CN117285922A - 一体化变粘压裂液及其制备方法 - Google Patents
一体化变粘压裂液及其制备方法 Download PDFInfo
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- CN117285922A CN117285922A CN202311262904.7A CN202311262904A CN117285922A CN 117285922 A CN117285922 A CN 117285922A CN 202311262904 A CN202311262904 A CN 202311262904A CN 117285922 A CN117285922 A CN 117285922A
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- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims abstract description 30
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- C09K8/60—Compositions for stimulating production by acting on the underground formation
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- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
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- D06M13/244—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing sulfur or phosphorus
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- D06M13/322—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing nitrogen
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- E—FIXED CONSTRUCTIONS
- E21—EARTH OR ROCK DRILLING; MINING
- E21B—EARTH OR ROCK DRILLING; OBTAINING OIL, GAS, WATER, SOLUBLE OR MELTABLE MATERIALS OR A SLURRY OF MINERALS FROM WELLS
- E21B43/00—Methods or apparatus for obtaining oil, gas, water, soluble or meltable materials or a slurry of minerals from wells
- E21B43/25—Methods for stimulating production
- E21B43/26—Methods for stimulating production by forming crevices or fractures
- E21B43/267—Methods for stimulating production by forming crevices or fractures reinforcing fractures by propping
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- C09K2208/00—Aspects relating to compositions of drilling or well treatment fluids
