CN114806535A - A modified nano-silica fluid and its preparation method and application, a slick water fracturing fluid and its application - Google Patents

A modified nano-silica fluid and its preparation method and application, a slick water fracturing fluid and its application Download PDF

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CN114806535A
CN114806535A CN202210404396.0A CN202210404396A CN114806535A CN 114806535 A CN114806535 A CN 114806535A CN 202210404396 A CN202210404396 A CN 202210404396A CN 114806535 A CN114806535 A CN 114806535A
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张甜甜
李治平
高明伟
杨婕
邹家乐
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China University of Geosciences Beijing
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Abstract

本发明提供了一种改性纳米二氧化硅流体及其制备方法和应用、一种滑溜水压裂液及其应用,属于页岩油开发技术领域。本发明的改性纳米二氧化硅流体可通过静电作用等方式增强改性纳米二氧化硅和滑溜水压裂液的相互作用,有效降低油水界面张力,以及改变润湿性。利用本发明改性纳米二氧化硅流体制备的滑溜水压裂液能够在油‑水‑岩石三相接触区形成楔形结构,所产生的结构分离压将原油从岩石表面剥离下来,从而提高渗吸采收率。实施例结果表明,改性后纳米二氧化硅流体的渗吸采收率最高达到12%,同时其界面张力降低至了0.11mN/m,润湿转变最高达到了158°,在8h油滴剥离的实验中达到了151°。

Figure 202210404396

The invention provides a modified nano-silica fluid, a preparation method and application thereof, a slick water fracturing fluid and application thereof, belonging to the technical field of shale oil development. The modified nano-silica fluid of the present invention can enhance the interaction between the modified nano-silica and the slick water fracturing fluid through electrostatic action, etc., effectively reduce the oil-water interfacial tension, and change the wettability. The slick water fracturing fluid prepared by using the modified nano-silica fluid of the present invention can form a wedge-shaped structure in the oil-water-rock three-phase contact zone, and the generated structural separation pressure peels off the crude oil from the rock surface, thereby improving imbibition recovery rate. The results of the examples show that the maximum imbibition recovery rate of the modified nano-silica fluid reaches 12%, while the interfacial tension is reduced to 0.11mN/m, and the wetting transition reaches a maximum of 158°, and the oil droplets peel off in 8h. 151° was reached in the experiment.

Figure 202210404396

Description

一种改性纳米二氧化硅流体及其制备方法和应用、一种滑溜 水压裂液及其应用A modified nano-silica fluid and its preparation method and application, a slick water fracturing fluid and its application

技术领域technical field

本发明属于页岩油开发技术领域,具体涉及一种改性纳米二氧化硅流体及其制备方法和应用、一种滑溜水压裂液及其应用。The invention belongs to the technical field of shale oil development, and in particular relates to a modified nano-silica fluid, a preparation method and application thereof, a slick water fracturing fluid and its application.

背景技术Background technique

页岩油已成为全球非常规油气资源勘探开发的热点,影响各国能源战略布局。在页岩油的开发过程中,渗吸置换开采技术已成为提高单井产量,延长生产有效期的重要研究方向,通过在入井流体中加入表面活性剂改变储层的润湿性能,从而借助毛细管力的驱动,使入井流体能够自发的渗吸进入基质岩石的细微孔道中,通过油水置换,将原油逐渐汇集到大孔道中,进而实现补充地层能量,提高终采收率的目的。Shale oil has become a hot spot in the exploration and development of unconventional oil and gas resources in the world, affecting the strategic layout of energy in various countries. In the development process of shale oil, the imbibition replacement technology has become an important research direction to improve the single well production and prolong the production validity period. The driving of the well inlet fluid can spontaneously imbibe into the fine pores of the matrix rock, and through oil-water replacement, the crude oil is gradually collected into the large pores, thereby realizing the purpose of supplementing the formation energy and improving the final recovery rate.

渗析置换开采技术中的滑溜水力压裂技术由于其成本低、对储层伤害性小且具有较高的支撑剂裂缝导流能力已经成为页岩油开采的核心技术之一。但是现有滑溜水压裂液主要由聚合物类减阻剂和少量助排剂、防膨剂构成,仍存在渗析采收率低的问题。Slippery hydraulic fracturing technology in dialysis replacement production technology has become one of the core technologies of shale oil production due to its low cost, little damage to the reservoir and high fracture conductivity of proppant. However, the existing slick water fracturing fluid is mainly composed of polymer drag reducing agent and a small amount of drainage aid and anti-swelling agent, and there is still the problem of low dialysis recovery.

发明内容SUMMARY OF THE INVENTION

本发明的目的在于提供一种改性纳米二氧化硅流体及其制备方法和应用、一种滑溜水压裂液及其应用,能够提高页岩油藏的采收率。The purpose of the present invention is to provide a modified nano-silica fluid and its preparation method and application, a slick water fracturing fluid and its application, which can improve the recovery rate of shale oil reservoirs.

本发明提供了一种改性纳米二氧化硅流体,包括以下制备原料:The invention provides a modified nano-silica fluid, comprising the following preparation raw materials:

Figure BDA0003601216360000011
Figure BDA0003601216360000011

所述亲水型纳米二氧化硅溶胶中二氧化硅的质量含量为20~40%;The mass content of silica in the hydrophilic nano-silica sol is 20-40%;

所述改性剂包括烷基葡萄糖苷、烷基聚氧乙烯醚、烷基硫酸钠、烷基磺酸钠、α-烯基磺酸钠、烷基醇磷酸酯钠、烷基羧基甜菜碱和烷基羟丙基磺基甜菜碱的一种或多种。The modifiers include alkyl glucoside, alkyl polyoxyethylene ether, sodium alkyl sulfate, sodium alkyl sulfonate, sodium α-alkenyl sulfonate, sodium alkyl alcohol phosphate, alkyl carboxybetaine and One or more of Alkyl Hydroxypropyl Sultaines.

优选的,所述亲水型纳米二氧化硅溶胶的平均粒径为8~15nm。Preferably, the average particle size of the hydrophilic nano-silica sol is 8-15 nm.

