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CN115433311B - Working fluid for blocking drilling fluid from transmitting pressure to stratum hole seam and preparation method thereof - Google Patents

Working fluid for blocking drilling fluid from transmitting pressure to stratum hole seam and preparation method thereof Download PDF

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Publication number
CN115433311B
CN115433311B CN202211011938.4A CN202211011938A CN115433311B CN 115433311 B CN115433311 B CN 115433311B CN 202211011938 A CN202211011938 A CN 202211011938A CN 115433311 B CN115433311 B CN 115433311B
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monomer
initiator
mass ratio
pressure
acrylamide
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CN115433311A (en
Inventor
欧阳伟
李晓阳
景岷嘉
吴正良
王兰
董泽坤
陈洋
杨梦莹
陶怀志
陈璇悦
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China National Petroleum Corp
CNPC Chuanqing Drilling Engineering Co Ltd
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China National Petroleum Corp
CNPC Chuanqing Drilling Engineering Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F220/00Copolymers 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
    • C08F220/02Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
    • C08F220/52Amides or imides
    • C08F220/54Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide
    • C08F220/58Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide containing oxygen in addition to the carbonamido oxygen, e.g. N-methylolacrylamide, N-(meth)acryloylmorpholine
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F2/00Processes of polymerisation
    • C08F2/38Polymerisation using regulators, e.g. chain terminating agents, e.g. telomerisation
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F4/00Polymerisation catalysts
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K8/00Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
    • C09K8/40Spacer compositions, e.g. compositions used to separate well-drilling from cementing masses
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K8/00Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
    • C09K8/42Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells
    • C09K8/426Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells for plugging
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K8/00Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
    • C09K8/42Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells
    • C09K8/44Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells containing organic binders only

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)

Abstract

The invention relates to the technical field of petroleum drilling, in particular to a working solution for blocking drilling fluid from transmitting pressure to stratum hole seams and a preparation method thereof, wherein the working solution comprises deionized water, a monomer, a crosslinking agent and an initiator; wherein the monomer is N- (2-hydroxyethyl) acrylamide, and is used for being dissolved in deionized water, and the concentration of the dissolved monomer is more than 15mg/mL; the mass ratio of the cross-linking agent to the monomer is 0.01-0.5 wt%, and the mass ratio of the initiator to the monomer is 0.024-10 wt%. Through the working solution and the preparation method thereof, rapid solidification can be accurately carried out in proper time, and the problem that the transmission of the liquid column pressure of drilling fluid to the stratum with low pore pressure can not be effectively blocked can be effectively solved.

Description

Working fluid for blocking drilling fluid from transmitting pressure to stratum hole seam and preparation method thereof
Technical Field
The invention relates to the technical field of petroleum drilling, in particular to a working fluid for blocking drilling fluid from transmitting pressure to stratum hole seams and a preparation method thereof.
Background
With the increasing complexity of the oil gas exploration drill meeting stratum conditions, the pressure difference drill sticking caused by the liquid column pressure balancing the abnormal high pressure of the stratum and the low pressure of the stratum in the same open hole section occurs due to the limitation of the well structure, so that great loss is brought to drilling engineering, and even the well is scrapped. The external cause of the differential pressure stuck drill is the existence of the differential pressure between the pore pressure of the stratum and the pressure of the liquid column of the drilling fluid, and the internal cause of the differential pressure stuck drill is the existence of a filter cake on the well wall. One of the reasons for the formation of the filter cake is the fluid loss effect of the drilling fluid, and in general, the greater the pressure difference in the same permeable rock stratum, the greater the fluid loss of the drilling fluid, the more solid phase particles are deposited on the surface of the permeable rock stratum, the thicker the filter cake, and the greater the possibility of differential pressure sticking.
At present, in the field of oil drilling, besides reducing the bottom hole liquid column pressure, common methods for preventing differential pressure sticking by blocking the transmission of the drilling liquid column pressure to a low pore pressure stratum are as follows.
First, after cross-linking and curing by using thermosetting resin or polyacrylamide, etc., the holes and seams of the stratum are plugged, and the transmission of the liquid column pressure of the drilling fluid to the stratum with low pore pressure is blocked. The thermoset or polyacrylamide precursor used in this process needs to be compounded at the surface, then pumped through the drill pipe to the corresponding location downhole, and cured after being pumped into the corresponding location. However, the existing thermosetting resin has a relatively high curing speed, and the drill pipe requires a relatively long operation time for pumping the thermosetting resin precursor to the downhole response position, which may result in a downhole accident caused by the fact that the thermosetting resin precursor has not reached the target position and has started curing during the pumping process. In addition, the thermosetting resin or the polyacrylamide precursor has higher viscosity, is not easy to enter stratum holes, seams or has less entering amount, can not achieve the purpose of effective plugging, and has the danger of inflammability and explosiveness because an organic solvent is needed when the precursor solution is prepared by the thermosetting resin.
Second, sodium silicate is the most commonly used inorganic gel currently used in WGSO (chemical water/gas plugging agents). It forms a sol or gel by reacting with various chemical agents, thereby blocking the transfer of drilling fluid column pressure to the low pore pressure formation. The specific procedure is to add 15% HCl slowly to the sodium silicate solution and inject the liquid into the formation. After injection of the sodium silicate liquid into the formation, the gel may form within a few hours under the influence of the formation temperature. Higher formation temperatures may allow for rapid solidification. Silicate may react with a variety of common ions, resulting in a decrease in its gel strength. In addition, the strength of silicate gel is related to the gel time. The longer the gel time, the weaker the gel strength, and the shorter the gel time, the better the gel strength. This results in the need to shorten the silicate gel time as much as possible in practical applications, which makes site construction difficult. Once the gel time is too long, the problems of poor pressure transmission blocking effect, poor gel stability and the like are caused, and meanwhile, HCl can greatly influence the performance of drilling fluid.