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Abstract
本发明公开了一体化变粘压裂液及其制备方法,涉及石油开采技术领域。本发明利用丙烯酸、乙烯基甲基二甲氧基硅烷、磺胺噻唑化合物、硅烷改性四氧化三铁在石英砂表面交联形成磁性水凝胶,在压裂液溶剂中均匀悬浮,同时在外加磁场下,嵌入压裂缝,减少返排液带出损失;再利用4‑羧基苯磺酰氯、4‑甲基‑2‑氨基噻唑改性聚酯纤维,与改性石英砂形成双核铜配合物,协同高分子乳液中的季铵结构,防止压裂液腐烂变质,并且二者形成三维网状结构,协助压裂液悬浮支撑剂,提高压裂液的携砂能力。本发明调整高分子乳液、改性石英砂、改性纤维以及其他助剂的浓度,实现压裂液体系在滑溜水与胶液间的智能切换,进行多级变粘,到达各种排量下携砂的要求。
Description
技术领域
本发明涉及石油开采技术领域,具体为一体化变粘压裂液及其制备方法。
背景技术
在压裂过程中除稠化剂外还须配备其它助剂如粘土稳定剂、助排剂、高温稳定剂、防水锁剂等,以满足压裂液所需要的性能,从而保证施工顺利、减小油气层损害。随着“井工厂”,压裂“工业化”的不断推进,一体化压裂液体系也不断得以现场实施,通过对混砂车上稠化剂加量的优化,实现在不同的施工阶段采用不同粘度压裂液的目的,最终实现一体化压裂施工,可操作性强,降低施工的复杂性,并且降低施工成本。然而,现有的压裂液无法同时满足多个性能,例如:低粘压裂液减阻效果好,可以实现大排量,但携砂效果较差,不能满足高砂量的要求;交联冻胶液携砂效果好,但减阻效果差,不能实现大排量,改造范围小。
发明内容
本发明的目的在于提供一体化变粘压裂液及其制备方法,以解决现有技术中存在的问题。
为了解决上述技术问题,本发明提供如下技术方案:一种一体化变粘压裂液,所述一体化变粘压裂液包括高分子乳液、改性石英砂、改性纤维、DL-8助排剂、DYAS系列解水锁剂、过硫酸铵、水。
进一步的,所述高分子乳液由以下方法制得,将丙烯酰胺、1-乙基-环戊醇丙烯酸酯、N-(2-丙烯酰氨基乙基)三乙基碘化铵配置成水相,将油相和乳化剂混合后,加入水相,升温、通氮气,加入过硫酸铵,恒温反应得高分子乳液。
进一步的,所述油相为溶剂油D110、柴油、煤油的一种或多种混合;所述乳化剂包括失水山梨醇单硬脂酸酯、聚氧乙烯失水山梨醇单硬脂酸酯。
进一步的,所述改性石英砂由丙烯酸、乙烯基甲基二甲氧基硅烷、磺胺噻唑化合物、硅烷改性四氧化三铁、石英砂制得;
所述磺胺噻唑化合物由2-氨基噻唑、4-(3-丁烯-1-基)苯磺酰氯制得;
所述硅烷改性四氧化三铁由乙烯基甲基二甲氧基硅烷、四氧化三铁制得。
进一步的,所述改性纤维由4-羧基苯磺酰氯、聚酯纤维、4-甲基-2-氨基噻唑制得。
进一步的,一种一体化变粘压裂液的制备方法,包括以下制备步骤:
(1)将丙烯酰胺、1-乙基-环戊醇丙烯酸酯、N-(2-丙烯酰氨基乙基)三乙基碘化铵、去离子水按质量比1:0.1~0.3:0.1~0.3:8~10混合,搅拌溶解过后,加入丙烯酰胺质量0.0001~0.001倍的尿素、丙烯酰胺质量0.0008~0.002倍的乙二胺四乙酸二钠,100rpm搅拌20~25min,加入氢氧化钠溶液至反应液pH为6.3~7.2,得水相;
(2)将油相、乳化剂按质量比8~20:1混合,乳化剂中失水山梨醇单硬脂酸酯、聚氧乙烯失水山梨醇单硬脂酸酯的质量比为3:7,300~500rpm下,加入油相质量1.1~2.3倍的水相,升温至40~60℃,以7L/min通入氮气20~35min,加入油相质量0.01~0.2倍的过硫酸铵,反应4~6h得高分子乳液;
(3)将丙烯酸、乙烯基甲基二甲氧基硅烷按质量比1:0.4~0.8混合,100~200rpm搅拌30min,加入丙烯酸质量0.1~0.3倍的硅烷改性四氧化三铁、丙烯酸质量0.2~0.4倍的磺胺噻唑化合物,得混合溶液;向混合溶液加入混合溶液质量0.3~0.6倍的石英砂、丙烯酸质量0.001~0.005倍的偶氮二异丁腈,混合均匀后,倒入聚乙烯密封袋中,把袋中的气泡赶尽,用玻璃片夹好,水平置于55~70℃的水浴中,恒温反应10~20h后,取出,按料液比1:20浸泡于蒸馏水中,浸泡24h,取出得改性石英砂;
