CN112480889B - Preparation method of retarder for slag cementing fluid - Google Patents
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Abstract
The invention relates to a preparation method of a retarder for slag cementing fluid, which comprises the following steps: (1) mixing sodium styrene sulfonate, maleic acid and methacryloyloxyethyl trimethyl ammonium chloride in a reaction container, dissolving in deionized water, and adjusting the pH value of a reaction solution to 7-8; introducing nitrogen to remove oxygen, and adding an initiator potassium persulfate when the temperature is raised to 70 ℃; cooling, purifying and drying the product to obtain a component A; (2) spreading natural vermiculite on a magnetic disk, placing in a microwave oven, treating for 1 min under high fire condition, adding into hydrochloric acid, and stirring in water bath at 70 deg.C to obtain acid modified vermiculite powder, i.e. component B; (3) mixing sodium tartrate and citric acid to obtain a component C; (4) mixing the component A, the component B and the component C in a mass ratio of 3:1: 1. The invention has reliable principle and simple and convenient operation, and the prepared retarder can effectively control the thickening time of the slag cementing fluid without influencing the sedimentation stability, and can be widely used for the cementing engineering taking the slag cementing material as the support.
Description
Technical Field
The invention relates to a preparation method of a retarder for a well cementation fluid in the field of oilfield chemistry, in particular to a preparation method of a retarder for a well cementation slag cementing material, which can effectively control the thickening time of a slag well cementation fluid and can improve the sedimentation stability of the slag well cementation fluid.
Background
The traditional well cementation refers to the process of setting a casing string in a drilled well after the well drilling operation reaches a certain well depth, then injecting cement slurry into an annular space between the casing string and the well wall to reach a certain preset position, and quickly condensing and hardening the cement slurry within preset time to form a high-quality and complete cement sheath with good interlayer packing capacity. In recent years, with the increase of the exploration and development difficulty of oil fields and the complexity of underground exploitation, the difficulty of well cementation is gradually increased. The traditional cement slurry well cementation technology has the problems of easy formation loss, slow strength development, high density, easy leakage and the like. Therefore, the cement slag which is a cementing material with hydraulic property similar to cement is widely concerned by related researchers due to the characteristics of strong activity, high early strength, strong displacement efficiency, low cost and the like, and the slag cementing fluid technology is generated at the same time.
The slag well cementing liquid is a novel well cementing liquid prepared by taking slag as an inorganic cementing material, sodium hydroxide, sodium carbonate, sodium silicate and a compound thereof as an activating agent, and sodium carboxymethylcellulose, hydroxyethyl cellulose and the like as a suspending agent. The slag well cementing liquid can replace cement slurry to fill an annular space between the casing and the casing or the stratum, support the casing and reinforce the well wall after solidification and hardening, and effectively seal an oil-gas-water layer, so that the slag well cementing liquid is used for solving the low-pressure easily-leaked stratum and long-sealing-section well cementing operation, and improving the sealing and filling operation of non-target layers such as simplified well body structures.
The slag well cementation liquid retarder is one of the most important three additives, plays an important role in delaying the setting time and maintaining the pumpable state of slurry, and is a key link for ensuring the smoothness of well cementation construction and the well cementation quality. The retarder used for cement slurry at present is not suitable for slag well cementing liquid, and development of the retarder suitable for the slag well cementing liquid is imminent.
Disclosure of Invention
The invention aims to provide a preparation method of a retarder for slag cementing fluid, which has reliable principle and simple and convenient operation, solves the problems of poor sedimentation stability, excessive dispersion, reduced consistency and the like of the existing slag cementing fluid, can effectively control and adjust the thickening time of the slag cementing fluid, does not influence the sedimentation stability, and can be widely applied to the well cementation engineering supported by the slag cementing material well cementation technology.
In order to achieve the technical purpose, the invention adopts the following technical scheme.
