CN116536035A - Controllable cured resin plugging system suitable for malignant lost circulation stratum and preparation method and application thereof - Google Patents

Controllable cured resin plugging system suitable for malignant lost circulation stratum and preparation method and application thereof Download PDF

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CN116536035A
CN116536035A CN202310350159.5A CN202310350159A CN116536035A CN 116536035 A CN116536035 A CN 116536035A CN 202310350159 A CN202310350159 A CN 202310350159A CN 116536035 A CN116536035 A CN 116536035A
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resin
malignant
lost circulation
plugging
combination
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CN116536035B (en
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白英睿
杨景斌
孙金声
吕开河
朗有明
刘源
杨珂晴
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China University of Petroleum East China
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China University of Petroleum East China
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    • 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
    • EFIXED CONSTRUCTIONS
    • E21EARTH OR ROCK DRILLING; MINING
    • E21BEARTH OR ROCK DRILLING; OBTAINING OIL, GAS, WATER, SOLUBLE OR MELTABLE MATERIALS OR A SLURRY OF MINERALS FROM WELLS
    • E21B33/00Sealing or packing boreholes or wells
    • E21B33/10Sealing or packing boreholes or wells in the borehole
    • E21B33/13Methods or devices for cementing, for plugging holes, crevices or the like

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Abstract

The invention provides a controllable curing resin plugging system suitable for a malignant lost circulation stratum, and a preparation method and application thereof. The controllable curing resin plugging system is prepared from the following raw materials in percentage by mass: 35-55% of resin matrix, 1-15% of curing agent, 1-10% of dispersing agent, 1-5% of solubilizer, 1-3% of catalyst, 1-3% of cross-linking agent, 1-5% of flow-type regulator, 1-8% of weighting material and the balance of water, wherein the total content of all components is hundred percent. The invention also provides a preparation method of the plugging system. The controllable curing resin plugging system is suitable for plugging the drilling fluid leakage of a malignant lost circulation stratum, has excellent high-temperature high-pressure controllability and long-term stable plugging capability, is wide in applicable temperature and crack types, is controllable in curing time and temperature, and can realize high one-time plugging success rate.

Description

Controllable cured resin plugging system suitable for malignant lost circulation stratum and preparation method and application thereof
Technical Field
The invention relates to a controllable curing resin plugging system suitable for a malignant lost circulation stratum, and a preparation method and application thereof, and belongs to the technical field of drilling fluid leakage prevention and plugging.
Background
The lost circulation is the phenomenon that a large amount of drilling fluid leaks into the stratum in the drilling process, so that a large amount of drilling fluid is lost, the drilling period is prolonged, and complex conditions such as well collapse, blowout, drill sticking and the like can be caused by improper treatment, so that serious engineering accidents are caused. At present, malignant lost circulation is one of the most common and difficult to manage complex accidents of drilling engineering, and has become one of the key difficulties in restricting the drilling engineering. Loss of return (Q) DFL ≥30m 3 And/h) is a malignant loss, and severe loss of a fracture (fracture hole) development stratum can be classified as malignant lost circulation. At present, the problems of well leakage, especially malignant well leakage of a fractured stratum, are not solved at home and abroad, the drilling time and economic loss are huge, and the worldwide difficult problem of restricting the progress of oil and gas exploration and development is already caused.
The Chinese patent document CN113897186A discloses an oil-based gel consolidation plugging system for oil-based drilling fluid applicable to a malignant leakage stratum and a preparation method thereof, wherein the oil-based gel in the plugging system is crosslinked by flexible monomers and matched with rigid units, so that the structural stability of the gel can be effectively improved; the curable material can be combined with the oil-based gel, and a medium-high temperature curing agent is matched to realize graded curing, so that the leakage of the oil-based plugging slurry in the stratum is reduced, and the consolidation strength of the oil-based gel is improved; the slow release time of cement is adjusted by using a capsule demulsifier in the oil-based cement part, and an plugging layer mainly comprising oil-based gel, a curable material and oil-based cement is formed, so that the malignant leakage stratum is effectively plugged. However, the plugging system provided by the invention has poor controllability and insufficient high-temperature stability, and long-term plugging in a malignant leakage stratum is difficult to realize. The Chinese patent document CN112980407A discloses a temperature-controllable gel plugging agent, a preparation method and application thereof, and the plugging agent can respectively regulate and control the gel forming time and the gel forming strength of a plugging gel system according to different leakage layer temperatures, thereby realizing intelligent controllability. But the high temperature stability is poor, and the controllable strength cannot be realized under the high temperature condition. Chinese patent document CN115160998A discloses a high-temperature-resistant high-strength curable resin gel plugging agent and a preparation method and application thereof, but the plugging agent is difficult to control in controllability and poor in long-term stable plugging effect under the high-temperature environment condition of a malignant lost circulation stratum. The Chinese patent document CN110003864A provides a plugging agent for plugging in drilling fluid, which comprises the following components in percentage by weight: 50-95% of main agent, 1-30% of curing agent, 0-10% of accelerator, 1-60% of density regulator and 1-20% of viscosity regulator, and all the components are added up to one hundred percent. The plugging agent has the advantages of complicated preparation method, higher viscosity and certain difficulty in on-site pumping.
