CN115322766A - Bi-component low-temperature curable coated proppant and preparation method thereof - Google Patents
Bi-component low-temperature curable coated proppant and preparation method thereof Download PDFInfo
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- CN115322766A CN115322766A CN202210993621.9A CN202210993621A CN115322766A CN 115322766 A CN115322766 A CN 115322766A CN 202210993621 A CN202210993621 A CN 202210993621A CN 115322766 A CN115322766 A CN 115322766A
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/60—Compositions for stimulating production by acting on the underground formation
- C09K8/80—Compositions for reinforcing fractures, e.g. compositions of proppants used to keep the fractures open
- C09K8/805—Coated proppants
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Abstract
The invention relates to a two-component low-temperature curable coated proppant and a preparation method thereof. A two-component curable tectorial membrane proppant comprises a component A and a component B, wherein the component A comprises a pre-cured tectorial membrane proppant, a liquid epoxy resin B, an epoxy resin diluent, a filler and a flow modifier; the component B comprises a pre-cured laminating propping agent, an epoxy resin curing agent, a curing accelerator, a filler and a flow modifier; the pre-cured film-coated propping agent is particles obtained by pre-curing and film-coating aggregate of quartz sand and/or ceramsite by using epoxy resin a, a coupling agent and a curing agent a.
Description
Technical Field
The invention relates to a bi-component low-temperature curable tectorial membrane proppant and a preparation method thereof, and the bi-component low-temperature curable tectorial membrane proppant is used in the field of petroleum and natural gas exploitation.
Background
Over 70 percent of the global conventional oil and gas reservoirs are weakly cemented loose sandstone oil and gas reservoirs, wherein the reservoirs are free from flowing sand and semi-flowing sand with extremely weak cementation degree. Such quicksand and semi-quicksand reservoirs are very heavily sanded during production. The sand production hazard is mainly shown as follows: severely abrade surface and downhole equipment and even cause sand sticking; maintenance workload such as sand washing pump inspection, ground tank cleaning and the like is increased sharply; the oil well is stopped due to sand blocking of a sand-buried oil layer or a shaft; when the sand production is serious, the sand production can also cause the well wall and even an oil reservoir to collapse to damage a casing and even cause the abandonment of an oil well. These hazards increase both the production cost of the crude oil and the difficulty of oil field exploitation. Therefore, a solution with high consolidation strength at low temperatures is needed.
Patent document 1 (chinese patent application 202010103380.7) discloses a low-temperature consolidated sand and a preparation method thereof, however, the solidification temperature of the low-temperature consolidated sand is not mentioned in patent document 1; in addition, since the low-temperature-bonded sand uses a self-emulsifying aqueous epoxy resin as the second binder, and the self-emulsifying epoxy resin is dispersed in water when the low-temperature-bonded sand is put into water, the bonding strength of the low-temperature-bonded sand in patent document 1 is low.
Patent document 2 (chinese patent application 201010004611.5) discloses a precoated sand curing system for low-temperature reservoir sand control, which uses a composite phenolic/epoxy resin as a cementing agent. Patent document 2 has a problem that the water-soluble curing agent injected into the formation at the later stage is not easy to be in complete contact with the precoated sand injected into the formation at the earlier stage, so that the consolidation strength of the precoated sand under the formation is low; meanwhile, the water-soluble curing agent has large dosage, can not completely react with resin, and seriously pollutes formation water.
Patent document 3 (chinese patent application 201811278488.9) discloses a sand control agent comprising quartz sand, a modified epoxy resin and a curing agent. Wherein the modified epoxy resin is phenolic resin modified epoxy resin; the curing agent is formed by mixing an oil-soluble curing agent and a water-soluble curing agent, wherein the oil-soluble curing agent is selected from one or more of cardanol amine, toluene diisocyanate, dimethyl imidazole and low molecular weight polyamide; the water-soluble curing agent is one or more selected from methanol, ethanol, glycerol, acetone, phenol and cresol. Patent document 3 has a problem that the consolidation strength is low, the resin and the amine curing agent coexist in the sand control agent, the resin and the amine curing agent react with each other, and the strength of the sand control agent is rapidly attenuated during storage.
Patent document 4 (chinese patent application 201610040991.5) discloses a coated sand for oil well sand control and a preparation method thereof, wherein the coated sand comprises a type a coated sand and a type B coated sand, and is characterized in that: the A-type coating sand is formed by sequentially coating organic silicon modified epoxy resin, ketimine curing agent and external isolating agent hydroxymethyl cellulose outside quartz sand; the B-type coating sand is prepared by sequentially coating alicyclic epoxy resin, amine curing agent and external isolating agent hydroxymethyl cellulose on the surface of quartz sand. The A and B type coating sands are mixed to generate a synergistic interaction effect, so that the requirements of low-temperature curing and high-temperature mining are met simultaneously. The low-temperature curing (lowest 40 ℃) is considered to form higher strength, and simultaneously, the low-temperature curing adhesive has good permeability and can stably work in a high-temperature resistant environment (about 280 ℃). Patent document 4 has a problem that the bond strength is not high, and the wet strength of the coated sand is lowered by the reaction of an amine formed by moisture absorption and hydrolysis of a ketimine-based curing agent with an epoxy resin in a humid environment.
Patent document 5 (chinese patent application 201510704656.6) discloses a low-temperature coating sand, which is prepared from two components a and B according to the weight ratio of 1: quartz sand, a binder, a coupling agent, a dispersant and an accelerator; the component B comprises: quartz sand, a curing agent, a coupling agent, a dispersing agent and an accelerating agent. The product can generate early strength after 24 hours at the temperature of 45-260 ℃.
Patent document 6 (Chinese patent application 95107817.8) discloses a sand-preventing process formula for coating sand on a low-temperature oil layer, which is characterized in that the sand-preventing process formula is suitable for preventing sand in an oil-water well with the oil layer temperature of 40-100 ℃, and a binder used in the document is thermosetting phenolic resin which is mixed with an acidic curing accelerator and cannot be stored.
Therefore, none of the products of patent documents 4 to 6 is suitable for sand control of oil and gas wells at a temperature of less than 40 ℃.
