技术领域technical field
本发明属于石油化工技术领域，具体涉及一种适合非常规储层压裂用无水压裂液及其制备方法。The invention belongs to the technical field of petrochemical industry, and in particular relates to an anhydrous fracturing fluid suitable for unconventional reservoir fracturing and a preparation method thereof.
背景技术Background technique
进入20世纪90年代，国外页岩气开发迅猛发展，技术逐步成熟。据统计全球页岩气资源量为456.24×1012m3，其中美国的页岩气资源量达到14×1012～20×1012m3，页岩气的勘探开发使美国天然气储量增加了40％。2010年页岩气产量超过了天然气总产量的15％，非常规页岩气已经成为美国的主力气源之一。In the 1990s, the development of foreign shale gas developed rapidly, and the technology gradually matured. According to statistics, the global shale gas resources are 456.24×1012 m3 , of which the shale gas resources in the United States reach 14×1012 to 20×1012 m3 , and the exploration and development of shale gas has increased the natural gas reserves in the United States by 40. %. In 2010, shale gas production exceeded 15% of the total natural gas production, and unconventional shale gas has become one of the main gas sources in the United States.
页岩气开采的核心技术是水力压裂，在美国超过一半的天然气都是通过压裂获得，开发使用的压裂液体系包括滑溜水压裂液和复合压裂液体系。由于非常规页岩气储集层物性较差，渗透率和孔隙度较低，常规压裂液容易造成水相圈闭伤害；另外，这种“万方液千方砂”式的大型压裂产生大量的返排液，处置不当会造成地表水的污染等问题，因此页岩气的开采在多个国家受到质疑。这也是目前页岩气储层水力压裂和开发面临的诸多亟待解决的问题之一。LPG压裂液的出现极大地缓解了压裂液对环境和水资源的压力。LPG压裂液是利用挥发性液化石油气取代水的一种新型压裂液体系，该压裂液的流变性、摩阻性、抗滤失性以及在支撑剂运移方面与传统的压裂液体系相似，很大程度上避免了传统压裂液的弊端，大大的提高了开采效率。The core technology of shale gas exploitation is hydraulic fracturing. More than half of the natural gas in the United States is obtained through fracturing. The fracturing fluid systems developed and used include slick water fracturing fluid and composite fracturing fluid systems. Due to poor physical properties, low permeability and porosity of unconventional shale gas reservoirs, conventional fracturing fluids are likely to cause damage to water phase traps; A large amount of flowback fluid is generated, and improper disposal will cause problems such as surface water pollution. Therefore, the exploitation of shale gas has been questioned in many countries. This is also one of the many urgent problems to be solved in the hydraulic fracturing and development of shale gas reservoirs. The emergence of LPG fracturing fluid has greatly relieved the pressure of fracturing fluid on the environment and water resources. LPG fracturing fluid is a new type of fracturing fluid system that uses volatile liquefied petroleum gas instead of water. The fluid system is similar, which largely avoids the disadvantages of traditional fracturing fluids and greatly improves the production efficiency.
我国陆域页岩气地质资源为134.42万亿立方米，开发经济价值巨大。页岩气资源开发在我国刚刚起步，经验不足，技术匮乏，这些因素制约着中国页岩气的发展。我国页岩层属于陆相沉积，这种岩层主要以粘土矿物伊蒙石为主，压裂时极易产生粘土膨胀，严重影响页岩气开发效果。my country's onshore shale gas geological resources are 134.42 trillion cubic meters, and the economic value of development is huge. The development of shale gas resources has just started in my country, with insufficient experience and technology. These factors restrict the development of shale gas in China. my country's shale formations belong to continental deposits. This kind of rock formations is mainly composed of clay mineral imonite. Clay swelling is very easy to occur during fracturing, which seriously affects the development effect of shale gas.
候向前等报道了非常规储集层低碳烃无水压裂液，主要介绍了一种无水压裂液交联剂。这种交联剂可以使煤油、正己烷和正辛烷形成LPG压裂液，该技术采用两步法成胶，速度慢，施工工艺复杂，压裂液耐高温性能差。在90℃时压裂液粘度为41.38mPa·s。Hou Xiangqian et al. reported anhydrous fracturing fluid for low-carbon hydrocarbons in unconventional reservoirs, and mainly introduced a crosslinking agent for anhydrous fracturing fluid. This cross-linking agent can make kerosene, n-hexane and n-octane to form LPG fracturing fluid. This technology adopts two-step method to form gel, which is slow, complicated construction process, and the fracturing fluid has poor high temperature resistance. At 90°C, the viscosity of the fracturing fluid is 41.38mPa·s.
申请号为201310359226.6公开了一种丁烷基压裂液及其制备方法，它以丁烷为基液，主要采用低碳醇合成的二烷基磷酸酯增稠剂，采用偏铝酸钠做交联剂。这种方法制备的压裂液在70℃时粘度只有50mPa·s左右，采用两步成胶法制备压裂液，制备工艺复杂，成胶速度慢，耐温能力差，满足不了页岩气井压裂施工对压裂液的要求。The application number is 201310359226.6, which discloses a butane-based fracturing fluid and its preparation method. It uses butane as the base fluid, mainly uses a dialkyl phosphate thickener synthesized from low-carbon alcohol, and uses sodium metaaluminate as the cross-linking agent. joint agent. The viscosity of the fracturing fluid prepared by this method is only about 50mPa·s at 70°C. The fracturing fluid is prepared by the two-step gelation method, which has complex preparation process, slow gelation speed, and poor temperature resistance, which cannot meet the pressure of shale gas wells. Fracturing fluid requirements for fracturing construction.
发明内容Contents of the invention
本发明所要解决的技术问题在于针对上述现有技术的不足，提供一种适合非常规储层压裂用无水压裂液。该无水压裂液采用一步法成胶且成胶速度可控，可满足130℃以下页岩层的压裂改造，该压裂液无需破胶剂，在地层温度和压力下，压裂液气化通过井管排出地面后可再回收利用，无废液外排和污染，具有环保等优点。压裂液在170s-1，130℃下压裂液粘度≥90mPa·s；在110℃，170s-1下连续剪切60min后压裂液粘度＞300mPa·s，同时压裂液具有剪切变稀的特性，压裂液对岩心伤害平均为4.94％。The technical problem to be solved by the present invention is to provide an anhydrous fracturing fluid suitable for unconventional reservoir fracturing in view of the above-mentioned deficiencies in the prior art. The anhydrous fracturing fluid adopts a one-step method of gelation and the gelation speed is controllable, which can meet the fracturing reconstruction of shale formations below 130 ° C. The fracturing fluid does not need a gel breaker. It can be recycled after being discharged to the ground through the well pipe, without waste liquid discharge and pollution, and has the advantages of environmental protection. The viscosity of the fracturing fluid is ≥90mPa·s at 170s-1 and 130°C; the viscosity of the fracturing fluid is >300mPa·s after continuous shearing at 110°C and 170s-1 for 60 minutes, and the fracturing fluid has shear deformation Due to the dilute characteristics, the average damage of fracturing fluid to core is 4.94%.
