CN111690430A - Carbon microsphere/nano SiO2Composite demulsifier and preparation method and application thereof - Google Patents
Carbon microsphere/nano SiO2Composite demulsifier and preparation method and application thereof Download PDFInfo
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- 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
- C10G33/00—Dewatering or demulsification of hydrocarbon oils
- C10G33/04—Dewatering or demulsification of hydrocarbon oils with chemical means
Abstract
The invention discloses a carbon microsphere/nano SiO2The preparation method of the composite demulsifier comprises the following steps: uniformly mixing a glucose solution and tetraethyl orthosilicate to obtain a mixed solution; carrying out hydrothermal reaction on the mixed solution to obtain carbon microspheres/nano SiO2Compounding a demulsifier precursor, wherein the hydrothermal reaction temperature is 140-180 ℃, and the reaction time is 8-20 h; mixing the carbon microsphere/nano SiO2Annealing the composite demulsifier precursor under the protection of inert gas to obtain the carbon microsphere/nano SiO2The composite demulsifier has the annealing temperature of 300-500 ℃ and the annealing time of 1-3 h. The preparation method is simple, low in cost, green and pollution-free, and the demulsifier has high demulsification efficiency, good effect and wide application range. The invention also discloses the carbon microsphere/nano SiO prepared by the preparation method2A composite demulsifier and an application thereof in a W/O crude oil emulsion.
Description
Technical Field
The invention belongs to the technical field of oilfield chemicals, and particularly relates to carbon microspheres/nano SiO2A composite demulsifier, a preparation method and application thereof.
Background
Natural emulsifiers are present in crude oil, while water injection recovery introduces large amounts of water, thus resulting in stable crude oil emulsions, mainly in the form of W/O emulsions and O/W emulsions. The emulsions bring great difficulty to links such as transportation, processing and the like, and can cause damages such as pipeline blockage, equipment corrosion and the like. Therefore, the demulsification of the crude oil and the complete separation of oil and water have very important significance.
Common demulsification methods include heating, membrane filtration, high-speed centrifugation, gravity separation, chemical and electrochemical demulsification, and the like. The chemical demulsification has the advantages of high activity, quick response and the like, so that the chemical demulsification is widely applied to the demulsification of the crude oil and has good development prospect. In recent years, organic polymers are mostly adopted as crude oil demulsifiers, and the main focus is on modifying the traditional demulsifiers by methods such as 'head changing, tail changing, chain extending, grafting, crosslinking and compounding' to meet new requirements of the demulsifiers. Although the demulsifier and the modification method can improve the demulsification efficiency, the problems of excessive reaction components, complex preparation process, expensive raw materials and the like still exist, and the demulsifier can stay in a water phase or an oil phase after demulsification, thereby causing environmental pollution. In addition, although the chemical demulsifier has a high demulsification rate, the chemical demulsifier is harsh to the application environment and is mostly neutral or alkaline.
Therefore, it is necessary to develop a crude oil demulsifier having a simple preparation method, excellent performance and a wide application range.
Disclosure of Invention
The present invention is to overcome the above technical disadvantages, and the first aspect of the present invention is to provide a carbon microsphere/nano SiO2The preparation method of the composite demulsifier is simple, green, pollution-free and low in cost; the second aspect of the invention aims to provide a preparation method for the compoundCarbon microsphere/nano SiO2The composite demulsifier has high demulsification efficiency, good effect and wide application range; the third aspect of the invention aims to provide the carbon microsphere/nano SiO2Application of the composite demulsifier in W/O crude oil emulsion.
In order to achieve the technical purpose, the technical scheme of the invention provides a carbon microsphere/nano SiO2The preparation method of the composite demulsifier comprises the following steps: uniformly mixing a glucose solution and tetraethyl orthosilicate to obtain a mixed solution; carrying out hydrothermal reaction on the mixed solution to obtain carbon microspheres/nano SiO2Compounding a demulsifier precursor, wherein the hydrothermal reaction temperature is 140-180 ℃, and the reaction time is 8-20 h; mixing the carbon microsphere/nano SiO2Annealing the composite demulsifier precursor under the protection of inert gas to obtain the carbon microsphere/nano SiO2The composite demulsifier has the annealing temperature of 300-500 ℃ and the annealing time of 1-3 h.