优选的,所述稳定剂包括第一低温稳定剂和第二低温稳定剂;所述第一低温稳定剂、第二低温稳定剂的质量分别独立地占所述改性纳米二氧化硅流体的5~15%;Preferably, the stabilizer includes a first low temperature stabilizer and a second low temperature stabilizer; the mass of the first low temperature stabilizer and the second low temperature stabilizer independently account for 5% of the modified nano-silica fluid. ~15%;

所述第一稳定剂包括氯化钠、氯化铵和尿素的一种或多种;The first stabilizer includes one or more of sodium chloride, ammonium chloride and urea;

所述第二稳定剂包括异丁醇、丙二醇、正丁醇、乙醇和甲醇的一种或多种。The second stabilizer includes one or more of isobutanol, propylene glycol, n-butanol, ethanol and methanol.

本发明还提供了上述方案所述改性纳米二氧化硅流体的制备方法,包括以下步骤:将亲水型纳米二氧化硅溶胶、改性剂、低温稳定剂和水混合进行改性,得到改性纳米二氧化硅流体;The present invention also provides a method for preparing the modified nano-silica fluid according to the above scheme, which includes the following steps: mixing and modifying the hydrophilic nano-silica sol, a modifier, a low-temperature stabilizer and water to obtain the modified nano-silica sol. Sexual nano silica fluid;

所述改性的温度为70~90℃。The temperature of the modification is 70-90°C.

本发明还提供了上述方案所述改性纳米二氧化硅流体或上述方案所述制备方法制得的改性纳米二氧化硅流体在页岩油开发中的应用。The present invention also provides the application of the modified nano-silica fluid described in the above scheme or the modified nano-silica fluid prepared by the preparation method described in the above scheme in the development of shale oil.

本发明还提供了一种滑溜水压裂液,包括以下组分:The present invention also provides a slick water fracturing fluid, comprising the following components:

Figure BDA0003601216360000021
Figure BDA0003601216360000021

所述改性纳米二氧化硅流体为上述方案所述的改性纳米二氧化硅流体或上述方案所述制备方法制得的改性纳米二氧化硅流体。The modified nano-silica fluid is the modified nano-silica fluid described in the above scheme or the modified nano-silica fluid prepared by the preparation method described in the above scheme.

优选的,所述减阻剂包括聚丙烯酰胺、部分水解聚丙烯酰胺、阳离子型聚丙烯酰胺、两性聚丙烯酰胺、胍胶、阳离子改性胍胶和羟丙基胍胶中的一种或多种。Preferably, the drag reducing agent comprises one or more of polyacrylamide, partially hydrolyzed polyacrylamide, cationic polyacrylamide, amphoteric polyacrylamide, guar gum, cationically modified guar gum and hydroxypropyl guar gum kind.

优选的,所述的多功能添加剂包括氯化钾、四甲基丙二胺与二氯丙烷的共聚物、四甲基乙二胺与二氯乙烷的共聚物和聚二烯丙基二甲基氯化铵的一种或多种与戊二醛和/或氯苯氧化物的混合物。Preferably, the multifunctional additives include potassium chloride, copolymers of tetramethylpropylenediamine and dichloropropane, copolymers of tetramethylethylenediamine and dichloroethane, and polydiallyl dimethyl A mixture of one or more ammonium chlorides with glutaraldehyde and/or chlorophenoxide.

本发明还提供了上述方案所述滑溜水压裂液在页岩油开发中的应用。The present invention also provides the application of the slick water fracturing fluid described in the above solution in the development of shale oil.

优选的,所述应用包括以下步骤:Preferably, the application includes the following steps:

将滑溜水压裂液泵入地层,形成裂缝后,向地层中泵入滑溜水压裂液和支撑剂的混合物使支撑剂支撑所述裂缝;然后继续泵入滑溜水压裂液,将井筒中支撑剂挤入储层中;不进行反排,闷井3~28天。The slick water fracturing fluid is pumped into the formation, and after the fracture is formed, a mixture of slick water fracturing fluid and proppant is pumped into the formation to make the proppant support the fracture; The proppant is squeezed into the reservoir; no reverse drainage is performed, and the well is stuffed for 3 to 28 days.

本发明提供了一种改性纳米二氧化硅流体,包括以下制备原料:亲水型纳米二氧化硅溶胶30wt%;改性剂30wt%;低温稳定剂20~30wt%;余量为水;所述亲水型纳米二氧化硅溶胶中二氧化硅的质量含量为40%;所述改性剂包括烷基葡萄糖苷、烷基聚氧乙烯醚、烷基硫酸钠、烷基磺酸钠、α-烯基磺酸钠、烷基醇磷酸酯钠、烷基羧基甜菜碱和烷基羟丙基磺基甜菜碱的一种或多种。本发明的改性纳米二氧化硅流体用于滑溜水压裂液中时,可通过静电作用、范德华力、氢键等方式增强改性纳米二氧化硅和滑溜水压裂液的相互作用,有效降低油水界面张力,以及改变储层岩石润湿性。利用本发明改性纳米二氧化硅流体制备的滑溜水压裂液可以在油-水-固三相接触区富集特性,在油-水-岩石三相接触区形成楔形结构,所产生的结构分离压将原油从岩石表面剥离下来,从而提高渗吸采收率。实施例结果表明,改性后纳米二氧化硅流体的渗吸采收率最高达到12%,同时其界面张力降低至了0.11mN/m,润湿转变最高达到了158°,在8h油滴剥离的实验中达到了151°。The invention provides a modified nano-silica fluid, comprising the following preparation raw materials: hydrophilic nano-silica sol 30wt%; modifier 30wt%; low temperature stabilizer 20-30wt%; the balance is water; The mass content of silica in the hydrophilic nano-silica sol is 40%; the modifier includes alkyl glucoside, alkyl polyoxyethylene ether, sodium alkyl sulfate, sodium alkyl sulfonate, alpha - One or more of sodium alkenyl sulfonate, sodium alkyl alcohol phosphate, alkyl carboxybetaine and alkyl hydroxypropyl sulfobetaine. When the modified nano-silica fluid of the present invention is used in slick water fracturing fluid, the interaction between the modified nano-silica and slick water fracturing fluid can be enhanced by electrostatic action, van der Waals force, hydrogen bonding, etc. Reduce oil-water interfacial tension and change reservoir rock wettability. The slick water fracturing fluid prepared by using the modified nano-silica fluid of the present invention can be enriched in the oil-water-solid three-phase contact area, and form a wedge-shaped structure in the oil-water-rock three-phase contact area. Separation pressure strips crude oil from the rock surface, thereby enhancing imbibition recovery. The results of the examples show that the maximum imbibition recovery rate of the modified nano-silica fluid reaches 12%, while the interfacial tension is reduced to 0.11mN/m, and the wetting transition reaches a maximum of 158°, and the oil droplets peel off in 8h. 151° was reached in the experiment.

