CN111518530B - 一种水驱井治理用有机锆交联凝胶调堵剂及其制备方法 - Google Patents
一种水驱井治理用有机锆交联凝胶调堵剂及其制备方法 Download PDFInfo
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- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 title claims abstract description 48
- 229910052726 zirconium Inorganic materials 0.000 title claims abstract description 47
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 239000003607 modifier Substances 0.000 title claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 32
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 30
- 238000004132 cross linking Methods 0.000 claims abstract description 25
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 24
- 229920000642 polymer Polymers 0.000 claims abstract description 17
- 239000012752 auxiliary agent Substances 0.000 claims abstract description 15
- 239000003381 stabilizer Substances 0.000 claims abstract description 10
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 claims description 16
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 13
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 12
- 229920000877 Melamine resin Polymers 0.000 claims description 9
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 9
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- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 claims description 8
- OFOBLEOULBTSOW-UHFFFAOYSA-N Malonic acid Chemical compound OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 claims description 8
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 claims description 8
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- OPGYRRGJRBEUFK-UHFFFAOYSA-L disodium;diacetate Chemical compound [Na+].[Na+].CC([O-])=O.CC([O-])=O OPGYRRGJRBEUFK-UHFFFAOYSA-L 0.000 claims description 4
- BEFDCLMNVWHSGT-UHFFFAOYSA-N ethenylcyclopentane Chemical compound C=CC1CCCC1 BEFDCLMNVWHSGT-UHFFFAOYSA-N 0.000 claims description 4
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- TYJJADVDDVDEDZ-UHFFFAOYSA-M potassium hydrogencarbonate Chemical compound [K+].OC([O-])=O TYJJADVDDVDEDZ-UHFFFAOYSA-M 0.000 claims description 3