A preparation method of a retarder for slag cementing fluid sequentially comprises the following steps:
(1) preparing a retarder A component:
1) mixing sodium styrene sulfonate SSS, maleic acid MA and methacryloyloxyethyl trimethyl ammonium chloride DMC in a mass ratio of 10-8: 7-5: 3-1 in a reaction vessel, dissolving in deionized water, and adjusting the pH value of a reaction solution to 7-8 by using sodium hydroxide;
2) introducing nitrogen into the reaction container for 10min to remove oxygen, and slowly adding an initiator potassium persulfate when the temperature of the reaction system rises to 70 ℃, wherein the mass of the potassium persulfate is 1.0-3.0% of the total mass of the monomers;
3) after the reaction is carried out for 4 hours, cooling the viscous liquid product to room temperature, purifying, drying and crushing the viscous liquid product by using acetone to obtain a retarder A component;
(2) preparing a retarder B component:
1) uniformly spreading natural Vermiculite (VER) as a raw material on a magnetic disc, placing the magnetic disc in a microwave oven, and treating for 1 min under the condition of microwave high fire to obtain microwave expanded vermiculite;
2) adding a certain amount of microwave expanded vermiculite powder into 2mol/L hydrochloric acid solution according to the solid-liquid mass ratio of 1: 20-25, and stirring for 2 hours at 70 ℃ in a water bath;
3) washing, filtering, drying and grinding to 200 meshes to obtain acid modified vermiculite powder, namely the retarder B component;
(3) preparing a retarder C component:
mixing sodium tartrate and citric acid in a mass ratio of 20-80: 80-20 to obtain a retarder C component;
(4) and preparing a retarder:
and mixing the component A, the component B and the component C in a mass ratio of 3:1:1 to obtain the slag well cementing liquid retarder.
The above substances are all available on the market.
The retarder for the slag cementing fluid prepared by the invention is white powder in appearance and is tasteless. The retarder has good solubility in water and good retarding effect, can obviously prolong the thickening time of a cementing fluid, and keeps good sedimentation stability.
Compared with the prior art, the invention has the following beneficial effects:
1. the invention adopts a free radical aqueous solution polymerization mode and uses potassium persulfate of inorganic peroxides as an initiator, the operation process is simple and easy, the success rate of synthesizing the polymer is high, and a certain conversion rate can be ensured.
2. Macromolecule and functional group monomers which are not easy to degrade are introduced, so that the temperature resistance of the obtained polymer is remarkably improved, and the thickening time of the well cementing fluid can be effectively prolonged.
3. The novel monomer is adopted to enable the polymer to generate intermolecular or intramolecular association at a certain temperature, and the strong hydrophilicity of the polymer molecular chain and the improvement of the compatibility stability are ensured due to the higher SSS content in the polymer molecule.
4. The vermiculite adopted by the invention is a natural and nontoxic mineral substance, consists of a large number of layers with certain structural units, and can expand under the action of high temperature. The vermiculite structure is not destroyed by a microwave modification method, but the pores between vermiculite layers are dredged, and the adsorption performance of the expanded vermiculite is improved along with the increase of the distance between the vermiculite layers, so that the vermiculite can be better adsorbed with other powder, and meanwhile, the vermiculite has good water absorption and stable chemical performance.
5. In the invention, the vermiculite acidification is to dissolve out tetrahedral cations and octahedral cations in a vermiculite structure by using inorganic strong acid so as to achieve the purposes of improving the specific surface area of the vermiculite, improving the layer charge and increasing surface active functional groups. The acidified vermiculite has better compatibility and can be better combined with an organic matrix.
6. The retarder adopts a mode of combining three components, and makes up the defects of single material and performance loss of the original retarder.
7. The retarder is specially used for controlling the retarding effect of slag cementing liquid for cementing wells, and the defects and shortcomings of the prior art are filled.
Drawings
FIG. 1 is a graph showing the thickening of a retarder for slag cementing fluids at 70 ℃.
FIG. 2 is a graph showing the thickening of a retarder for slag cementing fluids at 80 ℃.
FIG. 3 is a graph showing the thickening of a retarder for slag cementing fluids at 90 ℃.
Detailed Description
The invention is further illustrated below with reference to the figures and examples.
Example 1
The preparation process of the retarder comprises the following steps:
(1) and preparation of the component A:
1) mixing sodium styrene sulfonate SSS, maleic acid MA and methacryloyloxyethyl trimethyl ammonium chloride DMC in a mass ratio of 10:7:3 in a reaction vessel, dissolving in deionized water, and adjusting the pH value of a reaction solution to 7-8 by using sodium hydroxide;
2) introducing nitrogen into the reaction vessel for 10min to remove oxygen, and slowly adding an initiator potassium persulfate when the temperature of the reaction system rises to 70 ℃, wherein the mass of the potassium persulfate is 1.0 percent of the total mass of the monomers;
3) after the reaction is carried out for 4 hours, cooling the viscous liquid product to room temperature, purifying, drying and crushing the viscous liquid product by using acetone to obtain a retarder component A;
(2) and preparing a component B:
1) uniformly spreading natural Vermiculite (VER) as a raw material on a magnetic disc, placing the magnetic disc in a microwave oven, and treating for 1 min under the condition of microwave high fire to obtain microwave expanded vermiculite;
2) adding a certain amount of microwave expanded vermiculite powder into an acid solution of hydrochloric acid of 2mol/L according to a solid-to-liquid ratio of 1:20, and magnetically stirring for 2 hours at 70 ℃ in a water bath;
3) standing for 2h in a natural environment after stirring, washing, performing suction filtration, then drying the mixture in a drying oven at 105 ℃ for 24 h, and grinding to 200 meshes to obtain acid modified vermiculite powder, namely a retarder component B;
(3) and C, preparation of a component C:
mixing sodium tartrate and citric acid at a ratio of 20:80 to obtain a retarder component C;
(4) and preparing a retarder:
A. b, C the components are mixed according to the proportion of 3:1:1 to prepare the retarder for the slag cementing liquid.
