CN111253970A - Based on CO2/N2Preparation method of paraffin particles of switch emulsion and application of paraffin particles - Google Patents
Based on CO2/N2Preparation method of paraffin particles of switch emulsion and application of paraffin particles Download PDFInfo
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- SVYKKECYCPFKGB-UHFFFAOYSA-N N,N-dimethylcyclohexylamine Chemical compound CN(C)C1CCCCC1 SVYKKECYCPFKGB-UHFFFAOYSA-N 0.000 claims abstract description 36
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 22
- 229910002092 carbon dioxide Inorganic materials 0.000 claims abstract description 22
- 238000004064 recycling Methods 0.000 claims abstract description 14
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- NWGKJDSIEKMTRX-AAZCQSIUSA-N Sorbitan monooleate Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)OC[C@@H](O)[C@H]1OC[C@H](O)[C@H]1O NWGKJDSIEKMTRX-AAZCQSIUSA-N 0.000 claims description 9
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G73/00—Recovery or refining of mineral waxes, e.g. montan wax
- C10G73/40—Physical treatment of waxes or modified waxes, e.g. granulation, dispersion, emulsion, irradiation
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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
- C09K8/02—Well-drilling compositions
- C09K8/03—Specific additives for general use in well-drilling compositions
- C09K8/035—Organic additives
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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
- C09K8/02—Well-drilling compositions
- C09K8/32—Non-aqueous well-drilling compositions, e.g. oil-based
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Abstract
The invention relates to a catalyst based on CO2/N2A preparation method of paraffin particles of switch emulsion and application of the paraffin particles relate to the technical field of paraffin particles; the preparation method specifically comprises the following steps: s1) preparing an oil phase; s2) preparing a water phase; s3) preparing an O/W emulsion: mixing the oil phase and the water phase, and stirring and emulsifying to obtain O/W emulsion; s4) preparing paraffin particles: introducing carbon dioxide into the O/W emulsion, separating out paraffin particles, and centrifuging to obtain paraffin particles and a protonated solvent; s5) recycling: introducing nitrogen into the protonized solvent to obtain N, N dimethyl cyclohexylamine and an emulsifier aqueous solution, and respectively recovering and reusing the N, N dimethyl cyclohexylamine and the emulsifier aqueous solution; the invention also discloses application of the paraffin particles. The invention discloses a paraffin particle with recyclable solvent and emulsifier aqueous solutionThe preparation method saves raw materials, reduces cost and reduces environmental pollution; also discloses the application of the product in the drilling fluid.
Description
Technical Field
The invention relates to the technical field of paraffin particles, in particular to a catalyst based on CO2/N2A preparation method of paraffin particles of switch emulsion and application of the paraffin particles.
Background
The preparation method of the particles mainly comprises the following steps:
(1) emulsion-chemical cross-linking method. The hydrophilic material can be prepared into particles by an emulsion-chemical crosslinking method, but the prepared particles are porous and have large burst release amount.
(2) Emulsion-heat curing method. Proteins are inactivated at high temperatures. Adding the water solution dissolved with the drug protein into the oil phase for emulsification, then dripping the mixture into the high-temperature oil, stirring, solidifying and separating to obtain the particles.
(3) Drying in liquid. The two immiscible liquids are emulsified by mechanical stirring and the like, the internal phase solvent is volatilized and removed, and the balling material is separated out and solidified into particles.
(4) Spray drying. The albumin is used as material, the medicine is dispersed in the solution of the material, and the mixture is sprayed into hot air flow by a spraying method to dry and solidify liquid drops to obtain the particles.
The emulsion method for preparing the particles has simple process steps and wide application at present, but most of the used emulsions have toxicity and have the harm of organic solvent residue.
In the prior art, the preparation method of the paraffin particles is usually a method of melting, liquefying and then solidifying, although the preparation method is simple, the prepared paraffin particles have large particle size, and micron-sized paraffin particles are difficult to prepare.
Disclosure of Invention
The invention provides a CO-based catalyst for solving the technical problems2/N2Preparation method of paraffin particles of switch emulsion by using CO2/N2Switching solution to prepare a solution of paraffin particlesThe separation is realized, the recycling of the solvent and the emulsifier is realized, the cost is saved, and the production efficiency is improved.
