CN114015471A - Preparation method of carbon-based nano magnetic demulsifier - Google Patents
Preparation method of carbon-based nano magnetic demulsifier Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 75
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- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims description 7
- 239000005642 Oleic acid Substances 0.000 claims description 7
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims description 7
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims description 7
- 238000000034 method Methods 0.000 claims description 7
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- WNLRTRBMVRJNCN-UHFFFAOYSA-N adipic acid Chemical compound OC(=O)CCCCC(O)=O WNLRTRBMVRJNCN-UHFFFAOYSA-N 0.000 claims description 6
- 239000011259 mixed solution Substances 0.000 claims description 6
- BDJRBEYXGGNYIS-UHFFFAOYSA-N nonanedioic acid Chemical compound OC(=O)CCCCCCCC(O)=O BDJRBEYXGGNYIS-UHFFFAOYSA-N 0.000 claims description 6
- 238000005119 centrifugation Methods 0.000 claims description 5
- LZKLAOYSENRNKR-LNTINUHCSA-N iron;(z)-4-oxoniumylidenepent-2-en-2-olate Chemical compound [Fe].C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O LZKLAOYSENRNKR-LNTINUHCSA-N 0.000 claims description 4
- OYHQOLUKZRVURQ-NTGFUMLPSA-N (9Z,12Z)-9,10,12,13-tetratritiooctadeca-9,12-dienoic acid Chemical compound C(CCCCCCC\C(=C(/C\C(=C(/CCCCC)\[3H])\[3H])\[3H])\[3H])(=O)O OYHQOLUKZRVURQ-NTGFUMLPSA-N 0.000 claims description 3
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- 239000005715 Fructose Substances 0.000 claims description 3
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- 235000011037 adipic acid Nutrition 0.000 claims description 3
- 239000001361 adipic acid Substances 0.000 claims description 3
- WQZGKKKJIJFFOK-PHYPRBDBSA-N alpha-D-galactose Chemical compound OC[C@H]1O[C@H](O)[C@H](O)[C@@H](O)[C@H]1O WQZGKKKJIJFFOK-PHYPRBDBSA-N 0.000 claims description 3
- 229930182830 galactose Natural products 0.000 claims description 3
- 125000002791 glucosyl group Chemical group C1([C@H](O)[C@@H](O)[C@H](O)[C@H](O1)CO)* 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 230000035484 reaction time Effects 0.000 claims description 3
- SZVJSHCCFOBDDC-UHFFFAOYSA-N iron(II,III) oxide Inorganic materials O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 description 25
- 230000000694 effects Effects 0.000 description 12
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- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 description 1
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Classifications
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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
- C10G33/00—Dewatering or demulsification of hydrocarbon oils
- C10G33/04—Dewatering or demulsification of hydrocarbon oils with chemical means
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- Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The invention discloses a preparation method of a carbon-based nano magnetic demulsifier, which comprises the steps of firstly weighing a certain amount of monosaccharide or chitosan, dissolving the monosaccharide or chitosan in water, reacting in a reaction kettle to obtain a product A, centrifuging the product A, and drying the centrifuged product A under a vacuum condition to obtain carbon nanospheres; then weighing a certain amount of ferric acetylacetonate, adding an acidic reducing agent to obtain a mixture B, adding carbon nanospheres into the mixture B, adding solvent dibenzyl ether, placing the mixture into a reaction kettle, purging the mixture with inert gas, and reacting for 3 to 10 hours at the temperature of between 200 and 260 ℃ to obtain a demulsifier mixture C; and (3) recovering the demulsifier product M in the demulsifier mixture D by using a magnet, washing the demulsifier product M by using a solvent N, and finally performing vacuum drying to obtain a pure demulsifier product. The technical problem that the demulsifier in the prior art can not be repeatedly utilized is solved.
Description
Technical Field
The invention belongs to the field of oilfield produced liquid treatment, and particularly relates to a preparation method of a carbon-based nano magnetic demulsifier.
Background
At present, because of the application of oil displacement technologies such as water injection and the like, the water content of crude oil is high, methods for crude oil dehydration in the prior art mainly focus on methods such as gravity settling and chemical demulsification, but the gravity settling is not enough to completely dehydrate the crude oil; currently, dewatering generally requires forcing the oil and water to separate by adding a demulsifier.
