CN108395883B - Honeycomb-shaped gap temporary plugging agent and preparation method thereof - Google Patents
Honeycomb-shaped gap temporary plugging agent and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a temporary plugging agent for honeycomb seams, which is prepared from water and the following raw materials in percentage by weight: 43.5 to 46 percent of acrylamide monomer, 45 to 50 percent of natural polyurethane, 1 to 3 percent of foaming agent sodium dodecyl sulfate, 1 to 5 percent of hydrophilic modified nano silicon dioxide particles, 1 to 3 percent of potassium persulfate and 0.5 to 1 percent of isopropanol. The preparation method comprises the following steps: (1) taking acrylamide monomer, natural polyurethane, foaming agent and nano silicon dioxide particles, adding water with equal mass, premixing, and introducing nitrogen to obtain a foam system; (2) adding potassium persulfate and isopropanol, adding water with equal mass, and reacting until the viscosity of the product rises to a non-flowable rubber plate shape to obtain a honeycomb-shaped rubber plate-shaped product; (3) drying and crushing to obtain the product. The temporary plugging agent for honeycomb seams has higher dissolving speed and lower density in water while keeping higher pressure-bearing capacity.
Description
Technical Field
The invention relates to a honeycomb-shaped gap temporary plugging agent for high-temperature stratum fracturing and a preparation method thereof, belonging to the field of oilfield chemical engineering.
Background
With the continuous development of oil and gas resources in China, reservoir geological conditions are more and more complex, and the exploitation difficulty is more and more high. In recent years, aiming at strong heterogeneity, low permeability and ultra low permeability reservoirs, in order to further improve the transformation efficiency and realize uniform transformation, a temporary blocking steering technology is provided, which is characterized in that a temporary blocking steering agent is added in real time in the hydraulic fracturing process, formed artificial cracks are temporarily blocked, the cracks are forced to initiate and expand in other directions, new cracks are pressed at high pressure, and the fracturing transformation effect is improved by increasing the communication probability. In this technique, a good temporary plugging material is the key to achieving effective temporary plugging of the fracture.
At present, the temporary plugging diversion agent used for fracturing construction at home and abroad is mainly divided into three types of water-soluble temporary plugging diversion agents, self-degradation diversion agents and diversion agents added with gel breakers. Chinese patent applications CN201310698481.3, CN201310698113.9, CN201510925153.1 and the like disclose a fracturing temporary plugging agent which takes degradable fibers as main components, and the fracturing temporary plugging agent is characterized in that plugs have higher pressure bearing capacity. The main components of the diverting agent of the additional gel breaker are copolymer and capsule gel breaker, and when the capsule gel breaker releases persulfate under certain pressure, the copolymer can be oxidized and degraded. In recent years, water-soluble temporary blocking diverters have been used in many cases, and chinese patent applications CN91101010.6, CN200410009408.1, CN103484095A, CN201010599287.6 and the like describe temporary blocking agents containing bone glue, guanidine glue and the like as main components, and chinese patent applications CN201310311159.0, CN201310393381.x, CN201510696920.6 and the like describe water-soluble temporary blocking agents containing modified starch, modified cellulose and the like as main components, which can be slowly dissolved in water to relieve blocking.
Although the temporary plugging agent is widely used in oil fields, the temporary plugging agent has two disadvantages: firstly, the blockage is slowly eliminated, so that the original permeability can be recovered after the blockage for a long time, and the water-soluble speed of the temporary plugging agent needs to be increased; secondly, the temporary plugging agent has high density, is easy to settle in water and needs to be carried by polymer, so the density of the temporary plugging agent needs to be reduced.
Disclosure of Invention
Aiming at the prior art, the invention provides a honeycomb-shaped temporary plugging agent between seams, which has higher dissolving speed and lower density in water while keeping higher pressure-bearing capacity. The invention also provides a preparation method of the composition.