The invention also provides application of the paraffin particles in drilling fluid, and the prepared paraffin particles are prepared into paraffin emulsion and applied to the drilling fluid, so that the plugging performance of the drilling fluid is improved, and the rheological property of mud is improved.
The technical scheme for solving the technical problems is as follows: based on CO2/N2The preparation method of the paraffin particles of the switch emulsion comprises the following steps:
s1) preparing an oil phase: adding paraffin into N, N dimethyl cyclohexylamine, stirring until the paraffin is completely dissolved, then adding an emulsifier A, and stirring until the emulsifier A is completely dissolved to obtain an oil phase;
s2) preparation of the aqueous phase: adding the emulsifier B into deionized water, and stirring until the emulsifier B is completely dissolved to obtain a water phase;
s3) preparing an O/W emulsion: mixing the oil phase and the water phase, and stirring and emulsifying to obtain O/W emulsion;
s4) preparing paraffin particles: introducing carbon dioxide into the O/W emulsion, separating out paraffin particles, and centrifuging to obtain paraffin particles and a protonated solvent;
s5) recycling: and introducing nitrogen into the protonized solvent to obtain N, N dimethyl cyclohexylamine and an emulsifier aqueous solution, and respectively recovering and reusing the N, N dimethyl cyclohexylamine and the emulsifier aqueous solution.
In the above technical scheme, the N, N dimethyl cyclohexylamine and the emulsifier aqueous solution are recycled, and the utilization thereof includes, but is not limited to, the re-application of the N, N dimethyl cyclohexylamine and the emulsifier aqueous solution to the preparation of paraffin particles. When the N, N dimethyl cyclohexylamine and the emulsifier aqueous solution are reused in the paraffin particles, the recycling method comprises the following steps:
adding paraffin into the recovered N, N dimethyl cyclohexylamine, stirring to completely dissolve the paraffin to obtain an oil phase, then adding the oil phase into an emulsifier aqueous solution, stirring, and emulsifying to obtain an O/W emulsion; and continuing to repeat the steps S4) and S5), thus completing the one-time recycling of the N, N dimethylcyclohexylamine and the emulsifier aqueous solution.
Due to the repeated utilization of the N, N dimethyl cyclohexylamine and the emulsifier aqueous solution, the use amount of the N, N dimethyl cyclohexylamine and the emulsifier aqueous solution in the preparation process of the paraffin particles can be reduced, the cost is reduced, and the environmental pollution is reduced; meanwhile, the recycled N, N dimethyl cyclohexylamine and the emulsifier aqueous solution are prepared in proportion and prepared in a water phase, the recycled N, N dimethyl cyclohexylamine and the emulsifier aqueous solution can be directly used for preparing paraffin particles, and workers only need to weigh paraffin raw materials in a proper proportion according to the quality of the recycled N, N dimethyl cyclohexylamine and the emulsifier aqueous solution, so that the production steps are reduced, the production efficiency is improved, and the production raw materials and the production process flow are better saved and simplified.
Further, the emulsifier A is Span-80; the emulsifier B is Tween-80.
Further, the conductivity of the O/W emulsion obtained in the S3) is 0.075-0.1 mS/cm; the conductivity of the system after carbon dioxide is introduced into the S4) is 7.0-8.0 mS/cm; and the conductivity of the system after the nitrogen is introduced into the S5) is 0.12-0.18 mS/cm.
Further, the mass ratio of the emulsifier A to the emulsifier B is 1: 1-3: 2.
Further, the mass ratio of the water phase to the oil phase is 6: 4; the content of paraffin in the O/W emulsion system prepared in the S3) is 8-10%, and the total mass of the emulsifier A and the emulsifier B accounts for 7-9% of the mass of the system.
Further, the introduction rate of carbon dioxide in each liter of O/W emulsion is 120-150 mL/min; the introduction rate of nitrogen in each liter of the protonated solvent is 100-120 mL/min.
The invention also discloses application of the paraffin particles prepared by the preparation method in microemulsion type oil-based drilling fluid.
The specific application method comprises the steps of preparing paraffin particles into paraffin emulsion and adding the paraffin emulsion into the drilling fluid; the paraffin emulsion comprises 8% of emulsifier, 10% of paraffin particles, 49.2% of water and 32.8% of oil according to mass fraction.
Further, the emulsifier is Span-80 and/Tween-80.
Further, the addition amount of the paraffin emulsion in the microemulsion oil-based drilling fluid is 0.8-1.2%.