(4)将改性纤维、改性石英砂、一水合乙酸铜、无水乙醇、去离子水、吡啶按质量比0.3~0.5:5~30:1.5~10:170~400:18~80:9~55混合,置于内衬聚四氟乙烯的不锈钢反应釜内,80~110℃反应4~6h后,过滤,取滤物,用蒸馏水洗涤5~8次后,30℃干燥6h得中间物B;
(5)向100重量份的去离子水加入0.1~1.6重量份高分子乳液,100~200rpm搅拌15min,加入0.3~0.5重量份DL-8助排剂、0.4~0.6重量份DYAS系列解水锁剂、0.01~0.03重量份过硫酸铵,继续搅拌3min,得混液,加入混液体积0.2~0.4倍的中间物B,得一体化变粘压裂液。
进一步的,步骤(3)所述硅烷改性四氧化三铁的制备方法为:将四氧化三铁、乙醇/水按料液比1:20~35混合,乙醇/水中无水乙醇和去离子水的体积比为1:1,氩气保护下,加入四氧化三铁质量0.05~0.3倍的乙烯基甲基二甲氧基硅烷,50~70℃、100~300rpm下搅拌反应60~80min后,抽滤,用无水乙醇洗涤3次,再用去离子水洗涤3次,60℃干燥6~9h。
进一步的,步骤(3)所述磺胺噻唑化合物的制备方法为:将2-氨基噻唑、吡啶、4-(3-丁烯-1-基)苯磺酰氯按质量比1:8~12:0.4~0.7混合,室温反应4~7h后,加入2-氨基噻唑质量40~50倍的乙酸乙酯,再依次用质量分数为10%柠檬酸水溶液、饱和氯化钠溶液洗涤3次,用无水硫酸镁干燥1~2h,过滤,真空度-0.06MPa、60℃下蒸馏5~8h。
进一步的,步骤(4)所述改性纤维的制备方法为:
a、将聚酯纤维按料液比1:10置于50g/L氢氧化钠溶液中,100~120℃下处理20min后,取出,用清水洗涤至洗液pH为7,40℃烘干10h,再置于大气低温等离子体设备中,空气气氛下,真空度50Pa、功率为100W下处理180~250s,得预处理聚酯纤维;
b、将预处理聚酯纤维按浴比1:30~50浸于4-羧基苯磺酰氯溶液,4-羧基苯磺酰氯溶液溶液中4-羧基苯磺酰氯、去离子水、过氧化苯甲酰的质量比为30~50:1000:1.1~2.7,60~80℃下反应2~4h,取出,40~50℃干燥5h得中间物A;
c、将4-甲基-2-氨基噻唑、吡啶、中间物A按质量比1:8~12:0.2~0.5混合,30~40℃反应3~4h后,取出,用乙酸乙酯洗涤6~8次,再分别用质量分数为10%柠檬酸水溶液、饱和氯化钠溶液洗涤3次,40℃干燥5h得改性纤维。
进一步的,所述压裂液的使用方法为:在人造裂缝处施加2~4T磁场,在井筒施加0.2~1.0T磁场,通过水力压裂车将压裂液输送进入人造裂缝。
与现有技术相比,本发明所达到的有益效果是:
本发明利用高分子乳液、改性石英砂、改性纤维制得压裂液,通过调整乳液浓度,实现压裂液体系在滑溜水与胶液间的智能切换,进行多级变粘,到达各种排量下携砂的要求。
本发明采用丙烯酰胺、1-乙基-环戊醇丙烯酸酯、N-(2-丙烯酰氨基乙基)三乙基碘化铵为水相,与溶剂油构建反相乳液体系,并在引发剂的作用下,水相聚合形成高分子乳液,高分子聚合物以丙烯酰胺为两端、以1-乙基-环戊醇丙烯酸酯和丙烯酸异戊酯为中间交联体,两端引入氨基,与压裂液的溶剂形成氢键作用,提高溶解性,在分子侧链引入较长的侧链和环状结构,具有高分子表面活性剂特征,增加压裂液粘度,还增加压裂液的耐温能力,使得压裂液在高温的深层油气井中,仍保持较好的粘性,同时,含有甲基等柔性基团,提高压裂液的降阻性;此外,引入季铵结构,抑制腐生菌等微生物生长,防止乳液腐烂变质,使压裂液长时间保持增粘性。
本发明利用2-氨基噻唑的氨基与4-(3-丁烯-1-基)苯磺酰氯的磺酰氯反应,形成磺胺噻唑化合物;接着,将丙烯酸、乙烯基甲基二甲氧基硅烷、磺胺噻唑化合物、乙烯基甲基二甲氧基硅烷改性四氧化三铁聚合交联,在石英砂表面形成磁性水凝胶,在压裂液溶剂中均匀悬浮,提高压裂液的携砂能力,同时在实际压裂工作中,施加磁场,磁场力推动支撑剂进入压裂缝中,由于水凝胶分子链中引入有机硅,降低表面张力,提高界面活性,加强在压裂缝中的渗吸作用,并且在水凝胶的弹性可变形能力的帮助下,支撑剂在压裂缝快速铺开,进一步嵌入其中,减少返排液带出损失。