The invention is realized by the following technical scheme:
a honeycomb temporary plugging agent for gaps is prepared from water and the following raw materials in percentage by weight: 43.5 to 46 percent of acrylamide monomer, 45 to 50 percent of natural polyurethane, 1 to 3 percent of foaming agent sodium dodecyl sulfate, 1 to 5 percent of hydrophilic modified nano silicon dioxide particles, 1 to 3 percent of potassium persulfate and 0.5 to 1 percent of isopropanol; is prepared by the following method:
(1) placing an acrylamide monomer, natural polyurethane, a foaming agent sodium dodecyl sulfate and hydrophilic modified nano silica particles (the hydrophilic modified nano silica particles are obtained by conventional purchase) into a wide-mouth bottle, adding water with the same mass as the sum of the mass of the four raw materials, premixing for 50-70 minutes at 60 +/-3 ℃, and then introducing nitrogen until uniform foam is formed to obtain a foam system;
the natural polyurethane is a chain-shaped natural high molecular substance, the molecular weight of the natural polyurethane is 3000-8000, and the natural polyurethane is yellow particles; the bone glue is used and is purchased in the conventional market;
preferably, the average particle size of the hydrophilic modified nano silicon dioxide particles is 30 nm;
(2) adding potassium persulfate (used as an initiator) and isopropanol (used as a chain transfer agent) into the foam system, adding water with the same mass as the sum of the mass of the potassium persulfate and the mass of the isopropanol, reacting at 60 +/-3 ℃ until the viscosity of the product rises to a non-flowable film shape (usually 110-130 minutes) (initiating acrylamide polymerization), and sealing the reaction system in the reaction process to isolate oxygen; after reaction, obtaining a cellular rubber plate-shaped product;
(3) drying the cellular rubber plate-shaped product, crushing the product by a crusher to obtain a cellular gap temporary plugging agent, and sieving the product to obtain cellular solid particle products with different particle sizes, such as a cellular gap temporary plugging agent with a particle size of 1-3 mm and a cellular gap temporary plugging agent with a particle size of 5-8 mm.
The honeycomb temporary plugging agent prepared by the method comprises the following components in percentage by weight: 45-50% of polyacrylamide, 45-50% of natural polyurethane, 1-3% of foaming agent sodium dodecyl sulfate and 1-5% of hydrophilic modified nano silicon dioxide particles.
The temporary plugging agent for the honeycomb seams has higher dissolving speed and lower density in water while keeping higher pressure-bearing capacity, and has the following beneficial effects:
(1) the invention provides a research idea for constructing a fracturing temporary plugging agent by initiating acrylamide polymerization in a low-molecular natural polyester solution which has a low softening point and is easy to dissolve and forming a cross interpenetrating network structure through physical and chemical crosslinking. The viscosity action of the polyamino acid ester controls the homopolymerized molecular weight of the acrylamide, the dissolution of the acrylamide is accelerated through water absorption and permeation, and the short-time temperature resistance and the toughness of the polyamino acid ester can be improved through a high-strength network structure formed by mutual crosslinking of the polyacrylamide and the polyamino acid ester.
(2) The nano silicon dioxide particles form hydrogen bonds with amide groups to construct another form of secondary network, so that the strength of the rubber plate is further enhanced.
(3) The cellular structure is endowed with the slab rubber by introducing the foam, so that the formed solid particles have low density and are easy to suspend, and in addition, the contact area of the solid particles and water is increased due to the cellular structure, and the dissolution speed in the water is increased.
Detailed Description
The present invention will be further described with reference to the following examples.
The instruments, reagents, materials and the like used in the following examples are conventional instruments, reagents, materials and the like in the prior art and are commercially available in a normal manner unless otherwise specified. Unless otherwise specified, the experimental methods, detection methods, and the like described in the following examples are conventional experimental methods, detection methods, and the like in the prior art.
The natural polyurethane used in the following examples was bone glue, which was commercially available.
EXAMPLE 1 preparation of Honeycomb Interval temporary plugging agent and evaluation of its Properties
Adding 44.75g of acrylamide, 47.5g of natural polyurethane, 2g of sodium dodecyl sulfate and 3g of hydrophilic modified nano silicon dioxide into a wide-mouth bottle, adding 97.25g of water, placing the wide-mouth bottle in a constant-temperature water bath at 60 ℃, preheating, stirring and uniformly mixing for 1 hour, and introducing nitrogen at a low speed to form uniform foam; adding 2g of potassium persulfate and 0.75g of isopropanol into a wide-mouth bottle, adding 2.75g of water, sealing, reacting at 60 ℃, taking out after the reaction is complete (namely the viscosity of the product is raised to be in a non-flowable film shape), cooling to room temperature, and stopping the reaction; and taking out the product, placing the product in an oven, drying for 72h at 35 ℃, crushing and sieving to obtain a honeycomb faint yellow solid granular temporary plugging agent product with different grain sizes of 1-3 mm, 5-8mm and the like, wherein the product is yellow granular, and honeycomb fine holes can be observed on the surface of the product.