The demulsifier in the prior art mainly focuses on phenolic amine resin polyether, phenolic resin polyether, hyperbranched polyamide-amine demulsifier and the like, and aims to increase molecular weight mainly, increase oil-water interfacial tension by increasing molecular weight, promote oil drops to coalesce and separate oil from water.
However, the existing demulsifiers cannot be reused, thus affecting environmental protection and not meeting the requirements of environmental protection.
Disclosure of Invention
The invention aims to provide a preparation method of a carbon-based nano magnetic demulsifier, which aims to solve the technical problem that the demulsifier in the prior art cannot be repeatedly utilized.
In order to realize the purpose, the invention adopts the following technical scheme:
a preparation method of a carbon-based nano magnetic demulsifier comprises the following steps:
(1) firstly, weighing a certain amount of monosaccharide or chitosan, dissolving the monosaccharide or chitosan in water, reacting in a reaction kettle at 180-250 ℃ for 10-12 hours to obtain a product A, centrifuging the product A, washing the centrifuged product A, and drying under a vacuum condition to obtain carbon nanospheres;
(2) weighing a certain amount of ferric acetylacetonate, and adding an acidic reducing agent to obtain a mixture B, wherein the mass ratio of the ferric acetylacetonate to the acidic reducing agent is 1: 3-1: 5; adding a certain amount of carbon nanospheres into the mixture B, wherein the carbon nanospheres account for 3-10% of the mass of the iron acetylacetonate; adding solvent dibenzyl ether, placing the mixture in a reaction kettle, purging the mixture by using inert gas, and reacting the mixture for 3 to 10 hours at the temperature of between 200 and 260 ℃ to obtain a demulsifier mixture C;
(3) and (3) recovering the demulsifier product in the demulsifier mixture C by using a magnet, washing the demulsifier product by using a solvent D, and finally performing vacuum drying to obtain a pure demulsifier product.
In some of these embodiments, in step (1), the monosaccharide is glucose, chitosan, fructose, or galactose.
In some embodiments, in step (1), the reaction temperature of the reaction kettle is 180 ℃ and the reaction time is 12 h.
In some embodiments, in step (1), the product A is washed 3-5 times with deionized water and then 3-5 times with absolute ethanol.
In some embodiments, in step (1), the rotation speed of the product A centrifugation is 4000-5000 r/min.
In some of these embodiments, the acidic reducing agent described in step (2) is oleic acid, linoleic acid, azelaic acid, or adipic acid.
In some embodiments, in step (2), the amount of benzyl ether added is 30-50 ml.
In some of the examples, in step (2), the solvent dibenzyl ether was added and placed in a reaction kettle and purged with an inert gas, and after reacting for 5 hours at 230 ℃, the demulsifier mixture C was obtained.
In some embodiments, in the step (2), the solvent D is a mixed solution of n-hexane and absolute ethyl alcohol in a volume ratio of 1: 1.
In some embodiments, in the step (1), 10g of glucose is weighed and dissolved in 100ml of deionized water, the mixture is reacted in a reaction kettle at 180 ℃ for 12 hours to obtain a product A, and the product A is centrifuged at the speed of 4000-5000 r/min; washing the obtained product A with deionized water and absolute ethyl alcohol for 3 times respectively, and carrying out vacuum drying for 12h at the temperature of 60 ℃ to obtain carbon nanospheres;
in the step (2), 0.7g of ferric acetylacetonate is weighed, 2.1g of oleic acid is added to obtain a mixture B, 0.03g of carbon nanospheres is added into the mixture B, solvent dibenzyl ether is added, the mixture is placed into a reaction kettle and is purged by nitrogen for 30min, and a demulsifier mixture C is obtained after the mixture reacts for 5 hours at 230 ℃;
in the step (3), a demulsifier product is recovered from the product by using a magnet, the product is washed for 5 times by using a mixed solution of normal hexane and absolute ethyl alcohol, and finally the product is carried and dried in vacuum at 60 ℃ for 12 hours to obtain the demulsifier product.