为解决上述技术问题，本发明采用的技术方案是：一种适合非常规储层压裂用无水压裂液，其特征在于，由以下质量百分比的原料制成：胶凝剂1.0％～2.0％，胶束促进剂2.0％～4.0％，温度稳定剂0.1％～0.5％，余量为烷基烃类；所述温度稳定剂为氨基磺酸或十二烷基苯磺酸，烷基烃类为丙烷、丁烷和戊烷中的一种或几种；所述胶凝剂为二烷基磷酸酯铁，二烷基磷酸酯铁中的混合醇包括低碳链烷基醇、中长碳链烷基醇和长碳链烷基醇，混合醇中低碳链烷基醇的质量百分含量为25％～40％，中长碳链烷基醇的质量百分含量为40％～70％，长碳链烷基醇的质量百分含量为5％～20％，所述低碳链烷基醇为C1-C4烷基醇中的一种或几种，中长碳链烷基醇为C6-C10烷基醇中的一种或几种，长碳链烷基醇为C12-C16烷基醇中的一种或几种；所述胶束促进剂为含三价金属离子的有机络合物，其中三价金属离子为三价铝离子或三价铁离子，含三价金属离子的有机络合物为三价金属离子的无机盐与油酸三乙醇胺反应的反应产物和乙二醇单丁醚的混合物，胶束促进剂中乙二醇单丁醚的质量百分含量为8％～15％。In order to solve the above technical problems, the technical solution adopted in the present invention is: a kind of anhydrous fracturing fluid suitable for unconventional reservoir fracturing, which is characterized in that it is made of the following raw materials in mass percentage: gelling agent 1.0% to 2.0% %, micellar accelerator 2.0% ~ 4.0%, temperature stabilizer 0.1% ~ 0.5%, the balance is alkyl hydrocarbons; the temperature stabilizer is sulfamic acid or dodecylbenzenesulfonic acid, alkyl hydrocarbon One or more of propane, butane, and pentane; the gelling agent is dialkyl iron phosphate, and the mixed alcohols in dialkyl iron phosphate include low-carbon chain alkyl alcohols, medium-length Carbon-chain alkanol and long-chain alkanol, the mass percentage of low-carbon alkanol in the mixed alcohol is 25% to 40%, and the mass percentage of medium and long-chain alkanol is 40% to 70% %, the mass percentage of long-chain alkanols is 5% to 20%, and the low-carbon alkanols are one or more of C1 -C4 alkanols. The base alcohol is one or more of the C6 -C10 alkyl alcohols, and the long-chain alkyl alcohol is one or more of the C12 -C16 alkyl alcohols; the micelle accelerator contains Organic complexes of trivalent metal ions, wherein trivalent metal ions are trivalent aluminum ions or ferric ions, organic complexes containing trivalent metal ions are inorganic salts of trivalent metal ions reacted with oleic acid triethanolamine The mixture of the reaction product and ethylene glycol monobutyl ether, the mass percentage of ethylene glycol monobutyl ether in the micelle accelerator is 8% to 15%.
上述的一种适合非常规储层压裂用无水压裂液，由以下质量百分比的原料制成：胶凝剂1.0％～1.5％，胶束促进剂2.5％～3.5％，温度稳定剂0.1％～0.3％，余量为烷基烃类。The above-mentioned anhydrous fracturing fluid suitable for unconventional reservoir fracturing is made of the following raw materials in mass percentage: 1.0% to 1.5% of gelling agent, 2.5% to 3.5% of micelle accelerator, and 0.1% of temperature stabilizer %～0.3%, the balance is alkyl hydrocarbons.
上述的一种适合非常规储层压裂用无水压裂液，所述混合醇中低碳链烷基醇的质量百分含量为30％～35％，中长碳链烷基醇的质量百分含量为50％～65％，长碳链烷基醇的质量百分含量为5％～15％。The above-mentioned anhydrous fracturing fluid suitable for unconventional reservoir fracturing, the mass percent content of low-carbon alkanol in the mixed alcohol is 30% to 35%, and the mass percentage of medium and long-chain alkanol is The percentage content is 50%-65%, and the mass percentage content of the long-carbon chain alkanol is 5%-15%.
上述的一种适合非常规储层压裂用无水压裂液，由以下质量百分比的原料制成：胶凝剂1.0％，胶束促进剂3.0％，温度稳定剂0.2％，余量为烷基烃类。The above-mentioned anhydrous fracturing fluid suitable for unconventional reservoir fracturing is made of the following raw materials in mass percentage: 1.0% gelling agent, 3.0% micelle accelerator, 0.2% temperature stabilizer, and the balance is alkane base hydrocarbons.
上述的一种适合非常规储层压裂用无水压裂液，所述混合醇中低碳链烷基醇的质量百分含量为30％，中长碳链烷基醇的质量百分含量为60％，长碳链烷基醇的质量百分含量为10％。The above-mentioned anhydrous fracturing fluid suitable for unconventional reservoir fracturing, the mass percentage of low-carbon alkanol in the mixed alcohol is 30%, and the mass percentage of medium-long chain alkanol is 60%, and the mass percentage of long-chain alkanol is 10%.
上述的一种适合非常规储层压裂用无水压裂液，所述二烷基磷酸酯铁的制备方法包括以下步骤：The above-mentioned anhydrous fracturing fluid suitable for unconventional reservoir fracturing, the preparation method of the dialkyl iron phosphate comprises the following steps:
步骤一、P2O5和磷酸三丁酯在反应温度为90℃～100℃的条件下搅拌反应0.5h～1h，然后向反应产物中加入混合醇，在反应温度为80℃～90℃的条件下搅拌反应6h～8h，得到二烷基磷酸酯；P2O5与磷酸三丁酯的摩尔比为1:(1～1.3)，混合醇与P2O5的摩尔比为(3～4):1；Step1 :P2O5 and tributyl phosphate are stirred and reacted at a reaction temperature of 90°C to 100°C for 0.5h to 1h, then mixed alcohol is added to the reaction product, and the reaction temperature is 80°C to 90°C Under the condition of stirring and reacting for 6h~8h, dialkyl phosphate is obtained; the molar ratio ofP2O5 to tributyl phosphate is 1:(1~1.3), and the molar ratio of mixed alcohol toP2O5 is (3 ~ 4): 1;
步骤二、向步骤一中所述二烷基磷酸酯中加入无水硫酸铁，在反应温度为100℃～120℃的条件下搅拌反应4h～6h，得到二烷基磷酸酯铁；所述二烷基磷酸酯与无水硫酸铁的摩尔比为(3～5):1。Step 2, adding anhydrous ferric sulfate to the dialkyl phosphate described in step 1, stirring and reacting for 4h to 6h at a reaction temperature of 100°C to 120°C to obtain iron dialkylphosphate; The molar ratio of alkyl phosphate to anhydrous iron sulfate is (3-5):1.
