CN118206688A - Temperature-sensitive type low-density well cementation cement slurry suspending agent, cement slurry and preparation method - Google Patents
Temperature-sensitive type low-density well cementation cement slurry suspending agent, cement slurry and preparation method Download PDFInfo
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- 239000004568 cement Substances 0.000 title claims abstract description 117
- 239000000375 suspending agent Substances 0.000 title claims abstract description 75
- 239000002002 slurry Substances 0.000 title claims abstract description 73
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 238000007613 slurry method Methods 0.000 title description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 37
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims abstract description 26
- JWYVGKFDLWWQJX-UHFFFAOYSA-N 1-ethenylazepan-2-one Chemical compound C=CN1CCCCCC1=O JWYVGKFDLWWQJX-UHFFFAOYSA-N 0.000 claims abstract description 19
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- XHZPRMZZQOIPDS-UHFFFAOYSA-N 2-Methyl-2-[(1-oxo-2-propenyl)amino]-1-propanesulfonic acid Chemical compound OS(=O)(=O)CC(C)(C)NC(=O)C=C XHZPRMZZQOIPDS-UHFFFAOYSA-N 0.000 claims abstract description 16
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000000725 suspension Substances 0.000 claims abstract description 16
- 229920000536 2-Acrylamido-2-methylpropane sulfonic acid Polymers 0.000 claims abstract description 14
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims abstract description 13
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 51
- 239000000243 solution Substances 0.000 claims description 51
- 238000003756 stirring Methods 0.000 claims description 38
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 24
- 239000003795 chemical substances by application Substances 0.000 claims description 20
- 239000011324 bead Substances 0.000 claims description 19
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- 239000007864 aqueous solution Substances 0.000 claims description 17
- 229920000642 polymer Polymers 0.000 claims description 16
- 239000012779 reinforcing material Substances 0.000 claims description 16
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- 229910052710 silicon Inorganic materials 0.000 claims description 15
- 239000010703 silicon Substances 0.000 claims description 15
- 238000005303 weighing Methods 0.000 claims description 15
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- 229910052757 nitrogen Inorganic materials 0.000 claims description 12
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- 150000001408 amides Chemical class 0.000 claims description 8
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 8
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- 238000005259 measurement Methods 0.000 description 5
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- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 description 2
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- DZSVIVLGBJKQAP-UHFFFAOYSA-N 1-(2-methyl-5-propan-2-ylcyclohex-2-en-1-yl)propan-1-one Chemical compound CCC(=O)C1CC(C(C)C)CC=C1C DZSVIVLGBJKQAP-UHFFFAOYSA-N 0.000 description 1
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- Curing Cements, Concrete, And Artificial Stone (AREA)
Abstract
The invention discloses a temperature-sensitive low-density well cementation cement slurry suspending agent, cement slurry and a preparation method thereof, wherein the suspending agent comprises the following components: 3 to 8 parts of N-vinyl caprolactam, 7 to 12 parts of acrylamide, 20 to 25 parts of 2-acrylamido-2-methylpropanesulfonic acid, 0.2 to 1.0 part of methyl methacrylate and 0.3 to 0.45 part of ammonium persulfate. The temperature-sensitive low-density well cementation cement slurry suspending agent can keep the viscosity unchanged basically within the temperature range of 40-160 ℃, can effectively avoid the problem of serious suspension instability of low-density cement slurry caused by self thermal motion aggravation during temperature change, prevents the problem of poor interval sealing caused by serious water separation, and reduces the floating of materials and the sinking of heavy materials in the low-density cement slurry.
Description
Technical Field
The invention belongs to the technical field of cementing slurry additives, and particularly relates to a temperature-sensitive low-density cementing slurry suspending agent, a temperature-sensitive low-density cementing slurry and a preparation method thereof.
Background
The development of oil and gas resource exploration and development provides new requirements for well cementation quality and well cementation safety, and the problems of suspension instability, serious sedimentation, low-temperature thickening, high-temperature dilution and serious water loss of well cementation cement paste are frequently encountered in the well cementation process. When the method relates to the well cementation of a deep well and an ultra-deep well, the well cementation process faces a great challenge due to the characteristics of overlong primary sealing section, complex geology, easy leakage and the like. In the well cementation of a long sealing section, due to the existence of a ground temperature gradient, a great temperature difference exists between the top of a cement slurry column in an annulus and the bottom of the well, and the high temperature of the bottom of the well easily causes the cement slurry to be diluted and the suspension instability to occur; meanwhile, in order to balance the formation pressure and prevent leakage, a low-density cement slurry system is often used for well cementation, and the suspension instability phenomenon of the low-density cement slurry system is more serious because the water-solid ratio is larger than that of the conventional density system, and the density difference between external admixtures such as materials and cement is reduced. The polymer suspending agent currently used is not suitable for the well cementation environment under the condition of large temperature difference or is not suitable for a floating bead low-density well cementation cement slurry system. Therefore, the low-density cement paste well cementation under the condition of large temperature difference still faces a great challenge, the suspension instability seriously affects the well cementation quality and the well cementation safety, and a suspending agent is urgently needed to be researched so as to solve the problem of suspension instability of a floating bead low-density well cementation cement paste system when the large temperature difference (40-160 ℃) exists.