Patent document 7 (chinese patent application No. 201911043534.1) discloses an epoxy resin coating proppant, a preparation method and a construction process thereof, the epoxy resin coating proppant comprises a type a coating particle and a type b coating particle; the mass ratio of the A-type coating particles to the B-type coating particles is 1; the A-type coating particles comprise A-type sand cores, A-type sand core coatings and A-type outer coatings; the first-type sand core coating comprises modified epoxy resin, an amine curing agent, an organosilicon coupling agent and an ether diluent; the B-type coating particles comprise a B-type sand core, a B-type sand core coating and a B-type outer cladding; the B-type sand core coating comprises organic silicon epoxy resin, glass fiber, benzene diluent and amine curing agent. Patent document 7 has a problem that the amine curing agent in the a-type coated particles is polyetherimide which does not react with epoxy resin, and the amine curing agent in the b-type coated particles is polyetherimide in claims and specifications, but in the examples, the amine curing agent is amine-terminated polyether which does not react with epoxy resin, and the amine-terminated polyether can react with epoxy resin, and the b-type coated particles have no storability.
Documents of the prior art
Patent document
Patent document 1: chinese patent application 202010103380.7
Patent document 2: chinese patent application 201010004611.5
Patent document 3: chinese patent application 201811278488.9
Patent document 4: chinese patent application 201610040991.5
Patent document 5: chinese patent application 201510704656.6
Patent document 6: chinese patent application 95107817.8
Patent document 7: chinese patent application No. 201911043534.1
Disclosure of Invention
Problems to be solved by the invention
When the temperature of the phenolic resin coated propping agent is lower than 40 ℃, the curing time is long, the consolidation compressive strength is low, and the phenolic resin coated propping agent is not alkali-resistant; in the epoxy resin coated propping agent, when the epoxy resin and the curing agent are coated on the quartz sand and/or the ceramsite simultaneously, the storage stability of the epoxy resin coated propping agent is poor, and the strength is reduced quickly. At present, most of main oil fields in China enter a high water content exploitation period, the temperature is lower and lower, oil and gas wells below 40 ℃ generally exist, and the sand prevention difficulty is higher and higher. In recent years, an oil displacement ternary complex technology containing alkali, a surfactant and a polymer is found, the recovery ratio can be improved by 15-20% on the basis of water flooding, and the oil displacement ternary complex technology becomes a development leading technology of sustainable development of an oil field and a hotspot of research in the field of tertiary oil recovery, and no proper coated sand is available for sand prevention of oil recovery of the oil ternary complex flooding at present.
Aiming at the problems existing in the prior art that the temperature is lower than 40 ℃ and (or) an alkaline medium is not suitable for using sand-proof coated sand, the invention aims to provide a two-component curable coated proppant which can be rapidly cured at the temperature of below 40 ℃ and (or) a strong alkaline liquid and has high consolidation strength, good particle flowability and good storage stability.
Another object of the present invention is to provide a method for preparing a two-component curable coated proppant which is easy to obtain raw materials and simple in preparation method.
Means for solving the problems
Through the research of the inventor, the technical problem can be solved through the implementation of the following technical scheme:
[1] the invention relates to a two-component curable tectorial membrane proppant, which is characterized by comprising an A component and a B component, wherein,
the component A comprises a pre-cured laminating propping agent, liquid epoxy resin b, an epoxy resin diluent, a filler and a flow modifier;
the component B comprises a pre-cured laminating propping agent, an epoxy resin curing agent, a curing accelerator, a filler and a flow modifier;
the pre-curing coated propping agent is particles obtained by pre-curing and coating aggregate of quartz sand and/or ceramsite by using epoxy resin a, a coupling agent and a curing agent a.
[2] The two-component curable coated proppant according to [1], wherein
The epoxy resin a comprises one or two of bisphenol A epoxy resin and bisphenol F epoxy resin, and the content of the epoxy resin a is 1.0-4.0 wt%, preferably 2.0-3.0 wt%, and more preferably 2.0-2.5 wt% relative to the weight of the aggregate.
[3] The two-component curable coated proppant according to [1], wherein
The coupling agent is a silane coupling agent, and the content of the coupling agent is 1.0 to 4.0 wt%, preferably 1.5 to 3.5 wt%, and more preferably 2.0 to 3.0 wt%, based on the weight of the epoxy resin a.
[4] The two-component curable coated proppant according to [1], wherein
The curing agent a used in the pre-curing coating treatment is an amine curing agent a, and the content of the curing agent a is 10.0 to 30.0 wt%, preferably 13.0 to 28.0 wt%, based on the weight of the epoxy resin a.
[5] The two-component curable film-coated proppant according to any one of [1] to [4], wherein
In the component A, the content of the liquid epoxy resin b is 4.0 to 8.0 wt%, preferably 4.1 to 7.0 wt%, and more preferably 4.3 to 7.0 wt% relative to the weight of the pre-cured coating propping agent in the component A; the content of the epoxy resin diluent is 0.4 to 2.0 wt%, preferably 0.4 to 1.3 wt%; the content of the filler is 10.0 to 50.0% by weight, preferably 20.0 to 40.0% by weight, more preferably 23.0 to 35.0% by weight; the flow modifier is present in an amount of 0.1 to 2.0 wt.%, preferably 0.12 to 1.0 wt.%, more preferably 0.15 to 0.5 wt.%.
[6] The two-component curable film-coated proppant according to any one of [1] to [4], wherein
In the component B, the content of the epoxy resin curing agent is 2.0 to 5.0 weight percent, preferably 2.5 to 4.0 weight percent, relative to the weight of the pre-cured coated propping agent in the component B; the content of the curing accelerator is 0.04 to 1.0% by weight, preferably 0.1 to 0.7% by weight, more preferably 0.15 to 0.5% by weight; the content of the filler is 10.0 to 50.0% by weight, preferably 15.0 to 40.0% by weight, more preferably 18.0 to 25.0% by weight; the flow modifier is present in an amount of 0.1 to 2.0 wt.%, preferably 0.11 to 1.0 wt.%, more preferably 0.12 to 0.3 wt.%.
[7] The two-component curable film-coated proppant according to any one of [1] to [6], wherein
The filler includes a water-soluble filler, or both a water-soluble filler and a water-insoluble filler, and when both the water-soluble filler and the water-insoluble filler are used, the weight ratio of the water-soluble filler to the water-insoluble filler is 10 or more, preferably 10 or more and 50 or less.