上述的一种适合非常规储层压裂用无水压裂液，所述三价金属离子的无机盐与油酸三乙醇胺反应的反应温度为50℃～60℃，反应时间为3h～5h，油酸三乙醇胺与三价金属离子的摩尔比为1:(1～2.5)。The above-mentioned anhydrous fracturing fluid suitable for unconventional reservoir fracturing, the reaction temperature of the reaction between the inorganic salt of the trivalent metal ion and oleic acid triethanolamine is 50°C-60°C, and the reaction time is 3h-5h, The molar ratio of triethanolamine oleate to trivalent metal ions is 1:(1-2.5).
上述的一种适合非常规储层压裂用无水压裂液，所述三价金属的无机盐为三价金属的硫酸盐或氯化物。In the aforementioned anhydrous fracturing fluid suitable for fracturing unconventional reservoirs, the inorganic salt of the trivalent metal is sulfate or chloride of the trivalent metal.
另外，本发明还提供了一种制备上述无水压裂液的方法，其特征在于，该方法为：在-30℃～-10℃的耐压密闭环境下，将胶凝剂加入烷基烃类中，搅拌均匀，然后加入温度稳定剂和胶束促进剂，搅拌1min～5min，得到无水压裂液。In addition, the present invention also provides a method for preparing the above-mentioned anhydrous fracturing fluid, which is characterized in that the method comprises: adding a gelling agent to an alkyl hydrocarbon Stir well, then add temperature stabilizer and micelle accelerator, stir for 1-5min to obtain anhydrous fracturing fluid.
本发明与现有技术相比具有以下优点：Compared with the prior art, the present invention has the following advantages:
1、本发明采用胶凝剂、胶束促进剂和温度稳定剂，基液以短碳链的烷基烃类为基液，采用低碳链烷基醇、中长碳链烷基醇和长碳链烷基醇合成不同碳链长度的二烷基磷酸酯铁胶凝剂，胶凝剂在常温下为液体，流动性好，一步成胶，简化了压裂液的制备工艺，同时加入胶束促进剂和温度稳定剂，加快了压裂液的成胶速度，使压裂液的抗温性等均得到显著提高。1, the present invention adopts gelling agent, micelle accelerator and temperature stabilizer, base liquid is base liquid with the alkyl hydrocarbons of short carbon chain, adopts low carbon chain alkyl alcohol, medium and long carbon chain alkyl alcohol and long carbon Synthesize dialkyl phosphate iron gelling agents with different carbon chain lengths from alkanols. The gelling agent is liquid at room temperature, has good fluidity, and can be gelled in one step, which simplifies the preparation process of fracturing fluid. At the same time, micelles are added Accelerators and temperature stabilizers accelerate the gelation speed of fracturing fluids and significantly improve the temperature resistance of fracturing fluids.
2、本发明的压裂液制备简单，无伤害，可满足130℃以下页岩层的压裂改造，该压裂液无需破胶剂，在地层温度和压力下，压裂液气化通过井管排出地面后可再回收利用，无废液外排和污染，具有环保等优点。2. The fracturing fluid of the present invention is easy to prepare, has no harm, and can satisfy the fracturing transformation of shale formations below 130°C. The fracturing fluid does not need a gel breaker. Under the formation temperature and pressure, the fracturing fluid gasifies and passes through the well pipe It can be recycled after being discharged to the ground, without waste liquid discharge and pollution, and has the advantages of environmental protection.
3、本发明的压裂液在170s-1，130℃下粘度≥90mPa·s；在110℃，170s-1下连续剪切60min后压裂液粘度＞300mPa·s，同时压裂液具有剪切变稀的特性，压裂液对岩心伤害平均为4.94％。3. The viscosity of the fracturing fluid of the present invention is ≥90mPa·s at 170s-1 and 130°C; the viscosity of the fracturing fluid is >300mPa·s after continuous shearing at 110°C and 170s-1 for 60min, and the fracturing fluid has shear Due to the characteristics of shear thinning, the average damage of fracturing fluid to core is 4.94%.
下面结合附图和实施例，对本发明的技术方案作进一步的详细描述。The technical solutions of the present invention will be further described in detail below in conjunction with the accompanying drawings and embodiments.
附图说明Description of drawings
图1为本发明实施例5的压裂液的抗剪切性能。Fig. 1 is the shear resistance performance of the fracturing fluid in Example 5 of the present invention.
图2为本发明实施例5的压裂液的耐温性能。Fig. 2 shows the temperature resistance performance of the fracturing fluid in Example 5 of the present invention.
