CN109609107B - High-temperature-resistant toughness material and preparation method thereof - Google Patents
High-temperature-resistant toughness material and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of oil and gas well cementation, and particularly relates to a high-temperature-resistant tough material and a preparation method thereof. The invention provides a high-temperature-resistant toughness material for well cementation cement slurry, which comprises the following components in parts by weight: 10-20 parts of latex powder; 10-40 parts of modified rubber powder; 20-50 parts of polyimide resin; 5-10 parts of an aminosilane coupling agent; 15-60 parts of modified nanotubes; the nanotube in the modified nanotube is a carbon nanotube and/or a boron nitride nanotube. The high-temperature resistant toughness material provided by the invention has good stability, and the prepared cement has excellent mechanical property and good toughness, not only can meet the construction requirement of field well cementation, but also can ensure the long-term sealing integrity of well cementation, is beneficial to reducing the damage of underground operation on a cement sheath, reducing the influence of various subsequent construction operations of well cementation on the sealing quality, and improving the recovery ratio.
Description
Technical Field
The invention belongs to the technical field of oil and gas well cementation, and particularly relates to a high-temperature-resistant tough material and a preparation method thereof.
Background
As high-temperature steam at 270-350 ℃ needs to be injected into the heavy oil well in the process of exploitation, the cement slurry system requiring well cementation can bear the high temperature of 350 ℃ after being solidified into set cement, the strength of the set cement is not attenuated or is weakly attenuated, and the alternating thermal stress from 45 ℃ to 350 ℃ can be borne. In special wells such as burning huff and puff wells, the cement paste is required to resist temperature of over 500 ℃ and has excellent CO resistance2Corrosion performance.
The casing pipe is also one of the important factors influencing the production because the casing pipe is also subjected to high temperature in the heavy oil thermal recovery process. When thermal stresses are applied to the casing, the set cement does not provide effective protection to the casing. When steam is injected, the temperature of the bottom of the well rises, and the sleeve expands under heat to generate acting force on the cement sheath. When the radial component of the acting force exceeds the compressive strength of the set cement, the cement sheath can be fractured; when the tangential component of the force exceeds the tensile strength of the set cement, the cement sheath is pulled apart. When the downhole temperature drops, the casing shrinks, which may cause the set cement to separate from the casing or from the formation to create a micro-annulus. The above fracturing, pulling or micro-annulus conditions can cause the annulus to lose integrity. After the integrity of the annulus is lost, the underground interlayer packing is lost firstly, and injected high-temperature steam is communicated and even leaked to the ground, so that the safety and the economy of the thermal production well are affected; secondly, the supporting and protecting effects of the cement ring on the casing are weakened, the casing is more prone to damage, and the safety and the economical efficiency of the thermal production well are further affected.
In order to improve the high temperature resistant toughness property of well cementation cement, elastomer materials, nano silicon, whiskers and the like are generally selected and added, but because the compatibility of the materials and a cement system is poor, the stability of slurry can be affected, and the mechanical property of the cement at higher temperature is not further improved.
Disclosure of Invention
In order to solve the technical problems, the first aspect of the invention provides a high-temperature resistant toughness material for well cementation cement slurry, which comprises the following components in parts by weight:
the nanotube in the modified nanotube is a carbon nanotube and/or a boron nitride nanotube.
As a preferable technical scheme, the latex powder is redispersible latex powder.
As a preferable technical scheme, the modified rubber powder is vinyl silane coupling agent modified rubber powder.
In a preferred embodiment, the vinyl silane coupling agent is at least one selected from the group consisting of vinyl triethoxysilane, vinyl tri-t-butylperoxy silane, vinyl trimethoxysilane, and vinyl tris (methoxyethoxy) silane.
As a preferable technical scheme, the length of the nanotube in the modified nanotube is 1-200 μm.
As a preferred technical scheme, the modified nanotube is a tartaric acid modified nanotube.
As a preferable technical scheme, the weight ratio of the modified rubber powder, the polyimide resin and the modified nanotube is 1: (1-1.5): (0.5-2).
As a preferable technical scheme, the weight ratio of the modified rubber powder, the polyimide resin and the modified nanotube is 1: (1-1.5): (1-2).
As a preferable technical solution, the high temperature resistant tough material component further includes nano silica.
The second aspect of the invention provides a preparation method of the high temperature resistant toughness material, which comprises the following steps:
s1, weighing the raw materials according to the parts by weight, and dissolving the polyimide resin in a solvent;
s2, adding the modified rubber powder and the modified nano-tubes into a mixed solution of ethanol and water, and carrying out ultrasonic treatment;
s3, heating the mixture obtained in the step S2 to 40-80 ℃, reacting for 5-10 h at the rotating speed of 800-1500 rpm, adding an aminosilane coupling agent, and continuing to react for 4-8 h;
s4, adding the polyimide resin dispersion liquid obtained in the step S1 into the mixture obtained in the step S3, and continuing to react for 1-2 hours; adding latex powder, and stirring for 1-2 h to obtain the product.
Has the advantages that: the high-temperature resistant toughness material provided by the invention has good stability, the prepared cement has excellent mechanical property and good toughness, the strength of the set cement cannot decline after high temperature, and the set cement still has good elastic modulus and mechanical property, so that the high-temperature resistant toughness material not only can meet the construction requirements of on-site well cementation, but also can ensure the long-term sealing integrity of well cementation, is beneficial to reducing the damage of underground operation to a cement sheath, reducing the influence of various subsequent construction operations of well cementation on the sealing quality, and improving the recovery ratio.