The invention has the beneficial effects that: (1) the invention discloses a method based on CO2/N2The preparation method of the paraffin particles of the switch emulsion approximately solves the problems of solvent residue and emulsifier waste in paraffin particle production, and the solvent and the emulsifier are repeatedly utilized, so that a method which is more environment-friendly and low in cost is provided for the preparation of the paraffin particles.
(2) The invention discloses a method based on CO2/N2The paraffin particle preparation method of the switch emulsion adopts a method of circulating the solvent and the emulsifier to prepare the paraffin particles, reduces the preparation procedures of the solvent and the emulsifier in the repeated circulation process, shortens the process flow, improves the production efficiency and saves the production labor cost.
(3) The invention discloses a method based on CO2/N2The paraffin particles prepared by the preparation method of the paraffin particles of the switch emulsion are uniform in particle size distribution, and the particle D90 is 8-10 microns.
(4) The invention also discloses application of the paraffin particles in the drilling fluid, and the paraffin particles are applied to the drilling fluid by a method for preparing a paraffin emulsion from the paraffin particles, so that the plugging property of the drilling fluid is improved, the rheological property of mud is improved, the dynamic-plastic ratio of the mud is improved, and the mud is favorable for carrying detritus; meanwhile, the paraffin emulsion is added into the drilling fluid, and can also act synergistically with a filtrate reducer in the drilling fluid to reduce the filtrate loss of mud.
Drawings
FIG. 1 is a schematic illustration of the particle size distribution of paraffin wax particles produced in some examples of the invention;
FIG. 2 is a schematic illustration of the particle size distribution of paraffin particles produced by recycling solvent and emulsifier in some embodiments of the invention;
FIG. 3 is a graph showing the change in conductivity of a gas introduced into a system containing paraffin particles according to some embodiments of the present invention;
FIG. 4 is a physical representation of a filter cake of a paraffin emulsion made from paraffin particles made in accordance with the present invention added to a slurry; wherein 1-no filter cake added with paraffin emulsion; 2-filter cake with 0.5% paraffin emulsion; 3-adding a filter cake of 1% paraffin emulsion; 4-filter cake with 1.5% paraffin emulsion; 5-filter cake with 2% paraffin emulsion; 6-Filter cake with 2.5% wax emulsion added.
Detailed Description
The principles and features of this invention are described below in conjunction with the following drawings, which are set forth by way of illustration only and are not intended to limit the scope of the invention.
In the prior art, most paraffin particles are prepared by liquefying paraffin and then cooling and forming the paraffin particles, the preparation process has high energy consumption and large granularity of the prepared paraffin particles, the granularity requirement of the particles is difficult to meet, and the application of the paraffin in various aspects is limited.
Based on the above technical problems, the inventor provides a CO-based catalyst in the present application2/N2The preparation method of the paraffin particles of the switch emulsion comprises the following steps: s1) preparing an oil phase: adding paraffin into N, N dimethyl cyclohexylamine, stirring until the paraffin is completely dissolved, then adding an emulsifier A, and stirring until the emulsifier A is completely dissolved to obtain an oil phase;
s2) preparation of the aqueous phase: adding the emulsifier B into deionized water, and stirring until the emulsifier B is completely dissolved to obtain a water phase;
s3) preparing an O/W emulsion: mixing the oil phase and the water phase, and stirring and emulsifying to obtain O/W emulsion;
s4) preparing paraffin particles: introducing carbon dioxide into the O/W emulsion, separating out paraffin particles, and centrifuging to obtain paraffin particles and a protonated solvent;
s5) recycling: and introducing nitrogen into the protonized solvent to obtain N, N dimethyl cyclohexylamine and an emulsifier aqueous solution, and respectively recovering and reusing the N, N dimethyl cyclohexylamine and the emulsifier aqueous solution.
It should be noted that in some embodiments, the recycling method of the N, N dimethyl cyclohexylamine and the emulsifier aqueous solution is as follows: adding paraffin into the recovered N, N dimethyl cyclohexylamine, stirring to completely dissolve the paraffin to obtain an oil phase, then adding the oil phase into an emulsifier aqueous solution, stirring, and emulsifying to obtain an O/W emulsion; and continuing to repeat the steps S4) and S5), thus completing the one-time recycling of the N, N dimethylcyclohexylamine and the emulsifier aqueous solution.