The technical scheme of the invention also provides the carbon microsphere/nano SiO prepared by the preparation method2A composite demulsifier.
The technical scheme of the invention also provides the carbon microsphere/nano SiO prepared by the preparation method2Application of the composite demulsifier in W/O crude oil emulsion.
Compared with the prior art, the invention has the beneficial effects that:
1. the preparation method provided by the invention carries out in-situ polymerization on glucose and tetraethyl orthosilicate under hydrothermal reaction, namely, in the process of generating carbon microspheres, nano SiO2Grafting to the surface of carbon microsphere to obtain carbon microsphere/nano SiO2Compounding demulsifier precursor, and mixing carbon microsphere/nano SiO2Annealing the composite demulsifier precursor to improve the defect structure of the composite material and reduce partial hydroxyl on the surface of the composite material to make the carbon microsphere/nano SiO2The composite demulsifier has the best hydrophilic and oleophilic properties, so that the demulsifier with high demulsification efficiency and good effect is prepared;
2. the preparation method provided by the invention has the advantages of easily available raw materials, low cost, simple preparation method, no generation of toxic and harmful substances in the preparation process, greenness and no pollution;
3. the carbon microsphere/nano SiO prepared by the preparation method of the invention2The composite demulsifier has high demulsification efficiency, wide application range, high salt tolerance, good demulsification effect on W/O crude oil emulsion, clear separated water phase and no wall-hanging phenomenon, and can be suitable for acid, neutral and alkaline environments; the carbon microsphere/nano SiO2The composite demulsifier does not generate other toxic and side effects in the use process, has the characteristic of environmental protection and no pollution, and is an environment-friendly demulsifier.
Drawings
FIG. 1 is a schematic diagram of the preparation of carbon microsphere/nano SiO2A process flow diagram of the composite demulsifier;
FIG. 2 is a schematic representation of the carbon microsphere/nano SiO solid composition of example 12A Scanning Electron Microscopy (SEM) image of the composite demulsifier;
FIG. 3 is a schematic representation of the carbon microsphere/nano SiO solid composition of example 12X-ray energy spectrum analysis (EDS) profile of the complex demulsifier;
FIG. 4 shows a schematic diagram of a carbon microsphere and nano SiO2And example 1 carbon microsphere/nano SiO2Fourier transform infrared spectroscopy contrast (FT-IR) of the composite demulsifier;
FIG. 5 shows a schematic diagram of a carbon microsphere and nano SiO2And example 1 carbon microsphere/nano SiO2Three-phase contact angle diagram of the composite demulsifier.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
FIG. 1 is a schematic diagram of a process for preparing carbon microspheres/nano SiO according to an embodiment of the present invention2The process flow diagram of the composite demulsifier is shown in figure 1, and the embodiment of the invention provides a carbon microsphere/nano SiO2The preparation method of the composite demulsifier comprises the following steps:
mixing fructus Vitis ViniferaeUniformly mixing the sugar solution and tetraethyl orthosilicate to obtain a mixed solution; carrying out hydrothermal reaction on the mixed solution to obtain carbon microspheres/nano SiO2Compounding a demulsifier precursor, wherein the hydrothermal reaction temperature is 140-180 ℃, and the reaction time is 8-20 h; mixing carbon microsphere/nano SiO2Annealing the composite demulsifier precursor under the protection of inert gas to obtain the carbon microsphere/nano SiO2The composite demulsifier has the annealing temperature of 300-500 ℃ and the annealing time of 1-3 h.
The embodiment of the invention provides carbon microspheres/nano SiO2The preparation method of the composite demulsifier comprises the step of carrying out in-situ polymerization on glucose and tetraethyl orthosilicate under the hydrothermal reaction, namely, in the process of generating carbon microspheres, nano SiO2Grafting to the surface of carbon microsphere to obtain carbon microsphere/nano SiO2Compounding demulsifier precursor, and mixing carbon microsphere/nano SiO2Annealing the composite demulsifier precursor to improve the defect structure of the composite material and reduce partial hydroxyl on the surface of the composite material to make the carbon microsphere/nano SiO2The composite demulsifier has the best hydrophilic and oleophilic properties, so that the demulsifier with high demulsification efficiency and good effect is prepared.
