CN112877048A - Sand consolidation agent for oil field and preparation method thereof - Google Patents
Sand consolidation agent for oil field and preparation method thereof Download PDFInfo
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- C09K8/56—Compositions for consolidating loose sand or the like around wells without excessively decreasing the permeability thereof
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Abstract
The invention discloses a sand consolidation agent for an oil field, which comprises the following raw materials in parts by weight: 0.8-1 part of modified silicon dioxide, 7-10 parts of epoxy resin, 3-6 parts of modified epoxy resin, 0.3-0.5 part of emulsifier, 30-40 parts of acidic aqueous solution and 0.5-1 part of curing agent; the modified epoxy resin is prepared by combining epoxy resin and organic silicon resin with hydroxyl and alkoxy at the tail end. The invention has the advantages of high consolidation strength and applicability to different sand grain sizes.
Description
Technical Field
The invention relates to the technical field of oilfield exploitation. More specifically, the invention relates to a sand consolidation agent for an oil field and a preparation method thereof.
Background
The rock structure of a well bottom accessory zone is easily damaged by various comprehensive factors such as oil well exploitation, operation and the like, so that part of dropped stratum sand flows into a shaft along with oil layer fluid, namely, the sand production phenomenon of the oil well occurs, and the sand production of the oil well causes a series of adverse effects such as sand burying of an oil layer, sand blockage of the shaft, sand clamping of equipment abrasion, collapse of a shaft wall and the like, so that the difficulty of oil field exploitation operation and the exploitation cost are greatly increased.
In order to reduce the risk of sand production from the oil well, sand control technology is required to ensure the normal production of the oil well. Chemical sand control is an important sand control means, and is popular in the technical field of oil fields because of the capability of treating both symptoms and root causes; the chemical sand-preventing method is to squeeze chemical agent or mixture of chemical agent and sand into natural consolidated unconsolidated stratum to make stratum grains cemented on contact points to form continuous penetrating skeleton, so as to reach the aims of filling, consolidation and raising stratum strength. The extruded chemical agent is a sand consolidation agent, and the sand consolidation agent used in the prior art generally exists: high production cost, low consolidation strength, narrow particle size application range and the like.
Disclosure of Invention
An object of the present invention is to solve at least the above problems and to provide at least the advantages described later.
Still another object of the present invention is to provide a sand consolidation agent for oil field, which has the beneficial effects of high consolidation strength and applicability to different sand production particle sizes.
The invention also aims to provide a preparation method of the sand consolidation agent for the oil field, which has simple preparation process and low production cost.
To achieve these objects and other advantages in accordance with the present invention, there is provided an oilfield sand consolidation agent comprising the following raw materials in parts by weight: 0.8-1 part of modified silicon dioxide, 7-10 parts of epoxy resin, 3-6 parts of modified epoxy resin, 0.3-0.5 part of emulsifier, 30-40 parts of acidic aqueous solution and 0.5-1 part of curing agent;
the modified epoxy resin is prepared by combining epoxy resin and organic silicon resin with hydroxyl and alkoxy at the tail end;
the outer surface of the modified epoxy resin is sequentially coated with ethylene-vinyl acetate copolymer and water-soluble polymer.
Preferably, the preparation method of the modified epoxy resin is as follows:
step a1, weighing 30-48 parts by weight of epoxy resin, adding the epoxy resin into a four-mouth reaction bottle preheated to 80-120 ℃, heating the reaction bottle to 120-200 ℃ after the epoxy resin is completely melted, vacuumizing the reaction bottle to-0.02-0.095 MPa, and keeping the vacuum for 20-40 min;
step a2, weighing 1-15 parts of organic silicon resin, adding into a reaction bottle, and stirring until the organic silicon resin and the molten epoxy resin are uniformly mixed; wherein the structural formula of the organic silicon resin is shown as follows:
wherein R in the above formula is alkoxy, and the dotted line represents a repeating unit; the molecular weight of the organic silicon resin is 600-3000, and the functionality is 3-20;
step a3, weighing 0.05-1 part of triethanolamine, adding the triethanolamine into a reaction bottle, heating the reaction bottle to 120-200 ℃, stirring and reacting for 3-5 hours, vacuumizing the reaction bottle to-0.02-0.095 MPa, maintaining for 20-40 min, and discharging to obtain the modified epoxy resin.
