技术领域Technical field
本发明涉及油田勘探技术领域，尤其涉及一种石油钻井耐高温油基钻井液固结堵漏材料及其使用方法。The invention relates to the technical field of oil field exploration, and in particular to a high-temperature-resistant oil-based drilling fluid consolidation and plugging material for oil drilling and a method of using the same.
背景技术Background technique
油基钻井液是石油钻井中必不可少的材料，其作用包括维持井筒压力防止地层坍塌、提供钻头旋转动力、携带或悬浮钻屑回地面、冷却钻头破碎工作面、堵漏操作时携带堵漏材料至漏点。而石油钻井深度在数千米到万米左右，钻井液压力随地层深度每增加100米就至少增加1Mpa，数千米到万米左右的深度静压可达数十兆帕到百兆帕，在如此高压下，微小的裂缝都可以产生较大的钻井液漏失，因此，需要利用油基钻井液携带堵漏剂进入漏失点，完成堵漏工作。Oil-based drilling fluid is an essential material in petroleum drilling. Its functions include maintaining wellbore pressure to prevent formation collapse, providing drill bit rotation power, carrying or suspending drill cuttings back to the surface, cooling the drill bit crushing working surface, and carrying leakage plugging during leakage plugging operations. material to the point of leakage. The depth of oil drilling is about several thousand meters to ten thousand meters, and the drilling fluid pressure increases by at least 1 MPa for every 100 meters of formation depth. The static pressure at depths of about several thousand meters to ten thousand meters can reach tens to hundreds of MPa. Under such high pressure, tiny cracks can produce large drilling fluid losses. Therefore, it is necessary to use oil-based drilling fluid to carry the loss-stopping agent into the loss point to complete the leak-stopping work.
石油钻井油基钻井液堵漏材料有多种，包括采用各种有机、无机、刚性、酸可溶、酸不溶等性质材料和各种颗粒、粉末、微粉、纤维、微纤维、片状、微片状形状结构的材料，根据石油钻井油基钻井液堵漏材料某种堵漏需求进行堵漏材料各种性能和结构、尺寸的搭配以及颗粒直径大小的复合级配，以获得满足石油钻井油基钻井液堵漏需求的堵漏材料。There are many kinds of leakage plugging materials for oil drilling oil-based drilling fluids, including various organic, inorganic, rigid, acid-soluble, acid-insoluble and other properties materials and various particles, powders, micro-powders, fibers, micro-fibers, flakes, micro- Materials with a sheet shape structure, according to the certain plugging requirements of oil-based drilling fluid plugging materials for oil drilling, the various properties, structures, sizes of the plugging materials, and the composite gradation of particle diameter sizes are matched to obtain the oil drilling fluid that meets the requirements. Plugging materials based on drilling fluid plugging requirements.
但是，通常的石油钻井油基钻井液堵漏材料在堵漏过程形成的滤塞或滤饼，很难或者几乎不具备固结成一体的能力，其原因在于，具有固结能力的材料大部分只能在水相中固结，而在油基钻井液例如柴油中无法发挥水化固结性能，其必须在水溶液中才能水化固结性能，所以无法在油基钻井液中实现。因此，需要提供一种石油钻井耐高温油基钻井液固结堵漏材料来解决堵漏材料无法在油基钻井液中固结而造成的堵漏效果差的问题。However, the filter plug or filter cake formed by ordinary oil-based drilling fluid plugging materials during the plugging process is difficult or almost incapable of being consolidated into one body. The reason is that most materials with the ability to consolidate are It can only be consolidated in the water phase, but cannot exert its hydration and consolidation performance in oil-based drilling fluids such as diesel. It must be in an aqueous solution to achieve hydration and consolidation performance, so it cannot be realized in oil-based drilling fluids. Therefore, there is a need to provide a high-temperature oil-based drilling fluid consolidation plugging material for oil drilling to solve the problem of poor plugging effect caused by the inability of the plugging material to consolidate in the oil-based drilling fluid.
发明内容Contents of the invention
有鉴于此，本申请提供一种石油钻井耐高温油基钻井液固结堵漏材料及其使用方法，用以解决油基钻井液钻井造成的漏失问题。In view of this, this application provides a high-temperature resistant oil-based drilling fluid consolidation and plugging material for oil drilling and a method of using it to solve the problem of lost circulation caused by oil-based drilling fluid drilling.