In some preferred embodiments of the present invention, the glucose solution is a mixture of glucose and distilled water in a mass ratio of 1: 7-15 by mixing.
In some preferred embodiments of the invention, the mass ratio of the glucose solution to the tetraethyl orthosilicate is 7-15: 2.
according to the embodiment of the invention, the concentration of the glucose solution and the dosage of the glucose solution and tetraethyl orthosilicate are optimized to improve the specific surface area of the carbon microspheres and reduce the carbon microspheres and nano SiO2And the emulsion breaking performance is better.
In some embodiments of the invention, the glucose solution and tetraethyl orthosilicate are uniformly mixed by using ultrasound, the ultrasound time is 5-15 min, the ultrasound frequency is 50Hz, and the ultrasound power is 200W; however, the glucose solution and tetraethyl orthosilicate may also be mixed by mechanical stirring, and the like, which is not further limited in the embodiment of the present invention, and those skilled in the art can adjust the mixing according to actual conditions as long as the glucose solution and tetraethyl orthosilicate are fully and uniformly mixed.
In some preferred embodiments of the present invention, the hydrothermal reaction temperature is 160 ℃, the reaction time is 18h, the hydrothermal reaction temperature and the reaction time are optimized to increase the specific surface area of the carbon microspheres and reduce the carbon microspheres and the nano SiO2And the emulsion breaking performance is better.
In some preferred embodiments of the present invention, after the hydrothermal reaction of the mixed solution, further comprising washing and drying the hydrothermal reaction product, wherein the washing is sequentially washing with ethanol and distilled water until the washing solution is clear; the drying is vacuum freeze drying.
In some preferred embodiments of the present invention, the vacuum freeze-drying temperature is-40 to-51 ℃ and the drying time is 1 to 4 days.
In some preferred embodiments of the present invention, the annealing temperature is 400 ℃ and the annealing time is 2 h; by optimizing annealing temperature and annealing time, the nano SiO2Better modifies the surface of the carbon microsphere and improves the carbon microsphere/nano SiO2The composite demulsifier has hydrophilic and oleophilic performances.
The inert gas may be helium, argon or nitrogen, in the embodiment of the present invention, nitrogen is selected, and those skilled in the art can select the kind of inert gas according to practical situations, which is not further limited in the present invention.
The embodiment of the invention also provides the carbon microsphere/nano SiO prepared by the preparation method2A composite demulsifier. The carbon microsphere/nano SiO prepared by the preparation method2The diameter of the carbon microsphere in the composite demulsifier is 0.8-1.2 um, and the average diameter is 1 um.
The embodiment of the invention also provides the carbon microsphere/nano SiO2Application of the composite demulsifier in W/O crude oil emulsion.
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The experimental methods in the present invention are conventional methods unless otherwise specified. The experimental materials used in the present invention were all purchased from the market unless otherwise specified.
Example 1:
embodiment 1 of the invention provides a carbon microsphere/nano SiO2The preparation method of the composite demulsifier comprises the following steps:
weighing 6 parts of glucose and 50 parts of distilled water, uniformly mixing the glucose and the distilled water to obtain a glucose solution, weighing 14 parts of tetraethyl orthosilicate, adding the tetraethyl orthosilicate into the glucose solution, and carrying out ultrasonic treatment for 10min under the conditions of 50Hz frequency and 200W power to obtain a mixed solution; pouring the mixed solution into a stainless steel reaction kettle with a polytetrafluoroethylene lining, sealing, carrying out hydrothermal reaction on the mixed solution at 160 ℃ for 18h to obtain a brown product, naturally cooling the brown product to normal temperature, sequentially washing the brown product with ethanol and distilled water until the washing liquid is clear, and carrying out vacuum freeze drying on the brown product at the temperature of-50 ℃ for 2 days to obtain the carbon microsphere/nano SiO2Compounding a demulsifier precursor; mixing carbon microsphere/nano SiO2Annealing the composite demulsifier precursor under the protection of nitrogen, wherein the annealing temperature is 400 ℃, and the annealing time is 2h, so as to obtain brown carbon microspheres/nano SiO2A composite demulsifier.