In addition, the N, N dimethyl cyclohexylamine and the emulsifier aqueous solution can also be recycled and then used in other production processes or utilization paths.
In the preparation method, before the carbon dioxide is introduced, the O/W emulsion is uniform milky white, after the carbon dioxide is introduced, the O/W emulsion is layered, the upper layer is a white substance, and the lower layer is turbid liquid, because the N, N dimethyl cyclohexylamine serving as a paraffin solvent is protonated and dissolved in water after the carbon dioxide is introduced, and paraffin is insoluble in water and is separated out in the O/W emulsion; because the paraffin particles are generated by directly separating out from the solution, the particle size of the generated particles is smaller, and the physical property of separation is mild and uniform, the particle size of the generated paraffin particles is very uniform, the appearance is smooth, and the application of the paraffin particles is very favorable. After paraffin particles are separated out and separated and filtered, nitrogen is introduced into the system to deprotonate protonated N, N dimethyl cyclohexylamine, the N, N dimethyl cyclohexylamine is separated from the water phase, the upper layer liquid and the lower layer liquid are separated, the recovery of the N, N dimethyl cyclohexylamine and the emulsifier aqueous solution can be completed, and the N, N dimethyl cyclohexylamine and the emulsifier aqueous solution can be reused in the preparation of the paraffin particles or other production processes and utilization ways.
In some embodiments, the emulsifier a is Span-80; the emulsifier B is Tween-80. The emulsifier A and the emulsifier B can also be selected from other emulsifiers, such as Span-60 or Tween-20; but is preferably Span-80 and Tween-80.
In some embodiments, the conductivity of the O/W emulsion obtained in S3) is 0.075-0.1 mS/cm; the conductivity of the system after carbon dioxide is introduced into the S4) is 7.0-8.0 mS/cm; and the conductivity of the system after the nitrogen is introduced into the S5) is 0.12-0.18 mS/cm.
In some embodiments, the mass ratio of the emulsifier A to the emulsifier B is 1: 1-3: 2, wherein the mass ratio is preferably: the mass ratio of the emulsifier A to the emulsifier B is 3: 2.
In some embodiments, the mass ratio of the aqueous phase to the oil phase is 6: 4; the content of paraffin in the O/W emulsion system prepared in the S3) is 8-10%, and the total mass of the emulsifier A and the emulsifier B accounts for 7-9% of the mass of the system. Preferably, the content of paraffin in the O/W emulsion system prepared in S3) is 10%, and the total mass of the emulsifier A and the emulsifier B accounts for 8% of the mass of the system.
The present application is described in the following by some specific preparation examples, and the products prepared by the method are characterized by detection.
Example 1
S1) completely dissolving 12.5g of paraffin into 37.5g of N, N dimethyl cyclohexylamine, then adding 2.208g of Span-80, and stirring until the Span80 is completely dissolved to form an oil phase;
s2) dissolving 1.472g of Tween-80 in deionized water to form an aqueous phase;
s3) under the stirring condition, slowly adding the oil phase into the water phase to ensure that the concentration of the emulsifier A + the emulsifier B is 8 percent, and forming O/W emulsion;
s4) introducing CO into the emulsion2Dissolving N, N dimethyl cyclohexylamine serving as a solvent in water, and centrifuging to obtain paraffin particles;
s5) introducing N into the supernatant after centrifugation2And separating the supernatant into a solvent and an emulsifier aqueous solution, separating the solvent and the emulsifier aqueous solution by using a separating funnel, and continuously putting the separated solvent and emulsifier aqueous solution into recycling.
And (3) recycling:
the solvent and the emulsifier aqueous solution obtained after the first preparation are continuously and repeatedly used for preparing the paraffin particles, and the preparation method comprises the following steps: adding paraffin into the recovered N, N dimethyl cyclohexylamine, stirring to completely dissolve the paraffin to obtain an oil phase, then adding the oil phase into an emulsifier aqueous solution, stirring, and emulsifying to obtain an O/W emulsion; continuing to repeat the steps S4) and S5), namely completing the one-time recycling of the N, N dimethylcyclohexylamine and the emulsifier aqueous solution;
the above cycle is repeated at least twice.