具体实施方式detailed description
实施例1Example 1
本实施例的适合页岩气层压裂用无水压裂液，由以下质量百分比的原料制成：胶凝剂1.0％，胶束促进剂2.0％，温度稳定剂0.1％，余量为烷基烃类；所述温度稳定剂为氨基磺酸，烷基烃类为丙烷；所述胶凝剂为二烷基磷酸酯铁，二烷基磷酸酯铁中的混合醇包括甲醇、正己醇和十二醇，混合醇中甲醇的质量百分含量为25％，正己醇的质量百分含量为70％，十二醇的质量百分含量为5％；所述胶束促进剂为含三价铁离子的有机络合物，胶束促进剂的制备方法为：无水硫酸铁与油酸三乙醇胺在60℃下反应3h，然后将反应产物与乙二醇单丁醚混合均匀，得到胶束促进剂，油酸三乙醇胺与铁离子的摩尔比为1:1，胶束促进剂中乙二醇单丁醚的质量百分含量为8％；The anhydrous fracturing fluid suitable for shale gas layer fracturing in this embodiment is made of the following raw materials in mass percentage: 1.0% gelling agent, 2.0% micelle accelerator, 0.1% temperature stabilizer, and the balance is alkane base hydrocarbons; the temperature stabilizer is sulfamic acid, and the alkyl hydrocarbons are propane; the gelling agent is dialkyl iron phosphate, and the mixed alcohol in dialkyl iron phosphate includes methanol, n-hexanol and decathanol Diol, the mass percentage of methanol in the mixed alcohol is 25%, the mass percentage of n-hexanol is 70%, and the mass percentage of dodecanol is 5%; The preparation method of ionic organic complexes and micellar accelerators is as follows: react anhydrous ferric sulfate and oleic acid triethanolamine at 60°C for 3 hours, and then mix the reaction product with ethylene glycol monobutyl ether to obtain micellar accelerators. Agent, the mol ratio of oleic acid triethanolamine and iron ion is 1:1, and the mass percentage composition of ethylene glycol monobutyl ether in the micelle accelerator is 8%;
所述二烷基磷酸酯铁的制备方法包括以下步骤：The preparation method of described dialkyl iron phosphate comprises the following steps:
步骤一、P2O5和磷酸三丁酯在反应温度为100℃的条件下搅拌反应1h，然后向反应产物中加入混合醇，在反应温度为80℃的条件下搅拌反应8h，得到二烷基磷酸酯；P2O5与磷酸三丁酯的摩尔比为1:1，混合醇与P2O5的摩尔比为3:1；Step1 ,P2O5 and tributyl phosphate were stirred and reacted for 1 hour at a reaction temperature of 100°C, then mixed alcohol was added to the reaction product, and stirred for 8 hours at a reaction temperature of 80°C to obtain dioxane base phosphate; the molar ratio of P2 O5 to tributyl phosphate is 1:1, and the molar ratio of mixed alcohol to P2 O5 is 3:1;
步骤二、向步骤一中所述二烷基磷酸酯中加入无水硫酸铁，在反应温度为120℃的条件下搅拌反应6h，得到二烷基磷酸酯铁；所述二烷基磷酸酯与无水硫酸铁的摩尔比为3:1。Step 2, adding anhydrous ferric sulfate to the dialkyl phosphate described in step 1, stirring and reacting for 6 hours at a reaction temperature of 120° C. to obtain iron dialkyl phosphate; the dialkyl phosphate and The molar ratio of anhydrous ferric sulfate is 3:1.
本实施例的无水压裂液的制备方法为：按比例称取温度稳定剂、胶凝剂、胶束促进剂和烷基烃类，在-30℃的耐压密闭环境下，将胶凝剂加入烷基烃类中，搅拌均匀，然后加入温度稳定剂和胶束促进剂，搅拌1min，得到无水压裂液。The preparation method of the anhydrous fracturing fluid in this example is as follows: Weigh the temperature stabilizer, gelling agent, micelle accelerator and alkyl hydrocarbons in proportion, and in a pressure-resistant and airtight environment at -30 ° C, the gelling Add the agent into the alkyl hydrocarbons, stir evenly, then add the temperature stabilizer and the micelle accelerator, and stir for 1 min to obtain anhydrous fracturing fluid.
实施例2Example 2
本实施例与实施例1相同，其中不同之处在于：所用温度稳定剂为十二烷基苯磺酸，烷基烃类为丁烷或戊烷，或者为丙烷、丁烷和戊烷中的至少两种，低碳链烷基醇为C1-C4烷基醇中的至少两种，或者为乙醇、丙醇或丁醇，中长碳链烷基醇为C6-C10烷基醇中的至少两种，或者为C7-C10烷基醇中的一种，长碳链烷基醇为C12-C16烷基醇中的至少两种，或者为C13-C16烷基醇中的一种。The present embodiment is the same as Example 1, except that the temperature stabilizer used is dodecylbenzenesulfonic acid, and the alkyl hydrocarbons are butane or pentane, or are propane, butane and pentane At least two, low-carbon alkyl alcohols are at least two of C1 -C4 alkyl alcohols, or ethanol, propanol or butanol, medium-long chain alkyl alcohols are C6 -C10 alkyl At least two of alcohols, or one of C7 -C10 alkyl alcohols, and long-chain alkyl alcohols of at least two of C12 -C16 alkyl alcohols, or C13 -C16 One of the alkanols.
实施例3Example 3
本实施例的适合页岩气层压裂用无水压裂液，由以下质量百分比的原料制成：胶凝剂2.0％，胶束促进剂4.0％，温度稳定剂0.5％，余量为烷基烃类；所述温度稳定剂为十二烷基苯磺酸，烷基烃类为丙烷、丁烷和戊烷(摩尔比1:1:2)；所述胶凝剂为二烷基磷酸酯铁，二烷基磷酸酯铁中的混合醇包括丙醇、辛醇和十四醇，混合醇中丙醇的质量百分含量为40％，辛醇的质量百分含量为40％，十四醇的质量百分含量为20％；所述胶束促进剂为含三价铝离子的有机络合物，胶束促进剂的制备方法为：氯化铝与油酸三乙醇胺在50℃下反应5h，然后将反应产物与乙二醇单丁醚混合均匀，得到胶束促进剂，油酸三乙醇胺与铝离子的摩尔比为1:2.5，胶束促进剂中乙二醇单丁醚的质量百分含量为15％；The anhydrous fracturing fluid suitable for shale gas layer fracturing in this embodiment is made of the following raw materials in mass percentage: 2.0% gelling agent, 4.0% micelle accelerator, 0.5% temperature stabilizer, and the balance is alkane base hydrocarbons; the temperature stabilizer is dodecylbenzenesulfonic acid, and the alkyl hydrocarbons are propane, butane and pentane (molar ratio 1:1:2); the gelling agent is dialkyl phosphoric acid Ester iron, the mixed alcohol in dialkyl phosphate iron comprises propanol, octanol and myristyl alcohol, and the mass percentage composition of propanol is 40% in the mixed alcohol, and the mass percentage composition of octanol is 40%, tetradecyl alcohol The mass percentage of alcohol is 20%; the micelle accelerator is an organic complex containing trivalent aluminum ions, and the preparation method of the micelle accelerator is: react aluminum chloride and triethanolamine oleate at 50°C 5h, then the reaction product is mixed uniformly with ethylene glycol monobutyl ether to obtain a micelle accelerator, the mol ratio of oleic acid triethanolamine and aluminum ion is 1:2.5, the quality of ethylene glycol monobutyl ether in the micelle accelerator The percentage content is 15%;
所述二烷基磷酸酯铁的制备方法包括以下步骤：The preparation method of described dialkyl iron phosphate comprises the following steps:
步骤一、P2O5和磷酸三丁酯在反应温度为90℃的条件下搅拌反应1h，然后向反应产物中加入混合醇，在反应温度为90℃的条件下搅拌反应6h，得到二烷基磷酸酯；P2O5与磷酸三丁酯的摩尔比为1:1.3，混合醇与P2O5的摩尔比为4:1；Step1 ,P2O5 and tributyl phosphate were stirred and reacted for 1 hour at a reaction temperature of 90°C, then mixed alcohol was added to the reaction product, and the reaction was stirred for 6 hours at a reaction temperature of 90°C to obtain dioxane base phosphate; the molar ratio of P2 O5 to tributyl phosphate is 1:1.3, and the molar ratio of mixed alcohol to P2 O5 is 4:1;
步骤二、向步骤一中所述二烷基磷酸酯中加入无水硫酸铁，在反应温度为120℃的条件下搅拌反应6h，得到二烷基磷酸酯铁；所述二烷基磷酸酯与无水硫酸铁的摩尔比为5:1。Step 2, adding anhydrous ferric sulfate to the dialkyl phosphate described in step 1, stirring and reacting for 6 hours at a reaction temperature of 120° C. to obtain iron dialkyl phosphate; the dialkyl phosphate and The molar ratio of anhydrous ferric sulfate is 5:1.
