CN114933674A - 一种温敏可控均质交联降解凝胶颗粒及其制备方法和应用 - Google Patents
一种温敏可控均质交联降解凝胶颗粒及其制备方法和应用 Download PDFInfo
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Abstract
本发明公开一种温敏可控均质交联降解凝胶颗粒及其制备方法和应用。凝胶颗粒原料组分为：丙烯酰胺类中性单体5‑90％；阳离子单体1‑70％；疏水性单体1‑40％；丙烯酸类酸性单体0.1‑10％；交联剂0.01‑10％；引发剂0.01‑2％；其中疏水性单体为甲基丙烯酸甲酯、甲基丙烯酸乙酯、甲基丙烯酸丁酯、丙烯酸甲酯、丙烯酸乙酯或其衍生物中至少一种；交联剂为三氧化铬、氧化锆、三氧化二铝、二氧化钛、碳酸钙中至少一种。该凝胶颗粒在缝洞中经温度诱导引发原位形成大块本体凝胶，机械强度高，耐温性能好，可高效封堵各种类型缝洞；同时本体凝胶后期可原位降解为聚合物溶液而失去封堵效果，恢复油层渗透率，达到保护储层的效果。
Description
技术领域
本发明属于油气勘探开发油田化学领域，具体涉及一种温敏可控均质交联降解凝胶颗粒及其制备方法和应用。
背景技术
目前在油气勘探开发领域，聚丙烯酰胺等类型聚合物冻胶及凝胶颗粒等封堵剂被广泛应用于缝洞性油藏封堵，通常具有较好的黏弹性和一定的封堵能力。但聚合物冻胶体系存在诸多缺陷，难以控制胶凝时间，机械强度弱、抗冲刷性能差、长期易丧失封堵性能等技术问题。尽管聚合物凝胶颗粒具有地面交联成胶、耐温抗盐等特点，使其“易注入，能封堵，可运移”，且廉价易得、成本低，因此作为高效封堵剂，大面积应用于地层非均质性较高的油田勘探开发。然而凝胶颗粒的高膨胀性导致其容易破碎、不耐冲刷、长期化学、热稳定性差，特别是，凝胶颗粒与大尺寸缝洞(厘米级，甚至更大)的配伍性差，颗粒堆积体承压能力差、易破碎，难于有效调整大尺寸缝洞剖面。
目前，聚合物凝胶和树脂类固体胶凝剂复合体系通过松散凝胶颗粒胶结固化形成高强度桥塞，一定程度上提高了桥塞复合体的机械性能。然而复合体系封堵效果弱、耐高温效果差、地层水稀释效应强、多组分作业复杂等因素严重削弱了工程作业的可行性。此外，前期的再交联凝胶产品皆为于凝胶颗粒界面间交联，此类交联由于收到凝胶颗粒间交联密度的限制，难以有效提高交联后本体凝胶的机械性能及耐高温特性。特别是在油藏基质无限水环境下，依靠金属离子包裹释放二次交联剂，由于水的稀释作用，使再交联凝胶颗粒在大量水的条件下，不具备再次交联功能。油藏高温对凝胶基质的化学破坏作用，导致由配位键形成后本体凝胶在高温条件下耐温性能胶差，不具备长期结构稳定性(机械、化学性能)，进而失去持久封堵效果，难以高效封堵高温缝洞油藏及恶性漏失等油气勘探开发中遇到的技术难题。更为重要的是，目前再交联颗粒缺乏对再次交联功能控制性，无法实现对特定温度地层的可控封堵。特别是交联后的本体凝胶不具备自催化自降解功能，对油藏基质造成不可逆损害。
发明内容
