KR101776377B1 - Micro capsule for inhibiting produntion of deposites and preparing method of the same - Google Patents
Micro capsule for inhibiting produntion of deposites and preparing method of the same Download PDFInfo
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- KR101776377B1 KR101776377B1 KR1020150046646A KR20150046646A KR101776377B1 KR 101776377 B1 KR101776377 B1 KR 101776377B1 KR 1020150046646 A KR1020150046646 A KR 1020150046646A KR 20150046646 A KR20150046646 A KR 20150046646A KR 101776377 B1 KR101776377 B1 KR 101776377B1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
- B01J13/06—Making microcapsules or microballoons by phase separation
- B01J13/14—Polymerisation; cross-linking
- B01J13/16—Interfacial polymerisation
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/52—Compositions for preventing, limiting or eliminating depositions, e.g. for cleaning
- C09K8/524—Compositions for preventing, limiting or eliminating depositions, e.g. for cleaning organic depositions, e.g. paraffins or asphaltenes
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Abstract
The present invention relates to a microcapsule containing a precipitate formation inhibitor, and more particularly, to a microcapsule in which a precipitate formation inhibitor is selectively discharged under a precipitate production condition and a method for producing the microcapsule.
When the microcapsule of the present invention is used to selectively release the precipitate formation inhibitor selectively only in the transport pipe sediment production condition inside the transport pipe, generation of precipitates in the transport pipe is effectively suppressed by using a small amount of inhibitor when transporting gas or crude oil . In addition, since the microcapsule of the present invention suppresses the formation of precipitates in the gas or crude oil conveying pipe by using a small amount of inhibitor, it is possible to reduce the cost of the additional separation process after the transfer of the crude oil and to reduce the environmental pollution burden by using a small amount of inhibitor .
By using the microcapsule of the present invention, it is possible to increase the inhibition efficiency by preventing cross-contamination among the respective precipitant inhibitors by releasing only one or more kinds of precipitant inhibitors on the respective capsules and releasing them only under the respective precipitate production conditions.
Description
The present invention relates to a microcapsule containing a precipitate formation inhibitor, and more particularly, to a microcapsule in which a precipitate formation inhibitor is selectively discharged under a precipitate production condition and a method for producing the microcapsule.
In the gas or oil production process, when transporting gas or crude oil from the process station to the processing plant through the platform, the sediments, such as wax, hydrate, and asphaltene, inhibit the flow of gas or crude oil in the gas or crude oil pipeline Causing serious problems.
For example, the gas hydrate is a kind of inclusion compound, which is a stable compound in which a gas molecule existing in a natural gas is physically bonded and formed in a cavity formed by water molecules under high pressure and low temperature conditions Crystal. It is known that more than 100 gas molecules form hydrate because the hydrate formers or the gas molecules of the object molecules are trapped in the solid phase lattice of the water molecules which are hydrogen-bonding molecules under the conditions of low temperature and high pressure. Since the above-mentioned gas hydrate is generally formed in an atmosphere of low temperature and high pressure, generation of the gas hydrate is not a serious problem in the atmosphere where the normal temperature and normal pressure are maintained. However, in the case of the deep sea at low temperature and high pressure, or at the production facility of the offshore oil-gas field where high pressure is maintained, the environment where the gas hydrate is generated naturally is formed, and as a result, gas hydrate is generated at an undesired place . In particular, in the case of the oil and gas industry, a pipe pipe for collecting and transporting oil or gas from the deep sea is placed for a long time under a low-temperature and high-pressure environment in the sea, and a low-molecular- The gases react with water and the like to form a solid state gas hydrate. As described above, the gas hydrate formed on the pipe pipe or the like blocks the pipe pipe to obstruct the transfer of the production fluid.
A great deal of effort has been made to suppress the formation of the precipitate in the oil and gas industry, and many inhibitors have been developed, since the once-occurring precipitate takes a lot of cost and time to remove and the work is stopped during the removal of the precipitate . However, existing sediment inhibitors required a large amount of inhibitor because the sediment inhibitor had to be delivered throughout the production line. This method uses an excess of inhibitor, which necessitates an additional separation step in the future, resulting in high costs and environmental problems. In addition, simultaneous infusion of various inhibitors may result in reduced inhibitor efficiency due to cross-contamination between inhibitors. Accordingly, there is a demand for development of a method capable of effectively suppressing the generation of sediments in the conveyance pipe during the transfer of gas or crude oil.
[Prior Patent]
1. Korean Patent No. 10-0263421
2. Korean Patent No. 10-0541753
The present invention provides a microcapsule capable of effectively preventing formation of a precipitate by releasing a precipitate formation inhibitor only in a precipitate producing condition inside a crude oil transportation pipe.