Thirdly, the cloud point effect of the polymeric alcohol is fully utilized, so that the polymeric alcohol is separated out under a certain temperature condition, stratum holes and seams are plugged, and the transmission of the liquid column pressure of the drilling fluid to the stratum with low pore pressure is blocked. However, because the particle size of the polymeric alcohol precipitates is small (typically on the order of nanometers or micrometers), it is difficult to effectively seal large pores and seams in the formation.
Fourth, in the prior art, a chinese invention patent document with publication number CN105694828a and publication date 2016, 06 and 22 is proposed, and the technical scheme disclosed in the patent document is as follows: the plugging agent for the organic salt drilling fluid is a copolymer obtained by copolymerizing 10-25 parts by weight of N-isopropyl acrylamide, 9-17 parts by weight of acrylamide and 1-3 parts by weight of N, N-methylene bisacrylamide under the action of an initiator and then drying the copolymer. The plugging agent for the organic salt drilling fluid has good temperature resistance and salt resistance, has temperature sensitivity, and has small influence on the viscosity cutting of the drilling fluid; is deformable and has good plugging effect.
In the practical use process, the following problems can occur: the method has the defects that the plugging agent has low plugging efficiency due to the fact that the particle size of the plugging agent is difficult to match with the stratum holes and seams, the pressure bearing capacity after plugging is low, and the like.
The method has the respective defects, and the problems that the transmission of the liquid column pressure of the drilling fluid to the stratum with low pore pressure cannot be effectively blocked due to weak drilling sticking or plugging capability are solved.
Disclosure of Invention
In order to solve the technical problems, the invention provides the working solution for blocking the transmission of the drilling fluid to the stratum hole and seam and the preparation method thereof, which can accurately and rapidly solidify in proper time and can effectively solve the problem that the transmission of the drilling fluid column pressure to the stratum with low pore pressure can not be effectively blocked.
The invention is realized by adopting the following technical scheme:
The working fluid for blocking the drilling fluid to transfer pressure to the stratum aperture is characterized in that: comprises deionized water, a monomer, a crosslinking agent and an initiator; wherein the monomer is N- (2-hydroxyethyl) acrylamide, and is used for being dissolved in deionized water, and the concentration of the dissolved monomer is more than 15mg/mL; the mass ratio of the cross-linking agent to the monomer is 0.01-0.5 wt%, and the mass ratio of the initiator to the monomer is 0.024-10 wt%.
The polymerization inhibitor is p-benzoquinone, and the mass ratio of the polymerization inhibitor to the monomer is 0.001-0.044 wt%.
The cross-linking agent is N-N methylene bisacrylamide or organozirconium.
The initiator is ammonium persulfate, potassium persulfate or sodium persulfate.
The cross-linking agent is methylene bisacrylamide, the initiator is ammonium persulfate, and the polymerization inhibitor is p-benzoquinone.
The concentration of the monomer is A-100 mg/mL, wherein A is more than 15mg/mL.
The preparation method of the working fluid for blocking the drilling fluid to transfer pressure to the stratum hole gap is characterized by comprising the following steps of: placing monomer N- (2-hydroxyethyl) acrylamide into a container, adding deionized water, and fully stirring for dissolution; after the monomer is completely dissolved, adding a corresponding cross-linking agent, an initiator and a polymerization inhibitor to prepare the working solution.
The initiator is in situ configured.
The working solution is used for monomer crosslinking reaction at the temperature of 80-120 ℃.
Compared with the prior art, the invention has the beneficial effects that:
1. During the drilling process, the formation temperature increases with increasing depth due to friction between the drill bit and the formation, and can reach 120 degrees celsius at 2000 meters. The invention uses N- (2-hydroxyethyl) acrylamide as a monomer to form the working solution, and the working solution has good fluidity, so that the problems that thermosetting resin or polyacrylamide precursor has higher viscosity, is difficult to enter stratum holes, seams or has less entering amount, and cannot achieve effective blocking are solved. When the device is used, the fluidity of the working solution is fully utilized to enable the working solution to enter a stratum hole gap, the working solution is initiated to be crosslinked and polymerized in situ through the stratum temperature, gel is formed at a seepage layer to realize the blocking of pressure transmission, so that the pressure difference formed by the liquid column pressure of the drilling solution and the stratum pore pressure is reduced or eliminated, the transmission of the liquid column pressure of the drilling solution to a stratum with low pore pressure is blocked or weakened, the fluid loss effect of the drilling solution is reduced, the formation of a virtual and thick mud cake on a well wall is reduced, the occurrence of complex accidents such as differential pressure sticking is prevented, and the device has the advantages of low cost, simplicity and convenience in operation, no toxicity of monomers, moderate crosslinking time and the like. The working fluid can be used alone in the drilling process, can also be matched with other bridging materials, and is used for drilling plugging operation.
2. The invention selects N- (2-hydroxyethyl) acrylamide as a monomer, and the crosslinking time is more controllable than that of acrylamide as a monomer. Furthermore, the N-N methylene bisacrylamide is used as a cross-linking agent, so that the cross-linking time can be regulated and the gel strength can be enhanced. Ammonium persulfate is used as an initiator for initiating the polymerization reaction of the monomers, and the crosslinking time can be regulated.
3. The preparation method also comprises a polymerization inhibitor, and the addition of the polymerization inhibitor can prolong the time for crosslinking, so that the working solution can be prepared in advance without being prepared on site. Through the cooperation of polymerization inhibitor and the rest ratio, finally make the continuous adjustable of operating fluid crosslinked polymerization in 1~3 hours even longer time span, can realize the abundant crosslinking of operating fluid in stratum hole gap to demonstrate better pressure transmission separation effect, reduce or eliminate the pressure differential that drilling fluid column pressure and stratum pore pressure formed. Solves the problem that silicate gel shortens the gel time for improving the strength and possibly brings about underground complex construction on site.