针对上述技术问题，本发明的目的在于提供一种温敏可控均质交联降解凝胶颗粒及其制备方法和应用。该凝胶颗粒在缝洞中经温度诱导引发可原位形成耐高温高强度大块本体凝胶，机械强度高，耐温性能好，可高效封堵各种类型缝洞；同时本体凝胶后期可原位降解为聚合物溶液而失去封堵效果，恢复油层渗透率，达到保护储层的效果。
为了解决上述技术问题，本发明所采用的技术方案如下：
提供一种温敏可控均质交联降解凝胶颗粒，以无溶剂计，其原料组分及质量百分比如下：
丙烯酰胺类中性单体，5.0-90.0％；
阳离子单体，1.0-70.0％；
疏水性单体，1.0-40.0％；
丙烯酸类酸性单体，0.1-10.0％；
交联剂，0.01-10.0％；
引发剂，0.01-2.0％；其中：
所述疏水性单体为甲基丙烯酸甲酯、甲基丙烯酸乙酯、甲基丙烯酸丁酯、丙烯酸甲酯、丙烯酸乙酯或其衍生物中的至少一种；
所述交联剂为三氧化铬、氧化锆、三氧化二铝、二氧化钛、碳酸钙过渡金属盐类中的至少一种。
按上述方案，所述丙烯酰胺类中性单体为甲基丙烯酰胺、二甲基丙烯酰胺、丙烯酰胺或其类似衍生物中的至少一种。
按上述方案，所述丙烯酸类酸性单体为甲基丙烯酸、丙烯酸或其类似衍生物中的至少一种。
按上述方案，所述阳离子单体为甲基丙烯酰氧乙基三甲基氯化铵、二烯丙基二甲基氯化铵、丙烯酰氧乙基三甲基氯化铵或其类似衍生物中的至少一种。
按上述方案，所述引发剂为氧化还原引发剂或光引发剂。优选地，氧化还原引发剂为水溶性过二硫酸铵或过二硫酸钾；或者油溶性偶氮二异丁氰、过二硫酸铵-亚硫酸钠、过二硫酸钾-亚硫酸钠；所述光引发剂为2-羟基-2-甲基-1-苯基丙酮(2959)或2,4,6-三甲基苯甲酰基-二苯基氧化膦。
提供一种上述温敏可控均质交联降解凝胶颗粒的制备方法，包括如下步骤：
1)将丙烯酰胺类中性单体、阳离子单体、疏水性单体、丙烯酸类酸性单体和交联剂以水溶解分散，得到均匀分散的混合物,通入氮气除去体系氧气；其中根据实际需要，在除氧前或是除氧后加入引发剂；
2)将步骤1)得到的混合物进行聚合，得聚合物本体凝胶；
3)将步骤2)得到的聚合物本体凝胶切块，真空干燥，自然冷却至室温，经破碎筛选，得到温敏可控均质交联降解凝胶颗粒。
按上述方案，所述步骤2)中，
当引发剂为氧化还原引发剂时，聚合条件为温度为室温到80℃，聚合时间为1～12小时，聚合结束后进行自然冷却，得到聚合物本体凝胶；
当引发剂为光引发剂时，在紫外光照射进行聚合1-3小时，得到聚合物本体凝胶。
按上述方案，所述步骤3)中，干燥温度为室温到60℃，干燥时间为1～24小时。
按上述方案，所述步骤3)中，经破碎筛选，得到的再交联凝胶颗粒粒径为毫米级或厘米级大小。
提供一种上述温敏均质可控再交联降解凝胶颗粒在油气勘探开发恶性漏失防漏堵漏、堵水调剖、滤失控制等的应用。
按上述方案，所述应用为：
将上述温敏均质再交联凝胶颗粒用水配制成悬浮液，使凝胶颗粒的质量百分比含量为0.01％～15.0％，泵入地层；在地层温度90-150℃条件下激发下，凝胶颗粒进行再交联，缝洞内原位形成高强度耐高温本体凝胶，实现对地层缝洞有效调剖和/或封堵、解堵。
优选地，水可为盐水，其中盐水浓度最高为26.5％(饱和食盐水)。