Preferably, the preparation method of the modified silica comprises the following steps:
b1, uniformly mixing cyclohexane, a surfactant and n-hexanol to obtain a mixed solution, adding water into the mixed solution, and stirring for 5min to obtain a microcapsule solution; wherein the volume ratio of the cyclohexane to the surfactant to the n-hexanol to the water is 4.2:1:1: 0.2;
step b2, uniformly mixing ethyl orthosilicate and N- (beta-aminoethyl) -gamma-aminopropyltriethoxysilane, adding the mixture into microcapsule liquid, uniformly stirring, adding ammonia water into the microcapsule liquid, stirring for reacting for 24 hours, adding acetone into the microcapsule liquid, removing filtrate through centrifugal separation, drying, and crushing to obtain aminated silicon dioxide with the particle size of 80-100 nm; the volume ratio of the ethyl orthosilicate to the N- (beta-aminoethyl) -gamma-aminopropyltriethoxysilane to the acetone to the N-hexanol is 1:1:5: 20;
step b3, dispersing the aminated silicon dioxide obtained in the step b2 in absolute ethyl alcohol, adding 3-aminopropyltriethoxysilane under stirring at normal temperature, stirring for reaction for 6 hours, centrifuging for 1-3 times, and washing to obtain an aminated silicon dioxide dispersion liquid, wherein the adding amount ratio of the aminated silicon dioxide, the absolute ethyl alcohol and the 3-aminopropyltriethoxysilane is 1g:200mL:2 mL;
step b4, dispersing graphene oxide in ultrapure water, performing ultrasonic treatment for 6-8 hours, centrifuging, and taking supernatant to obtain graphene oxide dispersion liquid, wherein the mass concentration of the graphene oxide dispersion liquid is 0.001 mg/mL; dropwise adding the graphene oxide dispersion liquid into the aminated silicon dioxide dispersion liquid under the stirring of the aminated silicon dioxide dispersion liquid, continuously stirring for 1h with strong force, gradually reducing the stirring speed until the mixture is static, then centrifugally collecting filter residues, and drying to obtain modified silicon dioxide; the volume ratio of the graphene oxide dispersion to the aminated silica dispersion was 1: 2.
Preferably, the sand consolidation agent for the oil field is characterized in that the outer surface of the modified silicon dioxide is sequentially coated with the ethylene-vinyl acetate copolymer and the water-soluble polymer from inside to outside.
Preferably, the sand consolidation agent for the oil field is cyclohexane diamine.
Preferably, the sand consolidation agent for the oil field is characterized in that the emulsifier is tween 80.
The invention provides a preparation method of a sand consolidation agent for an oil field, which comprises the following steps of dissolving 7-10 parts of epoxy resin by 20-24 parts of acetone according to parts by weight to obtain an epoxy resin solution; adding 0.8-1 part of modified silicon dioxide and 3-6 parts of modified epoxy resin into 30-40 parts of acidic aqueous solution, and stirring to obtain modified liquid; heating the epoxy resin solution to 40-50 ℃, stirring, sequentially adding 0.3-0.5 part of emulsifier and modifying solution into the epoxy resin solution, keeping the temperature, stirring, reacting for 2-4 h, stopping heating, and naturally cooling to room temperature to obtain a reaction solution; and dropwise adding 0.5-1 part of curing agent into the reaction liquid under stirring, and continuously stirring for 10-15 min to obtain the high-performance organic silicon/inorganic composite material.