In one aspect,
A core containing a precipitate formation inhibitor; And
Wherein the shell is broken under the condition of producing a precipitate in a transport tube during transport of the capsule along with the gas or crude oil in the transport tube to release the precipitate formation inhibitor, The present invention relates to a microcapsule for inhibiting the formation of a precipitate.
In another aspect,
Forming a droplet using a first fluid comprising a precipitate formation inhibitor as an internal phase, and a second fluid comprising an externally polymerizable polymer monomer; And
And a step of photocuring or thermosetting the droplet. The present invention also relates to a method for producing microcapsules for inhibiting the formation of precipitates.
When the microcapsule of the present invention is used to selectively release the precipitate formation inhibitor selectively only in the transport pipe sediment production condition inside the transport pipe, generation of precipitates in the transport pipe is effectively suppressed by using a small amount of inhibitor when transporting gas or crude oil . In addition, since the microcapsule of the present invention suppresses the formation of precipitates in the gas or crude oil transfer tube by using a small amount of inhibitor, it is possible to reduce the cost of the additional separation process after the transfer of the crude oil and to reduce the environmental pollution burden by using a small amount of inhibitor .
By using the microcapsules of the present invention, one or more precipitant inhibitors can be separately loaded into different capsules and released only under the conditions of each precipitate, thereby preventing mutual contamination between the respective precipitant inhibitors, thereby increasing the inhibition efficiency.
1 is a conceptual diagram showing destruction of a microcapsule of the present invention and a capsule under a condition of producing a precipitate.
2 is a schematic diagram showing the destruction characteristics of microcapsules according to the content of the phase change material.
3 is an optical microscope image of HDDA microcapsules containing PVP.
Figure 4 is an optical microscope image of ETPTA microcapsules containing PVcap.
5 is an image showing destruction of a microcapsule according to temperature and stirring conditions.
FIG. 6 is an optical microscope image showing destruction of microcapsules under agitation under hydrate production conditions. FIG.
7 and 8 are schematic views showing a microfluidic device capable of producing microcapsules.
The present invention relates to a microcapsule which releases a precipitate formation inhibitor under the condition of producing a precipitate in a gas or a crude oil transfer tube. Embodiments of the present invention will be described in detail.
1 is a conceptual diagram showing destruction of a microcapsule of the present invention and a capsule under a condition of producing a precipitate.
1, the microcapsule of the present invention comprises a
The
The precipitate is a substance which precipitates in the transfer pipe during the transfer of gas or crude oil and interferes with the transfer of gas or crude oil. For example, the precipitate may be wax, hydrate or the like, but is not limited thereto.
The wax is a complex consisting of normal paraffin, isoparaffin, and cycloparaffin having 18 to 65 carbon atoms. When the temperature of the oil becomes below the wax production temperature, the kinetic energy of the paraffin particles, which is the main component of the wax, decreases, and the particles are formed as crystals due to the reduction of the intergranular distance. The wax is usually produced at 40 DEG C or lower, but crystals are formed to increase the viscosity of the fluid below about 20 DEG C to interfere with the fluidity of the tube.
Hydrates are produced by physically bonding water molecules and hydrocarbon molecules such as methane, ethane, propane, nitrogen, carbon dioxide and hydrogen sulfide molecules, and are produced under low temperature and high pressure conditions, ie, at pressures of 25 bar or less and 26 bar or less.
The precipitate formation inhibitor can be used without any particular limitation as long as it is commonly used in the art. For example, the hydrate inhibitor may be polyvinylcaprolactam (PVcap) or polyvinylpyrrolidone (PVP), and the wax inhibitor may be polycarboxylate or polyacrylate, but is not limited thereto. The hydrate inhibitor may be contained in the core in a state dissolved or dispersed in ethylene glycol or water, and the wax inhibitor may be contained in the core in a state dissolved or dispersed in an organic solvent.