本发明提供了一种滑溜水压裂液,通过改性纳米二氧化硅流体与减阻剂、多功能添加剂三者之间的协同增效作用,使本发明中的滑溜水压裂液具有优异的分散稳定性、减阻性、携砂性和造缝能力。实施例结果表明,本发明提供的滑溜水压裂液渗吸采收率最高为16.1%,减阻率最高为83.5%。The present invention provides a slick water fracturing fluid. Through the synergistic effect between the modified nano-silica fluid, drag reducing agent and multifunctional additive, the slick water fracturing fluid of the present invention has excellent performance. Dispersion stability, drag reduction, sand carrying and seam-making ability. The results of the examples show that the maximum imbibition recovery rate of the slick water fracturing fluid provided by the present invention is 16.1%, and the maximum drag reduction rate is 83.5%.

附图说明Description of drawings

为了更清楚地说明本发明实施例或现有技术中的技术方案,下面将对实施例中所需要使用的附图作简单地介绍,显而易见地,下面描述中的附图仅仅是本发明的一些实施例,对于本领域普通技术人员来讲,在不付出创造性劳动性的前提下,还可以根据这些附图获得其他的附图。In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the accompanying drawings required in the embodiments will be briefly introduced below. Obviously, the drawings in the following description are only some of the present invention. In the embodiments, for those of ordinary skill in the art, other drawings can also be obtained according to these drawings without creative labor.

图1为对比例2~3和实施例1~8中所用亲水型纳米二氧化硅溶胶的SEM图;Fig. 1 is the SEM image of the hydrophilic nano-silica sol used in Comparative Examples 2-3 and Examples 1-8;

图2为对比例3制备得到的改性纳米二氧化硅流体的SEM图;Fig. 2 is the SEM image of the modified nano-silica fluid prepared by comparative example 3;

图3为对比例2~3和实施例1~8中所用亲水型纳米二氧化硅溶胶与对比例3制备得到的改性纳米二氧化硅流体的DLS图。3 is a DLS diagram of the hydrophilic nano-silica sol used in Comparative Examples 2-3 and Examples 1-8 and the modified nano-silica fluid prepared in Comparative Example 3. FIG.

具体实施方式Detailed ways

本发明提供了一种改性纳米二氧化硅流体,包括以下制备原料:The invention provides a modified nano-silica fluid, comprising the following preparation raw materials:

Figure BDA0003601216360000031
Figure BDA0003601216360000031

所述亲水型纳米二氧化硅溶胶中二氧化硅的质量含量为20~40%;The mass content of silica in the hydrophilic nano-silica sol is 20-40%;

所述改性剂包括烷基葡萄糖苷、烷基聚氧乙烯醚、烷基硫酸钠、烷基磺酸钠、α-烯基磺酸钠、烷基醇磷酸酯钠、烷基羧基甜菜碱和烷基羟丙基磺基甜菜碱的一种或多种。The modifiers include alkyl glucoside, alkyl polyoxyethylene ether, sodium alkyl sulfate, sodium alkyl sulfonate, sodium α-alkenyl sulfonate, sodium alkyl alcohol phosphate, alkyl carboxybetaine and One or more of Alkyl Hydroxypropyl Sultaines.

本发明中所述改性纳米二氧化硅流体的粒径优选为1~100nm,更优选为5~20nm。The particle size of the modified nano-silica fluid in the present invention is preferably 1-100 nm, more preferably 5-20 nm.

以质量百分数计,本发明提供的改性纳米二氧化硅流体的制备原料包括亲水型纳米二氧化硅溶胶20~40wt%,更优选为25~35wt%;所述亲水型纳米二氧化硅溶胶中二氧化硅的质量含量为20~40wt%,更优选为25~35wt%。在本发明中,所述亲水型纳米二氧化硅溶胶的平均粒径优选为8~15nm,更优选为10~12nm;密度优选为1.28~1.30g/mL,更优选为1.29g/mL;pH值优选为7~11,更优选为7.5~9.5。In terms of mass percentage, the preparation raw materials of the modified nano-silica fluid provided by the present invention include 20-40 wt% of hydrophilic nano-silica sol, more preferably 25-35 wt%; the hydrophilic nano-silica The mass content of silica in the sol is 20-40 wt %, more preferably 25-35 wt %. In the present invention, the average particle size of the hydrophilic nano-silica sol is preferably 8-15 nm, more preferably 10-12 nm; the density is preferably 1.28-1.30 g/mL, more preferably 1.29 g/mL; The pH value is preferably 7 to 11, and more preferably 7.5 to 9.5.

本发明提供的改性纳米二氧化硅流体的制备原料包括改性剂20~40wt%,更优选为25~35wt%。在本发明中,所述改性剂包括烷基葡萄糖苷、烷基聚氧乙烯醚、烷基硫酸钠、烷基磺酸钠、α-烯基磺酸钠、烷基醇磷酸酯钠、烷基羧基甜菜碱和烷基羟丙基磺基甜菜碱的一种或多种,优选为两种及两种以上的改性剂组成,更优选为由三种改性剂组成。在本发明中,所述改性剂中C原子的数量优选为12~16,更优选为13~15。在本发明的实施例中,具体选用C原子的数量为12(如十二烷基磺酸钠、十二烷基羟丙基磺基甜菜碱)和/或14(如十四烷基羧基甜菜碱、十四烷基硫酸钠、十四烷基聚氧乙烯醚)的改性剂。本发明中改性剂的作用是对亲水型纳米二氧化硅溶胶进行改性,使其具有活性。The preparation raw material of the modified nano-silica fluid provided by the present invention includes 20-40 wt% of the modifier, more preferably 25-35 wt%. In the present invention, the modifier includes alkyl glucoside, alkyl polyoxyethylene ether, sodium alkyl sulfate, sodium alkyl sulfonate, sodium α-alkenyl sulfonate, sodium alkyl alcohol phosphate, alkyl alcohol One or more of carboxybetaine and alkylhydroxypropyl sulfobetaine, preferably two or more modifiers, more preferably three modifiers. In the present invention, the number of C atoms in the modifier is preferably 12-16, more preferably 13-15. In the embodiment of the present invention, the number of specific C atoms selected is 12 (such as sodium dodecyl sulfonate, dodecyl hydroxypropyl sulfobetaine) and/or 14 (such as tetradecyl carboxy betaine) Alkali, sodium tetradecyl sulfate, tetradecyl polyoxyethylene ether) modifier. The function of the modifier in the present invention is to modify the hydrophilic nano-silica sol to make it active.