Therefore, a continuous phase controllable curing resin plugging system which is easy to prepare, is filled strongly, is resident strongly, is high-temperature resistant and is high-strength and is cured or crosslinked underground is developed, so that the plugging system is not limited by a fracture-cavity leakage channel, meets the plugging requirements of different combinations of fracture-cavity carbonate rock, and has important significance for effectively solving the problem of leakage of drilling fluid in a malignant leakage stratum.
Disclosure of Invention
Aiming at the defects of the prior art, in particular to the problems of complex preparation process, insufficient pressure bearing plugging capability, poor long-term temperature resistance, limited applicable temperature and crack size range, poor controllability and the like of the plugging material conventionally used in the existing malignant lost circulation stratum, the invention provides a controllable curing resin plugging system suitable for the malignant lost circulation stratum and a preparation method and application thereof. The controllable curing resin plugging system is suitable for plugging the drilling fluid leakage of a malignant lost circulation stratum, has excellent high-temperature high-pressure controllability and long-term stable plugging capability, is wide in applicable temperature and crack types, is controllable in curing time and temperature, and can realize high one-time plugging success rate.
The technical scheme of the invention is as follows:
a controllable curing resin plugging system suitable for a malignant lost circulation stratum is prepared from the following raw materials in percentage by mass: 35-55% of resin matrix, 1-15% of curing agent, 1-10% of dispersing agent, 1-5% of solubilizer, 1-3% of catalyst, 1-3% of cross-linking agent, 1-5% of flow-type regulator, 1-8% of weighting material and the balance of water, wherein the total content of all components is hundred percent.
According to the invention, the resin matrix is preferably one or more than two of urea resin, phenolic resin, unsaturated polyester resin and polyimide resin; further preferably, the resin matrix is a combination of urea-formaldehyde resin, phenolic resin and unsaturated polyester resin, wherein the mass ratio of the urea-formaldehyde resin to the phenolic resin to the unsaturated polyester resin is 2-5:2-3:0.5-1.
According to the invention, the urea-formaldehyde resin is a water-soluble urea-formaldehyde resin, the molecular weight of which is not particularly limited, and urea-formaldehyde resin with weight average molecular weight of 1000-3000 is preferable; the phenolic resin is water-soluble phenolic resin, is granular or powdery, has a molecular weight not particularly limited, and is preferably a phenolic resin with a weight average molecular weight of 1000-2000; the unsaturated polyester resin is a combination of isophthalic acid unsaturated polyester resin and bisphenol A unsaturated polyester resin, and the mass ratio of the isophthalic acid unsaturated polyester resin to the bisphenol A unsaturated polyester resin is 1-5:1; the polyimide resin is water-soluble polyimide resin.
According to the invention, preferably, the curing agent is an amine curing agent and/or an anhydride curing agent; the amine curing agent is one or the combination of more than two of ethylenediamine, diethylenetriamine and dicyandiamide; the anhydride curing agent is one or the combination of more than two of phthalic anhydride, tetrahydrophthalic anhydride and 2, 3',4' -diphenyl ether tetracarboxylic dianhydride; further preferably, the curing agent is a combination of ethylenediamine, dicyandiamide and phthalic anhydride, wherein the mass ratio of ethylenediamine, dicyandiamide and phthalic anhydride is 1-5:2-3:1-5.
According to the invention, the dispersing agent is one or a combination of more than two of polyethylene glycol, ethanol and n-butanol; further preferred is a combination of polyethylene glycol and n-butanol, wherein the mass ratio of polyethylene glycol to n-butanol is 1-5:1, and the weight average molecular weight of the polyethylene glycol is 600-1000.
According to a preferred embodiment of the present invention, the solubilizing agent is a combination of sodium dodecyl sulfate, sorbitan fatty acid (span 60) and betaine type surfactant, wherein the mass ratio of sodium dodecyl sulfate, sorbitan fatty acid (span 60) and betaine type surfactant is 3-5:2-4:1-2, and the betaine type surfactant is an alkyl betaine surfactant such as dodecyl dimethyl betaine.
According to the invention, the catalyst is preferably one or a combination of more than two of amine catalysts, phenol catalysts and substituted urea catalysts; the amine catalyst is one or the combination of more than two of pyridine, N-dimethylcyclohexylamine and triethanolamine; the phenolic catalyst is one or a combination of more than two of phenol, resorcinol and bisphenol A; the substituted urea catalyst is one or the combination of more than two of N-p-chlorophenyl-N, N '-dimethyl urea, N' - (3, 4-dichlorophenyl) -N, N-dimethyl urea (CAS number: 330-54-1) and dimethyl imidazole urea; further preferred, the catalyst is a combination of triethanolamine, phenol and N '- (3, 4-dichlorophenyl) -N, N-dimethylurea, wherein the mass ratio of triethanolamine, phenol and N' - (3, 4-dichlorophenyl) -N, N-dimethylurea is from 1 to 11:1 to 3:1 to 4.
According to the invention, the cross-linking agent is one or a combination of more than two of hydroxyethyl methacrylate, hydroxypropyl methacrylate, N-methylolacrylamide and ethylene glycol dimethacrylate; further preferably, the cross-linking agent is a combination of N-methylolacrylamide, hydroxyethyl methacrylate and ethylene glycol dimethacrylate, wherein the mass ratio of the N-methylolacrylamide, the hydroxyethyl methacrylate and the ethylene glycol dimethacrylate is 1-5:2-3:1-3.
