CN111732689A - Expansion type fluid loss agent and preparation method thereof - Google Patents
Expansion type fluid loss agent and preparation method thereof Download PDFInfo
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- CN111732689A CN111732689A CN202010624432.5A CN202010624432A CN111732689A CN 111732689 A CN111732689 A CN 111732689A CN 202010624432 A CN202010624432 A CN 202010624432A CN 111732689 A CN111732689 A CN 111732689A
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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
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/52—Amides or imides
- C08F220/54—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide
- C08F220/58—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide containing oxygen in addition to the carbonamido oxygen, e.g. N-methylolacrylamide, N-(meth)acryloylmorpholine
- C08F220/585—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide containing oxygen in addition to the carbonamido oxygen, e.g. N-methylolacrylamide, N-(meth)acryloylmorpholine and containing other heteroatoms, e.g. 2-acrylamido-2-methylpropane sulfonic acid [AMPS]
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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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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/42—Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells
- C09K8/46—Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells containing inorganic binders, e.g. Portland cement
- C09K8/467—Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells containing inorganic binders, e.g. Portland cement containing additives for specific purposes
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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
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Abstract
The invention discloses an intumescent fluid loss agent, which is prepared from the following raw materials in parts by weight: 20-40 parts of 2-acrylamide-2-methylpropanesulfonic acid, 3-13 parts of acrylamide, 1-5 parts of acrylic acid, 2-13 parts of ethylene glycol, 2-13 parts of N-vinyl pyrrolidone, 0.1-0.5 part of initiator and 70-110 parts of water. Also provides a corresponding preparation method. According to the invention, the fluid loss agent prepared by graft copolymerization of monomers such as 2-acrylamide-2-methylpropanesulfonic acid, acrylamide and acrylic acid with N-vinyl pyrrolidone and ethylene glycol is added into a cement paste system, so that the 48h relative expansion rate is 0.4-3.2%, and the water loss amount is controlled within 50ml, therefore, the fluid loss agent disclosed by the invention not only can well control the water loss amount of the cement paste system, but also improves the expansibility of the cement paste, the performance of the fluid loss agent is far superior to that of the fluid loss agent in the common market, and the well cementation cost is reduced; the fluid loss agent has the advantages of easily available raw materials, simple synthesis and easy popularization and use.
Description
Technical Field
The invention relates to the technical field of oil and gas exploitation well cementation cement slurry.
Background
At present, with the continuous reduction of petroleum reserves and the deep development of exploitation technologies, the number of deep wells and ultra-deep wells is continuously increased, the difficulty of well cementation is increased, and various yield-increasing processes, measures and later-period operations also put higher requirements on the well cementation quality of oil and gas wells. In some subsequent operations after cementing is completed, such as: the perforation, the fracturing and the acidification all have influence on the set cement, and the main reason of the theoretical analysis is that the set cement deformation capability of the existing cement paste system is insufficient. In the hydration, setting and hardening process of ordinary Portland oil well cement, the problems of high water loss and self shrinkage exist, so that the cementing quality between a cement sheath and a stratum casing is poor, and the cementing quality is influenced.
Water loss reducing agent
When cement slurry is injected into an annular space between the casing and the well wall, under the action of pressure, liquid phase in the cement slurry can seep into a stratum, and a cement filter cake can be formed on the well wall due to the loss of the liquid phase, so that the annular space is reduced, and the possibility of well injection failure can be increased due to the increase of the circulating friction resistance. The percolated liquid phase will enter the formation and the cement slurry will become unpumpable causing formation contamination. The second stage in the cement slurry water loss process is the main stage in the formation of cement filter cake.
Therefore, a fluid loss additive needs to be added into the cement paste to solve the problem of filtrate percolation leakage. Fluid loss additives to cement slurry systems typically control water loss by two actions: firstly, through the permeability that reduces cement filter cake, prevent that cement slurry liquid from permeating the stratum under the pressure differential effect, cause the injury to the reservoir. And secondly, the resistance of the liquid phase in the cement paste to the stratum permeation is improved by increasing the viscosity of the cement paste, so that the water loss is reduced. Therefore, the effect of the fluid loss agent is obvious and can not be ignored.
Since the last century, a plurality of series products of oil well cement fluid loss additives have been formed, and can be generally divided into the following two categories: the water-soluble polymer material comprises a modified natural product and a polymer material. The synthesized polymer fluid loss agent has various varieties and excellent performance, and is the most widely applied fluid loss agent at present.
