CN114805914A - Magnetic nanofiber aerogel for thick oil separation - Google Patents

Magnetic nanofiber aerogel for thick oil separation Download PDF

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CN114805914A
CN114805914A CN202210544672.3A CN202210544672A CN114805914A CN 114805914 A CN114805914 A CN 114805914A CN 202210544672 A CN202210544672 A CN 202210544672A CN 114805914 A CN114805914 A CN 114805914A
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magnetic
aerogel
nanofiber
hydrophobic
thick oil
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CN114805914B (en
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王栋
武艺
徐桂林
刘轲
夏明�
程芹
徐佳
李青云
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Wuhan Textile University
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Abstract

The invention provides a magnetic nanofiber aerogel for thick oil separation, which is prepared by melting and blending magnetic particles and nanofibers, crosslinking the magnetic nanofiber aerogel with a crosslinking agent to obtain the magnetic nanofiber aerogel, and performing surface hydrophobic modification treatment on the magnetic nanofiber aerogel to obtain the super-hydrophobic magnetic nanofiber aerogel. The magnetic particles can be uniformly and effectively attached to the nanofibers by melting and blending the magnetic particles and the nanofibers, so that the magnetic particles are uniformly distributed in the finally prepared aerogel; by using the hydrophobic resin solution mixed with the hydrophobic particles to perform surface hydrophobic modification on the nanofiber aerogel, the hydrophobic particles can be attached to the surface of the aerogel by means of the viscosity of the hydrophobic resin solution, and meanwhile, the hydrophobic particles can be fixed on the surface of the aerogel as the hydrophobic resin solution is cured on the surface of the aerogel. Through the method, the magnetic particles in the prepared super-hydrophobic magnetic nanofiber aerogel are uniformly distributed and have uniform hydrophobicity.

Description

Magnetic nanofiber aerogel for thick oil separation
Technical Field
The invention relates to the technical field of oil-water separation materials, in particular to a magnetic nanofiber aerogel for thick oil separation.
Background
The aerogel is a porous material obtained by processing hydrogel by utilizing a freeze drying or supercritical carbon dioxide drying technology and replacing liquid in the hydrogel with gas, and has the network structure and volume characteristics of the hydrogel. The unique performance and the characteristic that the aerogel can be modified enable the aerogel to become an ideal base material of the functionalized composite material, and the magnetic nanofiber aerogel is the aerogel with magnetic performance. The method for imparting magnetism to the aerogel generally comprises a pretreatment mode of directly preparing the aerogel by using a mixture of a nanofiber solution and nano magnetic particles, and firstly preparing the aerogel and then modifying the nano magnetic particles on the aerogel. In the former method, aggregation of nano magnetic particles is easy to occur, so that the prepared aerogel has nonuniform magnetism, and the nano magnetic particles are easy to fall off from nano fibers, so that the function of the nano magnetic particles cannot be fully exerted; in the latter method, the aerogel may be treated several times, which may affect the structure of the aerogel, such as by collapsing the aerogel during the treatment process, and thus affect the properties of the magnetic aerogel.
In the prior art, chinese patent application No. 201410773097.X, publication date 2016, 7, 13 months, the invention patent named "a magnetic aerogel and its preparation method" discloses a magnetic aerogel and its preparation method, in the above technical scheme, through spraying the aerogel substrate with the solution containing magnetic ions evenly, until the aerogel substrate absorbs moisture and is saturated; removing the moisture of the aerogel base material after moisture absorption saturation by adopting a drying method, and ensuring that the aerogel base material is not completely dried; adsorbing the precipitation solution on the aerogel substrate until the aerogel substrate is completely soaked; and after the color of the aerogel substrate is not changed any more, washing with water, and drying to obtain the magnetic aerogel. Magnetic aerogel has been prepared with the help of the electrostatic force between magnetic ion and the aerogel substrate among the above-mentioned technical scheme, but the aerogel that above-mentioned method made is hydrophilic, is not suitable for the oil water separation field.