Disclosure of Invention
Aiming at the problems, the invention discloses a temperature-sensitive low-density well cementation cement slurry suspending agent, which comprises the following components: 3 to 8 parts of N-vinyl caprolactam, 7 to 12 parts of acrylamide, 20 to 25 parts of 2-acrylamido-2-methylpropanesulfonic acid, 0.2 to 1.0 part of methyl methacrylate and 0.3 to 0.45 part of ammonium persulfate.
Still further, a 1wt% aqueous solution of the suspending agent has an apparent viscosity at 25 ℃ of greater than 280 mpa.s at a shear rate of 170s -1.
Further, the mass of the ammonium persulfate accounts for 0.8-1.2% of the total mass of the reaction monomers;
wherein the reaction monomers comprise N-vinyl caprolactam, acrylamide, 2-acrylamido-2-methylpropanesulfonic acid and methyl methacrylate.
The preparation method of the temperature-sensitive low-density well cementation cement slurry suspending agent comprises the following steps:
preparing a 20% sodium hydroxide aqueous solution, and placing the solution in an ice water bath for standby;
Firstly, weighing 7-12 parts of acrylamide and 20-25 parts of 2-acrylamido-2-methylpropanesulfonic acid, adding into 150-230 parts of deionized water, stirring a glass rod until the mixture is completely dissolved, regulating the pH to 7-8 by using a prefabricated 20% sodium hydroxide solution, continuously adding 3-8 parts of N-vinyl caprolactam and 0.2-1 part of methyl methacrylate, uniformly stirring, transferring the mixture aqueous solution to a three-neck flask, introducing nitrogen for 30min under the ice water bath condition, and placing the mixture aqueous solution with the introduced nitrogen into a constant-temperature oil bath pot at 50-70 ℃;
Weighing 0.3-0.45 part of ammonium persulfate to prepare an initiator solution, adding the initiator solution when the temperature of the mixture water solution is increased to 50-70 ℃, and starting stirring reaction for 15-20 hours under the constant temperature condition to obtain a suspending agent solution;
Drying, grinding and sieving the suspending agent solution to obtain the suspending agent product.
Further, the specific conditions of the drying are as follows:
Baking at 50-70 deg.C for 24 hr.
A temperature-sensitive low density well cementing slurry comprising: 45 to 60 parts of oil well grade G cement, 25 to 35 parts of floating beads, 12 to 17 parts of reinforcing materials, 1.5 to 3.2 parts of micro silicon, 2.0 to 3.6 parts of fly ash, 2.0 to 3.0 parts of fluid loss additive, 0.23 to 0.60 part of retarder, 0.1 to 0.3 part of defoamer, 80 to 95 parts of water and 0.5 to 1.0 part of suspending agent.
Further, the density of the cement paste is 1.30-1.40 g/cm 3.
Furthermore, the fluid loss agent and retarder are amide organic high molecular polymers.
The preparation method of the temperature-sensitive low-density well cementation cement paste comprises the following steps:
Weighing 45-60 parts of oil well grade G cement, 25-35 parts of floating beads, 12-17 parts of reinforcing materials, 1.5-3.2 parts of micro silicon, 2.0-3.6 parts of fly ash, 2.0-3.0 parts of fluid loss agent, 0.23-0.60 part of retarder and 0.5-1.0 part of suspending agent, and uniformly stirring the raw materials in a container until no obvious color lump exists;
then weighing 80-95 parts of water, pouring the uniformly stirred raw materials into the water while stirring for 15-20 seconds, uniformly stirring, and adding 0.1-0.3 part of defoaming agent in the stirring process.
Further, the specific operation of stirring is as follows:
Stirring at a first speed for 15s and then at a second speed for 45s;
wherein the second speed is greater than the first speed.
