CN113980663B - High-temperature-resistant self-foaming expansion silicone rubber plugging material and preparation method thereof - Google Patents
High-temperature-resistant self-foaming expansion silicone rubber plugging material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a high temperature resistant self-foaming expansion silicon rubber plugging material and a preparation method thereof, wherein the material comprises 0.1-1% of a flow pattern regulator, 5-30% of a temperature control self-foaming expansion plugging agent and 1-5% of rigid particles; 3-15% of carbon nano tube; 0.5-1% of temperature activator, 40-60% of density regulator and the balance of deionized water. And uniformly mixing the monomer and the catalyst organic solvent, volatilizing at room temperature, solidifying, freezing, crushing and sieving to obtain the temperature-controlled self-foaming expansion plugging agent. And uniformly mixing the rest raw materials and the temperature-controlled self-foaming expansion plugging agent in deionized water to obtain the composite material. The material prepared by the method has a self-adaptive function, the foaming degree and the foaming starting temperature can be adjusted by adjusting the content of the catalyst in the dynamic cross-linked network structure and the content of the temperature activator, and the material is suitable for plugging cracks under different complicated address conditions. The plugging material is aged for 24 hours at 200 ℃, the rheological property change of the plugging material is very small, and the application range is wide.
Description
Technical Field
The invention belongs to the field of materials, and particularly relates to a preparation method of a high-temperature-resistant self-foaming expansion silicone rubber plugging material and the high-temperature-resistant self-foaming expansion silicone rubber plugging material prepared by the preparation method.
Background
Traditional silicone rubber cannot be thermoplastically processed due to the presence of a permanent crosslinked network, and is relatively poor in adaptivity. The prior patent reports that the thermoplastic processing of the silicon rubber can be realized by initiating dynamic reversible covalent bonds in a silicon rubber network, but the introduction of the dynamic bonds reduces the temperature resistance and can not be used in a high-temperature environment for a long time. The self-adaptive silicone rubber material has a plurality of application fields, such as 3D printing, and has no report on the application in the field of oil and gas field exploitation and leakage stoppage.
Lost circulation is one of the most common technical problems in drilling engineering. At present, serious leakage problems still exist in deep ultra-deep layer, deep water and unconventional oil and gas exploration. Lost circulation severely restricts the drilling speed, causes huge economic loss and even causes immeasurable damage to the reservoir. The chemical plugging material has various types and wide application, and can effectively plug different leakage layers according to respective performance characteristics. At present, many novel drilling fluid leakage-proof plugging materials are researched and developed at home and abroad, such as intelligent plugging materials with shape memory characteristics, nano-micron plugging agents for nano-micron pore leakage stratum and the like. The leakage passage of the complex stratum usually has multi-scale characteristics and uncertainty, the traditional inert bridging plugging material (mineral, plant particles and the like) has poor deformability, the plugging effect is sensitive to the size of a leakage layer, the adaptivity and the broad spectrum are poor, and the door sealing or the leakage to the deep part is easy to generate, so that the leakage plugging failure is often caused. When treating malignant leakage with larger crack opening, the conventional large-size and high-density plugging material has poor suspension stability, is easy to settle in a mud tank and a shaft, and has the risk of plugging a drilling tool.
In recent years, intelligent polymer materials such as hydrogel, shape memory elastomers, gel polymers and water-swellable resins are widely applied to plugging materials, have certain elastoplasticity after water swelling, and have certain improvement on the adaptability of plugging cracks, but the swelling speed and strength after water swelling are difficult to control, the rheological property and the temperature resistance of a plugging system are insufficient, and the plugging pressure-bearing capacity and the plugging effect are not ideal. The polymer material which can resist high temperature (more than 200 ℃) is generally a special rigid high polymer material, and has poor adaptability and poor plugging effect along with the change of the size of the crust crack.
In view of the defects, the field puts higher requirements on the comprehensive performance of the plugging material for the well leakage of the complex stratum, so that the exploration and development of a new generation of intelligent plugging material with high-efficiency pressure bearing, high temperature resistance and self-adaption is urgent.
Disclosure of Invention
Based on the analysis, the invention provides a leaking stoppage material which can effectively solve the problems that the molecular chain of the traditional silicone rubber is particularly flexible and has poor mechanical property; the thermoplastic processing cannot be carried out, and the self-adaptability is poor; the temperature resistance of a plugging material for oil and gas field exploitation is poor; the self-adaptability of the plugging material for oil and gas field exploitation is poor, and when the crack of the ground shell is enlarged, the technical problem of further leakage can occur.
