技术人员,在不脱离本发明技术方案范围内,当可利用上述揭示的技术内容作出些许更动或修饰为等同变化的等效实施例,但凡是未脱离本发明技术方案的内容,依据本发明的技术实质对以上实施例所作的任何简单修改、等同变化与修饰,均仍属于本发明技术方案的范围内。
Claims (4)
1.一种竞争交联型高密度抗盐固化水微凝胶暂堵剂,其特征在于,按质量百分数,包括45%~64%的磷酸盐类化合物,3.3%~4.7%的固化剂,以及1.4%~6.7%的交联剂,其余为水;所述磷酸盐类化合物为磷酸氢二钾、七水磷酸钾、焦磷酸钾中的一种或多种,所述固化剂为柔性微凝胶,所述交联剂为所述柔性微凝胶的交联剂;
所述柔性微凝胶的制备方法如下:取丙烯酸,并将其中和度调节至50%~70%,再依次加入丙烯酰胺、N,N'-亚甲基双丙烯酰胺、木质素硫酸镁和过硫酸钾,将其依次在50~60℃、60~70℃、70~80℃反应2~3h,反应结束后对其进行分离、提纯、干燥、造粒即得;以摩尔比计,所述丙烯酸、丙烯酰胺、N,N'-亚甲基双丙烯酰胺和过硫酸钾的比例为1000:900~1100:0.4~0.6:3~5,且每加入1mol丙烯酸,需加入1.5~1.8g木质素磺酸镁。
2.根据权利要求1所述的竞争交联型高密度抗盐固化水微凝胶暂堵剂,其特征在于,所述交联剂为乌洛托品、聚乙烯亚胺中的至少一种。
3.根据权利要求1所述的竞争交联型高密度抗盐固化水微凝胶暂堵剂,其特征在于,所述柔性微凝胶的分离、提纯、干燥、造粒步骤具体为:将反应产物取出并切片,后用无水乙醇浸泡至少8h,取出产物,将其置于真空干燥箱中干燥,对其进行粉碎、过筛,选取60~100目的颗粒即得。
4.一种竞争交联型高密度抗盐固化水微凝胶暂堵剂的制备方法,其特征在于,包括以下步骤:取磷酸盐类化合物,将其加入水中溶解;加入柔性微凝胶,搅拌10~30min,加入交联剂溶液搅拌均匀即得。
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