CN113912769A - 一种耐温耐盐凝胶泡沫体系及其制备方法和应用 - Google Patents
一种耐温耐盐凝胶泡沫体系及其制备方法和应用 Download PDFInfo
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Abstract
本发明公开了一种耐温耐盐凝胶泡沫体系及其制备方法和应用;该制备包括:(1)在保护气体存在下,将含苯环的双尾疏水单体、2‑丙烯酰胺‑2‑甲基丙磺酸单体、改性纳米SiO2、第一交联剂、第二交联剂、除氧剂、起泡剂、引发剂和水进行反应,得到反应液;(2)向所述反应液中通入气体,然后将气液混合物凝胶化,得到所述耐温耐盐凝胶泡沫体系。本发明相比于普通的凝胶泡沫体系,具有更强的耐温耐盐性能和很好的选择性堵水性能,应用于石油工业开发环节中,能实现有效增产的目的。
Description
技术领域
本发明属于油田化学技术领域,更具体地,涉及一种耐温耐盐凝胶泡沫体系及其制备方法和应用。
背景技术
凝胶泡沫是一种气体均匀分散在凝胶中的分散体系,具有高渗透层选择性强、封堵性能强、用液量少、价格低廉、机械强度较好、滤失量小、效率高及对储层伤害低的优势,具有剪切稳定性能与热稳定性能较高的特点,现已得到广泛的室内研究和矿场试验。在油田的实际生产中,凝胶泡沫体系采用的凝胶体系一般为聚丙烯酰胺类聚合物及其衍生物,但其在高温高盐油藏中易发生热降解、剪切降解及氧化降解等,导致其黏度急剧下降,在实际应用中暴露出许多不足,从而限制了其在堵水技术上的应用。因此,常采用在聚丙烯酰胺类聚合物上引入耐温耐盐单体的形式来增强其耐温耐盐性能,例如引入磺酸基团、2-丙烯酰胺-2-甲基丙磺酸(AMPS)和N-乙烯基吡咯烷酮(NVP)等,但实际耐温效果都不理想,在较高温度仍易降解脱水,热稳定性差,且强度不高。
专利CN104342095B公开了一种自生气可膨胀泡沫冻胶及其制备方法与应用,所述自生气可膨胀泡沫冻胶,在水中的质量百分比组成为聚丙烯酰胺0.4~0.6wt%,交联剂Na2Cr2O7 0.4~0.6wt%和Na2SO3 0.5~0.7wt%,生热剂NH4Cl 1mol/L和NaNO2 1mol/L;用盐酸调溶液的pH值为6.5~7、在20~50℃下形成泡沫冻胶。该发明的泡沫冻胶在pH为6.5~7时性能最佳,成胶时间在20h~90h可控。但是该反应生成的泡沫冻胶耐温性差,并且NaNO2属于有毒物质,控制不好用量会对地层造成污染和伤害。
专利申请CN105461860A公开了一种耐温耐盐生物聚合物凝胶调剖剂的制备方法,包括如下步骤:将大分子生物胶溶于蒸馏水配置成0.05~5%的溶液,向溶液中分别加入占反应体系质量分数为5~15%的单体丙烯酰胺、0.1~5%的单体2-丙烯酰胺-2-甲基丙磺酸和0.01~1%的交联剂,通入氮气隔绝空气,然后加入占反应体系质量分数为0.05~1%的引发剂,并在温度为40~100℃下恒温反应制得调剖剂。但是该方法合成的凝胶耐温耐盐性不强,且堵水效果一般。
综上所述,凝胶泡沫体系作为一种有着广泛应用前景的体系,却因其较差的耐温性和耐盐性而应用受限,因此研发出一种耐高温耐盐的凝胶泡沫体系,仍是本领域有待解决的问题之一。
发明内容
本发明的目的是针对目前油气开发中用到的凝胶泡沫体系耐温耐盐性能差的问题,提供一种耐温耐盐凝胶泡沫体系及其制备方法,使得制备的凝胶泡沫体系具有良好的耐温耐盐性。