The invention at least comprises the following beneficial effects:
1. the invention takes epoxy resin as a primary agent and takes modified epoxy resin and modified silicon dioxide as a candidate agent; the outer surfaces of the modified silicon dioxide and the modified epoxy resin are coated with a layer of ethylene-vinyl acetate copolymer, so that the modified silicon dioxide and the modified epoxy resin can be effectively prevented from contacting with other raw materials of the sand consolidation agent before operation, the release of the modified silicon dioxide and the modified epoxy resin is delayed, the sand consolidation performance in a high-temperature environment in the deep part of an oil well is ensured, and the storage stability of the sand consolidation agent is improved; when the sand consolidation agent enters an oil well, the modified epoxy resin plays a leading role, when the sand consolidation agent continues to enter the deep part of the oil well, the temperature rises, the ethylene-vinyl acetate copolymer melts, the modified epoxy resin is released to supplement the main sand consolidation agent, the influence of the temperature rise on the sand consolidation performance is reduced, and the sand consolidation efficiency of the sand consolidation agent is improved;
2. according to the invention, the silicone resin with silanol hydroxyl and alkoxy at the tail end is modified on the outer surface of the epoxy resin, and the alkoxy and silanol at the tail end of the silicone resin and the polar group on the surface of sand grains form a stable Si-O-Si covalent bond under the heating action in an acidic sand consolidation agent system under a high-temperature oil well, so that a layer of viscous film is formed on the surface of the sand grains, and the consolidation strength and the sand consolidation efficiency of the sand consolidation agent can be greatly improved by matching with the sand consolidation effect of an epoxy resin body; meanwhile, the modified silicon dioxide is added into the sand consolidation agent, so that the consolidation strength and the sand consolidation efficiency can be further improved;
3. the invention utilizes the organic silicon resin with the tail end containing silanol hydroxyl and alkoxy to carry out bulk chemical reaction modification on the epoxy resin, effectively improves the compatibility of the two resins, has simple process in the whole modification process, does not use organic solvent, has a small amount of water or recyclable methanol as a byproduct, and has the advantages of environmental protection;
4. firstly, in-situ synthesis of aminated silica nanoparticles is carried out, so that the silica nanoparticles can effectively generate net positive electricity, then the aminated silica is modified by graphene oxide, the graphene oxide contains a large number of oxygen-containing polar groups such as hydroxyl, carboxyl and epoxy groups, has a high specific surface area, can well adsorb fine silt, and under the action of positive charges of the silica, the fine silt is aggregated to form a large fine silt combination body, so that the consolidation of the fine silt is realized; the modified silicon dioxide is nano-scale and can enter the pores and then be released to solidify the fine sand in the pores, so that the application range of the sand grain size of the sand solidification agent is enlarged.
Additional advantages, objects, and features of the invention will be set forth in part in the description which follows and in part will become apparent to those having ordinary skill in the art upon examination of the following or may be learned from practice of the invention.
Detailed Description
The present invention is further described in detail below with reference to examples so that those skilled in the art can practice the invention with reference to the description.
It will be understood that terms such as "having," "including," and "comprising," as used herein, do not preclude the presence or addition of one or more other elements or groups thereof.
It is to be noted that the experimental methods described in the following embodiments are all conventional methods unless otherwise specified, and the reagents and materials are commercially available unless otherwise specified.
< example 1a >
The sand consolidation agent for the oil field comprises the following raw materials in parts by weight: 0.8 part of modified silicon dioxide, 7 parts of epoxy resin, 3 parts of modified epoxy resin, 0.3 part of Tween 80, 30 parts of acidic aqueous solution and 0.5 part of cyclohexanediamine;
the modified epoxy resin is prepared by combining epoxy resin and organic silicon resin with hydroxyl and alkoxy at the tail end;
the outer surface of the modified silicon dioxide and the outer surface of the modified epoxy resin are sequentially coated with ethylene-vinyl acetate copolymer and water-soluble polymer from inside to outside;
the preparation method of the modified epoxy resin comprises the following steps:
step a1, weighing 30 parts of epoxy resin by weight, adding the epoxy resin into a four-mouth reaction bottle preheated to 80 ℃, heating the reaction bottle to 120 ℃ after the epoxy resin is completely melted, vacuumizing the reaction bottle to-0.02 MPa, and keeping the reaction bottle in vacuum for 20 min;
step a2, weighing 1 part of organic silicon resin, adding the organic silicon resin into a reaction bottle, and stirring until the organic silicon resin and the molten epoxy resin are uniformly mixed; wherein the structural formula of the organic silicon resin is shown as follows:
wherein R in the above formula is alkoxy, and the dotted line represents a repeating unit; the molecular weight of the organic silicon resin is 600-3000, and the functionality is 3-20;
step a3, weighing 0.05 part of triethanolamine, adding into a reaction bottle, heating the reaction bottle to 120 ℃, stirring for reaction for 3 hours, vacuumizing the reaction bottle to-0.02 MPa, maintaining for 20min, and discharging to obtain the modified epoxy resin.
