CN111139040A - 一种钻井液用温度响应型铝基封堵处理剂及其制备方法 - Google Patents
一种钻井液用温度响应型铝基封堵处理剂及其制备方法 Download PDFInfo
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Abstract
本发明涉及钻井用化学助剂领域的一种钻井液用温度响应型铝基封堵处理剂及其制备方法；所述钻井液用温度响应型铝基封堵处理剂，包含聚乙二醇、异氰酸酯、铝化合物在内的组分为原料，溶于有机溶剂中，在催化剂的作用下，通过一锅法而合成。所述处理剂可有效封堵地层微裂缝，增强井壁稳定性；所述钻井液用温度响应型铝基封堵处理剂为液体型，更易于使用且不会出现粉尘问题，可有效提高钻井液的封堵性，提高多梯度温差条件下含微裂隙地层的井壁稳定性；而且该封堵处理剂的制备方法简单、易于操作、易于工业化。
Description
技术领域
本发明涉及钻井用化学助剂领域，更进一步说，涉及一种钻井液用温度响应型铝基封堵处理剂及其制备方法。
背景技术
随着钻遇地层条件日益复杂，钻井作业对钻井液的防塌性能和强化井壁能力要求越来越高。封堵防塌处理剂能够通过封堵地层原生孔隙和微裂缝，阻隔水化作用通道，提高钻井液的封堵能力，减少钻井液中的自由水侵入地层，降低地层坍塌压力从而起到稳定井壁的作用。封堵防塌处理剂主要有沥青类处理剂、硅酸盐和聚合醇等处理剂。
近年来，铝化合物具有独特的物理化学性质，可根据pH的不同发生形态变化，能够通过电性中和、离子吸附和化学沉淀作用，减弱泥页岩膨胀，封堵孔喉和微裂缝，强化井壁。铝基钻井液防塌处理剂研究与应用已成为钻井液研究领域的热点之一。国外研究人员已研发出多种铝基防塌处理剂，如贝克休斯等公司开发出MAX-PLEX铝基防塌处理剂等产品，在阿拉伯海湾地区、澳大利亚、墨西哥湾、哥伦比亚、巴西、美国大陆等地区应用，均取得良好效果。
国内关于铝基处理剂的研究起步较晚，但发展迅速，除在钻井液中引入Al2(SO4)3·16H2O、AlCl3·6H2O和NaAlO2等无机盐外，还研发出铝聚合物处理剂AOP-1、DLP-1和PF-Chemseal等产品。上述铝基处理剂均可在钻进过程中，钻遇地层原生地层水(pH<5)或较低pH值地层表面，利用铝化合物的性质迅速发生化学反应，生成氢氧化铝沉淀，并进一步与地层矿物反应，形成致密的络合铝矿物内滤饼，封堵地层微裂缝和微裂隙，阻隔水力作用通道，增强页岩半透膜效应，增强井壁的稳定性。与常规处理剂物理封堵防塌不同，新型铝基处理剂为化学反应型防塌处理剂，适用于造浆性强地层的防泥包，硬脆性微裂缝泥页岩地层的封堵防塌。此外，研究发现新型铝基处理剂具有抑制石膏溶解和固相清洁的作用，可有效防止石膏侵对钻井液性能影响，提高钻井液的抗钙能力。
上述铝基处理剂在钻井液环境中主要以非水溶形式存在且配伍性问题突出，降低了其进入地层与地层粘土矿物的反应能力，影响了防塌效果，限制了其应用范围和使用性能。
发明内容
为了解决现有技术中存在的上述问题，本发明提出一种钻井液用温度响应型铝基封堵处理剂，具体地说涉及一种钻井液用温度响应型铝基封堵处理剂及其制备方法。本发明利用地层环境和钻井液环境存在明显不同，借鉴环境响应材料的设计思路，利用钻井液环境与地层环境的温度不同，研发一种可对100～150℃地层温度响应的温度响应型铝基封堵处理剂，实现其进入地层后能够迅速化学反应和物理形态变化、自行调整，及时孔喉或微裂缝，从而强化井壁。
本发明以聚乙二醇、异氰酸酯、铝化合物、多元醇等为原料，溶于有机溶液中，在催化剂的作用下通过一锅法合成了具有亲疏水链段交替结构的温度响应型铝基处理剂。通过调节聚合物中亲水链段或者疏水链段的比例(聚乙二醇为亲水链，异氰酸酯为疏水链，可调控这两种反应原料的比例及铝化合物的加量，提高异氰酸酯链的比例和铝的加量，则处理剂的响应温度上升，提高聚乙二醇链的比例则相应温度下降)，可以控制温度响应型铝基处理剂的相转变温度在100～150℃内调节，从而实现其在地层环境的温度响应，封堵地层孔喉或微裂缝。
