Patent ID: 12215274

DETAILED DESCRIPTION OF THE EMBODIMENTS

The present disclosure will now be further described with reference to specific embodiments, without being limited thereto. The raw materials used in the embodiments are all conventional raw materials, and may be obtained commercially or prepared according to existing methods. The methods are existing technologies unless otherwise specified.

In the examples, phenolic resin is a water-soluble phenolic resin, commercially available from Jining Huakai Resin Co., Ltd.

Epoxy resin is a water-soluble epoxy resin, commercially available from Guangdong Zhongke Zhiyuan New Material Technology Co., Ltd.

An isocyanate-terminated polyurethane prepolymer is an MDI-terminated polyurethane prepolymer, commercially available from Jining Liduo Chemical Co., Ltd.

A tackifying polymer is a copolymer of 2-acrylamide-2-methylpropane sulfonic acid and acrylic acid, commercially available from Shanghai Macklin Biochemical Co., Ltd.

Bisphenol A-benzoxazine is commercially available from Jinan Shengquan Group Share-Holding Co., Ltd.

Preparative Example 1

A method for preparing the composite resin plugging agent includes the following steps:(1) 25 g of phenolic resin was added into a three-necked flask equipped with a stirrer and a thermometer, and the three-necked flask was heated to 100° C., vacuumized for 0.5 h and then cooled to 50° C., followed by pumping 0.5 g of isocyanate-terminated polyurethane prepolymer, warming to 100° C. and then reacting at a constant temperature under vacuum for 2 h to prepare a modified phenolic resin.(2) The obtained modified phenolic resin, 10 g of epoxy resin and 10 g of unsaturated polyester resin (3198-type) were uniformly mixed and added into 30 g of water, followed by sequentially adding 0.6 g of styrene, 0.3 g of trimethylolpropane and 0.4 g of tackifying polymer and stirring at a speed of 250 rpm until fully mixed and uniformly dispersed to obtain a mixed solution.(3) The mixed solution was put into a vacuum drying oven and dried at 60° C. for 24 h, and the dried solid was crushed to form a granular powder to obtain a composite resin plugging agent with a particle size of 1.0-2.5 mm.

Preparative Example 2

A method for preparing a bio-based latent consolidating agent (imidazole-oxazine consolidating agent (IMBA)) includes the following steps:(1) 20 g of imidazole (IM) and 16.5 g of phytic acid (PA) were dissolved in 50 mL of methanol to obtain solution A and solution B, respectively.(2) Solution B obtained was added dropwise to solution A to obtain solution C, and 20 g of bisphenol A-benzoxazine (BA-a) was added to solution C to obtain a mixed solution, which was stirred at 30° C. for 0.5 h and allowed to stand for layering.(3) Supernatant liquid of the mixed solution was poured out, and anhydrous ethanol was added to obtain solution D, which was stirred continuously at room temperature for 1 h.(4) The stirred solution D was allowed to stand at 0° C. for 1 h, step (3) was repeated three times, and the supernatant liquid was extracted each time.(5) The anhydrous ethanol was removed by using a rotary evaporator to finally obtain an imidazole-oxazine consolidating agent (IMBA).

Preparative Example 3

A method for preparing a flow pattern regulator (composite polymer high temperature resistant flow pattern regulator) includes the following steps:(1) 15 g of 2-acrylamide-2-methylpropane sulfonic acid (AMPS), 7.5 g of N,N-methylene bisacrylamide (MBA), 22.5 g of acrylic acid (AA) and 22.5 g of deionized water were added into a four-necked flask equipped with a thermometer, a stirring rod and a condenser tube, followed by successively adding 15 g of N-vinylpyrrolidone (NVP) and 7.5 g of divinylbenzene (DVB).(2) 2.5 g of sodium dodecyl sulfate was continuously added, sodium hydroxide was used for adjusting the pH to neutral, and the temperature was increased to 40° C., followed by full stirring for full dissolution.(3) 6.25 g of modified hydrophilic inorganic nano-material nano-silica (hydrophilic nano-silica, with a particle size of 20 nm, model PST-H20, available from Nanjing Baokete New Material Co., Ltd.) was added continuously.(4) Nitrogen was introduced, the temperature was increased to 70° C., 0.25 g of azobis(isobutyronitrile) was added and stirred continuously, followed by adding 0.375 g of sodium bisulfite and 0.75 g of ammonium persulfate, maintaining the temperature, and performing the stirring reaction for 4 h.(5) After the reaction was completed, the reaction product was naturally cooled to room temperature, precipitated with acetone, repeatedly washed, dried under vacuum at 50° C. for 15 h, and ground to obtain a composite polymer high temperature resistant flow pattern regulator with a particle size of 0.5-1.5 mm.