Compared with the prior art, the invention has the beneficial effects that:
1) The temperature-sensitive low-density well cementation cement slurry suspending agent can keep the viscosity unchanged basically within the temperature range of 40-160 ℃, can effectively avoid the problem of serious suspension instability of low-density cement slurry caused by the aggravation of self thermal motion during temperature change, prevents the problems of floating of materials and sinking of heavy materials in the low-density cement slurry, and prevents poor interval sealing caused by serious water separation;
2) The temperature-difference-resistant high-polymer suspending agent can effectively slow down the phenomenon that the viscosity of the high-polymer suspending agent becomes alkene due to temperature rise, has wider temperature-difference-resistant range, can be used for one-time well cementation of a longer sealing section, and saves the well cementation cost.
Additional features and advantages of the invention will be set forth in the description which follows, and in part will be obvious from the description, or may be learned by practice of the invention. The objectives and other advantages of the invention may be realized and attained by the structure particularly pointed out in the written description and claims hereof as well as the appended drawings.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions of the prior art, the following description will briefly explain the drawings used in the embodiments or the description of the prior art, and it is obvious that the drawings in the following description are some embodiments of the present invention, and other drawings can be obtained according to these drawings without inventive effort for a person skilled in the art.
Fig. 1 shows a technical scheme of a suspending agent according to an embodiment of the present invention.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention, and it is apparent that the described embodiments are some embodiments of the present invention, but not all embodiments of the present invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The invention provides a temperature-sensitive low-density well cementation cement slurry suspending agent, which comprises the following components: 3 to 8 parts of N-vinyl caprolactam, 7 to 12 parts of acrylamide, 20 to 25 parts of 2-acrylamido-2-methylpropanesulfonic acid, 0.2 to 1.0 part of methyl methacrylate and 0.3 to 0.45 part of ammonium persulfate.
The quaternary amide hydrophobic association temperature response type suspending agent is polymerized by an aqueous solution free radical polymerization method at a certain temperature, the apparent viscosity of a 1wt% aqueous solution thereof at 25 ℃ is more than about 280 mPa.s under the shearing rate of 170s -1, and the critical phase transition temperature reaches 70 ℃.
In some embodiments, the mass of ammonium persulfate is from 0.8 to 1.2% of the total mass of the reaction monomers; preferably, the mass of ammonium persulfate accounts for 1% of the total mass of the reaction monomers.
Wherein the reaction monomers comprise N-vinyl caprolactam, acrylamide, 2-acrylamido-2-methylpropanesulfonic acid and methyl methacrylate.
The temperature response type suspending agent takes a C-C long chain with strong temperature resistance as a main chain, and contains a rigid Wen Minji group with strong water repellency, a hydrophilic group (acrylamide and 2-acrylamide-2-methylpropanesulfonic acid) and a hydrophobic group. The introduction of the hydrophobic monomer methyl methacrylate enables the suspending agent to form a stable space grid structure, the viscosity of the suspending agent does not drop sharply along with the temperature rise within a certain temperature range (40-160 ℃), and the suspension stability of the low-density well cementation cement slurry is ensured. Meanwhile, the introduction of the hydrophobic monomer methyl methacrylate can adjust the flexibility of a macromolecular chain segment, so that the viscosity is kept in a proper range while the molecular weight is ensured, and cement slurry is not thickened in the slurry mixing process, so that the grouting is difficult. In addition, the critical phase transition temperature of the suspending agent can reach 70 ℃ by adjusting the proportion of the hydrophilic monomer and the hydrophobic monomer, and Wen Minji groups in the suspending agent can adjust the viscosity change by changing the flexibility of the molecular chain of the suspending agent after the temperature exceeds 70 ℃, so that the suspension stability of the low-density well cementation cement paste under the medium-high temperature condition can be ensured.
Suspending agents are linear macromolecules, the technical route of which is shown in figure 1. The invention also discloses a preparation method of the temperature-sensitive low-density well cementation cement slurry suspending agent, which comprises the following steps:
preparing a 20% sodium hydroxide aqueous solution, and placing the solution in an ice water bath for standby;
Firstly, weighing 7-12 parts of acrylamide and 20-25 parts of 2-acrylamido-2-methylpropanesulfonic acid, adding into 150-230 parts of deionized water, stirring a glass rod until the mixture is completely dissolved, regulating the pH to 7-8 by using a prefabricated 20% sodium hydroxide solution, continuously adding 3-8 parts of N-vinylcaprolactam and 0.2-1 part of methyl methacrylate, uniformly stirring, transferring the mixture aqueous solution to a three-neck flask, sequentially connecting a temperature recorder, a stirring rod and an N 2 channel, introducing nitrogen for 30min under the ice water bath condition, and placing the mixture aqueous solution with introduced nitrogen into a constant-temperature oil bath pot at 50-70 ℃;
Weighing 0.3-0.45 part of ammonium persulfate to prepare an initiator solution, adding the prepared initiator solution when the temperature of the aqueous solution of the mixture is increased to 50-70 ℃, and starting stirring reaction for 15-20 h under the constant temperature condition to obtain a suspending agent solution; preferably, the mass concentration of the initiator solution is 2%;
drying, grinding and sieving the suspending agent solution to obtain the suspending agent product. Illustratively, the screen is a 60 mesh standard screen.