本发明目的之一是提供一种钻井液用温度响应型铝基封堵处理剂，包含以聚乙二醇、异氰酸酯、铝化合物在内的组分为原料，溶于有机溶剂中，在催化剂的作用下，在有机溶剂中，通过一锅法而合成。
其中，
所述聚乙二醇、异氰酸酯、铝化合物的质量比为(1～10)：(1～15)：(1～2)，优选(1～4)：(1～6)：(1～2)，更优选(1～2)：(1～3)：(1～2)。
所述聚乙二醇的分子量可为500～5000；优选所述聚乙二醇的分子量可为1000～4000。
所述铝化合物可选自AlCl3·6H2O、Al2(SO4)3·16H2O、KAl(SO4)2·12H2O、AlCl3、Al(C3H5O3)3、Al[O2C(CH2)16CH3]3和NaAlO2中的至少一种；优选所述铝化合物可选自AlCl3·6H2O、Al2(SO4)3·16H2O和KAl(SO4)2·12H2O中的至少一种。
所述异氰酸酯可选自甲苯二异氰酸酯(TDI)、异佛尔酮二异氰酸酯(IPDI)、二苯基甲烷二异氰酸酯(MDI)、二环己基甲烷二异氰酸酯(HMDI)、六亚甲基二异氰酸酯(HMDI)中的至少一种。
所述有机溶剂可选自丙酮、四氢呋喃、1，4-二氧六环、N,N-二甲基甲酰胺、N,N-二甲基甲酰胺、二甲亚砜中的至少一种。有机溶剂的加量为将各反应原料充分溶解即可，一般加量可为所述反应物重量的2倍以上。
所述钻井液用温度响应型铝基封堵处理剂还可包含填充辅料，所述填充辅料可选自200～10000目碳酸钙和/或滑石粉。
所述催化剂可选自辛酸亚锡、钛酸丁酯、二月硅酸二丁基锡和三异丙醇铝中的至少一种；优选所述催化剂可选自辛酸亚锡和/或二月硅酸二丁基锡；
所述催化剂的用量范围可为反应原料总质量(即聚乙二醇、异氰酸酯、铝化合物三种原料总质量之和)的0.02％～0.12％。
所述通过一锅法而合成的产物可进一步用无机碱中和产物至pH＝7～10；所述无机碱可选自KOH、NaOH；如具体可选自5～40％KOH水溶液。
所述一锅法的反应温度可为60～90℃；反应时间可为6～10小时。
所述钻井液用温度响应型铝基封堵处理剂还可包含填充辅料，所述填充辅料选自200～10000目碳酸钙和/或滑石粉；所述辅料的用量根据实际情况进行调节，具体可为反应产物总重量的0～20％。
本发明目的之二是提供所述钻井液用温度响应型铝基封堵处理剂的制备方法，可包括以下步骤在内：包含聚乙二醇、异氰酸酯、铝化合物在内的组分为原料，溶于有机溶剂中，在催化剂的作用下通过一锅法而合成。合成产物再经调节pH值，去除溶剂，即得最终产物钻井液用温度响应型铝基封堵处理剂。具体地，可包括以下步骤：
将聚乙二醇和铝化合物溶于有机溶剂中，置于反应容器内，反应容器加热至60～90℃，氮气保护下加入催化剂，滴加异氰酸酯，搅拌条件下持续反应6～10小时，得到乳白色液体。用无机碱将该乳白色液体调节pH至8～10，减压蒸馏，去除反应溶剂，即得到所述钻井液用温度响应型铝基封堵处理剂。
本发明利用无机铝化合物通过一锅法合成了具有亲疏水链段交替结构的温度响应型铝基封堵处理剂，可有效封堵地层微裂缝，增强井壁稳定性。而且配伍性好，属于一种惰性材料，加入钻井液中后，对钻井液的其它性能影响较小。且该封堵处理剂为液体型，更易于使用且不会出现粉尘问题，可有效提高钻井液的封堵性，提高多梯度温差条件下含微裂隙地层的井壁稳定性。而且该封堵处理剂的制备方法简单、易于操作、易于工业化，可广泛应用于水基钻井液，强化井壁的稳定性，满足复杂地层勘探开发的要求。
具体实施方式
下面结合实施例，进一步说明本发明。但本发明不受这些实施例的限制。
实施例1
