CN111171226B - Preparation method of water-soluble filtrate reducer for drilling fluid and drilling fluid - Google Patents

Preparation method of water-soluble filtrate reducer for drilling fluid and drilling fluid Download PDF

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CN111171226B
CN111171226B CN201811338548.1A CN201811338548A CN111171226B CN 111171226 B CN111171226 B CN 111171226B CN 201811338548 A CN201811338548 A CN 201811338548A CN 111171226 B CN111171226 B CN 111171226B
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chain transfer
drilling fluid
water
transfer agent
agent
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CN111171226A (en
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苏雪霞
孙举
王中华
王旭
徐生婧
胡晓燕
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Sinopec Oilfield Service Corp
Sinopec Zhongyuan Petroleum Engineering Co Ltd
Drilling Engineering Technology Research Institute of Sinopec Zhongyuan Petroleum Engineering Co Ltd
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Sinopec Oilfield Service Corp
Sinopec Zhongyuan Petroleum Engineering Co Ltd
Drilling Engineering Technology Research Institute of Sinopec Zhongyuan Petroleum Engineering Co Ltd
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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
    • C08F220/56—Acrylamide; Methacrylamide
    • 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
    • C08F2/00—Processes of polymerisation
    • C08F2/38—Polymerisation using regulators, e.g. chain terminating agents, e.g. telomerisation
    • 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
    • C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
    • C08F283/06—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals
    • C08F283/065—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals on to unsaturated polyethers, polyoxymethylenes or polyacetals
    • C—CHEMISTRY; METALLURGY
    • 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
    • C09K8/02—Well-drilling compositions
    • C09K8/03—Specific additives for general use in well-drilling compositions
    • C09K8/035—Organic additives
    • C—CHEMISTRY; METALLURGY
    • 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
    • C09K8/02—Well-drilling compositions
    • C09K8/04—Aqueous well-drilling compositions
    • C09K8/14—Clay-containing compositions
    • C09K8/18—Clay-containing compositions characterised by the organic compounds
    • C09K8/22—Synthetic organic compounds
    • C09K8/24—Polymers
    • 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
    • C08F2438/00—Living radical polymerisation
    • C08F2438/03—Use of a di- or tri-thiocarbonylthio compound, e.g. di- or tri-thioester, di- or tri-thiocarbamate, or a xanthate as chain transfer agent, e.g . Reversible Addition Fragmentation chain Transfer [RAFT] or Macromolecular Design via Interchange of Xanthates [MADIX]

Abstract

The invention provides a preparation method of a water-soluble filtrate reducer for drilling fluid, which comprises the following steps: reacting a branching agent with a macromolecular chain transfer agent to obtain a water-soluble filtrate reducer for drilling fluid; the branching agent is prepared from materials comprising acrylamide monomers and a branching agent; the macromolecular chain transfer agent is prepared from materials including an acrylamide monomer, an RAFT chain transfer agent and an organic acid monomer. The method provided by the invention adopts a reversible addition-fragmentation chain transfer polymerization method, adopts a semi-continuous polymerization process, uses a diene monomer and a low-proportion chain transfer agent, and is prepared in an aqueous solution or buffer solution system, the polymerization reaction is easy to control, the reaction temperature is stable, the obtained product has good temperature resistance and low viscosity effect, and the technical problems of large viscosity effect of high-temperature and high-density drilling fluid, limited addition of a treating agent and difficulty in considering both rheological property and suspensibility are met. The invention also provides a drilling fluid.

Description

Preparation method of water-soluble filtrate reducer for drilling fluid and drilling fluid
Technical Field
The invention relates to the technical field of filtrate reducer, in particular to a preparation method of a water-soluble filtrate reducer for drilling fluid and the drilling fluid.