The preparation method of the modified silicon dioxide comprises the following steps:
b1, uniformly mixing cyclohexane, a surfactant and n-hexanol to obtain a mixed solution, adding water into the mixed solution, and stirring for 5min to obtain a microcapsule solution; wherein the volume ratio of the cyclohexane to the surfactant to the n-hexanol to the water is 4.2:1:1: 0.2;
step b2, uniformly mixing ethyl orthosilicate and N- (beta-aminoethyl) -gamma-aminopropyltriethoxysilane, adding the mixture into microcapsule liquid, uniformly stirring, adding ammonia water into the microcapsule liquid, stirring for reacting for 24 hours, adding acetone into the microcapsule liquid, removing filtrate through centrifugal separation, drying, and crushing to obtain aminated silicon dioxide with the particle size of 80 nm; the volume ratio of the ethyl orthosilicate to the N- (beta-aminoethyl) -gamma-aminopropyltriethoxysilane to the acetone to the N-hexanol is 1:1:5: 20;
step b3, dispersing the aminated silicon dioxide obtained in the step b2 in absolute ethyl alcohol, adding 3-aminopropyltriethoxysilane under stirring at normal temperature, stirring for reacting for 6 hours, centrifuging for 1 time, and washing with water to obtain an aminated silicon dioxide dispersion liquid, wherein the adding amount ratio of the aminated silicon dioxide, the absolute ethyl alcohol and the 3-aminopropyltriethoxysilane is 1g:200mL:2 mL;
step b4, dispersing graphene oxide in ultrapure water, performing ultrasonic treatment for 6 hours, centrifuging and taking supernate to obtain graphene oxide dispersion liquid, wherein the mass concentration of the graphene oxide dispersion liquid is 0.001 mg/mL; dropwise adding the graphene oxide dispersion liquid into the aminated silicon dioxide dispersion liquid under the stirring of the aminated silicon dioxide dispersion liquid, continuously stirring for 1h with strong force, gradually reducing the stirring speed until the mixture is static, then centrifugally collecting filter residues, and drying to obtain modified silicon dioxide; the volume ratio of the graphene oxide dispersion liquid to the silica dioxide-based dispersion liquid is 1: 2.
< example 2a >
The sand consolidation agent for the oil field comprises the following raw materials in parts by weight: 1 part of modified silicon dioxide, 10 parts of epoxy resin, 6 parts of modified epoxy resin, 0.5 part of Tween 80, 40 parts of acidic aqueous solution and 1 part of cyclohexanediamine;
the modified epoxy resin is prepared by combining epoxy resin and organic silicon resin with hydroxyl and alkoxy at the tail end;
the outer surface of the modified silicon dioxide and the outer surface of the modified epoxy resin are sequentially coated with ethylene-vinyl acetate copolymer and water-soluble polymer from inside to outside;
the preparation method of the modified epoxy resin comprises the following steps:
step a1, weighing 48 parts by weight of epoxy resin, adding the epoxy resin into a four-mouth reaction bottle preheated to 120 ℃, heating the reaction bottle to 200 ℃ after the epoxy resin is completely melted, vacuumizing the reaction bottle to 0.095MPa, and keeping the reaction bottle in vacuum for 40 min;
step a2, weighing 15 parts of organic silicon resin, adding the organic silicon resin into a reaction bottle, and stirring until the organic silicon resin and the molten epoxy resin are uniformly mixed; wherein the structural formula of the organic silicon resin is shown as follows:
wherein R in the above formula is alkoxy, and the dotted line represents a repeating unit; the molecular weight of the organic silicon resin is 600-3000, and the functionality is 3-20;
step a3, weighing 1 part of triethanolamine, adding into a reaction bottle, heating the reaction bottle to 200 ℃, stirring for reaction for 5 hours, vacuumizing the reaction bottle to 0.095MPa, maintaining for 40min, and discharging to obtain the modified epoxy resin.
