CN117510121B - A method for preparing low-density cementing material - Google Patents

A method for preparing low-density cementing material

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CN117510121B
CN117510121B CN202311465630.1A CN202311465630A CN117510121B CN 117510121 B CN117510121 B CN 117510121B CN 202311465630 A CN202311465630 A CN 202311465630A CN 117510121 B CN117510121 B CN 117510121B
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epoxy resin
low
modified epoxy
density
acrylic acid
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CN117510121A (en
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程小伟
王英
高飞
和建勇
张晔
田宝振
张春梅
梅开元
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Southwest Petroleum University
CNPC Bohai Drilling Engineering Co Ltd
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Southwest Petroleum University
CNPC Bohai Drilling Engineering Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B40/00—Processes, in general, for influencing or modifying the properties of mortars, concrete or artificial stone compositions, e.g. their setting or hardening ability
    • C04B40/0028—Aspects relating to the mixing step of the mortar preparation
    • C04B40/0039—Premixtures of ingredients
    • C04B40/0046—Premixtures of ingredients characterised by their processing, e.g. sequence of mixing the ingredients when preparing the premixtures
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B18/00—Use of agglomerated or waste materials or refuse as fillers for mortars, concrete or artificial stone; Treatment of agglomerated or waste materials or refuse, specially adapted to enhance their filling properties in mortars, concrete or artificial stone
    • C04B18/04—Waste materials; Refuse
    • C04B18/18—Waste materials; Refuse organic
    • C04B18/24—Vegetable refuse, e.g. rice husks, maize-ear refuse; Cellulosic materials, e.g. paper, cork
    • C04B18/26—Wood, e.g. sawdust, wood shavings
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B24/00—Use of organic materials as active ingredients for mortars, concrete or artificial stone, e.g. plasticisers
    • C04B24/24—Macromolecular compounds
    • C04B24/28—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • C04B24/281—Polyepoxides
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
    • C04B28/02—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing hydraulic cements other than calcium sulfates
    • C04B28/04—Portland cements
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
    • C08F283/10—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polymers containing more than one epoxy radical per molecule
    • 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
    • C09K8/42—Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells
    • C09K8/426—Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells for plugging
    • 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
    • C09K8/42—Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells
    • C09K8/46—Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells containing inorganic binders, e.g. Portland cement
    • C09K8/467—Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells containing inorganic binders, e.g. Portland cement containing additives for specific purposes
    • C09K8/473—Density reducing additives, e.g. for obtaining foamed cement compositions
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
    • C04B2111/00474—Uses not provided for elsewhere in C04B2111/00
    • C04B2111/00724—Uses not provided for elsewhere in C04B2111/00 in mining operations, e.g. for backfilling; in making tunnels or galleries

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
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  • Polymers & Plastics (AREA)
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  • Environmental & Geological Engineering (AREA)
  • Civil Engineering (AREA)
  • Curing Cements, Concrete, And Artificial Stone (AREA)

Abstract

The invention discloses a preparation method of a low-density material for well cementation, which comprises the steps of S1, ball-milling and crushing bassa wood to obtain bassa wood powder, S2, modifying epoxy resin by using an acrylic acid monomer mixed solution to obtain water-based acrylic acid modified epoxy resin, wherein the monomer mixed solution is prepared by mixing methyl methacrylate, acrylic acid, butyl acrylate and benzoyl tert-butyl peroxide together according to parts by weight, S3, diluting the water-based acrylic acid modified epoxy resin into a water-based acrylic acid modified epoxy resin solution by deionized water, S4, stirring the bassa wood powder and the water-based acrylic acid modified epoxy resin solution to obtain a mixed solution after the bassa wood powder and the water-based acrylic acid modified epoxy resin solution are uniformly mixed, and S5, carrying out spray drying on the mixed solution to obtain the low-density material for well cementation. The invention can ensure that the cement sheath of the stratum which is easy to leak has better integrity, meets the requirement of well cementation construction under complex conditions, has low-cost and easily-obtained raw materials, controllable production process and wide industrialized prospect.