Second, swelling agent
In the process of setting cement paste, the internal structural force is continuously enhanced, the gel strength with the well wall and the casing is continuously increased, the weight of a cement sheath is gradually suspended on the casing and the well wall, and the pressure on the stratum is reduced; due to hydration, in the process of setting cement paste, the inside of a cement stone matrix shrinks to form micro gaps, the appearance volume also shrinks to a certain extent, the control effect on the pore pressure is reduced, the shrinkage rate of common cement in initial setting is 0.1-0.5%, and the shrinkage rate in final setting is more than 2%; the separation of free water in the cement paste reduces the pressure on the stratum.
The expanding agent is added into a cement paste system to realize the stable volume expansion in different hydration stages (the later stage of plastic state saturated solidification) of cement, thereby improving the pressure of a cement paste column on a gas layer, ensuring that the cement paste column has good applicability, compatibility and harmony of expansion time, and improving the gas channeling resistance and the cementation quality when being applied to the process of deep oil gas well cementation.
Therefore, the existing fluid loss agent and the existing expanding agent respectively have the function of singly controlling the water loss and the expansion performance of cement slurry, and the well cementation cost is increased.
Disclosure of Invention
The invention aims to provide an intumescent fluid loss agent, and simultaneously provides a corresponding preparation method thereof, which is another aim of the invention.
Based on the purpose, the invention adopts the following technical scheme:
an expansion type fluid loss agent is prepared from the following raw materials in parts by weight: 20-40 parts of 2-acrylamide-2-methylpropanesulfonic acid, 3-13 parts of acrylamide, 1-5 parts of acrylic acid, 2-13 parts of ethylene glycol, 2-13 parts of N-vinyl pyrrolidone, 0.1-0.5 part of initiator and 70-110 parts of water.
An expansion type fluid loss agent is prepared from the following raw materials in parts by weight: 25-35 parts of 2-acrylamide-2-methylpropanesulfonic acid, 5-10 parts of acrylamide, 2-3 parts of acrylic acid, 5-10 parts of ethylene glycol, 5-10 parts of N-vinyl pyrrolidone, 0.2-0.4 part of initiator and 80-100 parts of water.
An expansion type fluid loss agent is prepared from the following raw materials in parts by weight: 26 parts of 2-acrylamide-2-methylpropanesulfonic acid, 7 parts of acrylamide, 2 parts of acrylic acid, 6 parts of ethylene glycol, 6 parts of N-vinyl pyrrolidone, 0.2 part of an initiator and 98 parts of water.
The initiator is ammonium persulfate; the water is deionized water.
A method of preparing an intumescent fluid loss additive comprising the steps of:
1) preparing an initiator solution from 8-9 parts of water and an initiator;
2) adding the rest water into a reactor, and sequentially adding 2-acrylamide-2-methylpropanesulfonic acid, acrylamide, acrylic acid, ethylene glycol and N-vinyl pyrrolidone under the stirring condition to obtain a mixed solution;
3) controlling the temperature of the mixed solution in the step 2) to be 10-50 ℃, adjusting the pH value of the mixed solution in the step 2) to be 5-6 by adopting an alkaline solution, adding the initiator solution in the step 1), carrying out polymerization reaction for 1-3h at the temperature of 80-85 ℃, cooling to room temperature, and discharging.
In the step 3), the alkaline solution is a sodium hydroxide solution with the mass fraction of 25-30%.
Compared with the prior art, the invention has the following beneficial effects:
1) according to the invention, the fluid loss agent prepared by graft copolymerization of monomers such as 2-acrylamide-2-methylpropanesulfonic acid, acrylamide and acrylic acid with N-vinyl pyrrolidone and ethylene glycol is added into a cement paste system, so that the 48h relative expansion rate is 0.4-3.2%, and the water loss amount is controlled within 50ml, therefore, the fluid loss agent disclosed by the invention not only can well control the water loss amount of the cement paste system, but also improves the expansibility of the cement paste, the performance of the fluid loss agent is far superior to that of the fluid loss agent in the common market, and the well cementation cost is reduced;
2) the fluid loss agent has the advantages of easily available raw materials, simple synthesis and easy popularization and use.
Detailed Description
Example 1
An expansion type fluid loss agent is prepared from the following raw materials in parts by weight: 26 parts of 2-acrylamide-2-methylpropanesulfonic acid, 7 parts of acrylamide, 2 parts of acrylic acid, 6 parts of ethylene glycol, 6 parts of N-vinyl pyrrolidone, 0.2 part of ammonium persulfate and 98 parts of deionized water.