本实施例的无水压裂液的制备方法为：按比例称取温度稳定剂、胶凝剂、胶束促进剂和烷基烃类，在-10℃的耐压密闭环境下，将胶凝剂加入烷基烃类中，搅拌均匀，然后加入温度稳定剂和胶束促进剂，搅拌3min，得到无水压裂液。The preparation method of the anhydrous fracturing fluid in this example is as follows: Weigh the temperature stabilizer, gelling agent, micelle accelerator and alkyl hydrocarbons in proportion, and in a pressure-resistant and airtight environment at -10°C, the gelling Add the agent into the alkyl hydrocarbons, stir evenly, then add the temperature stabilizer and micelle accelerator, and stir for 3 minutes to obtain anhydrous fracturing fluid.
实施例4Example 4
本实施例与实施例3相同，其中不同之处在于：所用温度稳定剂为氨基磺酸，烷基烃类为丙烷、丁烷和戊烷中的一种或两种，低碳链烷基醇为C1-C4烷基醇中的至少两种，或者为甲醇、乙醇或丁醇，中长碳链烷基醇为C6-C10烷基醇中的至少两种，或者为C6-C7烷基醇或C9-C10烷基醇中的一种，长碳链烷基醇为C12-C16烷基醇中的至少两种，或者为C12-C13烷基醇或C15-C16烷基醇中的一种。This embodiment is the same as Example 3, except that the temperature stabilizer used is sulfamic acid, the alkyl hydrocarbons are one or both of propane, butane and pentane, and the low-carbon alkanols It is at least two of C1 -C4 alkyl alcohols, or methanol, ethanol or butanol, and the medium and long chain alkanols are at least two of C6 -C10 alkyl alcohols, or it is C6 -C7 alkyl alcohol or one of C9 -C10 alkyl alcohol, long-chain alkyl alcohol is at least two of C12 -C16 alkyl alcohol, or C12 -C13 alkyl One of alcohols or C15 -C16 alkyl alcohols.
实施例5Example 5
本实施例的适合页岩气层压裂用无水压裂液，由以下质量百分比的原料制成：胶凝剂1.0％，胶束促进剂3.0％，温度稳定剂0.2％，余量为烷基烃类；所述温度稳定剂为十二烷基苯磺酸，烷基烃类为丁烷；所述胶凝剂为二烷基磷酸酯铁，二烷基磷酸酯铁中的混合醇包括丁醇、正癸醇和十六醇，混合醇中丁醇的质量百分含量为30％，正癸醇的质量百分含量为60％，十六醇的质量百分含量为10％；所述胶束促进剂为含三价铁离子的有机络合物，胶束促进剂的制备方法为：氯化铁与油酸三乙醇胺在60℃下反应3h，然后将反应产物与乙二醇单丁醚混合均匀，得到胶束促进剂，油酸三乙醇胺与铁离子的摩尔比为1:2，胶束促进剂中乙二醇单丁醚的质量百分含量为10％；The anhydrous fracturing fluid suitable for shale gas layer fracturing in this embodiment is made of the following raw materials in mass percentage: 1.0% gelling agent, 3.0% micelle accelerator, 0.2% temperature stabilizer, and the balance is alkane base hydrocarbons; the temperature stabilizer is dodecylbenzenesulfonic acid, and the alkyl hydrocarbons are butane; the gelling agent is dialkyl iron phosphate, and the mixed alcohol in dialkyl iron phosphate includes Butanol, n-decyl alcohol and cetyl alcohol, the mass percentage of butanol in the mixed alcohol is 30%, the mass percentage of n-decyl alcohol is 60%, and the mass percentage of cetyl alcohol is 10%; The micelle accelerator is an organic complex containing ferric ions. The preparation method of the micelle accelerator is: react ferric chloride and triethanolamine oleate at 60°C for 3 hours, and then mix the reaction product with ethylene glycol monobutyl The ether is mixed evenly to obtain a micelle accelerator, the mol ratio of triethanolamine oleate and iron ion is 1:2, and the mass percentage of ethylene glycol monobutyl ether in the micelle accelerator is 10%;
所述二烷基磷酸酯铁的制备方法包括以下步骤：The preparation method of described dialkyl iron phosphate comprises the following steps:
步骤一、P2O5和磷酸三丁酯在反应温度为95℃的条件下搅拌反应45min，然后向反应产物中加入混合醇，在反应温度为85℃的条件下搅拌反应7h，得到二烷基磷酸酯；P2O5与磷酸三丁酯的摩尔比为1:1.1，混合醇与P2O5的摩尔比为3.5:1；Step 1, P2 O5 and tributyl phosphate were stirred and reacted for 45 minutes at a reaction temperature of 95°C, then mixed alcohol was added to the reaction product, and the reaction was stirred for 7 hours at a reaction temperature of 85°C to obtain dioxane base phosphate; the molar ratio of P2 O5 to tributyl phosphate is 1:1.1, and the molar ratio of mixed alcohol to P2 O5 is 3.5:1;
步骤二、向步骤一中所述二烷基磷酸酯中加入无水硫酸铁，在反应温度为120℃的条件下搅拌反应6h，得到二烷基磷酸酯铁；所述二烷基磷酸酯与无水硫酸铁的摩尔比为4:1。Step 2, adding anhydrous ferric sulfate to the dialkyl phosphate described in step 1, stirring and reacting for 6 hours at a reaction temperature of 120° C. to obtain iron dialkyl phosphate; the dialkyl phosphate and The molar ratio of anhydrous ferric sulfate is 4:1.
本实施例的无水压裂液的制备方法为：按比例称取温度稳定剂、胶凝剂、胶束促进剂和烷基烃类，在-20℃的耐压密闭环境下，将胶凝剂加入烷基烃类中，搅拌均匀，然后加入温度稳定剂和胶束促进剂，搅拌5min，得到无水压裂液。The preparation method of the anhydrous fracturing fluid in this example is as follows: Weigh the temperature stabilizer, gelling agent, micelle accelerator and alkyl hydrocarbons in proportion, and in a pressure-resistant and airtight environment at -20 ° C, the gelling Add the agent into the alkyl hydrocarbons, stir evenly, then add the temperature stabilizer and micelle accelerator, stir for 5 minutes to obtain anhydrous fracturing fluid.
