CN115491183A - Preparation method and application of high-temperature and high-pressure resistant microspheres for actively cooling high-temperature drilling fluid - Google Patents
Preparation method and application of high-temperature and high-pressure resistant microspheres for actively cooling high-temperature drilling fluid Download PDFInfo
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- 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
- C09K8/02—Well-drilling compositions
- C09K8/03—Specific additives for general use in well-drilling compositions
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- C—CHEMISTRY; METALLURGY
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- C09K5/02—Materials undergoing a change of physical state when used
- C09K5/06—Materials undergoing a change of physical state when used the change of state being from liquid to solid or vice versa
- C09K5/063—Materials absorbing or liberating heat during crystallisation; Heat storage materials
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- 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
- C09K8/02—Well-drilling compositions
- C09K8/04—Aqueous well-drilling compositions
- C09K8/14—Clay-containing compositions
- C09K8/18—Clay-containing compositions characterised by the organic compounds
- C09K8/20—Natural organic compounds or derivatives thereof, e.g. polysaccharides or lignin derivatives
- C09K8/206—Derivatives of other natural products, e.g. cellulose, starch, sugars
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract
The invention relates to preparation and application of high-temperature phase change microspheres suitable for a high-temperature drilling fluid system. The phase change core material can generate phase change when the temperature rises, a temperature platform can be generated when the phase change occurs, the temperature of the material is kept unchanged in the phase change process before and after the phase change, and a large amount of phase change heat is transferred to the environment. The phase change temperature of the high-temperature phase change material microsphere can reach 130-150 ℃, the latent heat of phase change can reach 180-240J/g, the particle size distribution of the phase change microsphere is uniform, and D 50 The grain diameter is 22-28 μm. The crushing rate is kept below 5 percent at the temperature of 200-220 ℃ and the pressure of 80-120 MPa; after 500 cycles of phase transition, the phase transition temperature changesThe transformation value is within 2 ℃, and the loss rate of latent heat of phase change is kept below 10%; the heat conducting material has the advantages of good heat conductivity, strong thermal stability, high temperature and high pressure resistance, capability of meeting the circulation requirement of the high-temperature drilling fluid of the ultra-deep well, reusability and better economical efficiency.
Description
Technical Field
The invention relates to a high-temperature water-based drilling fluid used in the field of high-temperature and high-pressure stratum exploration and development, and belongs to high-temperature water-based drilling fluids applied to deep wells and ultra-deep wells.
Background
With the increase of the world energy demand and the development of drilling technology, the oil and gas buried in shallow stratum can not meet the demand, and the finding of oil and gas in deep stratum is inevitable. Most of the petroleum resources in oil fields such as Tarim, quanguor, sichuan basin and the like are buried in deep strata. In this situation, the drilling of deep and ultra-deep wells is inevitably an important development direction in the petroleum industry in China and even all over the world.
In deep wells and ultra-deep wells, the quality of the drilling fluid is the key of success or failure of engineering, high drilling speed and low drilling cost. Compared with the conventional well, the deep well has higher requirements on the used drilling fluid, particularly the high temperature resistance of the drilling fluid, which is the most basic and important performance of the drilling fluid of the deep well. The main slurrying material of water-based drilling fluids is bentonite. Such as sodium bentonite, is used for viscosity increasing, filtration loss reducing and lubricating performance improving. The high-temperature environment can cause clay dispersion and passivation in the drilling fluid and failure of a drilling fluid treating agent, so that the performance of the drilling fluid is deteriorated; and the high temperature environment also has serious negative effects on the well drilling tool and the well logging equipment, the high temperature can reduce the sealing property of the underground tool and seriously shorten the service life of the drilling tool, and the high temperature can also reduce the service life of the equipment while drilling, thereby improving the production cost.
To solve the problem of high temperature drilling, the high temperature drilling fluid is required to have the following characteristics: (1) Good high-temperature stability, high-quality bentonite or other high-quality soil is required, the main chain of the molecule of the treating agent is not easy to degrade at high temperature, the hydrophilic performance of functional groups is strong, and the high-temperature dehydration phenomenon is not easy to occur; (2) low solids, especially low bentonite content; (3) The lubricating property is good, and because the bottom pressure difference of the deep well is large, thick mud cakes are easily formed, so that the probability of drill sticking caused by pressure difference is higher, and the good lubricating property plays an important role in reducing the complexity in the well; (4) The viscosity and the shearing force are proper, and the rock debris carrying capacity is good, so that the well bottom cleaning is ensured; (5) The density adjusting range is wide, so that the density requirements of different well sections can be met.
The passive high-temperature resistant drilling fluid is developed mainly by the following measures: (1) Compared with water-based drilling fluid, the oil-based drilling fluid has the advantages of high temperature resistance, salt calcium resistance, good lubricity, small damage to an oil-gas layer and the like, but the oil-based drilling fluid has great environmental pollution and is not suitable for environment-sensitive areas such as deep water and the like; (2) The method needs a large amount of high temperature resistant additives and has higher cost.
The active drilling fluid cooling technique generally takes the following measures. (1) And naturally cooling, namely, the purpose of cooling the drilling fluid can be achieved to a certain extent by prolonging the circulation route of the drilling fluid groove. The method is generally applied to the situations that the discharge amount of the drilling fluid is not large and the temperature of the returned drilling fluid is not too high. The cooling mode is completely influenced by weather conditions, the effect on deep wells, ultra-deep wells and high-temperature and high-pressure wells is not obvious, and the requirement of safe drilling on the temperature of circulating drilling fluid on natural gas hydrate wells cannot be met. (2) And (3) mixing and cooling the low-temperature medium, putting low-temperature solid (such as ice blocks) or liquid into the drilling fluid pool, and cooling the drilling fluid in a mixed heat conduction mode. This method is generally used for cooling of water-based drilling fluids and is only used as an emergency solution in situations where a low temperature water source is readily available. (3) The cooling device is used for forced cooling, and when the temperature of the returned drilling fluid is too high, a drilling fluid cooling system is used for forced cooling. The working principle of the drilling fluid cooling system mainly comprises 3 modes of air cooling, spraying and interactive heat exchange. However, the external cooling device requires energy input, and has huge energy loss.
Chinese patent document CN108251066B discloses a polyacrylonitrile-coated paraffin nano phase change microcapsule and a preparation method thereof, wherein the microcapsule takes alkane phase change paraffin as a core material and polyacrylonitrile as a shell layer, and is prepared by a dissolving-emulsifying-high temperature spraying method; the phase-change microcapsule has small particle size, high latent heat and good thermal stability, can be subjected to high-temperature heat setting treatment, can effectively adjust the temperature by high latent heat energy, takes high-molecular-weight polyacrylonitrile as a wall material through a dissolving-spraying technology, coats alkane phase-change paraffin to prepare the high-temperature-resistant phase-change microcapsule, does not use an acrylonitrile monomer in the whole process, and has safe and simple process and no monomer pollution. However, the phase-change microcapsules have low compressive strength and are easily broken in a high-temperature and high-pressure environment.