为达到上述技术目的，本申请采用以下技术方案：In order to achieve the above technical objectives, this application adopts the following technical solutions:
第一方面，本申请提供一种石油钻井耐高温油基钻井液固结堵漏材料，包括质量份数如下的组分：5-50份酸溶性材料、0.05-1份润湿剂、5-50份密度调节剂、0.5-20份纤维材料、5-30份水不溶且油不溶性树脂粉末；水不溶且油不溶性树脂的固化温度≥120℃。In the first aspect, this application provides a high-temperature resistant oil-based drilling fluid consolidation and plugging material for oil drilling, including the following components by mass: 5-50 parts of acid-soluble material, 0.05-1 part of wetting agent, 5- 50 parts of density regulator, 0.5-20 parts of fiber material, 5-30 parts of water-insoluble and oil-insoluble resin powder; the curing temperature of water-insoluble and oil-insoluble resin is ≥120°C.
优选的，水不溶且油不溶性树脂的制备方法包括以下步骤：Preferably, the preparation method of water-insoluble and oil-insoluble resin includes the following steps:
S1.将苯酚加热至70-75℃后，加入碱性催化剂，再加入甲醛，于70-85℃下反应25-30min，再升温至105℃反应1.5-2h，得粗产物A；S1. After heating phenol to 70-75℃, add alkaline catalyst, then add formaldehyde, react at 70-85℃ for 25-30min, then raise the temperature to 105℃ and react for 1.5-2h to obtain crude product A;
S2.将粗产物A降温至90-95℃，加入无水乙酸调节pH值至酸性，再真空脱水，进行缩聚反应，再降温至70℃以下，即得水不溶且油不溶性树脂；水不溶且油不溶性树脂的固化温度大于等于120℃；苯酚、甲醛、碱性催化剂、无水乙酸的质量比为(0.9-1.1):(1.3-1.4):(0.033-0.05)：(0.066-0.08)。S2. Cool the crude product A to 90-95°C, add anhydrous acetic acid to adjust the pH value to acidic, then dehydrate in a vacuum, perform a polycondensation reaction, and then cool down to below 70°C to obtain a water-insoluble and oil-insoluble resin; water-insoluble and oil-insoluble resin The curing temperature of the oil-insoluble resin is greater than or equal to 120°C; the mass ratio of phenol, formaldehyde, alkaline catalyst, and anhydrous acetic acid is (0.9-1.1): (1.3-1.4): (0.033-0.05): (0.066-0.08).
优选的，水不溶且油不溶性树脂的制备方法包括以下步骤：Preferably, the preparation method of water-insoluble and oil-insoluble resin includes the following steps:
K1.将苯酚加热至70-75℃后，加入硼酸，再加入硫酸铜催化剂，于100-120℃回流反应7-8h，再升温至180-190℃反应1-2h，得粗产物B；K1. After heating phenol to 70-75°C, add boric acid, then add copper sulfate catalyst, reflux and react at 100-120°C for 7-8 hours, then raise the temperature to 180-190°C and react for 1-2 hours to obtain crude product B;
K2.将粗产物B降温至80-90℃，加入甲醛反应，再降温至70℃以下，即得水不溶且油不溶性树脂；水不溶且油不溶性树脂的固化温度大于等于150℃；苯酚：硼酸：硫酸铜：甲醇的质量比为(0.9-1.1)：(0.85-1.05)：(0.01-0.03)：(1.1-1.5)。K2. Cool the crude product B to 80-90°C, add formaldehyde to react, and then lower the temperature to below 70°C to obtain a water-insoluble and oil-insoluble resin; the curing temperature of the water-insoluble and oil-insoluble resin is greater than or equal to 150°C; phenol: boric acid : The mass ratio of copper sulfate: methanol is (0.9-1.1): (0.85-1.05): (0.01-0.03): (1.1-1.5).
优选的，酸溶性材料包括碳酸钙、碳酸镁中的一种或几种。Preferably, the acid-soluble material includes one or more of calcium carbonate and magnesium carbonate.