The temporary plugging agent prepared by the method is subjected to solubility test and plugging performance measurement to evaluate the stratum pollution and temporary plugging performance:
(1) solubility test
About 0.5g of temporary plugging agent is added into a test tube with a plug, water is added to 50g (namely the mass fraction of the temporary plugging agent is 1 percent), and the complete dissolution time of the temporary plugging agent with different particle sizes is measured at different temperatures. The results are shown in Table 1, and show that the dissolution time of the temporary plugging agent is influenced by the particle size and the dissolution temperature, and the temporary plugging agent can be completely dissolved within 11 hours, has no residue and has no harm to the stratum.
TABLE 1 dissolution time of different particle size temporary plugging agents
| Particle size/mm | Dissolution time at 80 ℃ per hour | 120 ℃ dissolution time/h |
| 1～3 | 8 | 2 |
| 5～8 | 11 | 3 |
(2) Experiment of pressure-resistant plugging performance
Quartz sand of 40-60 meshes is selected, a sand filling pipe is filled in a wet filling mode, and the permeability is about 3000 mD. A10 mm gap is reserved at the injection end of the sand filling pipe, temporary plugging agent particles are used for filling, a water injection experiment is carried out at different temperatures at a rate of 5ml/min, and the maximum injection pressure is used for representing the plugging breakthrough pressure. The results are shown in table 2, and the results show that the temporary plugging agent can form an effective filter cake, plug a hypertonic channel, has strong plugging effect and can bear high pressure, the maximum breakthrough pressure at 80 ℃ reaches 9MPa, and the maximum breakthrough pressure at 120 ℃ reaches 8MPa, so that the temporary plugging agent plays an effective plugging effect; the plugging agent has good plugging effect at 120 ℃ high-temperature stratum and is suitable for temporary plugging of the high-temperature stratum.
TABLE 2 breakthrough pressures for different particle sizes of temporary plugging agents
| Particle size/mm | 80 ℃ breakthrough pressure/MPa | 120 ℃ breakthrough pressure/MPa |
| 1～3 | 7 | 6 |
| 5～8 | 9 | 8 |
The solubility and plugging performance results show that the product can be dissolved in a short time, the high-temperature stratum (120 ℃) is dissolved more quickly, the stratum is free from pollution, and the production recovery is rapid; and the product can form an effective filter cake, and generates an excellent plugging effect after water absorption and expansion. The temporary plugging agent has two performances, and the temporary plugging agent has wide adaptability.
EXAMPLE 2 preparation of Honeycomb Intergap temporary plugging agent and evaluation of its Properties
Taking 46g of acrylamide, 45g of natural polyurethane, 2g of sodium dodecyl sulfate and 3g of hydrophilic modified nano-silica (compared with example 1, the content of the polyacrylamide is increased, and the content of the natural polyurethane is reduced), adding the obtained mixture into a wide-mouth bottle, adding 96g of water, placing the wide-mouth bottle in a constant-temperature water bath at 60 ℃, preheating, stirring and uniformly mixing for 1 hour, and introducing nitrogen at a low speed to form uniform foam; adding 3g of potassium persulfate and 1g of isopropanol into a wide-mouth bottle, adding 4g of water, sealing, and reacting at 60 ℃; taking out after the reaction is complete (namely the viscosity of the product is raised to be in a shape of a non-flowable rubber plate), cooling to room temperature, and stopping the reaction; and taking out the product, placing the product in an oven, drying for 72h at 35 ℃, crushing and sieving to obtain honeycomb faint yellow solid granular temporary plugging agent products with different grain sizes of 1-3 mm, 5-8mm and the like.
The temporary plugging agent prepared by the method is subjected to solubility test and plugging performance measurement to evaluate the stratum pollution and temporary plugging performance:
(1) solubility test
About 0.5g of temporary plugging agent is added into a test tube with a plug, water is added to 50g (namely the mass fraction of the temporary plugging agent is 1 percent), and the complete dissolution time of the temporary plugging agent with different particle sizes is measured at different temperatures. The results are shown in Table 3.
TABLE 3 dissolution time of different particle size temporary plugging agents
| Particle size/mm | Dissolution time at 80 ℃ per hour | 120 ℃ dissolution time/h |
| 1～3 | 9 | 3 |
| 5～8 | 12 | 5 |
(2) Experiment of pressure-resistant plugging performance
Quartz sand of 40-60 meshes is selected, a sand filling pipe is filled in a wet filling mode, and the permeability is about 3000 mD. A10 mm gap is reserved at the injection end of the sand filling pipe, temporary plugging agent particles are used for filling, a water injection experiment is carried out at different temperatures at a rate of 5ml/min, and the maximum injection pressure is used for representing the plugging breakthrough pressure. The results are shown in Table 4.