优选地，上述配制悬浮液的水可为清水、注入水或者回注水。
本发明的温敏可控均质再交联降解凝胶颗粒，在地层温度大于90℃条件下激发下，凝胶颗粒之间及凝胶颗粒内部基质再次有机化学交联，缝洞内原位形成高强度本体凝胶；其机理为：凝胶颗粒中，聚合物丙烯酸单体与交联剂适度聚合交联形成离子交联凝胶，聚丙烯酰胺单体与疏水性单体不参与化学交联，而在凝胶颗粒之间及凝胶颗粒基质内部原位形成潜在的再交联化学基团，由此得到具有再交联功能的凝胶颗粒。凝胶颗粒悬浮液注入地层后，吸收地层水而膨胀，在地层温度的激发下，丙烯酰胺中胺基与疏水化学基团在凝胶颗粒界面间及界面内形成稳定的有机化学键，赋予了凝胶颗粒的再交联性能，进而于大尺寸缝洞内形成大块本体凝胶。同时疏水单体通过调控酯基水解可有效控制凝胶自降解，交联后本体凝胶可完成数周内到数个月内的可控解堵，实现了对缝洞的有效封堵并可在后期解堵。
本发明的有益效果如下：
1.本发明提供一种温敏原位重构可再交联凝胶颗粒，凝胶颗粒界面之间及凝胶颗粒基质内部形成有机共价键，经温度诱导激发凝胶颗粒之间及凝胶颗粒基质内部重构形成有机化学交联高强度整体凝胶，从而可实现对大孔道、裂缝或缝洞的有效封堵；在需要封堵部位原位形成双重交联本体凝胶，机械强度由原来的200-500帕，可提高到2000到5000帕，是原凝胶颗粒5到10倍，通过室内模拟实验，对直径3厘米大孔道封堵压力可达10兆帕，增强了本体凝胶的封堵效果，同时从整体上提高本体凝胶的耐温性能高达150℃，此外凝胶颗粒还可以实现在高浓度盐水如饱和食盐水或过量盐溶液中再交联，适应地层无限水极端条件，具有广泛的适用性。
2.本发明的再交联凝胶颗粒中，疏水单体具有原位催化降解作用，利用油藏地层的激发活化作用，有效调控再交联后本体凝胶的降解性能，本体凝胶可原位降解为聚合物溶液而失去封堵效果，恢复油层渗透率，达到保护储层的效果。
3.本发明通过改变疏水性单体的疏水性，可以调控凝胶颗粒的再次交联温度，实现了根据地层特定温度按需选择和制备。
4.本发明的可再交联凝胶颗粒在制备过程中，形成金属弱交联凝胶颗粒，再次交联功能得化学基团皆以有机化学键形式均匀存在于凝胶基质，保证了凝胶注入不受地层因素影响，保持了再交联颗粒的完整性及在地层无限水极端条件下的再交联性，制备过程简单，易于工业化生产。
附图说明
图1为实施例1凝胶颗粒原位构筑高性能本体凝胶。
图2为实施例1凝胶颗粒交联前后机械强度。
图3为实施例3凝胶颗粒降解为高分子溶液。
图4为实施例3凝胶颗粒在过量盐溶液中的交联性；其中从左至右分别为：
第一个：1g凝胶颗粒，10mL 1％NaCl；第二个：1g凝胶颗粒，20mL 1％NaCl；第三个：1g凝胶颗粒，30mL 1％NaCl。
具体实施方式
下面结合附图，说明本发明的具体实施方式，但是以下说明不会构成对本发明的限制。
实施例1
提供一种温敏均质再交联凝胶颗粒的制备方法，包括以下步骤：