[8] The method for producing a two-component curable film-coated proppant according to any one of [1] to [7], characterized in that,
the a component was prepared as follows: heating the aggregate to 170-210 ℃, adding the epoxy resin a and the coupling agent, and uniformly mixing; adding a curing agent a, and performing pre-curing to obtain the pre-cured coated proppant; cooling to 60-90 ℃, adding the liquid epoxy resin b and the epoxy resin diluent, and uniformly mixing; adding the filler and the flow modifier, continuously stirring, completely dispersing, sieving and packaging; and
the B component was prepared as follows: heating the aggregate to 170-210 ℃, adding the epoxy resin a and the coupling agent, and uniformly mixing; adding a curing agent a, and performing pre-curing to obtain the pre-cured coated proppant; cooling to 60-90 ℃, adding the epoxy resin curing agent and the curing accelerator, and uniformly mixing; adding the filler and the flow modifier, continuously stirring, completely dispersing, sieving and packaging.
[9] The process according to [8], wherein the aggregate is heated to 180 to 200 ℃.
[10] The use of the two-component curable coated proppant as set forth in any one of [1] to [7] for low-temperature prevention of sand production from a formation, prevention of proppant flowback and embedment into a formation in oil and gas well production.
ADVANTAGEOUS EFFECTS OF INVENTION
The two-component curable film-coated proppant provided by the invention can be rapidly cured at the temperature below 40 ℃ and/or in strong alkaline liquid, has high consolidation strength, and has good particle fluidity and good storage stability.
In addition, the invention provides a preparation method of the two-component curable film-coated proppant, which has the advantages of easy acquisition of raw materials and simple preparation method.
Detailed Description
Various exemplary embodiments, features and aspects of the invention will be described in detail below. The word "exemplary" is used exclusively herein to mean "serving as an example, embodiment, or illustration. Any embodiment described herein as "exemplary" is not necessarily to be construed as preferred or advantageous over other embodiments.
Furthermore, in the following detailed description, numerous specific details are set forth in order to provide a better understanding of the present invention. It will be understood by those skilled in the art that the present invention may be practiced without some of these specific details. In other instances, methods, means, devices and steps which are well known to those skilled in the art have not been described in detail so as not to obscure the invention.
All units used in the specification are international standard units unless otherwise stated, and numerical values and numerical ranges appearing in the present invention should be understood to include systematic errors inevitable in industrial production.
In the present specification, the term "may" includes both the case where a certain process is performed and the case where no process is performed.
In the present specification, the terms "particular/preferred embodiment," "other particular/preferred embodiments," "embodiment," and the like, mean that a particular element (e.g., feature, structure, property, and/or characteristic) described in connection with the embodiment is included in at least one embodiment described herein, and may or may not be present in other embodiments. In addition, it is to be understood that the described elements may be combined in any suitable manner in the various embodiments.
In the present specification, the numerical range represented by "numerical value XX to numerical value YY" means a range including the end point numerical value XX and the end point numerical value YY.
In this specification, the meaning of "including" includes "including 8230 \8230:" composed of "8230:" and "including" includes "including 8230:" composed of "8230:" 8230 "".
Unless otherwise indicated, "parts" and "%" used in the specification are based on weight in all cases.
First aspect
A first aspect of the invention provides a two-component curable coated proppant comprising, e.g., consisting of, an a-component and a B-component. The component A comprises a pre-cured coated propping agent, liquid epoxy resin b, an epoxy resin diluent, a filler and a flow modifier. The component B comprises a pre-cured laminating propping agent, an epoxy resin curing agent, a curing accelerator, a filler and a flow modifier.
< precured coated proppant >
In one embodiment of the invention, the pre-cured film-coated propping agent is particles obtained by pre-curing and film-coating aggregate of quartz sand and/or ceramsite by using epoxy resin a, a coupling agent and a curing agent a. The pre-curing treatment of the coating can not only improve the strength of aggregate and the flow conductivity of the propping agent, but also enhance the bonding strength between the aggregate and the resin, and is beneficial to reducing the dosage of the curable resin.
Aggregate material
In one embodiment of the invention, the aggregate used in the pre-cured coated proppant is quartz sand and/or ceramsite, and the performance of the aggregate meets the industrial standard SY/T5108-2014.
Epoxy resin a
In one embodiment of the present invention, epoxy a may be used in the pre-cured coated proppant. Examples of the epoxy resin a of the present invention include one or both of a bisphenol a epoxy resin of the general type and a bisphenol F epoxy resin.
Specific examples of the general bisphenol a epoxy resin of the present invention include: one or more than two of E-51, E-44, E-42, E-20, E-14 and E-13; specific examples of the bisphenol F epoxy resin of the present invention include: one or more than two of CYDF170 and CYDF-180 of Yue epoxy resin company and 6445 and 6458 of Shanghai Xinhua resin factory.
The content of the epoxy resin a is 1.0 to 4.0 wt%, preferably 2.0 to 3.0 wt%, more preferably 2.0 to 2.5 wt%, relative to the weight of the aggregate of the quartz sand and/or the ceramsite. When the content of the epoxy resin a is lower than 1.0%, the epoxy resin a does not completely coat the aggregate and the epoxy resin a and the aggregate are not firmly bonded, so that the consolidation strength of the coated sand in the oil-gas well is influenced; when the content of the epoxy resin a is more than 4.0%, the cost of the coated proppant is too high, and the aggregate particles are bonded to each other and are not easily separated.
Coupling agent
In one embodiment of the present invention, a coupling agent may be used in the pre-cured coated proppant. The coupling agent of the present invention is selected from a variety of coupling agents known to those skilled in the art. The coupling agent is preferably a silane coupling agent for the purpose of improving the adhesive strength of the proppant aggregate with the epoxy resin binder.
Examples of the silane coupling agent of the present invention include: one or more of gamma-aminopropyltriethoxysilane, gamma-aminopropyltrimethoxysilane (KH 550), gamma-glycidoxypropyltrimethoxysilane (KH 560), anilinomethylenetriethoxysilane, dodecyltrimethoxysilane and octadecyltrimethoxysilane. By selecting the type of the coupling agent and adjusting the content of the coupling agent, the bonding strength between the epoxy resin binder and the aggregate can be enhanced, and the water resistance between the epoxy resin binder and the aggregate can be improved.