TABLE 4 breakthrough pressures of different particle sizes of temporary plugging agents
| Particle size/mm | 80 ℃ breakthrough pressure/MPa | 120 ℃ breakthrough pressure/MPa |
| 1～3 | 9 | 7 |
| 5～8 | 11 | 9 |
The solubility and plugging performance results show that the solubility of the product is slightly reduced after the content of polyacrylamide in the product is increased and the content of natural polyurethane is reduced, but the high-temperature stratum (120 ℃) can be completely dissolved within 5 hours, so that the pollution to the stratum is avoided, and the production is quickly recovered; the plugging performance is also improved along with the increase of the content of polyacrylamide and the reduction of the content of natural polyurethane, because the polyacrylamide has higher molecular weight and generates excellent plugging effect by water absorption expansion. Considering the solubility effect of the product, namely the product can be completely dissolved in a short time, the addition amount of the polyacrylamide is ensured to be less than 50 percent, and the addition amount of the natural polyurethane is not less than 45 percent.
EXAMPLE 3 preparation of Honeycomb Interval temporary plugging agent and evaluation of its Properties
Adding 43.5g of acrylamide, 50g of natural polyurethane, 2g of sodium dodecyl sulfate and 3g of hydrophilic modified nano silicon dioxide (compared with example 1, the content of the natural polyurethane is improved, and the content of the polyacrylamide is reduced) into a wide-mouth bottle, adding 98.5g of water, placing the wide-mouth bottle in a constant-temperature water bath at 60 ℃ for preheating, stirring and uniformly mixing for 1 hour, and introducing nitrogen at low speed to form uniform foam; adding 1g of potassium persulfate and 0.5g of isopropanol into a wide-mouth bottle, adding 1.5g of water, sealing, reacting at 60 ℃, taking out after the reaction is complete (namely the viscosity of the product is increased to be in a non-flowable film shape), cooling to room temperature, and stopping the reaction; and taking out the product, placing the product in an oven, drying for 72h at 35 ℃, crushing and sieving to obtain honeycomb faint yellow solid granular temporary plugging agent products with different grain sizes of 1-3 mm, 5-8mm and the like.
The temporary plugging agent prepared by the method is subjected to solubility test and plugging performance measurement to evaluate the stratum pollution and temporary plugging performance:
(1) solubility test
About 0.5g of temporary plugging agent is added into a test tube with a plug, water is added to 50g (namely the mass fraction of the temporary plugging agent is 1 percent), and the complete dissolution time of the temporary plugging agent with different particle sizes is measured at different temperatures. The results are shown in Table 5.
TABLE 5 dissolution time of different particle size temporary plugging agents
| Particle size/mm | Dissolution time at 80 ℃ per hour | 120 ℃ dissolution time/h |
| 1～3 | 7 | 1.5 |
| 5～8 | 9 | 2 |
(2) Experiment of pressure-resistant plugging performance
Quartz sand of 40-60 meshes is selected, a sand filling pipe is filled in a wet filling mode, and the permeability is about 3000 mD. A10 mm gap is reserved at the injection end of the sand filling pipe, temporary plugging agent particles are used for filling, a water injection experiment is carried out at different temperatures at a rate of 5ml/min, and the maximum injection pressure is used for representing the plugging breakthrough pressure. The results are shown in Table 6.
TABLE 6 breakthrough pressures of different particle sizes of temporary plugging agents
| Particle size/mm | 80 ℃ breakthrough pressure/MPa | 120 ℃ breakthrough pressure/MPa |
| 1～3 | 6 | 5 |
| 5～8 | 8 | 7 |
The solubility and plugging performance results of the temporary plugging agent show that after the content of natural polyurethane in the product is increased and the content of polyacrylamide is reduced, the water solubility of the product is enhanced, even if large particles (5-8mm) in a low-temperature stratum can be completely dissolved within 9h, plugging is rapidly removed, production can be recovered within a short time, and the temporary plugging agent has no harm to the stratum; but the plugging performance is reduced along with the increase of the content of the natural polyurethane and the reduction of the content of the polyacrylamide, because the molecular weight of the natural polyurethane is low, the water absorption and the dissolution are faster, the skeleton strength of the temporary plugging agent is reduced after partial dissolution, and the integral pressure-bearing capacity is slightly reduced. Considering the plugging performance of the temporary plugging agent, namely the temporary plugging agent can bear the pressure required by fracturing at high temperature, the addition amount of the natural polyurethane is not higher than 50%, and the addition amount of the polyacrylamide is not lower than 45%.