Preparative Comparative Example 1

A method for preparing a composite resin plugging agent is different from the method described in Preparative Example 1 in that the unsaturated polyester resin was not added. The other steps and conditions were the same as in Preparative Example 1.

Preparative Comparative Example 2

A method for preparing a composite resin plugging agent is different from the method described in Preparative Example 1 in that the modifier was not added. The specific steps are as follows:(1) 25 g of modified phenolic resin, 10 g of epoxy resin and 10 g of unsaturated polyester resin (3198-type) were uniformly mixed and added into 30 g of water, followed by sequentially adding 0.6 g of styrene, 0.3 g of trimethylolpropane and 0.4 g of tackifying polymer and stirring at a speed of 250 rpm until fully mixed and uniformly dispersed to obtain a mixed solution.(2) The mixed solution was put into a vacuum drying oven and dried at 60° C. for 24 h, and the dried solid was crushed to form a granular powder to obtain a composite resin plugging agent with a particle size of 1.0-2.5 mm.

Preparative Comparative Example 3

A method for preparing a composite resin plugging agent is different from the method described in Preparative Example 1 in that the tackifying polymer was not added. The other steps and conditions were the same as in Preparative Example 1.

Preparative Comparative Example 4

A method for preparing a composite resin plugging agent is different from the method described in Preparative Example 1 in that the trimethylolpropane was not added and the amount of styrene used was 0.9 g. The other steps and conditions were the same as in Preparative Example 1.

Preparative Comparative Example 5

A method for preparing a bio-based latent consolidating agent is different from the method described in Preparative Example 2 in that the imidazole was not added. The other steps and conditions were the same as in Preparative Example 1.

Preparative Comparative Example 6

A method for preparing a bio-based latent consolidating agent is different from the method described in Preparative Example 2 in that the phytic acid was not added. The other steps and conditions were the same as in Preparative Example 1.

Preparative Comparative Example 7

A method for preparing a flow pattern regulator is different from the method described in Preparative Example 3 in that the modified hydrophilic inorganic nano-material was not added. The other steps and conditions were the same as in Preparative Example 1.

Example 1

An ultra-high temperature resistant resin slurry plugging system suitable for a fractured-vuggy formation is composed of the following raw materials in mass percentage: 35.0% of composite resin plugging agent (prepared by the method in Preparative Example 1), 3.0% of imidazole-oxazine consolidating agent (prepared by the method in Preparative Example 2), 3.0% of composite polymer high temperature resistant flow pattern regulator (prepared by the method in Preparative Example 3), 0.6% of diethylene triamine, 0.3% of dimethyl triphenyl methane tetraisocyanate, 0.5% of sodium lignosulfonate, 0.5% of sugar calcium, 2.0% of ultra-fine calcium carbonate (with a particle size of 20-100 nm), 8.0% of quartz sand (with a particle size of 80-120 m), and the balance of water.

The method for preparing the ultra-high temperature resistant composite resin plugging system suitable for a fractured-vuggy formation includes the following steps:(a) The composite resin plugging agent was added into water, and stirred at a speed of 500 rpm until fully dispersed to obtain mixed solution E.(b) The sodium lignosulfonate and the calcium saccharate were added into mixed solution E, and stirred at a speed of 500 rpm until fully dispersed to obtain mixed solution F.(c) The diethylenetriamine, the dimethyl triphenyl methane tetraisocyanate, the imidazole-oxazine consolidating agent and the composite polymer high temperature resistant flow pattern regulator were added into mixed solution F, and stirred at a speed of 400 rpm until uniformly dispersed to obtain mixed solution G.(d) The ultra-fine calcium carbonate and the quartz sand were successively added into mixed solution G, and stirred at a speed of 600 rpm until uniformly dispersed, so as to obtain an ultra-high temperature resistant composite resin plugging system suitable for a fractured-vuggy formation, which was denoted as sample I1.