The preparation method of the modified silicon dioxide comprises the following steps:
b1, uniformly mixing cyclohexane, a surfactant and n-hexanol to obtain a mixed solution, adding water into the mixed solution, and stirring for 5min to obtain a microcapsule solution; wherein the volume ratio of the cyclohexane to the surfactant to the n-hexanol to the water is 4.2:1:1: 0.2;
step b2, uniformly mixing ethyl orthosilicate and N- (beta-aminoethyl) -gamma-aminopropyltriethoxysilane, adding the mixture into microcapsule liquid, uniformly stirring, adding ammonia water into the microcapsule liquid, stirring for reacting for 24 hours, adding acetone into the microcapsule liquid, removing filtrate through centrifugal separation, drying, and crushing to obtain aminated silicon dioxide with the particle size of 100 nm; the volume ratio of the ethyl orthosilicate to the N- (beta-aminoethyl) -gamma-aminopropyltriethoxysilane to the acetone to the N-hexanol is 1:1:5: 20;
step b3, dispersing the aminated silicon dioxide obtained in the step b2 in absolute ethyl alcohol, adding 3-aminopropyltriethoxysilane under stirring at normal temperature, reacting for 6 hours under stirring, centrifuging for 3 times, washing with water to obtain an aminated silicon dioxide dispersion, wherein the adding amount ratio of the aminated silicon dioxide, the absolute ethyl alcohol and the 3-aminopropyltriethoxysilane is 1g:200mL:2 mL;
step b4, dispersing graphene oxide in ultrapure water, performing ultrasonic treatment for 8 hours, centrifuging and taking supernate to obtain graphene oxide dispersion liquid, wherein the mass concentration of the graphene oxide dispersion liquid is 0.001 mg/mL; dropwise adding the graphene oxide dispersion liquid into the aminated silicon dioxide dispersion liquid under the stirring of the aminated silicon dioxide dispersion liquid, continuously stirring for 1h with strong force, gradually reducing the stirring speed until the mixture is static, then centrifugally collecting filter residues, and drying to obtain modified silicon dioxide; the volume ratio of the graphene oxide dispersion to the aminated silica dispersion was 1: 2.
< example 3a >
The sand consolidation agent for the oil field comprises the following raw materials in parts by weight: 0.9 part of modified silicon dioxide, 9 parts of epoxy resin, 5 parts of modified epoxy resin, 0.4 part of Tween 80, 35 parts of acidic aqueous solution and 0.8 part of cyclohexanediamine;
the modified epoxy resin is prepared by combining epoxy resin and organic silicon resin with hydroxyl and alkoxy at the tail end;
the outer surface of the modified silicon dioxide and the outer surface of the modified epoxy resin are sequentially coated with ethylene-vinyl acetate copolymer and water-soluble polymer from inside to outside;
the preparation method of the modified epoxy resin comprises the following steps:
step a1, weighing 39 parts by weight of epoxy resin, adding the epoxy resin into a four-mouth reaction bottle preheated to 100 ℃, heating the reaction bottle to 160 ℃ after the epoxy resin is completely melted, vacuumizing the reaction bottle to 0.048MPa, and keeping the reaction bottle in vacuum for 30 min;
step a2, weighing 8 parts of organic silicon resin, adding the organic silicon resin into a reaction bottle, and stirring until the organic silicon resin and the molten epoxy resin are uniformly mixed; wherein the structural formula of the organic silicon resin is shown as follows:
wherein R in the above formula is alkoxy, and the dotted line represents a repeating unit; the molecular weight of the organic silicon resin is 600-3000, and the functionality is 3-20;
step a3, weighing 0.08 part of triethanolamine, adding into a reaction bottle, heating the reaction bottle to 160 ℃, stirring for reaction for 4 hours, vacuumizing the reaction bottle to 0.048MPa, maintaining for 30min, and discharging to obtain the modified epoxy resin.
The preparation method of the modified silicon dioxide comprises the following steps:
b1, uniformly mixing cyclohexane, a surfactant and n-hexanol to obtain a mixed solution, adding water into the mixed solution, and stirring for 5min to obtain a microcapsule solution; wherein the volume ratio of the cyclohexane to the surfactant to the n-hexanol to the water is 4.2:1:1: 0.2;
step b2, uniformly mixing ethyl orthosilicate and N- (beta-aminoethyl) -gamma-aminopropyltriethoxysilane, adding the mixture into microcapsule liquid, uniformly stirring, adding ammonia water into the microcapsule liquid, stirring for reacting for 24 hours, adding acetone into the microcapsule liquid, removing filtrate through centrifugal separation, drying, and crushing to obtain aminated silicon dioxide with the particle size of 90 nm; the volume ratio of the ethyl orthosilicate to the N- (beta-aminoethyl) -gamma-aminopropyltriethoxysilane to the acetone to the N-hexanol is 1:1:5: 20;
step b3, dispersing the aminated silicon dioxide obtained in the step b2 in absolute ethyl alcohol, adding 3-aminopropyltriethoxysilane under stirring at normal temperature, stirring for reacting for 6 hours, centrifuging for 2 times, washing with water to obtain an aminated silicon dioxide dispersion liquid, wherein the adding amount ratio of the aminated silicon dioxide, the absolute ethyl alcohol and the 3-aminopropyltriethoxysilane is 1g:200mL:2 mL;
step b4, dispersing graphene oxide in ultrapure water, performing ultrasonic treatment for 7 hours, centrifuging and taking supernate to obtain graphene oxide dispersion liquid, wherein the mass concentration of the graphene oxide dispersion liquid is 0.001 mg/mL; dropwise adding the graphene oxide dispersion liquid into the aminated silicon dioxide dispersion liquid under the stirring of the aminated silicon dioxide dispersion liquid, continuously stirring for 1h with strong force, gradually reducing the stirring speed until the mixture is static, then centrifugally collecting filter residues, and drying to obtain modified silicon dioxide; the volume ratio of the graphene oxide dispersion to the aminated silica dispersion was 1: 2.
