CN110079295A - Curable proppant and its preparation method and application - Google Patents
Curable proppant and its preparation method and application Download PDFInfo
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- CN110079295A CN110079295A CN201910320093.9A CN201910320093A CN110079295A CN 110079295 A CN110079295 A CN 110079295A CN 201910320093 A CN201910320093 A CN 201910320093A CN 110079295 A CN110079295 A CN 110079295A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
- C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
- C08G59/40—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
- C08G59/50—Amines
- C08G59/5033—Amines aromatic
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
- C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
- C08G59/68—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the catalysts used
- C08G59/686—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the catalysts used containing nitrogen
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/60—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 present invention provides a kind of curable proppant and its preparation method and application.The curable proppant includes: precuring overlay film proppant, liquid epoxy resin A, latent curing agent, filler and flow ability modifying agent；Wherein, with the total weight of the precuring overlay film proppant, the additional amount of the liquid epoxy resin A is 2%-6%；The additional amount of the latent curing agent is 0.2%-1.8%；The additional amount of the filler is 10%-30%；The additional amount of the flow ability modifying agent is 0.1%-1%.The storage of curable proppant of the invention is stable and resistance to alkali ability is strong, can consolidate in highly basic liquid, such as: it can be consolidated in the sodium hydroxide solution that 40 DEG C of temperature or more of mass concentration is 1.5%, consolidation strength is greater than 5MPa.
Description
Technical field
The present invention relates to a kind of curable proppant and its preparation method and application, in particular to a kind of ternary composite driving can
Solidify proppant, belongs to technical field of tertiary oil recovery.
Background technique
Petroleum is a kind of mineral reserve fluid for being stored in underground, is the indispensable energy composition of industrialization development.Currently, I
Each main force oil field of state has largely entered the High water cut productive life, and the exploitation difficulty of petroleum is increasing, production decline width
Degree also gradually increases, and disparities between supply and demand become increasingly conspicuous.In order to alleviate the disparities between supply and demand to become increasingly conspicuous, people adopt to improve in various manners
The recovery ratio in existing oil field.In recent years, the ASP Oil-Displacing Technology containing alkali, surfactant and polymer is found, it can be
Recovery ratio 15~20% is improved on the basis of water drive, becomes the exploitation dominant technology in oil field and the hot spot of tertiary oil recovery field research.
It is high that part injection well injection pressure is exposed in ternary compound oil drive field operation, cannot be completed with fluence,
Common Fracturing Technology measure is correspondingly taken in injection well thus, measure effect is poor.The reason is that ternary composite displacement system
Viscosity is higher, and prop-carrying capacity is strong, and proppant band people's earth formation deep is easily caused near wellbore crack closure in high pressure injection,
Injectability reduces, and even results in pressure break failure.Equally, after Ternary composite drive well is imitated, Produced Liquid occur emulsion and
Viscosity is big, easily leads to proppant backflow, crack closure, and improvement is short.It drives in Fracturing Technology poly- using phenolic aldehyde in hot pursuit
Coated sand technique solves the problems, such as this, but due to the presence of highly basic in ternary composite displacement system, seriously destroys phenol resin sand
Cementing strength, phenol resin sand technology in hot pursuit are restricted in the application of ternary composite driving.
Summary of the invention
Problems to be solved by the invention
Phenolic resin is be easy to cause for example, existing proppant is not alkaline-resisting in view of the technical problems existing in the prior art
Precoated sand does not have consolidation strength, the problems such as proppant returns the decline of Tuhe injection well injectability occurs, present invention firstly provides
A kind of curable proppant.The curable proppant can not only solidify in highly basic liquid, consolidation strength is high, but also particle
Good fluidity, storage are stablized.
Further, it is easy to obtain the present invention also provides a kind of raw material, the system of the simply curable proppant of preparation method
Preparation Method.
The solution to the problem
[1], a kind of curable proppant, wherein include: precuring overlay film proppant, liquid epoxy resin A, dive
Volt property curing agent, filler and flow ability modifying agent；Wherein,
With the total weight of the precuring overlay film proppant, the additional amount of the liquid epoxy resin A is 2%-
6%；The additional amount of the latent curing agent is 0.2%-1.8%；The additional amount of the filler is 10%-30%；The stream
The additional amount of dynamic modifying agent is 0.1%-1%.
[2], the curable proppant according to [1], wherein the precuring overlay film proppant includes aggregate, epoxy
Resin B, coupling agent and precuring agent；Wherein, with the total weight of the aggregate, the additional amount of the epoxy resin B is
0.5%-2%；The additional amount of the coupling agent is 0.0025%-0.08%；The additional amount of the precuring agent is 0.05%-
0.6%.