EXAMPLE 4 preparation of Honeycomb Interval temporary plugging agent and evaluation of its Properties
Taking 44.5g of acrylamide, 47g of natural polyurethane, 3g of sodium dodecyl sulfate and 3g of hydrophilic modified nano silicon dioxide (compared with the embodiment 1, the content of the foaming agent is improved), adding the mixture into a wide-mouth bottle, adding 97.5g of water, placing the wide-mouth bottle in a constant-temperature water bath at 60 ℃, preheating, stirring and uniformly mixing for 1 hour, and introducing nitrogen at a low speed to form uniform foam; adding 1.8g of potassium persulfate and 0.7g of isopropanol into a wide-mouth bottle, adding 2.5g of water, sealing, reacting at 60 ℃, taking out after the reaction is complete (namely the viscosity of the product is increased to be in a non-flowable film shape), cooling to room temperature, and stopping the reaction; and taking out the product, placing the product in an oven, drying for 72h at 35 ℃, crushing and sieving to obtain honeycomb faint yellow solid granular temporary plugging agent products with different grain sizes of 1-3 mm, 5-8mm and the like.
The temporary plugging agent prepared by the method is subjected to solubility test and plugging performance measurement to evaluate the stratum pollution and temporary plugging performance:
(1) solubility test
About 0.5g of temporary plugging agent is added into a test tube with a plug, water is added to 50g (namely the mass fraction of the temporary plugging agent is 1 percent), and the complete dissolution time of the temporary plugging agent with different particle sizes is measured at different temperatures. The results are shown in Table 7.
TABLE 7 dissolution time of different particle size temporary plugging agents
| Particle size/mm | Dissolution time at 80 ℃ per hour | 120 ℃ dissolution time/h |
| 1～3 | 7 | 1 |
| 5～8 | 10 | 1.5 |
(2) Experiment of pressure-resistant plugging performance
Quartz sand of 40-60 meshes is selected, a sand filling pipe is filled in a wet filling mode, and the permeability is about 3000 mD. A10 mm gap is reserved at the injection end of the sand filling pipe, temporary plugging agent particles are used for filling, a water injection experiment is carried out at different temperatures at a rate of 5ml/min, and the maximum injection pressure is used for representing the plugging breakthrough pressure. The results are shown in Table 8.
TABLE 8 breakthrough pressures of different particle sizes of temporary plugging agents
| Particle size/mm | 80 ℃ breakthrough pressure/MPa | 120 ℃ breakthrough pressure/MPa |
| 1～3 | 7 | 5 |
| 5～8 | 8 | 6 |
After the product is prepared, more honeycomb-shaped air holes can be observed in appearance, because the foam generation amount and the stability are increased in the synthesis process after the proportion of the foaming agent is increased, the foam loss in the process of polymerizing into the rubber plate is less, and the product shows that the honeycomb-shaped air holes are increased. The solubility and plugging performance results of the temporary plugging agent show that the proportion of the foaming agent is improved, the water solubility of the product is enhanced, and particularly the dissolution in a high-temperature stratum is obviously accelerated, which is caused by the increase of the number of honeycomb-shaped air holes and the increase of the contact area with a solvent; the plugging performance is reduced with the increase of the foaming agent, because the increase of the honeycomb-shaped air holes leads to the accelerated softening of the particles, the reduction of the framework strength and the reduction of the plugging pressure. In order to ensure that the product has good blocking performance, the addition amount of the foaming agent in the system is not higher than 3%.
EXAMPLE 5 preparation of Honeycomb Intergap temporary plugging agent and evaluation of its Properties
Taking 45g of acrylamide, 48g of natural polyurethane, 1g of sodium dodecyl sulfate and 3g of hydrophilic modified nano silicon dioxide (compared with the embodiment 1, the content of a foaming agent is reduced), adding the mixture into a wide-mouth bottle, adding 97g of water, placing the wide-mouth bottle in a constant-temperature water bath at 60 ℃, preheating, stirring and uniformly mixing the mixture for 1 hour, and introducing nitrogen at a low speed to form uniform foam; adding 2.2g of potassium persulfate and 0.8g of isopropanol into a wide-mouth bottle, adding 3g of water, sealing, reacting at 60 ℃, taking out after the reaction is complete (namely the viscosity of the product is increased to be in a non-flowable film shape), cooling to room temperature, and stopping the reaction; and taking out the product, placing the product in an oven, drying for 72h at 35 ℃, crushing and sieving to obtain honeycomb faint yellow solid granular temporary plugging agent products with different grain sizes of 1-3 mm, 5-8mm and the like.