< example 1b >
A preparation method of a sand consolidation agent for an oil field comprises the following steps: dissolving 7 parts of epoxy resin by 20 parts of acetone according to parts by weight to obtain an epoxy resin solution; adding 0.8 part of modified silicon dioxide and 3 parts of modified epoxy resin into 30 parts of acidic aqueous solution, and stirring to obtain modified liquid; heating the epoxy resin solution to 40 ℃, stirring, sequentially adding 0.3 part of emulsifier and modification solution into the epoxy resin solution, keeping the temperature, stirring and reacting for 2 hours, stopping heating, and naturally cooling to room temperature to obtain a reaction solution; and dropwise adding 0.5 part of cyclohexanediamine into the reaction solution under stirring, and continuously stirring for 10min to obtain the catalyst.
< example 2b >
A method for preparing a sand consolidation agent for oil fields, which comprises the following steps according to the raw material formula and dosage of < example 2a >: dissolving 10 parts of epoxy resin by using 24 parts of acetone according to parts by weight to obtain an epoxy resin solution; adding 1 part of modified silicon dioxide and 3-6 parts of modified epoxy resin into 40 parts of acidic aqueous solution, and stirring to obtain modified liquid; heating the epoxy resin solution to 50 ℃, stirring, sequentially adding 0.5 part of emulsifier and modification solution into the epoxy resin solution, keeping the temperature, stirring and reacting for 4 hours, stopping heating, and naturally cooling to room temperature to obtain a reaction solution; dropwise adding 1 part of cyclohexanediamine into the reaction solution under stirring, and continuously stirring for 15min to obtain the catalyst.
< example 3b >
A method for preparing a sand consolidation agent for oil fields, which comprises the following steps according to the raw material formula and dosage of < example 3a >: dissolving 9 parts of epoxy resin by 22 parts of acetone according to parts by weight to obtain an epoxy resin solution; adding 0.9 part of modified silicon dioxide and 5 parts of modified epoxy resin into 35 parts of acidic aqueous solution, and stirring to obtain modified liquid; heating the epoxy resin solution to 45 ℃, stirring, sequentially adding 0.4 part of tween 80 and the modifying solution into the epoxy resin solution, keeping the temperature, stirring and reacting for 3 hours, stopping heating, and naturally cooling to room temperature to obtain a reaction solution; and dropwise adding 0.8 part of cyclohexanediamine into the reaction solution under stirring, and continuously stirring for 13min to obtain the catalyst.
< comparative example 1>
The sand consolidation agent for the oil field comprises the following raw materials in parts by weight: 14.9 parts of epoxy resin, 0.4 part of Tween 80, 35 parts of acidic aqueous solution and 0.8 part of cyclohexanediamine;
a preparation method of a sand consolidation agent for an oil field comprises the following steps: dissolving 14.9 parts of epoxy resin by 22 parts of acetone according to parts by weight to obtain an epoxy resin solution; heating the epoxy resin solution to 45 ℃, stirring, sequentially adding 0.4 part of Tween 80 and 35 parts of acidic aqueous solution into the epoxy resin solution, keeping the temperature, stirring and reacting for 3 hours, stopping heating, and naturally cooling to room temperature to obtain a reaction solution; and dropwise adding 0.8 part of cyclohexanediamine into the reaction solution under stirring, and continuously stirring for 13min to obtain the catalyst.
< comparative example 2>
The sand consolidation agent for the oil field comprises the following raw materials in parts by weight: 14 parts of epoxy resin, 0.9 part of silicon dioxide, 80 parts of tween, 35 parts of acidic aqueous solution and 0.8 part of cyclohexanediamine;
a preparation method of a sand consolidation agent for an oil field comprises the following steps: dissolving 14 parts of epoxy resin by 22 parts of acetone according to parts by weight to obtain an epoxy resin solution; dispersing 0.9 part of silicon dioxide in 35 parts of acidic aqueous solution to obtain silicon dioxide dispersion liquid; heating the epoxy resin solution to 45 ℃, stirring, sequentially adding 0.4 part of tween 80 and the silicon dioxide dispersion liquid into the epoxy resin solution, keeping the temperature, stirring and reacting for 3 hours, stopping heating, and naturally cooling to room temperature to obtain a reaction solution; and dropwise adding 0.8 part of cyclohexanediamine into the reaction solution under stirring, and continuously stirring for 13min to obtain the catalyst.