Detailed Description
In order to solve the problems, the invention provides a high-temperature resistant toughness material for well cementation cement slurry, which comprises the following components in parts by weight:
the nanotube in the modified nanotube is a carbon nanotube and/or a boron nitride nanotube.
As a preferred embodiment, the high-temperature resistant toughness material for the well cementation cement slurry comprises the following components in parts by weight:
the nanotube in the modified nanotube is a carbon nanotube and/or a boron nitride nanotube.
Latex powder
In a preferred embodiment, the latex powder is a redispersible latex powder.
The latex powder is conventionally used redispersible latex powder and can be purchased from the market. Specifically, the redispersible latex powder is at least one selected from the group consisting of copolymer rubber powder of vinyl acetate and ethylene, ternary copolymer powder of ethylene, vinyl chloride and vinyl laurate, ternary copolymer powder of vinyl acetate, ethylene and vinyl ester of higher fatty acid, vinyl acetate homopolymerization rubber powder and copolymer rubber powder of styrene and butadiene.
In a preferred embodiment, the latex powder has an average particle size of 200 to 800 μm.
Preferably, the average particle size of the latex powder is 400-700 μm.
Modified rubber powder
The applicant finds that the toughness and the thermal responsiveness of the well cementation cement slurry can be effectively improved by adding the modified rubber powder.
The rubber powder in the modified rubber powder refers to powder obtained by processing rubber products by a normal-temperature crushing method, a freezing method, a normal-temperature chemical method and the like. The rubber product refers to various rubber products produced by taking natural and synthetic rubber as raw materials, and also includes rubber products produced by utilizing waste rubber. For example, the rubber powder can be obtained by freeze-drying, pulverizing, and sieving waste tires.
In a preferred embodiment, the modified rubber powder is a silane coupling agent modified rubber powder.
In a preferred embodiment, the modified rubber powder is a vinyl silane coupling agent modified rubber powder.
In the invention, the preparation steps of the vinyl silane coupling agent modified rubber powder are as follows:
(1) adding 10g of rubber powder into 200mL of mixed solution of ethanol and water, and carrying out ultrasonic treatment;
(2) and (2) dripping 5g of vinyl silane coupling agent into the mixture obtained in the step (1), reacting for 5 hours, filtering, washing and drying to obtain the vinyl silane coupling agent modified rubber powder.
Wherein the weight ratio of the ethanol to the water in the step (1) is 1: 0.5.
the raw material rubber of the rubber powder contains more unreacted carbon-carbon double bonds, the carbon black as a part of rubber filler contains a plurality of hydroxyl groups, and the vinyl and silicon hydroxyl groups of the vinyl silane coupling agent can react with the active groups, so that the surface of the rubber powder is coated with a coupling agent polymerization layer.
In a preferred embodiment, the vinyl silane coupling agent is at least one member selected from the group consisting of vinyl triethoxysilane, vinyl tri-t-butylperoxy silane, vinyl trimethoxysilane, and vinyl tris (methoxyethoxy) silane.
Preferably, the vinyl silane coupling agent is vinyl triethoxysilane.
Polyimide resin
In the present application, the polyimide resin is at least one of an aliphatic polyimide resin, a semi-aromatic polyimide resin, and an aromatic polyimide resin.
In a preferred embodiment, the polyimide resin is an aromatic polyimide resin.
In a preferred embodiment, the aromatic polyimide resin is at least one selected from the group consisting of a homopolybenzene-type aromatic polyimide resin, a monoether-type aromatic polyimide resin, a diether anhydride-type aromatic polyimide resin, a polyetheracyl aromatic polyimide resin, a polybismaleimide resin, a norbornene diacid-modified polyimide resin, and a polyamideimide resin.
Preferably, the aromatic polyimide resin is at least one selected from the group consisting of polyetherimides, aromatic polyimide resins, polybismaleimides, and polyamideimide resins.
Amino silane coupling agent
In a preferred embodiment, the aminosilane coupling agent is at least one selected from the group consisting of 3-aminopropyltrimethoxysilane, 3-aminopropyltriethoxysilane, anilinomethyltriethoxysilane, 4-anilinotritriethoxysilane, gamma-aminopropyltriethoxysilane, N' -bis [ (3-trimethoxysilyl) propyl ] ethylenediamine, N- (2-aminoethyl) -3-aminopropyltrimethoxysilane, and N-2- (vinylbenzylamino) -ethyl-aminopropyltrimethoxysilane.
Preferably, the aminosilane coupling agent is selected from at least one of 3-aminopropyltrimethoxysilane, 3-aminopropyltriethoxysilane, aniline methyl triethoxysilane, 4-anilino triethoxysilane, and gamma-aminopropyltriethoxysilane.
More preferably, the aminosilane coupling agent is 3-aminopropyltriethoxysilane.
Modified nanotubes
The modified nanotube is a seamless hollow tube rolled from a layered structure. The strength and toughness of the cement paste system can be improved by adding the modified nano tube.
In a preferred embodiment, the nanotubes in the modified nanotubes are carbon nanotubes and/or boron nitride nanotubes.