The specific conditions for drying are as follows: baking at 50-70 deg.C for 24 hr.
Preferably, the drying is carried out at 60℃for 24 hours.
The dropping sequence of the temperature-sensitive monomer N-vinyl caprolactam is added after the pH is regulated, so as to prevent the micro-phase transformation from being generated in advance due to the temperature rise in the pH regulating process and influence the generation of free radical reaction.
The initiation temperature of the polymerization reaction needs to reach 50-70 ℃, the reaction is stable in the temperature range, the parallel repeatability is good, and different polymerization products can be generated at different initiation temperatures.
The invention also discloses a temperature-sensitive low-density well cementation cement paste, which comprises the following components: 45 to 60 parts of oil well grade G cement, 25 to 35 parts of floating beads, 12 to 17 parts of reinforcing materials, 1.5 to 3.2 parts of micro silicon, 2.0 to 3.6 parts of fly ash, 2.0 to 3.0 parts of fluid loss additive, 0.23 to 0.60 part of retarder, 0.1 to 0.3 part of defoamer, 80 to 95 parts of water and 0.5 to 1.0 part of suspending agent. The cement is oil well G-grade Jiahua cement.
In some embodiments, the density of the floating beads is 0.50 to 0.70g/cm 3 and the particle size is 80 to 100 mesh. The reinforcing material is superfine cement.
In some embodiments, the cement paste has a density of 1.30 to 1.40g/cm 3, preferably a density of 1.35g/cm 3. The cement slurry is prepared into low-density well cementation cement slurry according to the water-solid ratio of 0.7-1.0.
In some embodiments, the fluid loss agent and the retarder are amide organic high molecular polymers, the defoamer is mineral oil defoamer or polyether defoamer, and the fluid loss agent and the retarder have good compatibility with the suspending agent and no incompatibility.
The invention also discloses a preparation method of the temperature-sensitive low-density well cementation cement paste, which comprises the following steps:
Weighing 45-60 parts of oil well grade G cement, 25-35 parts of floating beads, 12-17 parts of reinforcing materials, 1.5-3.2 parts of micro silicon, 2.0-3.6 parts of fly ash, 2.0-3.0 parts of fluid loss agent, 0.23-0.60 part of retarder and 0.5-1.0 part of suspending agent, and uniformly stirring the raw materials in a container until no obvious color lump exists;
Then weighing 80-95 parts of water, pouring the uniformly stirred raw materials into the water while stirring for 15-20 seconds, uniformly stirring, and adding 0.1-0.3 part of defoaming agent in the stirring process.
In some embodiments, the specific operation of stirring is:
Stirring at a first speed for 15s and then at a second speed for 45s;
Wherein the second speed is greater than the first speed. Preferably, the first rotational speed is 4000r/s and the second rotational speed is 12000r/s.
Example 1
The embodiment discloses a temperature-sensitive low-density well cementation cement slurry suspending agent, wherein the critical phase transition temperature is 70 ℃. The suspending agent comprises 3 parts of N-vinylcaprolactam (NVCL), 7 parts of Acrylamide (AM), 20 parts of 2-acrylamido-2-methylpropanesulfonic Acid (AMPS), 0.2 part of Methyl Methacrylate (MMA), 0.3 part of ammonium persulfate ((NH 4)2S2O8) and 151 parts of water.
According to the temperature-sensitive low-density well cementation cement slurry suspending agent provided by the invention, the microphase transition temperature is 70 ℃, the temperature-responsive polymer is a polymer which undergoes liquid-liquid phase separation from a homogeneous phase solution to a concentrated polymer solution and a diluted polymer solution in response to temperature change, the microphase separation is carried out between the concentrated polymer solution and the diluted polymer solution along with the temperature, the phase transition behavior of the polymer solution is called as the phase transition behavior of the polymer solution when the phase transition occurs. When the temperature of the temperature-responsive hydrophobic association suspending agent reaches 70 ℃, the absorbance of the suspending agent begins to drop sharply, microphase separation is carried out on the suspending agent solution, the solution is changed from a transparent state to a turbid opaque state, at the moment, hydrophobic association is carried out, the hydrophobic capacity of hydrophobic groups in the suspending agent is enhanced, the apparent viscosity of the suspending agent is obviously increased, the water separation amount in cement paste at high temperature is better controlled, and the good suspension stability of low-density cement paste is ensured.