本发明利用4-羧基苯磺酰氯的羧基接枝于聚酯纤维表面,4-甲基-2-氨基噻唑的氨基与4-羧基苯磺酰氯的磺酰氯反应,形成磺胺噻唑基团,获得改性纤维,在铜离子的交联作用下,改性纤维与改性石英砂形成双核铜配合物,从而使改性纤维与改性石英砂形成三维网状结构,协助压裂液悬浮支撑剂,提高压裂液的携砂能力,同时双核铜结构的存在,加强压裂液抗菌能力,提高压裂液保存时间;并且网状结构中引入较大键能的硅氧键,提高压裂液的热稳定性,此外,改性纤维、改性石英砂与溶剂、高分子乳液氢键连接,提高压裂液表观粘度和结构强度,形成可逆结构,从而提高压裂液抗温抗剪切性能。
具体实施方式
下面将结合本发明实施例,对本发明实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例仅仅是本发明一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例,都属于本发明保护的范围。
实施例
(1)将丙烯酰胺、1-乙基-环戊醇丙烯酸酯、N-(2-丙烯酰氨基乙基)三乙基碘化铵、去离子水按质量比1:0.1:0.1:8混合,搅拌溶解过后,加入丙烯酰胺质量0.0001倍的尿素、丙烯酰胺质量0.0008倍的乙二胺四乙酸二钠,100rpm搅拌20min,加入氢氧化钠溶液至反应液pH为6.3,得水相;
(2)将溶剂油D110、乳化剂按质量比8:1混合,乳化剂中失水山梨醇单硬脂酸酯、聚氧乙烯失水山梨醇单硬脂酸酯的质量比为3:7,300rpm下,加入溶剂油D110质量1.1倍的水相,升温至40℃,以7L/min通入氮气20min,加入溶剂油D110质量0.01倍的过硫酸铵,反应4h得高分子乳液;
(3)将四氧化三铁、乙醇/水按料液比1:20混合,乙醇/水中无水乙醇和去离子水的体积比为1:1,氩气保护下,加入四氧化三铁质量0.05倍的乙烯基甲基二甲氧基硅烷,50℃、100rpm下搅拌反应60min后,抽滤,用无水乙醇洗涤3次,再用去离子水洗涤3次,60℃干燥6h得硅烷改性四氧化三铁;
(4)将2-氨基噻唑、吡啶、4-(3-丁烯-1-基)苯磺酰氯按质量比1:8:0.4混合,室温反应4h后,加入2-氨基噻唑质量40倍的乙酸乙酯,再依次用质量分数为10%柠檬酸水溶液、饱和氯化钠溶液洗涤3次,用无水硫酸镁干燥1h,过滤,真空度-0.06MPa、60℃下蒸馏5h,得磺胺噻唑化合物;
(5)将丙烯酸、乙烯基甲基二甲氧基硅烷按质量比1:0.4混合,100rpm搅拌30min,加入丙烯酸质量0.1倍的硅烷改性四氧化三铁、丙烯酸质量0.2倍的磺胺噻唑化合物,得混合溶液;向混合溶液加入混合溶液质量0.3倍的石英砂、丙烯酸质量0.001倍的偶氮二异丁腈,混合均匀后,倒入聚乙烯密封袋中,把袋中的气泡赶尽,用玻璃片夹好,水平置于55℃的水浴中,恒温反应10h后,取出,按料液比1:20浸泡于蒸馏水中,浸泡24h,取出得改性石英砂;
(6)将聚酯纤维按料液比1:10置于50g/L氢氧化钠溶液中,100℃下处理20min后,取出,用清水洗涤至洗液pH为7,40℃烘干10h,再置于大气低温等离子体设备中,空气气氛下,真空度50Pa、功率为100W下处理180s,得预处理聚酯纤维;
(7)将预处理聚酯纤维按浴比1:30浸于4-羧基苯磺酰氯溶液,4-羧基苯磺酰氯溶液溶液中4-羧基苯磺酰氯、去离子水、过氧化苯甲酰的质量比为30:1000:1.1,60℃下反应2h,取出,40℃干燥5h得中间物A;
(8)将4-甲基-2-氨基噻唑、吡啶、中间物A按质量比1:8:0.2混合,30℃反应3h后,取出,用乙酸乙酯洗涤6次,再分别用质量分数为10%柠檬酸水溶液、饱和氯化钠溶液洗涤3次,40℃干燥5h得改性纤维;
(9)将改性纤维、改性石英砂、一水合乙酸铜、无水乙醇、去离子水、吡啶按质量比0.3:5:1.5:170:18:9混合,置于内衬聚四氟乙烯的不锈钢反应釜内,80℃反应4h后,过滤,取滤物,用蒸馏水洗涤5次后,30℃干燥6h得中间物B;
(10)向100重量份的去离子水加入0.1重量份高分子乳液,100rpm搅拌15min,加入0.3重量份DL-8助排剂、0.4重量份DYAS系列解水锁剂、0.01重量份过硫酸铵,继续搅拌3min,得混液,加入混液体积0.2倍的中间物B,得一体化变粘压裂液。