A method of preparing an intumescent fluid loss additive comprising the steps of:
1) preparing an initiator solution from the initiator and 8 parts of deionized water;
2) putting 90 parts of deionized water into a reactor, and sequentially adding 2-acrylamide-2-methylpropanesulfonic acid, acrylamide, acrylic acid, ethylene glycol and N-vinyl pyrrolidone at a stirring speed of 200r/min to obtain a mixed solution;
3) controlling the temperature of the mixed solution in the step 2) to be 30 ℃, adjusting the pH value of the mixed solution in the step 2) to be 5-6 by adopting a sodium hydroxide solution with the mass fraction of 30%, adding the initiator solution in the step 1), carrying out polymerization reaction for 2h at the temperature of 80 ℃, cooling to room temperature, and discharging.
Example 2
An expansion type fluid loss agent is prepared from the following raw materials in parts by weight: 25 parts of 2-acrylamide-2-methylpropanesulfonic acid, 6 parts of acrylamide, 2 parts of acrylic acid, 8 parts of ethylene glycol, 6 parts of N-vinyl pyrrolidone, 0.3 part of ammonium persulfate and 100 parts of deionized water.
A method of preparing an intumescent fluid loss additive comprising the steps of:
1) preparing an initiator solution from the initiator and 10 parts of deionized water;
2) adding 90 parts of deionized water into a reactor, and sequentially adding 2-acrylamide-2-methylpropanesulfonic acid, acrylamide, acrylic acid, ethylene glycol and N-vinyl pyrrolidone at a stirring speed of 100r/min to obtain a mixed solution;
3) controlling the temperature of the mixed solution in the step 2) to be 45 ℃, adjusting the pH value of the mixed solution in the step 2) to be 5-6 by adopting a sodium hydroxide solution with the mass fraction of 30%, adding the initiator solution in the step 1), carrying out polymerization reaction for 2h at 82 ℃, cooling to room temperature, and discharging.
Example 3
An expansion type fluid loss agent is prepared from the following raw materials in parts by weight: 35 parts of 2-acrylamide-2-methylpropanesulfonic acid, 10 parts of acrylamide, 3 parts of acrylic acid, 10 parts of ethylene glycol, 9 parts of N-vinyl pyrrolidone, 0.4 part of ammonium persulfate and 90 parts of deionized water.
The process for the preparation of the intumescent fluid loss additive is referred to example 1.
Example 4
An expansion type fluid loss agent is prepared from the following raw materials in parts by weight: 30 parts of 2-acrylamide-2-methylpropanesulfonic acid, 5 parts of acrylamide, 3 parts of acrylic acid, 5 parts of ethylene glycol, 10 parts of N-vinyl pyrrolidone, 0.4 part of ammonium persulfate and 80 parts of deionized water.
The process for the preparation of the intumescent fluid loss additive is referred to example 1.
Example 5
An expansion type fluid loss agent is prepared from the following raw materials in parts by weight: 20 parts of 2-acrylamide-2-methylpropanesulfonic acid, 3 parts of acrylamide, 5 parts of acrylic acid, 2 parts of ethylene glycol, 2 parts of N-vinyl pyrrolidone, 0.1 part of ammonium persulfate and 70 parts of deionized water.
The process for the preparation of the intumescent fluid loss additive is referred to example 1.
Example 6
An expansion type fluid loss agent is prepared from the following raw materials in parts by weight: 40 parts of 2-acrylamide-2-methylpropanesulfonic acid, 13 parts of acrylamide, 1 part of acrylic acid, 13 parts of ethylene glycol, 13 parts of N-vinyl pyrrolidone, 0.5 part of ammonium persulfate and 110 parts of deionized water.
The process for the preparation of the intumescent fluid loss additive is referred to example 2.
Example 7 evaluation of Properties
Physical and chemical indexes of the fluid loss additive prepared in the examples 1 to 6 and the cement paste performance of the fluid loss additive are tested according to API specification 10A oil well cement specification, and compared with the common fluid loss additive on the market, the performance evaluation of the fluid loss additive is carried out according to the part 2 of the evaluation method of the oil well cement additive of the national standard SY/T5504.2-2013: carrying out related experiments by using the fluid loss agent reducing method; evaluation of expansion Properties reference was made to SY/T5504.8-2013 oil well cement admixture evaluation method part 8: swelling agents relevant experiments were performed. The evaluation results are shown in table 1 below.
The formula of the cement paste is as follows: the addition ratio of the fluid loss additive of the G-grade oil well cement is 4 percent (BWOC), the water cement ratio is 0.44, and the cement paste density is 1.90G/cm3And mixing the slurry with distilled water.