Example 2

An ultra-high temperature resistant resin slurry plugging system suitable for a fractured-vuggy formation is composed of the following raw materials in mass percentage: 20.0% of composite resin plugging agent (prepared by the method in Preparative Example 1), 1.0% of imidazole-oxazine consolidating agent (prepared by the method in Preparative Example 2), 3.0% of composite polymer high temperature resistant flow pattern regulator (prepared by the method in Preparative Example 3), 0.6% of diethylene triamine, 0.3% of dimethyl triphenyl methane tetraisocyanate, 0.5% of sodium lignosulfonate, 0.5% of sugar calcium, 2.0% of ultra-fine calcium carbonate (with a particle size of 20-100 nm), 8.0% of quartz sand (with a particle size of 80-120 m), and the balance of water.

With the method for preparing the ultra-high temperature resistant resin slurry plugging system suitable for a fractured-vuggy formation as described in Example 1, an ultra-high temperature resistant resin slurry plugging system suitable for a fractured-vuggy formation was obtained, which was denoted as sample I2.

Example 3

An ultra-high temperature resistant resin slurry plugging system suitable for a fractured-vuggy formation is composed of the following raw materials in mass percentage: 35.0% of composite resin plugging agent (prepared by the method in Preparative Example 1), 3.0% of imidazole-oxazine consolidating agent (prepared by the method in Preparative Example 2), 1.0% of composite polymer high temperature resistant flow pattern regulator (prepared by the method in Preparative Example 3), 0.6% of diethylene triamine, 0.3% of dimethyl triphenyl methane tetraisocyanate, 0.5% of sodium lignosulfonate, 0.5% of sugar calcium, 2.0% of ultra-fine calcium carbonate (with a particle size of 20-100 nm), 8.0% of quartz sand (with a particle size of 80-120 m), and the balance of water.

With the method for preparing the ultra-high temperature resistant resin slurry plugging system suitable for a fractured-vuggy formation as described in Example 1, an ultra-high temperature resistant resin slurry plugging system suitable for a fractured-vuggy formation is obtained, which was denoted as sample I3.

Example 4

An ultra-high temperature resistant resin slurry plugging system suitable for a fractured-vuggy formation is composed of the following raw materials in mass percentage: 35.0% of composite resin plugging agent (prepared by the method in Preparative Example 1), 3.0% of imidazole-oxazine consolidating agent (prepared by the method in Preparative Example 2), 3.0% of composite polymer anti-high temperature flow pattern regulator (prepared by the method in Preparative Example 3), 0.3% of diethylene triamine, 0.1% of dimethyl triphenyl methane tetraisocyanate, 0.5% of sodium lignosulfonate, 0.5% of sugar calcium, 2.0% of ultra-fine calcium carbonate (with a particle size of 20-100 nm), 8.0% of quartz sand (with a particle size of 80-120 m), and the balance of water.

With the method for preparing the ultra-high temperature resistant resin slurry plugging system suitable for a fractured-vuggy formation as described in Example 1, an ultra-high temperature resistant resin slurry plugging system suitable for a fractured-vuggy formation is obtained, which was denoted as sample I4.

Example 5

An ultra-high temperature resistant resin slurry plugging system suitable for a fractured-vuggy formation is composed of the following raw materials in mass percentage: 35.0% of composite resin plugging agent (prepared by the method in Preparative Example 1), 3.0% of imidazole-oxazine consolidating agent (prepared by the method in Preparative Example 2), 3.0% of composite polymer high temperature resistant flow pattern regulator (prepared by the method in Preparative Example 3), 0.6% of diethylene triamine, 0.3% of dimethyl triphenyl methane tetraisocyanate, 0.25% of sodium lignosulfonate, 0.25% of sugar calcium, 2.0% of ultra-fine calcium carbonate (with a particle size of 20-100 nm), 8.0% of quartz sand (with a particle size of 80-120 m), and the balance of water.

With the method for preparing the ultra-high temperature resistant resin slurry plugging system suitable for a fractured-vuggy formation as described in Example 1, an ultra-high temperature resistant resin slurry plugging system suitable for a fractured-vuggy formation was obtained, which was denoted as sample Is.

Example 6

An ultra-high temperature resistant resin slurry plugging system suitable for a fractured-vuggy formation is composed of the following raw materials in mass percentage: 35.0% of composite resin plugging agent (prepared by the method in Preparative Example 1), 3.0% of imidazole-oxazine consolidating agent (prepared by the method in Preparative Example 2), 3.0% of composite polymer high temperature resistant flow pattern regulator (prepared by the method in Preparative Example 3), 0.6% of diethylene triamine, 0.3% of dimethyl triphenyl methane tetraisocyanate, 0.5% of sodium lignosulfonate, 0.5% of sugar calcium, 1.0% of ultra-fine calcium carbonate (with a particle size of 20-100 nm), 4.0% of quartz sand (with a particle size of 80-120 m), and the balance of water.