< test example >
1. Consolidation Performance at different temperatures
The sand consolidation agent prepared in the embodiment 3b and the comparative examples 1-2 of the invention is subjected to performance test, and the consolidation performance of the sand consolidation agent on 20-40-mesh sand grains is tested, wherein the method specifically comprises the following steps: 100g of sand grains and 25mL of sand consolidation agent were charged into a glass tube, and cured at different temperatures (60 ℃, 80 ℃, 120 ℃ and 200 ℃) for 12 hours, and the compressive strength and the flexural strength of the consolidated core were measured, and the results are shown in Table 1:
TABLE 1 Sand consolidation Performance of sand consolidation agent on sand grains at different temperatures
As can be seen from Table 1, the sand consolidation agent prepared in the embodiment 3b of the invention has good temperature resistance compared with the comparative examples 1-2, and has good applicability to the exploitation of high-temperature oil wells;
at 60 ℃, the epoxy resin is mainly used as a curing main agent, so that the curing performance of the sand consolidation agent in the embodiment 1 is most excellent, when the temperature is 80 ℃, the self-aggregation of the epoxy resin is intensified, the curing efficiency of sand grains is reduced, while the film formed by the ethylene-vinyl acetate copolymer in the sand consolidation agent in the embodiment 3b begins to crack, the modified epoxy resin and the modified silicon dioxide are released, the sand grains can be well aggregated to form a stable curing layer, and the modified epoxy resin and the modified silicon dioxide have better permeability compared with the curing layer of the epoxy resin; when the temperature is 120 ℃, the film formed by the ethylene-vinyl acetate copolymer is rapidly cracked, and a large amount of modified epoxy resin and modified silicon dioxide are released, so that the compressive strength and the permeability of the bonding layer are further improved.
2. Consolidation of sand grains of different sizes: respectively putting quartz sand of 60-80 meshes and quartz sand of 100-120 meshes and the sand consolidation agent prepared in the embodiment 3b of the invention into a glass tube, solidifying for 12 hours at 120 ℃, measuring the compressive strength of the consolidated body to be 6.42MPa and 7.21 respectively, the flexural strength to be 2.93MPa and 3.28MPa respectively, and the permeability to be 1.78 mu m respectively2And 0.18 μm2Therefore, it can be seen that the embodiment 3b of the present invention is applicable to sand grains with different grain sizes, and the larger the mesh number is, the smaller the surface grain size is, the smaller the voids of the sand grains with small grain sizes after consolidation become smaller, the strength is increased, and the permeability is reduced.
The number of apparatuses and the scale of the process described herein are intended to simplify the description of the present invention. Applications, modifications and variations of the present invention will be apparent to those skilled in the art.
While embodiments of the invention have been disclosed above, it is not limited to the applications listed in the description and the embodiments, which are fully applicable in all kinds of fields of application of the invention, and further modifications may readily be effected by those skilled in the art, so that the invention is not limited to the specific details without departing from the general concept defined by the claims and the scope of equivalents.
Claims (7)
1. The sand consolidation agent for the oil field is characterized by comprising the following raw materials in parts by weight: 0.8-1 part of modified silicon dioxide, 7-10 parts of epoxy resin, 3-6 parts of modified epoxy resin, 0.3-0.5 part of emulsifier, 30-40 parts of acidic aqueous solution and 0.5-1 part of curing agent;
the modified epoxy resin is prepared by combining epoxy resin and organic silicon resin with hydroxyl and alkoxy at the tail end;
the outer surface of the modified epoxy resin is sequentially coated with ethylene-vinyl acetate copolymer and water-soluble polymer.