[3], the curable proppant according to [2], wherein the epoxy resin B includes bisphenol A type epoxy resin；
And/or
The precuring agent includes amine curing agent, and it is solid to preferably include alicyclic polyamine class curing agent, aromatic polyamine class
The combination of one or more of agent, modified allicylic polyamine and modified aromatic polyamine；And/or
The coupling agent includes silane coupling agent, preferably includes γ-aminopropyltrimethoxysilane, γ-glycidol ether
Propyl trimethoxy silicane, anilino- methylene triethoxysilane, dodecyltrimethoxysilane and octadecyl trimethoxy
The combination of one or more of base silane.
[4], according to [1]-[3] described in any item curable proppants, wherein the liquid epoxy resin A packet
Include bisphenol A type epoxy resin and/or bisphenol f type epoxy resin.
[5], according to [1]-[4] described in any item curable proppants, wherein the latent curing agent includes poly- second
The curing agent of enol cladding processing；The preferably imidazole curing agent of polyvinyl alcohol cladding processing.
[6], according to [1]-[5] described in any item curable proppants, wherein the flow ability modifying agent includes silicone oil,
Preferably include the combination of one or more of hydroxy silicon oil, methyl-silicone oil, epoxy silicon oil and hydrogenation silicone oil.
[7], according to [1]-[6] described in any item curable proppants, wherein the filler include water soluble filler and
Water-insoluble filler；Preferably, the mass ratio of the water soluble filler and the water-insoluble filler is 8~30:1.
[8], the curable proppant according to [7], wherein the water soluble filler includes potassium acetate, sodium chloride, chlorine
Change the combination of one or more of potassium, dextrin, sodium alginate and sodium benzoate；And/or
The water-insoluble filler includes one or both of silica flour, alumina powder, Paris white and blanc fixe
Above combination.
[9], a kind of described in any item curable proppants in basis [1]-[8], wherein including by the curable support
The step of each component mixing of agent.
[10], a kind of according to [1]-[8] described in any item curable proppants or the preparation method according to [9]
Application of the curable proppant being prepared in ternary composite driving.
The effect of invention
The storage stability of curable proppant of the invention is excellent and resistance to alkali ability is strong, can consolidate in highly basic liquid
Knot, such as: it can be consolidated in the sodium hydroxide solution that 40 DEG C of temperature or more of mass concentration is 1.5%, consolidation strength is greater than
5MPa。
Further, the raw material of the preparation method of curable proppant of the invention is easy to obtain, and preparation method is simple.
Further, curable proppant of the invention can be also used in ternary composite displacement system.
Specific embodiment
It will be detailed below various exemplary embodiments, feature and aspect of the invention.Dedicated word " example herein
Property " mean " being used as example, embodiment or illustrative ".Here as any embodiment illustrated by " exemplary " should not necessarily be construed as
Preferred or advantageous over other embodiments.
In addition, in order to better illustrate the present invention, numerous details is given in specific embodiment below.
It will be appreciated by those skilled in the art that without certain details, the present invention equally be can be implemented.In other example,
Method well known to those skilled in the art, means, equipment and step are not described in detail, in order to highlight master of the invention
Purport.
Such as without Special Statement, unit used in the present invention is SI units, and the number occurred in the present invention
Value, numberical range should all be interpreted as containing the inevitable Systematic Errors of institute in industrial production.
First embodiment
First embodiment of the invention provides a kind of curable proppant.The curable proppant includes that precuring is covered
Film proppant, liquid epoxy resin A, latent curing agent, filler and flow ability modifying agent；Wherein,
With the total weight of the precuring overlay film proppant, the additional amount of the liquid epoxy resin A is 2%-
6%；The additional amount of the latent curing agent is 0.2%-1.8%；The additional amount of the filler is 10%-30%；The stream
The additional amount of dynamic modifying agent is 0.1%-1%.
Curable proppant of the invention can not only solidify in highly basic liquid, consolidation strength is high, but also the flowing of particle
Property good, storage stablize.
<precuring overlay film proppant>
Precuring overlay film proppant of the invention preferably use epoxy resin B, coupling agent and precuring agent to aggregate into
The particle of row precuring coating processing.Specifically:
Aggregate
Aggregate in precuring overlay film proppant of the invention has been the granular loose material of skeleton, support or filling effect
Material.Aggregate of the invention can be proppant aggregate commonly used in the art, as long as it meets finger specified in SY/T5108-2014
Mark.In the present invention, the aggregate can be quartz sand or haydite, and the partial size of particle is 850~425 μm (20/40
Mesh), 600~300 μm (30/50 mesh) or 425~212 μm (40/70 mesh) etc..