The invention is realized by the following means:
a high-temperature resistant self-foaming expansion silicone rubber plugging material comprises:
0.1-1% of flow pattern regulator;
5-30% of temperature control self-foaming expansion plugging agent;
1-5% of rigid particles;
3-15% of carbon nano tube;
0.5-1% of temperature activator;
40-60% of density regulator; and
the balance being deionized water.
Further, the high-temperature-resistant self-foaming expansion silicone rubber plugging material comprises:
flow pattern regulator 0.5%;
15% of temperature control self-foaming expansion plugging agent;
2% of rigid particles;
10% of carbon nano tube;
0.7% of temperature activator;
50% of density regulator; and
the balance being deionized water.
The invention also discloses a method for preparing the high-temperature-resistant self-foaming expansion silicon rubber plugging material, which comprises the following steps:
uniformly mixing a flow pattern regulator, a temperature control self-foaming expansion plugging agent, rigid particles, carbon nano tubes, a temperature activator and a density regulator in deionized water.
Further, the flow pattern regulator is selected from any one of polyacrylamide-polybutyl acrylate, scleroglucan and sodium styrene sulfonate mixture.
Further, the temperature control self-foaming expansion plugging agent is silicon rubber particles, the particle size of the silicon rubber particles is 100 mu m-10 mm, and the activation temperature is more than or equal to 70 ℃;
the temperature-control self-foaming expansion plugging agent is prepared by the following method:
uniformly mixing hydroxyl-terminated polydimethylsiloxane, tetramethyl m-xylylene diisocyanate, hexamethylene diisocyanate trimer, silicon-hydrogen bond-terminated polydimethylsiloxane, double bond-terminated polydimethylsiloxane and dibutyltin dilaurate in tetrahydrofuran, pouring into a mold, volatilizing at room temperature, curing, freezing and crushing the cured material under liquid nitrogen, and sieving to obtain the temperature-controlled self-foaming expansion plugging agent.
Further, the rigid particles are selected from ground calcium carbonate or ultrafine calcium carbonate.
Further, the carbon nanotube is selected from any one of a single-arm carbon nanotube, a multi-arm carbon nanotube, and a mixture of a single-arm carbon nanotube and a multi-arm carbon nanotube.
Further, the density regulator is selected from any one of a saturated potassium formate solution, a saturated zinc bromide solution, and a mixed solution of a saturated potassium formate solution and a saturated zinc bromide solution.
Further, the temperature activator is zinc perchlorate.
The invention also discloses a high-temperature-resistant self-foaming expansion silicone rubber plugging material prepared by any one of the preparation methods.
The invention has the beneficial effects that:
(1) the self-made temperature control self-foaming expansion plugging agent contains two cross-linked networks and forms an interpenetrating network structure, one is a permanent cross-linked network, the other is a dynamic self-foaming expansion network, the dynamic network can be recombined under thermal stimulation, and the self-adaptive temperature control self-foaming expansion plugging agent has a self-adaptive function; based on the existence of the double-network structure, the particles can be fused at the high-temperature crust crack, so that the plugging effect is enhanced; meanwhile, the mechanical strength of the silicon rubber material reaches 11 MPa. Under the conditions of high temperature and water existence, the dynamic crosslinking network reacts with water to generate gas foaming, the volume of the material expands, and the permanent network can maintain the mechanical property and the shape of the material. The temperature-control self-foaming expansion plugging agent can be used for oil and gas field exploitation plugging materials, and particles can foam and self-expand when entering a crust crack. In addition, the temperature-control self-foaming expansion plugging agent has high elasticity, and the volume of the material can change along with the size change of a crack after the material enters the crack of the earth crust, so that the intelligent plugging effect is achieved.
(2) The high-temperature-resistant self-foaming expansion silicone rubber plugging material prepared by the invention and the formula can be used for a long time at the temperature of 200 ℃; the foaming degree and the foaming starting temperature can be adjusted by adjusting the content of the catalyst and the content of the temperature activator in the dynamic cross-linked network structure, and the method is suitable for plugging cracks under different complicated address conditions. The plugging material is aged for 24 hours at 200 ℃, and the rheological property change of the plugging material is very small (the ratio of the dynamic shear force at 200 ℃ to the dynamic shear force at 2 ℃ is 0.9-1.5).
Drawings
FIG. 1 is a stress-strain curve of the temperature-controlled self-foaming intumescent plugging agent prepared in example 1.
Fig. 2 is thermal degradation data of the temperature controlled self-foaming intumescent plugging agent prepared in example 1.