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- BJEPYKJPYRNKOW-REOHCLBHSA-N (S)-malic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O BJEPYKJPYRNKOW-REOHCLBHSA-N 0.000 description 2
- AEQDJSLRWYMAQI-UHFFFAOYSA-N 2,3,9,10-tetramethoxy-6,8,13,13a-tetrahydro-5H-isoquinolino[2,1-b]isoquinoline Chemical compound C1CN2CC(C(=C(OC)C=C3)OC)=C3CC2C2=C1C=C(OC)C(OC)=C2 AEQDJSLRWYMAQI-UHFFFAOYSA-N 0.000 description 2
- CHHHXKFHOYLYRE-UHFFFAOYSA-M 2,4-Hexadienoic acid, potassium salt (1:1), (2E,4E)- Chemical compound [K+].CC=CC=CC([O-])=O CHHHXKFHOYLYRE-UHFFFAOYSA-M 0.000 description 2
- CYDQOEWLBCCFJZ-UHFFFAOYSA-N 4-(4-fluorophenyl)oxane-4-carboxylic acid Chemical compound C=1C=C(F)C=CC=1C1(C(=O)O)CCOCC1 CYDQOEWLBCCFJZ-UHFFFAOYSA-N 0.000 description 2
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 2
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- ABBQHOQBGMUPJH-UHFFFAOYSA-M Sodium salicylate Chemical compound [Na+].OC1=CC=CC=C1C([O-])=O ABBQHOQBGMUPJH-UHFFFAOYSA-M 0.000 description 2
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- 229910052804 chromium Inorganic materials 0.000 description 2
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- WPUMTJGUQUYPIV-JIZZDEOASA-L disodium (S)-malate Chemical compound [Na+].[Na+].[O-]C(=O)[C@@H](O)CC([O-])=O WPUMTJGUQUYPIV-JIZZDEOASA-L 0.000 description 2
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- 229960002635 potassium citrate Drugs 0.000 description 2
- QEEAPRPFLLJWCF-UHFFFAOYSA-K potassium citrate (anhydrous) Chemical compound [K+].[K+].[K+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O QEEAPRPFLLJWCF-UHFFFAOYSA-K 0.000 description 2
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- PHZLMBHDXVLRIX-UHFFFAOYSA-M potassium lactate Chemical compound [K+].CC(O)C([O-])=O PHZLMBHDXVLRIX-UHFFFAOYSA-M 0.000 description 2