4. The working solution can be fully filled in stratum pores and seams, and the defects of low plugging efficiency, low bearing capacity after plugging and the like caused by difficult effective matching of the polymerized alcohol and plugging agent with the sizes of the stratum pores and seams are overcome.
5. Because the initiator is easy to hydrolyze, the problem can be well solved by the instant preparation during use.
6. The working solution is used for monomer crosslinking reaction at the temperature of 80-120 ℃ so that the working solution can be matched with the temperature of the stratum, the reaction condition is mild, and the consumed energy is low.
Drawings
The invention will be described in further detail with reference to the drawings and detailed description, wherein:
FIG. 1 is a schematic diagram showing the effect of monomer concentration on gel forming time in the present invention;
FIG. 2 is a schematic diagram showing the effect of monomer concentration on monomer conversion efficiency in the present invention;
FIG. 3 is a schematic diagram showing the effect of the initiator ammonium persulfate content on the gel forming time in the present invention;
FIG. 4 is a schematic diagram showing the effect of the initiator ammonium persulfate content on monomer conversion efficiency in the present invention;
FIG. 5 is a schematic diagram showing the effect of temperature on the gel forming time in the present invention;
FIG. 6 is a schematic diagram showing the effect of temperature on monomer conversion efficiency in the present invention;
FIG. 7 is a graph showing the effect of crosslinker N-N methylene bisacrylamide content on gel time in accordance with the present invention;
FIG. 8 is a graph showing the effect of crosslinker N-N methylene bisacrylamide content on monomer conversion efficiency in accordance with the present invention;
FIG. 9 is a schematic diagram showing the influence of the polymerization inhibitor content on the gel forming time in the present invention;
FIG. 10 is a graph showing the effect of the organozirconium content of the crosslinker on the gel time in accordance with the present invention;
FIG. 11 is a graph showing the effect of initiator sodium persulfate content on gel formation time in accordance with the present invention;
FIG. 12 is a graph showing the effect of initiator potassium persulfate content on gel formation time in accordance with the present invention;
FIG. 13 is a graph showing the results of a viscoelastic test of a pressure transmission barrier agent according to the present invention at various temperatures;
FIG. 14 is a second schematic diagram of the results of a viscoelastic test of a pressure transmission barrier according to the present invention at different temperatures;
FIG. 15 is a graph III showing the results of a viscoelastic test of a pressure transmission barrier agent according to the present invention at various temperatures.
Detailed Description
Example 1
Deionized water is used as a solvent, 50mL of monomer N- (2-hydroxyethyl) acrylamide with the concentration of 15mg/mL is taken at room temperature, and a cross-linking agent N-N methylene bisacrylamide and an initiator ammonium persulfate are proportionally taken and mixed, so that the pressure transfer barrier working solution is obtained. Wherein the mass ratio of the cross-linking agent to the monomer is 1:200 (0.5%) of initiator to monomer mass ratio 1:4167 (0.024%). When the reaction is carried out at a constant temperature of 80 ℃, the monomer N- (2-hydroxyethyl) acrylamide is not crosslinked, and gel is not formed. Condensation is added to prevent the whole process of water evaporation.
Example 2
Taking deionized water as a solvent, taking 50mL of monomer N- (2-hydroxyethyl) acrylamide of 20mg/mL at room temperature, and proportionally mixing crosslinking agent N-N methylene bisacrylamide and initiator ammonium persulfate to obtain the pressure transfer barrier working solution. Wherein the mass ratio of the cross-linking agent to the monomer is 1:200 (0.5%) of initiator to monomer mass ratio 1:4167 (0.024%). And (3) carrying out constant temperature treatment at 80 ℃ for 30min, and crosslinking the monomer N- (2-hydroxyethyl) acrylamide to form gel. Condensation is added to prevent the whole process of water evaporation.
Example 3
Taking deionized water as a solvent, taking 50mL of monomer N- (2-hydroxyethyl) acrylamide of 40mg/mL at room temperature, and proportionally mixing crosslinking agent N-N methylene bisacrylamide and initiator ammonium persulfate to obtain the pressure transfer barrier working solution. Wherein the mass ratio of the cross-linking agent to the monomer is 1:200 (0.5%) of initiator to monomer mass ratio 1:4167 (0.024%). And (3) carrying out constant temperature treatment at 80 ℃ for 15min, and crosslinking the monomer N- (2-hydroxyethyl) acrylamide to form gel. Condensation is added to prevent the whole process of water evaporation.
Example 4
Deionized water is used as a solvent, 50mL of monomer N- (2-hydroxyethyl) acrylamide with the concentration of 100mg/mL is taken at room temperature, and a cross-linking agent N-N methylene bisacrylamide and an initiator ammonium persulfate are proportionally taken and mixed, so that the pressure transfer barrier working solution is obtained. Wherein the mass ratio of the cross-linking agent to the monomer is 1:200 (0.5%) of initiator to monomer mass ratio 1:10 (10%). And (3) processing at the constant temperature of 80 ℃ for 10min, and crosslinking the monomer N- (2-hydroxyethyl) acrylamide to form gel. Condensation is added to prevent the whole process of water evaporation.
Example 5
Deionized water is used as a solvent, 50mL of monomer N- (2-hydroxyethyl) acrylamide with the concentration of 100mg/mL is taken at room temperature, and a cross-linking agent N-N methylene bisacrylamide and an initiator ammonium persulfate are proportionally taken and mixed, so that the pressure transfer barrier working solution is obtained. Wherein the mass ratio of the cross-linking agent to the monomer is 1:200 (0.5%) of initiator to monomer mass ratio 1:100 (1%). And (3) carrying out constant temperature treatment at 80 ℃ for 15min, and crosslinking the monomer N- (2-hydroxyethyl) acrylamide to form gel. Condensation is added to prevent the whole process of water evaporation.