优选的，密度调节剂包括重晶石粉、赤铁矿中的一种或几种。Preferably, the density regulator includes one or more of barite powder and hematite.
优选的，纤维材料包括天然纤维、合成纤维中的一种或几种，例如玻璃纤维、碳纤维。Preferably, the fiber material includes one or more of natural fibers and synthetic fibers, such as glass fiber and carbon fiber.
第二方面，本申请提供一种石油钻井耐高温油基钻井液固结堵漏材料的堵漏浆料，其包括质量比为1-2:1的油基材料与所述石油钻井耐高温油基钻井液固结堵漏材料，所述油基材料包括柴油、白油、油包水乳液中的一种或几种。In a second aspect, this application provides a leakage plugging slurry for consolidating leakage plugging materials with high-temperature resistant oil-based drilling fluid for oil drilling, which includes an oil-based material and the oil-drilling high-temperature resistant oil with a mass ratio of 1-2:1. The oil-based material includes one or more of diesel oil, white oil, and water-in-oil emulsion.
第三方面，本申请提供一种使用堵漏浆料的堵漏方法，包括如下步骤：将堵漏浆料注入井温大于等于120℃的堵漏段进入漏失缝隙，待堵漏浆料固化后得到油基堵漏结构，即完成堵漏操作。In the third aspect, the present application provides a method for plugging leakage using a leakage plugging slurry, which includes the following steps: inject the leakage plugging slurry into the leakage plugging section with a well temperature greater than or equal to 120°C into the leakage gap, and wait for the leakage plugging slurry to solidify. The oil-based leakage plugging structure is obtained, which completes the leakage plugging operation.
优选的，漏失缝隙的大小为0.1-5mm。Preferably, the size of the leakage gap is 0.1-5mm.
优选的，油基堵漏结构的抗压强度为4-20Mpa。Preferably, the compressive strength of the oil-based leakage plugging structure is 4-20Mpa.
本申请的有益效果如下：通过原料配比并使用具有不同固结温度的水不溶且油不溶性树脂作为堵漏材料，在油基钻井液(例如柴油)携带下，水不溶且油不溶性树脂配合其他堵漏材料进入漏失缝隙形成滤塞或滤饼，同时在漏失压差的作用下粘合成整体，随着时间的延长和温度的升高，水不溶且油不溶性树脂在熔融状态下与其他堵漏材料固化成高强度的整体结构，完成堵漏工作，形成的堵漏结构稳定性高、强度高、耐高温，堵漏效果好。The beneficial effects of this application are as follows: by proportioning raw materials and using water-insoluble and oil-insoluble resins with different solidification temperatures as leakage plugging materials, the water-insoluble and oil-insoluble resins are combined with other materials when carried by oil-based drilling fluids (such as diesel). The plugging material enters the leakage gap to form a filter plug or filter cake. At the same time, it is bonded into a whole under the action of the leakage pressure difference. As time goes by and the temperature rises, the water-insoluble and oil-insoluble resin will melt with other plugging materials in the molten state. The leakage material is solidified into a high-strength overall structure to complete the leakage plugging work. The formed leakage plugging structure has high stability, high strength, high temperature resistance, and good leakage plugging effect.
具体实施方式Detailed ways
为了使本发明的目的、技术方案及优点更加清楚明白，以下结合实施例，对本发明进行进一步详细说明。应当理解，此处所描述的具体实施例仅仅用以解释本发明，并不用于限定本发明。In order to make the purpose, technical solutions and advantages of the present invention clearer, the present invention will be further described in detail below in conjunction with examples. It should be understood that the specific embodiments described here are only used to explain the present invention and are not intended to limit the present invention.
本申请提供一种石油钻井耐高温油基钻井液固结堵漏材料，包括质量份数如下的组分：5-50份酸溶性材料、0.05-1份润湿剂、5-50份密度调节剂、0.5-20份纤维材料、5-30份水不溶且油不溶性树脂粉末；水不溶且油不溶性树脂的固化温度≥120℃。This application provides a high-temperature resistant oil-based drilling fluid consolidation and plugging material for oil drilling, including the following components by mass: 5-50 parts of acid-soluble material, 0.05-1 part of wetting agent, 5-50 parts of density adjustment Agent, 0.5-20 parts of fiber material, 5-30 parts of water-insoluble and oil-insoluble resin powder; the curing temperature of water-insoluble and oil-insoluble resin is ≥120°C.