Fig. 3 is an optical photograph of the temperature-controlled self-foaming intumescent plugging agent prepared in example 2.
Fig. 4 is an optical photograph of the temperature controlled self-foaming intumescent plugging agent prepared in example 4 before and after heating.
FIG. 5 is an optical photograph of the temperature controlled self-foaming intumescent plugging agent prepared in example 4 before and after heating at 20MPa and 130 ℃.
Fig. 6 is a schematic diagram of a dual-network structure of the temperature-controlled self-foaming expansion plugging agent prepared in examples 1 to 4.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other examples, which may be modified or appreciated by those of ordinary skill in the art based on the examples given herein, are intended to be within the scope of the present invention.
The raw materials used in the examples are conventional raw materials and can be obtained commercially; the method is a conventional method and the prior art unless otherwise specified.
Example 1
A preparation method of a temperature-control self-foaming expansion plugging agent comprises the following steps:
5g of hydroxyl-terminated polydimethylsiloxane (molecular weight is less than 300g/mol), 3g of tetramethyl m-xylylene diisocyanate, 4g of hexamethylene diisocyanate trimer, 6g of silicon hydrogen bond-terminated polydimethylsiloxane, 6g of double bond-terminated polydimethylsiloxane and 5 drops of dibutyltin dilaurate are uniformly mixed in 40ml of tetrahydrofuran, poured into a polytetrafluoroethylene mold, volatilized at room temperature for 16h, and then cured at 100 ℃ for 24 h. And (3) freezing and crushing the cured silicone rubber elastomer under the assistance of liquid nitrogen, and sieving to obtain the temperature-controlled self-foaming expansion plugging agent. The stress-strain curve of the temperature-controlled self-foaming expansion plugging agent is shown in figure 1: the elongation at break reaches 440%, and the tensile strength exceeds 11MPa, which shows that the temperature-controlled self-foaming expansion plugging agent has good mechanical property and toughness.
The plugging agent prepared in example 1 was subjected to a thermal stability test, the material was heated in air to 800 ℃ at a heating rate of 3 ℃/min, and the weight change was observed. The thermal degradation data of the silicone rubber powder plugging agent is shown in figure 2, and the heat-resistant temperature of the silicone rubber powder plugging agent reaches more than 260 ℃.
Example 2
A preparation method of a temperature-control self-foaming expansion plugging agent comprises the following steps:
5g of hydroxyl-terminated polydimethylsiloxane (molecular weight is less than 300g/mol), 3g of tetramethyl m-xylylene diisocyanate, 4g of hexamethylene diisocyanate trimer, 4g of silicon-hydrogen bond-terminated polydimethylsiloxane, 4g of polydimethylsiloxane with a side chain containing a double-bond group with functionality of more than or equal to 2 and 5 drops of dibutyltin dilaurate are uniformly mixed in 30ml of tetrahydrofuran, poured into a polytetrafluoroethylene mold, volatilized at room temperature for 16h, and then cured at 100 ℃ for 24 h. And (3) freezing and crushing the cured silicone rubber elastomer under the assistance of liquid nitrogen, and sieving the crushed silicone rubber elastomer with a 100-mesh sieve to obtain the temperature-controlled self-foaming expansion plugging agent. The optical photo of the temperature-controlled self-foaming expansion plugging agent is shown in figure 3: the temperature-controlled self-foaming expansion plugging agent is white powder particles with the particle size of about 100 mu m.
And (3) testing the foaming self-expansion performance of the plugging agent:
the material obtained in example 2 was cut into cubes having a length, width and height of 1cm, respectively, placed in a reaction vessel containing ionized water, aged at 70 ℃, 100 ℃, 130 ℃, 160 ℃ and 190 ℃ for 12 hours, and the system change was measured, as shown in table 1:
TABLE 1 swell at various temperatures% for example 8
| Serial number | 70 |
100℃ | 130℃ | 160℃ | 190℃ |
| Example 1 | 30 | 170 | 480 | 345 | 305 |
| Example 2 | 53 | 350 | 750 | 550 | 405 |
| Example 3 | 20 | 135 | 394 | 314 | 283 |
| Example 4 | 30 | 170 | 475 | 339 | 300 |
According to the results in table 1, the plugging agent has different foaming effects in aqueous solutions at different temperatures, and the foaming degree of the plugging agent can be changed by changing the temperature or adjusting the dosage of the catalyst, which indicates that the plugging agent is suitable for plugging cracks under various temperature environments, and the foaming degree can be adjusted, so that the plugging agent is suitable for plugging cracks with various sizes.