Depending on the kind of the precipitate formation inhibitor, the
The
The carbon-carbon unsaturated group-containing polymeric monomer may be selected from the group consisting of aryl acrylate, benzyl acrylate, butoxy ethyl acrylate, butoxy triethylene glycol acrylate, cyclohexyl acrylate, dicyclopentyl acrylate, dicyclopentenyl acrylate , 2-ethylhexyl acrylate, glycerol acrylate, glycidyl acrylate, heptadecafluorodecyl acrylate, 2-hydroxyethyl acrylate, isobornyl acrylate, 2-hydroxyethyl methacrylate, 2- Methoxyethyl acrylate, methoxyethylene glycol acrylate, methoxyethylene glycol acrylate, methoxyethylene glycol acrylate, methoxyethylene glycol acrylate, methoxyethylene glycol acrylate, isopropyl methacrylate, Methoxy dipropylene glycol acrylate, octafluorophene Acrylate, phenoxyethyl acrylate, stearyl acrylate, trifluoroethyl acrylate, acrylated cyclohexyl diacrylate, diethylene glycol diacrylate, (tri) ethylene glycol diacrylate, polyethylene glycol diacrylate Acrylate, dipentaerythritol hexaacrylate, dipentaerythritol monohydroxypentaacrylate, ditrimethylol propane tetraacrylate, glycerol diacrylate, methoxylated cyclohexyl diacrylate, neopentyl glycol di Acrylate, pentaerythritol triacrylate, pentaerythritol tetraacrylate, propylene glycol diacrylate, polypropylene glycol diacrylate, triglycerol diacrylate, trimethylolpropane triacrylate, HDDA (1, 6-hexanediol diacrylate), EGPEA (Ethylene glycol phenyl ether acrylate), HDDA (1,6-hexanediol diacrylate), silicone methacrylate monomer (SB4722), ETPTA (ethoxylated trimethylolpropane triacrylate), or a compound containing methacrylate instead of acrylate or γ-methacryloxypropyl trimethylene Butoxysilane, and the like, but is not limited thereto.
Preferably, the polymeric monomer forming the
The
The capsule may be broken by the shear stress of the gas or crude oil due to the increase in the brittleness of the polymer shell due to a decrease in the temperature in the transport pipe to release the inhibitor.
Specifically, when the precipitate is hydrate, the temperature in the transport pipe is 25 ° C or lower, preferably 18 ° C or lower, and the shear stress applied to the shell is 5 Pa or higher, preferably 6 Pa or higher, more preferably 6.7 Pa or higher The polymer shell may be destroyed.
In addition, when the precipitate is wax, the polymer shell may be broken if the temperature in the transport pipe is 40 ° C or lower, preferably 30 ° C or lower, but the present invention is not limited thereto. For example, in the case of crude oil having an API viscosity of about 22, wax may be produced at about 30 degrees or less.
The shell of the
The larger the radius of the polymer shell or the thinner the thickness, the more the embrittlement increases. Therefore, it is necessary to adjust the radius and the thickness of the polymer shell so that the shell is easily broken under the condition of producing the precipitate. If the radius of the polymer shell is too large or the thickness is too small, the capsule may be broken before the capsule is subjected to the conditions for producing the precipitate. Therefore, the radius and thickness of the polymer shell should be adjusted for stabilization of the capsule. For example, the radius and thickness of the ETPTA polymer shell releasing the hydrate formation inhibitor under hydrate formation conditions may be 0.01 <thickness / radius <0.3, more preferably 0.05 <thickness / radius <0.2.
The capsule may further include a phase change material in the
Referring to FIG. 2, referring to FIG. 2, FIG. 2 (a) is a microcapsule in which a phase change material is not contained in a shell. On the other hand, FIG. 2 (b) shows a case where the phase change material is contained in the shell and has a fragile characteristic (brittleness) when the ambient temperature of the microcapsule is below the freezing point of the phase change material. As a result, the present invention can provide a microcapsule that is easily broken by an external impact at a temperature lower than the precipitate production temperature in the gas or petroleum pipeline by using a phase change (liquid to solid) of the phase change material dispersed in the shell. Furthermore, the microcapsule of the present invention can appropriately select a phase change material to break the shell in various kinds of precipitate production temperature ranges, thereby releasing the precipitation inhibitor of the core.
The phase-change material is mixed with a monomer to form a shell. However, during the polymerization of the monomer, the phase-change material is uniformly dispersed in the shell without being affected by polymerization and is retained in its properties. Fine phase separation can occur from the polymer formed.
The phase change material may be any known phase change material without limitation. For example, the phase change material may be oil, paraffinic hydrocarbon or organic solvent.
The phase change material may have a freezing point of 1 to 40 占 폚, and desirably 4 to 30 占 폚.
The paraffinic hydrocarbon may be selected from the group consisting of n-octanoic acid (freezing point 61.4 ° C), n-heptacoic acid (freezing point 59 ° C), n-hexanoic acid (freezing point 56.4 ° C) N-nonadecane (32.1 占 폚), n-nonadecane (32.1 占 폚), n-heptanoic acid (44.9 占 폚) n-hexadecane (18.2 占 폚), n-pentadecane (10 占 폚), n-tetradecane (5.9 占 폚), and n-tridecane (-5.5 DEG C), and is not limited thereto.