According to the suspending agent, a C-C chain with strong temperature resistance is used as a main chain of a polymer molecule, meanwhile, a strong hydrophilic monomer AM is introduced to provide a hydrophilic side group to improve the hydrophilicity of the polymer molecule, the compatibility with a cement slurry system is improved, AMPS and MMA are introduced to further improve the temperature difference resistance of the suspending agent, a temperature sensitive monomer NVCL is introduced to provide a rigid Wen Minji group, the macromolecular chain generates intermolecular and intramolecular hydrophobic association along with the temperature rise, the viscosity of the system is greatly increased, the large temperature difference resistance of the suspending agent is effectively improved, and the suspension stability of the low-density large temperature difference well cementation cement slurry is enhanced.
The temperature change resistance of the suspending agent according to the embodiment can reach 40-160 ℃.
Example 2
In example 2, a temperature-sensitive low density cement slurry is provided. The cement slurry comprises the suspending agent, the oil well cement and various well cementation cement slurry materials in the embodiment 1, wherein the adding amount of the suspending agent is 0.8 part, and the water-solid ratio is 0.8.
In example 2, various well cementing slurry materials include: 55 parts of grade G oil well cement, 35 parts of floating beads, 15 parts of reinforcing materials, 3 parts of micro-silicon, 3 parts of fly ash, 2.2 parts of fluid loss agent G31S, 0.36 part of retarder GH-I, 0.2 part of defoamer XP-3 and 91 parts of water.
In the embodiment 2 of the invention, the fly ash and the floating beads are lightening materials, and are key materials for ensuring the density of the well cementation cement slurry to be 1.35g/cm 3.
In example 2 of the present invention, the main component of micro-silicon (90% or more) is silica, which is capable of filling the pores between cement particles. The performances of compression resistance, fracture resistance, impermeability and the like can be obviously improved; meanwhile, the water-retaining agent has the functions of water retention, segregation prevention and the like.
In example 2 of the present invention, the reinforcing material may be an oil well cement reinforcing agent provided by the Toyo oil field engineering Co., ltd.
In example 2 of the present invention, the fluid loss agent code is G31S, and the retarder code is GH-I, which is an amide organic polymer available from Wei Hui chemical industry Co. The defoamer with the code XP-3 can be polyether defoamer provided by Wei Hui chemical industry Co.
The cement paste prepared in example 2 was measured, and the measurement results are shown in table 1 below.
Table 1 determination results of cement slurries
Example 3
In the embodiment 3 of the invention, a preparation method of a temperature-sensitive low-density well cementation cement slurry suspending agent is provided, and comprises the following steps:
(1) Weighing 20 parts of sodium hydroxide, preparing a sodium hydroxide aqueous solution with the mass concentration of 20%, and placing the aqueous solution in an ice water bath for later use;
In particular, sodium hydroxide is required to be placed in an ice-water bath because it gives a lot of heat when it encounters water.
(2) 12 Parts of acrylamide and 25 parts of 2-acrylamido-2-methylpropanesulfonic acid are weighed into 230 parts of deionized water, completely dissolved by stirring with a glass rod and pH adjusted with a preformed 20% sodium hydroxide solution.
Specifically, the pH is regulated to 7-8, and when the pH in the solution is slightly alkaline, the-COO-in the molecule is in an ionic state, and the electrostatic effect of the ions is relatively strong.
(3) 8 Parts of N-vinylcaprolactam and 1 part of methyl methacrylate were added, and after stirring uniformly, the aqueous mixture was transferred to a three-necked flask.
Specifically, the addition of sodium hydroxide solution releases heat, so that the local temperature of the solution instantaneously reaches the phase transition temperature of the temperature-sensitive monomer N-vinyl caprolactam, and the monomer undergoes self-polymerization reaction, so that the N-vinyl caprolactam needs to be added after the pH is adjusted.
(4) The temperature recorder, the stirring rod and the N 2 channel are connected in sequence, nitrogen is introduced for 30min under the ice water bath condition, and the water solution with the introduced nitrogen is placed in a constant temperature oil bath pot at 65 ℃.
The inert gas nitrogen is introduced under the ice bath, so that the precondition is provided for preventing the residual oxygen in the system from generating side reactions such as self-polymerization reaction and the like in the nitrogen introducing process.
(5) 0.45 Part of ammonium persulfate is weighed to prepare an initiator solution with the mass concentration of 2%. When the temperature of the solution is raised to 65 ℃, adding the prepared initiator, and starting stirring reaction for 18 hours under the constant temperature condition to obtain the suspending agent solution.