Background
The polymer fluid loss additive for drilling fluid is an additive with the largest dosage in a drilling auxiliary agent, the widely used fluid loss additive at present mainly comprises 2-acrylamide-2-methylpropanesulfonic acid, acrylamide, N-vinylacetamide, N-vinyl pyrrolidone, disubstituted amide and water-soluble copolymers thereof, the fluid loss additive mainly has a linear structure, and has the defects of large viscosity effect, easy breakage at high temperature and weak degradation resistance although having certain high temperature resistance, and the cost of the used monomer is higher.
Therefore, it is an urgent problem to be solved by those skilled in the art to provide a fluid loss additive with good temperature resistance and low viscosity effect.
Disclosure of Invention
In view of the above, the invention aims to provide a water-soluble filtrate reducer for drilling fluid, which has good temperature resistance, low viscosity effect, good rheological property and good suspension stability.
The invention provides a preparation method of a water-soluble filtrate reducer for drilling fluid, which comprises the following steps:
reacting the branching agent with the macromolecular chain transfer agent to obtain the water-soluble filtrate reducer for the drilling fluid.
In the present invention, the preparation method of the branching agent is preferably:
the acrylamide monomer and branching agent are dissolved in a polar solvent to provide the branching agent.
In the present invention, the polar solvent used to prepare the branching agent is identified as the first polar solvent; the acrylamide monomer used to prepare the branching agent was designated as the first acrylamide monomer.
In the present invention, the mass of the first acrylamide monomer is preferably 15 to 30%, and more preferably 20 to 25% of the mass of the first polar solvent.
In the present invention, the branching agent is preferably a diene-based compound or a polyene-based compound, more preferably N, N-methylene bisacrylamide or polyethylene glycol dimethacrylate.
In the present invention, the branching agent is preferably 0.1 to 1% by mass, more preferably 0.2 to 0.8% by mass, most preferably 0.3 to 0.6% by mass of the acrylamide monomer.
In the present invention, the first polar solvent is preferably water or a buffer solution; the buffer solution is preferably a buffer solution formed by acetic acid and sodium acetate.
In the present invention, oxygen removal is preferably performed after the first acrylamide monomer and the branching agent are dissolved in the first polar solvent. In the invention, the method for removing oxygen is preferably to remove oxygen by introducing nitrogen, and the time for removing oxygen is preferably 25-35 min, more preferably 28-32 min, and most preferably 30 min.
In the present invention, the preparation method of the macromolecular chain transfer agent is preferably:
dissolving an organic acid monomer in a polar solvent to obtain an organic acid monomer solution;
under the action of an initiator, carrying out polymerization reaction on an acrylamide monomer, an RAFT chain transfer agent and an organic acid monomer solution to obtain a macromolecular chain transfer agent.
In the present invention, the organic acid monomer is preferably 2-acrylamido-2-methylpropanesulfonic acid or 2-acryloyloxy-2-methylpropanesulfonic acid.
In the present invention, the polar solvent for preparing the organic acid-based monomer solution is referred to as a second polar solvent.
In the present invention, the mass of the organic acid monomer is preferably 15 to 30%, more preferably 20 to 25%, and most preferably 22 to 23% of the mass of the second polar solvent.
In the present invention, the acrylamide monomer used to prepare the macromolecular chain transfer agent is referred to as the second acrylamide monomer.
In the present invention, the mass of the second acrylamide monomer is preferably 15 to 30%, more preferably 20 to 25%, and most preferably 22 to 23% of the mass of the second polar solvent.
In the present invention, the RAFT chain transfer agent is preferably a dithio-or trithio-compound, more preferably 4-cyanovaleric acid dithiobenzoate or (3-benzylmercaptothiocarbonylthio) propionic acid.
In the present invention, the sum of the amount of the first acrylamide monomer and the amount of the second acrylamide monomer is the total amount of the acrylamide monomers. In the present invention, the amount of the first acrylamide monomer is preferably 10 to 30%, more preferably 15 to 25%, and most preferably 20% of the total amount of the acrylamide monomer.
In the present invention, the second polar solvent is preferably water or a buffer solution, and the buffer solution is preferably a buffer solution formed by acetic acid and sodium acetate.