为了实现上述目的,本发明的第一方面提供一种耐温耐盐凝胶泡沫体系的制备方法,该制备包括:
(1)在保护气体存在下,将含苯环的双尾疏水单体、2-丙烯酰胺-2-甲基丙磺酸单体、改性纳米SiO2、第一交联剂、第二交联剂、除氧剂、起泡剂、引发剂和水进行反应,得到反应液;
(2)向所述反应液中通入气体,然后将气液混合物凝胶化,得到所述耐温耐盐凝胶泡沫体系。
优选地,所述含苯环的双尾疏水单体由如下方法制得:
(1)在第一有机溶剂和催化剂的存在下,将丙烯酸类衍生物和氯化亚砜进行接触反应,得到丙烯酸类衍生物酰氯;
(2)在保护气体和第二有机溶剂的存在下,将芳香胺和溴代烷烃进行接触反应,得到胺盐中间体;
(3)在第三有机溶剂的存在下,将所述胺盐中间体和所述丙烯酸类衍生物酰氯进行接触反应,得到所述含苯环的双尾疏水单体。
优选地,步骤(1)中,所述丙烯酸类衍生物为3-(2-噻吩基)丙烯酸、3-(4-吡啶基)丙烯酸、丙烯酸、2-苯基丙烯酸、2-噻吩丙烯酸和α-甲基丙烯酸中的至少一种;
所述第一有机溶剂为氯仿;
所述催化剂为N,N-二甲基甲酰胺,所述催化剂的用量为丙烯酰胺类衍生物的用量的0.9~10wt%;
所述氯化亚砜和丙烯酸类衍生物的摩尔比为1.02~1.1:1;
所述接触反应的温度为0~10℃,时间为10~16h;
步骤(2)中,所述芳香胺为N-甲基-2-苯乙胺、β-苯乙胺、3-甲氧基苯乙胺、2-(3-氯苯基)乙胺和(S)-(-)-N,α-二甲基苯甲基胺中的至少一种;
所述溴代烷烃为溴代十六烷、1-溴二十烷、1-溴二十二烷和1-溴十八烷中的至少一种;
所述第二有机溶剂为氯仿;
所述接触反应的温度为75~85℃,时间为6~12h;
所述芳香胺和溴代烷与步骤(1)中的丙烯酸类衍生物的摩尔比均为1.6~1.8:1;
步骤(3)中,所述接触反应的温度为20~30℃,时间为4~10h;
所述胺盐中间体和所述丙烯酸类衍生物酰氯的摩尔比为1.1~1.5:1;
所述第三有机溶剂为氯仿。
优选地,所述改性纳米SiO2由如下方法制得:在保护气体和溶剂存在下,将纳米SiO2和硅烷偶联剂进行接触反应,得到所述改性纳米SiO2。
优选地,所述溶剂为无水乙醇和水;所述接触反应的温度为60~70℃,时间为0.5~2h;
所述纳米SiO2的平均粒径为15~30nm;所述硅烷偶联剂为3-氨基丙基三乙氧基硅烷;
所述纳米SiO2和硅烷偶联剂的料液比为1g:(40-60)ml。
优选地,所述第一交联剂为酚类交联剂,所述酚类交联剂为苯酚、邻苯二酚、间苯二酚和对苯二酚中的至少一种;
所述第二交联剂为醛类交联剂和/或六亚甲基四胺,所述醛类交联剂为甲醛和/或多聚甲醛;
所述除氧剂为亚硫酸钠、亚硫酸钾和硫代硫酸钠中的至少一种;
所述起泡剂为烷基苯磺酸盐、α-烯烃磺酸盐、烷基二苯磺醚二磺酸盐和脂肪酸聚氧乙烯酯中的至少一种;
所述引发剂为Na2SO3和/或K2S2O8。
优选地,步骤(1)中,所述保护气体为氮气;
以步骤(1)的反应所用各原料的总重量计,所述含苯环的双尾疏水单体的用量为0.4~0.8wt%、2-丙烯酰胺-2-甲基丙磺酸单体的用量为0.4~0.8wt%、改性纳米SiO2的用量为0.1~0.6wt%、第一交联剂的用量为0.3%~0.7wt%、第二交联剂的用量为0.3~0.7wt%、除氧剂的用量为0.2~0.5wt%、起泡剂的用量为0.1~0.5wt%、引发剂的用量为0.2~0.4wt%,余量为水;