Specifically, the initiator is added when the temperature is increased to 65 ℃, because a large amount of heat is released from the free radical polymerization reaction after the initiator is added, and the aqueous solution is volatilized in a large amount due to the excessively high temperature; when the temperature is too low, the temperature generated by the active free radicals of the initiator cannot be reached, so that the reaction cannot be initiated.
(6) Drying, grinding and sieving the suspending agent solution to obtain the suspending agent product. Baking at 60deg.C for 24 hr.
Example 4
In example 4 of the present invention, a temperature-sensitive low density cement slurry is provided. The cement slurry comprises the temperature-sensitive low-density well cementation cement slurry suspending agent, oil well cement and various well cementation cement slurry materials in the embodiment 3, wherein the adding amount of the suspending agent is 0.8 part, and the water-solid ratio is 0.8.
In example 4 of the present invention, various well cementing slurry materials include: 55 parts of grade G well cementation cement, 35 parts of floating beads, 15 parts of reinforcing materials, 3 parts of micro-silicon, 3 parts of fly ash, 2.2 parts of fluid loss agent G31S, 0.36 part of retarder GH-I, 0.2 part of defoamer XP-3 and 91 parts of water.
In the embodiment 4 of the invention, the fly ash and the floating beads are lightening materials, and are key materials for ensuring the density of the well cementation cement slurry to be 1.35g/cm 3.
In example 4 of the present invention, the main component of micro-silicon (90% or more) is silica, which is capable of filling the pores between cement particles. The performances of compression resistance, fracture resistance, impermeability and the like can be obviously improved; meanwhile, the water-retaining agent has the functions of water retention, segregation prevention and the like.
In example 4 of the present invention, the reinforcing material may be an oil well cement reinforcing agent provided by the Toyo oil field engineering Co., ltd.
In example 4 of the present invention, the fluid loss agent has a code number of G31S, the retarder has a code number of GH-I, and the fluid loss agent can be an amide organic polymer provided by Wei Hui chemical industry Co. The defoamer with the code XP-3 can be polyether defoamer provided by Wei Hui chemical industry Co.
The cement paste prepared in example 4 was measured, and the measurement results are shown in Table 2 below.
Table 2 determination results of cement slurries
Example 5
In embodiment 5 of the present invention, there is provided a method for preparing a low density cement slurry for well cementation, the method comprising the steps of:
(1) Weighing 45 parts of oil well grade G cement, 35 parts of floating beads, 17 parts of reinforcing materials, 3.2 parts of micro-silicon, 3.6 parts of fly ash, 2.8 parts of fluid loss agent, 0.30 part of retarder and 1.0 part of temperature-sensitive low-density well cementation cement slurry suspending agent in the embodiment 3;
(2) Uniformly stirring the raw materials in a container until no obvious color lump exists;
(3) Then weighing 95 parts of water, pouring the uniformly stirred raw materials into the water while stirring for 15 seconds, firstly stirring for 15 seconds at a low speed, then stirring for 45 seconds at a high speed, and adding 0.2 part of defoamer in the process.
Specifically, the low speed is 4000r/s and the high speed is 12000r/s, and the floating of the light material is to be noted.
Comparative example 1
In comparative example 1 of the present invention, a temperature-sensitive low density cement slurry suspension is provided, which is synthesized by the following steps:
(1) Firstly, pre-preparing 20mL of 20% sodium hydroxide (NaOH) solution for later use;
(2) 12 parts of acrylamide, 8 parts of N-vinyl caprolactam and 17 parts of 2-acrylamido-2-methylpropanesulfonic acid are weighed and added into 185 parts of deionized water, the deionized water is stirred by a glass rod to be completely dissolved, and a prepared 20% sodium hydroxide solution is used for regulating the pH value to be 7-8;
(3) Then pouring the solution into a three-neck round bottom flask after fully stirring, introducing nitrogen for 0.5h under ice bath condition, putting the three-neck flask into an oil bath pot with the temperature of 70 ℃ for heating, and adding 0.37 part of potassium persulfate as an initiator when the temperature in the flask reaches 70 ℃;
(4) Reacting for 20h to obtain a viscous liquid, washing the obtained solution product with ethanol, drying at 60 ℃, and crushing to obtain a white suspending agent.
Comparative example 2
In comparative example 2 of the present invention, a temperature-sensitive low density cement slurry is provided. The cement slurry comprises the suspending agent, oil well cement and various well cementation cement slurry materials described in the comparative example 1, wherein the adding amount of the suspending agent is 0.8 part, and the water-solid ratio is 0.8.
In comparative example 2 of the present invention, various well cementing slurry materials include: 55 parts of grade G oil well cement, 35 parts of floating beads, 15 parts of reinforcing materials, 3 parts of micro-silicon, 3 parts of fly ash, 2.2 parts of fluid loss agent G31S, 0.36 part of retarder GH-I, 0.2 part of defoamer XP-3 and 91 parts of water.