2. The sand consolidation agent for the oil field according to claim 1, wherein the preparation method of the modified epoxy resin comprises the following steps:
step a1, weighing 30-48 parts by weight of epoxy resin, adding the epoxy resin into a four-mouth reaction bottle preheated to 80-120 ℃, heating the reaction bottle to 120-200 ℃ after the epoxy resin is completely melted, vacuumizing the reaction bottle to-0.02-0.095 MPa, and keeping the vacuum for 20-40 min;
step a2, weighing 1-15 parts of organic silicon resin, adding into a reaction bottle, and stirring until the organic silicon resin and the molten epoxy resin are uniformly mixed; wherein the structural formula of the organic silicon resin is shown as follows:
wherein R in the above formula is alkoxy, and the dotted line represents a repeating unit; the molecular weight of the organic silicon resin is 600-3000, and the functionality is 3-20;
step a3, weighing 0.05-1 part of triethanolamine, adding the triethanolamine into a reaction bottle, heating the reaction bottle to 120-200 ℃, stirring and reacting for 3-5 hours, vacuumizing the reaction bottle to-0.02-0.095 MPa, maintaining for 20-40 min, and discharging to obtain the modified epoxy resin.
3. The sand consolidation agent for the oil field according to claim 2, wherein the preparation method of the modified silica comprises the following steps:
b1, uniformly mixing cyclohexane, a surfactant and n-hexanol to obtain a mixed solution, adding water into the mixed solution, and stirring for 5min to obtain a microcapsule solution; wherein the volume ratio of the cyclohexane to the surfactant to the n-hexanol to the water is 4.2:1:1: 0.2;
step b2, uniformly mixing ethyl orthosilicate and N- (beta-aminoethyl) -gamma-aminopropyltriethoxysilane, adding the mixture into microcapsule liquid, uniformly stirring, adding ammonia water into the microcapsule liquid, stirring for reacting for 24 hours, adding acetone into the microcapsule liquid, removing filtrate through centrifugal separation, drying, and crushing to obtain aminated silicon dioxide with the particle size of 80-100 nm; the volume ratio of the ethyl orthosilicate to the N- (beta-aminoethyl) -gamma-aminopropyltriethoxysilane to the acetone to the N-hexanol is 1:1:5: 20;
step b3, dispersing the aminated silicon dioxide obtained in the step b2 in absolute ethyl alcohol, adding 3-aminopropyltriethoxysilane under stirring at normal temperature, stirring for reaction for 6 hours, centrifuging for 1-3 times, and washing to obtain an aminated silicon dioxide dispersion liquid, wherein the adding amount ratio of the aminated silicon dioxide, the absolute ethyl alcohol and the 3-aminopropyltriethoxysilane is 1g:200mL:2 mL;
step b4, dispersing graphene oxide in ultrapure water, performing ultrasonic treatment for 6-8 hours, centrifuging, and taking supernatant to obtain graphene oxide dispersion liquid, wherein the mass concentration of the graphene oxide dispersion liquid is 0.001 mg/mL; dropwise adding the graphene oxide dispersion liquid into the aminated silicon dioxide dispersion liquid under the stirring of the aminated silicon dioxide dispersion liquid, continuously stirring for 1h with strong force, gradually reducing the stirring speed until the mixture is static, then centrifugally collecting filter residues, and drying to obtain modified silicon dioxide; the volume ratio of the graphene oxide dispersion to the aminated silica dispersion was 1: 2.
4. The sand consolidation agent for the oil field according to claim 3, wherein the outer surface of the modified silica is coated with the ethylene-vinyl acetate copolymer and the water-soluble polymer in sequence from inside to outside.
5. The oilfield sand consolidating agent of claim 4, wherein the curing agent is cyclohexanediamine.
6. The oilfield sand-fixation agent of claim 5, wherein the emulsifier is Tween 80.
7. The preparation method of the sand consolidation agent for the oil field according to any one of the claims 1 to 6, characterized in that, according to the parts by weight, 7 to 10 parts of epoxy resin are dissolved by 20 to 24 parts of acetone to obtain an epoxy resin solution; adding 0.8-1 part of modified silicon dioxide and 3-6 parts of modified epoxy resin into 30-40 parts of acidic aqueous solution, and stirring to obtain modified liquid; heating the epoxy resin solution to 40-50 ℃, stirring, sequentially adding 0.3-0.5 part of emulsifier and modifying solution into the epoxy resin solution, keeping the temperature, stirring, reacting for 2-4 h, stopping heating, and naturally cooling to room temperature to obtain a reaction solution; and dropwise adding 0.5-1 part of curing agent into the reaction liquid under stirring, and continuously stirring for 10-15 min to obtain the high-performance organic silicon/inorganic composite material.
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Application publication date: 20210601 |