In the present invention, the organic acid monomer is dissolved in the second polar solvent, and then the pH is preferably adjusted, and the pH is preferably adjusted to 6 to 8, more preferably 6.5 to 7.5, and most preferably 7.
According to the invention, an acrylamide monomer and an RAFT chain transfer agent are adopted to keep reversible balance in a polymerization process, so that termination reaction is inhibited, and a polymer chain keeps activity.
In the present invention, the polymerization is preferably preceded by oxygen removal of the reaction system. In the invention, the method for removing oxygen is preferably to remove oxygen by introducing nitrogen, and the time for removing oxygen is preferably 25-35 min, more preferably 28-32 min, and most preferably 30 min.
In the invention, the polymerization reaction temperature is preferably 35-60 ℃, more preferably 40-55 ℃, and most preferably 45-50 ℃; the time of the polymerization reaction is preferably 2.5 to 4 hours, and more preferably 3 to 3.5 hours.
In the invention, the initiator is a peroxy initiator or oxidation-reduction initiator suitable for a polar solvent system, and is preferably potassium persulfate, ammonium persulfate-sodium bisulfite, ammonium persulfate-sodium metabisulfite or ammonium persulfate-sodium sulfite.
In the present invention, the mass of the initiator is preferably 0.1 to 0.2%, more preferably 0.12 to 0.18%, and most preferably 0.14 to 0.16% of the total mass of the second acrylamide monomer and the organic acid monomer.
In the present invention, the molar ratio of the initiator to RAFT chain transfer agent is preferably 1: (1.1 to 1.2), more preferably 1: (1.12 to 1.18), most preferably 1: (1.14-1.16).
In the present invention, the preparation method of the macromolecular chain transfer agent is more preferably:
dissolving an organic acid monomer in a second polar solvent, and adjusting the pH value to 6-8 to obtain an organic acid monomer solution; adding a second acrylic acid monomer and an RAFT (reversible addition-fragmentation chain transfer) agent into the organic acid monomer solution, transferring the solution into a 250mL four-mouth bottle, introducing nitrogen to remove oxygen for 30min, heating the system to 35-60 ℃, adding an oxidation-reduction initiator to initiate polymerization reaction, and carrying out polymerization reaction for 2.5-4 hours to obtain the active macromolecular chain transfer agent.
In the invention, the preparation method of the water-soluble filtrate reducer for the drilling fluid is preferably as follows:
and dropwise adding the branching agent into the macromolecular chain transfer agent to form a star-shaped branching structure, continuously reacting for 3-5 hours after dropwise adding is finished, and preparing the water-soluble star-shaped polymer filtrate reducer through high conversion.
In the present invention, the branching agent is preferably the branching agent after the nitrogen-scavenging and the oxygen-scavenging. In the invention, the dripping is preferably constant speed dripping, and the dripping speed is preferably 20-50 mL/h, more preferably 30-40 mL/h, and most preferably 35 mL/h.
In the invention, the reaction temperature for preparing the water-soluble filtrate reducer for the drilling fluid is preferably 35-60 ℃, the reaction temperature for the reaction of the macromolecular chain transfer agent prepared by adopting the peroxy initiator is more preferably 35-40 ℃, and the most preferably 35 ℃; the reaction temperature of the macromolecular chain transfer agent prepared by adopting the oxidation-reduction initiator is more preferably 50-60 ℃ and most preferably 55 ℃.
The invention adopts a RAFT (reversible addition fragmentation chain) method to prepare the water-soluble star polymer fluid loss additive for drilling fluid, and no relevant report is found in any literature on the preparation of the water-soluble star polymer fluid loss additive for drilling fluid by using a RAFT polymerization method.
The method provided by the invention adopts a reversible addition-fragmentation chain transfer (RAFT) polymerization method, adopts a semi-continuous polymerization process, uses a diene monomer and a chain transfer agent with a low proportion, and is prepared in an aqueous solution or buffer solution system, the polymerization reaction is easy to control, the reaction temperature is stable, the obtained product has good temperature resistance and low viscosity effect, and the technical problems of large viscosity effect of high-temperature and high-density drilling fluid, limited addition of a treating agent and difficulty in considering both rheological property and suspension property are met.