Description

Preparation method of low-density material for well cementation
Technical Field
The invention relates to a low-density material for well cementation, and a preparation method and application thereof, and belongs to the technical field of oil well solid seal cement.
Background
With the rapid development of petroleum industry, the demand of oil well cement for the well cementation engineering of oil and gas wells is continuously increased, and especially the problems of deep well, ultra-deep well, low-pressure easy-to-leak well, easy-to-leak long sealing well sections and the like are also of great concern due to the deepening of well depths and poor geological conditions. The interlayer sealing does not suggest the use of ordinary Portland cement, and the ordinary Portland cement is easy to be brittle destroyed under the action of external force, so that serious oil and gas channeling phenomenon and oil and gas resource waste are caused, and the environment effects such as groundwater pollution, fluid overflowing to the ground surface and the like are caused. Therefore, maintaining the integrity of the underground cement sheath is of great importance in ensuring normal production of oil and gas and prolonging the service life of oil and gas wells.
For the problem that the block with low stratum bearing capacity is difficult to meet the well cementation requirement, low-density cement is often used, the low-density cement can reduce the liquid column pressure, avoid leakage and have positive effects on reducing pollution caused by setting time, meanwhile, the low-density cement can also replace two-stage well cementation operation, long open hole sealing is realized, the problems of leakage and long sealing section are favorably solved, and the method has important significance on reservoir protection.
At present, two methods for preparing low-density cement slurry are provided, namely, hollow glass beads, fly ash, floating beads and the like are added into oil well cement, the cement slurry density is reduced through the lower density of the material, and the method has the advantages of quick response and good density reduction effect, but the hollow glass beads can influence the compressive strength of a cement slurry system at low temperature, and the cost is higher; the fly ash cement slurry has limited preparation density, poor strength and water separation performance, poor floating bead compression resistance and easy crushing under compression, and the actual density is relatively far higher than the ground density. The second is to add a single super absorbent lightweight inorganic admixture such as bentonite, diatomite, expanded perlite and the like into cement to increase the water-solid ratio of the cement slurry system, so as to reduce the density of the cement slurry system to 1.40-1.60 g/cm 3, however, the density of the single admixture low-density system has the lowest limit, such as bentonite cement slurry with the lowest density of 1.6g/cm 3 and diatomite cement slurry with the lowest density of 1.5g/cm 3, and the compressive strength is lower. In addition, the density of the lightening material in the low-density cement paste is greatly different from the density of cement, the cement paste performance cannot be stabilized, the cement particles are settled, the material is lightened to float upwards, the cement paste layering is caused, and the well cementation quality is seriously influenced, so that the settlement stability of the ultra-low-density cement paste is an important performance index.
If the block with lower stratum bearing capacity can not meet the well cementation quality standard, the transformation requirement of the hydrocarbon reservoir and the perforation requirement of the hydrocarbon reservoir section can not be met. The block with low bearing capacity is limited by the restriction, in order to ensure the cement to return to high, a forward injection and reverse extrusion well cementation process is generally adopted, and partial well section empty sections are easy to cause, and the well cementation quality of the low-density section is poor.
The low density cement sheath can generate complex alternating loads during subsequent production processes, causing stress changes in the cement sheath. When the stress is exceeded, cracks and holes form in the interior and surface of the cement sheath, potentially resulting in failure of the integrity of the cement sheath.
At present, a great number of scholars at home and abroad develop a great deal of researches on cement slurry systems with the density of less than 1.40g/m 3, but the problems of low performance, high application cost and poor plugging effect of cement stones are not solved well all the time.
In order to ensure that the cement sheath of the stratum easy to leak has better integrity, save the cost, maximize the economic benefit of exploration and development, and have important significance in researching novel low-density cement materials.
Disclosure of Invention
The invention aims to provide a preparation method of a low-density material for well cementation, which has the advantages of reliable principle, adjustable cement paste thickening time, good integrity of cement rings, low-cost and easily-obtained raw materials, controllable production process and wide industrialized prospect, and the density of cement paste is reduced by adding balsa wood.
In order to achieve the technical purpose, the invention adopts the following technical scheme.