Compared with the prior art, the invention has the advantages and beneficial effects that:
the invention synthesizes Fe3O4The carbon nanospheres are added in the process, and are compounded together through the van der Waals force between molecules, and the carbon nanospheres can play a strong adsorption role with colloids, asphaltine and the like in oil drops through pi-pi bonds depending on the conjugated aromatic ring structure of the carbon nanospheres. In addition, the characteristics of the nano structures of the ferroferric oxide and the carbon nanospheres determine that the ferroferric oxide and the carbon nanospheres have higher specific surface areas, and the ferroferric oxide and the carbon nanospheres have strong synergistic adsorption effect. Meanwhile, as ferroferric oxide can be adsorbed by the magnet, the prepared magnetic demulsifier has a good demulsification effect on one hand and has a recoverable capability on the other hand. Therefore, the technical problem that the demulsifier in the prior art cannot be repeatedly utilized is solved.
Drawings
FIG. 1 is a schematic diagram of the reaction process;
FIG. 2 is an infrared spectrum of a carbon-based magnetic demulsifier;
FIG. 3 is a XRD pattern of a carbon-based magnetic demulsifier;
FIG. 4 is a SEM image of a carbon-based magnetic demulsifier;
FIG. 5 shows the demulsifying effect of the magnetic demulsifier at different demulsifier concentrations;
FIG. 6 shows the demulsifying effect of the magnetic demulsifier B at different demulsifier concentrations;
FIG. 7 shows the demulsifying effect of the magnetic demulsifier C at different demulsifier concentrations;
FIG. 8 shows the demulsifying effect of the magnetic demulsifier D at different demulsifier concentrations;
FIG. 9 shows the demulsification effect of the magnetic demulsifier A at different demulsification times;
FIG. 10 shows the demulsifying effect of the magnetic demulsifier A at different demulsifying times;
FIG. 11 shows the recovery performance of the demulsifiers.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
According to the invention, the carbon nanospheres are added in the process of synthesizing Fe3O4, the carbon nanospheres and the Fe3O4 are compounded together through the action of intermolecular van der Waals force, and the carbon nanospheres can play a strong adsorption role with colloids, asphaltenes and the like in oil drops through pi-pi bonds depending on the conjugated aromatic ring structure of the carbon nanospheres. In addition, the characteristics of the nano structures of the ferroferric oxide and the carbon nanospheres determine that the ferroferric oxide and the carbon nanospheres have higher specific surface areas, and the ferroferric oxide and the carbon nanospheres have strong synergistic adsorption effect. Meanwhile, as ferroferric oxide can be adsorbed by the magnet, the prepared magnetic demulsifier has a good demulsification effect on one hand and has a recoverable capability on the other hand. Therefore, the technical problem that the demulsifier in the prior art cannot be repeatedly utilized is solved.
Specifically, the method comprises the following steps:
(1) firstly, weighing a certain amount of monosaccharide or chitosan, dissolving the monosaccharide or chitosan in water, reacting in a reaction kettle at 180-250 ℃ for 10-12 hours to obtain a product A, centrifuging the product A, washing the centrifuged product A, and drying the washed product A under a vacuum condition to obtain the carbon nanospheres;
(2) weighing a certain amount of ferric acetylacetonate, and adding an acidic reducing agent to obtain a mixture B, wherein the mass ratio of the ferric acetylacetonate to the acidic reducing agent is 1: 3-1: 5; adding carbon nanospheres into the mixture B, wherein the mass of the carbon nanospheres is 3-10% of that of the iron acetylacetonate, adding solvent dibenzyl ether, placing the mixture into a reaction kettle, purging the mixture by using inert gas, and reacting the mixture for 3-10 hours at 200-260 ℃ to obtain a demulsifier mixture C;
(3) and (3) recovering the demulsifier product M in the demulsifier mixture D by using a magnet, washing the demulsifier product M by using a solvent N, and finally performing vacuum drying to obtain a pure demulsifier product.
In a preferred embodiment, in the step (1), the reaction temperature of the reaction kettle is 180 ℃ to 250 ℃, specifically 180 ℃, and the reaction time is 10h to 12h, specifically 12 h.
In a preferred embodiment, in the step (1), the rotation speed required by the centrifugation of the product A is 4000-5000 r/min, specifically 5000 r/min; the centrifugation time of the product is 10-15 min, specifically 10 min.