The star polymer synthesized by the prior art mostly adopts methods such as atom transfer radical ATRP, ring-opening polymerization and the like, the reaction conditions of the methods are harsh, high temperature and organic solvent are generally adopted, the regulation and control effects on acidic functional group monomers and water-soluble monomers are poor, and the star polymer researched by the prior art is mostly used in the fields of medicine, papermaking, leather and the like.
The star polymer prepared by the prior art has complex process, high reaction temperature and great operational difficulty, or the filtrate reducer is prepared by adopting a conventional aqueous solution polymerization mode, all the monomers are high-temperature resistant monomers, and the used monomers are various and have high cost.
The water-soluble filtrate reducer prepared by the method is a hyperbranched polymer, and has a highly branched structure, so that the water-soluble filtrate reducer shows different performances from a linear polymer, such as molecular chains of the polymer are not easy to tangle, and the viscosity of the solution and the bulk is low, so that the water-soluble filtrate reducer is more favorable for being applied to high-density drilling fluid compared with the linear polymer; the hyperbranched polymer has a spherical molecular structure, a large number of functional groups at the tail end of a molecular chain, high branching density, short branched chains and good shear resistance, and is beneficial to the long-term stability of a high-temperature drilling fluid system.
The invention provides a water-soluble filtrate reducer prepared by the method in the technical scheme, and the structural schematic diagram of the water-soluble filtrate reducer is shown in figure 1.
The invention provides a water-soluble star polymer fluid loss additive and a preparation method thereof, which are suitable for water-based drilling fluid and can control the rheological property of non-viscosifying and high-density drilling fluid.
The invention provides a drilling fluid, which comprises the water-soluble filtrate reducer for the drilling fluid in the technical scheme. The components of the drilling fluid are not particularly limited, and a person skilled in the art can select a proper drilling fluid system according to actual conditions, and the water-soluble filtrate reducer for the drilling fluid is added into the drilling fluid.
In the present invention, the drilling fluid preferably comprises:
base slurry, SMC (sulfonated lignite), SMP (sulfonated phenolic resin), water-soluble fluid loss additive for drilling fluid, KCl and barite.
In the present invention, the base slurry preferably has the following composition: water, soda ash and sodium bentonite.
In the invention, the mass content of the soda ash in the base slurry is preferably 0.2-0.4%, and more preferably 0.3%.
In the invention, the mass content of the sodium bentonite in the base pulp is preferably 3-5%, more preferably 3.5-4.5%, and most preferably 4%.
In the invention, the preparation method of the base slurry comprises the following steps:
mixing and stirring water, soda ash and sodium bentonite for 8 hours, and standing for 48 hours at room temperature.
In the invention, the mass content of the SMC in the drilling fluid is preferably 4-6%, more preferably 4.5-5.5%, and most preferably 5%.
In the invention, the mass content of the SMP in the drilling fluid is preferably 4-6%, more preferably 4.5-5.5%, and most preferably 5%.
In the invention, the mass content of the water-soluble filtrate reducer for the drilling fluid in the drilling fluid is preferably 1-2%, more preferably 1.2-1.8%, and most preferably 1.4-1.6%.
In the invention, the mass content of the KCl in the drilling fluid is preferably 4-6%, more preferably 4.5-5.5%, and most preferably 5%.
In the invention, the mass content of the barite in the drilling fluid is preferably 150-200%, more preferably 160-180%, and most preferably 170%.
According to the method for preparing the water-soluble star polymer fluid loss additive, a special chain transfer agent with a high chain transfer constant is used in the RAFT polymerization process, the chain transfer agent and a growing free radical undergo reversible addition-fragmentation regenerative transfer, the activity of the free radical is maintained, controllable and active free radical polymerization is realized, meanwhile, a semi-continuous operation process is adopted, a low-proportion chain transfer agent is used, the polymerization temperature is controlled to be 35-60 ℃, the dripping speed of a diene compound is controlled to be 20-50 mL/h, and the water-soluble star polymer fluid loss additive with the final conversion rate of 92% is obtained.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the provided drawings without creative efforts.