The content of the coupling agent is 1.0 to 4.0% by weight, preferably 1.5 to 3.5% by weight, and more preferably 2.0 to 3.0% by weight, based on the weight of the epoxy resin a. When the content of the coupling agent is lower than 1.0%, the bonding between the epoxy resin binder and the aggregate is poor, and the formed resin film is easy to fall off from the aggregate, so that the consolidation strength of the coated proppant in the oil-gas well is influenced; when the content of the coupling agent is more than 4.0%, the cost of the coated proppant is high, and the compressive strength of the coated proppant is affected, thereby resulting in the conductivity of the coated proppant.
Curing agent a
In one embodiment of the present invention, curing agent a may be used in the pre-cured coated proppant. The curing agent a of the present invention may be an amine curing agent a. When the active hydrogen of the amine curing agent a reacts with the epoxy group in the epoxy resin a in an equimolar manner, the strength and water resistance of the pre-cured coated proppant are best.
Examples of the amine-based curing agent a of the present invention include: one or more alicyclic polyamines such as Menthanediamine (MDA), isophoronediamine (IPDA) and 1, 3-cyclohexanedimethylamine (1, 3-BAC); one or more kinds of aromatic polyamines such as m-xylylenediamine (m-XDA), diaminodiphenylmethane (DDM), and diaminodiphenylsulfone (DDS); one or more of modified alicyclic polyamine and/or modified aromatic polyamine.
The content of the curing agent a is 10.0 to 30.0% by weight, preferably 13.0 to 28.0% by weight, based on the weight of the epoxy resin a. When the using amount of the curing agent a is insufficient, the pre-curing is incomplete, and the strength of the pre-cured coated propping agent can be influenced; when the content of the curing agent a is excessive, the water resistance of the pre-cured coating film proppant may be affected.
< Filler >
In one embodiment of the invention, fillers may be used in the A and B components. The filler of the present invention may be in the form of particles having a particle diameter of 150 μm or less.
The filler of the present invention may be either one or both of a water-soluble filler and a water-insoluble filler. Examples of the water-soluble filler of the present invention include: one or more of sodium citrate, potassium acetate, potassium nitrate, sodium chloride or potassium chloride, dextrin, sodium alginate, sodium benzoate and sodium pyrophosphate; examples of the water-insoluble filler of the present invention include: one or more of quartz powder, alumina powder, calcium carbonate powder and barite powder.
The filler of the present invention may be used either alone or in combination with both of the water-soluble filler and the water-insoluble filler. In the case where both are used simultaneously, the weight ratio of the water-soluble filler to the water-insoluble filler is 10 or more, preferably 10 or more and 50 or less. When the content of the filler is too low, the component A and the component B are not easy to dry, easy to agglomerate under pressure and poor in fluidity, and cannot be uniformly metered into a sand mixing truck; when the content of the filler is too high, the fine powder filler in the component A and the component B is more, the components are not uniform, the consolidation strength is influenced, and dust is generated during construction, so that the construction environment is influenced.
< flow modifier >
In one embodiment of the invention, flow modifiers may be used in the A and B components. Examples of flow modifiers of the present invention include: one or more than two of talcum powder, hydroxyl silicone oil, methyl silicone oil, epoxy silicone oil and hydrogenated silicone oil.
The A-component and B-component of the present invention are described in detail below.
<Component A>
In the two-component curable tectorial membrane proppant, the component A comprises a pre-cured tectorial membrane proppant, a liquid epoxy resin b, an epoxy resin diluent, a filler and a flow modifier. For example, the a-component consists of a pre-cured coated proppant, a liquid epoxy resin b, an epoxy diluent, a filler, and a flow modifier.
The pre-cured coated proppant in the a component is the pre-cured coated proppant described in the above section "< pre-cured coated proppant >.
< liquid epoxy resin b >
In one embodiment of the present invention, a liquid epoxy resin b may be used in the a component. The liquid epoxy resin b is one or more of bisphenol A epoxy resin, novolac epoxy resin and bisphenol F epoxy resin.
Examples of bisphenol a epoxy resins of the present invention include: one or more than two of E-56D, E-54, E-51 and E-44; examples of the novolac epoxy resin of the invention include: one or more of F-51, F-54, F-76 and 638S; examples of bisphenol F epoxy resins of the present invention include: one or more of CYDF170 and CYDF180 of Yueyaide epoxy resin company and 6445 and 6458 of Shanghai Xinhua resin factory.
The content of the liquid epoxy resin b is 4.0 to 8.0 wt%, preferably 4.1 to 7.0 wt%, and more preferably 4.3 to 7.0 wt%, based on the weight of the precured coated proppant in the a component. When the content of the liquid epoxy resin b is lower than 4.0 percent, the consolidation strength in the oil-gas well is insufficient, the liquid epoxy resin is easily damaged by fluid, and the liquid epoxy resin cannot resist the formation sand; when the content of the liquid epoxy resin b is more than 8.0%, the consolidation strength is excessive, and the excessive liquid epoxy resin b can block gaps among aggregates, so that the diversion is influenced, the cost is high, and the application is influenced.
< epoxy resin diluent >
In one embodiment of the present invention, an epoxy diluent may be used in the A component. The epoxy resin diluent is one or two of dihydric alcohol diglycidyl ether and glycidyl ester.
Examples of the glycol glycidyl ether of the present invention include: one or more of 1, 6-hexanediol diglycidyl ether (632), 1, 4-cyclohexanedimethanol diglycidyl ether (630), 1, 4-butanediol diglycidyl ether (622), dipropylene glycol diglycidyl ether (208), and neopentyl glycol diglycidyl ether (678); examples of glycidyl esters of the present invention include: one or more than two of diglycidyl tetrahydrophthalate (711, CY-182) and diglycidyl hexahydrophthalate (S-184, CY-184).
The content of the epoxy resin diluent is 0.4 to 2.0% by weight, preferably 0.4 to 1.3% by weight, based on the weight of the precured coated proppant in the a component. When the content of the epoxy resin diluent is less than 0.4%, the overall viscosity of the resin in the component A is high, so that the contact reaction of the resin and the curing agent is not facilitated; when the content of the epoxy resin diluent is higher than 2.0%, the overall viscosity of the resin in the component A is too low, so that the resin is not favorable for adhering the filler on the surface of the pre-cured laminated proppant, and the consolidation strength is influenced.