本发明提供的改性纳米二氧化硅流体的制备原料包括低温稳定剂10~30wt%。在本发明中,所述稳定剂优选包括第一低温稳定剂和第二低温稳定剂;所述第一低温稳定剂、第二低温稳定剂的质量优选分别独立地占所述改性纳米二氧化硅流体的5~15%,更优选为8~12wt%。在本发明中,所述第一稳定剂优选包括氯化钠、氯化铵和尿素的一种或多种;所述第二稳定剂优选包括异丁醇、丙二醇、正丁醇、乙醇和甲醇的一种或多种。在本发明中,第一稳定剂的作用是降低改性纳米二氧化硅流体的冰点,并防止亲水型纳米二氧化硅溶胶和改性剂低温析出;所述第二稳定剂的作用是降低改性纳米二氧化硅流体的冰点,并减小改性纳米二氧化硅流体的粘度,增强注入性。低温稳定剂使改性纳米二氧化硅流体在储藏温度为-5℃及以上时可维持体系均一不结冰。The preparation raw materials of the modified nano-silica fluid provided by the present invention include 10-30 wt% of a low-temperature stabilizer. In the present invention, the stabilizer preferably includes a first low temperature stabilizer and a second low temperature stabilizer; the quality of the first low temperature stabilizer and the second low temperature stabilizer preferably respectively independently account for the modified nano-dioxide 5 to 15% of the silicon fluid, more preferably 8 to 12 wt%. In the present invention, the first stabilizer preferably includes one or more of sodium chloride, ammonium chloride and urea; the second stabilizer preferably includes isobutanol, propylene glycol, n-butanol, ethanol and methanol one or more of. In the present invention, the function of the first stabilizer is to reduce the freezing point of the modified nano-silica fluid and prevent the hydrophilic nano-silica sol and the modifier from precipitation at low temperature; the function of the second stabilizer is to reduce the The freezing point of the modified nano-silica fluid is reduced, the viscosity of the modified nano-silica fluid is reduced, and the injectability is enhanced. The low-temperature stabilizer enables the modified nano-silica fluid to maintain a uniform system without freezing when the storage temperature is -5 °C and above.

本发明还提供了上述方案所述改性纳米二氧化硅流体的制备方法,包括以下步骤:将亲水型纳米二氧化硅溶胶、改性剂、低温稳定剂和水混合进行改性,得到改性纳米二氧化硅流体;The present invention also provides a method for preparing the modified nano-silica fluid according to the above scheme, which includes the following steps: mixing and modifying the hydrophilic nano-silica sol, a modifier, a low-temperature stabilizer and water to obtain the modified nano-silica sol. Sexual nano silica fluid;

所述改性的温度为70~90℃。The temperature of the modification is 70-90°C.

在本发明中,所述将亲水型纳米二氧化硅溶胶、改性剂、低温稳定剂和水混合优选包括:将水加热至改性的温度,加热期间向水中加入低温稳定剂,然后向所得第一混合液中加入亲水型纳米二氧化硅溶胶,再向所得第二混合液中加入改性剂。In the present invention, the mixing of the hydrophilic nano-silica sol, the modifier, the low-temperature stabilizer and the water preferably includes: heating the water to a modified temperature, adding the low-temperature stabilizer to the water during the heating, and then adding the low-temperature stabilizer to the water. The hydrophilic nano-silica sol is added to the obtained first mixed solution, and then a modifier is added to the obtained second mixed solution.

在本发明中,所述混合优选在搅拌条件下进行。加入亲水型纳米二氧化硅溶胶后本发明优选搅拌1h。In the present invention, the mixing is preferably carried out under stirring conditions. The present invention preferably stirs for 1h after adding the hydrophilic nano-silica sol.

在本发明中,所述改性的温度为70~90℃,优选为75~85℃;所述改性的时间优选为2~5h,更优选为3~4h。在本发明中,所述改性优选在搅拌条件下进行。改性后纳米流体活性升高,耐温耐盐性能增强。将改性的温度控制在上述范围,改性的效果最佳且改性后体系稳定。若温度过高或过低,产物性能不稳定且反应效率差。In the present invention, the modification temperature is 70-90°C, preferably 75-85°C; the modification time is preferably 2-5h, more preferably 3-4h. In the present invention, the modification is preferably carried out under stirring conditions. After modification, the activity of the nanofluid increases, and the temperature and salt resistance performance is enhanced. When the temperature of modification is controlled within the above range, the effect of modification is the best and the system after modification is stable. If the temperature is too high or too low, the product properties are unstable and the reaction efficiency is poor.

完成所述改性后,本发明优选将所得改性产物搅拌至其温度降至室温,得到改性纳米二氧化硅流体。After completing the modification, the present invention preferably stirs the obtained modified product until its temperature drops to room temperature to obtain a modified nano-silica fluid.

本发明还提供了上述方案所述改性纳米二氧化硅流体或上述方案所述制备方法制得的改性纳米二氧化硅流体在页岩油开发中的应用。The present invention also provides the application of the modified nano-silica fluid described in the above scheme or the modified nano-silica fluid prepared by the preparation method described in the above scheme in the development of shale oil.

在本发明中,所述应用优选包括以下步骤:将活性纳米流体泵入地层闷井3~28天后开井生产。In the present invention, the application preferably includes the following steps: pumping the active nanofluid into the formation for 3-28 days and then opening the well for production.

在本发明中,所述的改性纳米二氧化硅流体适用的页岩油储层条件优选为矿化度处于0~80000mg/L之间,温度优选处于室温至120℃之间。In the present invention, the suitable shale oil reservoir conditions for the modified nano-silica fluid are preferably a salinity between 0 and 80000 mg/L, and a temperature between room temperature and 120°C.