Epoxy resin B
The present invention using epoxy resin B to bond aggregate, to form precuring overlay film proppant.With the total of the aggregate
Poidometer, the additional amount of the epoxy resin B are 0.5%-2%；Such as: the additional amount of the epoxy resin B can be
0.7%, 0.9%, 1.2%, 1.5%, 1.7% etc..When the additional amount of the epoxy resin B is between 0.5%-2%, not only
The intensity of curable proppant is improved, more mainly changes the interface performance of aggregate, advantageously reduces liquid asphalt mixtures modified by epoxy resin
The dosage of rouge A is advantageous to the flow conductivity of curable proppant.
In the present invention, the epoxy resin B can be identical as liquid epoxy resin A of the invention, can also not
Together.Such as: epoxy resin B can also be the epoxy resin of solid-like.Specifically, bisphenol-A also can be used in the epoxy resin B
Type epoxy resin, bisphenol A type epoxy resin is condensed under alkaline condition by bisphenol-A, epoxychloropropane, through washing, desolventizing
Refined high-molecular compound.For example, the bisphenol A type epoxy resin can be E-51 epoxy resin, E-44
Epoxy resin, E-42 epoxy resin, E-20 epoxy resin and E-14 epoxy resin etc..
Coupling agent
In the present invention, in order to play the effect of epoxy resin B more effectively, precuring overlay film branch of the invention
Supportting agent also includes coupling agent.In the present invention, with the total weight of the aggregate, the additional amount of the coupling agent is
0.0025%-0.08%, preferably 0.005%-0.04%；Such as: the additional amount of coupling agent can be 0.003%,
0.004%, 0.008%, 0.01%, 0.015%, 0.02%, 0.025%, 0.03%, 0.035%, 0.05%, 0.055%,
0.06%, 0.07% etc..It, can effectively reinforced epoxy B when the additional amount of coupling agent is between 0.0025%-0.08%
With the adhesion strength between aggregate.
In the present invention, the coupling agent can be selected from various coupling agents well known by persons skilled in the art.In order to improve
For aggregate with the adhesive strength of epoxy resin B, the preferably described coupling agent is silane coupling agent.The silane coupling agent can be selected from:
γ-aminopropyltrimethoxysilane, γ-glycidol ether propyl trimethoxy silicane, anilino- methylene triethoxysilane, ten
The combination of one or more of dialkyl group trimethoxy silane, octadecyl trimethoxysilane etc..Selection is more closed
Epoxy resin B can be enhanced with the adhesion strength between aggregate in suitable coupling agent.
Precuring agent
By the present invention in that with precuring agent, to obtain precuring overlay film proppant.In the present invention, with the aggregate
Total weight, the additional amount of the precuring agent are 0.05%-0.6%；Such as: the additional amount of precuring agent can for 0.1%,
0.15%, 0.2%, 0.25%, 0.3%, 0.35%, 0.4%, 0.45%, 0.5%, 0.55% etc..Precuring agent of the invention
The solidfied material of tridimensional network can be generated, improve the intensity of aggregate with the epoxy reaction of epoxy resin B.
In the present invention, the precuring agent can be selected from conventional solidified dose usually used in this field.Preferably, institute
Stating precuring agent includes amine curing agent, preferably includes alicyclic polyamine class curing agent, aromatic polyamine class curing agent, modified rouge
The combination of one or more of the polynary amine curing agent of ring race and modified aromatic polyamine class curing agent.
For example, the alicyclic polyamine class curing agent can be Meng's alkane diamines (MDA), isophorone diamine (IPDA)
With the combination of one or more of 1,3- hexamethylene dimethylamine etc.；The aromatic polyamine class curing agent can be isophthalic
Dimethylamine (m-XDA), diaminodiphenyl-methane (DDM), diamino diphenyl sulfone (DDS)；Modified allicylic polyamine and change
The combination of one or more of property aromatic polyamine etc..And modified allicylic polyamine class curing agent can be to upper
It states alicyclic polyamine class curing agent and is modified processing；Modified aromatic polyamine class curing agent can be more to above-mentioned aromatic series
Amine curing agent is modified processing.
By the present invention in that the intensity of aggregate can be improved with the precuring overlay film proppant and change the superficiality of aggregate
Can, the dosage of curable resin is advantageously reduced, proppant flow conductivity is conducive to.