实施例
(1)将丙烯酰胺、1-乙基-环戊醇丙烯酸酯、N-(2-丙烯酰氨基乙基)三乙基碘化铵、去离子水按质量比1:0.2:0.2:9混合,搅拌溶解过后,加入丙烯酰胺质量0.00055倍的尿素、丙烯酰胺质量0.0014倍的乙二胺四乙酸二钠,100rpm搅拌22min,加入氢氧化钠溶液至反应液pH为6.8,得水相;
(2)将柴油、乳化剂按质量比14:1混合,乳化剂中失水山梨醇单硬脂酸酯、聚氧乙烯失水山梨醇单硬脂酸酯的质量比为3:7,400rpm下,加入柴油质量1.7倍的水相,升温至50℃,以7L/min通入氮气28min,加入柴油质量0.1倍的过硫酸铵,反应5h得高分子乳液;
(3)将四氧化三铁、乙醇/水按料液比1:27.5混合,乙醇/水中无水乙醇和去离子水的体积比为1:1,氩气保护下,加入四氧化三铁质量0.18倍的乙烯基甲基二甲氧基硅烷,60℃、200rpm下搅拌反应70min后,抽滤,用无水乙醇洗涤3次,再用去离子水洗涤3次,60℃干燥7.5h得硅烷改性四氧化三铁;
(4)将2-氨基噻唑、吡啶、4-(3-丁烯-1-基)苯磺酰氯按质量比1:10:0.55混合,室温反应5.5h后,加入2-氨基噻唑质量45倍的乙酸乙酯,再依次用质量分数为10%柠檬酸水溶液、饱和氯化钠溶液洗涤3次,用无水硫酸镁干燥1.5h,过滤,真空度-0.06MPa、60℃下蒸馏6.5h,得磺胺噻唑化合物;
(5)将丙烯酸、乙烯基甲基二甲氧基硅烷按质量比1:0.6混合,150rpm搅拌30min,加入丙烯酸质量0.2倍的硅烷改性四氧化三铁、丙烯酸质量0.3倍的磺胺噻唑化合物,得混合溶液;向混合溶液加入混合溶液质量0.45倍的石英砂、丙烯酸质量0.003倍的偶氮二异丁腈,混合均匀后,倒入聚乙烯密封袋中,把袋中的气泡赶尽,用玻璃片夹好,水平置于63℃的水浴中,恒温反应15h后,取出,按料液比1:20浸泡于蒸馏水中,浸泡24h,取出得改性石英砂;
(6)将聚酯纤维按料液比1:10置于50g/L氢氧化钠溶液中,110℃下处理20min后,取出,用清水洗涤至洗液pH为7,40℃烘干10h,再置于大气低温等离子体设备中,空气气氛下,真空度50Pa、功率为100W下处理215s,得预处理聚酯纤维;
(7)将预处理聚酯纤维按浴比1:40浸于4-羧基苯磺酰氯溶液,4-羧基苯磺酰氯溶液溶液中4-羧基苯磺酰氯、去离子水、过氧化苯甲酰的质量比为40:1000:1.9,70℃下反应3h,取出,45℃干燥5h得中间物A;
(8)将4-甲基-2-氨基噻唑、吡啶、中间物A按质量比1:10:0.35混合,35℃反应3.5h后,取出,用乙酸乙酯洗涤7次,再分别用质量分数为10%柠檬酸水溶液、饱和氯化钠溶液洗涤3次,40℃干燥5h得改性纤维;
(9)将改性纤维、改性石英砂、一水合乙酸铜、无水乙醇、去离子水、吡啶按质量比0.4:17.5:5.8:285:49:32混合,置于内衬聚四氟乙烯的不锈钢反应釜内,95℃反应5h后,过滤,取滤物,用蒸馏水洗涤6次后,30℃干燥6h得中间物B;
(10)向100重量份的去离子水加入0.7重量份高分子乳液,150rpm搅拌15min,加入0.4重量份DL-8助排剂、0.5重量份DYAS系列解水锁剂、0.02重量份过硫酸铵,继续搅拌3min,得混液,加入混液体积0.3倍的中间物B,得一体化变粘压裂液。
实施例
(1)将丙烯酰胺、1-乙基-环戊醇丙烯酸酯、N-(2-丙烯酰氨基乙基)三乙基碘化铵、去离子水按质量比1:0.3:0.3:10混合,搅拌溶解过后,加入丙烯酰胺质量0.001倍的尿素、丙烯酰胺质量0.002倍的乙二胺四乙酸二钠,100rpm搅拌25min,加入氢氧化钠溶液至反应液pH为7.2,得水相;
(2)将煤油、乳化剂按质量比20:1混合,乳化剂中失水山梨醇单硬脂酸酯、聚氧乙烯失水山梨醇单硬脂酸酯的质量比为3:7,500rpm下,加入煤油质量2.3倍的水相,升温至60℃,以7L/min通入氮气35min,加入煤油质量0.2倍的过硫酸铵,反应6h得高分子乳液;