所述反应的温度为70~90℃,时间为0.5~2h;
步骤(2)中,所述气体为氮气;所述气液混合物的气液体积比为30~60:1;
所述凝胶化的温度为120~160℃。
优选地,步骤(1)中,所述含苯环的双尾疏水单体的用量为0.5~0.6wt wt%、所述改性纳米SiO2的用量为0.1~0.3wt%、第一交联剂的用量为0.4~0.5wt%、第二交联剂的用量为0.4~0.5wt%、除氧剂的用量为0.3~0.4wt%。
本发明的第二方面提供上述制备方法制备的耐温耐盐凝胶泡沫体系。
本发明的第三方面提供上述耐温耐盐凝胶泡沫体系作为油藏堵水剂的应用。
本发明的技术方案具有如下有益效果:
(1)本发明提供的耐温耐盐凝胶泡沫体系,其耐温耐盐凝胶的聚合物主剂部分为含有苯环结构的双尾疏水单体缔合聚合物,在疏水单体中引入刚性的苯环,聚合物的热稳定性得到显著提高。另外,聚合物的疏水能力也会因苯环的引入而得到显著提高,聚合物溶液的黏度也相应提高。由于苯环体积较大,增加了疏水链的刚性,疏水链舒展,有利于分子间的缔合同时引入长链烷基,可以进一步提高聚合物的疏水缔合效果,增强聚合物的耐温耐盐性能。对于加入的改性纳米SiO2来说,在其表面引入的-NH2活性基团,不仅可以减少SiO2团聚现象,还可提高纳米SiO2与聚合物相容性,从而使聚合物凝胶的强度得到提高,并且对聚合物凝胶的耐温耐盐性能也有提升。
(2)本发明的耐温耐盐凝胶泡沫体系可广泛用于石油工业的各个工艺环节,例如酸化、压裂、调剖等方面;本发明的耐温耐盐凝胶泡沫体系堵水选择性强,起泡剂易溶于油,不形成泡沫,不堵塞油流通道,但在水相形成的泡沫稳定,堵塞水流通道,显著降低水的渗流能力,进而使得本发明的凝胶泡沫体系具有良好的堵水性;本发明的耐温耐盐凝胶泡沫体系中含有的起泡剂为表面活性剂,能够降低油水界面张力,提高洗油效率,提高原油采收率。
本发明的其它特征和优点将在随后具体实施方式部分予以详细说明。
附图说明
通过结合附图对本发明示例性实施方式进行更详细的描述,本发明的上述以及其它目的、特征和优势将变得更加明显,其中,在本发明示例性实施方式中,相同的参考标号通常代表相同部件。
图1示出了根据本发明的实施例1的凝胶泡沫体系的实物图。
具体实施方式
下面将更详细地描述本发明的优选实施方式。虽然以下描述了本发明的优选实施方式,然而应该理解,可以以各种形式实现本发明而不应被这里阐述的实施方式所限制。相反,提供这些实施方式是为了使本发明更加透彻和完整,并且能够将本发明的范围完整地传达给本领域的技术人员。
本发明的第一方面提供一种耐温耐盐凝胶泡沫体系的制备方法,该制备包括:
(1)在保护气体存在下,将含苯环的双尾疏水单体、2-丙烯酰胺-2-甲基丙磺酸单体、改性纳米SiO2、第一交联剂、第二交联剂、除氧剂、起泡剂、引发剂和水进行反应,得到反应液;
(2)向所述反应液中通入气体,然后将气液混合物凝胶化,得到所述耐温耐盐凝胶泡沫体系。
本发明中,在疏水单体的疏水链中引入刚性的苯环,以此来提高聚合物的耐温性能,并在一定程度上可以抑制酰胺基的水解,提高聚合物的长期稳定性和疏水缔合性能,得到含苯环结构的双尾疏水单体;通过对纳米SiO2的表面进行修饰以改善其分散性能,不仅可以减少SiO2团聚现象,还可提高纳米二氧化硅与聚合物相容性。综合以上两种技术,将含苯环结构的双尾疏水单体、其它单体和改性纳米SiO2通过反应形成耐高温耐盐的聚合物,然后向聚合物内注入一定量气体,进行凝胶化,得到耐温耐盐的凝胶泡沫体系。