In the prior art, a super-hydrophobic magnetic mixture and a preparation method and application thereof are disclosed in an invention patent named as 'a super-hydrophobic magnetic mixture and a preparation method and application thereof' with Chinese patent application number 201910975905.3 and publication date of 2020, 1, 24 days, and the technical scheme utilizes CNF aqueous suspension, Fe aqueous suspension and Fe aqueous suspension 3 O 4 The aerogel is prepared by the method, and has hydrophobicity and magnetism, but the hydrophobic modifier in the finally prepared aerogel is not uniform due to the fact that the hydrophobic modifier is not mutually soluble with the nano CNF aqueous suspension, so that the hydrophobicity of the aerogel is not uniform; in addition, because the magnetic nanoparticles are not in the effect of chemical bonds with the CNF, the magnetic nanoparticles are only loaded on the CNF, and therefore the magnetic nanoparticles on the aerogel are usedThe seed is easy to fall off, and finally the magnetism of the aerogel is influenced.
In view of the above, there is a need to design an improved magnetic nanofiber aerogel for thick oil separation to solve the above problems.
Disclosure of Invention
The invention aims to provide a magnetic nanofiber aerogel for thick oil separation.
In order to achieve the above object, the present invention provides a magnetic nanofiber aerogel for thick oil separation, which is prepared by the following steps:
s1, melting and blending the magnetic particles and the nano fibers to prepare magnetic nano fibers;
s2, preparing the magnetic nanofiber prepared in the step S1 into a magnetic nanofiber suspension, uniformly mixing the magnetic nanofiber suspension with a cross-linking agent to obtain a mixture, pouring the mixture into a mold, pre-freezing and molding the mold containing the mixture at a low temperature, and then performing freeze drying treatment to obtain the magnetic particle doped nanofiber aerogel;
s3, soaking the magnetic particle doped nanofiber aerogel prepared in the step S2 in a modification solution for surface hydrophobic modification, and preparing the super-hydrophobic magnetic nanofiber aerogel.
Preferably, in step S3, the modifying solution is obtained by dissolving hydrophobic particles in a resin solution; preferably, the resin solution is prepared from a hydrophobic resin.
Preferably, in step S3, the resin solution is a solution of polydimethylsiloxane or epoxy resin, and the viscosity of the resin solution is 500 to 20000 cps.
Preferably, in step S3, the time for soaking the magnetic particle doped nanofiber aerogel in the modification solution is 10 to 30 min.
Preferably, in step S3, the hydrophobic particles are fumed silica-based substances.
Preferably, in step S1, the mass percentage of the added amount of the magnetic particles to the sum of the mass of the magnetic particles and the mass of the nanofibers is 3 to 8%; preferably, the magnetic particles are iron-based nanoparticles and a coating thereof.
Preferably, in step S1, the nanofiber is one of PVA-co-PE nanofiber, polyester fiber, and polylactic acid nanofiber.
Preferably, in step S2, the cross-linking agent is one of glutaraldehyde, dialdehyde, and polyvinylpyrrolidone, and the amount of the cross-linking agent is 0.5-1 g; the mass of the magnetic nanofiber suspension in the mixture is 50-100 g, and the magnetic nanofiber suspension is obtained by dispersing the magnetic nanofibers in water and isopropanol; preferably, the mass ratio of the magnetic nanofibers, water and isopropanol in the magnetic nanofiber suspension is 3:5: 5.
Preferably, in step S2, the freeze-drying process is performed for 24 to 72 hours.
Preferably, in step S2, the mixing is performed by mechanical stirring or ultrasonic treatment.