本申请通过原料配比并使用具有不同固结温度的水不溶且油不溶性树脂作为堵漏材料，在油基钻井液(例如柴油)携带下完成堵漏工作，水不溶且油不溶性树脂配合其他堵漏材料进入漏失缝隙形成滤塞或滤饼，同时在漏失压差的作用下粘合成整体，随着时间的延长和温度的升高，水不溶且油不溶性树脂在熔融状态下将其他堵漏材料粘合，再固化成高强度的整体结构，完成堵漏工作，形成的堵漏结构稳定性高、强度高、耐高温，堵漏效果好。This application uses raw material proportioning and uses water-insoluble and oil-insoluble resins with different solidification temperatures as leakage plugging materials, and is carried by oil-based drilling fluids (such as diesel) to complete the leakage plugging work. The water-insoluble and oil-insoluble resins are combined with other plugging materials. The leakage material enters the leakage gap to form a filter plug or filter cake. At the same time, it is bonded into a whole under the action of the leakage pressure difference. As time goes by and the temperature increases, the water-insoluble and oil-insoluble resin plugs other leaks in the molten state. The materials are bonded and then solidified into a high-strength overall structure to complete the leakage plugging work. The formed leakage plugging structure has high stability, high strength, high temperature resistance, and good leakage plugging effect.
本申请使用酸溶性材料的原因在于，在堵漏材料固结堵漏工序完成，后期要连通油气产层恢复油气通道因而采用酸蚀的酸溶性材料以打通油气通道。The reason why acid-soluble materials are used in this application is that after the sealing and sealing process of leakage plugging materials is completed, the oil and gas production layers must be connected to restore the oil and gas channels in the later stage. Therefore, acid-etched acid-soluble materials are used to open the oil and gas channels.
本申请使用的润湿剂为本领域技术人员常在油相中使用的润湿剂，例如十二烷基三甲基溴化铵。The wetting agent used in this application is a wetting agent commonly used in the oil phase by those skilled in the art, such as dodecyltrimethylammonium bromide.
本申请基于水不溶且油不溶性树脂粉末在油中不溶且到一定温度时开始熔融(但不溶)并且一定温度下经过一定固结时间后形成不溶不融的结构特性实现堵漏功能，具体的，本申请制备水不溶且油不溶性树脂粉末有两种方法：This application is based on the water-insoluble and oil-insoluble resin powder which is insoluble in oil and starts to melt (but is insoluble) when it reaches a certain temperature and forms an insoluble and infusible structure after a certain solidification time at a certain temperature to achieve the plugging function. Specifically, There are two methods for preparing water-insoluble and oil-insoluble resin powder in this application:
其中一种水不溶且油不溶性树脂的制备方法包括以下步骤：One of the preparation methods of water-insoluble and oil-insoluble resin includes the following steps:
S1.将苯酚加热至70-75℃后，加入碱性催化剂，再加入甲醛，于70-85℃下反应25-30min，再升温至105℃反应1.5-2h，得粗产物A；S1. After heating phenol to 70-75℃, add alkaline catalyst, then add formaldehyde, react at 70-85℃ for 25-30min, then raise the temperature to 105℃ and react for 1.5-2h to obtain crude product A;
S2.将粗产物A降温至90-95℃，加入无水乙酸调节pH值至酸性，再真空脱水，进行缩聚反应，再降温至70℃以下，即得水不溶且油不溶性树脂；水不溶且油不溶性树脂的固化温度大于等于120℃；苯酚、甲醛、碱性催化剂、无水乙酸的质量比为(0.9-1.1):(1.3-1.4):(0.033-0.05)：(0.066-0.08)。S2. Cool the crude product A to 90-95°C, add anhydrous acetic acid to adjust the pH value to acidic, then dehydrate in a vacuum, perform a polycondensation reaction, and then cool down to below 70°C to obtain a water-insoluble and oil-insoluble resin; water-insoluble and oil-insoluble resin The curing temperature of the oil-insoluble resin is greater than or equal to 120°C; the mass ratio of phenol, formaldehyde, alkaline catalyst, and anhydrous acetic acid is (0.9-1.1): (1.3-1.4): (0.033-0.05): (0.066-0.08).