本发明,为了克服普通丙烯酰胺类聚合物耐温耐盐性能差的缺点,本发明通过合成含苯环结构的双尾疏水单体来向聚合物凝胶中引入刚性基团,增强其耐温耐盐性能。利用丙烯酰胺类化合物生产双尾疏水单体,不仅原料价格低廉、来源丰富,而且所得产品易制得、性能优良、环境相容性较好。
根据本发明,优选地,所述含苯环的双尾疏水单体由如下方法制得:
(1)在第一有机溶剂和催化剂的存在下,将丙烯酸类衍生物和氯化亚砜进行接触反应,得到丙烯酸类衍生物酰氯;
(2)在保护气体和第二有机溶剂的存在下,将芳香胺和溴代烷烃进行接触反应,得到胺盐中间体;
(3)在第三有机溶剂的存在下,将所述胺盐中间体和所述丙烯酸类衍生物酰氯进行接触反应,得到所述含苯环的双尾疏水单体。
根据本发明,优选地,步骤(1)中,所述丙烯酸类衍生物为3-(2-噻吩基)丙烯酸、3-(4-吡啶基)丙烯酸、丙烯酸、2-苯基丙烯酸、2-噻吩丙烯酸和α-甲基丙烯酸中的至少一种;
所述第一有机溶剂为氯仿;
所述催化剂为N,N-二甲基甲酰胺,所述催化剂的用量为丙烯酰胺类衍生物的用量的0.9~10wt%,优选为0.9~3wt%;
本发明,优选先将丙烯酸类衍生物溶解在第一有机溶剂中,然后加入催化剂,在低温条件下搅拌使其混合均匀;所述低温条件为0~15℃,优选为0~10℃。
所述氯化亚砜和丙烯酸类衍生物的摩尔比为1.02~1.1:1;
所述接触反应的温度为0~10℃,时间为10~16h,优选为12~14h;
步骤(2)中,所述芳香胺为N-甲基-2-苯乙胺、β-苯乙胺、3-甲氧基苯乙胺、2-(3-氯苯基)乙胺和(S)-(-)-N,α-二甲基苯甲基胺中的至少一种;
所述溴代烷烃为溴代十六烷、1-溴二十烷、1-溴二十二烷和1-溴十八烷中的至少一种;
所述第二有机溶剂为氯仿;
所述接触反应的温度为75~85℃,时间为6~12h,优选为8~12h;
所述芳香胺和溴代烷与步骤(1)中的丙烯酸类衍生物的摩尔比均为1.6~1.8:1;
本发明中,优选地,所述芳香胺和溴代烷烃的接触反应结束后,冷却后得到固化的胺盐,将胺盐置于烧杯中,加入一定量的KOH溶液,用氯仿萃取,在分液漏斗中静置分层,上层为无色溶液,下层为黄色液体,将下层液体旋蒸除去溶剂,得到的液体再用氯仿重结晶,干燥后得到胺盐中间体。其中,所述KOH溶液的质量浓度为30%~40%,用量为大于芳香胺和溴代烷烃的体积和。
步骤(3)中,所述接触反应的温度为20~30℃,时间为4~10h,优选为6~10h;
所述胺盐中间体和所述丙烯酸类衍生物酰氯的摩尔比为1.1~1.5:1,优选为1.1~1.3:1;
所述第三有机溶剂为氯仿。
根据本发明,优选地,所述改性纳米SiO2由如下方法制得:在保护气体和溶剂存在下,将纳米SiO2和硅烷偶联剂进行接触反应,得到所述改性纳米SiO2。
根据本发明,优选地,所述溶剂为无水乙醇和水;所述接触反应的温度为60~70℃,时间为0.5~2h;
所述纳米SiO2的平均粒径为15~30nm;所述硅烷偶联剂为3-氨基丙基三乙氧基硅烷;
所述纳米SiO2和硅烷偶联剂的料液比为1g:(40-60)ml。
根据本发明,优选地,所述第一交联剂为酚类交联剂,所述酚类交联剂为苯酚、邻苯二酚、间苯二酚和对苯二酚中的至少一种;
所述第二交联剂为醛类交联剂和/或六亚甲基四胺,所述醛类交联剂为甲醛和/或多聚甲醛;