The carbon nano tube is a one-dimensional tubular structure material, and mainly comprises carbon atoms which are arranged in a hexagonal shape to form coaxial circular tubes with different layers. The carbon nanotube can be divided into single-walled carbon nanotubes and multi-walled carbon nanotubes according to the number of the layers of the tube wall, the interlayer spacing is generally 0.34nm, and the tube diameter of the carbon nanotube is 1-80 nm. Due to the special microstructure, the carbon nano tube has good performances in the aspects of electric conduction, heat conduction, electrochemistry and the like.
The boron nitride nanotubes have a microstructure and mechanical properties similar to carbon nanotubes. The boron nitride nanotube is formed by rolling single-layer or multi-layer boron nitride sheets, and finally forms the single-wall or multi-wall boron nitride nanotube. The B-N bond in the boron nitride nanotube has certain ionic bond characteristics, and B, N atoms are continuously stacked along the C-axis direction and tend to form a two-layer or multi-layer tubular structure. Since stronger interaction between the layers will make the two-or multi-layer tubular structure more stable.
In a preferred embodiment, the length of the nanotubes in the modified nanotubes is 1 to 200 μm.
In the present application, the length of the nanotube is 1 to 200 μm, which means that the nanotube having a length in the range of 1 to 200 μm is included. The length of the nanotubes was measured by scanning electron microscopy.
In a preferred embodiment, the modified nanotubes are tartaric acid modified nanotubes.
The tartaric acid modified nanotube comprises the following steps:
(1) and (3) uniformly mixing 0.5g of nanotube and 10g of tartaric acid, adding the mixture into a flask, heating to 120-160 ℃, stirring for 5 days for reaction, and cooling to room temperature.
(2) Washing with water and ethanol until the washing liquid is neutral, filtering, collecting filter cakes, and drying to obtain the tartaric acid modified nanotube.
The tartaric acid is a strong organic acid, can ionize a plurality of H + at the same time, and can be connected with active groups such as-OH, -COOH and the like on the nanotube.
The second aspect of the invention provides a preparation method of the high temperature resistant toughness material, which comprises the following steps:
s1, weighing the raw materials according to the parts by weight, and dissolving the polyimide resin in a solvent;
s2, adding the modified rubber powder and the modified nano-tubes into a mixed solution of ethanol and water, and carrying out ultrasonic treatment;
s3, heating the mixture obtained in the step S2 to 40-80 ℃, reacting for 5-10 h at the rotating speed of 800-1500 rpm, adding an aminosilane coupling agent, and continuing to react for 4-8 h;
s4, adding the polyimide resin dispersion liquid obtained in the step S1 into the mixture obtained in the step S3, and continuing to react for 1-2 hours; adding latex powder, and stirring for 1-2 h to obtain the product.
The solvent used in step S1 is not particularly limited, and the polyimide resin may be dissolved.
The weight ratio of ethanol to water in the step S2 is 1: (0.5-2).
In the application, the modified rubber powder is added, so that the toughness and the thermal responsiveness of the well cementation cement slurry can be effectively improved. However, the modified rubber powder is not resistant to high temperature, and the rubber powder can change in properties after the temperature exceeds 130 ℃, so that the cement paste cannot improve the toughness. The method comprises the following steps of reacting modified rubber powder and a modified nano tube for 5-10 hours at 40-80 ℃, and reacting active groups on the surface of the modified rubber powder and active groups on the modified nano tube to form nano tube-coated rubber powder; the nano tube has high toughness, high temperature resistance, high temperature inactivation prevention of rubber powder and high mechanical strength of cement.
However, the applicant finds that the compatibility of the rubber powder coated by the nanotube and a cement system is poor, the content of the rubber powder coated by the nanotube is limited, and the content of the rubber powder coated by the nanotube is limited. The modified rubber powder, the polyimide resin and the modified nano tube are mutually cooperated to form an organic-inorganic co-coated rubber powder system, so that the respective properties can be maintained, the defects of the other two substances can be supplemented, and the mechanical property and the high temperature resistance of the cement are improved. In addition, O on the polyimide contains lone pair electrons, and can coordinate with metal ions in the cement to form strong binding force. When the cement is subjected to bending deformation or tension, the cement is not easy to crack under the action of internal binding force.
As a preferred embodiment, the ratio of the modified rubber powder, the polyimide resin and the modified nanotubes in parts by weight is 1: (1-1.5): (0.5-2).
As a preferred embodiment, the ratio of the modified rubber powder, the polyimide resin and the modified nanotubes in parts by weight is 1: (1-1.5): (1-2).
Preferably, the weight ratio of the modified rubber powder to the polyimide resin to the modified nanotube is 1: 1.5: 2.
the applicant unexpectedly finds that when the weight ratio of the modified rubber powder to the polyimide resin to the modified nanotube is 1: 1.5: 2, the toughness of the material is further improved. The probable reason is that the content of the polyimide resin is less than that of the modified nanotubes, part of the nanotubes do not react with the polyimide, the diameter of the nanotubes which do not react with the polyimide is smaller than that of the nanotubes which do react with the polyimide, and the nanotubes and the modified nanotubes are reasonably matched to fill the defects in the cement and form a uniform and dense spatial network structure with a cement system. When the nanotube is damaged by external force, the nanotube which does not react with polyimide firstly limits the expansion of the microcrack, eliminates the stress at the tip of the microcrack, and the nanotube which reacts with polyimide starts to play a role of a bridge along with the continuous integration of the microcrack into a large crack.