According to the invention, the flow pattern regulator is one or a combination of more than two of sodium bentonite, lithium bentonite, starch and sodium carboxymethyl cellulose; further preferably, the flow pattern regulator is a combination of sodium bentonite, lithium bentonite and sodium carboxymethyl cellulose, wherein the mass ratio of the sodium bentonite, the lithium bentonite and the sodium carboxymethyl cellulose is 1-5:1-4:1-3.
According to the invention, preferably, the weighting material is one or the combination of more than two of barite, calcium carbonate, asbestos, ceramsite, walnut shells and sand grains; further preferred is a combination of barite, asbestos and sand particles, wherein the mass ratio of barite, asbestos and sand particles is 3-12:3:1-4.
According to the invention, the preparation method of the controllable curing resin plugging system suitable for the malignant lost circulation stratum comprises the following steps:
(1) Sequentially adding a catalyst, a dispersing agent, a solubilizer and a curing agent into water, and uniformly dispersing to obtain a curing agent system A;
(2) Adding the resin matrix into the curing agent system A, and uniformly stirring to obtain a mixed system B;
(3) Adding a cross-linking agent, a flow pattern regulator and a weighting material into the mixed system B, and uniformly stirring to obtain a mixed system C;
(4) And stirring the mixed system C under the heating condition to obtain the controllable curing resin plugging system suitable for the malignant lost circulation stratum.
According to a preferred embodiment of the present invention, the dispersing step in step (1) is: firstly, carrying out mechanical dispersion by using a vortex machine and then carrying out ultrasonic dispersion, wherein the rotating speed of the mechanical dispersion is 500-1000rpm, and more preferably 700-800rpm; the temperature of the mechanical dispersion is 20-40 ℃, and more preferably 25-30 ℃; the dispersing time is 5-20min, more preferably 10-15min; the temperature of ultrasonic dispersion is 20-30 ℃, and more preferably 24-28 ℃; the ultrasonic dispersion time is 10-20min, and more preferably 13-17min.
According to a preferred embodiment of the invention, the temperature of the stirring in step (2) is 20-35 ℃, further preferably 25-30 ℃; the stirring speed is 300 to 500 rpm, more preferably 350 to 450 rpm; the stirring time is 30 to 60 minutes, more preferably 40 to 50 minutes.
According to a preferred embodiment of the invention, the temperature of the stirring in step (3) is 25-30 ℃, further preferably 26-28 ℃; the stirring speed is 500 to 1000rpm, more preferably 700 to 800rpm; the stirring time is 50 to 80 minutes, more preferably 60 to 70 minutes.
Preferably according to the invention, the heating in step (4) is to a temperature of 40-70 ℃, further preferably 48-62 ℃; the stirring speed is 400-700 rpm, and more preferably 500-600 rpm; the stirring time is 40-100 minutes, more preferably 50-80 minutes; the stirring is performed under nitrogen or argon atmosphere.
According to the invention, the application of the controllable curing resin plugging system suitable for the malignant lost circulation stratum is used for plugging the drilling fluid leakage of the carbonate fracture-cavity type malignant lost circulation stratum.
According to the invention, the following method is preferred: the prepared controllable curing resin plugging system suitable for the malignant lost circulation stratum is mixed with the drilling fluid and then is injected into a stratum lost circulation hole, and the high-strength plugging layer is formed by crosslinking and curing under the stratum temperature condition; or the controllable curing resin plugging system is cured in advance to generate a consolidated body, then particles are prepared and injected into the stratum while drilling, and at the stratum temperature, the bonding effect is generated among the resin particles to form an integral plugging layer, so that the fracture and hole can be plugged.
The invention has the technical characteristics and beneficial effects that:
1. the controllable curing resin plugging system uses the resin material as a main material, adjusts and controls the curing time, the curing temperature and the curing strength of the resin by adjusting the addition amount and the concentration of the curing agent, the catalyst, the dispersing agent, the solubilizer and other external additives, and prepares the controllable curing resin plugging system by optimizing the weighting material, so that the application temperature range is wide, the bonding strength is high, the curing process is controllable, and the integral effective high-strength plugging of a malignant lost circulation stratum under the high-temperature condition can be realized. The invention selects a specific resin matrix as a main material, and the resin matrix is adhered to form a high-strength three-dimensional net structure after solidification; the addition of the cross-linking agent can effectively improve the cross-linking degree of the resin, effectively improve the curing strength of the plugging system and effectively fill cracks.
2. The controllable curing resin plugging system disclosed by the invention has the advantages that the raw material components act synergistically, so that the plugging system disclosed by the invention has high curing bonding strength, small slurry viscosity and high quality stability, the strength is rapidly improved under the condition of pressure bearing plugging, and the plugging system can be subjected to self-crosslinking reaction in cracks, cracks and karst cave to form a three-dimensional network structure. Meanwhile, the controllable curing resin plugging system is bonded with sand grains to form a high-strength consolidated body, so that strong resident filling is realized, and the strength of a plugging layer is improved.
3. The controllable curing resin plugging system has 160 ℃ temperature resistance, 3-10h controllable curing time, the compressive strength of the consolidated body is more than 60MPa, and the plugging strength of the plugging system for cracks is more than 15MPa. The controllable curing resin plugging system can realize strong residence capacity in a leakage channel, can realize integral plugging, has wide application range to crack size, can realize long-term stable high-strength plugging under high temperature conditions, can effectively slow down the leakage of drilling fluid in a malignant lost circulation stratum, and improves the one-time plugging success rate.