所述除氧剂为亚硫酸钠、亚硫酸钾和硫代硫酸钠中的至少一种;
所述起泡剂为烷基苯磺酸盐、α-烯烃磺酸盐、烷基二苯磺醚二磺酸盐和脂肪酸聚氧乙烯酯中的至少一种;
所述引发剂为Na2SO3和/或K2S2O8。
根据本发明,优选地,步骤(1)中,所述保护气体为氮气;
以步骤(1)的反应所用各原料的总重量计,所述含苯环的双尾疏水单体的用量为0.4~0.8wt%、2-丙烯酰胺-2-甲基丙磺酸单体的用量为0.4~0.8wt%、改性纳米SiO2的用量为0.1~0.6wt%、第一交联剂的用量为0.3%~0.7wt%、第二交联剂的用量为0.3~0.7wt%、除氧剂的用量为0.2~0.5wt%、起泡剂的用量为0.1~0.5wt%、引发剂的用量为0.2~0.4wt%,余量为水;
所述反应的温度为70~90℃,时间为0.5~2h;
步骤(2)中,所述气体为氮气;所述气液混合物的气液体积比为30~60:1;
所述凝胶化的温度为120~160℃。
根据本发明,优选地,步骤(1)中,所述含苯环的双尾疏水单体的用量为0.5~0.6wt wt%、所述改性纳米SiO2的用量为0.1~0.3wt%、第一交联剂的用量为0.4~0.5wt%、第二交联剂的用量为0.4~0.5wt%、除氧剂的用量为0.3~0.4wt%。
本发明的第二方面提供上述制备方法制备的耐温耐盐凝胶泡沫体系。
本发明的第三方面提供上述耐温耐盐凝胶泡沫体系作为油藏堵水剂的应用。
以下通过实施例进一步说明本发明:
以下各实施例和对比例所用的硅烷偶联剂均为3-氨基丙基三乙氧基硅烷;纳米SiO2的平均粒径为15nm;α-烯烃磺酸盐为α-烯烃磺酸钠;烷基二苯磺醚二磺酸盐为烷基二苯磺醚二磺酸钠;多聚甲醛购自国药集团化学试剂有限公司。
实施例1
1、含苯环的双尾疏水单体的合成
将3.73g的3-(2-噻吩基)丙烯酸溶解在20mL氯仿中,而后放入三口烧瓶中,加入0.035g的催化剂N,N-二甲基甲酰胺,在10℃低温条件下搅拌让其充分混合;然后用恒压滴液漏斗加入用20mL氯仿溶解的3.1g氯化亚砜,在10℃下,反应12h;反应结束后,旋转蒸发除去溶剂氯仿以及过量的氯化亚砜,得到无色透明的3-(2-噻吩基)丙烯酸酰氯。
在三口烧瓶中加入用10mL氯仿溶解的5.508g的N-甲基-2-苯乙胺,并向烧瓶中通氮气,升温至80℃,用恒压滴液漏斗加入用20mL氯仿溶解的14.73g的1-溴二十烷,滴加结束后,在80℃下,反应10h。反应结束,冷却后得到固化的胺盐。将胺盐置于烧杯中,加入20mL的质量浓度为30%的KOH水溶液,用氯仿萃取。在分液漏斗中静置分层,上层为无色溶液,下层为黄色液体。将下层液体旋蒸除去溶剂,得到的液体再用氯仿重结晶,干燥后得到胺盐中间体。
在三口烧瓶中加入用20mL氯仿溶解的上一步得到的全部中间体,在冰水浴中不停搅拌,用恒压滴液漏斗滴加溶有前一步得到的3-(2-噻吩基)丙烯酸酰氯的氯仿溶液(将上述步骤中制备的全部3-(2-噻吩基)丙烯酸酰氯溶解于20ml氯仿中),升温至室温25℃,反应8h。反应结束后,用Na2CO3溶液洗涤,分液,将有机层用蒸馏水洗至中性,再分液,将有机相旋蒸干燥,得到含苯环的双尾疏水单体。
2、改性纳米SiO2的合成