The preparation method of the low-density material for well cementation sequentially comprises the following steps:
s1, ball-milling and crushing the balsa wood to obtain balsa wood powder;
S2, modifying epoxy resin by using an acrylic acid monomer mixed solution to obtain water-based acrylic acid modified epoxy resin, wherein the acrylic acid monomer mixed solution is a monomer mixed solution obtained by mixing methyl methacrylate, acrylic acid, butyl acrylate and benzoyl tert-butyl peroxide according to a certain weight part;
s3, diluting the aqueous acrylic acid modified epoxy resin with deionized water to obtain an aqueous acrylic acid modified epoxy resin solution;
s4, stirring the bazaar powder and the aqueous acrylic acid modified epoxy resin solution to uniformly mix the bazaar powder and the aqueous acrylic acid modified epoxy resin solution to obtain a mixed solution;
And S5, spray drying the mixed solution by a spray dryer to obtain the low-density material for well cementation.
In the above preparation method, in step S1, the average particle size of the bar Sha Mufen is 100-400 mesh, and the density is 0.05-0.15 g/cm 3.
In the above preparation method, in step S2, the preparation process of the aqueous acrylic acid modified epoxy resin is as follows:
1) Mixing 120-200 parts by weight of methyl methacrylate, 10-100 parts by weight of acrylic acid, 120-225 parts by weight of butyl acrylate and 3-15 parts by weight of benzoyl peroxide to obtain a monomer mixed solution;
2) Adding 500-1000 parts by weight of epoxy resin into a reaction bottle, heating to 120-130 ℃, then dripping a monomer mixture into the reaction bottle for 2-3 hours, and then preserving heat for 1-2 hours at 120-130 ℃;
3) Adding 2-5 parts by weight of benzoyl tert-butyl peroxide, keeping the temperature at 120-130 ℃ for 1-2 hours, and then reducing the temperature to 60 ℃ to obtain the aqueous acrylic acid modified epoxy resin.
In the preparation method, in the step S2, the viscosity of the aqueous acrylic acid modified epoxy resin is 200-600 mPa.s, the solid content is 70%, and the pH is 7-10.
In the preparation method, in the step S3, the mass ratio of the deionized water to the aqueous acrylic acid modified epoxy resin is 90-100:4-10.
In the preparation method, in the step S4, the mass ratio of the aqueous acrylic acid modified epoxy resin solution to the bazaar powder is 80-100:40-60, the stirring temperature is normal temperature, and the stirring time is 60-80 min.
In the above preparation method, in step S5, the spray drying conditions are as follows:
The air inlet temperature is 100-120 ℃, the air outlet temperature is 30-40 ℃, and the maximum evaporation water quantity is 1500-2000 mL/h;
The feeding mode is that a peristaltic pump is used for adjusting, and the maximum feeding amount of the peristaltic pump is 500-800 mL/h;
the power of the electric heater is 3.5KW AC220V single-phase grounding;
the fan has the power of 0.4KW, the air flow of 4.5m 3/min and the air pressure of 500Pa;
the power of the air compressor is 0.6KW, and the gas yield is 3.2m 3/h;
the working pressure of the compressed air is 2-5 Bar, and the caliber of the nozzle is 0.75mm.
The low-density material for well cementation prepared by the method also belongs to the protection scope of the invention.
And adding the low-density material into oil well cement to obtain a low-density well cementation cement slurry system with good leakage prevention and long sealing section well cementation.
The addition amount of the low-density material is 5-25% of the mass of the oil well cement.
The oil well cement is G-grade oil well cement or Portland cement, and the G-grade oil well cement or Portland cement are the most commonly used cement in the oil-gas well cementation construction process.
The preparation of the well cementing slurry also needs to add conventional additives and external additives, such as toughening agents, fluid loss agents, defoaming agents, self-healing agents and the like, and is determined according to specific requirements.
The well cementation cement paste added with the low-density material is particularly suitable for well cementation environments with severe requirements on the gas channeling prevention performance and the cement sheath integrity of well cementation cement stones, such as deep wells, ultra-deep wells, low-pressure easily-lost wells and the like, can seal the easily-lost wells for a long time and seal long sealed well sections which are easily lost, and can reduce the occurrence of gas channeling.