4. The controllable curing resin plugging system can be directly compounded and injected with drilling fluid, can be used in cooperation with bridging plugging materials, is injected in a pumping-while-drilling mode, and is simple and feasible in preparation method, low in cost and convenient to produce and operate.
Detailed Description
The invention is further illustrated by, but not limited to, the following specific examples.
The raw materials used in the examples are all conventional raw materials and are commercially available; the methods are prior art unless specified otherwise.
The urea-formaldehyde resin used in the examples is water-soluble urea-formaldehyde resin with weight average molecular weight of 2000;
the phenolic resin is water-soluble phenolic resin, and the weight average molecular weight is 1200;
the unsaturated polyester resin is the combination of isophthalic acid unsaturated polyester resin and bisphenol A unsaturated polyester resin, the mass ratio of the isophthalic acid unsaturated polyester resin to the bisphenol A unsaturated polyester resin is 2:1, the weight average molecular weight of the isophthalic acid unsaturated polyester resin is 800, and the weight average molecular weight of the bisphenol A unsaturated polyester resin is 600;
the polyethylene glycol used had a weight average molecular weight of 800.
Example 1
A controllable curing resin plugging system suitable for a malignant lost circulation stratum is prepared from the following raw materials in percentage by mass: 45% of resin matrix, 7% of curing agent, 5% of dispersing agent, 3% of solubilizer, 2% of catalyst, 2% of cross-linking agent, 3% of flow-pattern regulator, 5% of weighting material and the balance of water, wherein the total content of the components is hundred percent.
The resin matrix is a combination of urea-formaldehyde resin, phenolic resin and unsaturated polyester resin, wherein the mass ratio of the urea-formaldehyde resin to the phenolic resin to the unsaturated polyester resin is 4:3:1.
The curing agent is a combination of ethylenediamine, dicyandiamide and phthalic anhydride, wherein the mass ratio of ethylenediamine, dicyandiamide and phthalic anhydride is 3:2:1.
The dispersing agent is a combination of polyethylene glycol and n-butanol, wherein the mass ratio of the polyethylene glycol to the n-butanol is 3:1.
The solubilizer is a combination of sodium dodecyl sulfate, fatty acid sorbitan (span 60) and dodecyl dimethyl betaine, wherein the mass ratio of the sodium dodecyl sulfate to the fatty acid sorbitan (span 60) to the dodecyl dimethyl betaine is 4:3:1.
The catalyst is a combination of triethanolamine, phenol and N '- (3, 4-dichlorophenyl) -N, N-dimethylurea, wherein the mass ratio of the triethanolamine to the phenol to the N' - (3, 4-dichlorophenyl) -N, N-dimethylurea is 6:3:1.
The cross-linking agent is a combination of N-methylolacrylamide, hydroxyethyl methacrylate and ethylene glycol dimethacrylate, wherein the mass ratio of the N-methylolacrylamide to the hydroxyethyl methacrylate to the ethylene glycol dimethacrylate is 5:2:1.
The flow-type regulator is a combination of sodium bentonite, lithium bentonite and sodium carboxymethyl cellulose, wherein the mass ratio of the sodium bentonite to the lithium bentonite to the sodium carboxymethyl cellulose is 5:4:2.
The weighting material is a combination of barite, asbestos and sand grains, wherein the mass ratio of the barite, the asbestos and the sand grains is 6:3:2.
The preparation method of the controllable curing resin plugging system suitable for the malignant lost circulation stratum comprises the following steps:
(1) Sequentially adding a catalyst, a dispersing agent, a solubilizer and a curing agent into a centrifuge tube filled with water, placing the centrifuge tube in a vortex instrument, mechanically dispersing at 25 ℃ and a rotating speed of 750rpm for 12min, and then ultrasonically dispersing the centrifuge tube at 25 ℃ for 15min to obtain a curing agent system A;
(2) Adding the resin matrix into the curing agent system A obtained in the step (1), stirring at the speed of 400 rpm for 45 minutes at the temperature of 25 ℃, and uniformly mixing to obtain a mixed system B;
(3) Adding a cross-linking agent, a flow pattern regulator and a weighting material into the mixed system B obtained in the step (2), and stirring for 75 minutes at the stirring temperature of 27 ℃ and the stirring speed of 750 revolutions per minute to obtain a mixed system C;
(4) Pouring the obtained mixed system C into a four-neck flask, heating in a water bath to 50 ℃, introducing nitrogen, stirring for 60min at the temperature of 50 ℃ and the rotating speed of 500 r/min to uniformly disperse the mixed system C, and obtaining a controllable curing resin plugging system suitable for a malignant lost circulation stratum, which is marked as a sample S1.
Example 2
A controllable curing resin plugging system suitable for a malignant lost circulation stratum is prepared from the following raw materials in percentage by mass: 55% of resin matrix, 7% of curing agent, 5% of dispersing agent, 3% of solubilizer, 2% of catalyst, 2% of cross-linking agent, 3% of flow-pattern regulator, 5% of weighting material, and the balance of water, wherein the total content of the components is hundred percent.