Fig. 1 is a schematic structural diagram of a water-soluble fluid loss additive for drilling fluid prepared by the method provided by the invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
Preparing a branching agent: 0.06g of N, N-methylenebisacrylamide and 5g of acrylamide were dissolved in 10mL of water and charged in a constant pressure dropping funnel.
Preparation of active macromolecular chain transfer agent: weighing 30g of 2-acrylamide-2-methylpropanesulfonic acid monomer, dissolving the monomer in water, adjusting the pH value to 6, adding 27.5g of acrylamide monomer and 0.09g of 4-cyanovaleric acid dithiobenzoate into the solution, transferring the solution into a 250mL four-neck flask, introducing nitrogen to remove oxygen for 30min, simultaneously heating the system to 35 ℃, adding 0.06g of Ammonium Persulfate (APS) and 0.06g of sodium bisulfite to initiate polymerization reaction, and obtaining the active macromolecular chain transfer agent after 2.5 hours of polymerization reaction.
Preparation of water-soluble star polymer fluid loss additive: and (3) dropwise adding a branching agent which is introduced with nitrogen and deoxidized for 30min into the prepared active macromolecular chain transfer agent, wherein the dropwise adding speed is at a constant rate of 20mL/h, and standing and reacting for 3 hours after the dropwise adding is finished to obtain the star polymer fluid loss additive.
Example 2
Preparing a branching agent: 0.75g of polyethylene glycol dimethacrylate and 5g of acrylamide were dissolved in 10mL of water and charged into a constant pressure dropping funnel.
Preparation of active macromolecular chain transfer agent: weighing 40g of 2-acrylamide-2-methylpropanesulfonic acid monomer, dissolving the monomer in water, adjusting the pH value to 7, adding 30g of acrylamide monomer and 0.2g of (3-benzylmercaptothiocarbonylthio) propionic acid into the solution, transferring the solution into a 250mL four-neck flask, introducing nitrogen to remove oxygen for 30min, heating the system to 40 ℃, adding 0.15g of Ammonium Persulfate (APS) and 0.15g of sodium bisulfite to initiate polymerization reaction, and obtaining the active macromolecular chain transfer agent after the polymerization reaction is carried out for 3 hours.
Preparation of water-soluble star polymer fluid loss additive: and (3) dropwise adding a branching agent which is introduced with nitrogen and deoxidized for 30min into the prepared active macromolecular chain transfer agent, wherein the dropwise adding speed is at a constant rate of 20mL/h, and standing and reacting for 4 hours after the dropwise adding is finished to obtain the star polymer fluid loss additive.
Example 3
Preparing a branching agent: 0.06g of N, N-methylenebisacrylamide and 4g of acrylamide were dissolved in 10mL of water and charged in a constant pressure dropping funnel.
Preparation of active macromolecular chain transfer agent: weighing 30g of 2-acrylamide-2-methylpropanesulfonic acid monomer, dissolving the monomer in water, adjusting the pH value to 8, adding 27.5g of acrylamide monomer and 0.09g of 4-cyanovaleric acid dithiobenzoate into the solution, transferring the solution into a 250mL four-neck flask, introducing nitrogen to remove oxygen for 30min, simultaneously heating the system to 60 ℃, adding 0.125g of Ammonium Persulfate (APS) to initiate polymerization reaction, and obtaining the active macromolecular chain transfer agent after 4 hours of polymerization reaction.
Preparation of water-soluble star polymer fluid loss additive: and (3) dropwise adding a branching agent which is introduced with nitrogen and deoxidized for 30min into the prepared active macromolecular chain transfer agent, wherein the dropwise adding speed is at a constant rate of 20mL/h, and standing and reacting for 5 hours after the dropwise adding is finished to obtain the star polymer fluid loss additive.
