CN105062455B - 一种水基压裂液稠化剂及其合成方法 - Google Patents
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Abstract
本发明属于化工领域,尤其涉及一种水基压裂液稠化剂及其合成方法。由下列物质按重量份数组成:丙烯酰胺,甲基丙烯酰胺,十一烯酸,2‑丙烯酰胺‑2‑甲基丙烷磺酸盐,甲基丙烯酰氧乙基三甲基氯化铵,甲基丙烯酸十二氟庚酯,乙烯基吡咯烷酮,改性玉米淀粉,引发剂和水。其合成方法:按照比例在去离子水中配置各种共聚单体及改性淀粉;调整溶液的PH值和温度;通入高纯氮气除氧;加入复合引发剂引发反应。本发明是一种易溶解、无污染、无伤害、携沙性能好、尤其是抗温、抗剪切携沙性能好的多官能团高分子聚合物,其主要特点是使用温度范围广、具有高的耐温、耐剪切性,具有高的携沙性和无残渣性,对储藏无伤害性等特性,可用作胍胶的优异替代品。
Description
技术领域
本发明属于化工领域,尤其涉及一种水基压裂液稠化剂及其合成方法。
背景技术
压裂技术是常规的增产技术。其目的是将储层压出裂缝,从而增产。压裂时所用的压裂液必须具有高的粘度、高的抗剪切性、高强的携沙性和破胶无残渣的环保性等特点。高的粘度以便其造缝,只有高的粘度才能使裂缝达到所需的宽度和深度。稠化剂作为水基压裂液的主剂,用以提高压裂液的粘度,降低压裂液滤失,悬浮和携带支撑剂。目前水基压裂液采用的稠化剂主要是天然植物胶及其衍生物,其中使用最多的羟丙基瓜胶。它们具有技术成熟、胶体稳定和货源充足的特点。但是据报道,通常使用的瓜胶压裂液体系不仅会在压开裂缝的表面形成滤饼,而且还会使部分残渣留在地层和裂缝中,造成二次伤害。在对压裂后由井中返排至地面的压裂液即返排液的分析后得出:压裂作业期间,返排出的压裂残液只占泵入井中的瓜胶压裂液的30%~50%,同时其具有配制工艺复杂、水不溶物含量高等缺点。
发明内容
针对以上瓜胶压裂液缺点,我们在原有合成聚合物的研究基础上通过科研攻关,开发了多官能团型聚合物为主体的新型聚合物清洁压裂液体系,合成的聚合物具有更好的粘温特性和抗剪切稳定性,增稠能力强、胶冻稳定性好、对细菌不敏感、低残渣,对地层造成的伤害小等传统合成聚合物压裂液的优点,而且在此基础上引入了含有疏水官能团、抗盐官能团,使得聚合物形成的基液,在交联剂的作用下,分子间疏水基团的疏水缔合作用增强,形成的交联体系具有显著的增粘性、耐盐性、抗剪切能力、长期稳定性;改善了压裂液体系延迟破胶、耐温性等缺陷,使压裂液体系温粘性可从30℃到180℃通用。
本发明的一个目的是提供一种应用于水基压裂中的聚合物稠化剂,该稠化剂具有试用度广阔、耐高温、耐剪切、耐盐、无残留等优点。 本发明的另一个目的合成上述聚合物稠化剂。 本发明的稠化剂是由多种乙烯基单体与其它天然改性材料根据水溶液聚合方法共聚而成。
所述乙烯基单体为非离子型单体、阴离子型单体、阳离子型单体、疏水型单体。
非离子型单体中,如丙烯酰胺、甲基丙烯酰胺。
阴离子型单体中,典型的离子型单体为不饱和羧酸,例如丙烯酸、甲基丙烯酸、十一烯酸、乙烯基磺酸、对乙烯苯磺酸和丙烯酰胺甲基丙烷磺酸(AMPS)及其他们的盐中的一种或多种。 阳离子单体的例子有,二甲基二烯丙基氯化铵、丙烯酰氧乙基三甲基氯化铵(DAC)、甲基丙烯酰氧乙基三甲基氯化铵(DMC)等。
