AU2020103898A4 - Method for Preparation Magnetic Porous Materials - Google Patents
Method for Preparation Magnetic Porous Materials Download PDFInfo
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- AU2020103898A4 AU2020103898A4 AU2020103898A AU2020103898A AU2020103898A4 AU 2020103898 A4 AU2020103898 A4 AU 2020103898A4 AU 2020103898 A AU2020103898 A AU 2020103898A AU 2020103898 A AU2020103898 A AU 2020103898A AU 2020103898 A4 AU2020103898 A4 AU 2020103898A4
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- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 claims description 3
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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 description 1
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Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/06—Silicon, titanium, zirconium or hafnium; Oxides or hydroxides thereof
- B01J21/063—Titanium; Oxides or hydroxides thereof
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/74—Iron group metals
- B01J23/745—Iron
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/74—Iron group metals
- B01J23/755—Nickel
-
- B01J35/19—
-
- B01J35/33—
-
- B01J35/39—
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- B01J35/60—
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/02—Impregnation, coating or precipitation
- B01J37/03—Precipitation; Co-precipitation
- B01J37/036—Precipitation; Co-precipitation to form a gel or a cogel
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/0004—Preparation of sols
- B01J13/0047—Preparation of sols containing a metal oxide
Abstract
The invention discloses a method for preparing magnetic porous material, in which a
magnetic, modified hydrophobic NiFe204 and hydrophilic TiO2 are used as stabilizers,
NiFe204 is prepared by solvent thermal method, TiO2 is prepared by sol-gel method, then
W/O/W multiple Pickering emulsion is prepared by sol-gel method; and a composite magnetic
catalyst TiO2/PS/NiFe24 is prepared by multiple Pickering emulsion polymerization. The
inner and outer layer of colloidal particles are fixed by polystyrene in this invention; the inner
layer NiFe204 serves as a magnetic medium, and the outer layer TiO2 acts as a catalyst; the
TiO2 is coated in the outer layer, which greatly reduces the influence of polystyrene on its
catalytic performance. Polystyrene is widely used in optical and chemical instrument parts,
transparent film and capacitor dielectric layer because of its excellent electrical properties, high
frequency characteristics and radiation resistance.
-1/3
A magnetic, modified hydrophobic NiFe204 and hydrophilic TiO 2 are used
as stabilizers, NiFe204 is prepared by solvent thermal method, TiO 2 is
prepared by sol-gel method, then W/O/W multiple Pickering emulsion is
prepared by sol-gel method.
4102
Preparation of TiO 2/PS/ NiFe204 composite magnetic catalyst by multiple
Pickering emulsion polymerization
Figure 1
Description
-1/3
A magnetic, modified hydrophobic NiFe 204 and hydrophilic TiO 2 are used as stabilizers, NiFe 204 is prepared by solvent thermal method, TiO 2 is prepared by sol-gel method, then W/O/W multiple Pickering emulsion is prepared by sol-gel method.
4102 Preparation of TiO 2/PS/ NiFe 2 04 composite magnetic catalyst by multiple Pickering emulsion polymerization
Figure 1
Method for Preparation Magnetic Porous Materials
The invention belongs to the field of polymer technology, in particular to a method for preparing magnetic porous material.
With the increasing demand for structural properties of materials, researchers have increased their research on the preparation methods, microstructure and properties of materials, and tried to improve the properties of materials by changing the microstructure of materials and by combining inorganic-organic materials. Because of the regular arrangement of pore structure, adjustable size, high specific surface area and large adsorption capacity, porous materials have been developed into one of the research fields attracting much attention. According to the regulations of International Union of Pure and Applied Chemistry, pore sizes can be divided into three categories: micropores (less than 2 nm), mesopores (2-50 nm), and macropores (greater than 50 nm). The preparation methods of porous materials include template method, gas foaming method, phase separation method, solvent-induced porosity method, etc. The emulsion template method in template method can realize the pre control of porous material structure by changing the type and size of emulsion template, so it has become a research hotspot and made some achievements. However, most of the template used at present is single emulsion template, in which single emulsion droplet is used as template, polymerization is carried out on the surface of droplet at a certain temperature, and the porous polymer material is obtained by washing and drying after the polymerization. The porous materials prepared by this method mainly comprise: oil-in-water (W/O) emulsion system method, water-in-oil (O/W) emulsion system method and supercritical C0 2 (C/W) method. Since the single emulsion has only one oil-water interface, it is impossible to realize the controlled recombination of inorganic particles with two different functions. Therefore, the preparation of porous materials by multi-emulsion polymerization is considered.