In the comparative example 2 of the present invention, fly ash and floating beads are lightening materials, and are key materials for ensuring the density of the well cementation cement slurry to be 1.35g/cm 3.
In comparative example 2 of the present invention, the main component of micro-silicon (90% or more) is silica, which is capable of filling the pores between cement particles. The performances of compression resistance, fracture resistance, impermeability and the like can be obviously improved; meanwhile, the water-retaining agent has the functions of water retention, segregation prevention and the like.
In comparative example 2 of the present invention, the reinforcing material may be an oil well cement reinforcing agent provided by the Toyang oil field engineering Co., ltd.
In comparative example 2 of the present invention, the fluid loss agent has a code number of G31S, the retarder has a code number of GH-I, and the amide organic polymer can be supplied by Wei Hui chemical industry Co., ltd. The defoamer with the code XP-3 can be polyether defoamer provided by Wei Hui chemical industry Co.
The cement paste prepared in comparative example 2 was measured, and the measurement results are shown in table 3 below.
Table 3 determination results of cement slurries
Comparative example 3
In comparative example 3 of the present invention, a temperature-sensitive low density cement slurry suspension is provided, which is synthesized by the following steps:
(1) Firstly, pre-preparing 20mL of 20% sodium hydroxide (NaOH) solution for later use;
(2) 12 parts of acrylamide, 8 parts of N-vinyl caprolactam and 25 parts of 2-acrylamido-2-methylpropanesulfonic acid are weighed and added into 225 parts of deionized water, the deionized water is stirred by a glass rod to be completely dissolved, and a prepared 20% sodium hydroxide solution is used for regulating the pH value to be 7-8;
(3) Then pouring the solution into a three-neck round bottom flask after fully stirring, introducing nitrogen for 0.5h under ice bath condition, putting the three-neck flask into an oil bath pot with the temperature of 70 ℃ for heating, and adding 0.45 part of potassium persulfate as an initiator when the temperature in the flask reaches 70 ℃;
(4) Reacting for 20h to obtain a viscous liquid, washing the obtained solution product with ethanol, drying at 60 ℃, and crushing to obtain a white suspending agent.
Comparative example 4
In comparative example 4 of the present invention, a temperature-sensitive low density cement slurry is provided. The cement slurry comprises the temperature-sensitive low-density well cementation cement slurry suspending agent, oil well cement and various well cementation cement slurry materials in comparative example 3, wherein the adding amount of the suspending agent is 0.8 part, and the water-solid ratio is 0.8.
In comparative example 4 of the present invention, various well cementing slurry materials included: 55 parts of grade G oil well cement, 35 parts of floating beads, 15 parts of reinforcing materials, 3 parts of micro-silicon, 3 parts of fly ash, 2.2 parts of fluid loss agent G31S, 0.36 part of retarder GH-I, 0.2 part of defoamer XP-3 and 91 parts of water.
In comparative example 4 of the present invention, fly ash and floating beads are lightening materials, which are key materials for ensuring the density of the well cementation cement slurry to be 1.35g/cm 3.
In comparative example 4 of the present invention, the main component of micro silicon (90% or more) is silica, which is capable of filling the pores between cement particles. The performances of compression resistance, fracture resistance, impermeability and the like can be obviously improved; meanwhile, the water-retaining agent has the functions of water retention, segregation prevention and the like.
In comparative example 4 of the present invention, the reinforcing material may be an oil well cement reinforcing agent provided by the Toyang oil field engineering Co., ltd.
In comparative example 4 of the present invention, the fluid loss agent code is G31S, the retarder code is GH-I, and the amide organic high polymer can be supplied by Wei Hui City chemical Co. The defoamer with the code XP-3 can be polyether defoamer provided by Wei Hui chemical industry Co.
The cement paste prepared in comparative example 4 was measured, and the measurement results are shown in table 4 below.
Table 4 determination results of cement slurries
As shown by the measurement results in tables 1,2, 3 and 4, compared with the comparative example, the temperature-sensitive type low-density well cementation cement slurry suspending agent in the embodiment can effectively improve the suspension stability of floating bead low-density well cementation cement slurry within the temperature difference range of 40-160 ℃, so that the water loss of the cement slurry can be controlled while the sectional density difference of the cement stone column is smaller than 0.02g/cm 3; tables 3 and 4 show that, by simply increasing the amount of monomer 2-acrylamido-2-methylpropanesulfonic Acid (AMPS), the temperature resistance of the suspending agent cannot be effectively improved, the cement paste is thickened at low temperature, and compared with the exemplary embodiment, the temperature resistance of the temperature-sensitive type low-density well cementation cement paste suspending agent can be improved by adding the fourth monomer Methyl Methacrylate (MMA), the temperature difference range applicable to the low-density well cementation cement paste is wider, and the consistency of the low-density well cementation cement paste is not influenced while the temperature resistance is ensured.