实施例6Example 6
本实施例与实施例5相同，其中不同之处在于：所用温度稳定剂为氨基磺酸，烷基烃类为丙烷或戊烷，或者为丙烷、丁烷和戊烷中的至少两种，低碳链烷基醇为C1-C4烷基醇中的至少两种，或者为C1-C3烷基醇中的一种，中长碳链烷基醇为C6-C10烷基醇中的至少两种，或者为C6-C9烷基醇中的一种，长碳链烷基醇为C12-C16烷基醇中的至少两种，或者为C12-C15烷基醇中的一种。This embodiment is the same as embodiment 5, wherein the difference is: the temperature stabilizer used is sulfamic acid, and the alkyl hydrocarbons are propane or pentane, or at least two of propane, butane and pentane, low The carbon chain alkyl alcohol is at least two kinds of C1 -C4 alkyl alcohols, or one of the C1 -C3 alkyl alcohols, and the medium and long carbon chain alkyl alcohols are C6 -C10 alkyl alcohols At least two of alcohols, or one of C6 -C9 alkyl alcohols, and long-chain alkyl alcohols of at least two of C12 -C16 alkyl alcohols, or C12 -C15 One of the alkanols.
实施例7Example 7
本实施例的适合页岩气层压裂用无水压裂液，由以下质量百分比的原料制成：胶凝剂1.5％，胶束促进剂2.5％，温度稳定剂0.3％，余量为烷基烃类；所述温度稳定剂为氨基磺酸，烷基烃类为丁烷和戊烷(摩尔比2:1)；所述胶凝剂为二烷基磷酸酯铁，二烷基磷酸酯铁中的混合醇包括低碳链烷基醇、中长碳链烷基醇和长碳链烷基醇，混合醇中低碳链烷基醇的质量百分含量为30％，中长碳链烷基醇的质量百分含量为65％，长碳链烷基醇的质量百分含量为5％，所述低碳链烷基醇为甲醇、乙醇、丙醇和丁醇按照1:4:2:1的摩尔比混合的混合物，中长碳链烷基醇为正己醇、正辛醇和正癸醇按照1:2:1的摩尔比混合的混合物，长碳链烷基醇为十二醇、十四醇和十六醇按照1:1:1的摩尔比混合的混合物；所述胶束促进剂为含三价铝离子的有机络合物，胶束促进剂的制备方法为：无水硫酸铝与油酸三乙醇胺在55℃下反应4h，然后将反应产物与乙二醇单丁醚混合均匀，得到胶束促进剂，油酸三乙醇胺与铝离子的摩尔比为1:1.5，胶束促进剂中乙二醇单丁醚的质量百分含量为12％；The anhydrous fracturing fluid suitable for shale gas reservoir fracturing in this embodiment is made of the following raw materials in mass percentage: 1.5% gelling agent, 2.5% micelle accelerator, 0.3% temperature stabilizer, and the balance is alkane base hydrocarbons; the temperature stabilizer is sulfamic acid, and the alkyl hydrocarbons are butane and pentane (molar ratio 2:1); the gelling agent is dialkyl phosphate iron, dialkyl phosphate Mixed alcohols in iron include low-carbon alkanols, medium-long-chain alkanols and long-chain alkanols, the mass percentage of low-carbon alkanols in mixed alcohols is 30%, and medium-long alkanes The mass percent composition of base alcohol is 65%, and the mass percent composition of long-carbon chain alkanol is 5%, and described low-carbon alkanol is methyl alcohol, ethanol, propanol and butanol according to 1:4:2: The mixture with a molar ratio of 1, the medium and long-chain alkanol is a mixture of n-hexanol, n-octanol and n-decyl alcohol in a molar ratio of 1:2:1, and the long-chain alkanol is dodecyl alcohol, decanol Tetrol and cetyl alcohol are mixed according to the molar ratio of 1:1:1; The micelle accelerator is an organic complex containing trivalent aluminum ions, and the preparation method of the micelle accelerator is: anhydrous aluminum sulfate and Triethanolamine oleate was reacted at 55°C for 4 hours, and then the reaction product was mixed evenly with ethylene glycol monobutyl ether to obtain a micelle accelerator. The molar ratio of triethanolamine oleate to aluminum ions was 1:1.5, and the micelle accelerator The mass percentage composition of ethylene glycol monobutyl ether in the medium is 12%;
所述二烷基磷酸酯铁的制备方法包括以下步骤：The preparation method of described dialkyl iron phosphate comprises the following steps:
步骤一、P2O5和磷酸三丁酯在反应温度为90℃的条件下搅拌反应1h，然后向反应产物中加入混合醇，在反应温度为80℃的条件下搅拌反应6h，得到二烷基磷酸酯；P2O5与磷酸三丁酯的摩尔比为1:1.2，混合醇与P2O5的摩尔比为4:1；Step1 ,P2O5 and tributyl phosphate are stirred and reacted for 1 hour at a reaction temperature of 90°C, then mixed alcohols are added to the reaction product, and the reaction is stirred for 6 hours at a reaction temperature of 80°C to obtain dioxane base phosphate; the molar ratio of P2 O5 to tributyl phosphate is 1:1.2, and the molar ratio of mixed alcohol to P2 O5 is 4:1;
步骤二、向步骤一中所述二烷基磷酸酯中加入无水硫酸铁，在反应温度为100℃的条件下搅拌反应4h，得到二烷基磷酸酯铁；所述二烷基磷酸酯与无水硫酸铁的摩尔比为3:1。Step 2, adding anhydrous ferric sulfate to the dialkyl phosphate described in step 1, stirring and reacting for 4 hours at a reaction temperature of 100° C. to obtain iron dialkyl phosphate; the dialkyl phosphate and The molar ratio of anhydrous ferric sulfate is 3:1.
本实施例的无水压裂液的制备方法为：按比例称取温度稳定剂、胶凝剂、胶束促进剂和烷基烃类，在-30℃的耐压密闭环境下，将胶凝剂加入烷基烃类中，搅拌均匀，然后加入温度稳定剂和胶束促进剂，搅拌2min，得到无水压裂液。The preparation method of the anhydrous fracturing fluid in this example is as follows: Weigh the temperature stabilizer, gelling agent, micelle accelerator and alkyl hydrocarbons in proportion, and in a pressure-resistant and airtight environment at -30 ° C, the gelling Add the agent into the alkyl hydrocarbons, stir evenly, then add the temperature stabilizer and micelle accelerator, and stir for 2 minutes to obtain anhydrous fracturing fluid.