Multiple emulsion is a kind of emulsion (i. e. colostrum) dispersed in another multi-emulsion formed in a continuous phase, commonly W/O/W and O/W/O, which usually take the emulsifier with amphiphilic as a stabilizer, prepared by one-step or two-step method, wherein the one-step method is to form multiple emulsions by emulsifying water phase, oil phase, lipophilic and hydrophilic emulsifier at the same time, and the two-step method is to prepare W/O (or O/W) colostrum and then add it to water phase ( or oil phase) to obtain W//W (or O/W/O) multi-emulsion. The one step method is simpler and less energy consumption, but the ratio of internal and external water phase and the distribution of active substance are difficult to control, so the two-step method is a more common preparation method.
The common emulsifiers include surfactants (such as SDS, CTAB, SPAN-80, etc.) and surface active polymers (such as proteins and polysaccharides, etc.). However, the multi-solutions prepared with these two emulsifiers have some disadvantages such as poor stability, high dosage of emulsifiers and high toxicity. In recent years, the use of colloidal particles instead of traditional emulsifiers to prepare different particle-stabilized emulsions (also known as Pickering emulsions) has attracted much attention. Compared with traditional emulsion, Pickering emulsion has the following advantages:
(1) good emulsifying effect, less dosage, low cost; (2) less toxicity than organic surfactants; (3) strong emulsion stability, not easily affected by environmental temperature; (4) separation is convenient or need not be separated, convenient for industrial production. Multiple Pickering Emulsion has a unique "two-film three phase" multi-compartment structure. If different particles can be stabilized on different membrane layers, porous materials with different functions on both sides of the hole can be prepared.
However, there are few researches in this field at present. The inorganic particles prepared by different methods have different lipophilic and hydrophilic properties. The lipophilic particles are easy to prepare oil-in-water W/O emulsion system, the hydrophilic particles are easy to prepare water-in-oil (O/W) emulsion system, and the multiple Pickering emulsion is W/O/W (or O/W/O). Therefore, the lipophilic and hydrophilic properties of the two inorganic particles will not be matched, otherwise, the lipophilic and hydrophilic properties of the two inorganic particles will not be matched; at the same time the inorganic particles prepared may not form stable colostrum and multiple emulsions, and need suitable hydrophobic or lipophilic modification. In addition, there are many factors affecting the preparation of multiple Pickering emulsion, such as particle size, oil/water ratio, pH value and so on.
In a word, it is difficult to match the multiple and hydrophilic properties of the two kinds of inorganic particles in the preparation of porous materials, and the prepared inorganic particles can not form stable colostrum and multiple emulsion; moreover, there is no polymerization after the preparation of multiple emulsions, and the prepared porous materials have a single function.
The invention aims at providing a method for preparing magnetic porous material, aiming at solving the problems that the lipophilic and hydrophilic properties of two kinds of inorganic particles in the preparation method of porous materials are difficult to match, and the prepared inorganic particles can not form stable colostrum and multiple emulsion; moreover, there is no polymerization after the preparation of multiple emulsions, and the prepared porous materials have a single function.
The invention relates to a method for preparing magnetic porous material, which comprises:
A magnetic, modified hydrophobic NiFe204 and hydrophilic TiO2 are used as stabilizers, NiFe204 is prepared by solvent thermal method, TiO2 is prepared by sol gel method, then W/O/W multiple Pickering emulsion is prepared by sol-gel method;
A composite magnetic catalyst TiO2/PS/NiFe2O4 is prepared by multiple Pickering emulsion polymerizationFurther, the preparation of NiFe204 by solvent thermal method comprises:
Dissolve 0.5g~Ig Ni (N03) 2 - 6 H20 and 1.5g2.5g Fe(N03) 3 - 9 H20 in about mL anhydrous alcohol, stir and transfer it to PTFE autoclave to react at 200 °C for 8 hours-10 hours, form red-brown precipitation, centrifugally separate and obtain NiFe204 solid powder.