Although the invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit and scope of the technical solutions of the embodiments of the present invention.
Claims (10)
1. The temperature-sensitive low-density well cementation cement slurry suspending agent is characterized by comprising the following components: 3 to 8 parts of N-vinyl caprolactam, 7 to 12 parts of acrylamide, 20 to 25 parts of 2-acrylamido-2-methylpropanesulfonic acid, 0.2 to 1.0 part of methyl methacrylate and 0.3 to 0.45 part of ammonium persulfate.
2. The temperature-sensitive low density cement slurry suspension of claim 1, wherein the apparent viscosity of a 1wt% aqueous solution of the suspension is greater than 280 mPa-s at a shear rate of 170s -1 at 25 ℃.
3. The temperature-sensitive low-density well cementation cement slurry suspending agent according to claim 1, wherein the mass of the ammonium persulfate is 0.8-1.2% of the total mass of the reaction monomers;
wherein the reaction monomers comprise N-vinyl caprolactam, acrylamide, 2-acrylamido-2-methylpropanesulfonic acid and methyl methacrylate.
4. The preparation method of the temperature-sensitive low-density well cementation cement slurry suspending agent is characterized by comprising the following steps of:
preparing a 20% sodium hydroxide aqueous solution, and placing the solution in an ice water bath for standby;
Firstly, weighing 7-12 parts of acrylamide and 20-25 parts of 2-acrylamido-2-methylpropanesulfonic acid, adding into 150-230 parts of deionized water, stirring a glass rod until the mixture is completely dissolved, regulating the pH to 7-8 by using a prefabricated 20% sodium hydroxide solution, continuously adding 3-8 parts of N-vinyl caprolactam and 0.2-1 part of methyl methacrylate, uniformly stirring, transferring the mixture aqueous solution to a three-neck flask, introducing nitrogen for 30min under the ice water bath condition, and placing the mixture aqueous solution with the introduced nitrogen into a constant-temperature oil bath pot at 50-70 ℃;
Weighing 0.3-0.45 part of ammonium persulfate to prepare an initiator solution, adding the initiator solution when the temperature of the mixture water solution is increased to 50-70 ℃, and starting stirring reaction for 15-20 hours under the constant temperature condition to obtain a suspending agent solution;
Drying, grinding and sieving the suspending agent solution to obtain the suspending agent product.
5. The method for preparing the temperature-sensitive low-density well cementation cement slurry suspending agent according to claim 4, wherein the specific drying conditions are as follows:
Baking at 50-70 deg.C for 24 hr.
6. The temperature-sensitive low-density well cementation cement paste is characterized by comprising the following components: 45 to 60 parts of oil well grade G cement, 25 to 35 parts of floating beads, 12 to 17 parts of reinforcing materials, 1.5 to 3.2 parts of micro silicon, 2.0 to 3.6 parts of fly ash, 2.0 to 3.0 parts of fluid loss additive, 0.23 to 0.60 part of retarder, 0.1 to 0.3 part of defoamer, 80 to 95 parts of water and 0.5 to 1.0 part of suspending agent according to claim 1.
7. The temperature-sensitive low-density well cementation cement paste of claim 6, wherein the cement paste has a density of 1.30-1.40 g/cm 3.
8. The temperature-sensitive low-density well cementation cement paste as claimed in claim 6 or 7, wherein the fluid loss agent and retarder are amide organic high-molecular polymers.
9. The preparation method of the temperature-sensitive low-density well cementation cement paste is characterized by comprising the following steps:
Weighing 45-60 parts of oil well grade G cement, 25-35 parts of floating beads, 12-17 parts of reinforcing materials, 1.5-3.2 parts of micro silicon, 2.0-3.6 parts of fly ash, 2.0-3.0 parts of fluid loss additive, 0.23-0.60 part of retarder and 0.5-1.0 part of suspending agent according to claim 1, and uniformly stirring the raw materials in a container until no obvious color lump exists;
then weighing 80-95 parts of water, pouring the uniformly stirred raw materials into the water while stirring for 15-20 seconds, uniformly stirring, and adding 0.1-0.3 part of defoaming agent in the stirring process.
10. The method for preparing the temperature-sensitive low-density well cementation cement paste according to claim 9, wherein the specific operation of stirring is as follows:
Stirring at a first speed for 15s and then at a second speed for 45s;
wherein the second speed is greater than the first speed.
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