CN106632917B - Preparation method of polymer fluid loss agent for sulphoaluminate cement - Google Patents
Preparation method of polymer fluid loss agent for sulphoaluminate cement Download PDFInfo
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- CN106632917B CN106632917B CN201611203107.1A CN201611203107A CN106632917B CN 106632917 B CN106632917 B CN 106632917B CN 201611203107 A CN201611203107 A CN 201611203107A CN 106632917 B CN106632917 B CN 106632917B
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F292/00—Macromolecular compounds obtained by polymerising monomers on to inorganic materials
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B24/00—Use of organic materials as active ingredients for mortars, concrete or artificial stone, e.g. plasticisers
- C04B24/16—Sulfur-containing compounds
- C04B24/161—Macromolecular compounds comprising sulfonate or sulfate groups
- C04B24/163—Macromolecular compounds comprising sulfonate or sulfate groups obtained by reactions only involving carbon-to-carbon unsaturated bonds
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2103/00—Function or property of ingredients for mortars, concrete or artificial stone
- C04B2103/46—Water-loss or fluid-loss reducers, hygroscopic or hydrophilic agents, water retention agents
Abstract
the invention discloses a preparation method of a polymer fluid loss agent for sulphoaluminate cement, which comprises the following steps: (1) carrying out modified polymerization on the nano material to obtain a modified nano material; (2) polymerizing the modified nanometer material and the aqueous solution of the monomer. The polymer fluid loss agent for sulphoaluminate cement prepared by the invention has good stability in sulphoaluminate cement, can effectively control the water loss amount of the cement paste, and is easy to adjust the thickening time of the cement paste.
Description
Technical Field
the invention relates to the field of oil and gas well cementation, in particular to a preparation method of a polymer fluid loss agent for sulphoaluminate cement.
Background
The performance of the common silicate cement for oil and gas well cementing construction can meet the requirements of common cementing construction, but the common silicate cement cannot meet the use requirements of special oil and gas well cementing such as superficial layer surface well cementing, thickened oil thermal recovery and the like due to the low-temperature hydration speed, slow development of early strength and the like. In recent years, the research and production of sulphoaluminate cement in China are greatly advanced, and the sulphoaluminate cement has the outstanding advantages of early strength, high strength, frost resistance, impermeability, corrosion resistance, low alkali and the like, and shows a very optimistic development prospect. Sulphoaluminate cement slurry systems are also gradually accepted by the well cementing industry of oil and gas wells. Because the sulphoaluminate cement has a fast hydration speed even at low temperature, in order to ensure the safety of well cementation construction and improve the well cementation quality, the thickening time and the water loss amount of the sulphoaluminate cement are strictly controlled, but the commonly used oil well cement (portland cement) water loss reducing agent has very thin slurry in the system, causes certain risk to the construction slurry preparation, has poor stability of the cement slurry and is difficult to control the density, so the water loss reducing agent specially used for the sulphoaluminate cement needs to be developed.
Disclosure of Invention
in view of the above, the invention provides a preparation method of a polymer fluid loss agent for sulphoaluminate cement, which has good stability in sulphoaluminate cement, can effectively control the water loss amount of the cement, and is easy to adjust the thickening time of the cement.
the invention is realized by the following technical scheme:
a preparation method of a polymer fluid loss agent for sulphoaluminate cement comprises the following steps:
(1) Carrying out modified polymerization on the nano material to obtain a modified nano material;
(2) polymerizing the modified nanometer material and the aqueous solution of the monomer.
in the step (1), the nano material is a nano silicon dioxide solution, and the modified polymerization comprises the following steps: (1-1) dropwise adding a silane coupling agent into the nano silicon dioxide solution, stirring and mixing to form a silane coupling agent/silica sol mixed system, and continuously stirring to obtain an initial silane coupling agent modified silica sol solution; (1-2) modifying the silica sol by using an initial silane coupling agent, and adjusting the pH value to 9-10 by using a sodium hydroxide solution to prepare the silane coupling agent modified silica sol, namely the modified nano material.
The preparation method of the polymer fluid loss agent for the sulphoaluminate cement comprises the following steps of (1-1): the adding amount of the silane coupling agent in the nano silicon dioxide solution is 0.5-1 wt% of the mass of the nano silicon dioxide solution.
the preparation method of the polymer fluid loss agent for the sulphoaluminate cement comprises the following steps of (1-1): in the nano-silica solution, the mass fraction of the nano-silica is 29 to 30 wt%.
The preparation method of the polymer fluid loss agent for the sulphoaluminate cement comprises the following steps (1-2): the concentration of the sodium hydroxide solution was 40 wt%.