<liquid epoxy resin A>
By the present invention in that precuring overlay film proppant can be made to solidify in the earth formation with liquid epoxy resin A, it will
Curable proppant is bonded to each other, and prevents proppant from entering stratum depths in high pressure injection and when liquid returns row prevents
Proppant, which returns, to be ejected.In the present invention, with the total weight of the precuring overlay film proppant, the liquid asphalt mixtures modified by epoxy resin
The additional amount of rouge A is 2%-6%；Such as: the additional amount of liquid epoxy resin A can for 2.5%, 3%, 3.5%, 4%,
4.5%, 5%, 5.5% etc..When the additional amount of liquid epoxy resin A is between 2%-6%, liquid ring can be made
The effect of oxygen Resin A effectively plays.If the additional amount of liquid epoxy resin A is lower than 2%, curable proppant particles
Between adhesion strength it is inadequate；If the additional amount of liquid epoxy resin A is higher than 6%, it will increase cost, can also reduce
The flow conductivity in crack.
Specifically, the liquid epoxy resin A can be selected from liquid asphalt mixtures modified by epoxy resin usually used in this field
Rouge A.Preferably, the liquid epoxy resin A of the invention includes bisphenol A type epoxy resin and/or bisphenol F type epoxy
Resin, for example, the bisphenol A type epoxy resin can be E-56D epoxy resin, E-54 epoxy resin, E-51 asphalt mixtures modified by epoxy resin
The combination of one or more of rouge, E-44 epoxy resin etc.；The bisphenol f type epoxy resin can be high mountain asphalt mixtures modified by epoxy resin
CYDF170, CYDF-180 of rouge company, one or more of 6445,6458 etc. the combination of Xinhua Resin Factory, Shanghai.
<latent curing agent>
Latent curing agent, referring to the single-component system for being added to and forming in epoxy resin with it at room temperature has centainly
Storage stability, and the curing agent of curing reaction can be carried out rapidly under the conditions ofs heating, illumination, moisture, pressurization etc..Asphalt mixtures modified by epoxy resin
Rouge/curative systems are cured to realize with step-reaction polymerization, therefore its storage working life is all shorter in general, this
Limit its further genralrlization application in certain fields.Realize that normal temperature storage is stablized, and in heating, illumination, moisture
Or under the action of pressure after initiation reaction, curing reaction will be carried out at once, this is just needed using latent curing agent.
According to geological conditions, the latent curing agent that the present invention uses is solid, forms a tunic by cladding processing, this
Tunic can prevent epoxy resin from contacting initiation reaction with curing agent in room temperature, can be dissolved in water, hide with water contact caudacoria
Property curing agent again can with epoxy resin contact react.In the present invention, with the total weight of the precuring overlay film proppant
Meter, the additive amount of the latent curing agent are 0.2%-1.8%；Such as: the additive amount of latent curing agent can be
0.4%, 0.6%, 0.8%, 1.0%, 1.2%, 1.4%, 1.6% etc..
Specifically, the latent curing agent includes the curing agent of cladding processing.Preferably, the latent curing agent packet
Include the curing agent of polyvinyl alcohol cladding processing；Preferably include the imidazole curing agent of polyvinyl alcohol cladding processing.For example, institute
The imidazole curing agent for stating polyvinyl alcohol cladding processing can be what the cladding that Beijing Qisintal Science & Tech Co., Ltd. produces was handled
2-methylimidazole (trade mark: Qx-2MZ-50), the 2- undecyl imidazole (trade mark: Qx-2UZ-50) of cladding processing, cladding processing
2- phenylimidazole (trade mark: Qx-2PZ-50) and cladding processing 1 benzyl 2 methyl imidazole (trade mark: Qx-B2MZ-50) etc.
One or more of combination, these cladding processing imidazole curing agent, have storage at normal temperature stablize, coating film meet
The characteristic that water can dissolve.
<filler>
Filler can be used for blotting liquid epoxy resin A in the present invention, is conducive to the change of overlay film proppant particles
It does and prevents from agglomerating, convenient for injection oil-well strata crack.With the total weight of the precuring overlay film proppant, the filler
Additional amount is 10%-30%；Such as: the additional amount of filler can be 12%, 15%, 18%, 20%, 22%, 25%, 28%
Deng.When the additional amount of filler is 10%-30%, liquid epoxy resin A can be effectively blotted；If the additional amount of filler
When less than 10%, it is not enough to blot liquid epoxy resin A, if the additional amount of filler is greater than 30%, excessive filler
It will lead to the strength reduction of proppant.
Specifically, in the present invention, the grain diameter of the filler is less than 75 μm.Preferably, the filler includes water
Insoluble filler and water-insoluble filler.The a small amount of water-insoluble filler of addition is conducive to improve consolidation strength and moisture-proof.Preferably,
The mass ratio of the water soluble filler and the water-insoluble filler is 8~30:1；Such as: the water soluble filler with it is described non-
The mass ratio of water soluble filler can be 10:1,12:1,15:1,18:1,20:1,22:1,25:1,28:1 etc..