The invention has the beneficial effects that:
1. the magnetic nanofiber aerogel for thick oil separation provided by the invention is prepared by melting and blending magnetic particles and nanofibers, then crosslinking the magnetic nanofiber aerogel with a crosslinking agent to obtain the magnetic nanofiber aerogel, and then performing surface hydrophobic modification treatment on the magnetic nanofiber aerogel to obtain the super-hydrophobic magnetic nanofiber aerogel. Through the method, the magnetic particles in the prepared super-hydrophobic magnetic nanofiber aerogel are uniformly distributed and have uniform hydrophobicity.
2. According to the magnetic nanofiber aerogel for thick oil separation, the magnetic particles and the nanofibers are melted and blended, so that the magnetic particles can be uniformly and effectively attached to the nanofibers, and the magnetic particles can be uniformly distributed in the finally prepared aerogel; in addition, the magnetic particles can be coated by the nano-fiber, so that the magnetic particles and the nano-fiber are integrated, the magnetic particles and the nano-fiber can be effectively combined in such a way, the amount of the magnetic particles effectively attached to the nano-fiber is increased, meanwhile, the magnetic particles are prevented from falling off in the use process of the aerogel, the effect of the magnetic particles is effectively exerted, and the addition amount of the magnetic particles in the preparation process is reduced. The method has the advantages that the surface hydrophobic modification is carried out on the nanofiber aerogel by using the hydrophobic resin solution mixed with the hydrophobic particles, the hydrophobic particles can be attached to the surface of the nanofiber aerogel by means of the viscosity of the hydrophobic resin solution, meanwhile, the hydrophobic particles can be fixed on the surface of the aerogel along with the further solidification of the hydrophobic resin solution on the surface of the aerogel, furthermore, the hydrophobic modification treatment is carried out by using the hydrophobic resin and the hydrophobic particles simultaneously, the surface hydrophobic modification effect is better, in addition, the method also effectively avoids the blockage of the pore structure of the aerogel by the viscous resin solution by adjusting the viscosity of the resin solution and the time of the hydrophobic modification treatment. Through the aftertreatment mode of preparing the aerogel earlier and then carrying out hydrophobic modification treatment to the aerogel, effectively reduced the processing procedure to the aerogel, avoided producing the influence to the structure of aerogel in the preparation process for the magnetism nanofiber aerogel that finally makes still can keep the three-dimensional network structure that runs through of aerogel. Through the mode, the magnetic nanofiber aerogel with uniformly distributed internal magnetic particles and super-hydrophobicity can be prepared under the condition that toxic hydrophobic substances are not used, and when the aerogel is applied to thick oil separation, the result shows that the magnetic nanofiber aerogel prepared by the method has an excellent separation effect on the thick oil.
Drawings
FIG. 1 is a flow chart of the preparation process of the magnetic nanofiber aerogel for thick oil separation according to the present invention;
FIG. 2 is an optical photograph of the process of separating thick oil using magnetic nanofiber aerogel in example 1 of the present invention under magnetic heating and without magnetic heating.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be described in detail with reference to the accompanying drawings and specific embodiments.
It should be noted that, in order to avoid obscuring the present invention with unnecessary details, only the structures and/or processing steps closely related to the aspects of the present invention are shown in the drawings, and other details not closely related to the present invention are omitted.
In addition, it is also to be noted that the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
Referring to fig. 1, the present invention provides a magnetic nanofiber aerogel for thick oil separation, which is prepared by first melting and blending magnetic particles and nanofibers, then adding a cross-linking agent to perform cross-linking to obtain a magnetic nanofiber aerogel, and then performing surface hydrophobic modification treatment to obtain a superhydrophobic magnetic nanofiber aerogel, including the following steps:
s1, melting and blending the magnetic particles and the nano fibers to obtain magnetic nano fibers;
s2, preparing the magnetic nanofiber prepared in the step S1 into magnetic nanofiber suspension, uniformly mixing the suspension with a cross-linking agent to obtain a mixture, pouring the mixture into a mold, pre-freezing and molding the mold at a low temperature, and then performing freeze drying treatment to obtain magnetic particle doped nanofiber aerogel;
s3, soaking the magnetic particle doped nanofiber aerogel obtained in the step S2 in a modification solution for surface hydrophobic modification, and obtaining the super-hydrophobic magnetic nanofiber aerogel.