Example 4
Preparing a branching agent: 0.06g of N, N-methylenebisacrylamide and 4g of acrylamide were dissolved in 10mL of water and charged in a constant pressure dropping funnel.
Preparation of active macromolecular chain transfer agent: weighing 37.5g of 2-acrylamide-2-methylpropanesulfonic acid monomer, dissolving the monomer in water, adjusting the pH value to 8, adding 25g of acrylamide monomer and 0.105g of (3-benzylmercaptothiocarbonylthio) propionic acid into the solution, transferring the solution into a 250mL four-mouth bottle, introducing nitrogen to remove oxygen for 30min, simultaneously heating the system to 50 ℃, adding 0.125g of Ammonium Persulfate (APS) to initiate polymerization reaction, and obtaining the active macromolecular chain transfer agent after 4 hours of polymerization reaction.
Preparation of water-soluble star polymer fluid loss additive: and (3) dropwise adding a branching agent which is introduced with nitrogen and deoxidized for 30min into the prepared active macromolecular chain transfer agent, wherein the dropwise adding speed is at a constant rate of 20mL/h, and standing and reacting for 4 hours after the dropwise adding is finished to obtain the star polymer fluid loss additive.
Example 5 temperature resistance test
The water-soluble star polymer fluid loss additive prepared in the embodiments 1-4 and the comparative example is prepared into 400mL of polymer aqueous solution with the mass concentration of 1.0% respectively, the polymer aqueous solution is sealed and maintained at 24 +/-3 ℃ for 24 hours, the polymer aqueous solution is stirred at a low speed for 5min after being fully dissolved, the apparent viscosity of the polymer aqueous solution is tested according to a method specified in 6.3 in GB/T16783.1-2006 part 1 of field test of drilling fluid in the petroleum and natural gas industry, namely water-based drilling fluid, and then the high-temperature aged apparent viscosity is tested after high-temperature aging at 150 ℃/16 h.
Comparative examples were prepared as follows:
dissolving the same monomers and raw materials in the same proportion as those in the embodiment 1 in water by adopting an aqueous solution polymerization method, adjusting the pH value to 9-10, adding 0.2% of initiator for polymerization, obtaining a cellular polymer after 5-10 min, and drying and crushing to obtain the linear polymer fluid loss additive.
The results of testing the temperature resistance of the fluid loss additives prepared in the examples of the present invention and the comparative examples are shown in table 1.
TABLE 1 temperature resistance of fluid loss additives prepared in inventive and comparative examples
Figure BDA0001861872920000081
As can be seen from Table 1, the concentration of the star polymer solution prepared in the embodiment of the invention is 1.0%, the viscosity retention rate after high-temperature aging is more than 80%, while the viscosity retention rate of the linear polymer in the comparative example is 5.9%, and the fluid loss additive prepared in the invention has good temperature resistance.
Example 6 fluid loss Performance test
Preparing composite brine slurry:
the preparation of the composite brine slurry is carried out according to the reference standard Q/SH 10250523-2008 < general technical conditions of synthetic polymers for drilling fluid >: weighing 350mL of distilled water, placing the distilled water in a cup, adding 16.0g of sodium chloride, 2.6g of anhydrous calcium chloride and 6.9g of magnesium chloride, adding 52.5g of calcium bentonite and 3.15g of anhydrous sodium carbonate after the distilled water is dissolved, stirring at a high speed for 20min, stopping at least twice during the stirring, scraping the clay adhered to the wall of the container, and performing closed maintenance at 24 +/-3 ℃ for 24 hours to obtain the composite saline water-based slurry.
And (3) performance testing:
the water-soluble star polymer fluid loss additive for drilling fluid prepared in the examples 1-4 and the comparative example is respectively added into the composite brine slurry, stirred at a high speed for 5min, sealed and maintained for 24h, then stirred at a high speed for 5min, and the apparent viscosity and the medium pressure fluid loss at room temperature and pressure of 690Pa at 24 +/-3 ℃ are tested according to the specification of 6.3 and the specification of 7.2 in GB/T16783.1-2006 part 1 of the on-site test of drilling fluid in the petroleum and gas industry, part 1 of water-based drilling fluid, and the performance after high-temperature aging is measured after high-temperature aging at 150 ℃/16 h.