在带搅拌器、冷凝器和滴液漏斗的干燥三口烧瓶中加入400mL丙酮，13.206g的聚乙二醇(分子量2000)和4.5211g AlCl3·6H2O、10g的Al2(SO4)3·16H2O，滴液漏斗中加入22.1496g的甲苯二异氰酸酯(TDI)。将三口烧瓶水浴加热至82℃，加热的同时抽真空2小时以除去水分。氮气保护下加入0.038g二月桂酸二丁基锡，将滴液漏斗中的甲苯二异氰酸酯(TDI)滴入三口烧瓶中，搅拌条件下持续反应6小时，得到乳白色液体。用20％的KOH溶液将该乳白色液体调节pH至7.5，减压蒸馏，去除反应溶剂丙酮，即得到目标产物。
实施例2
在带搅拌器、冷凝器和滴液漏斗的干燥三口烧瓶中加入350mL1，4-二氧六环，10.2250的聚乙二醇(分子量4000)和12.3221g KAl(SO4)2·12H2O，滴液漏斗中加入22.1496g的二环己基甲烷二异氰酸酯(HMDI)。将三口烧瓶水浴加热至76℃，加热的同时抽真空2小时以除去水分。氮气保护下加入0.048g辛酸亚锡，将滴液漏斗中的二环己基甲烷二异氰酸酯(HMDI)滴入三口烧瓶中，搅拌条件下持续反应7.5小时，得到乳白色液体。用20％的KOH溶液将该乳白色液体调节pH至8.0，减压蒸馏，去除反应溶剂丙酮，即得到目标产物。
实施例3
在带搅拌器、冷凝器和滴液漏斗的干燥三口烧瓶中加入400mL四氢呋喃，13.206g的聚乙二醇(分子量1000)和10.251g KAl(SO4)2·12H2O，滴液漏斗中加入22.1496g的异佛尔酮二异氰酸酯(IPDI)。将三口烧瓶水浴加热至60℃，加热的同时抽真空2小时以除去水分。氮气保护下加入0.016g二月桂酸二丁基锡，将滴液漏斗中的异佛尔酮二异氰酸酯(IPDI)滴入三口烧瓶中，搅拌条件下持续反应8小时，得到乳白色液体。用20％的KOH溶液将该乳白色液体调节pH至7.0，减压蒸馏，去除反应溶剂丙酮，即得到目标产物。
实施例4
在带搅拌器、冷凝器和滴液漏斗的干燥三口烧瓶中加入450mL N,N-二甲基甲酰胺，16.36g的聚乙二醇(分子量2000)和15.2775gAl2(SO4)3·16H2O，滴液漏斗中加入17.6695g六亚甲基二异氰酸酯。将三口烧瓶水浴加热至80℃，加热的同时抽真空2小时以除去水分。氮气保护下加入0.014二月桂酸二丁基锡，将滴液漏斗中的六亚甲基二异氰酸酯(HMDI)滴入三口烧瓶中，搅拌条件下持续反应6.5h得到乳白色液体。用20％的KOH溶液将该乳白色液体调节pH至7.5，减压蒸馏，去除反应溶剂丙酮，即得到目标产物。
实施例5
在带搅拌器、冷凝器和滴液漏斗的干燥三口烧瓶中加入450mL二甲亚砜，18.5569g的聚乙二醇(分子量3500)和14.78gAlCl3·6H2O，滴液漏斗中加入20.2553g二苯基甲烷二异氰酸酯(MDI)。将三口烧瓶水浴加热至90℃，加热的同时抽真空2小时以除去水分。氮气保护下加入0.016二月桂酸二丁基锡，将滴液漏斗中的二苯基甲烷二异氰酸酯(MDI)滴入三口烧瓶中，搅拌条件下持续反应6h得到乳白色液体。用20％的KOH溶液将该乳白色液体调节pH至8.0，减压蒸馏，去除反应溶剂丙酮，即得到目标产物。
实施例6
微裂隙封堵性能评价
所述测试方法可参见文献出处：褚奇，孔勇，杨帆，等.多苯基芳基硅烷偶联剂改性纳米SiO2封堵剂[J].断块油气田，2017,24(2)：281～284。
所述测试方法具体步骤包括：以膨润土和重晶石为原料，利用GG42-2型高温高压滤失仪制备3.8mm厚度的泥饼以模拟纳微米级地层(渗透率683.010-2mD)，通过测量含有1.0wt％的实施例1～5制备的所述温度响应型铝基封堵剂在不同温度条件下模拟地层中的平均流量，结合达西公式，计算封堵前后模拟地层的渗透率，从而得到不同温度相应型铝基封堵剂对模拟地层的封堵率，结果见表1。
表1温度响应型铝基封堵剂对模拟地层封堵率的影响