另一种水不溶且油不溶性树脂的制备方法包括以下步骤：Another preparation method of water-insoluble and oil-insoluble resin includes the following steps:
K1.将苯酚加热至70-75℃后，加入硼酸，再加入硫酸铜催化剂，于100-120℃回流反应7-8h，再升温至180-190℃反应1-2h，得粗产物B；K1. After heating phenol to 70-75°C, add boric acid, then add copper sulfate catalyst, reflux and react at 100-120°C for 7-8 hours, then raise the temperature to 180-190°C and react for 1-2 hours to obtain crude product B;
K2.将粗产物B降温至80-90℃，再加入甲醛反应，再降温至70℃以下，即得水不溶且油不溶性树脂；水不溶且油不溶性树脂的固化温度大于等于150℃；其中，苯酚：硼酸：硫酸铜：甲醇的质量比为(0.9-1.1)：(0.85-1.05)：(0.01-0.03)：(1.1-1.5)。K2. Cool the crude product B to 80-90°C, then add formaldehyde to react, and then lower the temperature to below 70°C to obtain a water-insoluble and oil-insoluble resin; the curing temperature of the water-insoluble and oil-insoluble resin is greater than or equal to 150°C; where, The mass ratio of phenol: boric acid: copper sulfate: methanol is (0.9-1.1): (0.85-1.05): (0.01-0.03): (1.1-1.5).
本申请制备的水不溶且油不溶性树脂粉末通过酚、醛在酸性或碱性催化剂存在下经过缩合而得，其不溶于水及油，但溶于乙醇。The water-insoluble and oil-insoluble resin powder prepared in this application is obtained by condensing phenol and aldehyde in the presence of an acidic or alkaline catalyst. It is insoluble in water and oil, but soluble in ethanol.
在一些实施例中，酸溶性材料包括碳酸钙、碳酸镁中的一种或几种，用于降低固结后材料的结构强度(低于水泥强度)，可以避免堵漏后复钻时因为堵漏材料强度太高而钻出新孔，同时酸溶性材料可以在需要时产生可溶酸沟通油层或气层，对应的，本方案的水不溶且油不溶性树脂粉末有利于提高固结后材料(即油基堵漏结构)的结构强度，本方案得到的油基堵漏结构的抗压强度在4-20Mpa之间。In some embodiments, the acid-soluble material includes one or more of calcium carbonate and magnesium carbonate, which is used to reduce the structural strength of the material after consolidation (lower than the strength of cement), which can avoid blockage due to re-drilling after the leakage is plugged. The strength of the leakage material is too high and new holes are drilled. At the same time, the acid-soluble material can produce soluble acid to communicate with the oil layer or gas layer when needed. Correspondingly, the water-insoluble and oil-insoluble resin powder in this solution is beneficial to improve the material after consolidation ( That is, the structural strength of the oil-based leakage plugging structure). The compressive strength of the oil-based leakage plugging structure obtained by this solution is between 4-20Mpa.
在一些实施例中，密度调节剂包括重晶石粉、赤铁矿中的一种或几种。In some embodiments, the density adjuster includes one or more of barite powder and hematite.
在一些实施例中，纤维材料包括天然纤维、合成纤维中的一种或几种，例如玻璃纤维、碳纤维，用于堵漏搭桥。In some embodiments, the fiber material includes one or more of natural fibers and synthetic fibers, such as glass fiber and carbon fiber, and is used for plugging and bridging.
本申请提供一种石油钻井耐高温油基钻井液固结堵漏材料的堵漏浆料，其包括质量比为1-2:1的油基材料与所述石油钻井耐高温油基钻井液固结堵漏材料，所述油基材料包括柴油、白油、油包水乳液中的一种或几种，以油基材料例如柴油作为油基钻井液携带堵漏材料完成堵漏工作。This application provides a leakage plugging slurry for solidifying leakage plugging materials with high temperature resistant oil-based drilling fluid for oil drilling, which includes an oil-based material with a mass ratio of 1-2:1 and the oil-based drilling fluid with a mass ratio of 1-2:1. The oil-based material includes one or more of diesel, white oil, and water-in-oil emulsion. The oil-based material, such as diesel oil, is used as the oil-based drilling fluid to carry the leakage-stopping material to complete the leakage-stopping work.