疏水型单体为十六烷基二甲基烯丙基氯化铵、丙烯酸十八酯、甲基丙烯酸十二氟庚酯、乙烯基吡咯烷酮的一种或多种。
天然改性材料主要有玉米淀粉、纤维素、木质素、植物胶。
本发明提供如下技术方案,一种水基压裂液稠化剂,是由下列物质按重量份数组成:丙烯酰胺5~20份,甲基丙烯酰胺1~5份,十一烯酸1~5份, 2-丙烯酰胺-2-甲基丙烷磺酸盐10~50份,甲基丙烯酰氧乙基三甲基氯化铵1~5份,甲基丙烯酸十二氟庚酯0.1~5份,乙烯基吡咯烷酮0.5~5份,改性玉米淀粉5~10份,引发剂0.001~0.003份,水为40~60份。
所述引发剂为偶氮二异丁腈、硝酸铈铵和四甲基乙二胺的复合体系,三者的配比是10:3:3。
进一步地,是由下列物质按重量份数组成:丙烯酰胺5份,甲基丙烯酰胺1份,十一烯酸2.5份,2-丙烯酰胺-2-甲基丙烷磺酸盐30份,甲基丙烯酰氧乙基三甲基氯化铵2.5份,甲基丙烯酸十二氟庚酯2.5份,乙烯基吡咯烷酮1份,改性玉米淀粉10份,引发剂偶氮二异丁腈0.001份、硝酸铈铵0.0003份和四甲基乙二胺0.0003份,去离子水45.5份。
本发明用于一种水基压裂液稠化剂的合成方法,是通过下列步骤制得:
a.将10~50份2-丙烯酰胺-2-甲基丙烷磺酸盐,十一烯酸1~5份,甲基丙烯酰氧乙基三甲基氯化铵1~5份与水混合搅拌溶解10~20分钟;
b.在搅拌条件下,加入碱性调节剂或者酸性调节剂,将a步骤溶液的PH值调整为6~7,调节温度为14~16℃;
c.在b步骤得到的溶液中加入丙烯酰胺5~20份,甲基丙烯酰胺1~5份,甲基丙烯酸十二氟庚酯0.1~5份,乙烯基吡咯烷酮0.5~5份,改性玉米淀粉5~10份,搅拌溶解30~40分钟;
d.在c步骤得到的溶液中通入高纯氮气,除氧30~40分钟;
e.在氮气保护下,向d步骤得到的溶液中依次加入复合引发剂偶氮二异丁腈、硝酸铈铵和四甲基乙二胺,继续通氮气15~20分钟;
f.步骤e的溶液体系变粘发生聚合反应,停止通氮气,密闭封口反应4~6小时,体系的最终温度控制在85~95℃;
g.将反应完成的胶体破碎、烘干、造粒,得到稠化剂成品。
进一步地,所述步骤b中的碱性调节剂为氢氧化钠或者氨水。
进一步地,所述步骤b中的酸性调节剂为磷酸、盐酸或者己二酸。
本合成反应由于改性淀粉的加入,传统的过硫酸盐引发剂不能很好地引发乙烯基单体与淀粉的复杂体系,本发明采用硝酸铈铵作为初始一段引发剂,偶氮二异丁腈为高温二段引发剂,四甲基乙二胺为三段扩链引发剂的复合引发体系能很好地引发乙烯基单体与淀粉的复杂体系。
本发明的稠化剂适用于油田的水基压裂液,是一种易溶解、无污染、无伤害、携沙性能好、尤其是抗温、抗剪切携沙性能好的多官能团高分子聚合物,其主要特点是使用温度范围广、具有高的耐温、耐剪切性,具有高的携沙性和无残渣性,对储藏无伤害性等特性,可用作胍胶的优异替代品。
具体实施方式
实施例1
各单体与水的重量百分比为丙烯酰胺∶甲基丙烯酰胺:十一烯酸: AMPS∶DMC∶甲基丙烯酸十二氟庚酯∶乙烯基吡咯烷酮∶改性玉米淀粉:去离子水=5∶1∶2.5∶30∶2.5∶2.5∶1∶10:45.5。 (1)溶液的配制在1000ml烧杯中加入去离子水455g,加入AMPS单体300g,十一烯酸单体25g,DMC单体25g,搅拌溶解10分钟,在搅拌条件下缓慢加入中和剂(氢氧化钠)至PH6。再加入丙烯酰胺50g,甲基丙烯酰胺单体10g,甲基丙烯酸十二氟庚酯单体5g,乙烯基吡咯烷酮单体10g,改性玉米淀粉100g,搅拌溶解30分钟。