Wherein the types of the resin matrix, the curing agent, the dispersing agent, the solubilizer, the catalyst, the crosslinking agent, the flow-pattern modifier, and the weighting material are selected as described in example 1.
The preparation method of the controllable curing resin plugging system suitable for the malignant lost circulation stratum is as described in the embodiment 1, and the prepared controllable curing resin plugging system suitable for the malignant lost circulation stratum is marked as a sample S2.
Example 3
A controllable curing resin plugging system suitable for a malignant lost circulation stratum is prepared from the following raw materials in percentage by mass: 35% of resin matrix, 7% of curing agent, 5% of dispersing agent, 3% of solubilizer, 2% of catalyst, 2% of cross-linking agent, 3% of flow-pattern regulator, 5% of weighting material and the balance of water, wherein the total content of the components is hundred percent.
Wherein the types of the resin matrix, the curing agent, the dispersing agent, the solubilizer, the catalyst, the crosslinking agent, the flow-pattern modifier, and the weighting material are selected as described in example 1.
The preparation method of the controllable curing resin plugging system suitable for the malignant lost circulation stratum is as described in the embodiment 1, and the prepared controllable curing resin plugging system suitable for the malignant lost circulation stratum is marked as a sample S3.
Example 4
A controlled cure resin plugging system suitable for use in a malignant lost circulation formation is as described in example 1, except that: the curing agent was ethylenediamine and the other conditions were the same as in example 1.
The preparation method of the controllable curing resin plugging system suitable for the malignant lost circulation stratum is as described in the embodiment 1, and the prepared controllable curing resin plugging system suitable for the malignant lost circulation stratum is marked as a sample S4.
Example 5
A controlled cure resin plugging system suitable for use in a malignant lost circulation formation is as described in example 1, except that: the dispersant was polyethylene glycol, and the other conditions were the same as in example 1.
The preparation method of the controllable curing resin plugging system suitable for the malignant lost circulation stratum is as described in the embodiment 1, and the prepared controllable curing resin plugging system suitable for the malignant lost circulation stratum is marked as a sample S5.
Example 6
A controlled cure resin plugging system suitable for use in a malignant lost circulation formation is as described in example 1, except that: the solubilizer was sodium dodecyl sulfate and the other conditions were the same as in example 1.
The preparation method of the controllable curing resin plugging system suitable for the malignant lost circulation stratum is as described in the embodiment 1, and the prepared controllable curing resin plugging system suitable for the malignant lost circulation stratum is marked as a sample S6.
Example 7
A controlled cure resin plugging system suitable for use in a malignant lost circulation formation is as described in example 1, except that: the catalyst was triethanolamine and the other conditions were the same as in example 1.
The preparation method of the controllable curing resin plugging system suitable for the malignant lost circulation stratum is as described in the embodiment 1, and the prepared controllable curing resin plugging system suitable for the malignant lost circulation stratum is marked as a sample S7.
Example 8
A controlled cure resin plugging system suitable for use in a malignant lost circulation formation is as described in example 1, except that: the crosslinking agent was N-methylolacrylamide, and the other conditions were the same as in example 1.
The preparation method of the controllable curing resin plugging system suitable for the malignant lost circulation stratum is as described in the embodiment 1, and the prepared controllable curing resin plugging system suitable for the malignant lost circulation stratum is marked as a sample S8.
Example 9
A controlled cure resin plugging system suitable for use in a malignant lost circulation formation is as described in example 1, except that: the flow regulator was sodium carboxymethyl cellulose, and the other conditions were the same as in example 1.
The preparation method of the controllable curing resin plugging system suitable for the malignant lost circulation stratum is as described in the embodiment 1, and the prepared controllable curing resin plugging system suitable for the malignant lost circulation stratum is marked as a sample S9.
Example 10
A controlled cure resin plugging system suitable for use in a malignant lost circulation formation is as described in example 1, except that: the weight material was asbestos, and the other conditions were the same as in example 1.
The preparation method of the controllable curing resin plugging system suitable for the malignant lost circulation stratum is as described in the embodiment 1, and the prepared controllable curing resin plugging system suitable for the malignant lost circulation stratum is marked as a sample S10.
Example 11
A controlled cure resin plugging system suitable for use in a malignant lost circulation formation is as described in example 1, except that: the resin matrix was urea-formaldehyde resin, and the other conditions were the same as in example 1.
The preparation method of the controllable curing resin plugging system suitable for the malignant lost circulation stratum is as described in the embodiment 1, and the prepared controllable curing resin plugging system suitable for the malignant lost circulation stratum is marked as a sample S11.
Example 12
A controlled cure resin plugging system suitable for use in a malignant lost circulation formation is as described in example 1, except that: the resin matrix was phenolic resin, and the other conditions were the same as in example 1.
The preparation method of the controllable curing resin plugging system suitable for the malignant lost circulation stratum is as described in the embodiment 1, and the prepared controllable curing resin plugging system suitable for the malignant lost circulation stratum is marked as a sample S12.
Example 13
A controlled cure resin plugging system suitable for use in a malignant lost circulation formation is as described in example 1, except that: the resin matrix was an unsaturated polyester resin, and the other conditions were the same as in example 1.
The preparation method of the controllable curing resin plugging system suitable for the malignant lost circulation stratum is as described in the embodiment 1, and the prepared controllable curing resin plugging system suitable for the malignant lost circulation stratum is marked as a sample S13.