The preparation method of the polymer fluid loss agent for the sulphoaluminate cement comprises the following steps of (2): the monomer consists of AMPS (2-acrylamido-2-methylpropanesulfonic acid), AM (acrylamide), NVP (N-vinylpyrrolidone), fumaric acid and AA (acrylic acid).
the preparation method of the polymer fluid loss agent for the sulphoaluminate cement comprises the following steps of (2): the mass ratio of each monomer to the modified nano material is as follows: AMPS (2-acrylamido-2-methylpropanesulfonic acid): AM (acrylamide): NVP (N-vinylpyrrolidone): fumaric acid: AA (acrylic acid): modified nano material is 0.4-0.6: 1.3-1.5: 0.1-0.4: 0.1: 0.3-0.5: (5-6).
In the step (2), the polymerization of the modified nano material and the aqueous solution of the monomer comprises the following steps:
(2-1) sequentially adding distilled water, AMPS (2-acrylamido-2-methylpropanesulfonic acid), AM (acrylamide), fumaric acid, NVP (N-vinyl pyrrolidone) and AA (acrylic acid) into a reaction vessel under the condition of stirring to prepare a monomer solution with the mass fraction of the monomer of 25-35 wt%;
(2-2) adjusting the pH value of the monomer solution to 5-6 by using a sodium hydroxide solution with the mass fraction of 40wt% of sodium hydroxide;
(2-3) adding a silane coupling agent modified silica sol solution, heating the materials to 50-60 ℃, adding an ammonium persulfate solution, stirring for 3 minutes, adding a sodium sulfite solution, stirring for 3 minutes, standing, and waiting for initiation of polymerization;
And (2-4) starting stirring when the temperature of the materials rises to 75 ℃, controlling the reaction temperature to be below 100 ℃, keeping the temperature to 80-90 ℃ when the reaction temperature does not rise any more, and continuing the reaction until the self-adding ammonium persulfate solution is full of 1 hour, thus obtaining the polymer fluid loss agent for the sulphoaluminate.
in the preparation method of the polymer fluid loss agent for the sulphoaluminate cement, ammonium persulfate accounts for 0.5-1 wt% of the total mass of the monomers, and sodium sulfite accounts for 0.5 wt% of the mass of the ammonium persulfate.
The invention has the beneficial effects that: the polymer fluid loss agent for sulphoaluminate cement prepared by the method is stable and does not delaminate (after a test is carried out on a centrifugal machine, the product is still stable and uniform after being kept for 60 minutes at 40000r/min, and if the nano-silica is not subjected to the test on the centrifugal machine, delamination can occur within 15 minutes at 40000 r/min), and the polymer fluid loss agent is suitable for various sulphoaluminate cements. The stability of the cement slurry in sulphoaluminate cement slurry is good, the water loss of the cement slurry can be effectively controlled, and the thickening time of the cement slurry is easy to adjust.
The sulphoaluminate cement fluid loss agent prepared by the invention can effectively control the water loss to be less than 50mL in sulphoaluminate, does not influence other properties of the sulphoaluminate cement slurry, has good compatibility with other additives, can effectively control the water loss in the silicate cement slurry, and can be widely applied to cement slurry systems for oil and gas field exploitation.
Drawings
Figure 1 results of thickening time testing.
Detailed Description
for the purpose of illustrating the invention in detail, preferred embodiments are given below with reference to the accompanying drawings.
example 1
A preparation method of a polymer fluid loss agent for sulphoaluminate cement comprises the following steps:
(1) carrying out modified polymerization on the nano material to obtain a modified nano material;
The nano material is nano silicon dioxide solution, and the modification polymerization comprises the following steps: (1-1) dropwise adding 2.4 kg of silane coupling agent into 477.6 kg of nano-silica solution, wherein the mass fraction of nano-silica in the nano-silica solution is 29wt%, the adding amount of the silane coupling agent in the nano-silica solution is 0.5-1 wt% of the mass of the nano-silica solution, stirring and mixing for 30 minutes to form a silane coupling agent/silica sol mixed system, and continuously stirring to obtain initial silane coupling agent modified silica sol; (1-2) adjusting the pH of the initial silane coupling agent modified silica sol to 10 by using a sodium hydroxide solution, wherein the concentration of the sodium hydroxide solution is 40wt%, and preparing the silane coupling agent modified silica sol solution, namely the modified nano material.
(2) Polymerizing the modified nanometer material and the aqueous solution of the monomer.
(2-1) stirring was started at 900 rpm, and 400 kg of distilled water, 40 kg of AMPS (2-acrylamido-2-methylpropanesulfonic acid), 120 kg of AM (acrylamide), 8 kg of fumaric acid, 16 kg of NVP (N-vinylpyrrolidone) and 32 kg of AA (acrylic acid) were sequentially charged into the reaction vessel to prepare a monomer solution having a monomer mass fraction of 35%.