取用丙烯酰胺10.0克，甲基丙烯酰氧乙基三甲基氯化铵10.0克，丙烯酸1.0克，过二硫酸铵100毫克，氧化锆0.5克，甲基丙烯酸甲酯2.0克，水100毫升，置于烧瓶中，通入氮气30分钟除去体系氧气；置于磁力加热搅拌器中，反应温度为80℃，聚合时间为12小时，自然冷却后，得到环境响应聚合物本体凝胶；将得到的聚合物本体凝胶粉碎，置于真空干燥箱干燥,干燥温度为60℃，干燥时间为12小时；自然冷却至室温，经进一步粉碎、筛选，根据需求可获得到一种环境响应尺寸为5毫米到2厘米凝胶颗粒。
含有甲基丙烯酸甲酯单体的凝胶颗粒再交联温度为90℃。
通过室内6个月老化实验，凝胶颗粒再交联后形成的本体凝胶耐温性能达到150℃。
图2为实施例1凝胶颗粒交联前后机械强度，图中显示，交联前机械强度为200帕，交联后可提高到2000帕。
实施例2
提供一种温敏均质再交联凝胶颗粒的制备方法，包括以下步骤：
取用2-丙烯酰胺-2-甲基丙磺酸10.0克，甲基丙烯酰氧乙基三甲基氯化铵10.0克，丙烯酰胺，5.0克，丙烯酸1.0克，甲基丙烯酸丁酯1.0克，三氧化二铝2.0克，水100毫升置于烧瓶中，通入氮气30分钟除去体系氧气，加入过二硫酸铵100毫克和亚硫酸钠200毫克，室温聚合1h制备聚合物本体凝胶；将得到的聚合物本体凝胶粉碎、筛选，置于真空干燥箱干燥,干燥温度为60℃，干燥时间为12小时；自然冷却至室温，得到一种环境响应尺寸为2毫到1厘米凝胶颗粒。
含有甲基丙烯酸丁酯单体的凝胶颗粒再交联温度为110℃。
实施例3
提供一种温敏均质再交联凝胶颗粒的制备方法，包括以下步骤：
取用甲基丙烯酸丁酯10.0克，甲基丙烯酰氧乙基三甲基氯化铵10.0克，丙烯酰胺，5.0克，丙烯酸1.0克，碳酸钙1.0克，水100毫升，置于烧瓶中，通入氮气30分钟除去体系氧气；加入光引发剂2959 100毫克，在紫外光照射2小时下，得到环境响应聚合物本体凝胶；将得到的聚合物本体凝胶粉碎、筛选，置于真空干燥箱干燥,干燥温度为60℃，干燥时间为12小时；自然冷却至室温，得到一种环境响应尺寸为0.5毫米到1厘米凝胶颗粒。
此凝胶颗粒在150℃下1％NaCl溶液(石油工程一般用盐水模拟地层条件)中再交联为大块本体凝胶，参见图4，可有效封堵缝洞。其中图4从左至右分别为：第一个：1g凝胶颗粒，10mL 1％NaCl；第二个：1g凝胶颗粒，20mL 1％NaCl；第三个：1g凝胶颗粒，30mL1％NaCl。因为凝胶颗粒有些时候遇到地层无限水的极端条件，图4也可以证明在大量盐溶液中凝胶依旧具有再交联性。
室内老化实验室证实，本体凝胶在150℃下可自动降解为聚合物溶液，降解时间为1周，参见图3。
实施例4
提供一种温敏均质再交联凝胶颗粒的制备方法，包括以下步骤：
取用甲基丙烯酸丁酯10.0克，甲基丙烯酰氧乙基三甲基氯化铵10.0克，丙烯酰胺，5.0克，丙烯酸1.0克，氧化铬0.5克，过二硫酸铵100毫克，水100毫升，置于烧瓶中，通入氮气30分钟除去体系氧气，加热至60℃反应一个小时，得到环境响应聚合物本体凝胶；将得到的聚合物本体凝胶粉碎、筛选，置于真空干燥箱干燥,干燥温度为60℃，干燥时间为12小时；自然冷却至室温，得到一种环境响应尺寸为0.5毫米到1厘米凝胶颗粒。
此凝胶颗粒在3％浓度下的盐溶液中130℃条件重新交联为本体凝胶。