FIG. 2 shows the carbon microsphere/nano SiO in this example2Scanning Electron Microscope (SEM) image of the composite demulsifier, and as can be seen from FIG. 2, the surface of the carbon microsphere is covered with a plurality of nano SiO2And simultaneously more nano SiO2Dispersed between carbon microspheres, carbon microspheres/nano SiO2The diameter of the composite demulsifier is 0.8-1.2 μm.
FIG. 3 shows the carbon microsphere/nano SiO in this example2EDS diagram of composite demulsifier, as can be seen from FIG. 3, carbosphere/nano SiO2Elements of composite demulsifierThe proportion of the elements.
FIG. 4 shows glucose carbon spheres and nano SiO2And the carbon microsphere/nano SiO in this example2Fourier transform infrared spectrum contrast (FT-IR) of the composite demulsifier, as can be seen from FIG. 4, the carbosphere/nano SiO2The composite demulsifier has hydroxyl and SiO2Characteristic peak of Si-O-C in (1).
FIG. 5 shows a schematic diagram of a carbon microsphere and nano SiO2And the carbon microsphere/nano SiO in this example2Three-phase contact angle diagram of composite demulsifier, wherein CS is glucose carbon sphere, SiO2Is nano SiO2，SiO2@ CS is carbon microsphere/nano SiO in this example2Composite demulsifier, as can be seen from FIG. 5, the carbon microsphere/nano SiO in this example2The three-phase contact angle of the composite demulsifier is 93 degrees, compared with the simple nano SiO2(three-phase contact angle is 36.3 degrees) and the carbon microsphere (three-phase contact angle is 131 degrees), the three-phase contact angle is closer to 90 degrees, which shows that the carbon microsphere/nano SiO in the embodiment is2The composite demulsifier has the best hydrophilic and oleophilic performance, so the composite demulsifier can be easily transferred to an oil-water interface to replace a natural emulsifier of the oil-water interface in the crude oil emulsion, thereby realizing demulsification.
Example 2:
weighing 3 parts of glucose and 40 parts of distilled water by weight, uniformly mixing the glucose and the distilled water to obtain a glucose solution, weighing 6 parts of tetraethyl orthosilicate, adding the tetraethyl orthosilicate into the glucose solution, and carrying out ultrasonic treatment for 5min under the conditions of 50Hz frequency and 200W power to obtain a mixed solution; pouring the mixed solution into a stainless steel reaction kettle with a polytetrafluoroethylene lining, sealing, carrying out hydrothermal reaction on the mixed solution at 180 ℃ for 12 hours to obtain a brown product, naturally cooling the brown product to normal temperature, sequentially washing the brown product with ethanol and distilled water until the washing liquid is clear, and carrying out vacuum freeze drying on the brown product at-51 ℃ for 1 day to obtain the carbon microsphere/nano-scale microsphere/nanoSiO2Compounding a demulsifier precursor; mixing carbon microsphere/nano SiO2Annealing the composite demulsifier precursor under the protection of nitrogen, wherein the annealing temperature is 300 ℃, and the annealing time is 3h, so as to obtain brown carbon microspheres/nano SiO2A composite demulsifier.
Example 3:
embodiment 3 of the invention provides a carbon microsphere/nano SiO2The preparation method of the composite demulsifier comprises the following steps:
weighing 4 parts of glucose and 45 parts of distilled water by weight, uniformly mixing the glucose and the distilled water to obtain a glucose solution, weighing 9.5 parts of tetraethyl orthosilicate, adding the tetraethyl orthosilicate into the glucose solution, and carrying out ultrasonic treatment for 8min under the conditions of 50Hz frequency and 200W power to obtain a mixed solution; pouring the mixed solution into a stainless steel reaction kettle with a polytetrafluoroethylene lining, sealing, carrying out hydrothermal reaction on the mixed solution at 140 ℃ for 20 hours to obtain a brown product, naturally cooling the brown product to normal temperature, sequentially washing the brown product with ethanol and distilled water until the washing liquid is clear, and carrying out vacuum freeze drying on the brown product at-48 ℃ for 3 days to obtain the carbon microsphere/nano SiO2Compounding a demulsifier precursor; mixing carbon microsphere/nano SiO2Annealing the composite demulsifier precursor under the protection of nitrogen, wherein the annealing temperature is 500 ℃, and the annealing time is 1h, so as to obtain brown carbon microspheres/nano SiO2A composite demulsifier.