(2-2) adjusting the pH value of the monomer solution to 5.5 by using 120 kg of a sodium hydroxide solution with the mass fraction of 40wt% of sodium hydroxide;
(2-3) adding 480 kg of silane coupling agent modified silica sol solution, heating the materials to 60 ℃, keeping the temperature for 3 minutes, adding an ammonium persulfate solution (2kg of ammonium persulfate +10 distilled water) into the mixture, stirring the mixture for 3 minutes, adding a sodium sulfite solution (1kg of sodium sulfite +10 distilled water) into the mixture, stirring the mixture for 3 minutes, standing the mixture, and waiting for initiation of polymerization;
(2-4) starting stirring until the material temperature rises to 75 ℃ until the stirring is carried out till 1200 revolutions per minute, controlling the reaction temperature to be below 100 ℃, keeping the temperature to 80-90 ℃ when the reaction temperature does not rise any more, and continuing the reaction until the ammonium persulfate solution is added for 1 hour, thus obtaining the polymer fluid loss agent for the sulphoaluminate. Ammonium persulfate accounts for 0.5-1 wt% of the total mass of the monomers, and sodium sulfite accounts for 0.5 wt% of the mass of the ammonium persulfate.
example 2
A preparation method of a polymer fluid loss agent for sulphoaluminate cement comprises the following steps:
(1) Carrying out modified polymerization on the nano material to obtain a modified nano material;
The nano material is nano silicon dioxide solution, and the modification polymerization comprises the following steps: (1-1) dropwise adding 2.4 kg of silane coupling agent into 477.6 kg of nano-silica solution, wherein the mass fraction of nano-silica in the nano-silica solution is 30 wt%, the adding amount of the silane coupling agent in the nano-silica solution is 0.5-1 wt% of the mass of the nano-silica solution, stirring and mixing for 30 minutes to form a silane coupling agent/silica sol mixed system, and continuously stirring to obtain initial silane coupling agent modified silica sol; (1-2) adjusting the pH of the initial silane coupling agent modified silica sol to 10 by using a sodium hydroxide solution, wherein the concentration of the sodium hydroxide solution is 40wt%, and preparing the silane coupling agent modified silica sol solution, namely the modified nano material.
(2) polymerizing the modified nanometer material and the aqueous solution of the monomer.
(2-1) stirring was started at 900 rpm, and 540 kg of distilled water, 40 kg of AMPS (2-acrylamido-2-methylpropanesulfonic acid), 120 kg of AM (acrylamide), 8 kg of fumaric acid, 16 kg of NVP (N-vinylpyrrolidone) and 32 kg of AA (acrylic acid) were sequentially charged into the reaction vessel to prepare a monomer solution having a monomer mass fraction of 29%.
(2-2) adjusting the pH value of the monomer solution to 5.5 by using 120 kg of a sodium hydroxide solution with the mass fraction of 40wt% of sodium hydroxide;
(2-3) adding 480 kg of silane coupling agent modified silica sol solution, heating the materials to 60 ℃, keeping the temperature for 3 minutes, adding ammonium persulfate solution (2kg of ammonium sulfate +10 distilled water) into the mixture, stirring the mixture for 3 minutes, adding sodium sulfite solution (1kg of sodium sulfite +10 distilled water) into the mixture, stirring the mixture for 3 minutes, standing the mixture, and waiting for initiation of polymerization;
(2-4) starting stirring until the material temperature rises to 75 ℃ until the stirring is carried out till 1200 revolutions per minute, controlling the reaction temperature to be below 100 ℃, keeping the temperature to 80-90 ℃ when the reaction temperature does not rise any more, and continuing the reaction until the ammonium persulfate solution is added for 1 hour, thus obtaining the polymer fluid loss agent for the sulphoaluminate. Ammonium persulfate accounts for 0.5-1 wt% of the total mass of the monomers, and sodium sulfite accounts for 0.5 wt% of the mass of the ammonium persulfate.
The monomer concentration of example 2 was lower than that of example 1, and the same amount lost water was greater than that of example 1 (the amount lost water was 46mL in example 2), but still less than 50 mL.
the experimental data for the polymer fluid loss additive for sulphoaluminate cement prepared in example 1 are as follows:
1. The results of the test in a sulphoaluminate slurry with a density of 1.9g/cm3 (80 ℃) are shown in Table 1:
TABLE 1
| Cement | Rheology of | Water loss/mL |
| Tangshan sulphoaluminate cement | -/170/116/59/3/1 | 20 |
| Zhengzhou sulphoaluminate cement | 280/149/103/54/3/1 | 34 |
| Jianai sulphoaluminate cement | -/213/150/80/4/3 | 22 |
| Tianjin sulphoaluminate cement | 246/130/90/46/2/1 | 28 |
The formula of the sulphoaluminate cement slurry comprises the following components: 600g cement +30g fluid loss additive +10.2g retarder (retarder known in the art) +225g tap water.