Chinese patent document CN104559967A discloses an ultra-density high-temperature-resistant saturated saline drilling fluid system, which comprises the following components in percentage by mass: 1.5% -4% of sodium bentonite; 8-14% of high temperature resistant sulfonated fluid loss additive; 2% -3% of emulsified asphalt; 2% to 3% of a lubricant; 0.2% -1.5% of pH regulator; 0.2% -1.0% of an emulsifier; 20-30% of inorganic salt; 20-40% of weighting agent; the balance of water. The high temperature resistance of the drilling fluid system is 200 ℃, but the adopted additives such as a high temperature resistant fluid loss agent, a high temperature resistant diluent, a high temperature resistant stabilizer and the like are expensive, the problem of high temperature at the bottom of a well is not solved, and high temperature resistance requirements are still provided for drilling equipment and while-drilling equipment.
Chinese patent document CN1657587A discloses a preparation method of microcapsules, which uses paraffin as a phase-change core material, uses two resins of polystyrene and polyethylene as basic supporting materials, and is mixed and wrapped by a heating melting method, and is cooled and crushed to prepare a paraffin-shaped phase-change material, and then the paraffin-shaped phase-change material is encapsulated by melamine modified urea-formaldehyde resin by an in-situ polymerization method. The phase change temperature of the microcapsule can be adjusted from 0 ℃ to 70 ℃, and the maximum phase change enthalpy value reaches 138kJ/kg. However, the phase change temperature of the microcapsule is too low, the latent heat of phase change is low, and the problem of high temperature at the bottom of a well cannot be effectively solved.
Chinese patent document CN110126385B discloses a high-temperature high-enthalpy phase change material multi-wall structure microcapsule and a preparation method thereof, wherein a shell layer structure comprises three layers, namely a volume expansion buffer layer, an anti-corrosion layer and a high-temperature-resistant strength layer. The material with the thermal decomposition temperature lower than the phase transition temperature of the core material is used as a volume expansion buffer layer, so that the occupied space effect can be achieved in the process of coating the outer shell layer at a low temperature, and the volume expansion caused by the phase transition of the core material is buffered through high-temperature thermal decomposition. The middle layer is an anti-corrosion layer and needs to be coated with a layer of compact anti-corrosion material to prevent the molten phase-change material from leaking and damaging the base material contacted with the molten phase-change material. The outermost layer is a high-temperature resistant strong layer which is required to have certain compactness, heat resistance and strength, so that the capsule is protected in the embedding and using processes of the matrix, and the service life and the thermal stability of the capsule are improved. The microcapsule three-layer structure causes low heat conductivity coefficient and slow heat conduction rate, and influences the heat exchange rate in the well.
Chinese patent document CN109652028A discloses a drilling fluid temperature control method based on a phase change material, and the technical scheme is as follows: the method comprises the following steps: (1) phase change materials for drilling fluids are preferred: selecting a phase change material with a proper phase change temperature according to the bottom temperature, wherein the phase change temperature point is selected to be at a certain point of the circulating temperature of the shaft, the closer the phase change temperature of the phase change material is to the bottom temperature, the better the temperature control effect is, and the latent heat of phase change is more than 160kJ/kg; (2) The phase-change material is preferably used as a drilling fluid treatment agent, the phase-change material with the phase-change temperature of 70-150 ℃ is preferably used for a high-temperature well, the phase-change material adopts crystalline hydrate, molten salt, metal alloy, paraffin, carboxylic acid, ester or polymeric alcohol, and the phase-change material can also adopt a shape-stabilized phase-change material, a microcapsule phase-change material or a composite phase-change material. The invention does not determine phase change wall materials, which can cause the melting and outflow of core materials and cause pollution to drilling fluid and underground environment.
Therefore, on the basis of the current high-temperature drilling research, a new drilling fluid cooling technology needs to be developed to form a new high-temperature drilling technology. The high-temperature drilling fluid system has the performance of reducing the temperature of the drilling fluid, and also needs to consider recycling to reduce the drilling cost and ensure that the subsequent drilling operation is carried out quickly.
With the acceleration of exploration and development of high and deep oil and gas resources in China, high-temperature drilling faces more serious challenges. Although some related researches on cooling of drilling fluid have been developed at present in China, the requirements of drilling operation in high-temperature environment cannot be completely met. Therefore, the active research on the novel high-temperature drilling fluid cooling technology has important significance for developing high and deep oil and gas resources in China.
Disclosure of Invention
Aiming at the defects of the prior art, in particular to overcome the problems of high temperature and high pressure of deep well and ultra-deep well stratum, the invention provides a high-temperature phase-change microsphere, a preparation method thereof and application thereof in drilling fluid cooling.
The invention has the advantages that:
1. the organic polymer phase change material is modified to have higher phase change temperature and phase change latent heat, wherein the phase change temperature is 130-150 ℃, and the phase change latent heat is 180-240J/g.
2. By carrying out high-pressure spraying treatment on the organic polymer phase-change material, the particle size is more uniform, the sphericity is higher, and the organic polymer phase-change material is more favorable for wrapping.
3. By optimizing the emulsifier, the temperature and the polymerization time in the in-situ polymerization method, the phase-change microsphere is more resistant to high temperature and high pressure.
4. The self-assembly deposition mode of the nano silicon dioxide is adopted, the controllable grain diameter of the phase-change microsphere is realized, the formed shell is more compact, and the continuous circulation requirement of the drilling fluid is met.
According to the high-temperature phase-change microsphere prepared by the invention, the phase-change core material of the microsphere is an organic polymer material, and the wall material of the microsphere is silicon dioxide.