Example 4:
weighing 5 parts of glucose and 50 parts of distilled water by weight, uniformly mixing the glucose and the distilled water to obtain a glucose solution, weighing 12 parts of tetraethyl orthosilicate, adding the tetraethyl orthosilicate into the glucose solution, and carrying out ultrasonic treatment for 10min under the conditions of 50Hz frequency and 200W power to obtain a mixed solution; pouring the mixed solution into a stainless steel reaction kettle with a polytetrafluoroethylene lining, sealing, carrying out hydrothermal reaction on the mixed solution at 155 ℃ for 18h to obtain a brown product,naturally cooling the brown product to normal temperature, sequentially cleaning with ethanol and distilled water until the cleaning solution is clear, and then carrying out vacuum freeze drying on the brown product at-45 ℃ for 4 days to obtain the carbon microsphere/nano SiO2Compounding a demulsifier precursor; mixing carbon microsphere/nano SiO2Annealing the composite demulsifier precursor under the protection of nitrogen, wherein the annealing temperature is 400 ℃, and the annealing time is 2h, so as to obtain brown carbon microspheres/nano SiO2A composite demulsifier.
Example 5:
embodiment 5 of the invention provides a carbon microsphere/nano SiO2The preparation method of the composite demulsifier comprises the following steps:
weighing 7 parts of glucose and 60 parts of distilled water by weight, uniformly mixing the glucose and the distilled water to obtain a glucose solution, weighing 16.6 parts of tetraethyl orthosilicate, adding the tetraethyl orthosilicate into the glucose solution, and carrying out ultrasonic treatment for 15min under the conditions of 50Hz frequency and 200W power to obtain a mixed solution; pouring the mixed solution into a stainless steel reaction kettle with a polytetrafluoroethylene lining, sealing, carrying out hydrothermal reaction on the mixed solution at 170 ℃ for 16h to obtain a brown product, naturally cooling the brown product to normal temperature, sequentially washing the brown product with ethanol and distilled water until the washing liquid is clear, and carrying out vacuum freeze drying on the brown product at the temperature of-50 ℃ for 1 day to obtain the carbon microsphere/nano SiO2Compounding a demulsifier precursor; mixing carbon microsphere/nano SiO2Annealing the composite demulsifier precursor under the protection of nitrogen, wherein the annealing temperature is 450 ℃, and the annealing time is 2.5h, so as to obtain brown carbon microspheres/nano SiO2A composite demulsifier.
Based on the carbon microsphere/nano SiO prepared in the embodiments 1-52Composite demulsifier, which is illustrated by the following tests2Application of composite demulsifier in crude oil emulsion.
Test example 1:carbon microsphere/nano SiO with different concentrations2Application of composite demulsifier in crude oil emulsion
1 part of carbon microsphere/nano SiO2Fully mixing the composite demulsifier with 1 part of water to form a suspension emulsion, and then respectively adding suspensions with different volume parts (0, 1, 2 and 3) into 5000 volume parts of 22 wt% W/O crude oil emulsion, namely carbon microsphere/nano SiO2The concentration of the composite demulsifier in the W/O crude oil emulsion is 0, 100mg/L, 200mg/L and 300mg/L in sequence, the mixed solution is kept still for 10min at 70 ℃, then is violently shaken for 100 times to be uniformly mixed, is kept still for 180min in a 70 ℃ water bath kettle, and finally the demulsification efficiency is calculated as shown in Table 1.
TABLE 1
| Group of | 0 | Demulsification efficiency of 100mg/L | Demulsification efficiency of 200mg/L | Demulsification efficiency of 300mg/L |
| Example 1 | 0 | 85.87％ | 85.87％ | 89.45％ |
| Example 2 | 0 | 81.56％ | 82.30％ | 84.96％ |
| Example 3 | 0 | 80.45％ | 81.52％ | 84.24％ |
| Example 4 | 0 | 83.22％ | 83.85％ | 86.76％ |
| Example 5 | 0 | 81.56％ | 82.75％ | 85.74％ |
As can be seen from Table 1, the carbon microsphere/nano SiO provided by the invention2The composite demulsifier has good demulsification performance, and the demulsification effect is increased along with the increase of the concentration of the demulsifier in the crude oil emulsion.