(3)将四氧化三铁、乙醇/水按料液比1:35混合,乙醇/水中无水乙醇和去离子水的体积比为1:1,氩气保护下,加入四氧化三铁质量0.3倍的乙烯基甲基二甲氧基硅烷,70℃、300rpm下搅拌反应80min后,抽滤,用无水乙醇洗涤3次,再用去离子水洗涤3次,60℃干燥9h得硅烷改性四氧化三铁;
(4)将2-氨基噻唑、吡啶、4-(3-丁烯-1-基)苯磺酰氯按质量比1:12:0.7混合,室温反应7h后,加入2-氨基噻唑质量50倍的乙酸乙酯,再依次用质量分数为10%柠檬酸水溶液、饱和氯化钠溶液洗涤3次,用无水硫酸镁干燥2h,过滤,真空度-0.06MPa、60℃下蒸馏8h,得磺胺噻唑化合物;
(5)将丙烯酸、乙烯基甲基二甲氧基硅烷按质量比1:0.8混合,200rpm搅拌30min,加入丙烯酸质量0.3倍的硅烷改性四氧化三铁、丙烯酸质量0.4倍的磺胺噻唑化合物,得混合溶液;向混合溶液加入混合溶液质量0.6倍的石英砂、丙烯酸质量0.005倍的偶氮二异丁腈,混合均匀后,倒入聚乙烯密封袋中,把袋中的气泡赶尽,用玻璃片夹好,水平置于70℃的水浴中,恒温反应20h后,取出,按料液比1:20浸泡于蒸馏水中,浸泡24h,取出得改性石英砂;
(6)将聚酯纤维按料液比1:10置于50g/L氢氧化钠溶液中,120℃下处理20min后,取出,用清水洗涤至洗液pH为7,40℃烘干10h,再置于大气低温等离子体设备中,空气气氛下,真空度50Pa、功率为100W下处理250s,得预处理聚酯纤维;
(7)将预处理聚酯纤维按浴比1:50浸于4-羧基苯磺酰氯溶液,4-羧基苯磺酰氯溶液溶液中4-羧基苯磺酰氯、去离子水、过氧化苯甲酰的质量比为50:1000:2.7,80℃下反应4h,取出,50℃干燥5h得中间物A;
(8)将4-甲基-2-氨基噻唑、吡啶、中间物A按质量比1:12:0.5混合,40℃反应4h后,取出,用乙酸乙酯洗涤8次,再分别用质量分数为10%柠檬酸水溶液、饱和氯化钠溶液洗涤3次,40℃干燥5h得改性纤维;
(9)将改性纤维、改性石英砂、一水合乙酸铜、无水乙醇、去离子水、吡啶按质量比0.5:30:10:400:80:55混合,置于内衬聚四氟乙烯的不锈钢反应釜内,110℃反应6h后,过滤,取滤物,用蒸馏水洗涤8次后,30℃干燥6h得中间物B;
(10)向100重量份的去离子水加入1.6重量份高分子乳液,200rpm搅拌15min,加入0.5重量份DL-8助排剂、0.6重量份DYAS系列解水锁剂、0.03重量份过硫酸铵,继续搅拌3min,得混液,加入混液体积0.4倍的中间物B,得一体化变粘压裂液。
对比例1
对比例1与实施例2的区别在于步骤(1)的不同,将步骤(1)改为:将丙烯酰胺、N-(2-丙烯酰氨基乙基)三乙基碘化铵、去离子水按质量比1:0.2:9混合,搅拌溶解过后,加入丙烯酰胺质量0.00055倍的尿素、丙烯酰胺质量0.0014倍的乙二胺四乙酸二钠,100rpm搅拌22min,加入氢氧化钠溶液至反应液pH为6.8,得水相。其余步骤同实施例2。
对比例2
对比例2与实施例2的区别在于步骤(1)的不同,将步骤(1)改为:将丙烯酰胺、1-乙基-环戊醇丙烯酸酯、去离子水按质量比1:0.2:9混合,搅拌溶解过后,加入丙烯酰胺质量0.00055倍的尿素、丙烯酰胺质量0.0014倍的乙二胺四乙酸二钠,100rpm搅拌22min,加入氢氧化钠溶液至反应液pH为6.8,得水相。其余步骤同实施例2。
对比例3
对比例3与实施例2的区别在于无步骤(4),步骤(5)改为:将丙烯酸、乙烯基甲基二甲氧基硅烷按质量比1:0.6混合,150rpm搅拌30min,加入丙烯酸质量0.2倍的硅烷改性四氧化三铁,得混合溶液;向混合溶液加入混合溶液质量0.45倍的石英砂、丙烯酸质量0.003倍的偶氮二异丁腈,混合均匀后,倒入聚乙烯密封袋中,把袋中的气泡赶尽,用玻璃片夹好,水平置于63℃的水浴中,恒温反应15h后,取出,按料液比1:20浸泡于蒸馏水中,浸泡24h,取出得改性石英砂。其余步骤同实施例2。
对比例4
对比例4与实施例2的区别在于无步骤(3),步骤(5)改为:将丙烯酸、丙烯酸质量0.3倍的磺胺噻唑化合物,150rpm搅拌30min,得混合溶液;向混合溶液加入混合溶液质量0.45倍的石英砂、丙烯酸质量0.003倍的偶氮二异丁腈,混合均匀后,倒入聚乙烯密封袋中,把袋中的气泡赶尽,用玻璃片夹好,水平置于63℃的水浴中,恒温反应15h后,取出,按料液比1:20浸泡于蒸馏水中,浸泡24h,取出得改性石英砂。其余步骤同实施例2。