(2)溶液的调整调节PH值到6.0,调节温度14℃。 (3)溶液吹氮气除氧30分钟,在氮气保护下依次加入复合引发剂偶氮二异丁腈1g,硝酸铈铵 0.3g,四甲基乙二胺0.3g,继续吹氮气15分钟,体系溶液变粘发生反应,停止通氮,封口。继续反应5小时,终温为86度。 产品的后处理将已聚合好的胶体上喷洒白油进行表面后处理,然后造粒,烘干,粉碎成40目成品RX928。
通过对成品RX928进行检测得出:
(1)多官能团聚合物分子量425万;
(2)3‰溶液粘度30mps;
(3)在30℃、60℃、90℃、120℃、180℃条件下进行流变测试,得出在各种温度下,经过120分钟,170-1的剪切,产品的流变粘度均大于200mps;
(4)加入破胶剂后,破胶粘度小于5mps。
实施例2
各单体与水的重量百分比为丙烯酰胺∶甲基丙烯酰胺:十一烯酸: AMPS∶DMC∶甲基丙烯酸十二氟庚酯∶乙烯基吡咯烷酮∶改性玉米淀粉:去离子水=7∶1.5∶1.5∶35∶2∶2∶3∶8:40。 (1)溶液的配制在1000ml烧杯中加入去离子水400g,加入AMPS单体350g,十一烯酸单体15g,DMC单体20g,搅拌溶解10分钟,在搅拌条件下缓慢加入中和剂(氢氧化钠)至PH6。再加入丙烯酰胺70g,甲基丙烯酰胺单体15g,甲基丙烯酸十二氟庚酯单体20g,乙烯基吡咯烷酮单体30g,改性玉米淀粉80g,搅拌溶解30分钟。
(2)溶液的调整调节PH值到6.5,调节温度15℃。 (3)溶液吹氮气除氧30分钟,在氮气保护下依次加入复合引发剂偶氮二异丁腈0.625g,硝酸铈铵 0.188g,四甲基乙二胺0.188g,继续吹氮气15分钟,体系溶液变粘发生反应,停止通氮,封口。继续反应5小时,终温为88度。 产品的后处理将已聚合好的胶体上喷洒白油进行表面后处理,然后造粒,烘干,粉碎成40目成品RX928。
通过对成品RX928进行检测得出:
(1)多官能团聚合物分子量457万;
(2)3‰溶液粘度32mps;
(3)在30℃、60℃、90℃、120℃、180℃条件下进行流变测试,得出在各种温度下,经过120分钟,170-1的剪切,产品的流变粘度均大于200mps;
(4)加入破胶剂后,破胶粘度小于4.5mps。
实施例3
各单体与水的重量百分比为丙烯酰胺∶甲基丙烯酰胺:十一烯酸: AMPS∶DMC∶甲基丙烯酸十二氟庚酯∶乙烯基吡咯烷酮∶改性玉米淀粉:去离子水=10∶1∶1∶25∶3∶0.5∶0.5∶5:54。 (1)溶液的配制在1000ml烧杯中加入去离子水540g,加入AMPS单体250g,十一烯酸单体10g,DMC单体30g,搅拌溶解10分钟,在搅拌条件下缓慢加入中和剂(氢氧化钠)至PH7。再加入丙烯酰胺100g,甲基丙烯酰胺单体10g,甲基丙烯酸十二氟庚酯单体5g,乙烯基吡咯烷酮单体5g,改性玉米淀粉50g,搅拌溶解30分钟。
(2)溶液的调整调节PH值到7,调节温度16℃。 (3)溶液吹氮气除氧30分钟,在氮气保护下依次加入复合引发剂偶氮二异丁腈1.875g,硝酸铈铵 0.56g,四甲基乙二胺0.56g,继续吹氮气15分钟,体系溶液变粘发生反应,停止通氮,封口。继续反应5小时,终温为90度。产品的后处理将已聚合好的胶体上喷洒白油进行表面后处理,然后造粒,烘干,粉碎成40目成品RX928。