Test example 2:carbon microsphere/nano SiO2Acid and alkali resistance of composite demulsifier
1 part of carbon microsphere/nano SiO2Fully mixing the composite demulsifier with 1 part of water to form a suspension emulsion, then respectively adding 3 parts by volume of suspension into 5000 parts by volume of 22 wt% W/O crude oil emulsion (the pH values of the crude oil emulsion are respectively 2, 4, 6, 8 and 10), standing for 10min at 70 ℃, then violently shaking for 100 times to uniformly mix, then standing for 180min in a 70 ℃ water bath kettle, and finally calculating the demulsification efficiency of the composite demulsifier and the water, wherein the demulsification efficiency is shown in table 2.
TABLE 2
| Group of | pH value of 2 | pH value of 4 | pH value of 6 | pH value of 8 | pH value of 10 |
| Example 1 | 82.86％ | 82.86％ | 89.45％ | 78.17％ | 78.17％ |
| Example 2 | 76.34％ | 76.68％ | 84.96％ | 73.65％ | 73.35％ |
| Example 3 | 76.21％ | 76.54％ | 84.24％ | 73.98％ | 73.49％ |
| Example 4 | 79.38％ | 79.68％ | 86.76％ | 76.82％ | 76.48％ |
| Example 5 | 78.25％ | 78.47％ | 85.74％ | 75.69％ | 75.31％ |
As can be seen from Table 2, the carbon microsphere/nano SiO provided by the invention2The demulsification efficiency of the composite demulsifier under the neutral condition is higher than that of the composite demulsifier under the acidic condition, and the demulsification efficiency of the composite demulsifier under the acidic condition is higher than that of the composite demulsifier under the alkaline condition, but the demulsification efficiency of the composite demulsifier under the acidic condition is also very high on the whole, and the results show that the carbon microsphere/nano SiO provided by the invention is high2The composite demulsifier has strong acid and alkali resistance.
Test example 3:carbon microsphere/nano SiO2Salt tolerance of composite demulsifier
1 part of carbon microsphere/nano SiO2Fully mixing the composite demulsifier with 1 part of water to form a suspension emulsion, then respectively adding 3 parts by volume of suspension into 5000 parts by volume of 22 wt% W/O crude oil emulsion (with the pH value of 6) with the salinity of 0, 5000mg/L, 10000mg/L, 15000mg/L, 20000mg/L and 25000mg/L, standing the mixed solution for 10min at 70 ℃, standing for 10min at 70 ℃, then violently shaking for 100 times to mix the mixed solution uniformly, standing for 180min in a 70 ℃ water bath kettle, and finally calculating the demulsification efficiency of the mixed solution, wherein the demulsification efficiency is shown in Table 3.
TABLE 3
| Group of | 0 | 5000mg/L | 10000mg/L | 15000mg/L | 20000mg/L | 25000mg/L |
| Example 1 | 89.45％ | 86.86％ | 86.86％ | 86.86％ | 86.86％ | 86.86％ |
| Example 2 | 84.96％ | 81.36％ | 80.67％ | 80.67％ | 80.67％ | 80.67％ |
| Example 3 | 84.24％ | 81.35％ | 81.35％ | 81.35％ | 81.35％ | 81.35％ |
| Example 4 | 86.76％ | 83.62％ | 83.43％ | 83.43％ | 83.43％ | 83.43％ |
| Example 5 | 85.74％ | 82.81％ | 82.52％ | 82.52％ | 82.52％ | 82.52％ |
As can be seen from Table 3, the carbon microsphere/nano SiO provided by the invention2The composite demulsifier has high demulsification efficiency on high-salinity crude oil emulsion, almost approaches to the demulsification efficiency in the absence of salinity, and shows that the carbon microsphere/nano SiO2The composite demulsifier has strong salt tolerance.