将0.2g纳米SiO2加入30ml无水乙醇和去离子水的混合溶液中(无水乙醇和去离子水的体积比为1:1),倒入三口烧瓶中,放入65℃的水浴锅中并通入氮气。一定时间后,倒入硅烷偶联剂的无水乙醇溶液20ml(其中,硅烷偶联剂与无水乙醇的体积比1:1),搅拌1h。在离心、超声波中用无水乙醇洗涤四次,最后烘干得到改性纳米SiO2。
3、耐温耐盐凝胶泡沫体系的制备
将含苯环的双尾疏水单体、2-丙烯酰胺-2-甲基丙磺酸单体、改性纳米SiO2、间苯二酚、六亚甲基四胺、硫代硫酸钠、α-烯烃磺酸盐和去离子水充分混合后,放入三口烧瓶中通入一定时间氮气,加入Na2SO3,在80℃条件下反应1h,得到反应液;其中,以步骤(1)的反应所用各原料的总重量计,所述含苯环的双尾疏水单体的用量为0.6wt%、2-丙烯酰胺-2-甲基丙磺酸单体的用量为0.6wt%、改性纳米SiO2的用量为0.2wt%、间苯二酚的用量为0.4wt%、六亚甲基四胺的用量为0.4wt%、硫代硫酸钠的用量为0.3wt%、α-烯烃磺酸盐的用量为0.3wt%、Na2SO3的用量为0.3wt%,余量为去离子水;
(2)然后按气液体积比60:1向所述反应液中通入氮气;而后将气液混合物倒入高压釜容器中,放在140℃恒温烘箱中成胶,得到耐温耐盐的凝胶泡沫体系(见图1)。
实施例2:
本实施例与实施例1的区别仅为将3.73g的3-(2-噻吩基)丙烯酸替换为2.08g的α-甲基丙烯酸,其它均同实施例1。
实施例3:
本实施例与实施例1的区别仅为将5.508g的N-甲基-2-苯乙胺替换为6.16g的3-甲氧基苯乙胺,其它均同实施例1。
实施例4:
本实施例与实施例1的区别仅为:以步骤(1)的反应所用各原料的总重量计,所述含苯环的双尾疏水单体的用量为0.7wt%、2-丙烯酰胺-2-甲基丙磺酸单体的用量为0.7wt%、改性纳米SiO2的用量为0.2wt%、间苯二酚的用量为0.4wt%、六亚甲基四胺的用量为0.4wt%、硫代硫酸钠的用量为0.4wt%、α-烯烃磺酸盐的用量为0.4wt%、Na2SO3的用量为0.3wt%,余量为去离子水;其它均同实施例1。
实施例5:
本实施例与实施例1的区别仅为将0.4wt%间苯二酚替换为0.4wt%苯酚,其它均同实施例1。
实施例6:
本实施例与实施例1的区别仅为将0.4wt%六亚甲基四胺替换为0.4wt%多聚甲醛,其它均同实施例1。
实施例7:
本实施例与实施例1的区别仅为将0.3wt%硫代硫酸钠替换为0.3wt%亚硫酸钾,其它均同实施例1。
实施例8:
本实施例与实施例1的区别仅为将0.3wt%α-烯烃磺酸盐替换为0.3wt%烷基二苯磺醚二磺酸盐,其它均同实施例1。
对比例1
本对比例提供一种凝胶泡沫体系,其与实施例1的区别仅为将0.6wt%的含苯环的双尾疏水单体替换为0.6wt%的α-甲基丙烯酸,其它均同实施例1。
对比例2
本对比例提供一种凝胶泡沫体系,其与实施例1的区别仅为将0.2wt%的改性纳米SiO2替换为0.2wt%的纳米SiO2,其它均同实施例1。
测试例1
通过室内实验,评价了实施例和对比例的制备的凝胶泡沫体系的热稳定性(脱水率计算为:从凝胶泡沫体系中脱出的水的质量与凝胶泡沫体系质量的比值),其结果见表1。
表1不同实施例和对比例的凝胶泡沫体系的热稳定性
产品编号 | 140℃条件下放置180天后的脱水率/% |
实施例1 | 4 |
实施例2 | 5 |
实施例3 | 8 |
实施例4 | 7 |
实施例5 | 12 |
实施例6 | 14 |
实施例7 | 5 |
实施例8 | 6 |
对比例1 | 52 |