The filler in the a component is the filler described in the above "< filler > section".
After the pre-cured coated propping agent in the component A is coated with the liquid epoxy resin b, the pre-cured coated propping agent becomes wet, so that the liquid epoxy resin b in the component A needs to be sucked dry by using a filler to dry the particles of the pre-cured coated propping agent so as to prevent the pre-cured coated propping agent from caking and facilitate the injection into the formation cracks of an oil well.
The content of the filler in the a component (in the case where two or more fillers are used, the total content of the fillers) is 10.0 to 50.0 wt%, preferably 20.0 to 40.0 wt%, and more preferably 23.0 to 35.0 wt% with respect to the weight of the precured coated proppant in the a component. When the content of the filler is less than 10.0%, the component A is over-wet and poor in fluidity, and is difficult to quantitatively feed into a sand mixing truck during field construction; when the content of the filler is more than 50.0 percent, a plurality of dry powders cannot be adhered to the proppant, so that the component A is uneven in composition, and the consolidation strength is influenced.
The flow modifier in the a component is the flow modifier described in the "< flow modifier > section" above.
The content of the flow modifier in the a component is 0.1 to 2.0 wt%, preferably 0.12 to 1.0 wt%, more preferably 0.15 to 0.5 wt%, relative to the weight of the precured coating proppant in the a component. When the content of the flow modifier is less than 0.1%, the flowability of the A component is poor; when the content of the flow modifier is more than 2.0%, the consolidation strength of the coated proppant may be affected.
<B component>
In the two-component curable tectorial membrane proppant, the component B comprises a pre-cured tectorial membrane proppant, an epoxy resin curing agent, a curing accelerator, a filler and a flow modifier. For example, the B component consists of a pre-cured coated proppant, an epoxy resin curing agent, a curing accelerator, a filler and a flow modifier.
The pre-cured coated proppant in the B component is the pre-cured coated proppant described in the above section "< pre-cured coated proppant >. The type and content of each component in the pre-cured coated proppant in the component B and the pre-cured coated proppant in the component A of the same proppant can be the same or different.
< epoxy resin curing agent >
In one embodiment of the present invention, an epoxy resin curing agent may be used in the B component. As the epoxy resin curing agent, an amine curing agent b can be used. The curing agent is not whitened in water, active groups participating in a curing reaction have good reactivity under water and are not influenced by water, and the retention rate of the bonding strength of a cured product of the curing agent is over 90 percent compared with that of the curing agent under a dry environment.
Examples of the epoxy resin curing agent of the present invention include: f-2101, F-2302 and F-2201 curing agents of Hongli exhibition chemical industry Co Ltd; SX-5129 and SX-5253 underwater special epoxy curing agents of mountain peak chemical industry Co; and one or more than two of MS-1085 series underwater special epoxy curing agents of general lighting biochemical technology limited company.
The content of the epoxy resin curing agent is 2.0 to 5.0% by weight, preferably 2.5 to 4.0% by weight, based on the weight of the precured coated proppant in the B component. When the content of the epoxy resin curing agent is lower than 2.0%, the component A and the component B are incompletely cured after being mixed, and the curing strength is low; when the content of the epoxy resin curing agent is more than 5.0 percent, excessive amino groups affect the water resistance of the A component and the B component after solidification and affect the long-term effectiveness of sand prevention.
< curing accelerators >
In one embodiment of the present invention, a curing accelerator may be used in the B component. Examples of the curing accelerator include one or both of an imidazole accelerator, which is insoluble in water, and a phenol accelerator.
Specific examples of the imidazole-based accelerator of the present invention include: one or more of 2-undecylimidazole, 2-phenylimidazole, 1-benzyl-2-methylimidazole and 1-cyanoethyl-2-undecyl-trimellitic acid imidazole salt; specific examples of phenolic accelerators of the invention include: one or more of bisphenol A, nonyl phenol, salicylic acid and cardanol.
The content of the curing accelerator is 0.04 to 1.0 wt%, preferably 0.1 to 0.7 wt%, more preferably 0.15 to 0.5 wt%, based on the weight of the precured coated proppant in the B component. When the content of the curing accelerator is less than 0.04%, the curing speed is too slow, and the consolidation strength cannot meet the requirement; when the content of the curing accelerator is more than 1.0%, although the curing speed is not greatly affected, the cost is too high, which affects the application.
The filler in the B component is the filler described in the above "< filler > section".
When the pre-cured coated proppant in the component B is coated with the epoxy resin curing agent, the pre-cured coated proppant becomes wet, so that the epoxy resin curing agent in the component B needs to be sucked dry by using a filler to dry the pre-cured coated proppant particles so as to prevent the pre-cured coated proppant from caking and facilitate injection into oil well formation cracks.
The content of the filler in the B component (in the case where two or more fillers are used, the total content of the fillers) is 10.0 to 50.0 wt%, preferably 15.0 to 40.0 wt%, and more preferably 18.0 to 25.0 wt% with respect to the weight of the precured coated proppant in the B component. When the content of the filler is less than 10.0 percent, the component B has poor fluidity, and is difficult to quantitatively feed into a sand mixer during field construction; when the content of the filler is more than 50.0 percent, a plurality of dry powders can not be adhered to the proppant, so that the component B is uneven, and the consolidation strength is influenced.
The type and content of the filler in the B component and the filler in the A component of the same proppant can be the same or different.
The flow modifier in the B component is the flow modifier described in the above section "< flow modifier >.
The flow modifier in the B-component is present in an amount of 0.1 to 2.0 wt%, preferably 0.11 to 1.0 wt%, more preferably 0.12 to 0.3 wt%, based on the weight of the pre-cured coated proppant in the B-component. When the content of the flow modifier is less than 0.1%, the fluidity of the B component is poor; when the content of the flow modifier is more than 2.0 percent, the consolidation strength of the coated proppant is influenced.
The flow modifier in the B component may be the same or different from the flow modifier in the A component of the same proppant in type and amount.