Compared with the prior art, the invention has the following beneficial effects:
(1) The low-density material disclosed by the invention adopts the bassa wood as a raw material, the weight is light, the density is small, the density is only 0.05-0.15 g/cm 3, the inside of the bassa wood is of a porous structure, and the water in cement can be absorbed, so that a thickening effect is generated, and the bassa wood is low in price and easy to obtain;
(2) The low-density material adopts the aqueous acrylic epoxy resin as the solvent, has good hydrophilicity and good compatibility with cement paste, can fill micropores of the bassal wood to the maximum extent, reduces the density of the cement paste, and shortens the thickening time to 330min;
(3) The low-density material is dried by adopting a spray dryer, so that the drying speed is high, the dispersibility of the material is good, the drying process is simple and controllable, the material can be better dissolved with cement paste, and the purpose of preventing 'gas channeling' is achieved, so that the cement sheath has better integrity;
(4) The preparation method disclosed by the invention is reliable in technology, high in yield, low in quality requirement on raw materials, high in uniformity, good in chemical stability and strong in hydration capability, and is suitable for large-scale industrial production.
Drawings
Fig. 1 is a cement paste thickening profile of example 1 at 104 ℃ 50mpa 52 min.
Fig. 2 is a plot of cement paste thickening at 104 ℃ 50mpa 52min for example 2.
Fig. 3 is a plot of cement paste thickening at 104 ℃ 50mpa 52min for example 3.
Fig. 4 is a graph of cement paste thickening for a blank group at 104 ℃ 50mpa 52 min.
Detailed Description
The invention is further described below with reference to the drawings and examples to facilitate an understanding of the invention by those skilled in the art. It should be understood that the invention is not limited to the precise embodiments, and that various changes may be effected therein by one of ordinary skill in the art without departing from the spirit or scope of the invention as defined and determined by the appended claims.
The experimental methods used in the following examples are conventional methods unless otherwise specified.
Materials, reagents and the like used in the examples described below are commercially available unless otherwise specified.
Example 1
(1) Crushing the balsa wood, namely selecting the balsa wood with the density of 0.1g/cm 3, ball-milling and crushing the balsa wood by adopting a ball mill, and controlling the particle size to be 200 meshes;
(2) Preparing water-based acrylic acid modified epoxy resin, namely 1) mixing methyl methacrylate, acrylic acid, butyl acrylate and benzoyl tert-butyl peroxide according to parts by weight of 140, 50, 120 and 3 respectively to obtain monomer mixed solution, 2) adding 500 parts by weight of epoxy resin into a reaction bottle, heating to 120 ℃, dripping the monomer mixed solution into the reaction bottle for 2 hours, then preserving the temperature at 120 ℃ for 1 hour, 3) adding 2 parts by weight of benzoyl tert-butyl peroxide, and then preserving the temperature at 120 ℃ for 1 hour and cooling to 60 ℃ to obtain the water-based acrylic acid modified epoxy resin;
(3) Diluting the aqueous acrylic acid modified epoxy resin, namely mixing the aqueous acrylic acid modified epoxy resin with deionized water according to the mass ratio of 4:90, stirring at normal temperature for 60min to obtain an aqueous acrylic acid modified epoxy resin solution, wherein the viscosity of the aqueous acrylic acid modified epoxy resin is 250 mPas, the solid content is 70%, and the pH is 8;
(4) Preparing a mixed solution, namely pouring the bazaar powder into the aqueous acrylic modified epoxy resin solution for uniform mixing, wherein the mass ratio of the bazaar powder to the aqueous acrylic modified epoxy resin solution is 44:80;
(5) And (3) spray drying, namely placing the uniformly mixed balsa wood-water-based acrylic acid modified epoxy resin mixed solution into a spray dryer for drying, so as to obtain the low-density material for well cementation.