本发明还提供了一种滑溜水压裂液,包括以下组分:The present invention also provides a slick water fracturing fluid, comprising the following components:

Figure BDA0003601216360000051
Figure BDA0003601216360000051

所述改性纳米二氧化硅流体为上述方案所述的改性纳米二氧化硅流体或上述方案所述制备方法制得的改性纳米二氧化硅流体。The modified nano-silica fluid is the modified nano-silica fluid described in the above scheme or the modified nano-silica fluid prepared by the preparation method described in the above scheme.

以质量百分数计,本发明提供的滑溜水压裂液包括改性纳米二氧化硅流体0.05~0.5wt%,优选为0.1~0.4wt%,更优选为0.2~0.3wt%。In terms of mass percentage, the slick water fracturing fluid provided by the present invention comprises 0.05-0.5wt% of modified nano-silica fluid, preferably 0.1-0.4wt%, more preferably 0.2-0.3wt%.

本发明提供的滑溜水压裂液包括减阻剂0.05~0.5wt%,优选为0.1~0.4wt%,更优选为0.2~0.3wt%。本发明所述减阻剂优选包括聚丙烯酰胺、部分水解聚丙烯酰胺、阳离子型聚丙烯酰胺、两性聚丙烯酰胺、胍胶、阳离子改性胍胶和羟丙基胍胶中的一种或多种,更优选为两性聚丙烯酰胺。在本发明中,所述聚丙烯酰胺的分子量优选为100~900万,所述阳离子型聚丙烯酰胺的分子量优选为100~600万,所述两性聚丙烯酰胺的分子量优选为100~500万,所述部分水解聚丙烯酰胺的水解度优选为1~10%,分子量优选为100~700万。The slick water fracturing fluid provided by the present invention includes 0.05-0.5wt% of drag reducing agent, preferably 0.1-0.4wt%, more preferably 0.2-0.3wt%. The drag reducing agent of the present invention preferably comprises one or more of polyacrylamide, partially hydrolyzed polyacrylamide, cationic polyacrylamide, amphoteric polyacrylamide, guar gum, cationically modified guar gum and hydroxypropyl guar gum species, more preferably amphoteric polyacrylamide. In the present invention, the molecular weight of the polyacrylamide is preferably 1 to 9 million, the molecular weight of the cationic polyacrylamide is preferably 1 to 6 million, and the molecular weight of the amphoteric polyacrylamide is preferably 1 to 5 million. The degree of hydrolysis of the partially hydrolyzed polyacrylamide is preferably 1-10%, and the molecular weight is preferably 1-7 million.

当所述减阻剂优选包括分子量为100~900万的聚丙烯酰胺、水解度为1~10%、分子量为100~700万的部分水解聚丙烯酰胺和分子量为100~500万两性聚丙烯酰胺时,上述3种减阻剂的质量之和不得小于减阻剂总质量的80%。When the drag reducing agent preferably includes polyacrylamide with a molecular weight of 1 to 9 million, a degree of hydrolysis of 1 to 10%, a partially hydrolyzed polyacrylamide with a molecular weight of 1 to 7 million, and an amphoteric polyacrylamide with a molecular weight of 1 to 5 million , the sum of the mass of the above three drag reducing agents shall not be less than 80% of the total mass of the drag reducing agents.

当所述减阻剂优选包括分子量为100~600万的阳离子型聚丙烯酰胺、胍胶、阳离子改性胍胶和羟丙基胍胶时,上述4种减阻剂的质量之和不得大于减阻剂总质量的20%。When the drag reducing agent preferably includes cationic polyacrylamide, guar gum, cationic modified guar gum and hydroxypropyl guar gum with a molecular weight of 1 million to 6 million, the sum of the masses of the above four drag reducing agents shall not be greater than 20% of the total mass of the resist.

在本发明中,所述减阻剂中分子量为100~600万的阳离子型聚丙烯酰胺和阳离子改性胍胶均不得与水解度为1~10%、分子量为100~700万的部分水解聚丙烯酰胺同时使用。若同时使用会聚沉而失效。In the present invention, the cationic polyacrylamide and the cationic modified guar gum with a molecular weight of 1 to 6 million in the drag reducing agent must not be polymerized with a partially hydrolyzed polymer with a degree of hydrolysis of 1 to 10% and a molecular weight of 1 to 7 million. Acrylamide is used simultaneously. If used at the same time, it will fail to converge.

本发明提供的滑溜水压裂液包括多功能添加剂0.1~0.5wt%,优选为0.2~0.4%。在本发明中,所述多功能添加剂优选包括氯化钾、四甲基丙二胺与二氯丙烷的共聚物、四甲基乙二胺与二氯乙烷的共聚物和聚二烯丙基二甲基氯化铵的一种或多种与戊二醛和/或氯苯氧化物的混合物。The slick water fracturing fluid provided by the present invention comprises 0.1-0.5wt% of multifunctional additives, preferably 0.2-0.4%. In the present invention, the multifunctional additive preferably includes potassium chloride, a copolymer of tetramethylpropylenediamine and dichloropropane, a copolymer of tetramethylethylenediamine and dichloroethane, and polydiallyl A mixture of one or more of dimethylammonium chloride with glutaraldehyde and/or chlorophenoxide.

在本发明中,所述四甲基丙二胺与二氯丙烷共聚物的共聚比优选为1:0.9~0.95,更优选为1:0.92~0.94;所述的四甲基乙二胺与二氯乙烷共聚物的共聚比优选为1:0.9~0.95,更优选为1:0.92~0.94。In the present invention, the copolymerization ratio of the tetramethylpropylenediamine and dichloropropane copolymer is preferably 1:0.9-0.95, more preferably 1:0.92-0.94; the tetramethylethylenediamine and dichloropropane copolymer The copolymerization ratio of the ethylene chloride copolymer is preferably 1:0.9 to 0.95, and more preferably 1:0.92 to 0.94.

在本发明中,所述多功能添加剂中氯化钾、四甲基丙二胺与二氯丙烷共聚物、四甲基乙二胺与二氯乙烷共聚物、聚二烯丙基二甲基氯化铵的一种或多种的重量之和优选为多功能添加剂总量的40%~60%,余量优选为戊二醛和/或氯苯氧化物。所述氯苯氧化物优选为氧化氯苯或氯苯嘧啶醇。本发明中的多功能添加剂作用为防膨和杀菌。In the present invention, among the multifunctional additives, potassium chloride, tetramethylpropylenediamine and dichloropropane copolymer, tetramethylethylenediamine and dichloroethane copolymer, polydiallyl dimethyl The weight sum of one or more ammonium chlorides is preferably 40% to 60% of the total amount of the multifunctional additive, and the balance is preferably glutaraldehyde and/or chlorophenoxide. The chlorophenoxide is preferably chlorobenzene oxide or chlorophenidol. The functions of the multifunctional additive in the present invention are anti-swelling and sterilization.