Comparative example 1
A resin plugging system as described in example 1, except that: no curing agent was added.
The preparation of the resin plugging system was as described in example 1, and the product obtained was designated as D1.
Comparative example 2
A resin plugging system as described in example 1, except that: no dispersant was added.
The preparation of the resin plugging system was as described in example 1, and the product obtained was designated as D2.
Comparative example 3
A resin plugging system as described in example 1, except that: no solubilizer was added.
The preparation of the resin plugging system was as described in example 1, and the product obtained was designated as D3.
Comparative example 4
A resin plugging system as described in example 1, except that: no catalyst was added.
The preparation of the resin plugging system was as described in example 1, and the product obtained was designated as D4.
Comparative example 5
A resin plugging system as described in example 1, except that: no crosslinking agent is added.
The preparation of the resin plugging system was as described in example 1, and the product obtained was designated as D5.
Comparative example 6
A resin plugging system as described in example 1, except that: no flow regulator was added.
The preparation of the resin plugging system was as described in example 1, and the product obtained was designated as D6.
Comparative example 7
A resin plugging system as described in example 1, except that: no weighting material is added.
The preparation of the resin plugging system was as described in example 1 and the product obtained was designated as D7.
Comparative example 8
A resin plugging system as described in example 1, except that: the resin matrix is epoxy resin.
The preparation of the resin plugging system was as described in example 1, and the product obtained was designated as D8.
Comparative example 9
A resin plugging system as described in example 1, except that: the resin matrix is bismaleimide resin.
The preparation of the resin plugging system was as described in example 1 and the product obtained was designated D9.
Test examples
The resin plugging systems prepared in the examples and the comparative examples are subjected to high-temperature high-pressure plugging performance test and compression resistance test.
Test 1: high-temperature high-pressure plugging performance test for controllable curing resin plugging system
And (3) researching the pressure-bearing plugging performance of the controllable curing resin plugging system on the cracks by using a high-temperature high-pressure crack physical simulation device. The steel fracture module is used for simulating a fractured leakage stratum, the fracture module is a single wedge-shaped fracture, the entrance fracture width is 1, 3 and 5mm respectively, the exit fracture width is 0.5, 1.5 and 2.5mm respectively, and the fracture length is 200mm.
Determination of the curing time: and (3) placing 30mL of the resin plugging system into a test tube, placing into an electric heating vacuum drying oven, standing at 160 ℃ for solidification, taking out at regular time, and observing the flowing condition of liquid in the temperature-resistant test tube, wherein the time when the resin is solidified and inverted and does not flow is the solidification time.
The high-temperature high-pressure plugging test steps are as follows: (a) Adjusting the temperature of the heating box to 160 ℃ of the simulated stratum; (b) Placing a steel crack core with the required seam width into a core holder, and adding confining pressure to 15MPa; (c) Injecting simulated drilling fluid (the main components of the simulated drilling fluid are bentonite and water, and the content is 3 wt%) into the fracture core at an injection rate of 2.5mL/min until the simulated drilling fluid is saturated; (d) Injecting the resin plugging system solution into the fractured rock at the injection rate of 2.5mL/min until the fracture outlet completely produces the solution; (e) Sealing the crack core model, and standing until the curing reaction of the solution of the controllable curing resin plugging system is completed; (f) And reversely injecting simulated drilling fluid into the fracture core at the injection rate of 2.5mL/min, recording the injection pressure change in real time by using data software, and obtaining the highest pressure when the drilling fluid leaks from the outlet end of the fracture model, namely the pressure-bearing plugging strength of the resin plugging system to the fracture.
Defining the plugging strength evaluation standard of the controllable curing resin plugging system as follows: the highest pressure of the outlet end of the wedge-shaped crack is more than 15MPa, and the plugging strength is strong; when the highest pressure of the outlet end of the wedge-shaped crack is between 10 and 15MPa, the plugging strength is medium; when the highest pressure of the outlet end of the wedge-shaped crack is between 5 and 10MPa, the plugging strength is qualified; the highest pressure of the outlet end of the wedge-shaped crack is less than 5MPa, and the plugging strength is low.
The results of the high temperature and high pressure plugging performance of the controlled curing resin plugging systems prepared in the examples and comparative examples are shown in Table 1.
TABLE 1 results of high temperature high pressure plugging performance of resin plugging systems in wedge-shaped cracks
As can be seen from the example data in table 1, the high temperature and high pressure plugging performance of the controllably curable resin plugging system is greatly affected by the resin matrix, curing agent, crosslinking agent and weighting material, and is secondarily affected by the catalyst, dispersant, flow pattern regulator and other externally added additives. As can be seen from the example data in Table 1, the controllable curing resin plugging system prepared in the example of the invention has better high-temperature high-pressure plugging performance, and the maximum pressure-bearing plugging capability in wedge-shaped cracks with outlet seam widths of 0.5mm, 1.5mm and 2.5mm can be respectively 20.5MPa, 19.3MPa and 18.9MPa. The resin matrix in the controllable curing resin plugging system can be cured to form a high-strength consolidated body under the synergistic effect of the curing agent, the cross-linking agent, the weighting material and other additive assistants, so that the efficient plugging of cracks is realized. The comparative example of the present invention was inferior to the examples, further demonstrating the synergy between the materials of the present invention.