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- SVICABYXKQIXBM-UHFFFAOYSA-L potassium malate Chemical compound [K+].[K+].[O-]C(=O)C(O)CC([O-])=O SVICABYXKQIXBM-UHFFFAOYSA-L 0.000 description 2
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Abstract
本发明涉及油田化学领域,提供一种水驱井治理用有机锆交联凝胶调堵剂及其制备方法。本发明为了解决近井水驱绕流造成低效无效循环现象突出问题而研制。本发明按重量百分比由下列成分组成:0.10%~0.15%的高分子调堵聚合物,0.25~1%的有机锆交联剂溶液,0.03%~0.07%的交联辅剂,0.03%~0.06%的稳定剂,余量为水;本发明还提供了该调堵剂制备方法。本发明无明显异味,对人体危害性较小,工业上尚未见锆中毒的报道;常温下性质稳定不易挥发、不易燃,利于存储、运输;且适用性良好,在较广的温度范围40‑100℃、及较宽的pH 5‑10范围内均可成胶,强度可控。
Description
技术领域:本发明涉及油田化学领域,提供可应用于水驱注入井厚油层层内低效无效循环治理需求的一种水驱井治理用有机锆交联凝胶调堵剂及其制备方法。
背景技术:随着油田水驱区块内采出程度不断提高,厚油层细分难度大,层内不具备完整的结构界面,长期水驱导致形成复杂的窜流大孔道,而常规调驱体系会加剧层内颗粒溶孔,导致出现新的粒间孔窜流通道,造成产层内注采低效无效循环问题突出。
通过化学调堵的方法是现下解决层内注采低效无效循环问题有效手段之一:目前油田常用调堵剂体系以Cr3+、铝交联剂为主,体系较为完整的,但Cr3+的毒性与其存在价态有关,Cr3+经氧化成高毒性的Cr6+,对人体危害严重;Al3+作为交联剂中心离子其成胶稳定性的问题制约铝离子交联剂性能进一步提升。锆离子交联体系以其环境友好性、良好注入性越来越来受到人们的关注,从根本上解决铬交联剂的毒性问题,但多见于压裂液配制,应用于油层酸压;此外还有少部分有机锆交联体系应用于驱油体系,以及低温油藏、中低渗透油层锆冻胶分散体型堵剂,例如:专利CN201410206657、专利 CN201210454820中都提到以有机锆为交联中心的分散型冻胶堵剂,具有低温油藏适用性。但同时受限于分散体堵剂特性,表现为整体性差、强度不足,多为微纳米级颗粒状结构,难以对大尺寸孔道形成有效支撑、实现有效封堵。因而在水驱注入井厚油层层内低效无效循环治理方面有机锆调堵剂仍有进一步研究需求。
本发明提供一种满足水驱注入井厚油层层内低效无效循环治理需求的有机锆交联凝胶调堵剂及其制备方法,成胶结构连续性、支撑性良好,能对较大孔隙通道进行有效封堵,填补现有有机锆调堵剂体系空缺,本发明所提供调堵剂体系具有耐温、延迟交联、低毒等方面特点。
发明内容:本发明的目的是提供了一种水驱井治理用有机锆交联凝胶调堵剂及其制备方法,注入的同时可有效支撑地层结构界面,抑制新的粒间孔窜流通道形成,更适合水驱区块产层内注采低效无效循环问题的治理。
本发明的技术方案是通过以下措施来实现的:一种水驱井治理用有机锆交联凝胶调堵剂,它按重量百分比由下列成分组成:0.10%~ 0.15%的高分子调堵聚合物,0.25~1%的有机锆交联剂溶液,0.03%~0.07%的交联辅剂,0.03%~0.06%的稳定剂,余量为水;
其制备方法如下:
(1)调节有机锆交联剂pH至6~7;在40~60℃下混合均匀,之后升温至70~90℃,至反应完全;恒温下静置熟化6~12h后使用;
(2)将0.15%的高分子调堵聚合物分散于水中,充分搅拌静置 4h后等待完全溶胀,得到高分子调堵聚合物溶液;
(3)在烧杯中加入0.25~1%的有机锆交联剂与足量水,取 (2)步聚中制得溶液,二者充分混合;
(4)加入0.03%~0.07%的交联辅剂;
(5)最后加入0.03%~0.06%的稳定剂和水,继续搅拌即得到一种水驱井治理用有机锆交联凝胶调堵剂。
高分子调堵聚合物为分子量1600-2500万、水解度为20-35的阴离子型聚丙烯酰胺类聚合物。
有机锆交联剂溶液为0.02%~0.05%的水溶性锆无机盐,0.03%~ 0.10%的多元复合羟基酸,0.06%~0.15%无机碱类/有机多元醇类pH 调节剂以及余量为水。
水溶性锆无机盐可以是四氯化锆、氧氯化锆中的一种或任意几种的组合。
多元复合羟基酸可以是几种多元羟基酸的复合酸,如:酒石酸、柠檬酸、乳酸,按质量比配比为0.5:0.25:1;酒石酸、苹果酸、乳酸,按质量比配比为0.5:0.5:1;酒石酸、乳酸、乙酸,按质量比配比为0.5:1:0.2等复配比例;也可以是几种多元羟基酸盐的复合酸盐,如:乳酸钠、乳酸钾、酒石酸钠、酒石酸钾、柠檬酸钠、柠檬酸钾、苹果酸钠、苹果酸钾、乙酸钠、乙酸钾中的一种或任意几种的组合。