The specific preparation scheme of the high-temperature phase change microsphere prepared by the invention is as follows:
(1) Carrying out modification treatment on the organic polymer phase-change core material: heating an organic polymer phase change core material to 132-152 ℃ for melting, adding bis (trimethoxysilylpropyl) amine which accounts for 5-12% of the mass of the organic polymer phase change material after hydrolysis in absolute ethyl alcohol, stirring for reaction for 1-2h, placing the modified organic polymer phase change material in a high-pressure sprayer, adjusting the diameter of a nozzle to be 1mm, adjusting the spraying pressure to be 12-16MPa, screening microsphere core material powder below 100 meshes to obtain the modified organic polymer phase change core material, wherein the particle size of the modified organic polymer phase change core material is 1-30 mu m, the phase change temperature is 130-150 ℃, and the phase change latent heat is 180-240J/g;
(2) Placing the modified organic polymer phase-change material powder into a high-pressure high-temperature reaction kettle, sequentially adding deionized water accounting for 300-450% of the mass percent of the core material and sodium dodecyl benzene sulfonate accounting for 0.2-0.6%, heating to 132-152 ℃ under the condition of stirring speed of 500-800r/min, keeping the pressure at 1.5-2 MPa, and carrying out an emulsion reaction for 1-2 hours;
(3) Sequentially weighing deionized water accounting for 100-200% of the mass percent of the core material, ethyl orthosilicate accounting for 150-240% of the mass percent of the core material and absolute ethyl alcohol accounting for 150-240%, uniformly mixing, adjusting the pH to 9-10, slowly injecting the mixed solution into a high-temperature high-pressure reaction kettle through a high-pressure injection pump, stirring at the dropping speed of 0.2-2 mL/min for 6-8 h, and naturally cooling;
(4) Washing the cooled reaction solution, filtering, drying at 96-98 deg.C to obtain high-temperature phase-change microsphere with phase-change temperature of 130-150 deg.C, latent heat of phase change of 180-240J/g, particle size distribution of 20-50 μm, and density of 900-1200 kg/m 3 In the meantime.
The high-temperature phase change microspheres are characterized in that the high-temperature phase change microspheres are added into water-based drilling fluid, so that the circulating temperature of the water-based drilling fluid can be reduced, the dosage of the high-temperature phase change microspheres is 5-15% of the mass of the water-based drilling fluid, and the reduction value of the circulating temperature of the drilling fluid is 8-18 ℃.
The high-temperature phase-change microspheres are characterized in that the high-temperature phase-change microspheres have small particle sizes, can smoothly pass through a 100-mesh drilling fluid vibrating screen and reenter a drilling fluid circulating pool, can be continuously and repeatedly used without interruption, and meet the requirement of continuous and cyclic use of field drilling fluid.
The high-temperature phase change microspheres are characterized in that the high-temperature phase change microspheres have no adverse effect on the filtration loss and rheological property of the water-based drilling fluid, the high-temperature phase change microspheres can be directly added into a water-based drilling fluid system to be uniformly mixed for use, and can also be directly added into a drilling fluid tank on site to be uniformly stirred and mixed for use, and the use and the mixing are simple and convenient, so that the on-site use is facilitated.
The high-temperature phase-change microspheres can be actively cooled, have stable properties such as sedimentation and filtration loss, and have remarkable effects and advantages when being applied to high-temperature and ultra-high-temperature environments such as deep wells, ultra-deep wells, geothermal wells and the like.
The high-temperature phase change microspheres can be recycled, and the recycling rate is more than or equal to 90%.
The invention has the advantages that:
(1) The high-temperature phase-change constant-temperature microsphere only absorbs heat and releases heat within a small temperature difference range near the phase-change temperature point, and has large phase-change latent heat, the phase-change temperature is between 130 and 150 ℃, and the phase-change latent heat is between 180 and 240J/g, so that the high-temperature drilling fluid can be cooled, and the cooling effect is good.
(2) According to the invention, the paraffin modified composite material is prepared by modifying the high-temperature phase-change microsphere core material, so that the phase-change temperature of the phase-change core material is increased.
(3) According to the invention, the phase change microsphere core material is subjected to high-pressure spraying treatment, so that the obtained phase change core material has the characteristics of good sphericity, finer particles and more uniform particle size distribution, and can better meet the requirement of continuous and cyclic use of field drilling fluid.
(4) The high-temperature phase change material microspheres obtained by means of microsphere wrapping and the like have better recovery rate, and the recovery rate can reach 90%.
(5) The high-temperature drilling fluid based on the high-temperature phase change microspheres absorbs heat when the temperature of the high-temperature drilling fluid rises to be close to the melting point, the drilling fluid automatically releases heat after being circulated out of a shaft, the recycling performance is good, the recovery rate is high, and the drilling cost can be obviously reduced.
Drawings
FIG. 1 is a laser particle size analysis curve of example 5 of the present invention.
FIG. 2 is an electron micrograph of a microstructure of example 5 of the present invention.
FIG. 3 is an infrared spectrum curve of example 5 of the present invention.
Figure 4 is an XRD spectrum of example 5 of the invention.
Fig. 5 is a step profile after a cold-hot cycle of example 5 of the present invention.
Detailed Description
The invention is further described, but not limited to, by the following specific examples in conjunction with the accompanying drawings.
The invention provides a high-temperature phase-change material microsphere and a synthesis method thereof, wherein a phase-change core material adopts an organic polymer phase-change material, and a wall material adopts silicon dioxide.
In the present invention, the formulation of the water-based drilling fluid is not particularly specified, and may be a routine choice for those skilled in the art.
Experimental methods used in the examples: reservoir drilling fluid prepared from the 1 st part of water-based drilling fluid is tested in situ according to the standard GB/T16783.1-2014 drilling fluid, and the performance of a drilling fluid system is tested by referring to the standard GB/T29170-2012 'oil and gas industry drilling fluid laboratory test'.
The "parts" described in the examples and test examples are "parts by mass".
The starting materials used in the examples are all conventional commercial products.
Example 1
This example illustrates phase change microspheres prepared by the method of the present invention.
Weighing 100 parts of organic polymer phase-change material, heating to 130 ℃ for melting, adding 5 parts of bis (trimethoxysilylpropyl) amine hydrolyzed in absolute ethyl alcohol, stirring for reacting for 1h, placing the modified organic polymer phase-change material in a high-pressure sprayer, adjusting the diameter of a nozzle to be 1mm, adjusting the spraying pressure to be 12MPa, and screening microsphere core material powder below 100 meshes to obtain the modified organic polymer phase-change material; placing 100 parts of modified organic polymer phase change material powder in a high-pressure high-temperature reaction kettle, sequentially weighing 300 parts of deionized water and 0.2 part of sodium dodecyl benzene sulfonate, heating to 132 ℃ at a stirring speed of 500r/min, keeping the pressure at 1.5MPa, and carrying out an emulsion reaction for 1 hour; weighing 100 parts of deionized water, 150 parts of ethyl orthosilicate and 150 parts of absolute ethyl alcohol in sequence in a container, uniformly mixing, adjusting the pH to 9, slowly injecting the mixed solution into a high-temperature high-pressure reaction kettle through a high-pressure injection pump, stirring at the dropping speed of 0.2mL/min for 6 hours, and naturally cooling; and washing the cooled reaction solution, performing suction filtration, and drying at 96 ℃ to obtain the high-temperature phase-change microsphere marked as S1.