For example, the water soluble filler can be potassium acetate, sodium chloride, potassium chloride, dextrin, sodium alginate and benzene first
The combination of one or more of sour sodium or potassium etc..The water-insoluble filler can be silica flour, alumina powder, carbonic acid
The combination of one or more of calcium powder and blanc fixe etc..
<flow ability modifying agent>
Flow ability modifying agent can be used in the present invention, so that particle can be made to divide completely when preparing curable proppant
It dissipates, improves the mobility of particle, to obtain the curable proppant haveing excellent performance.In the present invention, the flow ability modifying agent
Additional amount be 0.1%-1%；The additional amount of flow ability modifying agent can for 0.15%, 0.2%, 0.3%, 0.35%, 0.4%,
0.45%, 0.5%, 0.6%, 0.65%, 0.7%, 0.75%, 0.8%, 0.9%, 0.95% etc..
Specifically, flow ability modifying agent of the invention can be flow ability modifying agent commonly used in the art.Preferably, the stream
Dynamic modifying agent can be silicone oil.For example, the silicone oil can be hydroxy silicon oil, methyl-silicone oil, epoxy silicon oil and silane
The combination of one or more of oil etc..
Second embodiment
Second embodiment of the present invention provides a kind of curable proppant of first embodiment according to the present invention
Preparation method comprising the step of mixing each component of the curable proppant.
Specifically, the curable proppant preparation method the following steps are included:
Step 1, it takes precuring overlay film proppant, liquid epoxy resin A and latent curing agent mixing cured, obtains
Cured product；
Step 2, disperse after filler and flow ability modifying agent being added in the cured product, obtain curable proppant.
Further, the curable proppant preparation method the following steps are included:
Step 1, at 50 DEG C hereinafter, taking precuring overlay film proppant, liquid epoxy resin A and latent curing agent mixed
It closes, and stirs 30 ± 10 seconds and solidified, obtain cured product；
Step 2, disperse after filler and flow ability modifying agent being added in the cured product, obtain curable proppant；
Step 3, it by after the curable proppant sieving, packs.
Wherein, the preparation method of the precuring overlay film proppant is the following steps are included: after taking aggregate to heat under stiring
Epoxy resin B and coupling agent is added and stirs evenly；Then precuring agent stirring solidification is added, obtains the support of precuring overlay film
Agent.
Specifically, the precuring overlay film proppant preparation method the following steps are included: by aggregate be heated to 150 DEG C~
230 DEG C, preferably 180 DEG C~210 DEG C, epoxy resin B and coupling agent is added under stiring and stirs evenly, mixing time is preferably
40 ± 10 seconds, it is adhered to epoxy resin B and coupling agent on quartz sand or haydite aggregate；Then precuring agent is added and stirs solid
Change 200 ± 50 seconds；Water is added to cool to 50 DEG C hereinafter, can be directly to prepare curable proppant.
Third embodiment
Third embodiment of the present invention provide a kind of curable proppant according to first embodiment or according to
Application of the curable proppant that the preparation method of second embodiment is prepared in ternary composite driving.
Curable proppant of the invention can solidify in highly basic liquid, consolidation strength is high, and the mobility of particle
Get well, store stabilization etc., it is suitable for ternary composite driving.
Embodiment
Embodiment of the present invention is described in detail below in conjunction with embodiment, but those skilled in the art will
Understand, the following example is merely to illustrate the present invention, and should not be taken as limiting the scope of the invention.It is not specified in embodiment specific
Condition person carries out according to conventional conditions or manufacturer's recommended conditions.Reagents or instruments used without specified manufacturer is
It can be with conventional products that are commercially available.
Convenient for experiment, aggregate used in the present invention selects quartz sand or haydite particles, and the partial size of particle is respectively 850~
425 μm (20/40 mesh) and 600~300 μm (30/50 mesh), particle diameter distribution meets professional standard SY/T5108-2014.
Embodiment 1
The quartz sand that 4 kilograms of partial sizes are 850~425 μm (20/40 mesh) is heated to be put into after 230 DEG C in self-control sand mixer
Stirring is added 0.6 gram of 60 grams of E-14 epoxy resin and gamma-aminopropyl-triethoxy-silane and stirs 40 seconds after being cooled to 210 DEG C；
Diaminodiphenyl-methane (DDM) 6 grams of stirrings are added to solidify 240 seconds；Be added after cooling to 45 DEG C 120 grams of E-54 epoxy resin and
2- undecyl imidazole (the manufacturer: Beijing Qisintal Science & Tech Co., Ltd. of latent curing agent cladding processing；The trade mark: Qx-
2UZ-50) 24 grams and stirring 20 seconds；Filler (60 grams of silica flour, 520 grams of potassium chloride) and flow ability modifying agent hydroxy silicon oil 10 is added
Gram stirring, until particle is completely dispersed, flows freely；Sieving can arrive curable proppant of the invention.