无机碱类/有机多元醇类pH调节剂可以是氢氧化钠、氢氧化钾、碳酸钠、碳酸钾、碳酸氢钠、碳酸氢钾之一或组合,也可以是有机多元醇类pH调节剂如三乙醇胺、二乙醇胺中的一种或任意几种的组合。
所述的交联辅剂是甲醚化三聚氰胺树脂复配交联辅剂,它还可以是高度甲醚化三聚氰胺树脂类交联剂与葡萄糖酸钠、丙二酸、水杨酸、丙二酸钠或水杨酸钠中的一种或任意几种的组合。
稳定剂可以是山梨酸、山梨酸钾、双乙酸钠、三偏磷酸钠中的一种或任意几种的组合。
本发明的一种水驱井治理用有机锆交联凝胶调堵剂原理为:
Zr4+作为交联中心离子,与铬、铝等三价结构金属离子相比具有更大原子半径,表现出更佳的负载能力;Zr失去电子后留下的空轨杂化后重新排布形成sp3d4杂化轨道,使配体能够稳定分布中心离子周围;同时,Zr4+形成的8个sp3d4杂化轨道,电子云更集中,相较于各原子的成键能力更强,与配位体结合紧密,进一步降低中心离子释放速率,可实现延缓交联的目的;所用交联辅剂为三聚氰胺类、有机羧酸或有机羧酸盐等混合辅剂,引入反应活性点,拓展交联网络结构,解决支撑性不足的问题,Zr4+离子交联凝胶体系与三聚氰胺类交联体系之间形成“交叉网络作用”,使得凝胶体系的完整性、结构支撑得到提升。因而以锆金属离子作为主反应离子的有机交联体系,具有实现延缓成胶周期特能。
本发明具有如下优点:
1)本发明所用Zr4+性质稳定、不挥发,且无明显异味,对人体危害性较小;
2)本发明所提供调堵体系成胶结构连续性、支撑性良好,能对较大尺寸孔隙通道进行有效封堵;
3)本发明可用于中高温度油藏,及中高渗透率层,尤其是水驱注入井厚油层层内低效无效循环治理,二者可相互补充,填补了现有有机锆调堵体系空缺;
4)本发明以Zr4+离子作为主反应离子,具有实现延缓成胶周期特能,成胶前易注入,直达油层深部,实现低效无效循环层内调堵。
附图说明:图1为本发明选用无机锆盐在聚合物中交联示意图;图2为本发明实施例6中试样ZR2-6与ZR-1成胶性能进行比较;图 3为本发明实施例6中凝胶调堵剂体系分别在不同pH条件下粘度随时间变化曲线;图4为本发明实施例6中凝胶调堵剂体系分别在不同温度条件下粘度随时间变化曲线。
具体实施方式:下面结合实施例对本发明作进一步说明:一种水驱井治理用有机锆交联凝胶调堵剂,它按重量百分比由下列成分组成: 0.10%~0.15%的高分子调堵聚合物,0.25~1%的有机锆交联剂溶液, 0.03%~0.07%的交联辅剂,0.03%~0.06%的稳定剂,余量为水;
其制备方法如下:
(1)调节有机锆交联剂pH至6~7;在40~60℃下混合均匀,之后升温至70~90℃,至反应完全;恒温下静置熟化6~12h后使用;
(2)将0.15%的高分子调堵聚合物分散于水中,充分搅拌静置 4h后等待完全溶胀,得到高分子调堵聚合物溶液;
(3)在烧杯中加入0.25~1%的有机锆交联剂与足量水,取 (2)步聚中制得溶液,二者充分混合;
(4)加入0.03%~0.07%的交联辅剂;
(5)最后加入0.03%~0.06%的稳定剂和水,继续搅拌即得到一种水驱井治理用有机锆交联凝胶调堵剂。
高分子调堵聚合物为分子量1600-2500万、水解度为20-35的阴离子型聚丙烯酰胺类聚合物。
有机锆交联剂溶液为0.02%~0.05%的水溶性锆无机盐,0.03%~ 0.10%的多元复合羟基酸,0.06%~0.15%无机碱类/有机多元醇类 pH调节剂以及余量为水。
水溶性锆无机盐可以是四氯化锆、氧氯化锆中的一种或任意几种的组合。
多元复合羟基酸可以是几种多元羟基酸的复合酸,如:酒石酸、柠檬酸、乳酸,按质量比配比为0.5:0.25:1;酒石酸、苹果酸、乳酸,按质量比配比为0.5:0.5:1;酒石酸、乳酸、乙酸,按质量比配比为0.5:1:0.2等复配比例;也可以是几种多元羟基酸盐的复合酸盐,如:乳酸钠、乳酸钾、酒石酸钠、酒石酸钾、柠檬酸钠、柠檬酸钾、苹果酸钠、苹果酸钾、乙酸钠、乙酸钾中的一种或任意几种的组合。
无机碱类/有机多元醇类pH调节剂可以是氢氧化钠、氢氧化钾、碳酸钠、碳酸钾、碳酸氢钠、碳酸氢钾之一或组合,也可以是有机多元醇类pH调节剂如三乙醇胺、二乙醇胺中的一种或任意几种的组合。
所述的交联辅剂是甲醚化三聚氰胺树脂复配交联辅剂,它还可以是高度甲醚化三聚氰胺树脂类交联剂与葡萄糖酸钠、丙二酸、水杨酸、丙二酸钠或水杨酸钠中的一种或任意几种的组合。
稳定剂可以是山梨酸、山梨酸钾、双乙酸钠、三偏磷酸钠中的一种或任意几种的组合。
实施例1
本实施例中ZR-1型有机锆交联凝胶调堵剂,其按重量百分比由下列成分组成:
制备流程:
(1)Zr4+交联剂制备:首先将氧氯化锆与酒石酸、柠檬酸及乳酸组成的多元复合羟基酸(复合酸比例0.5:0.25:1),加入氢氧化钠调节pH至6-7;在40-60℃下混合均匀,之后升温至70-90℃,至反应完全;恒温下静置熟化6-12h后使用;
(2)将0.15%的阴离子型聚丙烯酰胺分散于水中,充分搅拌静置4h后等待聚丙烯酰胺完全溶胀,得到阴离子型聚丙烯酰胺溶液;
(3)在烧杯中加入步骤(1)中Zr4+交联剂1%与足量水,取步聚(2)制得阴离子型聚丙烯酰胺溶液,二者充分混合;
(4)向步骤(3)中加入0.03%甲醚化三聚氰胺树脂、丙二酸及水杨酸复合交联辅剂0.03%,其复合比例为1:0.5:0.25;
(5)最后加入山梨酸、双乙酸钠及三偏磷酸钠复合稳定剂 0.05%,其复合比例为1:0.25:0.45,余量为水,继续搅拌即得到有机锆交联凝胶调堵剂。
实施例2
本实施例中试样ZR-2,不加入甲醚化三聚氰胺树脂复配交联辅剂,其按重量百分比由下列成分组成:
制备方法同实施例1。
实施例3
试样ZR-3为单酒石酸交联有机锆交联凝胶调堵剂,其按重量百分比由下列成分组成:
制备方法同实施例1。
实施例4
试样ZR-4为单柠檬酸交联有机锆交联凝胶调堵剂,其按重量百分比由下列成分组成:
制备方法同实施例1。
实施例5
试样ZR-5为单苹果交联有机锆交联凝胶调堵剂,其按重量百分比由下列成分组成:
制备方法同实施例1。
实施例6
试样ZR-6为单乳酸交联有机锆交联凝胶调堵剂,其按重量百分比由下列成分组成:
制备方法同实施例1。
与ZR-1成胶性能进行比较,试样ZR-2在缺少交联辅剂作用情况下,凝胶体系结构强度不足,长期稳定性不足;试样ZR-3-6由于是单羧酸络合,存在成胶速率过急或过缓的问题,难以实现现场调堵应用,实验结果见图2。
实施例7
本实施例对上述实施例1提供的有机锆交联凝胶调堵剂ZR-1在不同pH、温度条件下进行各项性能测试,如下:
耐酸碱性:
使用无机酸碱,调节pH=6-10,然后配制1500mg/L凝胶调堵剂体系,观察其成胶性能,实验结果见图3;
耐温性:
配制1500mg/L凝胶调堵剂体系,分别在不同温度条件下(45- 100℃)反应成胶,观察其成胶热稳定性,实验结果见图4。
封堵性:
实施例中凝胶调堵剂强度能过流变仪测得,型号TA-2000EX;所用岩芯参数对400-4000mD渗透率范围内的方岩心进行1500mg/L凝胶调堵剂体系的驱替封堵实验,评价其成胶性能、封堵率和残余阻力系数,实验结果见表1。
表1
Claims (4)
1.一种水驱井治理用有机锆交联凝胶调堵剂,其特征在于:它按重量百分比由下列成分组成:0.10%~0.15%的高分子调堵聚合物,0.25~1%的有机锆交联剂溶液,0.03%~0.07%的交联辅剂,0.03%~0.06%的稳定剂,余量为水;
所述高分子调堵聚合物为分子量1600-2500万、水解度为20-35的阴离子型聚丙烯酰胺类聚合物;
所述有机锆交联剂溶液为0.02%~0.05%的水溶性锆无机盐,0.03%~0.10%的多元复合羟基酸,0.06%~0.15%无机碱类/有机多元醇类pH调节剂以及余量为水;
其中所述多元复合羟基酸为酒石酸、柠檬酸、乳酸复配,其复配比例为0.5:0.25:1;
所述交联辅剂为甲醚化三聚氰胺树脂、丙二酸及水杨酸复配,其复配比例为1:0.5:0.25;
所述稳定剂为山梨酸、双乙酸钠及三偏磷酸钠复配,其复配比例为1:0.25:0.45。
2.根据权利要求1所述的一种水驱井治理用有机锆交联凝胶调堵剂,其特征在于:所述水溶性锆无机盐为四氯化锆、氧氯化锆中的一种或任意几种的组合。
3.根据权利要求1所述的一种水驱井治理用有机锆交联凝胶调堵剂,其特征在于:所述无机碱类pH调节剂为氢氧化钠、氢氧化钾、碳酸钠、碳酸钾、碳酸氢钠、碳酸氢钾之一或组合,有机多元醇类pH调节剂为三乙醇胺、二乙醇胺中的一种或任意几种的组合。
4.利用权利要求1所述的一种水驱井治理用有机锆交联凝胶调堵剂的制备方法,其特征在于:制备方法步骤如下:
(1)调节有机锆交联剂pH至6~7;在40~60℃下混合均匀,之后升温至70~90℃,至反应完全;恒温下静置熟化6~12h后使用;
(2)将0.15%的高分子调堵聚合物分散于水中,充分搅拌静置4h后等待完全溶胀,得到高分子调堵聚合物溶液;
(3)在烧杯中加入0.25~1%的有机锆交联剂与足量水,取(2)步聚中制得溶液,二者充分混合;
(4)加入0.03%~0.07%的交联辅剂;
(5)最后加入0.03%~0.06%的稳定剂和水,继续搅拌即得到一种水驱井治理用有机锆交联凝胶调堵剂。
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