The freezing point of the paraffinic hydrocarbon may range from 1 to 40 캜.
The phase change material and the polymer material may be present in a weight ratio of 1: 100, preferably 1: 0.1 to 50.
The microcapsules may contain magnetic nanoparticles in the
In another aspect, the present invention relates to a method of making the microcapsule.
The method for manufacturing a microcapsule of the present invention includes forming droplets using a first fluid and a second fluid, and photocuring or thermally curing the droplet.
The first fluid comprises a precipitate formation inhibitor to form an internal phase. The precipitate may be a substance that interferes with transport in the transport pipe during the transfer of the crude oil or gas, i.e. wax, hydrate, asphaltene or resin.
The second fluid comprises a polymeric monomer to form an outer phase. At this time, the second fluid may contain a surfactant if necessary for interfacial stabilization.
The first fluid and the second fluid are each a material that is not well mixed with each other. For example, when the precipitation inhibitor contained in the first fluid is a wax inhibitor dissolved in a fat-soluble solvent, the polymer contained in the second fluid may be a hydrophilic polymer. In addition, when the sediment formation inhibitor contained in the first fluid is a hydrate inhibitor dissolved in a water-soluble solvent, the polymer contained in the second fluid may be a lipophilic polymer.
The droplets of the present invention can be prepared by various known methods. For example, the droplet can form a double droplet through a microfluidic device or a bulk emulsion production method, but is not limited thereto.
More specifically, referring to Fig. 7, there is shown a microfluidic device used as one device for forming droplets. The microfluidic device includes an
The curing step can be used without particular limitation as long as it is a photo-curing or thermosetting method of curing the polymer monomer with a polymer. For example, the curing step may be performed by irradiating ultraviolet light onto the lipophilic or hydrophilic polymer monomer contained in the droplet formed of w / o / w or o / w / o. More specifically, for example, the ultraviolet ray irradiation may be performed for 0.1 to 10 seconds at a light intensity of 1 to 100 mW / cm 2. In the microfluidic device of FIG. 5, 150) can be used to polymerize the polymer monomer.
As another concrete example, Fig. 8 shows a microfluidic device used as one device for forming droplets. The droplet forming apparatus includes an
The first fluid and the second fluid are separated from each other in the
The curing step can be used without particular limitation as long as it is a photo-curing or thermosetting method of curing the polymer monomer with a polymer. For example, the curing step may be performed by irradiating ultraviolet light onto the lipophilic or hydrophilic polymer monomer contained in the droplet formed of w / o / w or o / w / o. More specifically, for example, the ultraviolet ray irradiation may be performed for 0.1 to 10 seconds at a light intensity of 1 to 100 mW / cm 2. In the microfluidic device of FIG. 5, 250) can be used to polymerize the polymer monomer.
The method of manufacturing the microcapsule may control the thickness of the second fluid, that is, the thickness of the polymer shell in the capsule, by controlling the volume ratio of the first fluid and the second fluid. Increasing the ratio of the second fluid to the first fluid may increase the thickness of the polymer shell of the capsule. The radius of the capsule can be adjusted by adjusting the flow rate of the third fluid relative to the first fluid and the second fluid. Also, the radius of the capsule can be adjusted by adjusting the size of the injection part and the collection part of the device.
The microcapsules formed by curing the liquid droplets may contain a phase change material in the second fluid at the time of manufacturing, and the phase of the phase change material may be changed in accordance with the change of the surrounding temperature of the capsule, Can be changed. More specifically, the phase change material may be converted into a solid phase at a temperature lower than the precipitate formation temperature in the transport tube, thereby increasing the embrittlement of the polymer shell formed upon curing of the droplet.
The phase change material and the polymer material may be present in a weight ratio of 1: 100, preferably 1: 0.1 to 50.
The content of the microcapsule described above with respect to the method for producing the microcapsule of the present invention can be all applied.
Hereinafter, the present invention will be described in more detail with reference to the following examples. However, the following examples are for illustrative purposes only and are not intended to limit the scope of the present invention.
Example 1: Preparation of microcapsules carrying precipitate formation inhibitor
(1) Preparation of HDDA microcapsules containing PVP
Microcapsules were prepared using the apparatus of FIG.
An aqueous phase containing 30wt% of PVP was injected into the injection capillary, the HDDA monomer was injected into the B space, and a continuous phase was formed by injecting 10% PVA in the C space. The droplets falling from the back of the collecting capillary to the collecting solvent were irradiated with UV for 10 seconds to cure the continuously generated droplets. FIG. 3 shows an optical microscope image of the HDDA microcapsules containing PVP.