The prepared retarder (named as H1) is added into a slag cementing fluid formula, and a test is carried out under the thickening condition of 70 ℃ of temperature and 25MPa of pressure to verify the retarding performance of the retarder.
The formula of the slag well cementing fluid comprises the following components: 150 parts of slag, 12 parts of an activator, 2 parts of a suspension stabilizer, 3 parts of a retarder and 100 parts of water.
Note: the slag is titanium extraction tailings, the activating agent is sodium hydroxide, and the suspension stabilizing agent is sodium carboxymethyl cellulose.
As shown in figure 1, the thickening time of the slag well cementation fluid is obviously prolonged in a high-temperature and high-pressure environment, the requirement of oil-gas well cementing site construction on the well cementation fluid injection time can be met, the thickening curve shows that the addition of the retarder does not have abnormal phenomena of bulging and core-spun under the high-temperature and high-pressure condition, the consistency of cement slurry is maintained around a relatively stable value, and the retarder has a good effect on maintaining the sedimentation stability of the slag well cementation fluid.
Example 2
The preparation process of the retarder comprises the following steps:
(1) and preparation of the component A:
1) mixing sodium styrene sulfonate SSS, maleic acid MA and methacryloyloxyethyl trimethyl ammonium chloride DMC in a mass ratio of 9:6:2 in a reaction vessel, dissolving in deionized water, and adjusting the pH value of a reaction solution to 7-8 by using sodium hydroxide;
2) introducing nitrogen into the reaction vessel for 10min to remove oxygen, and slowly adding an initiator potassium persulfate when the temperature of the reaction system rises to 70 ℃, wherein the mass of the potassium persulfate is 2.0 percent of the total mass of the monomers;
3) after the reaction is carried out for 4 hours, cooling the viscous liquid product to room temperature, purifying, drying and crushing the viscous liquid product by using acetone to obtain a retarder component A;
(2) and preparing a component B:
1) uniformly spreading natural Vermiculite (VER) as a raw material on a magnetic disc, placing the magnetic disc in a microwave oven, and treating for 1 min under the condition of microwave high fire to obtain microwave expanded vermiculite;
2) adding a certain amount of microwave expanded vermiculite powder into an acid solution of 2mol/L hydrochloric acid according to a solid-to-liquid ratio of 1:23, and magnetically stirring for 2 hours at 70 ℃ in a water bath;
3) standing for 2h in natural environment after stirring, washing, performing suction filtration, then drying for 24 h in a drying oven at 105 ℃, and grinding to 200 meshes to obtain acid modified vermiculite powder, namely a retarder component B;
(3) and C, preparation of a component C:
mixing sodium tartrate and citric acid at a ratio of 50:50 to obtain a retarder component C;
(4) and preparing a retarder:
A. b, C the components are mixed according to the proportion of 3:1:1 to prepare the retarder for the slag cementing liquid.
The prepared retarder (named as H2) is added into a slag cementing fluid formula, and a test is carried out under the thickening condition of 80 ℃ and 30MPa of pressure to verify the retarding performance of the retarder.
The formula of the slag well cementing fluid comprises the following components: 120 parts of slag, 10 parts of activating agent, 1.5 parts of suspension stabilizer, 4 parts of retarder and 100 parts of water.
Note: the slag is titanium extraction tailings, the activating agent is sodium hydroxide, and the suspension stabilizing agent is sodium carboxymethyl cellulose.
As shown in figure 2, the thickening time of the slag cementing fluid is obviously prolonged in a high-temperature and high-pressure environment, the requirement of oil-gas well cementing site construction on the cementing time of a cementing fluid pump can be met, the thickening curve shows that the addition of the retarder does not have abnormal phenomena of 'bulging' and 'core-spun' under the high-temperature and high-pressure condition, the consistency of cement slurry is maintained around a relatively stable value, and the retarder has a good effect on maintaining the sedimentation stability of the slag cementing fluid.