Example 6
Deionized water is used as a solvent, 50mL of monomer N- (2-hydroxyethyl) acrylamide with the concentration of 100mg/mL is taken at room temperature, and a cross-linking agent N-N methylene bisacrylamide and an initiator ammonium persulfate are proportionally taken and mixed, so that the pressure transfer barrier working solution is obtained. Wherein the mass ratio of the cross-linking agent to the monomer is 1:200 (0.5%) of initiator to monomer mass ratio 1:1000 (0.1%). And (3) treating at the constant temperature of 80 ℃ for 16min, and crosslinking the monomer N- (2-hydroxyethyl) acrylamide to form gel. Condensation is added to prevent the whole process of water evaporation.
Example 7
Deionized water is used as a solvent, 50mL of monomer N- (2-hydroxyethyl) acrylamide with the concentration of 100mg/mL is taken at room temperature, and a cross-linking agent N-N methylene bisacrylamide and an initiator ammonium persulfate are proportionally taken and mixed, so that the pressure transfer barrier working solution is obtained. Wherein the mass ratio of the cross-linking agent to the monomer is 1:200 (0.5%) of initiator to monomer mass ratio 1:1667 (0.06%). And (3) treating at the constant temperature of 80 ℃ for 16min, and crosslinking the monomer N- (2-hydroxyethyl) acrylamide to form gel. Condensation is added to prevent the whole process of water evaporation.
Example 8
Deionized water is used as a solvent, 50mL of monomer N- (2-hydroxyethyl) acrylamide with the concentration of 100mg/mL is taken at room temperature, and a cross-linking agent N-N methylene bisacrylamide and an initiator ammonium persulfate are proportionally taken and mixed, so that the pressure transfer barrier working solution is obtained. Wherein the mass ratio of the cross-linking agent to the monomer is 1:200 (0.5%) of initiator to monomer mass ratio 1:3333 (0.03%). And (3) processing at the constant temperature of 80 ℃ for 40min, and crosslinking the monomer N- (2-hydroxyethyl) acrylamide to form gel. Condensation is added to prevent the whole process of water evaporation.
Example 9
Deionized water is used as a solvent, 50mL of monomer N- (2-hydroxyethyl) acrylamide with the concentration of 100mg/mL is taken at room temperature, and a cross-linking agent N-N methylene bisacrylamide and an initiator ammonium persulfate are proportionally taken and mixed, so that the pressure transfer barrier working solution is obtained. Wherein the mass ratio of the cross-linking agent to the monomer is 1:200 (0.5%) of initiator to monomer mass ratio 1:3571 (0.028%). And (3) processing at the constant temperature of 80 ℃ for 45min, and crosslinking the monomer N- (2-hydroxyethyl) acrylamide to form gel. Condensation is added to prevent the whole process of water evaporation.
Example 10
Deionized water is used as a solvent, 50mL of monomer N- (2-hydroxyethyl) acrylamide with the concentration of 100mg/mL is taken at room temperature, and a cross-linking agent N-N methylene bisacrylamide and an initiator ammonium persulfate are proportionally taken and mixed, so that the pressure transfer barrier working solution is obtained. Wherein the mass ratio of the cross-linking agent to the monomer is 1:200 (0.5%) of initiator to monomer mass ratio 1:4167 (0.024%). And (3) processing at the constant temperature of 80 ℃ for 80min, and crosslinking the monomer N- (2-hydroxyethyl) acrylamide to form gel. Condensation is added to prevent the whole process of water evaporation.
Example 11
Deionized water is used as a solvent, 50mL of monomer N- (2-hydroxyethyl) acrylamide with the concentration of 100mg/mL is taken at room temperature, and a cross-linking agent N-N methylene bisacrylamide, an initiator ammonium persulfate and a polymerization inhibitor p-benzoquinone are proportionally taken and mixed, so that the pressure transfer barrier working solution is obtained. Wherein the mass ratio of the cross-linking agent to the monomer is 1:200 (0.5%) of initiator to monomer mass ratio 1:1667 (0.06%) of polymerization inhibitor to monomer in a mass ratio of 1:2300 (0.044%). And (3) processing at the constant temperature of 80 ℃ for 48min, and crosslinking the monomer N- (2-hydroxyethyl) acrylamide to form gel. Condensation is added to prevent the whole process of water evaporation.
Example 12
Deionized water is used as a solvent, 50mL of monomer N- (2-hydroxyethyl) acrylamide with the concentration of 100mg/mL is taken at room temperature, and a cross-linking agent N-N methylene bisacrylamide, an initiator ammonium persulfate and a polymerization inhibitor p-benzoquinone are proportionally taken and mixed, so that the pressure transfer barrier working solution is obtained. Wherein the mass ratio of the cross-linking agent to the monomer is 1:200 (0.5%) of initiator to monomer mass ratio 1:1667 (0.06%) of polymerization inhibitor to monomer in a mass ratio of 1:2300 (0.044%). And (3) processing at the constant temperature of 75 ℃ for 50min, and crosslinking the monomer N- (2-hydroxyethyl) acrylamide to form gel. Condensation is added to prevent the whole process of water evaporation.
Example 13
Deionized water is used as a solvent, 50mL of monomer N- (2-hydroxyethyl) acrylamide with the concentration of 100mg/mL is taken at room temperature, and a cross-linking agent N-N methylene bisacrylamide, an initiator ammonium persulfate and a polymerization inhibitor p-benzoquinone are proportionally taken and mixed, so that the pressure transfer barrier working solution is obtained. Wherein the mass ratio of the cross-linking agent to the monomer is 1:200 (0.5%) of initiator to monomer mass ratio 1:1667 (0.06%) of polymerization inhibitor to monomer in a mass ratio of 1:2300 (0.044%). And (3) carrying out constant temperature treatment at 70 ℃ for 200min, and crosslinking the monomer N- (2-hydroxyethyl) acrylamide to form gel. Condensation is added to prevent the whole process of water evaporation.