Test 2: compression resistance test of controllable curing resin plugging system
The mould specification for preparing the compressive strength sample of the controllable curing resin plugging system is 50.8x50.8x50.8mm 3 . Pouring the prepared resin plugging system solution into a mould coated with a release agent, putting into an electrothermal vacuum drying oven, solidifying and molding at 160 ℃, demoulding, cooling to room temperature, and performing sample test, wherein the pressure loading rate during test is 1.2kN/s, and the compressive strength is calculated according to a formulaThe following is shown:
wherein P is the compressive strength of a resin plugging system sample, and the unit is MPa; f is data obtained during compression testing of a resin plugging system sample, namely an external force load loaded by the compression-resistant and fracture-resistant integrated machine, and the unit is kN; s is the stress area of a resin plugging system sample, and the unit is mm 2 . The sample in this test was 2580.64mm 2
Defining the compressive strength of the resin plugging system to be more than or equal to 50MPa, and the deformation recovery rate to be more than or equal to 90% as the priority; the compressive strength is between 20MPa and 50MPa, and the deformation recovery rate is 80 to 90 percent; the compressive strength is less than 20MPa, and the deformation recovery rate is less than 80 percent, so that the product is unqualified.
The compressive properties of the controlled curing resin plugging systems prepared in the examples and comparative examples are shown in Table 2.
Table 2 results of compressive strength test of samples of resin plugging systems
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Table 2 shows the compression resistance test results of samples formed from the controlled cure resin plugging system at a cure temperature of 160 ℃. As can be seen from the data in Table 2, the samples of the controllable curing resin plugging system in the examples have compressive strength of more than 20MPa, deformation recovery rate of more than 80% and qualified compressive strength grades. Under the optimal formula, as shown in the results of the example 1, the compressive strength of the sample of the controllable curing resin plugging system is more than 60MPa, the deformation recovery rate is more than 90%, and the compressive strength grade is excellent. The comparative examples of the present invention, however, reduced the addition of some adjuvants and deteriorated the effect, as compared with the examples, further demonstrated the synergistic interaction between the raw materials of the present invention. In conclusion, the resin matrix in the controllable curing resin plugging system can be better cured to form a high-strength consolidated body only under the synergistic effect of the curing agent, the cross-linking agent, the weighting material and other external additives in a certain proportion, so that excellent compressive strength is achieved.
After the controllable curing resin plugging system is mixed with formation water and drilling fluid, standing and observing, the two systems after being mixed are found to be uniform and basically unchanged, no obvious precipitate is found, and the compatibility of the system is good; overcomes the defect of incompatibility between the existing resin plugging system and reservoir fluid or working fluid.
The preferred embodiments of the present invention have been described in detail above, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, a number of simple variants of the technical solution of the invention are possible, including combinations of the individual technical features in any other suitable way, which simple variants and combinations should likewise be regarded as being disclosed by the invention, all falling within the scope of protection of the invention.

Claims (10)

1. The controllable curing resin plugging system suitable for the malignant lost circulation stratum is characterized by being prepared from the following raw materials in percentage by mass: 35-55% of resin matrix, 1-15% of curing agent, 1-10% of dispersing agent, 1-5% of solubilizer, 1-3% of catalyst, 1-3% of cross-linking agent, 1-5% of flow-type regulator, 1-8% of weighting material and the balance of water, wherein the total content of all components is hundred percent.
2. The controllable curing resin plugging system suitable for the malignant lost circulation stratum is characterized in that the resin matrix is one or a combination of more than two of urea formaldehyde resin, phenolic resin, unsaturated polyester resin and polyimide resin; preferably, the resin matrix is a combination of urea-formaldehyde resin, phenolic resin and unsaturated polyester resin, wherein the mass ratio of the urea-formaldehyde resin to the phenolic resin to the unsaturated polyester resin is 2-5:2-3:0.5-1.
3. The controllable curing resin plugging system suitable for the malignant lost circulation stratum is characterized in that the urea-formaldehyde resin is water-soluble urea-formaldehyde resin; the phenolic resin is water-soluble phenolic resin; the unsaturated polyester resin is a combination of isophthalic acid unsaturated polyester resin and bisphenol A unsaturated polyester resin, and the mass ratio of the isophthalic acid unsaturated polyester resin to the bisphenol A unsaturated polyester resin is 1-5:1; the polyimide resin is water-soluble polyimide resin.
4. The controllable curing resin plugging system suitable for the malignant lost circulation stratum is characterized in that the curing agent is an amine curing agent and/or an anhydride curing agent; the amine curing agent is one or the combination of more than two of ethylenediamine, diethylenetriamine and dicyandiamide; the anhydride curing agent is one or the combination of more than two of phthalic anhydride, tetrahydrophthalic anhydride and 2, 3',4' -diphenyl ether tetracarboxylic dianhydride; preferably, the curing agent is a combination of ethylenediamine, dicyandiamide and phthalic anhydride, wherein the mass ratio of ethylenediamine, dicyandiamide and phthalic anhydride is 1-5:2-3:1-5.
5. The controllable curing resin plugging system suitable for the malignant lost circulation stratum is characterized in that the dispersing agent is one or the combination of more than two of polyethylene glycol, ethanol and n-butanol; preferably a combination of polyethylene glycol and n-butanol, wherein the mass ratio of polyethylene glycol to n-butanol is 1-5:1, and the weight average molecular weight of the polyethylene glycol is 600-1000.