通过对成品RX928进行检测得出:
(1)多官能团聚合物分子量478万;
(2)3‰溶液粘度33.5mps;
(3)在30℃、60℃、90℃、120℃、180℃条件下进行流变测试,得出在各种温度下,经过120分钟,170-1的剪切,产品的流变粘度均大于200mps;
(4)加入破胶剂后,破胶粘度小于5mps。
Claims (4)
1.一种水基压裂液稠化剂,是由下列物质按重量份数组成:丙烯酰胺5~20份,甲基丙烯酰胺1~5份,十一烯酸1~5份, 2-丙烯酰胺-2-甲基丙烷磺酸盐10~50份,甲基丙烯酰氧乙基三甲基氯化铵1~5份,甲基丙烯酸十二氟庚酯0.1~5份,乙烯基吡咯烷酮0.5~5份,改性玉米淀粉5~10份,引发剂0.001~0.003份,水为40~60份;
所述引发剂为偶氮二异丁腈、硝酸铈铵和四甲基乙二胺的复合体系,三者的配比是10:3:3;
水基压裂液稠化剂按照以下步骤进行:
a.将 2-丙烯酰胺-2-甲基丙烷磺酸盐,十一烯酸,甲基丙烯酰氧乙基三甲基氯化铵与水混合搅拌溶解10~20分钟;
b.在搅拌条件下,加入碱性调节剂或者酸性调节剂,将a步骤溶液的p H值调整为6~7,调节温度为14~16℃;
c.在b步骤得到的溶液中加入丙烯酰胺,甲基丙烯酰胺,甲基丙烯酸十二氟庚酯,乙烯基吡咯烷酮,改性玉米淀粉,搅拌溶解30~40分钟;
d.在c步骤得到的溶液中通入高纯氮气,除氧30~40分钟;
e.在氮气保护下,向d步骤得到的溶液中依次加入引发剂,继续通氮气15~20分钟;
f.步骤e的溶液体系变粘发生聚合反应,停止通氮气,密闭封口反应4~6小时,体系的最终温度控制在85~95℃;
g.将反应完成的胶体破碎、烘干、造粒,得到稠化剂成品。
2.如权利要求1所述的一种水基压裂液稠化剂,是由下列物质按重量份数组成:丙烯酰胺5份,甲基丙烯酰胺1份,十一烯酸2.5份,2-丙烯酰胺-2-甲基丙烷磺酸盐30份,甲基丙烯酰氧乙基三甲基氯化铵2.5份,甲基丙烯酸十二氟庚酯2.5份,乙烯基吡咯烷酮1份,改性玉米淀粉10份,引发剂偶氮二异丁腈0.001份、硝酸铈铵0.0003份和四甲基乙二胺0.0003份,去离子水45.5份。
3.如权利要求1所述的一种水基压裂液稠化剂的合成方法,所述步骤b中的碱性调节剂为氢氧化钠或者氨水。
4.如权利要求1所述的一种水基压裂液稠化剂的合成方法,所述步骤b中的酸性调节剂为磷酸、盐酸或者己二酸。
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Denomination of invention: A water-based fracturing fluid thickener and its synthesis method Effective date of registration: 20231211 Granted publication date: 20180206 Pledgee: Yantai financing guarantee Group Co.,Ltd. Pledgor: YANTAI RUNXING ENVIRONMENTAL PROTECTION TECHNOLOGY DEVELOPMENT Co.,Ltd. Registration number: Y2023980070609 |