With the method for preparing the ultra-high temperature resistant resin slurry plugging system suitable for a fractured-vuggy formation as described in Example 1, an ultra-high temperature resistant resin slurry plugging system suitable for a fractured-vuggy formation was obtained, which was denoted as sample I6.

Example 7

An ultra-high temperature resistant resin slurry plugging system suitable for a fractured-vuggy formation is different from the plugging system described in Example 1 in that the imidazole-oxazine consolidating agent was replaced with hexamethylene tetramine. The other raw material compositions were the same as in those in Example 1.

With the method for preparing the ultra-high temperature resistant resin slurry plugging system suitable for a fractured-vuggy formation as described in Example 1, an ultra-high temperature resistant resin slurry plugging system suitable for a fractured-vuggy formation was obtained, which was denoted as sample I7.

Example 8

An ultra-high temperature resistant resin slurry plugging system suitable for a fractured-vuggy formation is different from the plugging system described in Example 1 in that the imidazole-oxazine consolidating agent was replaced with methyl tetrahydrophthalic anhydride. The other raw material compositions were the same as in those in Example 1.

With the method for preparing the ultra-high temperature resistant resin slurry plugging system suitable for a fractured-vuggy formation as described in Example 1, an ultra-high temperature resistant resin slurry plugging system suitable for a fractured-vuggy formation was obtained, which was denoted as sample Is.

Example 9

An ultra-high temperature resistant resin slurry plugging system suitable for a fractured-vuggy formation is different from the plugging system described in Example 1 in that the composite polymer high temperature resistant flow pattern regulator was replaced with hydroxypropyl guar gum. The other raw material compositions were the same as in those in Example 1.

With the method for preparing the ultra-high temperature resistant resin slurry plugging system suitable for a fractured-vuggy formation as described in Example 1, an ultra-high temperature resistant resin slurry plugging system suitable for a fractured-vuggy formation was obtained, which was denoted as sample I9.

Example 10

An ultra-high temperature resistant resin slurry plugging system suitable for a fractured-vuggy formation is different from the plugging system described in Example 1 in that the diethylene triamine was replaced with hydroxypropyl acrylate. The other raw material compositions are the same as in those in Example 1.

With the method for preparing the ultra-high temperature resistant resin slurry plugging system suitable for a fractured-vuggy formation as described in Example 1, an ultra-high temperature resistant resin slurry plugging system suitable for a fractured-vuggy formation was obtained, which was denoted as sample I10.

Example 11

An ultra-high temperature resistant resin slurry plugging system suitable for a fractured-vuggy formation is different from the plugging system described in Example 1 in that the dimethyl triphenyl methane tetraisocyanate was replaced with p-toluenesulfonic acid. The other raw material compositions are the same as in those in Example 1.

With the method for preparing the ultra-high temperature resistant resin slurry plugging system suitable for a fractured-vuggy formation as described in Example 1, an ultra-high temperature resistant resin slurry plugging system suitable for a fractured-vuggy formation was obtained, which was denoted as sample I11.

Example 12

An ultra-high temperature resistant resin slurry plugging system suitable for a fractured-vuggy formation is different from the plugging system described in Example 1 in that the sodium lignosulfonate was replaced with sodium gluconate. The other raw material compositions are the same as in those in Example 1.

With the method for preparing the ultra-high temperature resistant resin slurry plugging system suitable for a fractured-vuggy formation as described in Example 1, an ultra-high temperature resistant resin slurry plugging system suitable for a fractured-vuggy formation was obtained, which was denoted as sample I12.

Example 13

An ultra-high temperature resistant resin slurry plugging system suitable for a fractured-vuggy formation is different from the plugging system described in Example 1 in that the sugar calcium was replaced with phosphogypsum. The other raw material compositions were the same as in those in Example 1.

With the method for preparing the ultra-high temperature resistant resin slurry plugging system suitable for a fractured-vuggy formation as described in Example 1, an ultra-high temperature resistant resin slurry plugging system suitable for a fractured-vuggy formation was obtained, which was denoted as sample I13.