Comparative example 1
The quartz sand that 4 kilograms of partial sizes are 850~425 μm (20/40 mesh) is put into self-control sand mixer and is stirred, E-54 is added
(manufacturer: Beijing caprice has up to science and technology for 180 grams of epoxy resin and the 2- undecyl imidazole of latent curing agent cladding processing
Limit company；The trade mark: Qx-2UZ-50) it 36 grams and stirs 20 seconds；Filler (90 grams of silica flour, 780 grams of potassium chloride) is added and flowing changes
Property 10 grams of hydroxy silicon oil of agent stirrings, until particle is completely dispersed, flows freely；Sieving can arrive curable proppant.
Comparative example 2
The quartz sand that 4 kilograms of partial sizes are 850~425 μm (20/40 mesh) is heated to be put into after 230 DEG C in self-control sand mixer
Stirring is added 0.6 gram of 60 grams of E-14 epoxy resin and gamma-aminopropyl-triethoxy-silane and stirs 40 seconds after being cooled to 210 DEG C；
Diaminodiphenyl-methane (DDM) 6 grams of stirrings are added to solidify 240 seconds；The phenolic aldehyde tree that the trade mark is 1901 is added after cooling to 160 DEG C
120 grams of rouge are stirred 40 seconds；72 grams of methenamine solution stirrings of mass percent concentration 25% are added after adding water to cool to 100 DEG C
20 seconds；4 grams of 8 grams of calcium stearate and hydroxy silicon oil are added when material starts conglomeration and stirs until particle is completely dispersed, cooling,
Sieving, obtains conventional curable proppant.
Performance test
The curable proppant of above-described embodiment 1 and comparative example 1-2 are carried out to consolidation compression strength performance test, knot respectively
Fruit is as shown in table 1.
Table 1
As can be seen from Table 1, the curable proppant of the embodiment of the present application 1 is in 40 DEG C, the NaOH solution of concentration 1.5%
The consolidation compression strength solidified for 24 hours is 8.6Mpa, much higher than the curable branch without using precuring overlay film proppant of comparative example 1
Support agent.
For 24 hours cannot in addition, the Conventional curable proppant of comparative example 2 solidifies in 40 DEG C, the NaOH solution of concentration 1.5%
Forming.
Embodiment 2
Low close haydite (the hundred million prosperous high-tech ceramics Co., Ltd of Pingxiang City for being 600~300 μm (30/50 mesh) by 4 kilograms of partial sizes
Production, bulk density 1.35g/cm3, apparent density 2.38g/cm3) be heated to 220 DEG C after be put into self-control sand mixer and stir, it is cooling
It 60 grams of E-14 epoxy resin and γ -0.6 gram of glycidol ether propyl trimethoxy silicon and is stirred 30 seconds after to 200 DEG C；Between addition
9 grams of stirrings of benzene dimethylamine (m-XDA) solidify 200 seconds；E-51 epoxy resin and CYDF170 epoxy resin are added after cooling to 45 DEG C
Each 80 grams 2- phenylimidazole (manufacturers: Beijing Qisintal Science & Tech Co., Ltd. handled with latent curing agent cladding；Board
Number: Qx-2PZ-50) 32 grams and stirring 20 seconds；It is added filler (140 grams of 80 grams of alumina powder, 540 grams of potassium chloride and Potassium Benzoate)
It is stirred with 12 grams of flow ability modifying agent methyl-silicone oil, until particle is completely dispersed, flows freely；Sieving can arrive of the invention consolidate
Change proppant.
Comparative example 3
The low close haydite same as Example 2 that 4 kilograms of partial sizes are 600~300 μm (30/50 mesh) is heated to 220 DEG C
After be put into self-control sand mixer and stir, E-51 epoxy resin and CYDF170 epoxy resin each 110 grams and latent curing agent is added
Coat the 2- phenylimidazole (manufacturer: Beijing Qisintal Science & Tech Co., Ltd. of processing；The trade mark: Qx-2PZ-50) it 44 grams and stirs
It mixes 20 seconds；Filler (110 grams of alumina powder, 742 grams of potassium chloride and Potassium Benzoate 190) and flow ability modifying agent methyl-silicone oil 12 is added
Gram stirring, until particle is completely dispersed, flows freely；Sieving can arrive curable proppant.