6. The controllable curing resin plugging system suitable for the malignant lost circulation stratum is characterized in that the solubilizer is a combination of sodium dodecyl sulfate, fatty acid sorbitan and betaine type surfactant, wherein the mass ratio of the sodium dodecyl sulfate to the fatty acid sorbitan to the betaine type surfactant is 3-5:2-4:1-2;
the catalyst is one or the combination of more than two of amine catalysts, phenol catalysts and substituted urea catalysts; the amine catalyst is one or the combination of more than two of pyridine, N-dimethylcyclohexylamine and triethanolamine; the phenolic catalyst is one or a combination of more than two of phenol, resorcinol and bisphenol A; the substituted urea catalyst is one or the combination of more than two of N-p-chlorophenyl-N, N '-dimethyl urea, N' - (3, 4-dichlorophenyl) -N, N-dimethyl urea and dimethyl imidazole urea; preferably, the catalyst is a combination of triethanolamine, phenol and N '- (3, 4-dichlorophenyl) -N, N-dimethylurea, wherein the mass ratio of the triethanolamine, the phenol and the N' - (3, 4-dichlorophenyl) -N, N-dimethylurea is 1-11:1-3:1-4.
7. The controllable curing resin plugging system suitable for the malignant lost circulation stratum is characterized in that the cross-linking agent is one or more than two of hydroxyethyl methacrylate, hydroxypropyl methacrylate, N-methylolacrylamide and ethylene glycol dimethacrylate; preferably, the cross-linking agent is a combination of N-methylolacrylamide, hydroxyethyl methacrylate and ethylene glycol dimethacrylate, wherein the mass ratio of the N-methylolacrylamide to the hydroxyethyl methacrylate to the ethylene glycol dimethacrylate is 1-5:2-3:1-3;
the flow pattern regulator is one or the combination of more than two of sodium bentonite, lithium bentonite, starch and sodium carboxymethyl cellulose; preferably, the flow pattern regulator is a combination of sodium bentonite, lithium bentonite and sodium carboxymethyl cellulose, wherein the mass ratio of the sodium bentonite to the lithium bentonite to the sodium carboxymethyl cellulose is 1-5:1-4:1-3;
the weighting material is one or the combination of more than two of barite, calcium carbonate, asbestos, ceramsite, walnut shell and sand grains; preferably, the weighting material is a combination of barite, asbestos and sand, wherein the mass ratio of the barite, the asbestos and the sand is 3-12:3:1-4.
8. A method of preparing a controlled cure resin plugging system for use in a malignant lost circulation formation according to any one of claims 1-7 comprising the steps of:
(1) Sequentially adding a catalyst, a dispersing agent, a solubilizer and a curing agent into water, and uniformly dispersing to obtain a curing agent system A;
(2) Adding the resin matrix into the curing agent system A, and uniformly stirring to obtain a mixed system B;
(3) Adding a cross-linking agent, a flow pattern regulator and a weighting material into the mixed system B, and uniformly stirring to obtain a mixed system C;
(4) And stirring the mixed system C under the heating condition to obtain the controllable curing resin plugging system suitable for the malignant lost circulation stratum.
9. The method of preparing a controlled cure resin plugging system for use in a malignant lost circulation formation according to claim 8, wherein the dispersing step in step (1) is: firstly, carrying out mechanical dispersion by using a vortex machine and then carrying out ultrasonic dispersion, wherein the rotating speed of the mechanical dispersion is 500-1000rpm, preferably 700-800rpm; the temperature of mechanical dispersion is 20-40 ℃, preferably 25-30 ℃; the dispersing time is 5-20min, preferably 10-15min; the temperature of ultrasonic dispersion is 20-30 ℃, preferably 24-28 ℃; the ultrasonic dispersion time is 10-20min, preferably 13-17min;
the temperature of the stirring in the step (2) is 20-35 ℃, preferably 25-30 ℃; the stirring speed is 300-500 rpm, preferably 350-450 rpm; the stirring time is 30-60 minutes, preferably 40-50 minutes;
the temperature of the stirring in the step (3) is 25-30 ℃, preferably 26-28 ℃; the stirring speed is 500-1000rpm, preferably 700-800rpm; the stirring time is 50-80 minutes, preferably 60-70 minutes;
the heating in step (4) is to 40-70 ℃, preferably 48-62 ℃; the stirring speed is 400-700 rpm, preferably 500-600 rpm; the stirring time is 40-100 minutes, preferably 50-80 minutes; the stirring is performed under nitrogen or argon atmosphere.
10. The use of a controllable cured resin plugging system for a malignant lost circulation formation according to claim 1 for drilling fluid leak-off plugging of a carbonate fracture-cave malignant lost circulation formation; preferably, the application method is as follows: the prepared controllable curing resin plugging system suitable for the malignant lost circulation stratum is mixed with the drilling fluid and then is injected into a stratum lost circulation hole, and the high-strength plugging layer is formed by crosslinking and curing under the stratum temperature condition; or the controllable curing resin plugging system is cured in advance to generate a consolidated body, then particles are prepared and injected into the stratum while drilling, and at the stratum temperature, the bonding effect is generated among the resin particles to form an integral plugging layer, so that the fracture and hole can be plugged.
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