Comparative Example 1

A resin slurry plugging system is different from the plugging system described in Example 1 in that the composite polymer high temperature resistant flow pattern regulator was not added. The omitted components were replaced with water in equal amounts. The other raw material compositions were the same as in those in Example 1.

With the method for preparing the resin slurry plugging system as described in Example 1, a resin slurry plugging system was obtained, which was denoted as sample II1.

Comparative Example 2

A resin slurry plugging system is different from the plugging system described in Example 1 in that the diethylenetriamine was not added. The omitted components were replaced with water in equal amounts. The other raw material compositions were the same as in those in Example 1.

With the method for preparing the resin slurry plugging system as described in Example 1, a resin slurry plugging system was obtained, which was denoted as sample II2.

Comparative Example 3

A resin slurry plugging system is different from the plugging system described in Example 1 in that the dimethyl triphenyl methane tetraisocyanate was not added. The omitted components were replaced with water in equal amounts. The other raw material compositions were the same as in those in Example 1.

With the method for preparing the resin slurry plugging system as described in Example 1, a resin slurry plugging system was obtained, which was denoted as sample II3.

Comparative Example 4

A resin slurry plugging system is different from the plugging system described in Example 1 in that neither diethylenetriamine nor dimethyl triphenyl methane tetraisocyanate was added. The omitted components were replaced with water in equal amounts. The other raw material compositions were the same as in those in Example 1.

With the method for preparing the resin slurry plugging system as described in Example 1, a resin slurry plugging system was obtained, which was denoted as sample II4.

Comparative Example 5

A resin slurry plugging system is different from the plugging system described in Example 1 in that neither sodium lignosulfonate nor calcium saccharate was added. The omitted components were replaced with water in equal amounts. The other raw material compositions were the same as in those in Example 1.

With the method for preparing the resin slurry plugging system as described in Example 1, a resin slurry plugging system was obtained, which was denoted as sample II5.

Comparative Example 6

A resin slurry plugging system is different from the plugging system described in Example 1 in that the ultra-fine calcium carbonate was not added. The omitted components were replaced with water in equal amounts. The other raw material compositions were the same as in those in Example 1.

With the method for preparing the resin slurry plugging system as described in Example 1, a resin slurry plugging system was obtained, which was denoted as sample II6.

Comparative Example 7

A resin slurry plugging system is different from the plugging system described in Example 1 in that the quartz sand was not added. The omitted components were replaced with water in equal amounts. The other raw material compositions were the same as in those in Example 1.

With the method for preparing the resin slurry plugging system as described in Example 1, a resin slurry plugging system was obtained, which was denoted as sample II7.

Comparative Example 8

A resin slurry plugging system is different from the plugging system described in Example 1 in that neither ultra-fine calcium carbonate nor quartz sand was added. The omitted components were replaced with water in equal amounts. The other raw material compositions were the same as in those in Example 1.

With the method for preparing the resin slurry plugging system as described in Example 1, a resin slurry plugging system was obtained, which was denoted as sample II8.

Comparative Example 9

A resin slurry plugging system is different from the plugging system described in Example 1 in that the composite resin plugging agent prepared by the method in Preparative Example 1 was replaced with the composite resin plugging agent prepared by the method in Preparative Comparative Example 1. The other raw material compositions were the same as in those in Example 1.

With the method for preparing the resin slurry plugging system as described in Example 1, a resin slurry plugging system was obtained, which was denoted as sample II9.

Comparative Example 10

A resin slurry plugging system is different from the plugging system described in Example 1 in that the composite resin plugging agent prepared by the method in Preparative Example 1 was replaced with the composite resin plugging agent prepared by the method in Preparative Comparative Example 2. The other raw material compositions were the same as in those in Example 1.

With the method for preparing the resin slurry plugging system as described in Example 1, a resin slurry plugging system was obtained, which was denoted as sample II10.

Comparative Example 11

A resin slurry plugging system is different from the plugging system described in Example 1 in that the composite resin plugging agent prepared by the method in Preparative Example 1 was replaced with the composite resin plugging agent prepared by the method in Preparative Comparative Example 3. The other raw material compositions were the same as in those in Example 1.

With the method for preparing the resin slurry plugging system as described in Example 1, a resin slurry plugging system was obtained, which was denoted as sample liii.

Comparative Example 12

A resin slurry plugging system is different from the plugging system described in Example 1 in that the composite resin plugging agent prepared by the method in Preparative Example 1 was replaced with the composite resin plugging agent prepared by the method in Preparative Comparative Example 4. The other raw material compositions were the same as in those in Example 1.