1.5g-2.5g NiFe204 is dispersed into a proper amount of water, 50% sodium pyrophosphate is added and dispersed at 75 °C for 30 minutes, the pH is adjusted to 7 ~ 8, then 6% CTAB is added to continue stirring for 1.5 h, centrifugally separate, and the deionized water is used for washing for three times, and the surface modified NiFe204 is obtained after being dried.
Further, the preparation of TiO2by sol-gel method comprises:
The 18 ml~25 ml anhydrous alcohol and a certain amount of tetrabutyl titanate are dispersed by ultrasonic for 30 min, and then 2-3 ml H20, 0.1-05 ml concentrated HCl and 18-25 mL anhydrous alcohol are added to form sol, aging to get wet gel; drying, grinding, and roasting the wet gel to obtain TiO2.
Further, the preparation method of W/O/W multiple Pickering emulsion comprises:
50 mg-100 mg modified NiFe204 is dispersed by ultrasonic in 5 mL-10 mL toluene, and 3 mL-6 mL distilled water is added and stirred fully to obtain the W/O colostrum 10 minutes later.
100-150mg TiO2 is dispersed in 8-10mL water and continually dispersed by ultrasonic for 10min. 6-9mL W/O colostrum is added to the TiO2 solution dispersed by ultrasonic and W/O/W Pickering emulsion is obtained after being stirred.
Further, the method for preparing TiO2/PS/NiFe2O4 composite magnetic catalyst by multiple Pickering emulsion polymerization comprises:
280-320 mg TiO2 is dispersed in 10 mg-15 mL water, and continually dispersed by ultrasonic for 5 minutes, marked as dispersed phase.
3mL-5mL W/O colostrum is taken, and then added 0.5mL-mL styrene; the solution is stirred evenly to add into the dispersed phase; the dispersed phase is stirred to obtain the emulsion whose oil phase is the W//W Pickering emulsion containing styrene monomer; the emulsion is polymerized at room temperature for 12h, centrifugally separated, and then washed by deionized water and anhydrous alcohol separately with each for three times to obtain the TiO2/PS/NiFe2O4 composite porous magnetic catalyst; that is, magnetic porous material.
Another purpose of the invention is to provide a nano-sized hybrid superstructure microsphere material prepared by the above-mentioned method for preparing magnetic porous material.
Another purpose of the invention is to provide a micron-sized hybrid superstructure microsphere material prepared by the above-mentioned method for preparing magnetic porous material.
The invention provides a method for preparing magnetic porous material, in which added NiFe204 can be effectively recovered under an applied magnetic field, and the recovery rate is 98%. The inner and outer layer of colloidal particles are fixed by polystyrene in this invention; the inner layer NiFe204 serves as a magnetic medium, and the outer layer TiO2 acts as a catalyst; the methylene blue is used as a substrate, and the degradation efficiency can reach 93.8% after 160 minutes under the ultraviolet lamp; the magnetic porous material prepared by the invention cleverly melts magnetic and catalytic properties into one body; the inner layer NiFe204 acts as a magnetic medium, facilitating the recovery of the catalyst under the action of an external magnetic field, and the outer layer TiO2 acts as a catalyst. The TiO2 of the invention is coated in the outer layer as the catalytic activity center, which reduces the coverage of the polystyrene to the active center to the greatest extent, and reduces the influence on the catalytic performance of the polystyrene. Polystyrene is widely used in optical and chemical instrument parts, transparent film and capacitor dielectric layer because of its excellent electrical properties, high frequency characteristics and radiation resistance.
Figure 1 is a flowchart of a method for preparing magnetic porous material provided by an embodiment of the invention.
Figure 2 is a hysteresis loop diagram of NiFe204 provided by the embodiment of the invention.