In a preferred embodiment, in step (1), the monosaccharide is glucose, chitosan, fructose or galactose.
In a preferred embodiment, in step (1), the product a after centrifugation is washed with deionized water for 3-5 times, specifically 3 times, and then washed with absolute ethanol for 3-5 times, specifically 3 times.
In a preferred embodiment, in the step (1) and the step (2), the product a and the demulsifier mixture C are dried for 10 to 12 hours, specifically 10 hours, under the condition that the vacuum drying temperature is 50 to 60 ℃, specifically 60 ℃.
In a preferred embodiment, in the step (2), the mass ratio of ferric acetylacetonate to oleic acid is 1: 3-1: 5,
in a preferred embodiment, in step (2), the acidic reducing agent is oleic acid, linoleic acid, azelaic acid or adipic acid.
In a preferred embodiment, in the step (2), the amount of the benzyl ether added is 30 to 50ml, specifically 30 ml.
In a preferred embodiment, in the step (2), adding a solvent of dibenzyl ether, placing the mixture in a reaction kettle, purging the reaction kettle by using inert gas, and reacting at 230 ℃ for 5 hours to obtain a demulsifier mixture C; .
In a preferred embodiment, in the step (2), the solvent D is a mixed solution of n-hexane and absolute ethyl alcohol in a volume ratio of 1: 1.
In order to better illustrate the preparation method of the carbon-based nano-magnetic demulsifier, the following description will be made in detail with reference to the comparative examples and examples.
Example 1
(1) Firstly weighing 10g of glucose and dissolving the glucose in deionized water, reacting for 12h at 180 ℃ in a reaction kettle, centrifuging the product at 5000r/min, washing for 3-5 times with deionized water and absolute ethyl alcohol respectively, and drying for 12h under vacuum at 60 ℃ to obtain the carbon nanospheres.
(2) Weighing 0.7g of iron acetylacetonate, adding 2.1g of oleic acid, adding 0.03g of carbon nanospheres into the mixture, adding benzyl ether serving as a solvent, placing the mixture into a 100ml reaction kettle, purging the mixture for 30min by using nitrogen, reacting the mixture for 5 hours at 230 ℃ to obtain a mixture, recovering a product by using a magnet, washing the product for 5 times by using a mixed solution of n-hexane and absolute ethyl alcohol, and finally performing vacuum drying for 12 hours at 60 ℃ to obtain a demulsifier product; the specific reaction process is as follows:
as shown in FIG. 2, the characteristic peak at 3430cm-1 is the-OH functional group. The characteristic peak near 3247cm-1 represents-COOH group, and the carbon nanosphere is compounded with ferroferric oxide through the two groups. The characteristic peak near 1643cm-1 is the carbonyl function, the characteristic peak at 1214cm-1 is the C ═ C function. The appearance of the above groups indicates that the aromatizing reaction of glucose occurs during the formation of the carbon nanoball. In addition, by comparing the magnetic carbon nanoball with Fe3O4FT-IR of @ C shows that the characteristic peak intensities of all functional groups except the Fe-O group are significantly weakened as compared with FT-IR of the carbon nanoball because the carbon nanoball is Fe-O-doped3O4Attached so that its strength is weakened.
As shown in fig. 3, the carbon nanoball shows 1 prominent hump at 20.87 ° 2 θ; the peak width of the peak indicates that the carbon nanosphere has low crystallization degree and Fe3O4@ C shows a diffraction peak at 6. Diffraction peaks of the magnetic carbon nanoball are respectively positioned at 30.17 °, 35.47 °, 43.17 °, 53.43 °, 57.17 ° and 62.63 ° of 2 θ, and the 6 diffraction peaks correspond to Fe3O4On the 6 crystal planes of (220), (311), (400), (422), (511) and (440). With Fe3O4Compared with the spectrum of the compound, the diffraction peaks with the 2 theta of 30.17 degrees, 35.47 degrees and 62.63 degrees are obviously enhanced. In addition, from the XRD spectrum, Fe3O4The diffraction peak intensity at 20.87 ℃ is low at @ C, which is comparable to Fe3O4Has higher crystallization degree than the C nanometer ball, resulting inThe diffraction peak intensity of the C nanosphere is low. The above results show that Fe3O4Have been successfully complexed with carbon nanospheres.