With the method for preparing the resin slurry plugging system as described in Example 1, a resin slurry plugging system was obtained, which was denoted as sample II12.

Comparative Example 13

A resin slurry plugging system is different from the plugging system described in Example 1 in that the imidazole-oxazine consolidating agent prepared by the method in Preparative Example 2 was replaced with the consolidating agent prepared by the method in Preparative Comparative Example 5. The other raw material compositions were the same as in those in Example 1.

With the method for preparing the resin slurry plugging system as described in Example 1, a resin slurry plugging system was obtained, which was denoted as sample II13.

Comparative Example 14

A resin slurry plugging system is different from the plugging system described in Example 1 in that the imidazole-oxazine consolidating agent prepared by the method in Preparative Example 2 was replaced with the consolidating agent prepared by the method in Preparative Comparative Example 6. The other raw material compositions were the same as in those in Example 1.

With the method for preparing the resin slurry plugging system as described in Example 1, a resin slurry plugging system was obtained, which was denoted as sample II14.

Comparative Example 15

A resin slurry plugging system is different from the plugging system described in Example 1 in that the composite polymer high temperature resistant flow pattern regulator prepared by the method in Preparative Example 3 was replaced with the flow pattern regulator prepared by the method in Preparative Comparative Example 7. The other raw material compositions were the same as in those in Example 1.

With the method for preparing the resin slurry plugging system as described in Example 1, a resin slurry plugging system was obtained, which was denoted as sample II15.

Experimental Example

The rheology, temperature resistance, initial consolidating time, compressive strength, and plugging effect of the resin slurry plugging system were tested.1. Rheology Test: The rheology of the resin slurry plugging system was tested using a six-speed rotary viscometer (model ZNN-D6).2. Temperature Resistance Test: The resin slurry plugging system was loaded into a temperature-resistant film, placed in a high-temperature aging oven, heated at a temperature of 180° C., 200° C., 220° C., 240° C., 260° C., or 280° C. for 48 h, and taken out for uniaxial compressive strength test to evaluate its temperature resistance.3. Initial Consolidating Time Test: The resin slurry plugging system was loaded into the temperature-resistant film, placed in the high-temperature aging oven, heated at a temperature of 180° C., 200° C., 220° C., 240° C., 260° C., or 280° C., and taken out at regular intervals to observe the consolidating, and the initial consolidating time of a sample at different temperatures was tested with 30 seconds of mold upside down without fluid outflow as the consolidating standard.4. Optimal Consolidating Time and Strength Test: The resin slurry plugging system was loaded into the temperature-resistant film, placed in the high-temperature aging oven, heated at a temperature of 260° C., and taken out regularly for uniaxial compression test to find its optimal consolidating time and compressive strength corresponding to the optimal consolidating time. The compressive strength of the consolidated resin slurry plugging system was calculated by formula.5. Test on Plugging Effect of Resin Slurry Plugging System: The plugging effect of the resin slurry plugging system on fractures was tested by a high-temperature and high-pressure plugging test device. The resin slurry plugging system was loaded into a steel fracture model with a length of 10 cm and a fracture width of 3.0 mm. The model was sealed and placed into the high-temperature aging oven for consolidating. After being consolidated, the resin slurry plugging system in the steel fracture model was taken out from a hot rolling furnace, cooled, and then pressurized by well slurry injected through a large displacement constant-flux pump, the pressure at an inlet end of the fracture model was recorded in real time, and the highest pressure when the well slurry was lost from an outlet end of the fracture model was taken as the pressure-bearing plugging capacity of the resin slurry plugging system on fractures. The test temperature was 180° C., 200° C., 220° C., 240° C., 260° C., or 280° C., and the consolidating time is the optimal consolidating time of the corresponding temperature of the sample.

The performance of the resin slurry plugging system was tested using the above method, and the test results are shown in Tables 1, 2, 3, and 4.