Figure 3 is a diagram of (A) 0.8 mL, (B) 0.6 mL, (C) 0.4 mL, (D) 0.2 mL styrene dosage and photocatalytic degradation rate provided by the embodiment of the invention.
In order that the purpose, technical scheme and advantages of the invention will become more apparent, the invention will be described in further detail below with reference to the following embodiments. It is to be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The polymer microsphere material with hybrid superstructure is prepared based on the polymerization technology of Pickering emulsion. The microsphere prepared by the invention has the superparticle structure with inorganic particles as shell layer, and can endow the microsphere with unique functions. The colloidal particles self assemble on the surface of the droplet to form an ordered spherical colloidal shell and immobilize the colloidal particles on the surface of the droplet to prepare the core shell microcapsules. The colloidal particles self-assembled on the oil-water interface are used to protect the stability of the emulsion instead of surfactants during the polymerization process, and then remained on the surface of the obtained polymer microspheres after the reaction, as the raw material for the construction of inorganic/organic complexes. Polymerization technology of Pickering emulsion can be used in dispersion polymerization, microemulsion polymerization and suspension polymerization to prepare hybrid superstructure microspheres from nano-sized to micron-sized effectively.The application principle of the invention is explained in detail with the figures below.
As shown in Figure 1, the method for preparing magnetic porous materials provided by embodiments of the invention comprises:
S101: A magnetic, modified hydrophobic NiFe204 and hydrophilic TiO2 are used as stabilizers, NiFe204 is prepared by solvent thermal method, TiO2 is prepared by sol-gel method, then W/O/W multiple Pickering emulsion is prepared by sol-gel method;
S102: A composite magnetic catalyst TiO2/PS/NiFe2O4 is prepared by multiple Pickering emulsion polymerization.
The application principle of the invention is further described with experiments.
1. Experimental section
1.1 Preparation and modification of NiFe204 by solvent thermal method
Dissolve 0.5863g Ni(N3)2-6 H20 and 1.6289g Fe(N03)3-9 H20 in about 48mL anhydrous alcohol, stir and transfer it to PTFE autoclave to react at 200 °C for 10 hours, form red-brown precipitation, centrifugally separate and obtain NiFe204 solid powder.
2g NiFe204 is dispersed into a proper amount of water, 50% sodium pyrophosphate is added and dispersed at 75 °C for 30 minutes, the pH is adjusted to 7 ~ 8, then 6% CTAB is added to continue stirring for 1.5 h, centrifugally separate, and the deionized water is used for washing for three times, and the surface modified NiFe204 is obtained after being dried.
1.2 Preparation of TiO2 by sol-gel method
The 20 ml anhydrous alcohol and a certain amount of tetrabutyl titanate are
dispersed by ultrasonic for 30 min, and then 1.5 ml H20, 0.1 ml concentrated HCl and mL anhydrous alcohol are added to form sol, aging to get wet gel; drying, grinding, and roasting the wet gel to obtain TiO2.
1.3 Preparation of 1.3W/O/W multiple Pickering emulsion
60 mg modified NiFe204 is dispersed by ultrasonic in 4 mL toluene, and 3 mL distilled water is added and stirred fully to obtain the W/O colostrum 10 minutes later. 120mg TiO2 is dispersed in 6mL water, and continue to disperse by ultrasonic for min; 4mL colostrum is added, and W/O/W Pickering emulsion is obtained after being stirred.
1.4 Preparation of TiO2/PS/ NiFe204 composite magnetic catalyst by multiple emulsion polymerization
300 mg TiO2 is dispersed in 12 mL water and 4 mL HC with concentration of lmol/mL is added to continue to disperse by ultrasonic for 5 min; 3 mL colostrum is taken, and 0.6 mL styrene it is added to the colostrum; stir the colostrum evenly to add to dispersed phase, and shake to obtain the emulsion whose oil phase is W/O/W Pickering emulsion containing styrene monomer; the emulsion is polymerized at room temperature for 12h, centrifugally separated, and then washed by deionized water and anhydrous alcohol separately with each for three times to obtain the Ti2/PS/NiFe2O4 composite porous magnetic catalyst;
1.5 Photocatalytic degradation of methylene blue
The photocatalytic reaction is carried out in a self-made photocatalytic reactor, which is a wooden dark box device with high pressure mercury lamp and sodium lamp as its light source. The light source is located directly above the reactor and the center of luminescence and liquid layer is about 10cm. Accurately prepare methylene blue solution, take 250 mL the methylene blue solution into beaker, add catalyst powder (catalyst dosage rate:1: 10), place beaker on mechanical mixer, stir in dark state for 30 min, take a small amount of this liquid to centrifuge for 10 min, measure the absorbency of the solution and record the data as CO; turn on UV lamp and start stir at the same time, measure the absorbance every 20 minutes and record the data as Ct; repeat the above operation under UV lamp.