As can be seen from Table 1, the transition time of the fluid loss agent cement slurry system is 6 min, the compressive strength is 28.2Mpa, the water loss is 26 ml, and the relative expansion rate of 48h is 1.2%; the transition time of the common filtrate reducer sold in the market is 24 min, the compressive strength is 21.8 Mpa, the water loss is 35 ml, and the relative expansion rate is-0.6% in 48 h. Therefore, the water loss, expansion rate and other performances of the water loss reducing agent cement paste system are superior to those of a commercially available common water loss reducing agent cement paste system and a detection performance standard. The compressive strength is higher than that of the common commercial fluid loss additive, which shows that the fluid loss additive has stronger dispersion effect on cement paste, so that the cement paste is uniformly dispersed, and the strength is increased. The fluid loss agent of the invention not only can well control the water loss amount of a cement paste system, but also improves the expansibility of cement paste, has performance far superior to that of the fluid loss agent in the common market, and reduces the well cementation cost.
Claims (6)
1. The intumescent fluid loss agent is characterized by being prepared from the following raw materials in parts by weight: 20-40 parts of 2-acrylamide-2-methylpropanesulfonic acid, 3-13 parts of acrylamide, 1-5 parts of acrylic acid, 2-13 parts of ethylene glycol, 2-13 parts of N-vinyl pyrrolidone, 0.1-0.5 part of initiator and 70-110 parts of water.
2. The intumescent fluid loss additive of claim 1, prepared from the following raw materials in parts by weight: 25-35 parts of 2-acrylamide-2-methylpropanesulfonic acid, 5-10 parts of acrylamide, 2-3 parts of acrylic acid, 5-10 parts of ethylene glycol, 5-10 parts of N-vinyl pyrrolidone, 0.2-0.4 part of initiator and 80-100 parts of water.
3. The intumescent fluid loss additive of claim 2, prepared from the following raw materials in parts by weight: 26 parts of 2-acrylamide-2-methylpropanesulfonic acid, 7 parts of acrylamide, 2 parts of acrylic acid, 6 parts of ethylene glycol, 6 parts of N-vinyl pyrrolidone, 0.2 part of an initiator and 98 parts of water.
4. The intumescent fluid loss additive of any of claims 1 to 3 wherein the initiator is ammonium persulfate; the water is deionized water.
5. A process for the preparation of the intumescent fluid loss agent of claim 4 comprising the steps of:
1) preparing an initiator solution from 8-9 parts of water and an initiator;
2) adding the rest water into a reactor, and sequentially adding 2-acrylamide-2-methylpropanesulfonic acid, acrylamide, acrylic acid, ethylene glycol and N-vinyl pyrrolidone under the stirring condition to obtain a mixed solution;
3) controlling the temperature of the mixed solution in the step 2) to be 10-50 ℃, adjusting the pH value of the mixed solution in the step 2) to be 5-6 by adopting an alkaline solution, adding the initiator solution in the step 1), carrying out polymerization reaction for 1-3h at the temperature of 80-85 ℃, cooling to room temperature, and discharging.
6. The process for the preparation of intumescent fluid loss additive of claim 5 wherein the alkaline solution in step 3) is a 25-30% by weight sodium hydroxide solution.
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN113087841A (en) * | 2021-05-14 | 2021-07-09 | 淄博锐捷新技术开发有限公司 | Anti-freezing type temperature-resistant salt-resistant fluid loss agent and preparation method thereof |
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WO2010112866A1 (en) * | 2009-04-03 | 2010-10-07 | Halliburton Energy Services, Inc. | Methods of using fluid loss additives comprising micro gels |
CN103509199A (en) * | 2012-06-26 | 2014-01-15 | 中国石油化工股份有限公司 | Polymer swelling particles for drilling fluid and preparation method thereof |
CN106543984A (en) * | 2016-10-21 | 2017-03-29 | 中国石油集团川庆钻探工程有限公司长庆固井公司 | A kind of oil well cement swelling agent and preparation method thereof |
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Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
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WO2010112866A1 (en) * | 2009-04-03 | 2010-10-07 | Halliburton Energy Services, Inc. | Methods of using fluid loss additives comprising micro gels |
CN103509199A (en) * | 2012-06-26 | 2014-01-15 | 中国石油化工股份有限公司 | Polymer swelling particles for drilling fluid and preparation method thereof |
CN106543984A (en) * | 2016-10-21 | 2017-03-29 | 中国石油集团川庆钻探工程有限公司长庆固井公司 | A kind of oil well cement swelling agent and preparation method thereof |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN113087841A (en) * | 2021-05-14 | 2021-07-09 | 淄博锐捷新技术开发有限公司 | Anti-freezing type temperature-resistant salt-resistant fluid loss agent and preparation method thereof |
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