实施例8Example 8
本实施例与实施例7相同，其中不同之处在于：所用温度稳定剂为硫酸，烷基烃类为丙烷、丁烷和戊烷中的一种或三种，或者为丙烷和丁烷，或者为丙烷和戊烷，低碳链烷基醇为C1-C4烷基醇中的至多三种，中长碳链烷基醇为C6-C10烷基醇中的一种、两种或四种以上，或者为C6-C9烷基醇中的三种，或者为C6-C7烷基醇和C9烷基醇中的两种与C10烷基醇的混合物，或者为C7烷基醇和C9烷基醇中的一种与C8烷基醇和C10烷基醇的混合物，长碳链烷基醇为C12-C16烷基醇中的一种、两种或四种以上，或者为C12-C15烷基醇中的三种，或者为C12-C13烷基醇和C15烷基醇中的两种与十六醇的混合物，或者为C13烷基醇和C15烷基醇中的一种与十四醇和十六醇的混合物。This embodiment is the same as Example 7, except that the temperature stabilizer used is sulfuric acid, and the alkyl hydrocarbons are one or three of propane, butane and pentane, or propane and butane, or Propane and pentane, low-carbon alkanols are at most three of C1 -C4 alkanols, and medium-long chain alkanols are one or two of C6 -C10 alkanols or four or more, or three of C6 -C9 alkyl alcohols, or a mixture of two of C6 -C7 alkyl alcohols and C9 alkyl alcohols with C10 alkyl alcohols, or A mixture of one of C7 alkyl alcohol and C9 alkyl alcohol and C8 alkyl alcohol and C10 alkyl alcohol, and the long-chain alkyl alcohol is one or two of C12 -C16 alkyl alcohol or four or more, or three of C12 -C15 alkyl alcohols, or a mixture of two of C12 -C13 alkyl alcohols and C15 alkyl alcohols with cetyl alcohol, or C13 A mixture of one of alkanol andC15 alkanol with myristyl alcohol and cetyl alcohol.
实施例9Example 9
本实施例的适合页岩气层压裂用无水压裂液，由以下质量百分比的原料制成：胶凝剂1.2％，胶束促进剂3.5％，温度稳定剂0.1％，余量为烷基烃类；所述温度稳定剂为十二烷基苯磺酸，烷基烃类为丙烷和丁烷(摩尔比1:1)；所述胶凝剂为二烷基磷酸酯铁，二烷基磷酸酯铁中的混合醇包括低碳链烷基醇、中长碳链烷基醇和长碳链烷基醇，混合醇中丙醇的质量百分含量为35％，辛醇的质量百分含量为50％，十四醇的质量百分含量为15％，所述低碳链烷基醇为甲醇和丁醇按照1:1的摩尔比混合的混合物，中长碳链烷基醇为正己醇、正辛醇和正癸醇按照1:2:1的摩尔比混合的混合物，长碳链烷基醇为十二醇、十四醇和十六醇按照2:3:1的摩尔比混合的混合物；所述胶束促进剂为含三价铁的有机络合物，胶束促进剂的制备方法为：硫酸铁与油酸三乙醇胺在50℃下反应5h，然后将反应产物与乙二醇单丁醚混合均匀，得到胶束促进剂，硫酸铁中的铁离子与油酸三乙醇胺的摩尔比为1:2，胶束促进剂中乙二醇单丁醚的质量百分含量为13％；The anhydrous fracturing fluid suitable for shale gas layer fracturing in this embodiment is made of the following raw materials in mass percentage: 1.2% gelling agent, 3.5% micelle accelerator, 0.1% temperature stabilizer, and the balance is alkane base hydrocarbons; the temperature stabilizer is dodecylbenzenesulfonic acid, and the alkyl hydrocarbons are propane and butane (molar ratio 1:1); the gelling agent is dialkyl phosphate iron, dialkyl The mixed alcohols in the iron-based phosphate ester include low-carbon alkanols, medium-long-chain alkanols and long-chain alkanols, and the mass percentage of propanol in the mixed alcohols is 35%, and the mass percentage of octanol The content is 50%, the mass percentage of myristyl alcohol is 15%, the low-carbon alkanol is a mixture of methanol and butanol in a molar ratio of 1:1, and the medium-long-chain alkanol is n-hexyl A mixture of alcohol, n-octanol and n-decyl alcohol in a molar ratio of 1:2:1, and a long-chain alkyl alcohol is a mixture of lauryl alcohol, tetradecyl alcohol and cetyl alcohol in a molar ratio of 2:3:1 The micelle accelerator is an organic complex containing ferric iron, and the preparation method of the micelle accelerator is: iron sulfate and oleic acid triethanolamine are reacted at 50°C for 5h, and then the reaction product is mixed with ethylene glycol mono The butyl ether is mixed evenly to obtain a micelle accelerator, the mol ratio of the iron ion in the ferric sulfate to triethanolamine oleate is 1:2, and the mass percentage of ethylene glycol monobutyl ether in the micelle accelerator is 13%;
所述二烷基磷酸酯铁的制备方法包括以下步骤：The preparation method of described dialkyl iron phosphate comprises the following steps:
步骤一、P2O5和磷酸三丁酯在反应温度为100℃的条件下搅拌反应0.5h，然后向反应产物中加入混合醇，在反应温度为80℃的条件下搅拌反应8h，得到二烷基磷酸酯；P2O5与磷酸三丁酯的摩尔比为1:1.2，混合醇与P2O5的摩尔比为4:1；Step 1, P2 O5 and tributyl phosphate were stirred and reacted for 0.5 h at a reaction temperature of 100° C., then mixed alcohol was added to the reaction product, and stirred and reacted for 8 h at a reaction temperature of 80° C. to obtain di Alkyl phosphate; the molar ratio of P2 O5 to tributyl phosphate is 1:1.2, and the molar ratio of mixed alcohol to P2 O5 is 4:1;
步骤二、向步骤一中所述二烷基磷酸酯中加入无水硫酸铁，在反应温度为110℃的条件下搅拌反应5h，得到二烷基磷酸酯铁；所述二烷基磷酸酯与无水硫酸铁的摩尔比为4.5:1。Step 2, adding anhydrous ferric sulfate to the dialkyl phosphate described in step 1, stirring and reacting for 5 hours at a reaction temperature of 110° C. to obtain iron dialkyl phosphate; the dialkyl phosphate and The molar ratio of anhydrous ferric sulfate is 4.5:1.