2. Test results in the System
2.1 Cement paste formula
The suspending agent WH-2 is a product publicly sold on the market by the applicant of the present application before the filing date.
2.2, rheological data:
| Φ600 | Φ300 | Φ200 | Φ100 | Φ6 | Φ3 |
| - | 271 | 190 | 100 | 8 | 5 |
| - | 268 | 186 | 94 | 7 | 4 |
2.3, loss of water in API: 30 mL.
2.4, thickening time [ see fig. 1 ]: 154.1 min. As can be seen from fig. 1: the initial consistency is 9Bc, and the requirement that the row standard is lower than 30Bc is met; the thickening curve has a sudden change value of 0, meets the requirement that the row mark is lower than 10, and shows that the slurry is very stable; transition time: close to right-angle thickening, and meets the requirement that the row mark is less than 40 min.
2.5 and 24h compressive strength: 43 MPa.
The above examples are provided for clarity of illustration only and are not intended to limit the invention to the particular embodiments described. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. Any obvious variations or modifications which come within the spirit and scope of the invention are desired to be protected by the following claims.
Claims (1)
1. A preparation method of a polymer fluid loss agent for sulphoaluminate cement is characterized by comprising the following steps:
(1) carrying out modified polymerization on the nano material to obtain a modified nano material;
(2) Polymerizing the modified nano material with the aqueous solution of the monomer;
in the step (1), the nano material is a nano silicon dioxide solution, and the modified polymerization comprises the following steps: (1-1) dropwise adding 2.4 kg of silane coupling agent into 477.6 kg of nano-silica solution, wherein the mass fraction of nano-silica in the nano-silica solution is 29wt%, the adding amount of the silane coupling agent in the nano-silica solution is 0.5-1 wt% of the mass of the nano-silica solution, stirring and mixing for 30 minutes to form a silane coupling agent/silica sol mixed system, and continuously stirring to obtain initial silane coupling agent modified silica sol; (1-2) adjusting the pH of the initial silane coupling agent modified silica sol to 10 by using a sodium hydroxide solution, wherein the concentration of the sodium hydroxide solution is 40wt%, and preparing a silane coupling agent modified silica sol solution, namely the modified nano material;
In step (2):
(2-1) starting stirring at 900 rpm, and sequentially adding 400 kg of distilled water, 40 kg of 2-acrylamido-2-methylpropanesulfonic Acid (AMPS), 120 kg of Acrylamide (AM), 8 kg of fumaric acid, 16 kg of N-vinyl pyrrolidone (NVP) and 32 kg of Acrylic Acid (AA) into a reaction vessel to prepare a monomer solution with the monomer mass fraction of 35%;
(2-2) adjusting the pH value of the monomer solution to 5.5 by using 120 kg of a sodium hydroxide solution with the mass fraction of 40wt% of sodium hydroxide;
(2-3) adding 480 kg of silane coupling agent modified silica sol solution, heating the materials to 60 ℃, keeping the temperature for 3 minutes, adding ammonium persulfate solution into the mixture, stirring the mixture for 3 minutes, adding sodium sulfite solution into the mixture, stirring the mixture for 3 minutes, standing the mixture, and waiting for initiation of polymerization;
(2-4) starting stirring until the material temperature rises to 75 ℃ until the stirring is carried out till 1200 revolutions per minute, controlling the reaction temperature to be below 100 ℃, keeping the temperature to 80-90 ℃ when the reaction temperature does not rise any more, and continuing the reaction until the ammonium persulfate solution is added for 1 hour, thus obtaining the polymer fluid loss agent for the sulphoaluminate; the ammonium persulfate solution was prepared from 2kg of ammonium persulfate and 10 kg of distilled water, and the sodium sulfite solution was prepared from 1kg of sodium sulfite and 10 kg of distilled water.
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| CN109503782A (en) * | 2017-09-14 | 2019-03-22 | 中石化石油工程技术服务有限公司 | A kind of inorganic-organic polymer oil-well cement filtrate reducer, preparation method and application |
| CN109265064B (en) * | 2018-09-28 | 2021-04-20 | 镇江苏博特新材料有限公司 | Preparation method of high-strength alkali-free chlorine-free accelerator |
| CN114163587B (en) * | 2021-11-30 | 2024-01-23 | 中国石油天然气集团有限公司 | Nano silicon dioxide grafted polymer, preparation method and application thereof, and filtrate reducer |
| CN114736339B (en) * | 2022-05-21 | 2024-03-12 | 库尔勒明洋工贸有限责任公司 | Method for synthesizing residual monomer-free filtrate reducer and filtrate reducer prepared by same |
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| CA1162951A (en) * | 1980-07-31 | 1984-02-28 | Arnold M. Rosenberg | Cement superplasticizer |
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