Detecting the particle size of the paraffin particles prepared for multiple times by adopting a laser light scattering instrument, wherein the result of detecting the particle size of the paraffin particles prepared for the first time is shown in figure 1; the particle size detection pair of the paraffin particles prepared for the first time and the paraffin particles prepared by recycling the solvent and emulsifier aqueous solution is shown in fig. 2.
During the preparation process, the detection is performed every 5minMeasuring the conductivity of the primary system to obtain a conductivity curve as shown in fig. 3, wherein the conductivity change trend of the system in the three preparation processes is unchanged from the conductivity change of the system in the first preparation and twice circulating preparation processes of the paraffin particles, and the conductivity of the system rapidly rises after carbon dioxide is introduced; the conductivity of the system rapidly decreases after the nitrogen is introduced and approaches the conductivity value of the W/O emulsion before returning to the first preparation system, and the fact that the emulsion system can pass through CO is also proved2/N2Realizing the repeated use of the N, N dimethyl cyclohexylamine and the emulsifier aqueous solution.
As can be seen from fig. 1 and 2, the first-prepared paraffin particles have an average particle size of 8814.48 nm; and the average particle diameters of the paraffin particles obtained by two times of circulation are 8932.64nm and 9017.29nm, which shows that the solvent and the emulsifier aqueous solution which are recycled and used can be reused for preparing the paraffin particles, and the particle diameters of the prepared paraffin particles are not changed greatly, thus proving that the N, N dimethyl cyclohexylamine and the emulsifier aqueous solution can be recycled.
Comparative example:
the first group of comparative examples was prepared at emulsifier concentrations of 2%, 4%, 6%, 10%, and the other preparation methods were substantially the same as example 1; the mass ratio of the emulsifier A to the emulsifier B is 5:5, 4:6, 3:7 and 2:8, and the other preparation implementation methods are basically the same as the examples; the third group of comparative examples were prepared by adding 15%, 20%, 25%, 30% of paraffin wax, and the other preparation methods were substantially the same as those of example 1; the fourth group of comparative examples were prepared by using the water phase and the oil phase at mass ratios of 5:5, 4:6, 3:7, and 2:8, and the other preparation methods were substantially the same as those of the examples, and orthogonal experiments were performed, and the experimental results are shown in table 1.
As can be seen from table 1: the uniform paraffin particles can be prepared by adopting other emulsifier contents, the mass ratio of the emulsifier A to the emulsifier B, the water-oil ratio and the mass fraction of the added paraffin, but the average particle size of the paraffin particles prepared by adopting the comparative example is more than 9 mu m, while the average particle size of the paraffin particles prepared by adopting the example is less than 9 mu m, which shows that the preparation of the paraffin particles by adopting the mixture ratio of the components in the example 1 is the optimal preparation condition.
The application document also discloses application of the paraffin particles prepared by the preparation method in microemulsion type oil-based drilling fluid.
The specific application method comprises the steps of preparing paraffin particles into paraffin emulsion and adding the paraffin emulsion into the drilling fluid; the paraffin emulsion comprises 8% of emulsifier, 10% of paraffin particles, 49.2% of water and 32.8% of oil according to mass fraction.
In some embodiments, the emulsifier is Span-80 and/Tween-80.
In some embodiments, the paraffin emulsion is added in the microemulsion-type oil-based drilling fluid in an amount of 0.8-1.2%.
The paraffin particles prepared in the above example 1 are prepared into a paraffin emulsion by the above application method, and added into a common commercially available microemulsion oil-based drilling fluid, and the influence of the paraffin emulsion on the plugging performance of the microemulsion oil-based drilling fluid is evaluated by an artificial filter cake, and the experimental results are shown in table 2:
TABLE 2
As can be seen from Table 2, the drilling fluid added with the paraffin emulsion has better plugging performance, when the addition amount of the paraffin emulsion is 0.5%, the mud cake permeability is reduced by 50.4%, and the plugging effect is better along with the increase of the dosage of the emulsion. The paraffin emulsion plays a certain plugging effect in the drilling fluid.
The paraffin wax particles prepared in the example 1 are prepared into paraffin wax emulsion by the application method, the paraffin wax emulsion is added into slurry, the slurry is stirred for 5min at a stirring speed of 6000r/min, the apparent viscosity, the plastic viscosity and the dynamic shear force of the slurry are detected, the influence of the slurry on the rheological property of the slurry is evaluated, and the detection result is shown in table 3.