Second aspect of the invention
A second aspect of the invention provides a method of making a two-part curable coated proppant.
In one embodiment of the invention, the a component is prepared as follows: heating quartz sand and/or ceramsite aggregate to 170-210 ℃, preferably 180-200 ℃, adding the epoxy resin a and the coupling agent under stirring, and uniformly stirring, wherein the stirring time is preferably 40-60 seconds, so that the epoxy resin a and the coupling agent are adhered to the quartz sand and/or ceramsite aggregate; then, adding a curing agent a, and stirring for pre-curing, wherein the pre-curing time is preferably 220-260 seconds; adding water to cool the mixture to below 90 ℃, then adding the liquid epoxy resin b and the epoxy resin diluent, and stirring for 20-40 seconds; adding the filler and the flow modifier, and continuously stirring until the particles are completely dispersed and freely flow; sieving the materials, and packaging.
In one embodiment of the invention, the B component is prepared as follows: heating quartz sand and/or ceramsite aggregate to 170-210 ℃, preferably 180-200 ℃, adding the epoxy resin a and the coupling agent under stirring, and uniformly stirring, wherein the stirring time is preferably 40-60 seconds, so that the epoxy resin a and the coupling agent are adhered to the quartz sand and/or ceramsite aggregate; then, adding a curing agent a, and stirring for pre-curing, wherein the pre-curing time is preferably 220-260 seconds; adding water to cool the mixture to below 90 ℃, then adding an epoxy resin curing agent and a curing accelerator, and stirring for 20-40 seconds; adding the filler and the flow modifier, and continuously stirring until the particles are completely dispersed and freely flow; sieving the materials, and packaging.
Third aspect
In a third aspect of the invention, the invention provides the use of a two-component curable coated proppant for low temperature production in oil and gas wells to prevent sand production from the formation, prevent proppant flowback and embed in the formation.
Examples
The present invention will be specifically described below based on examples and comparative examples. However, the present invention is not limited to these examples and the like.
The following examples are provided to provide a better understanding of the present invention and are not intended to limit the invention to the preferred embodiments described. The embodiments do not limit the content and the protection scope of the present invention, and any products similar or similar to the present invention, which are obtained by combining the present invention with other features of the prior art, or the present invention, fall into the protection scope of the present invention defined by the claims.
The examples of the present invention are carried out according to conventional techniques or conditions described in the literature in the art, unless otherwise specified. The raw materials or instruments used are not indicated by manufacturers, and are all conventional raw materials or instrument products which can be obtained commercially.
The aggregate used in the examples and comparative examples of the invention is quartz sand and/or ceramsite particles, the particle size of the particles is 850/425 mu m (20/40 mesh), 600/300 mu m (30/50 mesh) and 425/212 mu m (40/70 mesh), and the particle size distribution meets the industrial standard SY/T5108-2014.
< example 1>
The component A comprises: heating 3.1 kg of quartz sand with the particle size of 850/425 mu m (20/40 meshes) to 220 ℃, putting the quartz sand into a self-made sand mixer for stirring, cooling to 210 ℃, adding 62 g of E-44 epoxy resin and 1.6 g of gamma-aminopropyltriethoxysilane, and stirring for 30 seconds; adding 13.5 g of DDM curing agent, stirring and curing for 240 seconds to obtain a pre-cured coated proppant; after the temperature is reduced to 90 ℃, 150 g of E-51 epoxy resin and 30 g of epoxy resin 678 diluent are added and stirred for 20 seconds; adding filler (20 g of quartz powder and 840 g of sodium pyrophosphate) and 5 g of hydroxyl silicone oil, and stirring until the particles are completely dispersed and freely flow; sieving to obtain A component.
And B component: heating 3.3 kg of quartz sand with the particle size of 850/425 mu m (20/40 meshes) to 220 ℃, putting the quartz sand into a self-made sand mixer for stirring, cooling to 210 ℃, adding 77.5 g of E-44 epoxy resin and 1.6 g of KH550 silane coupling agent, and stirring for 30 seconds; adding 16.9 g of DDM curing agent, stirring and curing for 240 seconds to obtain a pre-cured coated propping agent; after the temperature is reduced to 90 ℃, 110 g of F-2101 epoxy resin curing agent and 10 g of salicylic acid are added and stirred for 20 seconds; adding filler (20 g of quartz powder and 620 g of sodium pyrophosphate) and 5 g of hydroxyl silicone oil, and stirring until the particles are completely dispersed and freely flow; sieving to obtain component B.
Equal weight of the component A and the component B were taken and mixed uniformly, and a sample was prepared by the following consolidation compressive strength sample preparation method, after which the consolidation compressive strength of the sample block was tested.
Testing the consolidation compressive strength: uniformly mixing the component A and the component B with equal weight, taking 30 g of the mixture, putting the mixture into a sample preparation pipe with the inner diameter of 25mm, adding 15ml of water into the sample preparation pipe, uniformly stirring, putting the sample preparation pipe into a cushion block, putting the sample preparation pipe on a press, keeping the sample under the set pressure (10 MPa) for 30 seconds, pouring 25ml of water into the sample preparation pipe to completely submerge the sample, and putting the sample preparation pipe into a constant-temperature water bath kettle with the set temperature for curing. And after the curing time is up, taking out the sample block for testing the consolidation compressive strength.
The results are shown in table 1.
< comparative example 1>
The component A comprises: heating 3.1 kg of quartz sand with the particle size of 850/425 mu m (20/40 meshes) to 120 ℃, and then putting the quartz sand into a self-made sand mixer for stirring; cooling to 90 ℃, adding 150 g of E-51 epoxy resin and 30 g of epoxy resin 678 diluent, and stirring for 20 seconds; adding filler (20 g of quartz powder and 840 g of sodium pyrophosphate) and 5 g of hydroxyl silicone oil, and stirring until the particles are completely dispersed and freely flow; sieving to obtain component A.
And B component: heating 3.1 kg of quartz sand with the particle size of 850/425 mu m (20/40 meshes) to 120 ℃, and then putting the quartz sand into a self-made sand mixer for stirring; cooling to 90 ℃, adding 110 g of F-2101 curing agent and 10 g of salicylic acid, and stirring for 20 seconds; adding filler (20 g of quartz powder and 620 g of sodium pyrophosphate) and 5 g of hydroxyl silicone oil, and stirring until the particles are completely dispersed and freely flow; sieving to obtain component B.