Comparative example 4
The low close haydite same as Example 2 that 4 kilograms of partial sizes are 600~300 μm (30/50 mesh) is heated to 220 DEG C
After be put into self-control sand mixer and stir, 60 grams of E-14 epoxy resin and γ-glycidol ether propyl trimethoxy after being cooled to 200 DEG C
0.6 gram of base silicon simultaneously stirs 30 seconds；The 9 grams of stirrings of m-xylene diamine (m-XDA) curing agent are added to solidify 200 seconds；After cooling to 160 DEG C
160 grams of phenolic resin that the trade mark is 1901 are added to stir 40 seconds；Mass percent concentration 25% is added after adding water to cool to 100 DEG C
96 grams of methenamine solution stir 20 seconds；4 grams of 10 grams of calcium stearate and methyl-silicone oil are added when material starts conglomeration and stirs
It mixes until particle is completely dispersed, cooling, sieving obtains conventional curable proppant.
Performance test
The curable proppant of above-described embodiment 2 and comparative example 3-4 are carried out to consolidation compression strength performance test, knot respectively
Fruit is as shown in table 2.
Table 2
As can be seen from Table 2, the curable proppant of the embodiment of the present application 2 is in 40 DEG C, the NaOH solution of concentration 1.5%
The consolidation compression strength solidified for 24 hours is 11.8Mpa, much higher than comparative example 3 without using the curable of precuring overlay film proppant
Proppant.
For 24 hours cannot in addition, the Conventional curable proppant of comparative example 4 solidifies in 40 DEG C, the NaOH solution of concentration 1.5%
Forming.
Embodiment 3
Low close haydite (the hundred million prosperous high-tech ceramics Co., Ltd of Pingxiang City for being 850~425 μm (20/40 mesh) by 4 kilograms of partial sizes
Production, bulk density 1.45g/cm3, apparent density 2.49g/cm3) be heated to 220 DEG C after be put into self-control sand mixer and stir, it is cooling
It 40 grams of E-51 epoxy resin and γ -0.8 gram of glycidol ether propyl trimethoxy silicon and is stirred 30 seconds after to 200 DEG C；It is added 1,3
The 7.2 grams of stirrings of hexamethylene dimethylamine solidify 160 seconds；140 grams of E-51 epoxy resin and latent curing agent are added after cooling to 45 DEG C
Coat the 2- phenylimidazole (manufacturer: Beijing Qisintal Science & Tech Co., Ltd. of processing；The trade mark: Qx-2PZ-50) it 28 grams and stirs
It mixes 20 seconds；Filler (120 grams of 25 grams of silica flour, 511 grams of potassium chloride and sodium alginate) and flow ability modifying agent methyl-silicone oil 12 is added
Gram stirring, until particle is completely dispersed, flows freely；Sieving can arrive curable proppant of the invention.
Embodiment 4
The quartz sand that 4 kilograms of partial sizes are 425~212 μm (40/70 mesh) is heated to be put into after 210 DEG C in self-control sand mixer
Stirring is added 0.6 gram of 48 grams of E-54 epoxy resin and gamma-aminopropyl-triethoxy-silane and stirs 30 seconds after being cooled to 200 DEG C；
1,3 hexamethylene dimethylamine, 9.6 grams of stirrings are added to solidify 180 seconds；E-54 epoxy resin and E44 epoxy resin are added after cooling to 45 DEG C
Each 100 grams 2-methylimidazole (manufacturers: Beijing Qisintal Science & Tech Co., Ltd. handled with latent curing agent cladding；Board
Number: Qx-2MZ-50) 48 grams and stirring 25 seconds；Filler (171 grams of 85 grams of silica flour, 730 grams of potassium acetate and dextrin) is added and flows
10 grams of modifying agent hydroxy silicon oil stirrings, until particle is completely dispersed, flows freely；Sieving can arrive curable support of the invention
Agent.
Performance test
The curable proppant of above-described embodiment 3-4 is carried out to consolidation compression strength performance test respectively, as a result such as 3 institute of table
Show.
Table 3
As can be seen from Table 3, the curable proppant of the embodiment of the present application 3-4 is at 40 DEG C, the NaOH solution of concentration 1.5%
The middle consolidation compression strength solidified for 24 hours is higher.
The above embodiment of the present invention be only to clearly illustrate example of the present invention, and not be to the present invention
Embodiment restriction.For those of ordinary skill in the art, it can also make on the basis of the above description
Other various forms of variations or variation.There is no necessity and possibility to exhaust all the enbodiments.It is all of the invention
Made any modifications, equivalent replacements, and improvements etc., should be included in the protection of the claims in the present invention within spirit and principle
Within the scope of.