The temporary plugging agent prepared by the method is subjected to solubility test and plugging performance measurement to evaluate the stratum pollution and temporary plugging performance:
(1) solubility test
About 0.5g of temporary plugging agent is added into a test tube with a plug, water is added to 50g (namely the mass fraction of the temporary plugging agent is 1 percent), and the complete dissolution time of the temporary plugging agent with different particle sizes is measured at different temperatures. The results are shown in Table 9.
TABLE 9 dissolution time of different particle size temporary plugging agents
| Particle size/mm | Dissolution time at 80 ℃ per hour | 120 ℃ dissolution time/h |
| 1～3 | 10 | 3 |
| 5～8 | 13 | 4 |
(2) Experiment of pressure-resistant plugging performance
Quartz sand of 40-60 meshes is selected, a sand filling pipe is filled in a wet filling mode, and the permeability is about 3000 mD. A10 mm gap is reserved at the injection end of the sand filling pipe, temporary plugging agent particles are used for filling, a water injection experiment is carried out at different temperatures at a rate of 5ml/min, and the maximum injection pressure is used for representing the plugging breakthrough pressure. The results are shown in Table 10.
TABLE 10 breakthrough pressures of different particle sizes of temporary plugging agents
| Particle size/mm | 80 ℃ breakthrough pressure/MPa | 120 ℃ breakthrough pressure/MPa |
| 1～3 | 8 | 6 |
| 5～8 | 10 | 8 |
After the product is prepared, the appearance of the product is obviously reduced in cellular pores, because the foaming agent ratio is reduced, the foam generation amount is reduced in the synthesis process, the stability is reduced, the number of the formed pores of the foam in the process of polymerizing the product into the rubber plate is less, and the product shows that the cellular pores are reduced. The solubility and plugging performance results of the temporary plugging agent show that the foaming agent proportion is reduced, the product solubility is reduced, and particularly the dissolution time in a low-temperature stratum is prolonged, which is caused by the reduction of the number of honeycomb-shaped air holes and the reduction of the contact area with a solvent; the plugging performance is increased with the decrease of the foaming agent, because the cellular air holes are decreased to make the particles more compact, the skeleton strength is increased, and the plugging pressure is improved. In order to ensure that the product has good solubility, the addition amount of the foaming agent in the system is not less than 1%.
EXAMPLE 6 preparation of Honeycomb Interval temporary plugging agent and evaluation of its Properties
Taking 44.25g of acrylamide, 46g of natural polyurethane, 2g of sodium dodecyl sulfate and 5g of hydrophilic modified nano-silica (compared with example 1, the content of the nano-silica is improved), adding the mixture into a wide-mouth bottle, adding 97.25g of water, placing the wide-mouth bottle in a constant-temperature water bath at 60 ℃, preheating, stirring and uniformly mixing for 1 hour, and introducing nitrogen at a low speed to form uniform foam; adding 1.6g of potassium persulfate and 0.65g of isopropanol into a wide-mouth bottle, adding 2.25g of water, sealing, reacting at 60 ℃, taking out after the reaction is complete (namely the viscosity of the product is increased to be in a non-flowable film shape), cooling to room temperature, and stopping the reaction; and taking out the product, placing the product in an oven, drying for 72h at 35 ℃, crushing and sieving to obtain honeycomb faint yellow solid granular temporary plugging agent products with different grain sizes of 1-3 mm, 5-8mm and the like.
The temporary plugging agent prepared by the method is subjected to solubility test and plugging performance measurement to evaluate the stratum pollution and temporary plugging performance:
(1) solubility test
About 0.5g of temporary plugging agent is added into a test tube with a plug, water is added to 50g (namely the mass fraction of the temporary plugging agent is 1 percent), and the complete dissolution time of the temporary plugging agent with different particle sizes is measured at different temperatures. The results are shown in Table 11.