Example 3
A preparation method of a temperature-control self-foaming expansion plugging agent comprises the following steps:
5g of hydroxyl-terminated polydimethylsiloxane (molecular weight is less than 300g/mol), 3g of tetramethyl m-xylylene diisocyanate, 4g of hexamethylene diisocyanate trimer, 9g of polydimethylsiloxane with a side chain containing a hydrosilyl group with functionality being more than or equal to 2, 9g of double-bond-terminated polydimethylsiloxane and 3 drops of dibutyltin dilaurate are uniformly mixed in 60ml of tetrahydrofuran, poured into a polytetrafluoroethylene mold, volatilized at room temperature for 16h, and then cured at 100 ℃ for 24 h. And (3) freezing and crushing the cured silicone rubber elastomer under the assistance of liquid nitrogen, and sieving to obtain the temperature-controlled self-foaming expansion plugging agent.
Example 4
A preparation method of a temperature-control self-foaming expansion plugging agent comprises the following steps:
5g of hydroxyl-terminated polydimethylsiloxane (molecular weight is less than 300g/mol), 3g of tetramethyl m-xylylene diisocyanate, 4g of hexamethylene diisocyanate trimer, 6g of polydimethylsiloxane with a side chain containing a hydrosilyl group with functionality more than or equal to 2, 6g of polydimethylsiloxane with a side chain containing a double bond group with functionality more than or equal to 2 and 3 drops of dibutyltin dilaurate are uniformly mixed in 40ml of tetrahydrofuran, poured into a polytetrafluoroethylene mold, volatilized for 16h at room temperature, and then cured for 24h at 100 ℃. And (3) freezing and crushing the cured silicone rubber elastomer under the assistance of liquid nitrogen, and sieving to obtain the temperature-controlled self-foaming expansion plugging agent.
The cured silicone rubber material of example 4 was cut with scissors to obtain silicone rubber powder particles.
The particles were heated in an air atmosphere at 180 ℃ for 1 hour, and the morphology change was observed, and the optical photographs before and after heating are shown in fig. 4: the material has the characteristic of self-combination at high temperature, and has better plugging effect when being used for plugging the oil and gas field exploitation cracks.
The particles were heated at 130 ℃ under a pressure of 20MPa for 1 hour, and the morphology change was observed. The optical photographs before and after heating are shown in FIG. 5: the plugging agent has the characteristics of changing shape and size along with the change of pressure, self-adaption and intelligent plugging effect along with the change of the size of the fracture when being used for plugging the fracture in oil and gas field exploitation.
The schematic diagram of the double-network structure of the temperature-controlled self-foaming expansion plugging agent prepared in examples 1-4 is shown in fig. 6.
Example 5
A preparation method of a high-temperature-resistant self-foaming expansion silicone rubber plugging material comprises the following steps:
0.5 percent of polyacrylamide-polybutyl acrylate and 15 percent of the temperature control self-foaming expansion plugging agent with the diameter of 0.5mm prepared in the example 1, 200g of saturated potassium formate solution, 0.5 percent of zinc perchlorate, 2 percent of superfine calcium carbonate particles and 5 percent of multi-arm carbon nano tubes are mixed in 80ml of deionized water, the ultrasonic treatment is carried out for 10min, and the stirring is carried out for 1 hour, thus obtaining the high temperature resistant self-foaming expansion silicon rubber plugging material.
The rheological property of the high-temperature resistant self-foaming expansion silicone rubber plugging material is measured as follows:
placing the high-temperature-resistant self-foaming expansion silicone rubber plugging material in a reaction kettle, aging for 16 hours at 200 ℃, then testing the apparent viscosity and the moulding viscosity by using a six-turn viscometer and calculating the dynamic shear force ratio, wherein the specific results are shown in table 2:
table 2 example 5 rheology Change before and after aging at different temperatures
| 2 |
200℃ | |
| θ 300 | 19 | 20 |
| θ 600 | 32 | 29 |
| AV | 16 | 14.5 |
| PV | 13 | 11 |
| YP | 3 | 3.5 |
According to the results in Table 2, the dynamic shear ratio of the plugging material before and after aging is 1.17, which shows that the change of rheological property of the plugging material before and after aging is very small, and the plugging material can stably work for a long time at 200 ℃.