本发明对所述滑溜水压裂液的制备方法没有特殊要求,直接将各组分混合均匀即可。在本发明的实施例中,具体为:将改性纳米二氧化硅流体、多功能添加剂加入到水中搅拌5~10min,然后加入减阻剂搅拌10~35min,得到滑溜水压裂液。The present invention has no special requirements on the preparation method of the slick water fracturing fluid, and the components can be directly mixed uniformly. In the embodiment of the present invention, it is specifically as follows: adding the modified nano-silica fluid and multifunctional additives into water and stirring for 5-10 minutes, and then adding a drag reducing agent and stirring for 10-35 minutes to obtain a slick water fracturing fluid.

本发明通过减阻剂、改性纳米二氧化硅流体、多功能添加剂三者之间的协同增效作用,不仅具有优于常规滑溜水压裂液的优异的减阻性、携砂性和造缝能力,同时具有独特的界面活性,能够有效降低界面张力、改变润湿性和油滴剥离,使其具有优异的渗吸排油能力。Through the synergistic effect among the drag reducing agent, the modified nano-silica fluid and the multifunctional additive, the present invention not only has the excellent drag reducing property, sand carrying property and creating property better than the conventional slick water fracturing fluid At the same time, it has unique interfacial activity, which can effectively reduce interfacial tension, change wettability and oil droplet peeling, so that it has excellent oil absorption and drainage ability.

本发明还提供了上述方案所述滑溜水压裂液在页岩油开发中的应用。所述应用的方法优选包括以下步骤:The present invention also provides the application of the slick water fracturing fluid described in the above solution in the development of shale oil. The method of said application preferably comprises the following steps:

将滑溜水压裂液泵入地层,形成裂缝后,向地层中泵入滑溜水压裂液和支撑剂的混合物使支撑剂支撑所述裂缝;然后继续泵入滑溜水压裂液,将井筒中支撑剂挤入储层中;不进行反排,闷井3~28天。The slick water fracturing fluid is pumped into the formation, and after the fracture is formed, a mixture of slick water fracturing fluid and proppant is pumped into the formation to make the proppant support the fracture; The proppant is squeezed into the reservoir; no reverse drainage is performed, and the well is stuffed for 3 to 28 days.

本发明对所述应用过程中各个步骤的实施条件没有特殊要求,采用本领域技术人员熟知的实施条件即可。The present invention has no special requirements on the implementation conditions of each step in the application process, and the implementation conditions well known to those skilled in the art can be used.

本发明的滑溜水压裂液体系在满足页岩油储层压裂施工需求的前提下,压裂施工后无需反排,可充分利用压裂能量和压裂液,后直接闷井3~28天后开井生产,绿色环保、降本增效。On the premise that the slick water fracturing fluid system of the present invention meets the requirements of shale oil reservoir fracturing construction, it does not need backflow after fracturing construction, and can fully utilize fracturing energy and fracturing fluid, and then directly fill up wells for 3-28 Tianhou opened a well for production, which is green and environmentally friendly, reducing costs and increasing efficiency.

为了进一步说明本发明,下面结合附图和实施例对本发明提供的一种改性纳米二氧化硅流体及其制备方法和应用、一种滑溜水压裂液及其应用进行详细地描述,但不能将它们理解为对本发明保护范围的限定。In order to further illustrate the present invention, a modified nano-silica fluid and its preparation method and application, a slick water fracturing fluid and its application provided by the present invention are described in detail below with reference to the accompanying drawings and examples, but not They are to be understood as limiting the scope of protection of the present invention.

改性纳米二氧化硅流体Modified Nano Silica Fluid

对比例1~3和实施例1~8的改性纳米二氧化硅流体的制备方法,步骤如下:The preparation methods of the modified nano-silica fluids of Comparative Examples 1-3 and Examples 1-8, the steps are as follows:

将水加热至80℃,期间向水中加入第一低温稳定剂和第一低温稳定剂搅拌均匀,将亲水型纳米二氧化硅溶胶缓慢加入反应容器后持续搅拌1h,将改性剂缓慢加入反应容器后搅拌3h,停止加热,利用余热继续搅拌至冷却至室温即获得改性纳米二氧化硅流体。Heat the water to 80°C, add the first low-temperature stabilizer and the first low-temperature stabilizer to the water and stir evenly, slowly add the hydrophilic nano-silica sol to the reaction vessel and continue stirring for 1 h, and slowly add the modifier to the reaction After the container was stirred for 3 hours, the heating was stopped, and the residual heat was used to continue stirring until it was cooled to room temperature to obtain the modified nano-silica fluid.

对比例1~3和实施例1~8中改性纳米二氧化硅流体总质量为100g,水的用量为改性纳米二氧化硅流体总质量100g-其他组分的用量。In Comparative Examples 1-3 and Examples 1-8, the total mass of the modified nano-silica fluid is 100 g, and the amount of water used is 100 g of the total mass of the modified nano-silica fluid - the amount of other components.

对比例1~3和实施例1~8的制备方法相同,且所用的纳米二氧化硅硅溶胶亲水型纳米二氧化硅溶胶中二氧化硅含量均为40%,所述亲水型纳米二氧化硅溶胶的平均粒径均为10nm;密度均为1.109g/mL,pH均为9。不同的地方如表1所示。The preparation methods of Comparative Examples 1 to 3 are the same as those of Examples 1 to 8, and the content of silica in the used nano-silica silica sol hydrophilic nano-silica sol is 40%. The average particle size of the silica sol is 10 nm; the density is 1.109 g/mL, and the pH is 9. The differences are shown in Table 1.