TABLE 11 dissolution times of different particle size temporary plugging agents
| Particle size/mm | Dissolution time at 80 ℃ per hour | 120 ℃ dissolution time/h |
| 1～3 | 7 | 2 |
| 5～8 | 10 | 3 |
(2) Experiment of pressure-resistant plugging performance
Quartz sand of 40-60 meshes is selected, a sand filling pipe is filled in a wet filling mode, and the permeability is about 3000 mD. A10 mm gap is reserved at the injection end of the sand filling pipe, temporary plugging agent particles are used for filling, a water injection experiment is carried out at different temperatures at a rate of 5ml/min, and the maximum injection pressure is used for representing the plugging breakthrough pressure. The results are shown in Table 12.
TABLE 12 breakthrough pressures of different particle sizes of temporary plugging agents
| Particle size/mm | 80 ℃ breakthrough pressure/MPa | 120 ℃ breakthrough pressure/MPa |
| 1～3 | 8 | 7 |
| 5～8 | 10 | 9 |
The solubility and the plugging performance of the temporary plugging agent show that the solubility of the product is almost unchanged or slightly reduced after the content of the nano particles in the product is improved, and the production is recovered quickly; the blocking performance is improved along with the increase of the nano particles, because the nano silicon dioxide particles form hydrogen bonds with amide groups to construct another form of secondary network, and the strength of the temporary blocking agent product is further enhanced. Considering the high cost of the nanoparticles, it is recommended that the amount of nanoparticles added in the product is not more than 5%.
Example 7 preparation of Honeycomb Intergap temporary plugging agent and evaluation of its Properties
Taking 45.5g of acrylamide, 49g of natural polyurethane, 2g of sodium dodecyl sulfate and 1g of hydrophilic modified nano-silica (compared with the embodiment 1, the content of the nano-silica is reduced), adding the mixture into a wide-mouth bottle, adding 97.5g of water, placing the wide-mouth bottle in a constant-temperature water bath at 60 ℃, preheating, stirring and uniformly mixing for 1 hour, and introducing nitrogen at a low speed to form uniform foam; adding 2.6g of potassium persulfate and 0.9g of isopropanol into a wide-mouth bottle, adding 3.5g of water, sealing, reacting at 60 ℃, taking out after the reaction is complete (namely the viscosity of the product is increased to be in a non-flowable film shape), cooling to room temperature, and stopping the reaction; and taking out the product, placing the product in an oven, drying for 72h at 35 ℃, crushing and sieving to obtain honeycomb faint yellow solid granular temporary plugging agent products with different grain sizes of 1-3 mm, 5-8mm and the like.
The temporary plugging agent prepared by the method is subjected to solubility test and plugging performance measurement to evaluate the stratum pollution and temporary plugging performance:
(1) solubility test
About 0.5g of temporary plugging agent is added into a test tube with a plug, water is added to 50g (namely the mass fraction of the temporary plugging agent is 1 percent), and the complete dissolution time of the temporary plugging agent with different particle sizes is measured at different temperatures. The results are shown in Table 13. The result shows that the dissolution time of the temporary plugging agent is influenced by the particle size and the dissolution temperature, and the temporary plugging agent can be completely dissolved within 11 hours without residues and damage to the stratum.
TABLE 13 dissolution times of different particle size temporary plugging agents
| Particle size/mm | Dissolution time at 80 ℃ per hour | 120 ℃ dissolution time/h |
| 1～3 | 9 | 2 |
| 5～8 | 11 | 3 |
(2) Experiment of pressure-resistant plugging performance
Quartz sand of 40-60 meshes is selected, a sand filling pipe is filled in a wet filling mode, and the permeability is about 3000 mD. A10 mm gap is reserved at the injection end of the sand filling pipe, temporary plugging agent particles are used for filling, a water injection experiment is carried out at different temperatures at a rate of 5ml/min, and the maximum injection pressure is used for representing the plugging breakthrough pressure. The results are shown in Table 14.
TABLE 14 breakthrough pressures for different particle sizes of temporary plugging agents
| Particle size/mm | 80 ℃ breakthrough pressure/MPa | 120 ℃ breakthrough pressure/MPa |
| 1～3 | 6 | 5 |
| 5～8 | 8 | 7 |
The results of the solubility and the plugging performance of the temporary plugging agent show that the solubility of the product is not greatly changed after the content of the nano particles in the product is reduced, and the production can be quickly recovered in a short time; the plugging performance is reduced along with the reduction of the nano particles, because the nano silicon dioxide particles can form hydrogen bonds with amide groups, the strength of the temporary plugging agent product can be enhanced, the nano particles are reduced, the cohesive force of the particles is reduced, and the pressure bearing capacity is limited. In order to ensure that the temporary plugging agent product has good plugging performance, the addition amount of the nano particles in the product is not less than 1 percent.