Equal weights of the A-component and the B-component were taken and mixed well, and the sample preparation and the testing of the compressive strength at consolidation were carried out in the same manner as in example 1, and the results are shown in Table 1.
TABLE 1 comparison of the results of example 1 and comparative example 1
As can be seen from table 1, in comparison with example 1, the a-component and the B-component of comparative example 1, the quartz sand of comparative example 1 was not pre-coated with the epoxy resin a, the coupling agent and the curing agent a, and the liquid epoxy resin B in the a-component and the epoxy resin curing agent in the B-component adhered to the quartz sand poorly, resulting in a low consolidation strength of the product when cured in water.
< example 2>
The component A comprises: heating 3.1 kg of ceramsite with the particle size of 600/300 mu m (30/50 meshes) to 240 ℃, putting the ceramsite into a self-made sand mixer for stirring, cooling to 200 ℃, adding 62 g of E-51 epoxy resin and 1.3 g of KH560 silane coupling agent, and stirring for 30 seconds; adding 11.3 g of 1,3-BAC curing agent, and stirring and curing for 200 seconds to obtain a pre-cured coated proppant; cooling to 80 ℃, adding 139.5 g of E-54 epoxy resin and 15.5 g of epoxy resin 622 diluent, and stirring for 20 seconds; adding filler (50 g of barite powder and 710 g of potassium nitrate powder) and 6.2 g of silicone oil, and stirring until the particles are completely dispersed and freely flow; sieving to obtain A component.
And the component B comprises: heating 3.1 kg of ceramsite with the particle size of 600/300 mu m (30/50 meshes) to 240 ℃, putting the ceramsite into a self-made sand mixer for stirring, cooling to 200 ℃, adding 62 g of E-51 epoxy resin and 1.3 g of KH560 silane coupling agent, and stirring for 30 seconds; adding 11.3 g of 1,3-BAC curing agent, and stirring and curing for 200 seconds to obtain a pre-cured coated proppant; cooling to 80 ℃, adding 87 g of MS-1085 curing agent and 5 g of bisphenol A accelerator, and stirring for 20 seconds; adding filler (20 g of barite powder and 600 g of sodium pyrophosphate) and 4 g of silicone oil, and stirring until the particles are completely dispersed and freely flow; sieving to obtain component B.
Equal weights of the A-component and the B-component were taken and mixed well, and sampling and testing of the compressive strength at consolidation were carried out in the same manner as in example 1, and the results are shown in Table 2.
< comparative example 2>
The component A comprises: heating 3.1 kg of ceramsite with the particle size of 600/300 mu m (30/50 meshes) to 100 ℃, putting the ceramsite into a self-made sand mixer for stirring, cooling to 80 ℃, adding 139.5 g of E-54 epoxy resin and 15.5 g of epoxy resin 622 diluent, and stirring for 20 seconds; adding filler (50 g of barite powder and 710 g of potassium nitrate powder) and 6.2 g of silicone oil, and stirring until the particles are completely dispersed and freely flow; sieving to obtain component A.
And B component: heating 3.1 kg of ceramsite with the particle size of 600/300 mu m (30/50 meshes) to 120 ℃, putting the ceramsite into a self-made sand mixer for stirring, cooling to 80 ℃, adding 87 g of MS-1085 curing agent and 5 g of bisphenol A accelerator, and stirring for 20 seconds; adding filler (20 g of barite powder and 600 g of sodium pyrophosphate) and 4 g of silicone oil, and stirring until the particles are completely dispersed and freely flow; sieving to obtain component B.
Equal weights of the A-component and the B-component were taken and mixed well, and sampling and testing of the compressive strength at consolidation were carried out in the same manner as in example 1, and the results are shown in Table 2.
TABLE 2 comparison of the results of example 2 and comparative example 2
As can be seen from Table 2, the A-component and B-component of comparative example 2 had low preheating temperatures, and had no coating after mixing the epoxy resin a and the coupling agent, nor had precuring with the curing agent a. In other words, in the a-component and the B-component of comparative example 2, the precured coated proppant of the present invention was not formed, and therefore, the product of comparative example 2 had a lower consolidation strength than that of example 2.
< example 3>
The component A comprises: heating 3.1 kg of quartz sand with the particle size of 425/212 mu m (40/70 meshes) to 220 ℃, putting the quartz sand into a self-made sand mixer for stirring, cooling to 210 ℃, adding 62 g of E-51 epoxy resin and 1.8 g of KH560 silane coupling agent, and stirring for 30 seconds; adding 15.7 g of DDM curing agent, stirring and curing for 250 seconds to obtain a pre-cured coated proppant; cooling to 90 ℃, adding 118 g of E-51 epoxy resin, 59 g of 638S novolac epoxy resin and 40 g of epoxy resin 678 diluent, and stirring for 20 seconds; adding filler (80 g of alumina powder and 1000 g of sodium citrate) and 9.3 g of epoxy silicone oil, and stirring until the particles are completely dispersed and freely flow; sieving to obtain component A.
And B component: heating 3.1 kg of quartz sand with the particle size of 425/212 mu m (40/70 meshes) to 220 ℃, putting the quartz sand into a self-made sand mixer for stirring, cooling to 210 ℃, adding 62 g of E-51 epoxy resin and 1.8 g of KH560 silane coupling agent, and stirring for 30 seconds; adding 15.7 g of DDM curing agent, stirring and curing for 250 seconds; cooling to 90 ℃, adding 126 g of SX-5129 curing agent and 15 g of 2-phenylimidazole, and stirring for 20 seconds; adding filler (30 g of alumina powder and 680 g of sodium citrate) and 8 g of epoxy silicone oil, and stirring until the particles are completely dispersed and freely flow; sieving to obtain component B.
Equal weights of the A-component and the B-component were taken and mixed well, and sampling and testing of the compressive strength at consolidation were carried out in the same manner as in example 1, and the results are shown in Table 3.