The relevant parameters are as follows:
Example 2
(1) Crushing the balsa wood, namely selecting the balsa wood with the density of 0.08g/cm 3, ball-milling and crushing the balsa wood by adopting a ball mill, and controlling the particle size to be 300 meshes;
(2) Preparing water-based acrylic acid modified epoxy resin, namely 1) mixing methyl methacrylate, acrylic acid, butyl acrylate and benzoyl tert-butyl peroxide according to the parts by weight of 200, 10, 180 and 10 respectively to obtain monomer mixed solution, 2) adding 800 parts by weight of epoxy resin into a reaction bottle, heating to 125 ℃, dripping the monomer mixed solution into the reaction bottle for 2.5h, then preserving the temperature at 125 ℃ for 1.5h, 3) adding 3 parts by weight of benzoyl tert-butyl peroxide, preserving the temperature at 125 ℃ for 1h, and then cooling to 60 ℃ to obtain the water-based acrylic acid modified epoxy resin;
(3) Diluting the aqueous acrylic acid modified epoxy resin, namely mixing the aqueous acrylic acid modified epoxy resin with deionized water according to the mass ratio of 6:98 for 70min at normal temperature after the viscosity of the aqueous acrylic acid modified epoxy resin is 500 mPas, the solid content is 70 percent and the pH is 8.5, so as to obtain an aqueous acrylic acid modified epoxy resin solution;
(4) Preparing a mixed solution, namely pouring the baxawood powder into the aqueous acrylic modified epoxy resin solution for uniform mixing, wherein the mass ratio of the baxawood powder to the aqueous acrylic modified epoxy resin solution is 40:90;
(5) And (3) spray drying, namely placing the uniformly mixed balsa wood-water-based acrylic acid modified epoxy resin mixed solution into a spray dryer for drying, so as to obtain the low-density material for well cementation.
The relevant parameters are as follows:
Example 3
(1) Crushing the balsa wood, namely selecting the balsa wood with the density of 0.12g/cm 3, ball-milling and crushing the balsa wood by adopting a ball mill, and controlling the particle size to be 150 meshes;
(2) Preparing water-based acrylic acid modified epoxy resin, namely 1) mixing methyl methacrylate, acrylic acid, butyl acrylate and benzoyl tert-butyl peroxide according to the parts by weight of 160, 30, 225 and 10 respectively to obtain monomer mixed solution, 2) adding 1000 parts by weight of epoxy resin into a reaction bottle, heating to 130 ℃, dripping the monomer mixed solution into the reaction bottle for 3 hours, then preserving the temperature at 125 ℃ for 2 hours, 3) adding 5 parts by weight of benzoyl tert-butyl peroxide, and then preserving the temperature at 130 ℃ for 2 hours and cooling to 60 ℃ to obtain the water-based acrylic acid modified epoxy resin;
(3) Diluting the aqueous acrylic acid modified epoxy resin, namely mixing the aqueous acrylic acid modified epoxy resin with deionized water according to the mass ratio of 8:95 for 80 minutes after the aqueous acrylic acid modified epoxy resin has the viscosity of 400 mPas, the solid content of 70 percent and the pH of 9, and obtaining an aqueous acrylic acid modified epoxy resin solution;
(4) Preparing a mixed solution, namely pouring the bazaar powder into the aqueous acrylic modified epoxy resin solution for uniform mixing, wherein the mass ratio of the bazaar powder to the aqueous acrylic modified epoxy resin solution is 50:95;
(5) And (3) spray drying, namely placing the uniformly mixed balsa wood-water-based acrylic acid modified epoxy resin mixed solution into a spray dryer for drying, so as to obtain the low-density material for well cementation.
The relevant parameters are as follows:
the prepared cement paste is subjected to density, fluidity, compressive strength under the conditions of 92 ℃ for 48 hours, API water loss under the conditions of 104 ℃ for 6.9MPa for 30 minutes and the like to test the basic properties of the cement paste, and the results are shown in table 1.