Example 14
Deionized water is used as a solvent, 50mL of monomer N- (2-hydroxyethyl) acrylamide with the concentration of 100mg/mL is taken at room temperature, and a cross-linking agent N-N methylene bisacrylamide and an initiator ammonium persulfate are proportionally taken and mixed, so that the pressure transfer barrier working solution is obtained. Wherein the mass ratio of the cross-linking agent to the monomer is 1:333 (0.3%) of initiator to monomer mass ratio 1:4167 (0.024%). And (3) processing at the constant temperature of 80 ℃ for 135min, and crosslinking the monomer N- (2-hydroxyethyl) acrylamide to form gel. Condensation is added to prevent the whole process of water evaporation.
Example 15
Deionized water is used as a solvent, 50mL of monomer N- (2-hydroxyethyl) acrylamide with the concentration of 100mg/mL is taken at room temperature, and a cross-linking agent N-N methylene bisacrylamide and an initiator ammonium persulfate are proportionally taken and mixed, so that the pressure transfer barrier working solution is obtained. Wherein the mass ratio of the cross-linking agent to the monomer is 1:1000 (0.1%) of initiator to monomer mass ratio 1:4167 (0.024%). And (3) processing at the constant temperature of 80 ℃ for 110min, and crosslinking the monomer N- (2-hydroxyethyl) acrylamide to form gel. Condensation is added to prevent the whole process of water evaporation.
Example 16
Deionized water is used as a solvent, 50mL of monomer N- (2-hydroxyethyl) acrylamide with the concentration of 100mg/mL is taken at room temperature, and a cross-linking agent N-N methylene bisacrylamide and an initiator ammonium persulfate are proportionally taken and mixed, so that the pressure transfer barrier working solution is obtained. Wherein the mass ratio of the cross-linking agent to the monomer is 1:10000 (0.01%) of initiator to monomer mass ratio 1:4167 (0.024%). And (3) processing at the constant temperature of 80 ℃ for 185min, and crosslinking the monomer N- (2-hydroxyethyl) acrylamide to form gel. Condensation is added to prevent the whole process of water evaporation.
Example 17
Deionized water is used as a solvent, 50mL of monomer N- (2-hydroxyethyl) acrylamide with the concentration of 100mg/mL is taken at room temperature, and a cross-linking agent N-N methylene bisacrylamide and an initiator ammonium persulfate are proportionally taken and mixed, so that the pressure transfer barrier working solution is obtained. Wherein the mass ratio of the cross-linking agent to the monomer is 1:200 (0.5%) of initiator to monomer mass ratio 1:1667 (0.06%). And (3) processing at the constant temperature of 80 ℃ for 48min, and crosslinking the monomer N- (2-hydroxyethyl) acrylamide to form gel. Condensation is added to prevent the whole process of water evaporation.
Example 18
Deionized water is used as a solvent, 50mL of monomer N- (2-hydroxyethyl) acrylamide with the concentration of 100mg/mL is taken at room temperature, and a cross-linking agent N-N methylene bisacrylamide and an initiator ammonium persulfate are proportionally taken and mixed, so that the pressure transfer barrier working solution is obtained. Wherein the mass ratio of the cross-linking agent to the monomer is 1:200 (0.5%) of initiator to monomer mass ratio 1:1667 (0.06%). And (3) carrying out constant temperature treatment at 70 ℃ for 50min, and crosslinking the monomer N- (2-hydroxyethyl) acrylamide to form gel. Condensation is added to prevent the whole process of water evaporation.
Example 19
Deionized water is used as a solvent, 50mL of monomer N- (2-hydroxyethyl) acrylamide with the concentration of 100mg/mL is taken at room temperature, and a cross-linking agent N-N methylene bisacrylamide and an initiator ammonium persulfate are proportionally taken and mixed, so that the pressure transfer barrier working solution is obtained. Wherein the mass ratio of the cross-linking agent to the monomer is 1:200 (0.5%) of initiator to monomer mass ratio 1:1667 (0.06%). And (3) carrying out constant temperature treatment at 60 ℃ for 200min, and crosslinking the monomer N- (2-hydroxyethyl) acrylamide to form gel. Condensation is added to prevent the whole process of water evaporation.
Example 20
Deionized water is used as a solvent, 50mL of monomer N- (2-hydroxyethyl) acrylamide with the concentration of 100mg/mL is taken at room temperature, and a cross-linking agent N-N methylene bisacrylamide, an initiator ammonium persulfate and a polymerization inhibitor p-benzoquinone are proportionally taken and mixed, so that the pressure transfer barrier working solution is obtained. Wherein the mass ratio of the cross-linking agent to the monomer is 1:200 (0.5%) of initiator to monomer mass ratio 1:1667 (0.06%) and the mass ratio of the polymerization inhibitor to the monomer was 0.005%. And (3) carrying out constant temperature treatment at 80 ℃ for 30min, and crosslinking the monomer N- (2-hydroxyethyl) acrylamide to form gel. Condensation is added to prevent the whole process of water evaporation.
Example 21
Deionized water is used as a solvent, 50mL of monomer N- (2-hydroxyethyl) acrylamide with the concentration of 100mg/mL is taken at room temperature, and a cross-linking agent N-N methylene bisacrylamide, an initiator ammonium persulfate and a polymerization inhibitor p-benzoquinone are proportionally taken and mixed, so that the pressure transfer barrier working solution is obtained. Wherein the mass ratio of the cross-linking agent to the monomer is 1:200 (0.5%) of initiator to monomer mass ratio 1:1667 (0.06%) and the mass ratio of the polymerization inhibitor to the monomer was 0.001%. And (3) processing at the constant temperature of 80 ℃ for 32min, and crosslinking the monomer N- (2-hydroxyethyl) acrylamide to form gel. Condensation is added to prevent the whole process of water evaporation.