Claims (10)
1. a kind of curable proppant characterized by comprising precuring overlay film proppant, is dived at liquid epoxy resin A
Volt property curing agent, filler and flow ability modifying agent；Wherein,
With the total weight of the precuring overlay film proppant, the additional amount of the liquid epoxy resin A is 2%-6%；
The additional amount of the latent curing agent is 0.2%-1.8%；The additional amount of the filler is 10%-30%；The flowing changes
Property agent additional amount be 0.1%-1%.
2. curable proppant according to claim 1, which is characterized in that the precuring overlay film proppant includes bone
Material, epoxy resin B, coupling agent and precuring agent；Wherein, with the total weight of the aggregate, the additional amount of the epoxy resin B
For 0.5%-2%；The additional amount of the coupling agent is 0.0025%-0.08%；The additional amount of the precuring agent is 0.05%-
0.6%.
3. curable proppant according to claim 2, which is characterized in that the epoxy resin B includes bisphenol type epoxy
Resin；And/or
The precuring agent includes amine curing agent, preferably include alicyclic polyamine class curing agent, aromatic polyamine class curing agent,
The combination of one or more of modified allicylic polyamine and modified aromatic polyamine；And/or
The coupling agent includes silane coupling agent, preferably includes γ-aminopropyltrimethoxysilane, γ-glycidol ether propyl
Trimethoxy silane, anilino- methylene triethoxysilane, dodecyltrimethoxysilane and octadecyl silicon
The combination of one or more of alkane.
4. curable proppant according to claim 1-3, which is characterized in that the liquid epoxy resin
A includes bisphenol A type epoxy resin and/or bisphenol f type epoxy resin.
5. curable proppant according to claim 1-4, which is characterized in that the latent curing agent includes
The curing agent of polyvinyl alcohol cladding processing；The preferably imidazole curing agent of polyvinyl alcohol cladding processing.
6. curable proppant according to claim 1-5, which is characterized in that the flow ability modifying agent includes silicon
Oil preferably includes the combination of one or more of hydroxy silicon oil, methyl-silicone oil, epoxy silicon oil and hydrogenation silicone oil.
7. curable proppant according to claim 1-6, which is characterized in that the filler is filled out including water solubility
Material and water-insoluble filler；Preferably, the mass ratio of the water soluble filler and the water-insoluble filler is 8~30:1.
8. curable proppant according to claim 7, which is characterized in that the water soluble filler includes potassium acetate, chlorine
Change the combination of one or more of sodium, potassium chloride, dextrin, sodium alginate and sodium benzoate；And/or
The water-insoluble filler includes one or more of silica flour, alumina powder, Paris white and blanc fixe
Combination.
9. a kind of curable proppant according to claim 1-8, which is characterized in that including will be described curable
The step of each component mixing of proppant.
10. a kind of curable proppant according to claim 1-8 or preparation according to claim 9
Application of the curable proppant that method is prepared in ternary composite driving.
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| CN110982509A (en) * | 2019-10-24 | 2020-04-10 | 白成才 | High-temperature self-curing proppant and preparation method thereof |
| CN111690399A (en) * | 2020-04-27 | 2020-09-22 | 北京大德广源石油技术服务有限公司 | Sand control agent for fracturing and use method thereof |
| CN111804373A (en) * | 2020-06-24 | 2020-10-23 | 程雅雯 | Method for manufacturing gravel special for sand prevention and thin production of heavy oil well |
| CN112680205A (en) * | 2019-10-17 | 2021-04-20 | 中国石油化工股份有限公司 | Surfactant oil displacement system and preparation method thereof |
| CN112680209A (en) * | 2019-10-17 | 2021-04-20 | 中国石油化工股份有限公司 | Proppant and preparation method thereof |
| CN114540003A (en) * | 2021-12-31 | 2022-05-27 | 新疆中凌工程技术有限公司 | Proppant fracture surface flow conductivity reinforcing agent for volume fracturing |
| CN115322766A (en) * | 2022-08-18 | 2022-11-11 | 北京奇想达新材料有限公司 | Bi-component low-temperature curable coated proppant and preparation method thereof |
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| CN114540003A (en) * | 2021-12-31 | 2022-05-27 | 新疆中凌工程技术有限公司 | Proppant fracture surface flow conductivity reinforcing agent for volume fracturing |
| CN115322766A (en) * | 2022-08-18 | 2022-11-11 | 北京奇想达新材料有限公司 | Bi-component low-temperature curable coated proppant and preparation method thereof |
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