Table 1 cement paste basic performance test results
Because the well cementation well is deepened, the geological conditions are poor, deep wells, ultra-deep wells, low-pressure easy-to-leak wells and the like are easy to occur, and a cement slurry system is easy to be brittle destroyed under the action of external force, so that serious oil-gas channeling phenomenon is caused. As shown in Table 1, the cement paste density of the cement paste without adding the low-density material is 1.9g/cm 3, the fluidity is 240mm, the compressive strength is 13.6MPa, the API water loss is 50mL, but the cement paste with the low-density material provided by the invention has the density of 1.2g/cm 3、1.4g/cm3、1.6g/cm3, which is obviously reduced compared with the blank cement paste (1.9 g/cm 3) and has adjustable density, the minimum limit density of common low-density materials such as fly ash, slag, bentonite and the like is 1.5g/cm 3, and the floating bead cement paste system has the density of 1.3g/cm 3, but is easy to break and is easily influenced by raw materials, and cannot meet the requirement of long-solid-section well cementation construction. The compressive strength of 48 hours is increased along with the increase of the density, and the fluidity is over 200mm, thereby meeting the construction requirements. The API water loss is less than 50mL under the condition of 104 ℃ and 6.9MPa and 30min, the mud cake is compact, and the permeability is low.
The formulation of the oil well cement paste low density material for preparing the cement paste for well cementation is shown in table 2. In table 2, all percentages are mass percentages with the well cement. The high sulfur-resistant G-grade cement is provided by Jiahua special cement Co-Ltd, and the fluid loss agent FL-33, the expansion agent FE-41, the toughening agent FT-43, the self-healing agent FS-46, the drag reducer GD-1, the anti-settling agent FA-2, the corrosion-resistant and channeling-resistant resin FC-1, the retarder FR-9 and the defoaming agent FR-R are provided by Henan Wei Hui chemical Co-Ltd. Cement slurries and set cements were prepared according to GB/T19139-2012 method for testing oil well cement.
Table 2 oil well cement paste formulation
The thickening curves of examples 1-3 are shown in fig. 1-3, and fig. 4 is a thickening curve without low density material.
According to the analysis results of figures 1-4, it can be known that the thickening experiment is carried out under the condition that the temperature and the pressure are kept stable and the thickening curve has no obvious abnormal phenomenon, the trend is stable and the thickening is at right angles under the condition that the cement paste is not added with low-density materials and the temperature is 50MPa for 52 min. The thickening time of the cement paste added with the low-density material can be shortened to 330min, the thickening time is adjustable, the cement paste has no phenomena of 'flash coagulation' and 'core inclusion', which shows that the cement paste can be filled with micropores to the maximum extent by adding the low-density material, the density of the cement paste is reduced, the 'gas channeling' is effectively prevented, and the integrity of cement rings is ensured.

Claims (10)