Although the specific embodiments of the present invention have been described with reference to the examples, the scope of the present invention is not limited thereto, and those skilled in the art will appreciate that various modifications and variations can be made without inventive effort by those skilled in the art based on the technical solution of the present invention.
Claims (5)
1. A temporary plugging agent for honeycomb seams is characterized in that: is prepared from water and the following raw materials in percentage by weight: 43.5 to 46 percent of acrylamide monomer, 45 to 50 percent of bone glue, 1 to 3 percent of foaming agent sodium dodecyl sulfate, 1 to 5 percent of hydrophilic modified nano silicon dioxide particles, 1 to 3 percent of potassium persulfate and 0.5 to 1 percent of isopropanol.
2. A honeycomb inter-slit temporary plugging agent according to claim 1, wherein: is prepared by the following method:
(1) taking an acrylamide monomer, bone glue, a foaming agent sodium dodecyl sulfate and hydrophilic modified nano silicon dioxide particles, adding water with the same mass as the sum of the mass of the four raw materials, premixing for 50-70 minutes at 60 +/-3 ℃, and then introducing nitrogen until uniform foam is formed to obtain a foam system;
(2) adding potassium persulfate and isopropanol into the foam system, adding water with the same mass as the sum of the mass of the potassium persulfate and the mass of the isopropanol, reacting at 60 +/-3 ℃ until the viscosity of the product rises to be in a non-flowable rubber plate shape, sealing the reaction system in the reaction process, and isolating oxygen; after reaction, obtaining a cellular rubber plate-shaped product;
(3) and drying and crushing the honeycomb-shaped rubber plate product to obtain the temporary plugging agent for the honeycomb seams.
3. A honeycomb inter-slit temporary plugging agent according to claim 1, wherein: the average particle diameter of the hydrophilic modified nano silicon dioxide particles is 30 nm.
4. A honeycomb-shaped interseam temporary plugging agent according to any one of claims 1 to 3, characterized in that: is prepared from water and the following raw materials in percentage by weight: 44.75 percent of acrylamide monomer, 47.5 percent of bone glue, 2 percent of foaming agent sodium dodecyl sulfate, 3 percent of hydrophilic modified nano silicon dioxide particles, 2 percent of potassium persulfate and 0.75 percent of isopropanol.
5. The method for preparing a honeycomb-shaped temporary plugging agent between seams according to any one of claims 1 to 4, wherein: the method comprises the following steps:
(1) taking an acrylamide monomer, bone glue, a foaming agent sodium dodecyl sulfate and hydrophilic modified nano silicon dioxide particles, adding water with the same mass as the sum of the mass of the four raw materials, premixing for 50-70 minutes at 60 +/-3 ℃, and then introducing nitrogen until uniform foam is formed to obtain a foam system;
(2) adding potassium persulfate and isopropanol into the foam system, adding water with the same mass as the sum of the mass of the potassium persulfate and the mass of the isopropanol, reacting at 60 +/-3 ℃ until the viscosity of the product rises to be in a non-flowable rubber plate shape, sealing the reaction system in the reaction process, and isolating oxygen; after reaction, obtaining a cellular rubber plate-shaped product;
(3) and drying and crushing the honeycomb-shaped rubber plate product to obtain the temporary plugging agent for the honeycomb seams.
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| CN109551626B (en) * | 2018-10-16 | 2021-04-30 | 中国石油天然气股份有限公司 | Sand washing temporary plugging agent particles and sand washing temporary plugging liquid prepared from waste ultralight clay and preparation |
| CN109777387B (en) * | 2019-03-05 | 2021-06-08 | 中国石油大学(华东) | Repeated fracturing temporary plugging agent and preparation method and application thereof |
| CN110156940A (en) * | 2019-06-05 | 2019-08-23 | 江西富诚生态环境科技集团有限公司 | A kind of diverting agent polymer and synthesis technology |
| CN111720102B (en) * | 2020-06-05 | 2022-05-20 | 青岛鑫源晟石油科技有限公司 | Fine temporary plugging volume fracturing technology replacing mechanical packing |
| CN117126340A (en) * | 2023-07-14 | 2023-11-28 | 西安川秦石油科技有限公司 | Water-soluble temporary plugging agent for oil well fracturing and preparation method thereof |
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