Example 22
Deionized water is used as a solvent, 50mL of monomer N- (2-hydroxyethyl) acrylamide with the concentration of 100mg/mL is taken at room temperature, and a cross-linking agent N-N methylene bisacrylamide, an initiator ammonium persulfate and a polymerization inhibitor p-benzoquinone are proportionally taken and mixed, so that the pressure transfer barrier working solution is obtained. Wherein the mass ratio of the cross-linking agent to the monomer is 1:200 (0.5%) of initiator to monomer mass ratio 1:1667 (0.06%) and the mass ratio of the polymerization inhibitor to the monomer was 0.004%. And (3) processing at the constant temperature of 80 ℃ for 40min, and crosslinking the monomer N- (2-hydroxyethyl) acrylamide to form gel. Condensation is added to prevent the whole process of water evaporation.
Example 23
Deionized water is used as a solvent, 50mL of monomer N- (2-hydroxyethyl) acrylamide with the concentration of 100mg/mL is taken at room temperature, and a cross-linking agent N-N methylene bisacrylamide, an initiator ammonium persulfate and a polymerization inhibitor p-benzoquinone are proportionally taken and mixed, so that the pressure transfer barrier working solution is obtained. Wherein the mass ratio of the cross-linking agent to the monomer is 1:200 (0.5%) of initiator to monomer mass ratio 1:1667 (0.06%) and the mass ratio of the polymerization inhibitor to the monomer was 0.0044%. And (3) processing at the constant temperature of 80 ℃ for 48min, and crosslinking the monomer N- (2-hydroxyethyl) acrylamide to form gel. Condensation is added to prevent the whole process of water evaporation.
Example 24
Deionized water is used as a solvent, 50mL of monomer N- (2-hydroxyethyl) acrylamide with the concentration of 100mg/mL is taken at room temperature, and a cross-linking agent N-N methylene bisacrylamide, an initiator ammonium persulfate and a polymerization inhibitor p-benzoquinone are proportionally taken and mixed, so that the pressure transfer barrier working solution is obtained. Wherein the mass ratio of the cross-linking agent to the monomer is 1:200 (0.5%) of initiator to monomer mass ratio 1:1667 (0.06%) and the mass ratio of the polymerization inhibitor to the monomer was 0.0054%. And (3) processing at the constant temperature of 80 ℃ for 50min, and crosslinking the monomer N- (2-hydroxyethyl) acrylamide to form gel. Condensation is added to prevent the whole process of water evaporation.
Example 25
Deionized water is used as a solvent, 10mL of monomer N- (2-hydroxyethyl) acrylamide with the concentration of 100mg/mL is taken at room temperature, and the cross-linking agent organic zirconium and the initiator ammonium persulfate are proportionally taken and mixed, so that the pressure transfer barrier working solution is obtained. Wherein the mass ratio of the cross-linking agent to the monomer is 1:333 (0.3%) of initiator to monomer mass ratio 1:5000 (0.02%). And (3) processing at the constant temperature of 120 ℃ for 4min, and crosslinking the monomer N- (2-hydroxyethyl) acrylamide to form gel. Condensation is added to prevent the whole process of water evaporation.
Example 26
Deionized water is used as a solvent, 10mL of monomer N- (2-hydroxyethyl) acrylamide with the concentration of 100mg/mL is taken at room temperature, and the cross-linking agent organic zirconium and the initiator ammonium persulfate are proportionally taken and mixed, so that the pressure transfer barrier working solution is obtained. Wherein the mass ratio of the cross-linking agent to the monomer is 1:1000 (0.1%) of initiator to monomer mass ratio 1:5000 (0.02%). And (3) processing at the constant temperature of 120 ℃ for 7min, and crosslinking the monomer N- (2-hydroxyethyl) acrylamide to form gel. Condensation is added to prevent the whole process of water evaporation.
Example 27
Deionized water is used as a solvent, 10mL of monomer N- (2-hydroxyethyl) acrylamide with the concentration of 100mg/mL is taken at room temperature, and the cross-linking agent organic zirconium and the initiator ammonium persulfate are proportionally taken and mixed, so that the pressure transfer barrier working solution is obtained. Wherein the mass ratio of the cross-linking agent to the monomer is 1:10000 (0.01%) of initiator to monomer mass ratio 1:5000 (0.02%). And (3) carrying out constant temperature treatment at 120 ℃ for 30min, and crosslinking the monomer N- (2-hydroxyethyl) acrylamide to form gel. Condensation is added to prevent the whole process of water evaporation.
Example 28
Deionized water is used as a solvent, 50mL of monomer N- (2-hydroxyethyl) acrylamide with the concentration of 100mg/mL is taken at room temperature, and a cross-linking agent N-N methylene bisacrylamide and an initiator sodium persulfate are proportionally taken and mixed, so that the pressure transfer barrier working solution is obtained. Wherein the mass ratio of the cross-linking agent to the monomer is 1:200 (0.5%) of initiator to monomer mass ratio 1:833 (0.12%). And (3) carrying out constant temperature treatment at 90 ℃ for 60min, and crosslinking the monomer N- (2-hydroxyethyl) acrylamide to form gel. Condensation is added to prevent the whole process of water evaporation.
Example 29
Deionized water is used as a solvent, 50mL of monomer N- (2-hydroxyethyl) acrylamide with the concentration of 100mg/mL is taken at room temperature, and a cross-linking agent N-N methylene bisacrylamide and an initiator sodium persulfate are proportionally taken and mixed, so that the pressure transfer barrier working solution is obtained. Wherein the mass ratio of the cross-linking agent to the monomer is 1:200 (0.5%) of initiator to monomer mass ratio 1:1250 (0.08%). And (3) processing at the constant temperature of 90 ℃ for 90min, and crosslinking the monomer N- (2-hydroxyethyl) acrylamide to form gel. Condensation is added to prevent the whole process of water evaporation.