TABLE 1Rheology test data of resin slurry plugging systemAbsolute viscosity at differentInitialApparentPlasticDynamicSamplerevolving speeds (mPa · s)shear/finalviscosityviscosityshearNo.Φ600Φ300Φ200Φ100Φ6Φ3shear (Pa)(mPa · s)(mPa · s)(Pa)I11851271068734219.5/11.592.55834.5I2163112986925167/9.581.55130.5II11047156341394/5523319

The ultra-high temperature resistant resin slurry plugging system suitable for a fractured-vuggy formation prepared in Examples 1 and 2 of the present disclosure exhibits better rheology (as shown inFIG.1aandFIG.1b). In Comparative Example 1, the performance of a suspension filling agent in a solution system was deteriorated (as shown inFIG.1c) without a flow pattern regulator, so that the rheology of the resin slurry plugging system was sharply decreased, which further illustrates that the ultra-high temperature resistant resin slurry plugging system suitable for a fractured-vuggy formation can maintain a certain viscosity and can effectively suspend and disperse filling agents such as ultra-fine calcium carbonate and quartz sand due to the addition of the flow pattern regulator.

TABLE 2Temperature resistance test data of resin slurry plugging system(heating at different temperatures for 48 h)Compressive strength (MPa) of various resinSampleslurry plugging systems at different temperaturesNo.180° C.200° C.220° C.240° C.260° C.280° C.I132.3530.1228.3327.5226.9720.23I228.2527.3725.1324.1523.6117.29I331.2329.8527.1826.7425.3219.17I430.1628.2226.4725.3724.1418.26I532.1429.8428.1927.3626.4819.65I630.3528.7627.1326.9426.0519.87II122.1221.5520.3718.3517.6310.35II218.3417.2416.5515.3514.558.97II320.1619.4818.5416.9615.849.72II416.2815.7714.8813.5712.336.83II530.2929.5628.4927.1926.2719.84II628.3727.4326.6925.1324.4518.47II724.1922.9422.0821.2420.1812.42II823.2822.4521.1620.3418.2410.31

The ultra-high temperature resistant resin slurry plugging system suitable for a fractured-vuggy formation prepared in Examples 1-6 of the present disclosure can form high-strength consolidated bodies at 180-280° C., and exhibit good compressive properties, as shown inFIG.2andFIG.3. The compressive strength of the resin slurry plugging system after consolidating is the highest at 180° C. The compressive strength is reduced with the increase of temperature. The compressive strength of the resin slurry plugging system after consolidating is reduced a little in the range of 180-260° C. When the temperature is higher than 260° C., the reduction of the compressive strength is increased. The compressive strength of the sample in Example 1 at 280° C. is 20.23 MPa, still higher than 20 MPa. Therefore, the ultra-high temperature resistant resin slurry plugging system suitable for a fractured-vuggy formation according to the present disclosure can meet the requirements of plugging at an ultra-high temperature of 280° C. In Comparative Example 1, the composite polymer high temperature resistant flow pattern regulator is not added, the compressive strength of the resin slurry plugging system after consolidating at various temperatures is reduced, and the overall temperature resistance is reduced. In Comparative Example 2, the diethylenetriamine is not added. In Comparative Example 3, the dimethyl triphenyl methane tetraisocyanate is not added. In Comparative Example 4, neither the diethylenetriamine nor the dimethyl triphenyl methane tetraisocyanate is added, which greatly reduces the compressive strength of the resin slurry plugging system after consolidating under ultra-high temperature conditions. In comparison, the influence of the cross-linking agent diethylenetriamine is greater. In Comparative Example 5, neither retarder sodium lignosulfonate nor calcium saccharate is added. It can be seen from the compressive strength data at various temperatures that the sodium lignosulfonate and the calcium saccharate have little effect on the temperature resistance and compressive strength of the resin slurry plugging system. In Comparative Example 6, the ultra-fine calcium carbonate is not added. In Comparative Example 7, the quartz sand is not added. In Comparative Example 8, neither ultra-fine calcium carbonate nor the quartz sand is added. By comparing the data with the data of the compressive strength in Example 1 at different temperatures, it can be concluded that the quartz sand is resistant to high temperature and can still provide a certain compressive strength for the resin slurry plugging system under the ultra-high temperature conditions.