Example 6
A preparation method of a high-temperature-resistant self-foaming expansion silicone rubber plugging material comprises the following steps:
0.1 percent of mixture of scleroglucan and sodium styrene sulfonate, 5 percent of temperature control self-foaming expansion plugging agent with the diameter of 0.1mm prepared in example 2, 80 percent of saturated zinc bromide solution, 0.5 percent of zinc perchlorate, 1 percent of heavy calcium carbonate particles and 3 percent of single-arm carbon nano tubes are mixed in 80ml of deionized water, and the mixture is subjected to ultrasonic treatment for 10min and stirred for 1 hour to obtain the high temperature resistant self-foaming expansion silicon rubber plugging material.
Example 7
A preparation method of a high-temperature-resistant self-foaming expansion silicone rubber plugging material comprises the following steps:
1% of polyacrylamide-polybutyl acrylate, 20% of silicone rubber particles, 70g of saturated potassium formate solution, 1% of zinc perchlorate, 3% of ultrafine calcium carbonate particles and 8% of multi-arm carbon nanotubes, which are prepared in example 3 and have the diameter of 5mm, are mixed in 80ml of deionized water, and the mixture is subjected to ultrasonic treatment for 10min and stirring for 1 hour to obtain the high-temperature-resistant self-foaming expanded silicone rubber plugging material.
Example 8
A preparation method of a high-temperature-resistant self-foaming expansion silicone rubber plugging material comprises the following steps:
1% of a mixture of scleroglucan and sodium styrene sulfonate, and the temperature-control self-foaming expansion plugging agent with the diameter of 10mm prepared in example 4 is 25% of silicone rubber particles, 90g of a mixed solution of a saturated potassium formate solution and a saturated zinc bromide solution, 0.8% of zinc perchlorate, 5% of heavy calcium carbonate particles, and 12% of a mixture of single-arm carbon nanotubes and multi-arm carbon nanotubes are mixed in 80ml of deionized water, and the mixture is subjected to ultrasonic treatment for 10min and stirred for 1 hour to obtain the high-temperature-resistant self-foaming expansion silicone rubber plugging material.
While only the preferred embodiments of the present invention have been described, it should be understood that various modifications and adaptations thereof may occur to one skilled in the art without departing from the spirit of the present invention and should be considered as within the scope of the present invention.
Claims (5)
1. A high-temperature resistant self-foaming expansion silicone rubber plugging material comprises:
0.1-1% of flow pattern regulator;
5-30% of temperature control self-foaming expansion plugging agent;
1-5% of rigid particles;
3-15% of carbon nano tube;
0.5-1% of temperature activator;
40-60% of density regulator; and
the balance of deionized water;
wherein:
the flow pattern regulator is selected from any one of polyacrylamide-polybutyl acrylate, scleroglucan and sodium styrene sulfonate mixture;
the temperature-control self-foaming expansion plugging agent is silicon rubber particles, the particle size of the silicon rubber particles is 100 mu m-10 mm, and the activation temperature is more than or equal to 70 ℃;
the rigid particles are selected from heavy calcium carbonate or superfine calcium carbonate;
the temperature activator is zinc perchlorate;
the density regulator is selected from any one of saturated potassium formate solution, saturated zinc bromide solution, and mixed solution of saturated potassium formate solution and saturated zinc bromide solution;
the temperature-controlled self-foaming expansion plugging agent is prepared by the following method:
uniformly mixing hydroxyl-terminated polydimethylsiloxane, tetramethyl m-xylylene diisocyanate, hexamethylene diisocyanate trimer, silicon-hydrogen bond-terminated polydimethylsiloxane, double bond-terminated polydimethylsiloxane and dibutyltin dilaurate in tetrahydrofuran, pouring into a mold, volatilizing at room temperature, curing, freezing and crushing the cured material under liquid nitrogen, and sieving to obtain the temperature-controlled self-foaming expansion plugging agent.
2. The high temperature resistant self-foaming expanded silicone rubber lost circulation material of claim 1, comprising:
flow pattern regulator 0.5%;
15% of temperature control self-foaming expansion plugging agent;
2% of rigid particles;
10% of carbon nano tube;
0.7% of temperature activator;
50% of density regulator; and
the balance being deionized water.
3. A method for preparing the high temperature resistant self-foaming expansion silicone rubber plugging material of claim 1 or 2, comprising:
uniformly mixing a flow pattern regulator, a temperature control self-foaming expansion plugging agent, rigid particles, carbon nano tubes, a temperature activator and a density regulator in deionized water.
4. The production method according to claim 3, wherein:
the carbon nano tube is selected from any one of single-arm carbon nano tube, multi-arm carbon nano tube and a mixture of the single-arm carbon nano tube and the multi-arm carbon nano tube.
5. The high-temperature-resistant self-foaming expansion silicone rubber plugging material prepared by the preparation method according to claim 3 or 4.
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