Example 30
Deionized water is used as a solvent, 50mL of monomer N- (2-hydroxyethyl) acrylamide with the concentration of 100mg/mL is taken at room temperature, and a cross-linking agent N-N methylene bisacrylamide and an initiator sodium persulfate are proportionally taken and mixed, so that the pressure transfer barrier working solution is obtained. Wherein the mass ratio of the cross-linking agent to the monomer is 1:200 (0.5%) of initiator to monomer mass ratio 1:1667 (0.06%). And (3) processing at the constant temperature of 90 ℃ for 180min, and crosslinking the monomer N- (2-hydroxyethyl) acrylamide to form gel. Condensation is added to prevent the whole process of water evaporation.
Example 31
Deionized water is used as a solvent, 50mL of monomer N- (2-hydroxyethyl) acrylamide with the concentration of 100mg/mL is taken at room temperature, and a crosslinking agent N-N methylene bisacrylamide and an initiator potassium persulfate are proportionally taken and mixed, so that the pressure transfer barrier working solution is obtained. Wherein the mass ratio of the cross-linking agent to the monomer is 1:200 (0.5%) of initiator to monomer mass ratio 1:500 (0.2%). And (3) processing at the constant temperature of 80 ℃ for 22min, and crosslinking the monomer N- (2-hydroxyethyl) acrylamide to form gel. Condensation is added to prevent the whole process of water evaporation.
Example 32
Deionized water is used as a solvent, 50mL of monomer N- (2-hydroxyethyl) acrylamide with the concentration of 100mg/mL is taken at room temperature, and a crosslinking agent N-N methylene bisacrylamide and an initiator potassium persulfate are proportionally taken and mixed, so that the pressure transfer barrier working solution is obtained. Wherein the mass ratio of the cross-linking agent to the monomer is 1:200 (0.5%) of initiator to monomer mass ratio 1:625 (0.16%). And (3) carrying out constant temperature treatment at 80 ℃ for 23min, and crosslinking the monomer N- (2-hydroxyethyl) acrylamide to form gel. Condensation is added to prevent the whole process of water evaporation.
Example 33
Deionized water is used as a solvent, 50mL of monomer N- (2-hydroxyethyl) acrylamide with the concentration of 100mg/mL is taken at room temperature, and a crosslinking agent N-N methylene bisacrylamide and an initiator potassium persulfate are proportionally taken and mixed, so that the pressure transfer barrier working solution is obtained. Wherein the mass ratio of the cross-linking agent to the monomer is 1:200 (0.5%) of initiator to monomer mass ratio 1:1000 (0.1%). And (3) carrying out constant temperature treatment at 80 ℃ for 30min, and crosslinking the monomer N- (2-hydroxyethyl) acrylamide to form gel. Condensation is added to prevent the whole process of water evaporation.
Example 34
Deionized water is used as a solvent, 50mL of monomer N- (2-hydroxyethyl) acrylamide with the concentration of 100mg/mL is taken at room temperature, and a crosslinking agent N-N methylene bisacrylamide and an initiator potassium persulfate are proportionally taken and mixed, so that the pressure transfer barrier working solution is obtained. Wherein the mass ratio of the cross-linking agent to the monomer is 1:200 (0.5%) of initiator to monomer mass ratio 1:1667 (0.06%). And (3) processing at the constant temperature of 80 ℃ for 33min, and crosslinking the monomer N- (2-hydroxyethyl) acrylamide to form gel. Condensation is added to prevent the whole process of water evaporation.
The working fluids prepared according to examples 1,2, 3, 10, which block the transmission of pressure to the formation aperture, were tested for the effect of monomer concentration on gel formation time under otherwise unchanged conditions. Referring to FIG. 1 of the specification, as the concentration of N- (2-hydroxyethyl) acrylamide monomer increases, the crosslinking time gradually shortens from 30min to 10min when the monomer crosslinking efficiency reaches 90% or more, and the monomer cannot crosslink when the monomer concentration is lower than 15 mg/mL.
The working fluids prepared according to examples 1,2,3, 10, which block the transmission of pressure to the formation aperture, were tested for the effect of monomer concentration on monomer conversion efficiency under otherwise unchanged conditions. Referring to the description of fig. 2, as the concentration of the monomer N- (2-hydroxyethyl) acrylamide increases, the conversion efficiency varies with the crosslinking time; the results showed that the monomer N- (2-hydroxyethyl) acrylamide crosslinked rapidly, and that the crosslinking time gradually shortened as the monomer N- (2-hydroxyethyl) acrylamide concentration increased from 15mg/mL to 100 mg/mL.
The working fluid prepared according to examples 4-10 was used to block the drilling fluid from transmitting pressure to the formation hole, the other conditions were unchanged, and the influence of the initiator content on the gel forming time was tested. Referring to FIG. 3 of the specification, when the monomer crosslinking efficiency reaches 90% or more with the decrease of the initiator ammonium persulfate, the crosslinking time is gradually prolonged from 10min to 80min.
And (3) the working fluid for blocking the drilling fluid from transmitting pressure to the formation hole seam prepared in the embodiment 4-10 is unchanged in other conditions, and the influence of the initiator content on the monomer conversion efficiency is tested. Referring to fig. 4 of the specification, as the initiator ammonium persulfate was reduced from 10% to 0.024%, the conversion efficiency was varied with crosslinking time; the results show that the monomer N- (2-hydroxyethyl) acrylamide crosslinks rapidly and that the crosslinking time gradually increases as the initiator decreases.