对比例5
对比例5与实施例2的区别在于无步骤(6)~(8),步骤(9)改为:将聚酯、改性石英砂、一水合乙酸铜、无水乙醇、去离子水、吡啶按质量比0.4:17.5:5.8:285:49:32混合,置于内衬聚四氟乙烯的不锈钢反应釜内,95℃反应5h后,过滤,取滤物,用蒸馏水洗涤6次后,30℃干燥6h得中间物B。其余步骤同实施例2。
效果例
下表1中给出了采用本发明实施例1至3与对比例1至5的一体化变粘压裂液的性能分析结果。
表1
降阻率(%) | 表观粘度(MPa·s) | 存放12个月后表观粘度(MPa·s) | 砂比(%) | 返排率(%) | |
实施例1 | 78 | 28.3 | 26.0 | 50 | - |
实施例2 | 79 | 85.2 | 82.1 | 100 | 70 |
实施例3 | 77 | 163.6 | 158.7 | 100 | 69 |
对比例1 | 66 | 77.9 | 73.2 | 88 | 66 |
对比例2 | 70 | 78.3 | 69.8 | 90 | 67 |
对比例3 | 71 | 60.2 | 48.1 | 58 | 67 |
对比例4 | 71 | 62.1 | 59.3 | 59 | 55 |
对比例5 | 72 | 66.5 | 55.3 | 62 | 68 |
从实施例与对比例的实验数据比较可发现,本发明利用高分子乳液、改性石英砂、改性纤维制得压裂液,通过调整乳液浓度,实现压裂液体系在滑溜水与胶液间的智能切换,进行多级变粘,到达各种排量下携砂的要求,同时含有柔性基团,提高压裂液的降阻性;高分子乳液具有高分子表面活性剂特征,增加压裂液粘度;低表面张力的改性石英砂在外加磁场下,在压裂缝快速铺开,嵌入其中,减少返排液带出损失;此外,改性纤维与改性石英砂形成双核铜配合,协同高分子乳液的季铵结构,抑制腐生菌等微生物生长,防止乳液腐烂变质,使压裂液长时间保持粘性。
对于本领域技术人员而言,显然本发明不限于上述示范性实施例的细节,而且在不背离本发明的精神或基本特征的情况下,能够以其他的具体形式实现本发明。因此,无论从哪一点来看,均应将实施例看作是示范性的,而且是非限制性的,本发明的范围由所附权利要求而不是上述说明限定,因此旨在将落在权利要求的等同要件的含义和范围内的所有变化囊括在本发明内。不应将权利要求中的任何标记视为限制所涉及的权利要求。
Claims (10)
1.一种一体化变粘压裂液,其特征在于,所述一体化变粘压裂液包括高分子乳液、改性石英砂、改性纤维、DL-8助排剂、DYAS系列解水锁剂、过硫酸铵、水。
2.根据权利要求1所述的一种一体化变粘压裂液,其特征在于,所述高分子乳液由以下方法制得,将丙烯酰胺、1-乙基-环戊醇丙烯酸酯、N-(2-丙烯酰氨基乙基)三乙基碘化铵配置成水相,将油相和乳化剂混合后,加入水相,升温、通氮气,加入过硫酸铵,恒温反应得高分子乳液。
3.根据权利要求2所述的一种一体化变粘压裂液,其特征在于,所述油相为溶剂油D110、柴油、煤油的一种或多种混合;所述乳化剂包括失水山梨醇单硬脂酸酯、聚氧乙烯失水山梨醇单硬脂酸酯。
4.根据权利要求1所述的一种一体化变粘压裂液,其特征在于,所述改性石英砂由丙烯酸、乙烯基甲基二甲氧基硅烷、磺胺噻唑化合物、硅烷改性四氧化三铁、石英砂制得;
所述磺胺噻唑化合物由2-氨基噻唑、4-(3-丁烯-1-基)苯磺酰氯制得;
所述硅烷改性四氧化三铁由乙烯基甲基二甲氧基硅烷、四氧化三铁制得。
5.根据权利要求1所述的一种一体化变粘压裂液,其特征在于,所述改性纤维由4-羧基苯磺酰氯、聚酯纤维、4-甲基-2-氨基噻唑制得。
6.一种一体化变粘压裂液的制备方法,其特征在于,包括以下制备步骤:
(1)将丙烯酰胺、1-乙基-环戊醇丙烯酸酯、N-(2-丙烯酰氨基乙基)三乙基碘化铵、去离子水按质量比1:0.1~0.3:0.1~0.3:8~10混合,搅拌溶解过后,加入丙烯酰胺质量0.0001~0.001倍的尿素、丙烯酰胺质量0.0008~0.002倍的乙二胺四乙酸二钠,100rpm搅拌20~25min,加入氢氧化钠溶液至反应液pH为6.3~7.2,得水相;