Example 2
This example illustrates phase change microspheres prepared by the method of the present invention.
Weighing 100 parts of organic polymer phase-change core material, heating to 140 ℃ for melting, adding 7 parts of bis (trimethoxysilylpropyl) amine hydrolyzed in absolute ethyl alcohol, stirring for reacting for 1h, placing the modified organic polymer phase-change material in a high-pressure sprayer, adjusting the diameter of a nozzle to be 1mm, adjusting the spraying pressure to be 13MPa, and screening microsphere core material powder below 100 meshes to obtain the modified organic polymer phase-change material; weighing 100 parts of modified organic polymer phase change material powder, placing the powder in a high-pressure high-temperature reaction kettle, sequentially adding 350 parts of deionized water and 0.3 part of sodium dodecyl benzene sulfonate, heating to 136 ℃ at a stirring speed of 600r/min, keeping the pressure at 1.6MPa, and carrying out an emulsion reaction for 1 hour; weighing 120 parts of deionized water, 180 parts of tetraethoxysilane and 180 parts of absolute ethyl alcohol in a container in sequence, uniformly mixing, adjusting the pH to 9, slowly injecting the mixed solution into a high-temperature high-pressure reaction kettle through a high-pressure injection pump, stirring at the dropping speed of 0.5mL/min for 6 hours, and naturally cooling; and washing the cooled reaction solution, performing suction filtration, and drying at 96 ℃ to obtain the high-temperature phase-change microsphere marked as S2.
Example 3
This example illustrates phase change microspheres prepared by the method of the present invention.
Weighing 100 parts of organic polymer phase-change core material, heating to 140 ℃ for melting, adding 9 parts of bis (trimethoxysilylpropyl) amine hydrolyzed in absolute ethyl alcohol, stirring for reacting for 1h, placing the modified organic polymer phase-change material in a high-pressure sprayer, adjusting the diameter of a nozzle to be 1mm, adjusting the spraying pressure to be 14MPa, and screening microsphere core material powder below 100 meshes to obtain the modified organic polymer phase-change material; weighing 100 parts of modified organic polymer phase change material powder, placing the powder in a high-pressure high-temperature reaction kettle, sequentially adding 400 parts of deionized water and 0.4 part of sodium dodecyl benzene sulfonate, heating to 140 ℃ at a stirring speed of 700r/min, keeping the pressure at 1.7MPa, and carrying out an emulsion reaction for 1 hour; sequentially weighing 140 parts of deionized water, 200 parts of tetraethoxysilane and 200 parts of absolute ethyl alcohol in a container, uniformly mixing, adjusting the pH to 9, then slowly injecting the mixed solution into a high-temperature high-pressure reaction kettle through a high-pressure injection pump for stirring, dropwise adding the mixed solution at the speed of 0.8mL/min for 6 hours, and naturally cooling; and washing the cooled reaction solution, performing suction filtration, and drying at 96 ℃ to obtain the high-temperature phase-change microsphere marked as S3.
Example 4
This example illustrates phase change microspheres prepared by the method of the present invention.
Weighing 100 parts of organic polymer phase-change core material, heating to 140 ℃ for melting, adding 12 parts of bis (trimethoxysilylpropyl) amine hydrolyzed in absolute ethyl alcohol, stirring for reacting for 2 hours, placing the modified organic polymer phase-change material in a high-pressure sprayer, adjusting the diameter of a nozzle to be 1mm, adjusting the spraying pressure to be 15MPa, and screening microsphere core material powder below 100 meshes to obtain the modified organic polymer phase-change material; weighing 100 parts of organic polymer phase change material powder, placing the powder in a high-pressure high-temperature reaction kettle, sequentially adding 450 parts of deionized water and 0.5 part of sodium dodecyl benzene sulfonate, heating to 146 ℃ at a stirring speed of 800r/min, keeping the pressure at 1.8MPa, and carrying out an emulsification reaction for 2 hours; weighing 180 parts of deionized water, 220 parts of tetraethoxysilane and 220 parts of absolute ethyl alcohol in a container in sequence, uniformly mixing, adjusting the pH to 10, slowly injecting the mixed solution into a high-temperature high-pressure reaction kettle through a high-pressure injection pump, stirring at the dropping speed of 1.2mL/min for 7 hours, and naturally cooling; and washing the cooled reaction solution, performing suction filtration, and drying at 98 ℃ to obtain the high-temperature phase-change microsphere marked as S4.
Example 5
This example illustrates phase change microspheres prepared by the method of the present invention.
Weighing 100 parts of organic polymer phase-change core material, heating to 150 ℃ for melting, adding 12 parts of bis (trimethoxysilylpropyl) amine hydrolyzed in absolute ethyl alcohol, stirring for reacting for 2 hours, placing the modified organic polymer phase-change material in a high-pressure sprayer, adjusting the diameter of a nozzle to be 1mm, adjusting the spraying pressure to be 16MPa, and screening microsphere core material powder below 100 meshes to obtain the modified organic polymer phase-change material; weighing 100 parts of modified organic polymer phase change material powder, placing the powder in a high-pressure high-temperature reaction kettle, sequentially adding 450 parts of deionized water and 0.6 part of sodium dodecyl benzene sulfonate, heating to 152 ℃ at a stirring speed of 800r/min, keeping the pressure at 2MPa, and carrying out an emulsification reaction for 2 hours; weighing 200 parts of deionized water, 240 parts of tetraethoxysilane and 240 parts of absolute ethyl alcohol in a container in sequence, uniformly mixing, adjusting the pH to 10, slowly injecting the mixed solution into a high-temperature high-pressure reaction kettle through a high-pressure injection pump for stirring, dropwise adding at the speed of 2mL/min for 8 hours, and naturally cooling; and washing the cooled reaction solution, performing suction filtration, and drying at 98 ℃ to obtain the high-temperature phase-change microsphere marked as S5.
Comparative example 1
High temperature phase change microspheres were prepared in the same manner as in example 5
The difference lies in that: bis (trimethoxysilylpropyl) amine is not added in the preparation process of the high-temperature phase-change microsphere core material.