本申请提供一种堵漏方法，包括如下步骤：将堵漏浆料注入井温大于等于120℃的堵漏段进入漏失缝隙，待堵漏浆料固化后即完成堵漏操作。This application provides a method for plugging leakage, which includes the following steps: inject the leakage plugging slurry into the leakage plugging section where the well temperature is greater than or equal to 120°C into the leakage gap, and the leakage plugging operation is completed after the leakage plugging slurry solidifies.
优选的，漏失缝隙的大小为0.1-5mm。Preferably, the size of the leakage gap is 0.1-5mm.
以下通过具体实施例对本方案进行进一步说明。This solution will be further described below through specific examples.
实施例1Example 1
一种石油钻井耐高温油基钻井液固结堵漏材料，包括质量份数如下的组分：40份碳酸钙、0.05份润湿剂、25份重晶石粉、20份玻璃纤维、15份水不溶且油不溶性树脂粉末；水不溶且油不溶性树脂的固化温度为120℃。A kind of high-temperature-resistant oil-based drilling fluid consolidation and plugging material for oil drilling, including the following components by mass: 40 parts of calcium carbonate, 0.05 parts of wetting agent, 25 parts of barite powder, 20 parts of glass fiber, 15 parts of water Insoluble and oil-insoluble resin powder; the curing temperature of water-insoluble and oil-insoluble resin is 120°C.
其中，水不溶且油不溶性树脂粉末的制备方法如下：Among them, the preparation method of water-insoluble and oil-insoluble resin powder is as follows:
S1.将苯酚投入反应釜中，升温至70-75℃后，加入碱性催化剂碳酸氢钠，再加入甲醛，升温并保持反应温度在70-85℃下反应25min，再升温至105℃反应1.5h，得粗产物A；S1. Put phenol into the reaction kettle, raise the temperature to 70-75°C, add alkaline catalyst sodium bicarbonate, then add formaldehyde, raise the temperature and maintain the reaction temperature at 70-85°C for 25 minutes, then raise the temperature to 105°C for reaction 1.5 h, get crude product A;
S2.将粗产物A降温至90℃，加入无水乙酸调节pH值至小于7，再真空脱水缩聚2h，直至无水分凝出，停止加热后，将反应釜降温至70℃以下，出料到连续冷却钢带输送机上冷却，即得水不溶且油不溶性树脂；水不溶且油不溶性树脂的固化温度为120℃；苯酚、甲醛、碱性催化剂、无水乙酸的质量比为0.9:1.3:0.04：0.07。本实施例的水不溶且油不溶性树脂低于120℃时是稳定的，当高于120℃时进入持续熔融状态，当温度进一步升高或维持当前温度一定时间后，其进入热固化状态。S2. Cool the crude product A to 90°C, add anhydrous acetic acid to adjust the pH value to less than 7, and then vacuum dehydration and polycondensation for 2 hours until no water condenses out. After stopping heating, cool the reaction kettle to below 70°C, and discharge the material to Cool on the continuous cooling steel belt conveyor to obtain water-insoluble and oil-insoluble resin; the curing temperature of the water-insoluble and oil-insoluble resin is 120°C; the mass ratio of phenol, formaldehyde, alkaline catalyst, and anhydrous acetic acid is 0.9:1.3:0.04 :0.07. The water-insoluble and oil-insoluble resin of this embodiment is stable when it is lower than 120°C, enters a continuous melting state when it is higher than 120°C, and enters a thermal solidification state when the temperature further increases or the current temperature is maintained for a certain period of time.
实施例2Example 2
一种石油钻井耐高温油基钻井液固结堵漏材料，包括质量份数如下的组分：30份碳酸钙、0.07份润湿剂、30份重晶石粉、20份玻璃纤维、20份水不溶且油不溶性树脂粉末；水不溶且油不溶性树脂的固化温度为150℃。A kind of high-temperature-resistant oil-based drilling fluid consolidation and plugging material for oil drilling, including the following components by mass: 30 parts of calcium carbonate, 0.07 parts of wetting agent, 30 parts of barite powder, 20 parts of glass fiber, 20 parts of water Insoluble and oil-insoluble resin powder; the curing temperature of water-insoluble and oil-insoluble resin is 150°C.