经室内驱替实验评价，对模拟大尺寸缝洞的3厘米管道的封堵压力达到10MPa。
Claims (10)
1.一种温敏可控均质交联降解凝胶颗粒，其特征在于，以无溶剂计，其原料组分及质量百分比如下：
丙烯酰胺类中性单体，5.0-90.0％；
阳离子单体，1.0-70.0％；
疏水性单体，1.0-40.0％；
丙烯酸类酸性单体，0.1-10.0％；
交联剂，0.01-10.0％；
引发剂，0.01-2.0％；其中：
所述疏水性单体为甲基丙烯酸甲酯、甲基丙烯酸乙酯、甲基丙烯酸丁酯、丙烯酸甲酯、丙烯酸乙酯或其衍生物中的至少一种；
所述交联剂为三氧化铬、氧化锆、三氧化二铝、二氧化钛、碳酸钙中的至少一种。
2.根据权利要求1所述的凝胶颗粒，其特征在于，所述丙烯酰胺类中性单体为甲基丙烯酰胺、二甲基丙烯酰胺、丙烯酰胺或其类似衍生物中的至少一种；所述阳离子单体为甲基丙烯酰氧乙基三甲基氯化铵、二烯丙基二甲基氯化铵、丙烯酰氧乙基三甲基氯化铵或其类似衍生物中的至少一种。
3.根据权利要求1所述的凝胶颗粒，其特征在于，所述丙烯酸类酸性单体为甲基丙烯酸、丙烯酸或其类似衍生物中的至少一种。
4.根据权利要求1所述的凝胶颗粒，其特征在于，所述引发剂为氧化还原引发剂或光引发剂。
5.根据权利要求1所述的凝胶颗粒，其特征在于，所述氧化还原引发剂为过二硫酸铵、过二硫酸钾、偶氮二异丁氰、过二硫酸铵-亚硫酸钠或过二硫酸钾-亚硫酸钠；所述光引发剂为2-羟基-2-甲基-1-苯基丙酮或2,4,6-三甲基苯甲酰基-二苯基氧化膦。
6.一种权利要求1-5任一项所述的温敏均质再交联凝胶颗粒的制备方法，其特征在于，包括如下步骤：
1)将丙烯酰胺类中性单体、阳离子单体、疏水性单体、丙烯酸类酸性单体和交联剂以水溶解分散，得到均匀分散的混合物,通入氮气除去体系氧气；其中根据实际需要，在除氧前或是除氧后加入引发剂；
2)将步骤1)得到的混合物进行聚合，得聚合物本体凝胶；
3)将步骤2)得到的聚合物本体凝胶切块，真空干燥，自然冷却至室温，经破碎筛选，得到再交联凝胶颗粒。
7.根据权利要求6所述的制备方法，其特征在于，所述步骤2)中，
当引发剂为氧化还原引发剂时，聚合条件为温度为室温到80℃，聚合时间为1～12小时，聚合结束后进行自然冷却，得到聚合物本体凝胶；
当引发剂为光引发剂时，在紫外光照射进行聚合1-3小时，得到聚合物本体凝胶。
8.根据权利要求6所述的制备方法，其特征在于，所述步骤3)中，干燥温度为室温到60℃，干燥时间为1～24小时；经破碎筛选，得到的再交联凝胶颗粒粒径为毫米级或厘米级大小。
9.一种权利要求1-5任一项所述的温敏均质可控再交联降解凝胶颗粒在油气勘探开发恶性漏失防漏堵漏、堵水调剖或滤失控制方面的应用。
10.根据权利要求9所述的应用，其特征在于，所述应用为：
将上述温敏均质再交联凝胶颗粒用水配制成悬浮液，使凝胶颗粒的质量百分比含量为0.01％～15.0％，泵入地层；在地层温度90-150℃条件下激发下，凝胶颗粒进行再交联，缝洞内原位形成高强度耐高温本体凝胶。
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