Weighing 100 parts of organic polymer phase-change core material, heating to 150 ℃ for melting, placing in a high-pressure spraying machine, adjusting the diameter of a nozzle to be 1mm, adjusting the spraying pressure to be 16MPa, and screening microsphere core material powder with the particle size of less than 100 meshes to obtain a modified organic polymer phase-change material; weighing 100 parts of modified organic polymer phase change material powder, placing the powder in a high-pressure high-temperature reaction kettle, sequentially adding 450 parts of deionized water and 0.6 part of sodium dodecyl benzene sulfonate, heating to 152 ℃ at a stirring speed of 800r/min, keeping the pressure at 2MPa, and carrying out an emulsion reaction for 2 hours; sequentially weighing 200 parts of deionized water, 240 parts of tetraethoxysilane and 240 parts of absolute ethyl alcohol in a container, uniformly mixing, adjusting the pH value to 10, then slowly injecting the mixed solution into a high-temperature high-pressure reaction kettle through a high-pressure injection pump for stirring, dropwise adding the mixed solution at the speed of 2mL/min for 8 hours, and naturally cooling; and washing the cooled reaction solution, performing suction filtration, and drying at 98 ℃, thus preparing the high-temperature phase-change microspheres, which are marked as DS1.
Comparative example 2
High temperature phase change microspheres were prepared in the same manner as in example 5
The difference lies in that: and spraying treatment is not carried out in the preparation process of the high-temperature phase-change microsphere core material.
Weighing 100 parts of organic polymer phase-change core material, heating to 150 ℃ for melting, adding 12 parts of bis (trimethoxysilylpropyl) amine hydrolyzed in absolute ethyl alcohol, stirring for reacting for 2 hours, naturally cooling, and grinding into powder to obtain a modified organic polymer phase-change material; weighing 100 parts of modified organic polymer phase change material powder, placing the powder in a high-pressure high-temperature reaction kettle, sequentially adding 450 parts of deionized water and 0.6 part of sodium dodecyl benzene sulfonate, heating to 152 ℃ at a stirring speed of 800r/min, keeping the pressure at 2MPa, and carrying out an emulsion reaction for 2 hours; weighing 200 parts of deionized water, 240 parts of tetraethoxysilane and 240 parts of absolute ethyl alcohol in a container in sequence, uniformly mixing, adjusting the pH to 10, slowly injecting the mixed solution into a high-temperature high-pressure reaction kettle through a high-pressure injection pump for stirring, dropwise adding at the speed of 2mL/min for 8 hours, and naturally cooling; and washing the cooled reaction solution, performing suction filtration, and drying at 98 ℃ to obtain the high-temperature phase-change microsphere, which is marked as DS2.
Comparative example 3
High temperature phase change microspheres were prepared in the same manner as in example 5
The difference lies in that: the pH was controlled to 4 while adding ethyl orthosilicate.
Weighing 100 parts of organic polymer phase-change core material, heating to 150 ℃ for melting, adding 12 parts of bis (trimethoxysilylpropyl) amine hydrolyzed in absolute ethyl alcohol, stirring for reacting for 2 hours, placing the modified organic polymer phase-change material in a high-pressure sprayer, adjusting the diameter of a nozzle to be 1mm, adjusting the spraying pressure to be 16MPa, and screening microsphere core material powder below 100 meshes to obtain the modified organic polymer phase-change material; weighing 100 parts of modified organic polymer phase change material powder, placing the powder in a high-pressure high-temperature reaction kettle, sequentially adding 450 parts of deionized water and 0.6 part of sodium dodecyl benzene sulfonate, heating to 152 ℃ at a stirring speed of 800r/min, keeping the pressure at 2MPa, and carrying out an emulsification reaction for 2 hours; weighing 200 parts of deionized water, 240 parts of tetraethoxysilane and 240 parts of absolute ethyl alcohol in a container in sequence, uniformly mixing, adjusting the pH to 4, slowly injecting the mixed solution into a high-temperature high-pressure reaction kettle through a high-pressure injection pump, stirring at the dropping speed of 2mL/min for 8 hours, and naturally cooling; and washing the cooled reaction solution, performing suction filtration, and drying at 98 ℃ to obtain the high-temperature phase-change microspheres, which are marked as DS3.
Test example 1
The phase transition temperature, the latent heat of phase transition, and the particle diameter of example 1, example 2, example 3, example 4, example 5, comparative example 1, comparative example 2, and comparative example 3 were measured by a METTLER differential scanning calorimeter and a laser particle sizer, respectively, and the results are shown in table 1.
TABLE 1 Performance testing of high temperature phase change microspheres
| High temperature phase change microspheres | Phase transition temperature/. Degree.C | Latent heat of phase change (J/g) | Particle size range/. Mu.m | D 50 Particle size/. Mu.m |
| High temperature phase change microsphere S1 | 132.2 | 185.5 | 1.6-50 | 27.8 |
| High temperature phase change microsphere S2 | 136.3 | 195.7 | 1.7-48 | 26.2 |
| High temperature phase change microsphere S3 | 139.9 | 203.6 | 1.5-44 | 25.6 |
| High temperature phase change microsphere S4 | 144.6 | 221.4 | 1.2-49 | 23.4 |
| High temperature phase change microsphere S5 | 149.1 | 237.3 | 2.1-45 | 22.1 |
| High-temperature phase-change microsphere DS1 | 113.3 | 236.1 | 1.9-51 | 36.9 |
| High temperature phase change microsphere DS2 | 130.4 | 209.2 | 15-147 | 67.1 |
| High-temperature phase-change microsphere DS3 | 131.5 | 199.7 | 1.1-15 | 5.7 |
The experimental result shows that the high-temperature phase change microsphere prepared by the invention has the advantages of better phase change temperature, large latent heat of phase change, more uniform and finer particle size, and is more suitable for cooling high-temperature drilling fluid.
Test example 2
The influence of the addition of the high-temperature phase-change microspheres of example 5 and comparative example 1 with different mass fractions on the circulating temperature of the high-temperature water-based drilling fluid is respectively tested by an indoor drilling simulated circulation experimental device.
The preparation method of the high-temperature water-based drilling fluid comprises the following specific steps: putting 100 parts of water into a stirring container, adding 6 parts of sodium bentonite while stirring, continuing to stir for 25 minutes, stopping stirring, and performing closed maintenance for more than 24 hours to obtain prehydrated bentonite slurry; under the high-speed stirring of 10000 r/min, 0.3 part of Na is added into the prehydrated bentonite slurry according to the proportion 2 CO 3 6 parts of lignite resin filtrate reducer, 3.6 parts of sulfonated lignite and 4 parts of lubricant, stirring each material for 40 minutes, continuing stirring for 75 minutes after all materials are added, and stirring at high speed for 35 minutes to obtain the high-temperature water-based drilling fluid.
The high-temperature water-based drilling fluid is heated and circulated until the circulating temperature of the drilling fluid reaches 180 ℃ and is stable, then the high-temperature phase-change microspheres with different mass fractions are added, the maximum reduction value of the circulating temperature is tested, and the test results are shown in table 2.