As a preferred embodiment, the high temperature resistant tough material component further includes nano silica.
Nano silicon dioxide
The nano silicon dioxide is a tetrahedral amorphous structure formed by taking Si atoms as a center and O atoms as a vertex, the Si atoms on the surface of the nano silicon dioxide are randomly arranged, and hydroxyl groups connected to the Si atoms are not equidistant and are not completely equivalent to participate in chemical reaction. The applicant has found that the surface of the nanosilica presents three hydroxyl groups: the first is geminal, i.e. two hydroxyl groups are attached to one Si atom; the second is an undisturbed, isolated free hydroxyl group; the third is the associative hydroxyl groups which form hydrogen bonds with each other. Neither geminal nor isolated hydroxyl groups form hydrogen bonds.
The nano silicon dioxide can be obtained commercially or by self.
The preparation method of the nano silicon dioxide comprises a dry method and a wet method. The dry method mainly comprises a gas phase method and an electric arc method, and the wet method comprises a precipitation method, a micro-emulsion method, a sol-gel method and the like.
The gas phase method adopts silicon tetrachloride as a raw material, and oxygen and hydrogen are introduced into the silicon tetrachloride gas at a high temperature to hydrolyze to prepare the fumed silica. The silicon dioxide product prepared by the method has high purity, small particle size, spherical shape, high dispersion degree and less surface hydroxyl.
The arc process refers to mixing air and hydrogen with a silicon compound, hydrolyzing at high temperature, separating large gel particles by a cyclone separator, and finally deacidifying to obtain silicon dioxide.
The precipitation method is to generate precipitation by acidifying silicate, and then drying and calcining to obtain the nano silicon dioxide microspheres.
The microemulsion method is characterized in that under the action of a surfactant, two mutually incompatible solvents form a solution, and the solution is subjected to nucleation, coalescence, agglomeration and heat treatment in microbubbles to obtain the nanoparticles. The nano silicon dioxide prepared by the method has the advantages of convenient particle size regulation and control, good particle dispersibility and narrow particle size distribution.
The sol-gel method is to mix silicate ester and absolute ethyl alcohol, adjust pH, add surfactant and stir to prepare the nano silicon dioxide. Preparing and forming uniform precursor solution in a solvent to perform hydrolysis or alcoholysis reaction gelation to generate a uniform and precipitate-free sol system, and drying to obtain target products such as powder, single crystal, thin film and the like. Factors influencing the preparation include the amount of water added, the rate of dropwise addition, the pH value and the reaction temperature in the reaction solution, and the like.
The template method is to use a surfactant as a template, aggregate silica particles on the template to form spherical silica particles, and remove the template by a calcination or decomposition method to obtain the hollow silica microspheres or mesoporous silica microspheres.
As a preferable embodiment, the high temperature resistant toughness material component further comprises 1-10 parts by weight of nano silicon dioxide.
In a preferred embodiment, the nanosilica has an average particle size of 10 to 50 nm.
On one hand, the nano silicon dioxide can promote the cementization process and improve the hydration degree of cement, and forms a cement stone network gel structure together with hydration products in the hydration process; on the other hand, the added nano silicon dioxide plays a volcanic ash effect and reduces the content of calcium hydroxide.
The preparation method of the high-temperature-resistant toughness material comprises the following steps:
s1, weighing the raw materials according to the parts by weight, and dissolving the polyimide resin in a solvent;
s2, adding the modified rubber powder, the modified nanotube and the nano silicon dioxide into a mixed solution of ethanol and water, and carrying out ultrasonic treatment;
s3, heating the mixture obtained in the step S2 to 40-80 ℃, reacting for 5-10 h at the rotating speed of 800-1500 rpm, adding an aminosilane coupling agent, and continuing to react for 4-8 h;
s4, adding the polyimide resin dispersion liquid obtained in the step S1 into the mixture obtained in the step S3, and continuing to react for 1-2 hours; adding latex powder, and stirring for 1-2 h to obtain the product.
In a third aspect of the invention, a cement slurry for well cementation is provided, the raw material of which at least comprises a high temperature resistant tough material.
The cement slurry for well cementation comprises the following components in parts by weight: 100 parts of cement; 10-50 parts of high-temperature resistant toughness material; 1-5 parts of 2-acrylamide-2-methylpropanesulfonic acid; 0.5-2 parts of sodium lignosulfonate; 1-2 parts of sodium tannate; 0.1-0.5 part of dimethyl silicone oil; 10-60 parts of water.
As a preferred embodiment, the cement slurry for well cementation comprises the following components in parts by weight: the cement slurry for well cementation comprises the following components in parts by weight: 100 parts of cement; 20 parts of high-temperature resistant toughness material; 2 parts of 2-acrylamide-2-methylpropanesulfonic acid; 1 part of sodium lignosulfonate; 1 part of sodium tannate; 0.3 part of dimethyl silicone oil; 50 parts of water.
The present invention will be specifically described below by way of examples. It should be noted that the following examples are only for illustrating the present invention and should not be construed as limiting the scope of the present invention, and that the insubstantial modifications and adaptations of the present invention by those skilled in the art based on the above disclosure are still within the scope of the present invention.