对比例2 | 33 |
由表1可知,在引入含苯环的双尾疏水单体和改性纳米SiO2后,凝胶泡沫体系的脱水率大大减小,并且效果最好的是实施例1。
测试例2
通过室内实验,评价实施例和对比例的凝胶泡沫体系在高矿化度条件下的成胶稳定性。具体实施方式为:按照以上实施例和对比例的方法制备凝胶泡沫体系,仅是将原料去离子水替换为250000mg/L的氯化钠水溶液;然后观察新制备的凝胶泡沫体系的强度变化;结果见表2。
表2耐盐特性评价结果
由表2可知,矿化度对各实施例的凝胶体系的凝胶强度几乎没有影响,但是对比例的强度却明显下降,说明未引入含苯环的双尾疏水单体和改性纳米SiO2的凝胶体系耐盐性差。(注:C、D、E、F、G、H为采用Sydansk提出的GSC强度代码法所规定的凝胶强度等级,字母排序越靠后说明凝胶强度越大。)
测试例3
通过室内实验,评价实施例1所制得的耐温耐盐凝胶泡沫体系的选择性堵水效果和岩心突破压力,具体测试结果见表3和表4。其中堵剂封堵率和岩心突破压力测试方法为:1.所用岩心抽真空,饱和水,测定孔隙度,随后测定水相或油相渗透率;2.注入0.3PV凝胶泡沫体系;3.然后将岩心在140℃下加热24h,随后用水或油驱替岩心,下游出现第一滴液体时的入口压力为岩心突破压力,而后测试封堵后的水相或油相渗透率,计算封堵率;4.整个实验过程中,监测注入端压力变化,维持围压一直高于入口压力约3MPa。
表3堵剂封堵率性能评价
表4岩心突破压力结果
通过表3可知,实施例1凝胶泡沫体系对饱和水相岩心的封堵率大于94%,对饱和油相岩心的封堵率小于14%,说明其具有良好的堵水选择性;通过表4可知,凝胶泡沫体系堵剂对饱和水相突破压力高,对饱和油相岩心突破压力低,说明凝胶泡沫体系具有良好的堵水选择性。
以上已经描述了本发明的各实施例,上述说明是示例性的,并非穷尽性的,并且也不限于所披露的各实施例。在不偏离所说明的各实施例的范围和精神的情况下,对于本技术领域的普通技术人员来说许多修改和变更都是显而易见的。
Claims (10)
1.一种耐温耐盐凝胶泡沫体系的制备方法,其特征在于,该制备包括:
(1)在保护气体存在下,将含苯环的双尾疏水单体、2-丙烯酰胺-2-甲基丙磺酸单体、改性纳米SiO2、第一交联剂、第二交联剂、除氧剂、起泡剂、引发剂和水进行反应,得到反应液;
(2)向所述反应液中通入气体,然后将气液混合物凝胶化,得到所述耐温耐盐凝胶泡沫体系。
2.根据权利要求1所述的制备方法,其中,所述含苯环的双尾疏水单体由如下方法制得:
(1)在第一有机溶剂和催化剂的存在下,将丙烯酸类衍生物和氯化亚砜进行接触反应,得到丙烯酸类衍生物酰氯;
(2)在保护气体和第二有机溶剂的存在下,将芳香胺和溴代烷烃进行接触反应,得到胺盐中间体;
(3)在第三有机溶剂的存在下,将所述胺盐中间体和所述丙烯酸类衍生物酰氯进行接触反应,得到所述含苯环的双尾疏水单体。
3.根据权利要求2所述的制备方法,其中,步骤(1)中,所述丙烯酸类衍生物为3-(2-噻吩基)丙烯酸、3-(4-吡啶基)丙烯酸、2-苯基丙烯酸、2-噻吩丙烯酸和α-甲基丙烯酸中的至少一种;
所述第一有机溶剂为氯仿;
所述催化剂为N,N-二甲基甲酰胺,所述催化剂的用量为丙烯酰胺类衍生物的用量的0.9~10wt%;
所述氯化亚砜和丙烯酸类衍生物的摩尔比为1.02~1.1:1;
所述接触反应的温度为0~10℃,时间为10~16h;