(2)将油相、乳化剂按质量比8~20:1混合,乳化剂中失水山梨醇单硬脂酸酯、聚氧乙烯失水山梨醇单硬脂酸酯的质量比为3:7,300~500rpm下,加入油相质量1.1~2.3倍的水相,升温至40~60℃,以7L/min通入氮气20~35min,加入油相质量0.01~0.2倍的过硫酸铵,反应4~6h得高分子乳液;
(3)将丙烯酸、乙烯基甲基二甲氧基硅烷按质量比1:0.4~0.8混合,100~200rpm搅拌30min,加入丙烯酸质量0.1~0.3倍的硅烷改性四氧化三铁、丙烯酸质量0.2~0.4倍的磺胺噻唑化合物,得混合溶液;向混合溶液加入混合溶液质量0.3~0.6倍的石英砂、丙烯酸质量0.001~0.005倍的偶氮二异丁腈,混合均匀后,倒入聚乙烯密封袋中,把袋中的气泡赶尽,用玻璃片夹好,水平置于55~70℃的水浴中,恒温反应10~20h后,取出,按料液比1:20浸泡于蒸馏水中,浸泡24h,取出得改性石英砂;
(4)将改性纤维、改性石英砂、一水合乙酸铜、无水乙醇、去离子水、吡啶按质量比0.3~0.5:5~30:1.5~10:170~400:18~80:9~55混合,置于内衬聚四氟乙烯的不锈钢反应釜内,80~110℃反应4~6h后,过滤,取滤物,用蒸馏水洗涤5~8次后,30℃干燥6h得中间物B;
(5)向100重量份的去离子水加入0.1~1.6重量份高分子乳液,100~200rpm搅拌15min,加入0.3~0.5重量份DL-8助排剂、0.4~0.6重量份DYAS系列解水锁剂、0.01~0.03重量份过硫酸铵,继续搅拌3min,得混液,加入混液体积0.2~0.4倍的中间物B,得一体化变粘压裂液。
7.根据权利要求6所述的一种一体化变粘压裂液的制备方法,其特征在于,步骤(3)所述硅烷改性四氧化三铁的制备方法为:将四氧化三铁、乙醇/水按料液比1:20~35混合,乙醇/水中无水乙醇和去离子水的体积比为1:1,氩气保护下,加入四氧化三铁质量0.05~0.3倍的乙烯基甲基二甲氧基硅烷,50~70℃、100~300rpm下搅拌反应60~80min后,抽滤,用无水乙醇洗涤3次,再用去离子水洗涤3次,60℃干燥6~9h。
8.根据权利要求6所述的一种一体化变粘压裂液的制备方法,其特征在于,步骤(3)所述磺胺噻唑化合物的制备方法为:将2-氨基噻唑、吡啶、4-(3-丁烯-1-基)苯磺酰氯按质量比1:8~12:0.4~0.7混合,室温反应4~7h后,加入2-氨基噻唑质量40~50倍的乙酸乙酯,再依次用质量分数为10%柠檬酸水溶液、饱和氯化钠溶液洗涤3次,用无水硫酸镁干燥1~2h,过滤,真空度-0.06MPa、60℃下蒸馏5~8h。
9.根据权利要求6所述的一种一体化变粘压裂液的制备方法,其特征在于,步骤(4)所述改性纤维的制备方法为:
a、将聚酯纤维按料液比1:10置于50g/L氢氧化钠溶液中,100~120℃下处理20min后,取出,用清水洗涤至洗液pH为7,40℃烘干10h,再置于大气低温等离子体设备中,空气气氛下,真空度50Pa、功率为100W下处理180~250s,得预处理聚酯纤维;
b、将预处理聚酯纤维按浴比1:30~50浸于4-羧基苯磺酰氯溶液,4-羧基苯磺酰氯溶液溶液中4-羧基苯磺酰氯、去离子水、过氧化苯甲酰的质量比为30~50:1000:1.1~2.7,60~80℃下反应2~4h,取出,40~50℃干燥5h得中间物A;
c、将4-甲基-2-氨基噻唑、吡啶、中间物A按质量比1:8~12:0.2~0.5混合,30~40℃反应3~4h后,取出,用乙酸乙酯洗涤6~8次,再分别用质量分数为10%柠檬酸水溶液、饱和氯化钠溶液洗涤3次,40℃干燥5h得改性纤维。
10.根据权利要求6~9所述的一种一体化变粘压裂液的使用方法,其特征在于,所述压裂液的使用方法为:在人造裂缝处施加4T磁场,在井筒施加0.6T磁场,通过水力压裂车将压裂液输送进入人造裂缝。
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