In addition, the starting materials used are all commercially available, unless otherwise specified.
Examples
Example 1
A high-temperature resistant toughness material for well cementation cement slurry comprises the following components in parts by weight:
wherein the latex powder is re-dispersible latex powder, and the latex powder (model: DY5020) is purchased from Guangzhou field industry Co.
The modified rubber powder is vinyl triethoxysilane modified rubber powder.
The polyimide resin (type: TY002) was purchased from Haiyang republic of Japan.
The amino silane coupling agent is 3-aminopropyl triethoxysilane.
The length of the nanotube in the modified nanotube is 3-15 μm.
The modified nanotube is tartaric acid modified carbon nanotube, and the carbon nanotube (cargo number: 102027) is purchased from Nanjing Xiifeng.
The preparation method of the high-temperature-resistant toughness material comprises the following steps:
s1, weighing the raw materials according to the parts by weight, and dissolving the polyimide resin in N, N-dimethylformamide;
s2, adding the modified rubber powder and the modified nano-tubes into a mixed solution of ethanol and water, and carrying out ultrasonic treatment;
s3, heating the mixture obtained in the step S2 to 50 ℃, reacting for 5 hours at the rotating speed of 1000rpm, adding an aminosilane coupling agent, and continuing to react for 4 hours;
s4, adding the polyimide resin dispersion liquid obtained in the S1 into the mixture obtained in the S3, and continuing to react for 1 hour; adding the latex powder, and stirring for 1h to obtain the product.
Wherein the mass ratio of ethanol to water in the step S2 is 1: 1.
example 2
A high-temperature resistant toughness material for well cementation cement slurry comprises the following components in parts by weight:
wherein the latex powder is re-dispersible latex powder, and the latex powder (model: DY5020) is purchased from Guangzhou field industry Co.
The modified rubber powder is vinyl triethoxysilane modified rubber powder.
The polyimide resin (type: TY002) was purchased from Haiyang republic of Japan.
The amino silane coupling agent is 3-aminopropyl triethoxysilane.
The length of the nanotube in the modified nanotube is 3-15 μm.
The modified nanotube is tartaric acid modified carbon nanotube, and the carbon nanotube (cargo number: 102027) is purchased from Nanjing Xiifeng.
The preparation method of the high-temperature-resistant toughness material comprises the following steps:
s1, weighing the raw materials according to the parts by weight, and dissolving the polyimide resin in N, N-dimethylformamide;
s2, adding the modified rubber powder and the modified nano-tubes into a mixed solution of ethanol and water, and carrying out ultrasonic treatment;
s3, heating the mixture obtained in the step S2 to 50 ℃, reacting for 8 hours at the rotating speed of 1000rpm, adding an aminosilane coupling agent, and continuing to react for 5 hours;
s4, adding the polyimide resin dispersion liquid obtained in the S1 into the mixture obtained in the S3, and continuing to react for 1 hour; adding the latex powder, and stirring for 1h to obtain the product.
Wherein the mass ratio of ethanol to water in the step S2 is 1: 1.
example 3
A high-temperature resistant toughness material for well cementation cement slurry comprises the following components in parts by weight:
wherein the latex powder is re-dispersible latex powder, and the latex powder (model: DY5020) is purchased from Guangzhou field industry Co.
The modified rubber powder is vinyl triethoxysilane modified rubber powder.
The polyimide resin (type: TY002) was purchased from Haiyang republic of Japan.
The amino silane coupling agent is 3-aminopropyl triethoxysilane.
The length of the nanotube in the modified nanotube is 3-15 μm.
The modified nanotube is tartaric acid modified carbon nanotube, and the carbon nanotube (cargo number: 102027) is purchased from Nanjing Xiifeng.
The specific steps of the preparation method of the high-temperature-resistant toughness material are the same as those of the example 2.
Example 4
A high-temperature resistant toughness material for well cementation cement slurry comprises the following components in parts by weight:
wherein the latex powder is re-dispersible latex powder, and the latex powder (model: DY5020) is purchased from Guangzhou field industry Co.
The modified rubber powder is vinyl triethoxysilane modified rubber powder.
The polyimide resin (type: TY002) was purchased from Haiyang republic of Japan.
The amino silane coupling agent is 3-aminopropyl triethoxysilane.
The length of the nanotube in the modified nanotube is 3-15 μm.
The modified nanotube is tartaric acid modified carbon nanotube, and the carbon nanotube (cargo number: 102027) is purchased from Nanjing Xiifeng.
The specific steps of the preparation method of the high-temperature-resistant toughness material are the same as those of the example 2.
Example 5
A high-temperature resistant toughness material for well cementation cement slurry comprises the following components in parts by weight:
wherein the latex powder is re-dispersible latex powder, and the latex powder (model: DY5020) is purchased from Guangzhou field industry Co.
The modified rubber powder is vinyl triethoxysilane modified rubber powder.
The polyimide resin (type: TY002) was purchased from Haiyang republic of Japan.
The amino silane coupling agent is 3-aminopropyl triethoxysilane.
The length of the nanotube in the modified nanotube is 3-15 μm.
The modified nanotube is tartaric acid modified carbon nanotube, and the carbon nanotube (cargo number: 102027) is purchased from Nanjing Xiifeng.