As shown in fig. 4, (a) is a carbon nanoball, and (b) is a carbon-based nanoball magnetic demulsifier. It can be seen that in Fe3O4The carbon nanosphere particles are compounded around the composite nano-emulsion, and the ferroferric oxide nanoparticles are dispersed and uniform in particle size, so that the successful synthesis of the carbon-based nanosphere magnetic demulsifier is proved.
As can be seen from FIG. 5, when the demulsification experiment is carried out on the prepared magnetic demulsifiers with different demulsifier concentrations at the experiment temperature of 65 ℃, the demulsification efficiency can reach 93.31% at 600 ppm.
Example 2
This example is different from example 1 in that the amount of the carbon nanoball added is changed to 0.07g in the step (2), and benzyl ether solvent is added and placed in the reaction kettle and purged with inert gas, and the temperature is adjusted to 200 ℃, and demulsifier mixture C is obtained after reaction for 3 hours.
As can be seen from fig. 6, the demulsification experiment was performed on the magnetic demulsifier B prepared in example 2 at an experimental temperature of 65 ℃. The oil removal rate was highest at 800p, 89.56%.
Example 3
The difference between this example and example 1 is that the carbon source is adjusted to be chitosan, and in step (2), the solvent dibenzyl ether is added and placed in the reaction kettle and purged with inert gas, and the temperature is adjusted to 260 ℃, and the demulsifier mixture C is obtained after 5 hours of reaction.
As can be seen from fig. 7, the demulsification experiment was performed on the magnetic demulsifier C prepared in example 3 at an experimental temperature of 65 ℃. The oil removal rate at 800ppm was the highest at 82.66%.
Example 4
This example is different from example 1 in that the amount of the carbon nanoball added is changed to 0.07g in the step (2), and benzyl ether solvent is added and placed in the reaction kettle and purged with inert gas, and the temperature is adjusted to 230 ℃, and demulsifier mixture C is obtained after 8 hours of reaction.
As can be seen from fig. 8, the demulsification experiment was performed on the magnetic demulsifier D prepared in example 4 at an experimental temperature of 65 ℃. The oil removal rate at 600ppm was the highest at 89.64%.
Fig. 9 and fig. 10 are graphs showing the demulsification effect at 65 ℃ at different times, that is, taking example 1 as an example, the demulsification rate of the magnetic demulsifier prepared in the example at different times is measured. Wherein (a)5min, (b)15min, (c)30min, (d)60min, (e)90min, and (f)120 min. It can be seen from the above examples that the carbon-based nanosphere magnetic demulsifier of the present invention is a high-efficiency demulsifier, and the demulsification experiment performed on the demulsifier prepared in example 1 shows that the demulsification efficiency of the demulsifier can reach 93.31%.
As shown in fig. 11, the magnetic demulsifier prepared in example 1 was subjected to a recovery performance test. As can be seen from the figure, in the previous 4 times of demulsification recovery experiments, the demulsification efficiency of the carbon-based nanosphere magnetic demulsifier disclosed by the invention is stabilized to be more than 90%, which indicates that the demulsification efficiency of the demulsifier has the recovery performance.
In conclusion, the carbon-based nanosphere magnetic demulsifier prepared in the invention is prepared by compounding carbon nanospheres and ferroferric oxide nanoparticles by a one-pot method. The carbon nanospheres are hydrolyzed from saccharides such as glucose, so that the carbon nanospheres are environment-friendly and have no damage to the environment. The magnetic demulsifier has both magnetism and demulsification capacity, on one hand, the carbon nanospheres adsorb oil drops through pi-pi bonds, and on the other hand, the hydrophobic effect of the ferroferric oxide and the carbon nanospheres also enhances the adsorption effect. Meanwhile, the two are nanoparticles, and the larger specific surface area also provides more adsorption sites. Therefore, the carbon-based nanosphere magnetic demulsifier prepared in the invention has great application potential.
The above description is only a preferred embodiment of the present invention, and not intended to limit the present invention in other forms, and any person skilled in the art may apply the above modifications or changes to the equivalent embodiments with equivalent changes, without departing from the technical spirit of the present invention, and any simple modification, equivalent change and change made to the above embodiments according to the technical spirit of the present invention still belong to the protection scope of the technical spirit of the present invention.