| 种类 | 温度(℃) | 渗透率(10<sup>-2</sup>mD) | 封堵率(％) |
| 实施例1 | 110 | 30.22 | 95.58 |
| 实施例2 | 120 | 21.3 | 96.88 |
| 实施例3 | 150 | 15.4 | 97.75 |
| 实施例4 | 140 | 25.1 | 96.33 |
| 实施例5 | 100 | 37.9 | 84.45 |
从上表1可以看出，钻井液中温度响应型铝基封堵剂在相应温度条件下的封堵率均高于80％，甚至超过90％，表明对纳微米孔隙地层具有良好的封堵能力。
Claims (10)
1.一种钻井液用温度响应型铝基封堵处理剂，包含以聚乙二醇、异氰酸酯、铝化合物在内的组分为原料，溶于有机溶剂中，在催化剂的作用下，通过一锅法而合成。
2.根据权利要求1所述的钻井液用温度响应型铝基封堵处理剂，其特征在于：
所述聚乙二醇、异氰酸酯、铝化合物的质量比为(1～10)：(1～15)：(1～2)，优选(1～4)：(1～6)：(1～2)。
3.根据权利要求1所述的钻井液用温度响应型铝基封堵处理剂，其特征在于：
所述聚乙二醇的分子量为500～5000；优选所述聚乙二醇的分子量为1000～4000。
4.根据权利要求1所述的钻井液用温度响应型铝基封堵处理剂，其特征在于：
所述铝化合物选自AlCl3·6H2O、Al2(SO4)3·16H2O、KAl(SO4)2·12H2O、AlCl3、Al(C3H5O3)3、Al[O2C(CH2)16CH3]3和NaAlO2中的至少一种；优选所述铝化合物选自AlCl3·6H2O、Al2(SO4)3·16H2O和KAl(SO4)2·12H2O中的至少一种。
5.根据权利要求1所述的钻井液用温度响应型铝基封堵处理剂，其特征在于：
所述异氰酸酯选自甲苯二异氰酸酯、异佛尔酮二异氰酸酯、二苯基甲烷二异氰酸酯、二环己基甲烷二异氰酸酯、六亚甲基二异氰酸酯中的至少一种。
6.根据权利要求1所述的钻井液用温度响应型铝基封堵处理剂，其特征在于：
所述有机溶剂选自丙酮、四氢呋喃、1，4-二氧六环、N,N-二甲基甲酰胺、N,N-二甲基甲酰胺、二甲亚砜中的至少一种。
7.根据权利要求1所述的钻井液用温度响应型铝基封堵处理剂，其特征在于：
所述催化剂选自辛酸亚锡、钛酸丁酯、二月桂酸二丁基锡和三异丙醇铝中的至少一种；优选所述引发剂为辛酸亚锡和/或二月硅酸二丁基锡；
所述催化剂用量为所述聚乙二醇、异氰酸酯、铝化合物三种原料总质量之和的0.02％～0.12％。
8.根据权利要求1所述的钻井液用温度响应型铝基封堵处理剂，其特征在于：
所述通过一锅法而合成的产物用无机碱中和至pH＝7～10。
9.根据权利要求1～8之任一项所述的钻井液用温度响应型铝基封堵处理剂的制备方法，其特征在于包括以下步骤：
包含以聚乙二醇、异氰酸酯、铝化合物在内的组分为原料，溶于有机溶剂中，在催化剂的作用下通过一锅法而合成。
10.根据权利要求9所述的钻井液用温度响应型铝基封堵处理剂的制备方法，其特征在于包括以下步骤：
所述一锅法的反应温度为60～90℃。
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| CN114106790A (zh) * | 2020-08-27 | 2022-03-01 | 中国石油化工股份有限公司 | 一种钻井液用封堵剂及其制备方法和应用 |
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| CN116064014A (zh) * | 2021-11-01 | 2023-05-05 | 中国石油化工股份有限公司 | 一种地层环境分子识响应型井壁稳定材料及其制备方法和应用 |
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