Table 2 cooling performance test of high temperature phase change microspheres
| High temperature phase |
5％ | 7％ | 10％ | 12％ | 15％ |
| Maximum cooling value of high-temperature phase-change microsphere S5 | 8.3 | 10.7 | 12.9 | 15.3 | 17.1 |
| Maximum cooling value of high-temperature phase-change microspheres DS1 | 4.1 | 6.9 | 8.7 | 9.8 | 11.3 |
The experimental result shows that the high-temperature phase change microspheres prepared by the invention have the best effect on cooling of the high-temperature water-based drilling fluid and are obviously superior to comparative examples.
Test example 3
The effect of the high temperature phase change microspheres prepared in example 1, example 2, example 3, example 4, example 5, comparative example 1, comparative example 2, and comparative example 3 on the fluid loss performance of the high temperature water-based drilling fluid was tested.
Experimental method of evaluation: putting 100 parts of water into a stirring container, adding 6 parts of sodium bentonite while stirring, continuing to stir for 25 minutes, stopping stirring, and performing closed maintenance for more than 24 hours to obtain prehydrated bentonite slurry; under the high-speed stirring of 10000 r/min, 0.3 part of Na is added into the prehydrated bentonite slurry according to the proportion 2 CO 3 6 parts of lignite resin filtrate reducer, 3.6 parts of sulfonated lignite, 4 parts of lubricant and 10 parts of high-temperature phase change microspheres, wherein each part is high-temperature phase change microsphereThe seed material was stirred for 40 minutes, after all the seed material was added, stirring was continued for 75 minutes, after stirring at high speed for 35 minutes, the fluid loss properties of the drilling fluid were compared by a fluid loss instrument, and the experimental results are shown in table 3.
TABLE 3 testing of the Effect of high temperature phase change microspheres on fluid loss properties of drilling fluids
The experimental result shows that the high-temperature phase change microspheres prepared by the invention have no influence on the filtration performance of the high-temperature water-based drilling fluid, the filtration performance of the high-temperature water-based drilling fluid is slightly improved after the high-temperature phase change microspheres are added, and the filtration loss is slightly reduced. Comparative example 2 has a large influence on the fluid loss properties of the high-temperature water-based drilling fluid due to a large particle size, so that the fluid loss is remarkably increased.
Test example 4
The influence of the high-temperature phase-change microspheres prepared in example 1, example 2, example 3, example 4, example 5, comparative example 1, comparative example 2 and comparative example 3 on the rheological property of the high-temperature water-based drilling fluid is tested.
Experimental method of evaluation: putting 100 parts of water into a stirring container, adding 6 parts of sodium bentonite while stirring, continuing to stir for 25 minutes, stopping stirring, and performing closed maintenance for more than 24 hours to obtain prehydrated bentonite slurry; under the high-speed stirring of 10000 r/min, 0.3 part of Na is added into the prehydrated bentonite slurry according to the proportion 2 CO 3 6 parts of lignite resin filtrate reducer, 3.6 parts of sulfonated lignite, 4 parts of lubricant and 10 parts of high-temperature phase change microspheres, wherein each material is stirred for 40 minutes, the stirring is continued for 75 minutes after all the materials are added, the rheological property change of the drilling fluid is tested by a rotary viscometer after the materials are stirred for 35 minutes at a high speed, and the experimental results are shown in Table 4.
TABLE 4 test of the effect of high-temperature phase-change microspheres on rheological properties of drilling fluids
| Drilling fluid composition | Φ600 | Φ300 | Φ200 | Φ100 | Φ6 | Φ3 | AV | PV |
| High-temperature water-based drilling fluid | 85 | 53 | 38 | 25 | 14 | 7 | 42.5 | 32 |
| S1 | 89 | 55 | 40 | 26 | 15 | 7 | 44.5 | 34 |
| S2 | 90 | 55 | 41 | 27 | 15 | 8 | 45 | 35 |
| S3 | 88 | 54 | 39 | 26 | 15 | 7 | 44 | 34 |
| S4 | 88 | 56 | 40 | 26 | 15 | 7 | 44 | 32 |
| S5 | 91 | 55 | 42 | 26 | 15 | 8 | 45.5 | 36 |
| DS1 | 96 | 58 | 44 | 30 | 17 | 9 | 48 | 38 |
| |
120 | 71 | 51 | 39 | 24 | 14 | 60 | 49 |
| DS3 | 98 | 59 | 47 | 31 | 19 | 11 | 49 | 39 |
The experimental result shows that the high-temperature phase change microspheres prepared by the invention have uniform and smaller particle size and high particle sphericity, and have little influence on the rheological property of the high-temperature water-based drilling fluid. In the comparative example, the particle size is larger, the influence on the rheological property of the drilling fluid is larger, and the apparent viscosity and the plastic viscosity of the drilling fluid are increased. Particularly, the high-temperature phase-change microspheres in the comparative example 2 have large and uneven particle size, greatly affect the rheological property of the high-temperature water-based drilling fluid and have obvious thickening effect.
Test example 5
The high-temperature phase-change microspheres prepared in example 1, example 2, example 3, example 4, example 5, comparative example 1, comparative example 2 and comparative example 3 were tested for their degradation rate of particle size and breakage rate against pressure.
After the high-temperature phase-change microspheres enter the underground environment along with the drilling fluid, when the external force exceeds the compressive strength of the high-temperature phase-change microspheres, the high-temperature phase-change microspheres are crushed by extrusion, so that the leakage of the phase-change core material is caused. And evaluating the compressive strength of the high-temperature phase-change microspheres by taking the compressive grain size degradation rate and the crushing rate of the high-temperature phase-change microspheres as indexes.
Experimental method of evaluation: pressurizing the high-temperature phase-change microspheres by using a high-temperature high-pressure reaction kettle, testing the D90, D50 and D10 particle size degradation rates of the high-temperature phase-change microspheres after stabilizing the pressure for 30min at 220 ℃,80MPa, 100MPa and 120MPa, weighing the screen allowance of the high-temperature phase-change microspheres after being pressurized and passing through a 400-mesh standard screen, and calculating the crushing rate, wherein the experimental results are shown in tables 5, 6 and 7.