Preferably, in step S1, the nanofiber is one of PVA-co-PE (ethylene/vinyl alcohol copolymer) nanofiber, polyester fiber, and polylactic acid nanofiber.
Preferably, in step S1, the magnetic particles are iron-based nanoparticles and a coating thereof, and the mass percentage of the amount of the magnetic particles added to the total mass of the magnetic particles and the nanofibers is 3 to 8%.
Preferably, in step S2, the crosslinking agent is one of glutaraldehyde, dialdehyde, and polyvinylpyrrolidone, and the amount of the crosslinking agent is 0.5-1 g.
Preferably, in step S2, the mass of the magnetic nanofiber suspension in the mixture is 50-100 g, wherein the magnetic nanofiber suspension is obtained by dispersing the magnetic nanofibers in water and isopropanol, and the mass ratio of the magnetic nanofibers to the water to the isopropanol is 3:5: 5.
Preferably, in step S2, the manner of mixing uniformly is mechanical stirring or ultrasonic treatment.
Preferably, in step S2, the drying time is 24 to 72 hours.
Preferably, in step S3, the modified solution is obtained by dissolving hydrophobic particles in a hydrophobic resin solution, the hydrophobic particles are fumed silica, the hydrophobic resin solution is polydimethylsiloxane or epoxy resin, the viscosity of the hydrophobic resin solution is 500 to 20000cps, and the soaking time is 10 to 30 min; it will be understood by those skilled in the art that the surface hydrophobic modification of the aerogel can be performed by chemical vapor deposition or surface spraying other than soaking, and is not limited thereto.
The invention is further defined by reference to the following specific examples:
example 1
S1, melting and blending 5g of ferroferric oxide and 95g of PVA-co-PE nano fiber to prepare the magnetic nano fiber, wherein the mass percentage of the addition amount of the magnetic particles to the total mass of the magnetic particles and the nano fiber is 5%;
s2, preparing the magnetic nanofiber prepared in the step S1 into magnetic nanofiber suspension under the condition of magnetic stirring, uniformly mixing 5g of the magnetic nanofiber suspension with 0.5g of glutaraldehyde to obtain a mixture, pouring the mixture into a mold, pre-freezing and molding the mold by using liquid nitrogen, putting the pre-frozen and molded mold into a pre-cooled freeze dryer, and freeze-drying for 48 hours to obtain the ferroferric oxide doped PVA-co-PE nanofiber aerogel, wherein the magnetic nanofiber suspension is obtained by dispersing the magnetic nanofiber in water and isopropanol, and the mass ratio of the magnetic nanofiber to the water to the isopropanol is 3:5: 5.
S3, soaking the ferroferric oxide-doped PVA-co-PE nano-fiber aerogel obtained in the step S2 in 5% of polydimethylsiloxane resin solution dispersed with fumed silica by mass percent for surface hydrophobic modification, wherein the viscosity of the resin solution is 5000cps, the soaking time is 15min, and finally the super-hydrophobic magnetic nano-fiber aerogel is prepared.
In order to verify the adsorption effect of the magnetic nanofiber aerogel prepared by the invention on thick oil, the magnetic nanofiber aerogel subjected to magnetic heating treatment is used for thick oil separation, and is compared with the magnetic nanofiber aerogel not subjected to magnetic heating treatment, the thick oil separation result of the magnetic nanofiber aerogel subjected to magnetic heating treatment is shown in fig. 2b, the thick oil separation result of the magnetic nanofiber aerogel not subjected to magnetic heating treatment is shown in fig. 2a, it can be seen from the figure that the adsorption effect of the aerogel subjected to magnetic heating treatment on thick oil is obviously superior to that of the aerogel not subjected to magnetic heating treatment, because the aerogel subjected to magnetic heating treatment has higher temperature, when the thick oil is contacted, the viscosity of the thick oil is reduced, the thick oil has fluidity and is easier to be adsorbed by the aerogel, and the aerogel not subjected to magnetic heating treatment can only adsorb part of the thick oil by utilizing the self gap structure, and thus the adsorption effect is inferior to the former.