TABLE 3
As can be seen from Table 3, the apparent viscosity, plastic viscosity and dynamic shear force of the slurry show a tendency of increasing with the increase of the paraffin emulsion in the slurry, but the rheological property of the slurry is not changed greatly when the dosage of the plugging agent is within 1%, and the influence is small. After the paraffin emulsion is added, the dynamic-plastic ratio is improved, and the carrying of rock debris is facilitated.
The paraffin wax particles prepared in the example 1 are prepared into paraffin wax emulsion by the application method, the paraffin wax emulsion is added into the slurry added with the fluid loss additive, the slurry is stirred and mixed evenly, the fluid loss of the slurry is measured by a medium-pressure slurry fluid loss instrument, the experimental result is shown in figure 4, the test result is shown in table 4,
TABLE 4
As shown in Table 4, the fluid loss of the mud is reduced with the increase of the paraffin emulsion in the mud, and the fact that the paraffin particles are added into the drilling fluid as a plugging agent and have a synergistic effect with a fluid loss reducer to reduce the fluid loss of the mud together is proved. As shown in fig. 4, the density and thickness of the filter cake was not much different from the blank cake.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (10)
1. Based on CO2/N2Stone for switching emulsionsThe preparation method of the wax particles is characterized by comprising the following steps:
s1) preparing an oil phase: adding paraffin into N, N dimethyl cyclohexylamine, stirring until the paraffin is completely dissolved, then adding an emulsifier A, and stirring until the emulsifier A is completely dissolved to obtain an oil phase;
s2) preparation of the aqueous phase: adding the emulsifier B into deionized water, and stirring until the emulsifier B is completely dissolved to obtain a water phase;
s3) preparing an O/W emulsion: mixing the oil phase and the water phase, and stirring and emulsifying to obtain O/W emulsion;
s4) preparing paraffin particles: introducing carbon dioxide into the O/W emulsion, separating out paraffin particles, and centrifuging to obtain paraffin particles and a protonated solvent;
s5) recycling: and introducing nitrogen into the protonized solvent to obtain N, N dimethyl cyclohexylamine and an emulsifier aqueous solution, and respectively recovering and reusing the N, N dimethyl cyclohexylamine and the emulsifier aqueous solution.
2. CO-based according to claim 12/N2The preparation method of the paraffin particles of the switch emulsion is characterized in that the emulsifier A is Span-80; the emulsifier B is Tween-80.
3. CO-based according to claim 12/N2The preparation method of the paraffin particles of the switch emulsion is characterized in that the conductivity of the O/W emulsion obtained in S3) is 0.075-0.1 mS/cm; the conductivity of the system after carbon dioxide is introduced into the S4) is 7.0-8.0 mS/cm; and the conductivity of the system after the nitrogen is introduced into the S5) is 0.12-0.18 mS/cm.
4. CO-based according to claim 12/N2The preparation method of the paraffin particles of the switch emulsion is characterized in that the mass ratio of the emulsifier A to the emulsifier B is 1: 1-3: 2.
5. CO-based according to any one of claims 1 to 42/N2Process for the preparation of paraffin particles for switch emulsions, characterized in that the aqueous and oily phases areThe mass ratio of (A) to (B) is 6: 4; the content of paraffin in the O/W emulsion system prepared in the S3) is 8-10%, and the total mass of the emulsifier A and the emulsifier B accounts for 7-9% of the mass of the system.
6. CO-based according to any one of claims 1 to 42/N2The preparation method of the paraffin particles for switching on and off the emulsion is characterized in that the carbon dioxide introducing speed in each liter of O/W emulsion is 120-150 mL-
min; the introduction rate of nitrogen in each liter of the protonated solvent is 100-120 mL/min.
7. The application of the paraffin particles prepared by the preparation method of any one of claims 1 to 6 in microemulsion type oil-based drilling fluid.
8. The use of claim 7, wherein the paraffin particles are formulated as a paraffin emulsion for addition to a drilling fluid; the paraffin emulsion comprises 8% of emulsifier, 10% of paraffin particles, 49.2% of water and 32.8% of oil according to mass fraction.
9. The use according to claim 8, wherein the emulsifier is Span-80 and/or Tween-80.
10. The use according to claim 8 or 9, wherein the paraffin emulsion is added in the microemulsion-type oil-based drilling fluid in an amount of 0.8-1.2%.
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