The specific steps of the preparation method of the high-temperature-resistant toughness material are the same as those of the example 2.
Example 6
A high-temperature resistant toughness material for well cementation cement slurry comprises the following components in parts by weight:
wherein the latex powder is re-dispersible latex powder, and the latex powder (model: DY5020) is purchased from Guangzhou field industry Co.
The modified rubber powder is vinyl triethoxysilane modified rubber powder.
The polyimide resin (type: TY002) was purchased from Haiyang republic of Japan.
The amino silane coupling agent is 3-aminopropyl triethoxysilane.
The length of the nanotube in the modified nanotube is 3-15 μm.
The modified nanotube is tartaric acid modified carbon nanotube, and the carbon nanotube (cargo number: 102027) is purchased from Nanjing Xiifeng.
The specific steps of the preparation method of the high-temperature-resistant toughness material are the same as those of the example 2.
Example 7
A high-temperature resistant toughness material for well cementation cement slurry comprises the following components in parts by weight:
wherein the latex powder is re-dispersible latex powder, and the latex powder (model: DY5020) is purchased from Guangzhou field industry Co.
The modified rubber powder is vinyl triethoxysilane modified rubber powder.
The polyimide resin (type: TY002) was purchased from Haiyang republic of Japan.
The amino silane coupling agent is 3-aminopropyl triethoxysilane.
The length of the nanotube in the modified nanotube is 3-15 μm.
The modified nanotube is tartaric acid modified carbon nanotube, and the carbon nanotube (cargo number: 102027) is purchased from Nanjing Xiifeng.
The specific steps of the preparation method of the high-temperature-resistant toughness material are the same as those of the example 2.
Example 8
A high-temperature resistant toughness material for well cementation cement slurry comprises the following components in parts by weight:
wherein the latex powder is re-dispersible latex powder, and the latex powder (model: DY5020) is purchased from Guangzhou field industry Co.
The modified rubber powder is vinyl triethoxysilane modified rubber powder.
The polyimide resin (type: TY002) was purchased from Haiyang republic of Japan.
The amino silane coupling agent is 3-aminopropyl triethoxysilane.
The length of the nanotube in the modified nanotube is 100-120 μm.
The modified nanotube is tartaric acid modified boron nitride nanotube, and the boron nitride nanotube (cargo number: 101953) is purchased from Nanjing Xiancheng.
The specific steps of the preparation method of the high-temperature-resistant toughness material are the same as those of the example 2.
Example 9
A high-temperature resistant toughness material for well cementation cement slurry comprises the following components in parts by weight:
wherein the latex powder is re-dispersible latex powder, and the latex powder (model: DY5020) is purchased from Guangzhou field industry Co.
The modified rubber powder is vinyl triethoxysilane modified rubber powder.
The polyimide resin (type: TY002) was purchased from Haiyang republic of Japan.
The amino silane coupling agent is 3-aminopropyl triethoxysilane.
The length of the nanotube in the modified nanotube is 100-120 μm.
The modified nanotube is tartaric acid modified boron nitride nanotube, and the boron nitride nanotube (cargo number: 101953) is purchased from Nanjing Xiancheng.
The average particle size of the nano silicon dioxide is 20nm, and the nano silicon dioxide (the product number is 100361) is purchased from Nanjing Xiapong.
The preparation method of the high-temperature-resistant toughness material comprises the following steps:
s1, weighing the raw materials according to the parts by weight, and dissolving the polyimide resin in a solvent;
s2, adding the modified rubber powder, the modified nanotube and the nano silicon dioxide into a mixed solution of ethanol and water, and carrying out ultrasonic treatment;
s3, heating the mixture obtained in the step S2 to 40 ℃, reacting for 10 hours at the rotating speed of 1000rpm, adding an aminosilane coupling agent, and continuing to react for 6 hours;
s4, adding the polyimide resin dispersion liquid obtained in the S1 into the mixture obtained in the S3, and continuing to react for 2 hours; adding the latex powder, and stirring for 2h to obtain the product.
Wherein the mass ratio of ethanol to water in the step S2 is 1: 1.
example 10
A high-temperature resistant toughness material for well cementation cement slurry comprises the following components in parts by weight:
wherein the latex powder is re-dispersible latex powder, and the latex powder (model: DY5020) is purchased from Guangzhou field industry Co.
The modified rubber powder is vinyl triethoxysilane modified rubber powder.
The polyimide resin (type: TY002) was purchased from Haiyang republic of Japan.
The amino silane coupling agent is 3-aminopropyl triethoxysilane.
The length of the nanotube in the modified nanotube is 100-120 μm.
The modified nanotube is tartaric acid modified boron nitride nanotube, and the boron nitride nanotube (cargo number: 101953) is purchased from Nanjing Xiancheng.
The average particle size of the nano silicon dioxide is 20nm, and the nano silicon dioxide (the product number is 100361) is purchased from Nanjing Xiapong.
The specific steps of the preparation method of the high temperature resistant toughness material are the same as those of example 9.
Comparative example 1
The specific components and weight portions of the high-temperature resistant toughness material for well cementation cement slurry are the same as those in example 8, and the difference is that the material does not contain polyimide resin and modified nanotubes.