表1对比例1~3和实施例1~8的制备原料、用量及改性温度Table 1 Preparation raw materials, dosage and modification temperature of Comparative Examples 1-3 and Examples 1-8

Figure BDA0003601216360000071
Figure BDA0003601216360000071

Figure BDA0003601216360000081
Figure BDA0003601216360000081

将0.1g对比例1~3和实施例1~8的改性纳米二氧化硅流体分别加入99.9g水中,搅拌均匀后,采用DLS仪评价其粒径分布,采用旋转滴法测试其油水界面张力,采用接触角评价装置评价其润湿转变能力和油滴剥离能力,采用渗吸瓶评价其渗吸采收率,评价结果如表2所示。Add 0.1 g of the modified nano-silica fluids of Comparative Examples 1 to 3 and Examples 1 to 8 into 99.9 g of water, respectively. After stirring evenly, the particle size distribution was evaluated by DLS instrument, and the oil-water interfacial tension was tested by rotating drop method. , the contact angle evaluation device was used to evaluate its wetting transition ability and oil droplet peeling ability, and the imbibition bottle was used to evaluate its imbibition recovery rate. The evaluation results are shown in Table 2.

表2对比例1~3和实施例1~8的实验结果Table 2 Experimental results of Comparative Examples 1-3 and Examples 1-8

Figure BDA0003601216360000091
Figure BDA0003601216360000091

由表2可知,改性后纳米流体界面张力、润湿转变性、油滴剥离性和渗吸采收率明显高于常规表面活性剂溶液和未改性纳米流体。It can be seen from Table 2 that the interfacial tension, wetting transition, oil droplet exfoliation and imbibition recovery of the modified nanofluid are significantly higher than those of the conventional surfactant solution and the unmodified nanofluid.

由表2可知,改性剂和低温稳定剂种类和加量相同的情况下,改性温度越高改性后纳米流体界面张力、润湿转变性、油滴剥离性和渗吸采收率越好。It can be seen from Table 2 that when the type and amount of modifier and low-temperature stabilizer are the same, the higher the modification temperature, the higher the interfacial tension, wetting transition, oil droplet exfoliation and imbibition recovery of the modified nanofluid. it is good.

由表2可知,在低温稳定剂种类和加量相同,改性剂加量相同,评价改性后纳米流体界面张力、润湿转变性、油滴剥离性和渗吸采收率等,三元复合改性效果优于二元复合改性优于单以改性剂改性。It can be seen from Table 2 that the type and amount of stabilizer at low temperature are the same, and the amount of modifier is the same. The effect of composite modification is better than that of binary composite modification than that of single modifier.

由表2可知,低温稳定剂种类和加量相同,改性剂总加量和种类相同情况下,不同改性剂加量相同时,改性后纳米流体界面张力、润湿转变性、油滴剥离性和渗吸采收率越好。It can be seen from Table 2 that when the type and amount of low-temperature stabilizer are the same, the total amount and type of modifier are the same, and when the amount of different modifiers is the same, the interfacial tension, wettability, and oil droplet of the modified nanofluid will be reduced. Strippability and imbibition recovery are better.

将对比例2~3和实施例1~8中所用亲水型纳米二氧化硅溶胶(改性前SiO2)进行SEM和DLS分析,结果如图1及图3所示;The hydrophilic nano-silica sols (SiO 2 before modification) used in Comparative Examples 2-3 and Examples 1-8 were analyzed by SEM and DLS, and the results are shown in Figures 1 and 3;

将对比例3制备得到的改性纳米二氧化硅流体(改性后SiO2)进行SEM和DLS分析,结果如图2及图3所示。由图1~3综合分析可知,改性后纳米流体粒径约10nm左右。The modified nano-silica fluid (modified SiO 2 ) prepared in Comparative Example 3 was analyzed by SEM and DLS, and the results are shown in FIG. 2 and FIG. 3 . It can be seen from the comprehensive analysis of Figures 1-3 that the particle size of the modified nanofluid is about 10 nm.

滑溜水压裂液Slippery water fracturing fluid

对比例4~15和实施例9~14的滑溜水压裂液的制备方法:Preparation methods of the slick water fracturing fluids of Comparative Examples 4 to 15 and Examples 9 to 14:

取一定量实施例所制备的改性纳米二氧化硅流体加入水中搅拌,加入多功能添加剂搅拌,加入一定量减阻剂搅拌,配置总量为100g的活性纳米流体强化滑溜水压裂液体系。A certain amount of the modified nano-silica fluid prepared in the example was added to water and stirred, multi-functional additives were added to stir, and a certain amount of drag reducing agent was added to stir, and a total amount of 100 g of active nano-fluid was used to strengthen the slick water fracturing fluid system.

对比例4~15和实施例9~14的滑溜水压裂液的制备方法不同,不同的地方详见表3。The preparation methods of the slick water fracturing fluids of Comparative Examples 4 to 15 and Examples 9 to 14 are different, and the differences are shown in Table 3.

表3对比例4~15和实施例9~14的滑溜水压裂液的原料及用量Table 3 Raw materials and dosages of slick water fracturing fluids of Comparative Examples 4 to 15 and Examples 9 to 14

Figure BDA0003601216360000101
Figure BDA0003601216360000101

Figure BDA0003601216360000111
Figure BDA0003601216360000111

10cm管内径、35L/min排量下评价对比例4~15和实施例9~14的滑溜水压裂液的减阻率。实验结果如表4所示。The drag reduction rates of the slick water fracturing fluids of Comparative Examples 4 to 15 and Examples 9 to 14 were evaluated under a pipe inner diameter of 10 cm and a displacement of 35 L/min. The experimental results are shown in Table 4.

将对比例4~15和实施例9~14的滑溜水压裂液在1000s-1剪切破胶30min后获得破胶液。采用渗吸瓶评价破胶液渗吸采收率。实验结果如表4所示。The slick water fracturing fluids of Comparative Examples 4 to 15 and Examples 9 to 14 were sheared at 1000 s −1 for 30 min to obtain gel breaking fluid. The imbibition recovery rate of broken gel was evaluated by imbibition bottle. The experimental results are shown in Table 4.

表4对比1~12和实施例1~6的滑溜水压裂液的实验结果Table 4 compares the experimental results of the slick water fracturing fluids of 1-12 and Examples 1-6

Figure BDA0003601216360000121
Figure BDA0003601216360000121

由表4可知,相较于只添加减阻剂的常规滑溜水,活性纳米流体强化滑溜水压裂液体系减阻率和渗吸采收率更佳,且纳米流体加量越高,减阻率和渗吸采收率越高。It can be seen from Table 4 that, compared with the conventional slick water only adding drag reducing agent, the drag reduction rate and imbibition recovery rate of the activated nanofluid enhanced slick water fracturing fluid system are better. rate and imbibition recovery.