其中，水不溶且油不溶性树脂粉末的制备方法如下：Among them, the preparation method of water-insoluble and oil-insoluble resin powder is as follows:
K1.将苯酚加热至70-75℃后，加入硼酸，再加入硫酸铜催化剂，于100℃回流反应7h，再升温至180℃反应1h，蒸出部分水分，得粗产物B；K1. After heating phenol to 70-75°C, add boric acid, then add copper sulfate catalyst, reflux and react at 100°C for 7 hours, then raise the temperature to 180°C and react for 1 hour, steam out part of the water to obtain crude product B;
K2.将粗产物B降温至80℃，再加入甲醛反应，低于100℃反应4h，停止加热，再降温至70℃以下，出料到连续冷却钢带输送机上冷却，即得水不溶且油不溶性树脂；水不溶且油不溶性树脂的固化温度大于等于150℃；其中，苯酚：硼酸：硫酸铜：甲醇的质量比为1：0.9：0.015：1.2。本实施例的水不溶且油不溶性树脂低于150℃时是稳定的，当大于等于150℃时进入持续熔融状态，当温度进一步升高或维持当前温度一定时间后，其进入热固化状态。K2. Cool the crude product B to 80°C, then add formaldehyde to react, react for 4 hours below 100°C, stop heating, then cool down to below 70°C, discharge the material to a continuous cooling steel belt conveyor for cooling, and obtain water-insoluble and oily products. Insoluble resin; the curing temperature of water-insoluble and oil-insoluble resin is greater than or equal to 150°C; among them, the mass ratio of phenol: boric acid: copper sulfate: methanol is 1:0.9:0.015:1.2. The water-insoluble and oil-insoluble resin of this embodiment is stable when it is lower than 150°C. It enters a continuous melting state when it is greater than or equal to 150°C. When the temperature further increases or the current temperature is maintained for a certain period of time, it enters a thermal solidification state.
实施例3Example 3
一种石油钻井耐高温油基钻井液固结堵漏材料的堵漏浆料，其包括质量比为1:1的柴油与实施例1得到的石油钻井耐高温油基钻井液固结堵漏材料。A leakage plugging slurry for oil drilling and high temperature resistant oil-based drilling fluid consolidation and plugging materials, which includes diesel oil with a mass ratio of 1:1 and the oil drilling and high temperature resistant oil base drilling fluid consolidation and plugging material obtained in Example 1 .
堵漏浆料的使用方法如下：将堵漏浆料泵入井温为120℃左右的漏失段，在漏失压差的作用下粘合并固化成整体，得到油基堵漏结构。The method of using the lost circulation slurry is as follows: Pump the lost circulation slurry into the lost circulation section where the well temperature is about 120°C. It will be bonded and solidified into a whole under the action of the loss pressure difference to obtain an oil-based lost circulation structure.
实施例4Example 4
一种石油钻井耐高温油基钻井液固结堵漏材料的堵漏浆料，其包括质量比为1:1的柴油与实施例2得到的石油钻井耐高温油基钻井液固结堵漏材料。A leakage plugging slurry for oil drilling and high temperature resistant oil-based drilling fluid consolidation and plugging materials, which includes diesel oil with a mass ratio of 1:1 and the oil drilling and high temperature resistant oil base drilling fluid consolidation and plugging material obtained in Example 2 .
堵漏浆料的使用方法如下：将堵漏浆料泵入井温为150℃左右的漏失段，在漏失压差的作用下粘合成整体，得到油基堵漏结构。The method of using the lost circulation slurry is as follows: pump the lost circulation slurry into the lost circulation section where the well temperature is about 150°C, and bond it into a whole under the action of the loss pressure difference to obtain an oil-based lost circulation structure.
对比例1Comparative example 1
一种固结堵漏材料，其他内容与实施例1相同，所不同的是，组分中不加水不溶且油不溶性树脂。A kind of consolidated leakage plugging material, other contents are the same as those in Embodiment 1, except that no water-insoluble and oil-insoluble resin is added to the components.