The specific steps of the preparation method of the high-temperature-resistant tough material are the same as those of the example 2, and the difference is that the polyimide resin and the modified nanotube are not added.
Comparative example 2
The specific components and weight portions of the high-temperature resistant toughness material for well cementation cement slurry are the same as those of the embodiment 8, and the difference is that the material does not contain polyimide resin.
The specific steps of the preparation method of the high-temperature-resistant tough material are the same as those of the example 2, but the polyimide resin is not added.
Comparative example 3
The specific components and weight portions of the high-temperature resistant toughness material for well cementation cement slurry are the same as those of the embodiment 8, and the difference is that the material does not contain modified nanotubes.
The specific steps of the preparation method of the high-temperature-resistant toughness material are the same as those of the example 2, and the difference is that no modified nanotube is added.
Comparative example 4
The specific components and weight parts of the high-temperature resistant toughness material for well cementation cement slurry are the same as those in example 8, and the difference is that the modified nanotube is a malic acid modified boron nitride nanotube.
The malic acid modified boron nitride nanotube comprises the following preparation steps:
(1) mixing 0.5g of boron nitride nanotube and 10g of malic acid uniformly, adding into a flask, heating to 160 ℃, stirring for reacting for 5 days, and cooling to room temperature.
(2) Washing with water and ethanol until the washing liquor is neutral, filtering, collecting a filter cake, and drying to obtain the malic acid modified boron nitride nanotube.
The specific steps of the preparation method of the high-temperature-resistant toughness material are the same as those of the example 2.
Comparative example 5
The specific components and weight parts of the high-temperature resistant toughness material for well cementation cement slurry are the same as those in example 8, and the difference is that the nanotube is a citric acid modified boron nitride nanotube.
The preparation steps of the citric acid modified boron nitride nanotube are as follows:
(1) 0.5g of boron nitride nanotube and 10g of citric acid are mixed uniformly, added into a flask, heated to 160 ℃, stirred for reaction for 5 days, and cooled to room temperature.
(2) Washing with water and ethanol until the washing solution is neutral, filtering, collecting a filter cake, and drying to obtain the citric acid modified boron nitride nanotube.
The specific steps of the preparation method of the high-temperature-resistant toughness material are the same as those of the example 2.
Comparative example 6
The specific components and weight parts of the high-temperature resistant toughness material for well cementation cement slurry are the same as those in example 8, and the difference is that the modified rubber powder is replaced by rubber powder, and the modified boron nitride nanotube is replaced by a boron nitride nanotube.
The specific steps of the preparation method of the high-temperature-resistant toughness material are the same as those of the example 2.
Performance testing
The high-temperature resistant toughness materials in the examples and the comparative examples are prepared into well cementation cement, the cement slurry for well cementation is maintained by a pressurization maintenance kettle, and performance test is carried out after maintenance is carried out for 3 days at 350 ℃. The specific test results are shown in table 1.
The cement slurry for well cementation comprises the following components in parts by weight: 100 parts of cement; 20 parts of high-temperature resistant toughness material; 2 parts of 2-acrylamide-2-methylpropanesulfonic acid; 1 part of sodium lignosulfonate; 1 part of sodium tannate; 0.3 part of dimethyl silicone oil; 50 parts of water.
A high-temperature high-pressure triaxial rock mechanical testing system (RTR-1000 of GCTS company in America) is adopted to carry out triaxial stress testing under the test condition of triaxial stress (confining pressure of 0MPa), and the compressive strength, the elastic modulus and the Poisson ratio under triaxial confining pressure are obtained through testing.
TABLE 1 concrete test results for cementing cement slurries
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention in other forms, and any person skilled in the art may modify or change the technical content of the above disclosure into equivalent embodiments with equivalent changes, but all those simple modifications, equivalent changes and modifications made to the above embodiments according to the technical spirit of the present invention still belong to the protection scope of the present invention.
Claims (8)
1. The high-temperature-resistant toughness material for well cementation cement slurry is characterized by comprising the following components in parts by weight:
10-20 parts of latex powder;
10-40 parts of modified rubber powder;
20-50 parts of polyimide resin;
5-10 parts of an aminosilane coupling agent;
15-60 parts of modified nanotubes;
the nanotube in the modified nanotube is a carbon nanotube and/or a boron nitride nanotube;
the modified rubber powder is vinyl silane coupling agent modified rubber powder;
the preparation method of the vinyl silane coupling agent modified rubber powder comprises the following steps: (1) adding 10g of rubber powder into 200mL of mixed solution of ethanol and water, and carrying out ultrasonic treatment; (2) dripping 5g of vinyl silane coupling agent into the mixture obtained in the step (1), reacting for 5 hours, filtering, washing and drying to obtain vinyl silane coupling agent modified rubber powder;
the modified nanotube is a tartaric acid modified nanotube;
the tartaric acid modified nanotube comprises the following steps: (1) uniformly mixing 0.5g of nanotube and 10g of tartaric acid, adding the mixture into a flask, heating to 120-160 ℃, stirring for 5 days, and cooling to room temperature;
(2) washing with water and ethanol until the washing liquid is neutral, filtering, collecting filter cakes, and drying to obtain the tartaric acid modified nanotube.
2. The high temperature resistant tough material according to claim 1, wherein the latex powder is a re-dispersible latex powder.