由表4可知,相同改性纳米流体加量下,减阻剂加量过大不利于其减阻和渗吸。It can be seen from Table 4 that under the same amount of modified nanofluid, an excessive amount of drag reducer is not conducive to its drag reduction and imbibition.

由表4可知,相同纳米流体和减阻剂加量下,两性聚丙烯酰胺作为减阻剂减阻率和采收率优于聚丙烯酰胺、部分水解聚丙烯酰胺、阳离子型聚丙烯酰胺、胍胶、阳离子改性胍胶和羟丙基改性胍胶。It can be seen from Table 4 that under the same amount of nanofluid and drag reducing agent, the drag reduction rate and recovery rate of amphoteric polyacrylamide as drag reducing agent are better than that of polyacrylamide, partially hydrolyzed polyacrylamide, cationic polyacrylamide, guanidine gum, cationically modified guar gum and hydroxypropyl modified guar gum.

不同体系闷井排驱性能Drainage performance of stuffy wells in different systems

采用页岩油动态排驱评价装置,评价不同闷井时间下改性纳米流体、对比例17中的普通滑溜水破胶液和实施例15~18的滑溜水压裂液破胶液动态排驱性,破胶液的制备方法为:将普通滑溜水或滑溜水压裂液以3000转/min的转速搅拌5min即得普通滑溜水破胶液或滑溜水压裂液破胶液。结果见表5。The shale oil dynamic displacement evaluation device was used to evaluate the dynamic displacement of the modified nanofluid, the ordinary slick water gel breaker in Comparative Example 17 and the slick water fracturing fluid gel breakers in Examples 15 to 18 under different well boring times. The preparation method of the glue breaking fluid is as follows: stirring ordinary slick water or slick water fracturing fluid at a speed of 3000 rpm for 5 minutes to obtain ordinary slick water glue breaking fluid or slick water fracturing fluid glue breaking fluid. The results are shown in Table 5.

表5改性纳米流体、普通滑溜水和滑溜水压裂液动态排驱性的测试结果Table 5 Test results of dynamic displacement of modified nanofluids, ordinary slick water and slick water fracturing fluids

Figure BDA0003601216360000122
Figure BDA0003601216360000122

Figure BDA0003601216360000131
Figure BDA0003601216360000131

由表5可知,活性纳米流体的滑溜水压裂液排驱采油率明显高于改性纳米流体、滑溜水破胶液;且随着闷井时间越长排驱采油率越高。It can be seen from Table 5 that the oil recovery rate of slick water fracturing fluid with active nanofluids is significantly higher than that of modified nanofluids and slick water gel breaking fluid; and the oil recovery rate increases with the longer the well boring time.

尽管上述实施例对本发明做出了详尽的描述,但它仅仅是本发明一部分实施例,而不是全部实施例,还可以根据本实施例在不经创造性前提下获得其他实施例,这些实施例都属于本发明保护范围。Although the above embodiment has made a detailed description of the present invention, it is only a part of the embodiments of the present invention, not all of the embodiments, and other embodiments can also be obtained according to the present embodiment without creativity. It belongs to the protection scope of the present invention.

Claims (10)

1. The modified nano-silica fluid is characterized by comprising the following preparation raw materials:
20-40 wt% of hydrophilic nano silica sol;
20-40 wt% of a modifier;
10-30 wt% of a low-temperature stabilizer;
the balance of water;
the mass content of silicon dioxide in the hydrophilic nano silicon dioxide sol is 20-40%;
the modifier comprises one or more of alkyl glucoside, alkyl polyoxyethylene ether, alkyl sodium sulfate, alkyl sodium sulfonate, alpha-alkenyl sodium sulfonate, alkyl alcohol phosphate sodium, alkyl carboxyl betaine and alkyl hydroxypropyl sulfobetaine.
2. The modified nanosilica fluid of claim 1, wherein the hydrophilic nanosilica sol has an average particle size of from 8 to 15 nm.
3. The modified nanosilica fluid of claim 1, wherein the stabilizer comprises a first low temperature stabilizer and a second low temperature stabilizer; the mass of the first low-temperature stabilizer and the mass of the second low-temperature stabilizer respectively and independently account for 5-15% of the modified nano silicon dioxide fluid;
the first stabilizer comprises one or more of sodium chloride, ammonium chloride and urea;
the second stabilizer comprises one or more of isobutanol, propylene glycol, n-butanol, ethanol, and methanol.
4. A method for preparing the modified nanosilica fluid of any of claims 1 to 3, comprising the steps of: mixing hydrophilic nano-silica sol, a modifier, a low-temperature stabilizer and water for modification to obtain modified nano-silica fluid;
the modification temperature is 70-90 ℃.
5. Use of the modified nanosilica fluid according to any of claims 1 to 3 or the modified nanosilica fluid obtained by the method of claim 4 in shale oil development.
6. The slickwater fracturing fluid is characterized by comprising the following components:
0.05-0.5 wt% of modified nano silicon dioxide fluid;
0.05 to 0.5 wt% of a drag reducer;
0.1-0.5 wt% of multifunctional additive;
the balance of water;
the modified nano-silica fluid is the modified nano-silica fluid described in any one of claims 1 to 3 or the modified nano-silica fluid prepared by the preparation method described in claim 4.
7. The slickwater fracturing fluid of claim 6, wherein the drag reducer comprises one or more of polyacrylamide, partially hydrolyzed polyacrylamide, cationic polyacrylamide, amphoteric polyacrylamide, guar gum, cationic modified guar gum, and hydroxypropyl guar gum.
8. The slickwater fracturing fluid of claim 6 wherein the multifunctional additive comprises a mixture of one or more of potassium chloride, a copolymer of tetramethylpropylenediamine and dichloropropane, a copolymer of tetramethylethylenediamine and dichloroethane, and polydiallyldimethylammonium chloride with glutaraldehyde and/or chlorobenzene oxide.
9. Use of the slickwater fracturing fluid of any one of claims 5 to 8 in shale oil development.
10. The application according to claim 9, characterized in that it comprises the following steps:
pumping slickwater fracturing fluid into a stratum to form a crack, and pumping a mixture of slickwater fracturing fluid and a propping agent into the stratum to enable the propping agent to prop the crack; then continuously pumping slickwater fracturing fluid, and extruding the proppant in the shaft into the reservoir stratum; and (4) carrying out reverse drainage, and closing the well for 3-28 days.
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