将上述固结堵漏材料与柴油按照1:1的比例配比，得到堵漏浆料；堵漏浆料的使用方法如下：将堵漏浆料泵入井温为150℃左右的漏失段，在漏失压差的作用下粘合成整体，得到油基堵漏结构。Mix the above-mentioned consolidated lost circulation material and diesel oil in a ratio of 1:1 to obtain a lost circulation slurry; the method of using the lost circulation slurry is as follows: Pump the lost circulation slurry into the loss section with a well temperature of about 150°C, and Under the action of the leakage pressure difference, they are bonded into a whole body to obtain an oil-based leakage plugging structure.
评价测试Evaluation test
使用高温高压滤失仪模拟深井在高温高压条件下测试钻井液滤失量，步骤如下：Use a high-temperature and high-pressure filter loss instrument to simulate deep wells and test drilling fluid fluid loss under high-temperature and high-pressure conditions. The steps are as follows:
(1)料杯底层先铺垫20mm100目石英砂；料杯再铺垫20mm60目石英砂；(1) The bottom layer of the material cup is first paved with 20mm100 mesh quartz sand; the material cup is then paved with 20mm60 mesh quartz sand;
(2)取400ml 0#柴油加入高搅杯中；取120g实施例或对比例的堵漏材料加入高搅杯中；12000rpm，搅拌5分钟待用；(2) Take 400ml of 0# diesel and add it to the high stirring cup; take 120g of the leak-stopping material of the Example or Comparative Example and add it to the high stirring cup; stir at 12000rpm for 5 minutes and set aside;
(3)将已经搅拌好的油基料浆倒满已经铺垫两层石英砂的料杯，紧固上盖；(3) Pour the mixed oil-based slurry into the material cup that has been paved with two layers of quartz sand, and tighten the upper cover;
(4)接好料杯上下配件及气管，打开下排料阀，接好上部气管；(4) Connect the upper and lower fittings of the material cup and the air pipe, open the lower discharge valve, and connect the upper air pipe;
(5)调整料杯上进气阀缓慢升压到0.7Mpa，维持5分钟；关闭下排料阀；维持0.7Mpa，关闭上进气阀；(5) Adjust the air inlet valve on the material cup to slowly increase the pressure to 0.7Mpa and maintain it for 5 minutes; close the lower discharge valve; maintain 0.7Mpa and close the upper air inlet valve;
(6)打开电源，升温到设定温度120℃，维持2小时；(6) Turn on the power, raise the temperature to the set temperature of 120°C, and maintain it for 2 hours;
(7)冷却降温到室温，卸开料筒上盖，倒出多余料浆；(7) Cool to room temperature, remove the upper cover of the barrel, and pour out excess slurry;
(8)卸开料筒下盖，顶出桶内的固结材料。(8) Remove the lower cover of the barrel and eject the consolidated material in the barrel.
经过上述测试，方案实施例1、2的堵漏材料在步骤(8)顶出的桶内材料与上层石英砂固结成一体，外观完整，规整切割整形为抗压试样后，20Mpa≧抗压强度≧4Mpa。而对比例1的堵漏材料固化不成型。After the above tests, the leak-stopping materials of Scheme Examples 1 and 2 were consolidated into one body with the upper layer of quartz sand ejected in step (8), and the appearance was complete. After being neatly cut and shaped into compression specimens, the resistance was 20Mpa≧ Compressive strength ≧4Mpa. However, the leak-stopping material of Comparative Example 1 solidified and did not take shape.
以上，仅为本发明较佳的具体实施方式，但本发明的保护范围并不局限于此，任何熟悉本技术领域的技术人员在本发明揭露的技术范围内，可轻易想到的变化或替换，都应涵盖在本发明的保护范围之内。The above are only preferred specific embodiments of the present invention, but the protection scope of the present invention is not limited thereto. Any person familiar with the technical field can easily think of changes or substitutions within the technical scope disclosed in the present invention. All are covered by the protection scope of the present invention.
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| CN202311416642.5ACN117567997B (en) | 2023-10-30 | 2023-10-30 | High temperature resistant oil-based drilling fluid consolidation plugging material for petroleum drilling and use method thereof |
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