TABLE 3Consolidating condition and plugging effect of resin slurry plugging systemConsolidatingInitialOptimalCompressiveSampletemperatureconsolidatingconsolidatingstrengthNo.(° C.)time (h)time (h)(MPa)I12604.56.026.95I22605.58.023.63I32604.06.025.35I42605.07.024.17I52603.54.026.49I62604.56.026.08II12602.03.517.65II22607.012.014.58II32606.510.015.82II42609.018.012.31II52601.53.026.22II62604.56.024.41II72603.55.020.15II82603.54.518.23

TABLE 4Test data of pressure-bearingplugging capacity at different temperaturesTest data (MPa) of pressure-bearing pluggingSamplecapacity at different temperaturesNo.180° C.200° C.220° C.240° C.260° C.280° C.I123.321.720.619.318.215.1I220.519.318.116.815.613.9I319.618.517.716.114.912.4I421.119.718.617.216.314.1I522.921.220.319.018.114.9I619.218.217.515.914.712.1I712.511.310.197.96.3I812.211.110.29.17.85.9I910.68.97.56.15.24I1011.210.19.286.95.6I1110.59.187.15.94.8I1211.110.28.97.46.55.2I1310.89.68.57.26.45.3II17.46.96.76.56.23.2II29.39.08.98.78.54.0II38.58.18.07.87.43.6II47.67.26.96.66.33.3II522.321.020.118.817.814.6II65.75.55.45.35.12.4II74.54.24.13.93.71.9II83.63.43.12.82.61.3II919.318.116.915.314.213II1012.31110.18.97.25.5II1110.59.18.275.94.2II1212.111.210.197.96.1II1312.211.110.29.17.85.9II1411.910.89.98.87.65.5II15121110.29.38.16.2

The initial consolidating time at 260° C. of the ultra-high temperature resistant resin slurry plugging system suitable for a fractured-vuggy formation prepared in Examples 1-6 of the present disclosure is 3.5-5.5 h, which can meet the construction safety of the plugging site and achieve the optimal consolidating effect in 4-8 h, so as to ensure that the plugging system is quickly consolidated after being pumped into a lost circulation location and the compressive strength after consolidating is greater than 20 MPa. The plugging effect test data shows that the resin slurry plugging system can play a better plugging function after being consolidated at 260° C. with the optimal consolidating time. As shown inFIG.4andFIG.5, the pressure-bearing plugging effect of the ultra-high temperature resistant resin slurry plugging system prepared in Example 1 in a fracture core model (the test temperature is 260° C., and the consolidating time is the optimal consolidating time of the sample) shows that the pressure-bearing plugging strength of the ultra-high temperature resistant resin slurry plugging system suitable for a fractured-vuggy formation in the fracture core may reach 18.2 MPa after consolidating at 260° C. In Comparative Example 1, due to no addition of the flow pattern regulator, the consolidating time of the resin slurry plugging system may be shortened, the rheology of the plugging system may be deteriorated, and the filling agent cannot be suspended and uniformly dispersed, thus affecting the compressive strength and pressure-bearing plugging capacity of the resin slurry plugging system. In Comparative Examples 2-4, the initial consolidating time of the resin slurry plugging system is prolonged without adding the cross-linking agent. Although the safety construction conditions are met, it takes a long time to achieve the optimal consolidating effect, and the consolidating condition is uncontrollable, and the strength and plugging effect of the plugging system are weakened due to the lack of the cross-linking agent. In Comparative Example 5, the retarder is not added. Although it has little effect on the strength and plugging effect of the resin slurry plugging system, but the consolidating time is greatly shortened, which cannot meet the safe construction conditions. In Comparative Examples 6-8, the filling agent is not added, which has a certain effect on the consolidating time of the resin slurry plugging system. According to the data of compressive strength and plugging effect, the filling agent plays an important role in improving the pressure-bearing plugging capacity of the resin slurry plugging system. The data of Comparative Examples 9-15 shows that the structural composition of the composite resin plugging agent, the imidazole-oxazine consolidating agent, and the composite polymer high temperature resistant flow pattern regulator have a significant impact on the pressure-bearing plugging capacity of the plugging system.

It can be seen from the above data that the ultra-high temperature resistant resin slurry plugging system suitable for a fractured-vuggy formation prepared in the Examples of the present disclosure has excellent temperature resistance, compression resistance and plugging effect, and can meet the plugging requirements of an ultra-high temperature reservoir of 180-280° C. By combining filling of flexible resin and bridging of a rigid material, the lose channel plugging of different scales can be adapted, and the problem of lost circulation of an ultra-high temperature fractured-vuggy reservoir can be solved.

The preferred embodiments of the present disclosure have been described in detail above, but the present disclosure is not limited thereto. Within the scope of the inventive concept, a number of simple variants of the technical solution of the present disclosure are possible, including any other suitable combination of the individual features. These simple variants and combinations should likewise be considered as being disclosed as falling within the scope of protection of the present disclosure.