(2) Preparation of ETPTA microcapsules containing PVcap
Microcapsules were prepared using the apparatus of FIG.
A 1: 1 mixture of ethylene glycol and water containing 50 wt% of PVcap was injected into the injection capillary, ETPTA monomer was injected into the B space, and a continuous phase was formed by injecting 10% PVA-containing water into the C space Respectively. The droplets falling from the back of the collecting capillary to the collecting solvent were irradiated with UV for 10 seconds to cure the continuously generated droplets. FIG. 4 shows an optical microscope image of ETPTA microcapsules containing PVcap.
Example 2 Preparation of Microcapsules in Response to Hydrate Production Conditions and Shear Stress
Microcapsules were prepared using the apparatus of Fig.
Water and red dye were mixed and injected into the injection capillary. ETPTA monomer was injected into the B space and a continuous phase was formed by injecting 10% PVA into the C space. The droplets falling from the back of the collecting capillary to the collecting solvent were irradiated with UV for 10 seconds to cure the continuously generated droplets.
Experimental Example 1: Destruction of microcapsules according to hydrate production condition and shear stress
The microcapsules prepared in Example 2 were dispersed in water and charged into the reactor.
The temperature of the reactor was controlled at 20 ° C., 15 ° C. or 10 ° C. under low temperature conditions in which hydrate was generated and the pressure was changed from 100 rpm (0.46 Pa) to 600 rpm (6.7 Pa) Were observed.
According to FIG. 5, it was observed that the pigment of the microcapsules was ejected at a temperature of 15 DEG C or lower and 600 rpm. The microcapsules did not eject dye at a shear pressure lower than 600 rpm, even though the microcapsule was below 15 ° C, and no dye was ejected at 20 ° C even at 600 rpm. Therefore, it can be confirmed that the polymer film of the microcapsule is broken and the substance contained in the core is released when the hydrate is well-produced at 15 ° C or less and when the shear stress condition is 600 rpm or more.
According to FIG. 6, in the case of stirring at 600 rpm under a low temperature condition in which hydrate is generated, the film of the capsule is broken and all of the pigments carried therein are released.
While the present invention has been particularly shown and described with reference to exemplary embodiments thereof, it is to be understood that the invention is not limited to the disclosed exemplary embodiments.
Claims (17)
A capsule comprising a polymer shell surrounding the core,
The brittleness of the polymer shell is increased under the condition of producing the precipitate in the transport pipe during the transportation of the capsule along with the gas or the crude oil in the transport pipe, the shell is broken to release the precipitate formation inhibitor,
Wherein the capsule further comprises a phase change material in the polymer shell and the phase change material is converted into a solid phase at a temperature below the precipitate formation temperature in the transport tube to increase the embrittlement of the polymer shell, Microcapsules for inhibition.
Forming a droplet by using a first fluid containing a precipitate formation inhibitor due to an internal phase, a polymer externally polymerizable monomer or a second fluid including a mixture of a polymer monomer and a phase-change material, and curing the droplet , ≪ / RTI &
Controlling the thickness of the polymer shell by controlling the volume ratio of the first fluid and the second fluid,
The polymer shell is broken due to increased brittleness,
Wherein the phase change material is converted into a solid phase at a temperature lower than the precipitate formation temperature in the transport tube to increase the brittleness of the polymer shell.
Forming a droplet by using a first fluid containing a precipitate formation inhibitor due to an internal phase, a polymer externally polymerizable monomer or a second fluid including a mixture of a polymer monomer and a phase-change material, and curing the droplet , ≪ / RTI &
The polymer shell, in which the polymer monomer is cured, increases in embrittlement in the condition of producing a precipitate in the transport tube,
Wherein the phase change material is converted into a solid phase at a temperature lower than the precipitate formation temperature in the transport tube to increase the brittleness of the polymer shell.
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KR102655398B1 (en) | 2018-10-01 | 2024-04-05 | 삼성전자주식회사 | Chariging method and apparatus optimized based on electrochemical modeling |
KR102227718B1 (en) * | 2019-07-17 | 2021-03-15 | 한국과학기술원 | Smart microcapsules and method of manufacturing the same |
CN110305636B (en) * | 2019-07-29 | 2021-04-09 | 北京印刷学院 | Magnetic phase change microcapsule and preparation method thereof |
KR20210077109A (en) | 2019-12-16 | 2021-06-25 | 현대자동차주식회사 | A method for manufacturing oilgel capsules and a method for manufacturing contact parts for a vehicle including the oilgel capsules |
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US20040043906A1 (en) * | 2000-06-06 | 2004-03-04 | Heath Stephen Mark | Microcapsule well treatment |
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