Example 3
The preparation process of the retarder comprises the following steps:
(1) and preparation of the component A:
1) mixing sodium styrene sulfonate SSS, maleic acid MA and methacryloyloxyethyl trimethyl ammonium chloride DMC in a mass ratio of 8:5:1 in a reaction vessel, dissolving in deionized water, and adjusting the pH value of a reaction solution to 7-8 by using sodium hydroxide;
2) introducing nitrogen into the reaction vessel for 10min to remove oxygen, and slowly adding an initiator potassium persulfate when the temperature of the reaction system rises to 70 ℃, wherein the mass of the potassium persulfate is 3.0 percent of the total mass of the monomers;
3) after the reaction is carried out for 4 hours, cooling the viscous liquid product to room temperature, purifying, drying and crushing the viscous liquid product by using acetone to obtain a retarder component A;
(2) and preparing a component B:
1) uniformly spreading natural Vermiculite (VER) as a raw material on a magnetic disc, placing the magnetic disc in a microwave oven, and treating for 1 min under the condition of microwave high fire to obtain microwave expanded vermiculite;
2) adding a certain amount of microwave expanded vermiculite powder into an acid solution of 2mol/L hydrochloric acid according to a solid-to-liquid ratio of 1:25, and magnetically stirring for 2 hours at 70 ℃ in a water bath;
3) standing for 2h in natural environment after stirring, washing, performing suction filtration, then drying for 24 h in a drying oven at 105 ℃, and grinding to 200 meshes to obtain acid modified vermiculite powder, namely a retarder component B;
(3) and C, preparation of a component C:
mixing sodium tartrate and citric acid at a ratio of 80:20 to obtain a retarder component C;
(4) and preparing a retarder:
A. b, C the components are mixed according to the proportion of 3:1:1 to prepare the retarder for the slag cementing liquid.
The prepared retarder (named as H3) is added into a slag cementing fluid formula, and a test is carried out under the thickening condition of the temperature of 90 ℃ and the pressure of 40MPa to verify the retarding performance of the retarder.
The formula of the slag well cementing fluid comprises the following components: 150 parts of slag, 10 parts of an activator, 2 parts of a suspension stabilizer, 6 parts of a retarder and 100 parts of water.
Note: the slag is titanium extraction tailings, the activating agent is sodium hydroxide, and the suspension stabilizing agent is sodium carboxymethyl cellulose.
As shown in figure 3, the thickening time of the slag cementing fluid is obviously prolonged in a high-temperature and high-pressure environment, the requirement of oil-gas well cementing site construction on the cementing time of a cementing fluid pump can be met, the thickening curve shows that the addition of the retarder does not have abnormal phenomena of 'bulging' and 'core-spun' under the high-temperature and high-pressure condition, the consistency of cement slurry is maintained around a relatively stable value, and the retarder has a good effect on maintaining the sedimentation stability of the slag cementing fluid.
As shown in figures 1-3, thickening time of the slag cementing fluid is obviously prolonged, the phenomenon of obvious reduction of the consistency is not caused, the construction requirement of a cementing site can be met, and a thickening curve shows that the retarder is suitable for the slag cementing fluid, and the problems of poor stability and serious sedimentation can be avoided and solved.
Claims (1)
1. A preparation method of a retarder for slag cementing fluid sequentially comprises the following steps:
(1) preparing a retarder A component:
1) mixing sodium styrene sulfonate SSS, maleic acid MA and methacryloyloxyethyl trimethyl ammonium chloride DMC in a mass ratio of 10-8: 7-5: 3-1 in a reaction vessel, dissolving in deionized water, and adjusting the pH value of a reaction solution to 7-8 by using sodium hydroxide;
2) introducing nitrogen into the reaction container for 10min to remove oxygen, and slowly adding an initiator potassium persulfate when the temperature of the reaction system rises to 70 ℃, wherein the mass of the potassium persulfate is 1.0-3.0% of the total mass of the monomers;
3) after the reaction is carried out for 4 hours, cooling the viscous liquid product to room temperature, purifying, drying and crushing the viscous liquid product by using acetone to obtain a retarder A component;
(2) preparing a retarder B component:
1) uniformly spreading natural Vermiculite (VER) as a raw material on a magnetic disc, placing the magnetic disc in a microwave oven, and treating for 1 min under the condition of microwave high fire to obtain microwave expanded vermiculite;
2) adding a certain amount of microwave expanded vermiculite powder into 2mol/L hydrochloric acid solution according to the solid-liquid mass ratio of 1: 20-25, and stirring for 2 hours at 70 ℃ in a water bath;
3) washing, filtering, drying, grinding to 200 meshes to obtain acid modified vermiculite powder, namely the retarder B component;
(3) preparing a retarder C component:
mixing sodium tartrate and citric acid in a mass ratio of 20-80: 80-20 to obtain a retarder C component;
(4) preparing a retarder:
and mixing the component A, the component B and the component C in a mass ratio of 3:1:1 to obtain the slag well cementing liquid retarder.
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