From the above results, it can be seen that the carbon microsphere/nano SiO provided by the invention2The composite demulsifier has good demulsification performance to acid-base and high-salinity crude oil emulsion, and the water phase is clear after demulsification and has no wall-hanging phenomenon, and the carbon microsphere/nano SiO provided by the invention2The preparation method of the composite demulsifier is simple, easy to operate and environment-friendly.
The above-described embodiments of the present invention should not be construed as limiting the scope of the present invention. Any other corresponding changes and modifications made according to the technical idea of the present invention should be included in the protection scope of the claims of the present invention.
Claims (10)
1. Carbon microsphere/nano SiO2The preparation method of the composite demulsifier is characterized by comprising the following steps: uniformly mixing a glucose solution and tetraethyl orthosilicate to obtain a mixed solution; carrying out hydrothermal reaction on the mixed solution to obtain carbon microspheres/nano SiO2Compounding a demulsifier precursor, wherein the hydrothermal reaction temperature is 140-180 ℃, and the reaction time is 8-20 h; mixing the carbon microsphere/nano SiO2Annealing the composite demulsifier precursor under the protection of inert gas to obtain the carbon microsphere/nano SiO2The composite demulsifier has the annealing temperature of 300-500 ℃ and the annealing time of 1-3 h.
2. The carbosphere/nanosio of claim 12The preparation method of the composite demulsifier is characterized in that the glucose solution is prepared from glucose and distilled water according to a mass ratio of 1: 7-15 by mixing.
3. The carbosphere/nanosio of claim 12The preparation method of the composite demulsifier is characterized in that the mass ratio of the glucose solution to tetraethyl orthosilicate is 7-15: 2.
4. the carbosphere/nanosio of claim 12The preparation method of the composite demulsifier is characterized in that the glucose solution and tetraethyl orthosilicate are uniformly mixed by ultrasound, the ultrasound time is 5-15 min, the ultrasound frequency is 50Hz, and the ultrasound power is 200W.
5. The carbosphere/nanosio of claim 12The preparation method of the composite demulsifier is characterized in that the hydrothermal reaction temperature is 160 ℃, and the reaction time is 18 h.
6. The carbosphere/nanosio of claim 12The preparation method of the composite demulsifier is characterized in that after the mixed solution is subjected to hydrothermal reaction, the mixed solution is further subjected to hydrothermal reactionThe method comprises the steps of cleaning and drying a hydrothermal reaction product, wherein the cleaning is sequentially performed by using ethanol and distilled water until a cleaning solution is clear; the drying is vacuum freeze drying.
7. The carbosphere/nanosio of claim 12The preparation method of the composite demulsifier is characterized in that the vacuum freeze drying temperature is-40 to-51 ℃, and the drying time is 1 to 4 days.
8. The carbosphere/nanosio of claim 12The preparation method of the composite demulsifier is characterized in that the annealing temperature is 400 ℃ and the annealing time is 2 hours.
9. Carbon microsphere/nano SiO prepared by the preparation method of any one of claims 1 to 82A composite demulsifier.
10. Carbon microsphere/nano SiO prepared by the preparation method of any one of claims 1 to 82Application of the composite demulsifier in W/O crude oil emulsion.
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| CN112210397A (en) * | 2020-09-27 | 2021-01-12 | 长江大学 | Carbon fiber/nano silicon dioxide compound and preparation method and application thereof |
| CN112480945A (en) * | 2020-10-30 | 2021-03-12 | 长江大学 | Rice hull charcoal, demulsifier, preparation method and application thereof |
| CN112877093A (en) * | 2021-01-14 | 2021-06-01 | 长江大学 | Demulsifier, demulsifier composition, and preparation method and application thereof |
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| CN112480945A (en) * | 2020-10-30 | 2021-03-12 | 长江大学 | Rice hull charcoal, demulsifier, preparation method and application thereof |
| CN112877093A (en) * | 2021-01-14 | 2021-06-01 | 长江大学 | Demulsifier, demulsifier composition, and preparation method and application thereof |
| CN112877093B (en) * | 2021-01-14 | 2023-12-05 | 长江大学 | Demulsifier, demulsifier composition, and preparation method and application of demulsifier composition |
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Application publication date: 20200922 |