TABLE 5 degradation rate and breakage rate of compression-resistant particle size (220 deg.C, 80 MPa) of the high-temperature phase-change microspheres
| Serial number | S1 | S2 | S3 | S4 | S5 | DS1 | DS2 | DS3 |
| D90 degradation Rate/%) | 0.4 | 0.6 | 0.8 | 0.3 | 0.1 | 3.3 | 3.7 | 3.2 |
| D50 degradation rate/%) | 1.5 | 1.7 | 1.8 | 1.3 | 0.5 | 5.3 | 5.9 | 5.8 |
| D10 degradation rate/%) | 2.3 | 2.8 | 2.1 | 2.9 | 0.9 | 8.2 | 8.5 | 8.9 |
| Mass loss rate/%) | 1.1 | 1.3 | 1.2 | 1.1 | 0.3 | 3.5 | 3.1 | 3.3 |
| Fraction of | 1.1 | 1.3 | 1.2 | 1.1 | 0.3 | 3.5 | 3.1 | 3.3 |
TABLE 6 degradation rate and breakage rate of compression-resistant particle size (220 deg.C, 100 MPa) of high-temperature phase-change microspheres
| Serial number | S1 | S2 | S3 | S4 | S5 | DS1 | DS2 | DS3 |
| D90 degradation Rate/%) | 1.2 | 1.6 | 1.8 | 1.3 | 0.6 | 5.3 | 5.7 | 6.2 |
| D50 degradation/% | 2.5 | 2.7 | 2.8 | 2.1 | 1.1 | 7.3 | 7.1 | 7.5 |
| D10 degradation rate/%) | 3.3 | 3.8 | 3.1 | 2.9 | 1.7 | 9.2 | 9.5 | 9.9 |
| Mass loss rate/%) | 2.1 | 2.3 | 2.2 | 2.1 | 0.9 | 4.5 | 4.1 | 4.1 |
| Fraction of | 2.1 | 2.3 | 2.2 | 2.1 | 0.9 | 4.5 | 4.1 | 4.1 |
TABLE 7 degradation rate and breakage rate of compression-resistant particle size (220 deg.C, 120 MPa) of high-temperature phase-change microspheres
| Serial number | S1 | S2 | S3 | S4 | S5 | DS1 | DS2 | DS3 |
| D90 degradation Rate/%) | 2.1 | 2.7 | 2.9 | 2.4 | 1.3 | 7.3 | 7.8 | 7.3 |
| D50 degradation rate/%) | 3.9 | 3.5 | 3.7 | 3.2 | 2.1 | 9.1 | 9.8 | 9.7 |
| D10 degradation rate/%) | 5.1 | 4.8 | 4.5 | 4.6 | 3.3 | 11.2 | 11.5 | 10.9 |
| Mass loss rate/%) | 5.3 | 4.5 | 5.1 | 5.2 | 2.2 | 7.6 | 7.2 | 7.1 |
| Fraction of | 5.3 | 4.5 | 5.1 | 5.2 | 2.2 | 7.6 | 7.2 | 7.1 |
Test example 6
The high-temperature phase-change microspheres prepared in example 1, example 2, example 3, example 4, example 5, comparative example 1, comparative example 2 and comparative example 3 were tested for their degradation rate of particle size and breakage rate against pressure.
After the high-temperature phase-change microspheres enter the underground environment along with the drilling fluid, when the external force exceeds the compressive strength of the high-temperature phase-change microspheres, the high-temperature phase-change microspheres are crushed by extrusion, so that the leakage of the phase-change core material is caused. And evaluating the compressive strength of the high-temperature phase-change microspheres by taking the compressive grain size degradation rate and the crushing rate of the high-temperature phase-change microspheres as indexes.
Experimental method of evaluation: heating the high-temperature phase-change microspheres by using a high-temperature high-pressure reaction kettle, testing the D90, D50 and D10 particle size degradation rates of the high-temperature phase-change microspheres after the high-temperature phase-change microspheres are stabilized for 30min at 200 ℃, 210 ℃, 220 ℃ and 120MPa, weighing the screen allowance of the high-temperature phase-change microspheres after being pressed and passing through a standard screen of 400 meshes, calculating the crushing rate, and showing the experimental results in tables 8, 9 and 10.
TABLE 8 degradation rate and crushing rate (200 deg.C, 120 MPa) of compression-resistant particle size of high-temperature phase-change microspheres
| Serial number | S1 | S2 | S3 | S4 | S5 | DS1 | DS2 | DS3 |
| D90 degradation Rate/%) | 1.8 | 2.4 | 2.6 | 2.1 | 1.0 | 7.0 | 7.5 | 7.0 |
| D50 degradation/% | 3.6 | 3.2 | 3.4 | 2.9 | 1.8 | 8.7 | 9.5 | 9.4 |
| D10 degradation rate/%) | 4.8 | 4.5 | 4.2 | 4.3 | 3.0 | 10.9 | 11.2 | 10.6 |
| Mass loss rate/%) | 5.0 | 4.2 | 4.8 | 4.9 | 1.8 | 7.3 | 6.9 | 6.8 |
| Fraction of | 5.0 | 4.2 | 4.8 | 4.9 | 1.8 | 7.3 | 6.9 | 6.8 |
TABLE 9 degradation rate and breakage rate of compression-resistant particle size (210 deg.C, 120 MPa) of the high-temperature phase-change microspheres
| Serial number | S1 | S2 | S3 | S4 | S5 | DS1 | DS2 | DS3 |
| D90 degradation Rate/%) | 2.0 | 2.5 | 2.8 | 2.2 | 1.1 | 7.2 | 7.7 | 7.1 |
| D50 degradation/% | 3.8 | 3.3 | 3.6 | 3.0 | 2.0 | 8.9 | 9.7 | 9.6 |
| D10 degradation rate/%) | 4.9 | 4.7 | 4.4 | 4.4 | 3.2 | 11.0 | 11.3 | 10.8 |
| Mass loss rate/%) | 5.1 | 4.3 | 5.0 | 5.0 | 2.1 | 7.4 | 7.1 | 6.9 |
| Fraction of | 5.1 | 4.3 | 5.0 | 5.0 | 2.1 | 7.4 | 7.1 | 6.9 |
TABLE 10 degradation rate and breakage rate of compression-resistant particle size (220 deg.C, 120 MPa) of the high-temperature phase-change microspheres
Experimental results show that the high-temperature phase-change microspheres prepared by the invention have smaller grain size degradation rate and breakage rate under high temperature and high pressure, and have high compressive strength.
Test example 7
The high temperature phase change microspheres prepared in example 1, example 2, example 3, example 4, example 5, comparative example 1, comparative example 2, and comparative example 3 were tested for thermal stability.
Putting the phase change microspheres into a high-low temperature alternating box, and setting a high-low temperature circulation program: 1) Heating to 170 deg.C, and maintaining for 25min; 2) Cooling to 120 deg.C, and maintaining for 25min; 3) Heating to 170 deg.C, and maintaining for 25min; after the phase change test is cycled for 500 times, the phase change temperature and the phase change latent heat of the cycled phase change microspheres are tested, and the experimental results are shown in table 11.