The working fluid prepared according to examples 11 to 13 was used to block the drilling fluid from transmitting pressure to the formation hole, the other conditions were unchanged, and the influence of temperature on the gel forming time was tested. Referring to FIG. 5 of the specification, when the crosslinking efficiency of the monomer reaches 90% or more with a decrease in the crosslinking temperature, the crosslinking time is gradually prolonged from 48 minutes to 100 minutes.
The working fluid prepared according to examples 11 to 13 was used to block the drilling fluid from transmitting pressure to the formation hole, and the other conditions were unchanged, and the temperature was tested for monomer conversion efficiency. Referring to the description of fig. 6, as the crosslinking temperature decreases from 80 ℃ to 70 ℃, the conversion efficiency varies with the crosslinking time; the results showed that the crosslinking time was gradually prolonged as the crosslinking temperature was lowered.
The working fluids prepared according to examples 10, 14, 15, 16, which block the transmission of pressure to the formation aperture, were tested for the effect of crosslinker content on gel formation time, with other conditions unchanged. Referring to FIG. 7 of the specification, as the content of the crosslinking agent decreases, the crosslinking time gradually increases from 80min to 185min when the monomer crosslinking efficiency reaches 90% or more.
The working fluids prepared according to examples 10, 14, 15, 16, which block the transmission of pressure to the formation aperture, were tested for the effect of crosslinker content on monomer conversion efficiency, with other conditions unchanged. Referring to fig. 8 of the specification, as the content of the crosslinking agent is reduced from 0.5% to 0.01%, the conversion efficiency varies with the crosslinking time; the results show that the crosslinking time gradually increases as the crosslinking agent content decreases.
The working fluids prepared according to examples 20, 21, 22, 23, 24, which block the drilling fluid from transmitting pressure to the formation hole, were tested for the effect of the inhibitor content on the gel formation time, without changing the other conditions. Referring to fig. 9 of the specification, as the content of the polymerization inhibitor increases, the crosslinking time gradually increases from 30min to 50min.
The barrier drilling fluids prepared according to examples 25, 26, 27 deliver pressure to the formation aperture without changing other conditions and the effect of the organozirconium content of the crosslinker on the gel formation time was tested. Referring to fig. 10 of the specification, as the content of organozirconium decreases, the crosslinking time gradually increases from 4min to 30min.
The working fluids prepared according to examples 28, 29, 30, which blocked the transmission of pressure to the formation aperture, were otherwise unchanged, and tested for the effect of the sodium persulfate content of the initiator on the gel formation time. Referring to fig. 11 of the specification, as the content of organozirconium decreases, the crosslinking time gradually increases from 60min to 180min.
The working fluids prepared according to examples 31, 32, 33, 34, which block the transmission of pressure to the formation aperture, were tested for the effect of the potassium persulfate content of the initiator on the gel formation time, with other conditions unchanged. Referring to fig. 12 of the specification, as the content of organozirconium decreases, the crosslinking time gradually increases from 22min to 33min.
The working fluids prepared according to examples 17, 18, 19, which block the transmission of pressure to the formation aperture, were tested for viscoelasticity of the pressure transmission barrier at different temperatures. Referring to fig. 13-15 of the specification, as can be seen from the comparison of the loss modulus with the storage modulus, the storage modulus is larger than the loss modulus, it can be shown that the gel mainly deforms elastically, the gel is close to a solid state, and the elasticity is good.
In view of the foregoing, it will be appreciated by those skilled in the art that, after reading the present specification, various other modifications can be made in accordance with the technical scheme and concepts of the present invention without the need for creative mental efforts, and the modifications are within the scope of the present invention.

Claims (6)

1. The preparation method of the working fluid for blocking the drilling fluid to transfer pressure to the stratum hole gap is characterized by comprising the following steps of: the working solution comprises deionized water, a monomer, a cross-linking agent, an initiator and a polymerization inhibitor; wherein the monomer is N- (2-hydroxyethyl) acrylamide, and is used for being dissolved in deionized water, and the concentration of the dissolved monomer is more than 15mg/mL; the mass ratio of the cross-linking agent to the monomer is 0.01-0.5 wt%, and the mass ratio of the initiator to the monomer is 0.024-10 wt%; the polymerization inhibitor is p-benzoquinone, and the mass ratio of the polymerization inhibitor to the monomer is 0.001-0.044 wt%; the working solution is used for carrying out monomer crosslinking reaction at the temperature of 90-120 ℃;
The preparation method comprises the following steps: placing monomer N- (2-hydroxyethyl) acrylamide into a container, adding deionized water, and fully stirring for dissolution; after the monomer is completely dissolved, adding a corresponding cross-linking agent, an initiator and a polymerization inhibitor to prepare the working solution.
2. The method for preparing the working fluid for blocking the transmission of pressure from the drilling fluid to the formation perforation according to claim 1, wherein the method comprises the following steps: the cross-linking agent is N-N methylene bisacrylamide or organozirconium.
3. The method for preparing the working fluid for blocking the transmission of pressure from the drilling fluid to the formation perforation according to claim 2, wherein the method comprises the following steps: the initiator is ammonium persulfate, potassium persulfate or sodium persulfate.
4. A method of preparing a working fluid for blocking the transmission of drilling fluid pressure to a formation perforation as claimed in claim 3, wherein: the cross-linking agent is N-N methylene bisacrylamide, the initiator is ammonium persulfate, and the polymerization inhibitor is p-benzoquinone.
5. The method for preparing the working fluid for blocking the transmission of pressure from the drilling fluid to the formation hole gap according to claim 1 or 4, wherein the method comprises the following steps: the concentration of the monomer is A-100 mg/mL, wherein A is more than 15mg/mL.
6. The method for preparing the working fluid for blocking the transmission of pressure from the drilling fluid to the formation perforation according to claim 1, wherein the method comprises the following steps: the initiator is in situ configured.
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