Comparative example 1
Comparative example 1 differs from example 1 only in that: the magnetic particles, the PVA-co-PE nano fibers and the glutaraldehyde are uniformly mixed to obtain a mixture, then the mixture is injected into a mold for pre-freezing molding, other steps are basically the same as those in the embodiment 1, and the details are not repeated. As a result of using the superhydrophobic magnetic nanofiber aerogel prepared in comparative example 1 to separate thick oil, it was found that the superhydrophobic magnetic nanofiber aerogel prepared in example 1 has a better separation effect on thick oil because the distribution of the magnetic particles in the superhydrophobic magnetic nanofiber aerogel prepared in example 1 is more uniform and the amount of the magnetic particles effectively attached to the nanofibers is more.
The following explains the formation mechanism of magnetic nanofiber aerogel for thick oil separation:
the PVA-co-PE nano-fiber and the magnetic particles are melted and blended to prepare the magnetic nano-fiber, so that the magnetic particles can be uniformly distributed in the finally prepared aerogel on the one hand; on the other hand, since there is usually no chemical bond between the magnetic particles and the nanofibers, the magnetic particles can only be loaded on the nanofibers, and at this time, the magnetic particles and the nanofibers are still independent entities, but in the present invention, the magnetic particles and the nanofibers can be integrated into one entity because the nanofibers can coat the magnetic particles, so that the strength of the aerogel obtained in this way is stronger than that of the aerogel obtained by directly loading the magnetic particles on the nanofibers. And then, crosslinking the magnetic nanofiber solution and a crosslinking agent to prepare the magnetic nanofiber aerogel, wherein the PVA-co-PE nanofiber has rich hydroxyl groups on the surface, so that the PVA-co-PE nanofiber can perform aldol condensation reaction with aldehyde groups on the surface of glutaraldehyde to form the nanofiber aerogel with a three-dimensional through network structure. Finally, performing hydrophobic treatment on the magnetic nanofiber aerogel by using a resin solution mixed with hydrophobic particles, wherein the hydrophobic particles can be attached to the surface of the nanofiber aerogel due to certain viscosity of the resin solution, and the hydrophobic particles can be fixed on the surface of the nanofiber aerogel along with the further solidification of the resin solution on the surface of the nanofiber aerogel; on the other hand, the hydrophobic resin solution and the hydrophobic particles modify the surface of the aerogel together, so that the effect of surface hydrophobic treatment is ensured. When the super-hydrophobic magnetic nanofiber aerogel prepared by the method is in a magnetic heating environment, under the action of a magnetic effect, the temperature of the nanofiber aerogel can be rapidly raised, when thick oil is contacted with the raised aerogel, the viscosity of the thick oil around the aerogel can be gradually reduced to form fluid with fluidity, and meanwhile, the thick oil is selectively adsorbed by the aerogel due to the super-hydrophobic characteristic of the aerogel, so that the purpose of separating the thick oil in a thick oil/water mixture is achieved.