TABLE 11 Change in phase transition temperature and latent Heat of phase transition microspheres before and after cycling
| Serial number | S1 | S2 | S3 | S4 | S5 | DS1 | DS2 | DS3 |
| Phase transition temperature/deg.C before cycling | 132.2 | 136.3 | 139.9 | 144.6 | 149.1 | 113.3 | 130.4 | 131.5 |
| Phase transition temperature/. Degree.C.after cycling | 131.1 | 135.3 | 138.5 | 143.3 | 147.9 | 110.1 | 127.2 | 127.9 |
| Rate of change of phase change% | 0.83 | 0.73 | 1.00 | 0.90 | 0.80 | 2.82 | 2.45 | 2.74 |
| Latent heat of phase change/kJ before cycle | 185.5 | 195.7 | 203.6 | 221.4 | 237.3 | 236.1 | 209.2 | 199.7 |
| Latent heat of phase Change/kJ after cycling | 169.3 | 178.3 | 185.9 | 201.9 | 220.8 | 200.9 | 176.7 | 168.8 |
| Rate of loss of latent heat of phase change/%) | 8.73 | 8.89 | 8.69 | 8.81 | 6.95 | 14.9 | 15.5 | 15.5 |
The experimental result shows that after 500 times of cyclic phase change, the phase change temperature value of the high-temperature phase change microsphere prepared by the invention is within 2 ℃, the loss rate of latent heat of phase change is below 10%, the high-temperature phase change microsphere has good thermal stability and reusability, and the reutilization rate is above 90%.
In conclusion, the high-temperature phase-change microspheres prepared by the invention can effectively regulate and control the temperature of the high-temperature water-based drilling fluid. After the high-temperature phase-change microspheres are added into the drilling fluid, the characteristics that the high-temperature phase-change microspheres absorb heat and keep relatively stable temperature in the phase-change process can be utilized, so that the purpose of reducing the circulating temperature of the water-based drilling fluid in a shaft is achieved, a lower working environment is provided for the drilling fluid and downhole tools, and the safety of deep ultra-deep high-temperature and ultra-high-temperature drilling is favorably ensured.
The preferred embodiments of the present invention have been described above in detail, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, many simple modifications can be made to the technical solution of the invention, including combinations of various technical features in any other suitable way, and these simple modifications and combinations should also be regarded as the disclosure of the invention, and all fall within the scope of the invention.
Claims (7)
1. The high-temperature phase-change microsphere is characterized by comprising a core material and a wall material coated on the outer surface of the core material, wherein the core material of the phase-change microsphere is an organic polymer phase-change material, the wall material of the phase-change microsphere is silicon dioxide, and the preparation method of the high-temperature phase-change microsphere comprises the following steps:
(1) Modifying the high-temperature phase change microsphere core material: heating an organic polymer phase change material to 132-152 ℃ for melting, adding bis (trimethoxysilylpropyl) amine which accounts for 5-12% of the content of the phase change core material after hydrolysis in absolute ethyl alcohol, stirring for reaction for 1-2h, placing the modified organic polymer phase change material in a high-pressure sprayer, adjusting the diameter of a nozzle to be 1mm, adjusting the spraying pressure to be 12-16MPa, screening microsphere core material powder below 100 meshes to obtain the modified organic polymer phase change core material, wherein the particle size of the modified organic polymer phase change core material is 1-30 mu m, the phase change temperature is 130-150 ℃, and the phase change latent heat is 180-240J/g;
(2) Placing modified organic polymer phase change material powder into a high-pressure high-temperature reaction kettle, sequentially adding deionized water accounting for 300-450% of the mass percent of the core material and sodium dodecyl benzene sulfonate accounting for 0.2-0.6%, heating to 132-152 ℃ under the condition of stirring speed of 500-800r/min, keeping the pressure at 1.5-2 Mpa, and carrying out emulsion reaction for 1-2 hours;
(3) Sequentially weighing deionized water accounting for 100-200% of the mass percent of the core material, ethyl orthosilicate accounting for 150-240% of the mass percent of the core material and absolute ethyl alcohol accounting for 150-240%, uniformly mixing, adjusting the pH to 9-10, slowly injecting the mixed solution into a high-temperature high-pressure reaction kettle through a high-pressure injection pump, stirring at the dropping speed of 0.2-2 mL/min for 6-8 h, and naturally cooling;
(4) Washing the cooled reaction solution, filtering, drying at 96-98 deg.C to obtain high-temperature phase-change microsphere with phase-change temperature of 130-150 deg.C, latent heat of phase change of 180-240J/g, particle size distribution of 20-50 μm, and density of 900-1200 kg/m 3 In the meantime.
2. The high-temperature phase-change microspheres as claimed in claim 1, wherein the high-temperature phase-change microspheres are added into a water-based drilling fluid, so that the circulating temperature of the water-based drilling fluid can be reduced, the dosage of the high-temperature phase-change microspheres is 5-15% of the mass of the water-based drilling fluid, and the reduction value of the circulating temperature of the drilling fluid is 8-18 ℃.
3. The high-temperature phase-change microsphere of claim 1, wherein the high-temperature phase-change microcapsule has a breakage rate of less than 5% at 200-220 ℃ and 80-120 MPa, and has good pressure resistance and high temperature resistance.
4. The high-temperature phase-change microsphere of claim 1, wherein after 500 cycles of phase change, the phase change temperature of the high-temperature phase-change microcapsule is within 2 ℃, the loss rate of latent heat of phase change is kept below 10%, and the high-temperature phase-change microcapsule has good thermal stability.
5. The high-temperature phase-change microsphere of claim 1, wherein the high-temperature phase-change microsphere has a small and uniform particle size and a high sphericity, can smoothly pass through a 100-mesh drilling fluid vibrating screen and reenter a drilling fluid circulating pool, can be continuously and repeatedly used without interruption, and meets the requirement of continuous and cyclic use of field drilling fluid.
6. The high-temperature phase-change microsphere of claim 1, wherein the high-temperature phase-change microsphere has no adverse effect on the filtration loss and rheological properties of the water-based drilling fluid, the high-temperature phase-change microsphere can be directly added into a water-based drilling fluid system to be uniformly mixed for use, or can be directly added into a drilling fluid tank on site to be uniformly stirred for use, and the use and the mixing are simple and convenient, and the on-site use is convenient.
7. The high-temperature phase-change microsphere of claim 1, which can be recycled, has remarkable effects and advantages when applied to high-temperature and ultra-high-temperature environments such as deep wells, ultra-deep wells, geothermal wells and the like, and has a recycling rate of more than or equal to 90%.
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