1.一种固井用低密度材料的制备方法，依次包括以下步骤：1. A method for preparing a low-density cementing material, comprising the following steps: S1、将巴沙木进行球磨粉碎，得到巴沙木粉体；S1. Balsa wood is ball-milled to obtain balsa wood powder; S2、用丙烯酸单体混合液改性环氧树脂，得到水性丙烯酸改性环氧树脂，所述丙烯酸单体混合液是指将甲基丙烯酸甲酯、丙烯酸、丙烯酸丁酯和过氧化苯甲酰叔丁酯按重量份混合在一起得到的单体混合液；S2. Modify epoxy resin with acrylic monomer mixture to obtain waterborne acrylic modified epoxy resin. The acrylic monomer mixture refers to a monomer mixture obtained by mixing methyl methacrylate, acrylic acid, butyl acrylate and tert-butyl peroxide in parts by weight. S3、将水性丙烯酸改性环氧树脂用去离子水稀释为水性丙烯酸改性环氧树脂溶液；S3. Dilute the waterborne acrylic modified epoxy resin with deionized water to prepare a waterborne acrylic modified epoxy resin solution. S4、将巴沙木粉体与水性丙烯酸改性环氧树脂溶液进行搅拌，使其混合均匀后得到混合溶液；S4. Stir the balsa wood powder and the water-based acrylic modified epoxy resin solution until they are mixed evenly to obtain a mixed solution. S5、将所述混合溶液经过喷雾干燥机喷雾干燥，得到固井用低密度材料。S5. The mixed solution is spray-dried using a spray dryer to obtain a low-density cementing material. 2. 如权利要求1所述的一种固井用低密度材料的制备方法，其特征在于，步骤S1中，所述巴沙木粉体的平均粒径为100~400目，密度为0.05~0.15 g/cm3。2. The method for preparing a low-density cementing material as described in claim 1, characterized in that, in step S1, the average particle size of the balsa wood powder is 100~400 mesh, and the density is 0.05~0.15 g/ cm3 . 3.如权利要求1所述的一种固井用低密度材料的制备方法，其特征在于，步骤S2中，所述水性丙烯酸改性环氧树脂的制备过程如下：3. The method for preparing a low-density cementing material as described in claim 1, characterized in that, in step S2, the preparation process of the water-based acrylic-modified epoxy resin is as follows: 1）将甲基丙烯酸甲酯、丙烯酸、丙烯酸丁酯、过氧化苯甲酰叔丁酯分别按重量份120~200、10~100、120~225、3~15混合，得到单体混合液；1) Methyl methacrylate, acrylic acid, butyl acrylate, and tert-butyl peroxide are mixed in parts by weight of 120-200, 10-100, 120-225, and 3-15, respectively, to obtain a monomer mixture. 2）加入500~1000重量份环氧树脂于反应瓶中，升温至120~130 ℃，再将单体混合液滴入反应瓶中，滴加时间为2~3 h，然后在120~130 ℃保温1~2 h；2) Add 500-1000 parts by weight of epoxy resin to the reaction flask, heat to 120-130 ℃, then drop the monomer mixture into the reaction flask over a period of 2-3 h, and then keep warm at 120-130 ℃ for 1-2 h. 3）补加2~5重量份过氧化苯甲酰叔丁酯，在120~130 ℃保温1~2 h，然后降低温度至60℃，得到水性丙烯酸改性环氧树脂。3) Add 2-5 parts by weight of benzoyl tert-butyl peroxide, keep warm at 120-130 ℃ for 1-2 h, and then lower the temperature to 60 ℃ to obtain waterborne acrylic modified epoxy resin. 4. 如权利要求3所述的一种固井用低密度材料的制备方法，其特征在于，步骤S2中，所述水性丙烯酸改性环氧树脂的粘度为200~600 mPa·s，固含量为70%，pH为7~10。4. The method for preparing a low-density cementing material as described in claim 3, characterized in that, in step S2, the waterborne acrylic modified epoxy resin has a viscosity of 200~600 mPa·s, a solid content of 70%, and a pH of 7~10. 5.如权利要求1所述的一种固井用低密度材料的制备方法，其特征在于，步骤S3中，所述去离子水与水性丙烯酸改性环氧树脂的质量比为90~100：4~10。5. The method for preparing a low-density cementing material as described in claim 1, characterized in that, in step S3, the mass ratio of deionized water to waterborne acrylic modified epoxy resin is 90~100:4~10. 6.如权利要求1所述的一种固井用低密度材料的制备方法，其特征在于，步骤S4中，所述水性丙烯酸改性环氧树脂溶液与巴沙木粉体的质量比为80~100：40~60。6. The method for preparing a low-density cementing material as described in claim 1, characterized in that, in step S4, the mass ratio of the water-based acrylic modified epoxy resin solution to balsa wood powder is 80~100:40~60. 7.如权利要求1—6任意一项所述的制备方法制备的固井用低密度材料的应用，其特征在于，将制备的固井用低密度材料添加至油井水泥中，得到固井水泥浆，适合于深井、超深井或低压易漏失井。7. The application of the low-density cementing material prepared by the preparation method according to any one of claims 1-6, characterized in that the prepared low-density cementing material is added to oil well cement to obtain cementing slurry, which is suitable for deep wells, ultra-deep wells or low-pressure wells prone to leakage. 8. 如权利要求7所述的应用，其特征在于，所述低密度材料的加量为油井水泥质量的5~25 %。8. The application as described in claim 7, wherein the amount of the low-density material added is 5-25% of the mass of the oil well cement. 9.如权利要求7所述的应用，其特征在于，所述油井水泥为G级油井水泥。9. The application as described in claim 7, wherein the oil well cement is grade G oil well cement. 10.如权利要求7所述的应用，其特征在于，固井水泥浆中，还需添加常规外加剂和外掺料，根据具体需要确定。10. The application as described in claim 7, characterized in that conventional admixtures and additives are also required in the cementing slurry, as determined according to specific needs.
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