In summary, the magnetic nanofiber aerogel for thick oil separation provided by the invention is prepared by melting and blending magnetic particles and nanofibers, then crosslinking the magnetic particles and the nanofibers with a crosslinking agent to obtain the magnetic nanofiber aerogel, and then performing surface hydrophobic modification treatment on the magnetic nanofiber aerogel to obtain the magnetic nanofiber aerogel with super-hydrophobicity. The magnetic particles can be uniformly and effectively attached to the nanofibers by melting and blending the magnetic particles and the nanofibers, so that the magnetic particles can be uniformly distributed in the finally prepared aerogel; by utilizing the hydrophobic resin solution mixed with the hydrophobic particles to carry out surface hydrophobic modification on the nanofiber aerogel, the hydrophobic particles can be attached to the surface of the nanofiber aerogel by means of the viscosity of the hydrophobic resin solution, and meanwhile, the hydrophobic particles can be fixed on the surface of the nanofiber aerogel as the hydrophobic resin solution is further solidified on the surface of the nanofiber aerogel. Through the mode, the magnetic nanofiber aerogel with the uniformly distributed internal magnetic particles and the super-hydrophobicity can be prepared under the condition that toxic hydrophobic substances are not used.
Although the present invention has been described in detail with reference to the preferred embodiments, it will be understood by those skilled in the art that various changes may be made and equivalents may be substituted for elements thereof without departing from the spirit and scope of the present invention.

Claims (10)

1. A magnetic nanofiber aerogel for thick oil separation is prepared by the following steps:
s1, melting and blending the magnetic particles and the nano fibers to prepare magnetic nano fibers;
s2, preparing the magnetic nanofiber prepared in the step S1 into a magnetic nanofiber suspension, uniformly mixing the magnetic nanofiber suspension with a cross-linking agent to obtain a mixture, pouring the mixture into a mold, pre-freezing and molding the mold containing the mixture at a low temperature, and then performing freeze drying treatment to obtain the magnetic particle doped nanofiber aerogel;
s3, soaking the magnetic particle doped nanofiber aerogel prepared in the step S2 in a modification solution for surface hydrophobic modification, and preparing the super-hydrophobic magnetic nanofiber aerogel.
2. The magnetic nanofiber aerogel for thick oil separation as claimed in claim 1, wherein in step S3, the modifying solution is obtained by dissolving hydrophobic particles in a resin solution; preferably, the resin solution is prepared from a hydrophobic resin.
3. The magnetic nanofiber aerogel for thick oil separation as claimed in claim 2, wherein in the step S3, the resin solution is a solution of polydimethylsiloxane or epoxy resin, and the viscosity of the resin solution is 500-20000 cps.
4. The magnetic nanofiber aerogel for thick oil separation as claimed in claim 2, wherein in the step S3, the time for soaking the magnetic particle doped nanofiber aerogel in the modification solution is 10-30 min.
5. The magnetic nanofiber aerogel for thick oil separation as claimed in claim 2, wherein in step S3, the hydrophobic particles are fumed silica type substances.
6. The magnetic nanofiber aerogel for thick oil separation as claimed in claim 1, wherein in step S1, the mass percentage of the added amount of the magnetic particles to the sum of the mass of the magnetic particles and the mass of the nanofibers is 3-8%; preferably, the magnetic particles are iron-based nanoparticles and a coating thereof.
7. The magnetic nanofiber aerogel for thick oil separation as claimed in claim 1, wherein in step S1, the nanofibers are one of PVA-co-PE nanofibers, polyester fibers, and polylactic acid nanofibers.
8. The magnetic nanofiber aerogel for thick oil separation as claimed in claim 1, wherein in step S2, the cross-linking agent is one of glutaraldehyde, dialdehyde, and polyvinylpyrrolidone, and the amount of the cross-linking agent is 0.5-1 g; the mass of the magnetic nanofiber suspension in the mixture is 50-100 g, and the magnetic nanofiber suspension is obtained by dispersing the magnetic nanofibers in water and isopropanol; preferably, the mass ratio of the magnetic nanofibers, water and isopropanol in the magnetic nanofiber suspension is 3:5: 5.
9. The magnetic nanofiber aerogel for thick oil separation as claimed in claim 1, wherein in the step S2, the freeze-drying treatment time is 24-72 h.
10. The magnetic nanofiber aerogel for thick oil separation as claimed in claim 1, wherein in step S2, the mixing is performed by mechanical stirring or ultrasonic treatment.
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