A comparative example linear polymer fluid loss additive was prepared according to the method of the comparative example in example 5.
The fluid loss properties of the fluid loss additives prepared in the examples of the present invention and the comparative examples are shown in table 2.
Table 2 fluid loss performance of fluid loss additives prepared in examples of the present invention and comparative examples
Figure BDA0001861872920000091
As can be seen from Table 2, when the addition amount of the star polymer is 1.5%, the API (American Petroleum institute) filtration loss after 150 ℃/16h high-temperature aging is 6.0-9.0 mL, and the viscosity retention rate after high temperature is more than 75%; under the same conditions, the API filtration loss after the linear polymer is aged at high temperature is 44mL, and the viscosity retention rate is 25.6%. The star polymer fluid loss agent prepared by the embodiment of the invention has better fluid loss performance in composite saline, and the performance is obviously better than that of a linear polymer.
Example 7
The water-soluble star polymer fluid loss additive for the drilling fluid prepared in the embodiments 1-4 and the comparative example is added into the fluid loss additive with the density of 2.0g/cm3In the polysulfonate potassium salt drilling fluid system (4 wt% of prehydration base slurry (1000mL of water, 3g of soda and 40g of sodium bentonite)), 5 wt% of SMC, 5 wt% of SMP and 1.5 wt% of fluid loss additive prepared in the example, 5 wt% of KCl and 200 wt% of barite, stirring at a high speed for 20min, maintaining in a sealed manner for 24h, then stirring at a high speed for 5min, measuring the apparent viscosity according to the specification of 6.3 in GB/T16783.1-2006 < petroleum and natural gas industry drilling fluid field test part 1: water-based drilling fluid >, measuring the medium pressure filtration loss at room temperature and pressure according to the specification of 7.2, measuring the pressure 690Pa at the temperature of 24 +/-3 ℃, and then measuring the performance after high-temperature aging at the temperature of 200 ℃/16 h.
A comparative example linear polymer fluid loss additive was prepared according to the preparation of the comparative example in example 5.
The performance test results of the fluid loss additive prepared in the examples and the comparative examples of the invention after being added into drilling fluid are shown in table 3.
TABLE 3 Performance of fluid loss additives prepared in examples of the invention and comparative examples after addition to drilling fluids
Figure BDA0001861872920000101
As can be seen from Table 3, when the addition amount of the star polymer is 1.5 wt%, the drilling fluid has better rheological property after aging at 200 ℃/16h, the viscosity retention rate is more than 95%, and the high-temperature high-pressure filtration loss at 180 ℃ is within 12.8 mL; in the comparative example, the viscosity retention rate of the linear polymer with the same amount is 32%, and the high-temperature high-pressure fluid loss is more than 20 mL.
From the above embodiments, the present invention provides a preparation method of a water-soluble fluid loss additive for drilling fluid, including: reacting a branching agent with a macromolecular chain transfer agent to obtain a water-soluble filtrate reducer for drilling fluid; the branching agent is prepared from materials comprising acrylamide monomers and a branching agent; the macromolecular chain transfer agent is prepared from materials including an acrylamide monomer, an RAFT chain transfer agent and an organic acid monomer. The method provided by the invention adopts a reversible addition-fragmentation chain transfer (RAFT) polymerization method, adopts a semi-continuous polymerization process, uses a diene monomer and a chain transfer agent with a low proportion, and is prepared in an aqueous solution or buffer solution system, the polymerization reaction is easy to control, the reaction temperature is stable, the obtained product has good temperature resistance and low viscosity effect, and the technical problems of large viscosity effect of high-temperature and high-density drilling fluid, limited addition of a treating agent and difficulty in considering both rheological property and suspension property are met.