步骤(2)中,所述芳香胺为N-甲基-2-苯乙胺、β-苯乙胺、3-甲氧基苯乙胺、2-(3-氯苯基)乙胺和(S)-(-)-N,α-二甲基苯甲基胺中的至少一种;
所述溴代烷烃为溴代十六烷、1-溴二十烷、1-溴二十二烷和1-溴十八烷中的至少一种;
所述第二有机溶剂为氯仿;
所述接触反应的温度为75~85℃,时间为6~12h;
所述芳香胺和溴代烷与步骤(1)中的丙烯酸类衍生物的摩尔比均为1.6~1.8:1;
步骤(3)中,所述接触反应的温度为20~30℃,时间为4~10h;
所述胺盐中间体和所述丙烯酸类衍生物酰氯的摩尔比为1.1~1.5:1;
所述第三有机溶剂为氯仿。
4.根据权利要求1所述的制备方法,其中,所述改性纳米SiO2由如下方法制得:在保护气体和溶剂存在下,将纳米SiO2和硅烷偶联剂进行接触反应,得到所述改性纳米SiO2。
5.根据权利要求4所述的制备方法,其中,所述溶剂为无水乙醇和水;所述接触反应的温度为60~70℃,时间为0.5~2h;
所述纳米SiO2的平均粒径为15~30nm;所述硅烷偶联剂为3-氨基丙基三乙氧基硅烷;
所述纳米SiO2和硅烷偶联剂的料液比为1g:(40-60)ml。
6.根据权利要求1所述的制备方法,其中,所述第一交联剂为酚类交联剂,所述酚类交联剂为苯酚、邻苯二酚、间苯二酚和对苯二酚中的至少一种;
所述第二交联剂为醛类交联剂和/或六亚甲基四胺,所述醛类交联剂为甲醛和/或多聚甲醛;
所述除氧剂为亚硫酸钠、亚硫酸钾和硫代硫酸钠中的至少一种;
所述起泡剂为烷基苯磺酸盐、α-烯烃磺酸盐、烷基二苯磺醚二磺酸盐和脂肪酸聚氧乙烯酯中的至少一种;
所述引发剂为Na2SO3和/或K2S2O8。
7.根据权利要求1所述的制备方法,其中,步骤(1)中,所述保护气体为氮气;
以步骤(1)的反应所用各原料的总重量计,所述含苯环的双尾疏水单体的用量为0.4~0.8wt%、2-丙烯酰胺-2-甲基丙磺酸单体的用量为0.4~0.8wt%、改性纳米SiO2的用量为0.1~0.6wt%、第一交联剂的用量为0.3%~0.7wt%、第二交联剂的用量为0.3~0.7wt%、除氧剂的用量为0.2~0.5wt%、起泡剂的用量为0.1~0.5wt%、引发剂的用量为0.2~0.4wt%,余量为水;
所述反应的温度为70~90℃,时间为0.5~2h;
步骤(2)中,所述气体为氮气;所述气液混合物的气液体积比为30~60:1;
所述凝胶化的温度为120~160℃。
8.根据权利要求1所述的制备方法,其中,步骤(1)中,所述含苯环的双尾疏水单体的用量为0.5~0.6wt wt%、所述改性纳米SiO2的用量为0.1~0.3wt%、第一交联剂的用量为0.4~0.5wt%、第二交联剂的用量为0.4~0.5wt%、除氧剂的用量为0.3~0.4wt%。
9.权利要求1-8中任意一项所述的制备方法制备的耐温耐盐凝胶泡沫体系。
10.权利要求9所述的耐温耐盐凝胶泡沫体系作为油藏堵水剂的应用。
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CN115093600A (zh) * | 2022-07-08 | 2022-09-23 | 中海石油(中国)有限公司 | 一种微泡/泡沫自交联自适应凝胶深部调驱体系及其应用 |
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