3. The high temperature resistant ductile material of claim 1 wherein said vinyl silane coupling agent is selected from at least one of vinyl triethoxysilane, vinyl tri-t-butylperoxy silane, vinyl trimethoxysilane, and vinyl tris (methoxyethoxy) silane.
4. The high temperature resistant ductile material of claim 1 wherein the length of the nanotubes in the modified nanotubes is 1 to 200 μm.
5. The high-temperature-resistant tough material as claimed in claim 1, wherein the weight ratio of the modified rubber powder, the polyimide resin and the modified nanotube is 1: (1-1.5): (0.5-2).
6. The high-temperature-resistant tough material according to claim 5, wherein the weight ratio of the modified rubber powder to the polyimide resin to the modified nanotube is 1: (1-1.5): (1-2).
7. The high temperature resistant toughness material of any one of claims 1 to 6, wherein the high temperature resistant toughness material component further comprises nano silica.
8. The preparation method of the high temperature resistant toughness material according to any one of claims 1 to 7, characterized by comprising the following steps:
s1, weighing the raw materials according to the parts by weight, and dissolving the polyimide resin in a solvent;
s2, adding the modified rubber powder and the modified nano-tubes into a mixed solution of ethanol and water, and carrying out ultrasonic treatment;
s3, heating the mixture obtained in the step S2 to 40-80 ℃, reacting for 5-10 h at the rotating speed of 800-1500 rpm, adding an aminosilane coupling agent, and continuing to react for 4-8 h;
s4, adding the polyimide resin dispersion liquid obtained in the step S1 into the mixture obtained in the step S3, and continuing to react for 1-2 hours; adding latex powder, and stirring for 1-2 h to obtain the product.
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| CN114644480A (en) * | 2020-12-17 | 2022-06-21 | 中石化石油工程技术服务有限公司 | Elastic and tough cement paste containing thermoplastic elastic material and preparation method thereof |
| CN114644732A (en) * | 2020-12-17 | 2022-06-21 | 中石化石油工程技术服务有限公司 | Thermoplastic elastic material for oil well cement and preparation method thereof |
| CN116040999A (en) * | 2022-12-22 | 2023-05-02 | 中国石油天然气集团有限公司 | Thermally responsive cement and cement paste |
| CN117304584A (en) * | 2023-11-29 | 2023-12-29 | 广州双一乳胶制品有限公司 | Anti-frosting glove latex, preparation method thereof and application thereof in preparation of anti-frosting glove |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102250596A (en) * | 2011-05-25 | 2011-11-23 | 天津中油渤星工程科技有限公司 | Novel cement paste for well cementation |
| CN104291733A (en) * | 2014-09-16 | 2015-01-21 | 陕西延长石油(集团)有限责任公司研究院 | Toughened anti-channeling agent for cement and toughened cement for cementing shale gas horizontal well |
| CN107216070A (en) * | 2017-01-24 | 2017-09-29 | 中国石油集团长城钻探工程有限公司固井公司 | Efficient anti-erosion channeling control cement slurry system |
| CN107628781A (en) * | 2017-08-29 | 2018-01-26 | 四川弘晟石油工程技术服务有限公司 | A kind of cementing slurry and preparation method thereof |
| CN107794012A (en) * | 2016-09-05 | 2018-03-13 | 中石化石油工程技术服务有限公司 | Toughness reinforcing expansion cement slurry is used in a kind of gas storage well cementation |
| CN108865087A (en) * | 2018-07-19 | 2018-11-23 | 中国石油集团工程技术研究院有限公司 | A kind of thermosetting epoxy resin anchorage liquid |
-
2019
- 2019-01-16 CN CN201910040381.9A patent/CN109609107B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102250596A (en) * | 2011-05-25 | 2011-11-23 | 天津中油渤星工程科技有限公司 | Novel cement paste for well cementation |
| CN104291733A (en) * | 2014-09-16 | 2015-01-21 | 陕西延长石油(集团)有限责任公司研究院 | Toughened anti-channeling agent for cement and toughened cement for cementing shale gas horizontal well |
| CN107794012A (en) * | 2016-09-05 | 2018-03-13 | 中石化石油工程技术服务有限公司 | Toughness reinforcing expansion cement slurry is used in a kind of gas storage well cementation |
| CN107216070A (en) * | 2017-01-24 | 2017-09-29 | 中国石油集团长城钻探工程有限公司固井公司 | Efficient anti-erosion channeling control cement slurry system |
| CN107628781A (en) * | 2017-08-29 | 2018-01-26 | 四川弘晟石油工程技术服务有限公司 | A kind of cementing slurry and preparation method thereof |
| CN108865087A (en) * | 2018-07-19 | 2018-11-23 | 中国石油集团工程技术研究院有限公司 | A kind of thermosetting epoxy resin anchorage liquid |
Non-Patent Citations (3)
| Title |
|---|
| 丁苯胶乳水泥浆体系在江苏油田的应用;王华东等;《小型油气藏》;20070325(第01期) * |
| 固井水泥石增韧材料的研究进展;俞嘉敏等;《硅酸盐通报》;20170915;第36卷(第09期);3013-3019 * |
| 陆相页岩气水平井中增韧防气窜固井水泥浆体系的研究;景丰;《石油化工应用》;20180725;第37卷(第07期);5-10 * |
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