本实施例的无水压裂液的制备方法为：按比例称取温度稳定剂、胶凝剂、胶束促进剂和烷基烃类，在-10℃的耐压密闭环境下，将胶凝剂加入烷基烃类中，搅拌均匀，然后加入温度稳定剂和胶束促进剂，搅拌5min，得到无水压裂液。The preparation method of the anhydrous fracturing fluid in this example is as follows: Weigh the temperature stabilizer, gelling agent, micelle accelerator and alkyl hydrocarbons in proportion, and in a pressure-resistant and airtight environment at -10°C, the gelling Add the agent into the alkyl hydrocarbons, stir evenly, then add the temperature stabilizer and micelle accelerator, stir for 5 minutes to obtain anhydrous fracturing fluid.
实施例10Example 10
本实施例与实施例9相同，其中不同之处在于：所用温度稳定剂为氨基磺酸，烷基烃类为丙烷、丁烷和戊烷中的一种或三种，或者为戊烷和丁烷，或者为丙烷和戊烷，低碳链烷基醇为C1-C4烷基醇中的一种、三种或四种，或者为乙醇、丙醇和丁醇中的两种，或者为甲醇和乙醇，或者为甲醇和丙醇，中长碳链烷基醇为C6-C10烷基醇中的一种、两种或四种以上，或者为C6-C9烷基醇中的三种，或者为C6-C7烷基醇和C9烷基醇中的两种与C10烷基醇的混合物，或者为C7烷基醇和C9烷基醇中的一种与C8烷基醇和C10烷基醇的混合物，长碳链烷基醇为C12-C16烷基醇中的一种、两种或四种以上，或者为C12-C15烷基醇中的三种，或者为C12-C13烷基醇和C15烷基醇中的两种与十六醇的混合物，或者为C13烷基醇和C15烷基醇中的一种与十四醇和十六醇的混合物。This embodiment is the same as Example 9, except that the temperature stabilizer used is sulfamic acid, and the alkyl hydrocarbons are one or three of propane, butane and pentane, or pentane and butane Alkanes, or propane and pentane, low-carbon alkanols are one, three or four of C1 -C4 alkyl alcohols, or two of ethanol, propanol and butanol, or Methanol and ethanol, or methanol and propanol, medium and long-chain alkyl alcohols are one, two or more of C6 -C10 alkyl alcohols, or C6 -C9 alkyl alcohols three, or a mixture of two of C6 -C7 alkyl alcohols and C9 alkyl alcohols with C10 alkyl alcohols, or one of C7 alkyl alcohols and C9 alkyl alcohols with C A mixture of8 alkyl alcohols and C10 alkyl alcohols, long-chain alkyl alcohols are one, two or more of C12 -C16 alkyl alcohols, or C12 -C15 alkyl alcohols three kinds of C12 -C13 alkanols and C15 alkanols and cetyl alcohol mixtures, or C13 alkanols and C15 alkanols with myristyl alcohol and A mixture of cetyl alcohols.
对本发明实施例5的压裂液性能进行测试：The fracturing fluid performance of the embodiment of the present invention 5 is tested:
1、抗剪切性能：在90℃下考察压裂液的抗剪切性能，结果见图1。从图中可以看出，在同一温度下，压裂液的粘度随剪切速率的增大而下降。由此可见：本发明的压裂液同其它类型压裂液一样具有剪切变稀的特性。1. Shear resistance: The shear resistance of the fracturing fluid was investigated at 90°C, and the results are shown in Figure 1. It can be seen from the figure that at the same temperature, the viscosity of the fracturing fluid decreases with the increase of the shear rate. It can be seen that the fracturing fluid of the present invention has the same shear-thinning characteristic as other types of fracturing fluids.
2、耐温性能：将压裂液加热到95℃后，在170s-1下进行剪切测试，结果见图2。从图中可以看出，实验温度由95℃开始，在170s-1下连续剪切70min后压裂液温度升至130℃。压裂液粘度由起初95℃的600mPa·s下降到90mPa·s。由此可见：本发明的压裂液耐温能力可达到130℃，压裂液具有良好的耐温性能。2. Temperature resistance: After heating the fracturing fluid to 95°C, conduct a shear test at 170s-1 , the results are shown in Figure 2. It can be seen from the figure that the experimental temperature starts at 95°C, and the temperature of the fracturing fluid rises to 130°C after continuous shearing at 170s-1 for 70 minutes. The viscosity of the fracturing fluid dropped from 600mPa·s at the initial temperature of 95°C to 90mPa·s. It can be seen that the temperature resistance of the fracturing fluid of the present invention can reach 130° C., and the fracturing fluid has good temperature resistance.
本发明其他实施例制备的压裂液的性能与实施例5类似，均具有剪切变稀的特性，且耐温能力可达130℃。The performance of the fracturing fluid prepared in other embodiments of the present invention is similar to that of embodiment 5, both have the characteristic of shear thinning, and the temperature resistance can reach 130°C.
对本发明实施例1、3、5、7、9制备的压裂液的成胶时间、粘度和岩心伤害进行检测，岩心取自长庆苏里格气田储层的岩心，岩心渗透率为4.36×10-3μm2～5.62×10-3μm2，结果见表1。The gelation time, viscosity and core damage of the fracturing fluids prepared in Examples 1, 3, 5, 7, and 9 of the present invention were detected. The cores were taken from the reservoirs of the Sulige Gas Field in Changqing, and the permeability of the cores was 4.36× 10-3 μm2 to 5.62×10-3 μm2 , see Table 1 for the results.
表1压裂液的性能Table 1 Properties of fracturing fluids
从表1中可以看出，本发明的压裂液成胶时间2min～5min之内，130℃时压裂液粘度＞50mPa·s，对储层岩心渗透率在4.36×10-3μm2～5.62×10-3μm2之间的平均伤害率为4.94％，显著低于水基压裂液对岩心的伤害。It can be seen from Table 1 that the gelling time of the fracturing fluid of the present invention is within 2 minutes to 5 minutes, the viscosity of the fracturing fluid at 130°C is >50mPa·s, and the permeability to the reservoir core is between 4.36×10-3 μm2 and The average damage rate between 5.62×10-3 μm2 is 4.94%, which is significantly lower than the damage of water-based fracturing fluid to cores.
以上所述，仅是本发明的较佳实施例，并非对本发明做任何限制，凡是根据发明技术实质对以上实施例所作的任何简单修改、变更以及等效结构变化，均仍属于本发明技术方案的保护范围内。The above are only preferred embodiments of the present invention, and do not limit the present invention in any way. All simple modifications, changes and equivalent structural changes made to the above embodiments according to the technical essence of the invention still belong to the technical solution of the present invention. within the scope of protection.
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| CN201410272506.8ACN104004506B (en) | 2014-06-18 | 2014-06-18 | A kind of applicable unconventional reservoir pressure break anhydrous fracturing fluid and preparation method thereof |
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