Claims (9)

1. A preparation method of a water-soluble filtrate reducer for drilling fluid comprises the following steps: reacting a branching agent with a macromolecular chain transfer agent to obtain a water-soluble filtrate reducer for drilling fluid;
the branching agent is prepared from materials comprising acrylamide monomers and a branching agent;
the macromolecular chain transfer agent is prepared from materials comprising an acrylamide monomer, an RAFT chain transfer agent and an organic acid monomer;
the preparation method of the branching agent comprises the following steps:
the acrylamide monomer and branching agent are dissolved in a polar solvent to provide the branching agent.
2. The process of claim 1, wherein the branching agent is a polyene compound.
3. The method according to claim 1, characterized in that the branching agent is N, N-methylenebisacrylamide or polyethylene glycol dimethacrylate.
4. The method according to claim 1, wherein the macromolecular chain transfer agent is prepared by a method comprising:
dissolving an organic acid monomer in a polar solvent to obtain an organic acid monomer solution;
under the action of an initiator, carrying out polymerization reaction on an acrylamide monomer, an RAFT chain transfer agent and an organic acid monomer solution to obtain a macromolecular chain transfer agent.
5. The method according to claim 4, wherein the organic acid monomer is 2-acrylamido-2-methylpropanesulfonic acid or 2-acryloxy-2-methylpropanesulfonic acid.
6. The method according to claim 4, wherein the initiator is a peroxy-based initiator or an oxidation-reduction-based initiator.
7. The method of claim 4, wherein the RAFT chain transfer agent is a dithio compound or a trithio compound.
8. The method of claim 7, wherein the RAFT chain transfer agent is 4-cyanovaleric acid dithiobenzoate or (3-benzylmercaptothiocarbonylthio) propionic acid.
9. A drilling fluid comprising the water-soluble fluid loss additive for drilling fluids prepared by the method of claim 1.
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Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6294622B1 (en) * 1999-09-27 2001-09-25 Ecole Polytechnique Federale De Lausanne (Epfl) Polymer flocculants with improved dewatering characteristics
CN101693749A (en) * 2009-10-22 2010-04-14 浙江大学 Method for preparing dissaving vinyl or propenyl amide polymer
CN101967369A (en) * 2010-08-16 2011-02-09 山东大学 Comb-like polymer fluid loss additive for drilling fluid and preparation method thereof
CN102153714A (en) * 2010-12-29 2011-08-17 浙江大学 Method for preparing cation type hyperbranched ethylene or acrylamide polymer
CN102604013A (en) * 2012-03-09 2012-07-25 山东轻工业学院 Preparation method for dendrimer-star cationic polyacrylamide
CN104357030A (en) * 2014-06-04 2015-02-18 中国石油化工集团公司 Branched polymer treatment agent for drilling liquid and preparation method of branched polymer treatment agent
CN105189643A (en) * 2012-08-30 2015-12-23 Atrp解决方案公司 Dual mechanism thickening agents for hydraulic fracturing fluids

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6294622B1 (en) * 1999-09-27 2001-09-25 Ecole Polytechnique Federale De Lausanne (Epfl) Polymer flocculants with improved dewatering characteristics
CN101693749A (en) * 2009-10-22 2010-04-14 浙江大学 Method for preparing dissaving vinyl or propenyl amide polymer
CN101967369A (en) * 2010-08-16 2011-02-09 山东大学 Comb-like polymer fluid loss additive for drilling fluid and preparation method thereof
CN102153714A (en) * 2010-12-29 2011-08-17 浙江大学 Method for preparing cation type hyperbranched ethylene or acrylamide polymer
CN102604013A (en) * 2012-03-09 2012-07-25 山东轻工业学院 Preparation method for dendrimer-star cationic polyacrylamide
CN105189643A (en) * 2012-08-30 2015-12-23 Atrp解决方案公司 Dual mechanism thickening agents for hydraulic fracturing fluids
CN104357030A (en) * 2014-06-04 2015-02-18 中国石油化工集团公司 Branched polymer treatment agent for drilling liquid and preparation method of branched polymer treatment agent

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