Claims (10)
1. A preparation method of a carbon-based nano magnetic demulsifier is characterized by comprising the following steps:
(1) firstly, weighing a certain amount of monosaccharide or chitosan, dissolving the monosaccharide or chitosan in water, reacting in a reaction kettle at 180-250 ℃ for 10-12 hours to obtain a product A, centrifuging the product A, washing the centrifuged product A, and drying under a vacuum condition to obtain carbon nanospheres;
(2) weighing a certain amount of ferric acetylacetonate, and adding an acidic reducing agent to obtain a mixture B, wherein the mass ratio of the ferric acetylacetonate to the acidic reducing agent is 1: 3-1: 5; adding a certain amount of carbon nanospheres into the mixture B, wherein the carbon nanospheres account for 3-10% of the mass of the iron acetylacetonate; adding solvent dibenzyl ether, placing the mixture in a reaction kettle, purging the mixture by using inert gas, and reacting the mixture for 3 to 10 hours at the temperature of between 200 and 260 ℃ to obtain a demulsifier mixture C;
(3) and (3) recovering the demulsifier product in the demulsifier mixture C by using a magnet, washing the demulsifier product by using a solvent D, and finally performing vacuum drying to obtain a pure demulsifier product.
2. The preparation method of the carbon-based nano-magnetic demulsifier according to claim 1, wherein in the step (1), the monosaccharide is glucose, chitosan, fructose, or galactose.
3. The preparation method of the carbon-based nano magnetic demulsifier according to claim 1 or 2, wherein in step (1), the reaction temperature of the reaction kettle is 180 ℃ and the reaction time is 12 h.
4. The preparation method of the carbon-based nano magnetic demulsifier according to claim 1 or 2, wherein in step (1), the product A is washed with deionized water for 3-5 times and then with anhydrous ethanol for 3-5 times.
5. The preparation method of the carbon-based nano magnetic demulsifier according to claim 4, wherein in step (1), the rotation speed of the product A during centrifugation is 4000-5000 r/min.
6. The method for preparing the carbon-based nano magnetic demulsifier according to claim 1, wherein the acidic reducing agent in step (2) is oleic acid, linoleic acid, azelaic acid or adipic acid.
7. The preparation method of the carbon-based nano magnetic demulsifier according to claim 1 or 6, wherein in step (2), the addition amount of the benzyl ether is 30-50 ml.
8. The preparation method of the carbon-based nano magnetic demulsifier according to claim 7, wherein in step (2), the solvent dibenzyl ether is added, the mixture is placed in a reaction kettle and purged with inert gas, and the demulsifier mixture C is obtained after 5 hours of reaction at 230 ℃.
9. The preparation method of the carbon-based nano magnetic demulsifier according to claim 7, wherein in step (2), the solvent D is a mixed solution of n-hexane and absolute ethanol at a volume ratio of 1: 1.
10. The preparation method of the carbon-based nano-magnetic demulsifier according to claim 1,
in the step (1), 10g of glucose is weighed and dissolved in 100ml of deionized water, the mixture is reacted in a reaction kettle at the temperature of 180 ℃ for 12 hours to obtain a product A, and the product A is centrifuged at the speed of 4000-5000 r/min; washing the obtained product A with deionized water and absolute ethyl alcohol for 3 times respectively, and carrying out vacuum drying for 12h at the temperature of 60 ℃ to obtain carbon nanospheres;
in the step (2), 0.7g of ferric acetylacetonate is weighed, 2.1g of oleic acid is added to obtain a mixture B, 0.03g of carbon nanospheres is added into the mixture B, solvent dibenzyl ether is added, the mixture is placed into a reaction kettle and is purged by nitrogen for 30min, and a demulsifier mixture C is obtained after the mixture reacts for 5 hours at 230 ℃;
in the step (3), a demulsifier product is recovered from the product by using a magnet, the product is washed for 5 times by using a mixed solution of normal hexane and absolute ethyl alcohol, and finally the product is carried and dried in vacuum at 60 ℃ for 12 hours to obtain the demulsifier product.
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| CN110182894A (en) * | 2019-05-20 | 2019-08-30 | 长江大学 | A kind of preparation method and applications of magnetic carbon nano-tube demulsifier |
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