< comparative example 3>
Heating 3.1 kg of quartz sand with the particle size of 425/212 mu m (40/70 meshes) to 220 ℃, putting the quartz sand into a self-made sand mixer for stirring, cooling to 210 ℃, adding 62 g of E-51 epoxy resin and 1.8 g of KH560 silane coupling agent, and stirring for 30 seconds; adding 15.7 g of DDM curing agent, stirring and curing for 250 seconds; cooling to 160 ℃, adding 155 grams of 1901 phenolic resin, and stirring for 40 seconds; adding water, cooling to 105 ℃, adding 70 g of urotropine solution (the mass ratio of urotropine to water is 2/1), and stirring for 20 seconds; and when the materials begin to agglomerate, adding 10 g of calcium stearate and 4 g of methyl silicone oil, stirring until the particles are completely dispersed, cooling and sieving to obtain the conventional sand control resin coated quartz sand proppant.
Equal weights of the A-component and the B-component were taken and mixed well, and sampling and testing of the compressive strength at consolidation were carried out in the same manner as in example 1, and the results are shown in Table 3.
TABLE 3 comparison of the results of example 3 and comparative example 3
As can be seen from table 3, the proppant of example 3 of the present invention has high consolidation compressive strength, while the conventional sand control resin coated quartz sand proppant of comparative example 3 has substantially no consolidation strength.
Industrial applicability
The bi-component curable film-coated propping agent can be rapidly cured at the temperature of below 40 ℃ and/or in strong alkali liquid, has high consolidation strength, good particle fluidity and good storage stability, and can be used for preventing formation sand from flowing out and propping agent from flowing back and being embedded into the formation at low temperature in oil and gas well exploitation. In addition, the preparation method of the two-component curable film-coated proppant disclosed by the invention is easy to obtain raw materials and simple in preparation method. The two-component curable tectorial membrane proppant and the preparation method thereof can realize simple, efficient and large-scale preparation of the two-component curable tectorial membrane proppant and can be applied to industry.
Claims (10)
1. A two-component curable coated proppant comprising an A-component and a B-component, wherein,
the component A comprises a pre-cured laminating propping agent, liquid epoxy resin b, an epoxy resin diluent, a filler and a flow modifier;
the component B comprises a pre-cured laminating propping agent, an epoxy resin curing agent, a curing accelerator, a filler and a flow modifier;
the pre-cured film-coated propping agent is particles obtained by pre-curing and film-coating aggregate of quartz sand and/or ceramsite by using epoxy resin a, a coupling agent and a curing agent a.
2. The two-part curable coated proppant of claim 1, wherein
The epoxy resin a comprises one or two of bisphenol A epoxy resin and bisphenol F epoxy resin, and the content of the epoxy resin a is 1.0-4.0 wt%, preferably 2.0-3.0 wt%, and more preferably 2.0-2.5 wt% relative to the weight of the aggregate.
3. The two-part curable coated proppant of claim 1, wherein
The coupling agent is a silane coupling agent, and the content of the coupling agent is 1.0 to 4.0 wt%, preferably 1.5 to 3.5 wt%, and more preferably 2.0 to 3.0 wt%, based on the weight of the epoxy resin a.
4. The two-part curable coated proppant of claim 1, wherein
The curing agent a used in the pre-curing coating treatment is an amine curing agent a, and the content of the curing agent a is 10.0 to 30.0 wt%, preferably 13.0 to 28.0 wt%, based on the weight of the epoxy resin a.
5. The two-part curable coated proppant of any one of claims 1-4, wherein
In the component A, the content of the liquid epoxy resin b is 4.0 to 8.0 wt%, preferably 4.1 to 7.0 wt%, and more preferably 4.3 to 7.0 wt% relative to the weight of the pre-cured coating propping agent in the component A; the content of the epoxy resin diluent is 0.4 to 2.0 wt%, preferably 0.4 to 1.3 wt%; the content of the filler is 10.0 to 50.0% by weight, preferably 20.0 to 40.0% by weight, more preferably 23.0 to 35.0% by weight; the flow modifier is present in an amount of 0.1 to 2.0 wt.%, preferably 0.12 to 1.0 wt.%, more preferably 0.15 to 0.5 wt.%.
6. The two-part curable coated proppant of any one of claims 1-4, wherein
In the component B, the content of the epoxy resin curing agent is 2.0 to 5.0 weight percent, preferably 2.5 to 4.0 weight percent, relative to the weight of the pre-cured coated propping agent in the component B; the content of the curing accelerator is 0.04 to 1.0% by weight, preferably 0.1 to 0.7% by weight, more preferably 0.15 to 0.5% by weight; the content of the filler is 10.0 to 50.0% by weight, preferably 15.0 to 40.0% by weight, more preferably 18.0 to 25.0% by weight; the flow modifier is present in an amount of 0.1 to 2.0 wt.%, preferably 0.11 to 1.0 wt.%, more preferably 0.12 to 0.3 wt.%.
7. The two-part curable coated proppant of any one of claims 1-6, wherein
The filler includes a water-soluble filler, or both a water-soluble filler and a water-insoluble filler, and when both the water-soluble filler and the water-insoluble filler are used, the weight ratio of the water-soluble filler to the water-insoluble filler is 10 or more, preferably 10 or more and 50 or less.
8. A method of making the two-part curable coated proppant of any of claims 1-7,
the a component was prepared as follows: heating the aggregate to 170-210 ℃, adding the epoxy resin a and the coupling agent, and uniformly mixing; adding a curing agent a, and performing precuring to obtain the precured coated proppant; cooling to 60-90 ℃, adding the liquid epoxy resin b and the epoxy resin diluent, and uniformly mixing; adding the filler and the flow modifier, continuously stirring, completely dispersing, sieving and packaging; and
the B component was prepared as follows: heating the aggregate to 170-210 ℃, adding the epoxy resin a and the coupling agent, and uniformly mixing; adding a curing agent a, and performing pre-curing to obtain the pre-cured coated proppant; cooling to 60-90 ℃, adding the epoxy resin curing agent and the curing accelerator, and mixing uniformly; adding the filler and the flow modifier, continuously stirring, completely dispersing, sieving and packaging.
9. The method of manufacturing according to claim 8, wherein the aggregate is heated to 180-200 ℃.
10. Use of the two-component curable coated proppant of any one of claims 1-7 for low temperature production of oil and gas wells to prevent sand production from the formation, prevent proppant flowback and embed in the formation.
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