2. Results and discussion
2.1 STRUCTURE DETERMINATION OF STABILIZED PARTICLE
According to the XRD spectrum of NiFe204, the sample keeps the structure of NiFe204 spinel completely. Through the XRD spectrum of TiO2, TiO2 is concluded to be a mixed crystal structure. The XRD test results show that the prepared solid particles are the target products.
In addition, the NiFe204 magnetic performance test in Figure 2 show that the prepared NiFe204 particles have good paramagnetism, and its saturation magnetization is 10.8 emu - g-1 and coercivity is 105.820e, which is a soft magnetic material. This material is characterized by high permeability and high magnetization, which ensures the strong magnetic responsiveness of the particles and the emulsion prepared later.
2.2 Micromorphology of stable particles
By SEM images of NiFe204, the morphology of NiFe204 is seen to be regular, the particle distribution is uniform and the particle size is about 140nm. By SEM images of TiO2, the morphology of TiO2 is seen to be regular, the particle distribution is uniform, and the size of TiO2 is about 75nm, which is similar to spherical particles. The particle distributions of the two prepared samples are uniform, which provides a reliable condition for preparing a stable and uniform Pickering emulsion.
2. Hydrophobic modification of NiFe204
The stable W/O Pickering emulsion is prepared by direct precipitation of NiFe204 particles, and the surface of the emulsion is modified by CTAB.
Before modification, there are two absorption peaks at 1047cm-1 and 595cm-1. This is because each 02- is shared by one tetrahedral cation and three octahedral cations in spinel ferrate molecules, so all vibration of 02- is related to both tetrahedron and octahedron. The absorption peak at 1047cm-i is the vibration of Ni 2 +-02- bond in tetrahedron and that at 595cm-i is the vibration of Fe*-02- bond in octahedron.
The symmetric stretching vibration peaks of methyl-CH3 and methylene-CH2 at 2915 cm-1 and 2843 cm-1 of NiFe204 modified by CTAB showed that the surface of NiFe204 is already bonded with organic groups, and the organic modification of NiFe204 is realized.
At the same time, the Zeta potential of the unmodified NiFe204 is measured before and after modification, and the surface potential of the unmodified potential is about zero.
After modification with CTAB, the surface of NiFe204 is introduced into organic group, the surface potential of NiFe204 is raised to about 12.5 mV, and the potential value of the particles is small, which showed that the particles are hydrophobic and suitable for making oil-in-water emulsion, which is consistent with the experimental phenomena and proved to be successful.
2.4 Preparation of multiple Pickering emulsion
A good multiple emulsion can be obtained by re-emulsification of colostrum with different water-oil ratio. Many small droplets are contained in these multiple emulsion droplets. The double emulsion is prepared by hand shake, so the structure of colostrum can be maintained basically. The size and density of droplet wrapped in the multiple emulsion are basically the same as that of colostrum.
2.5 Morphology and photocatalytic properties of porous materials
When polymerizing multiple Pickering emulsion prepared by two-step method, other conditions are kept unchanged, the amount of styrene monomer is changed, and its photocatalytic properties are measured.
Figure 3 is a photocatalytic degradation curve of (A) 0.8 mL, (B) 0.6 mL, (C) 0.4 mL, (D) 0.2 mL styrene polymer provided by embodiments of the invention; it can be seen from Figure 3 that the photocatalytic performance of the polymer monomer decreases when the dosage of styrene monomer increases, mainly due to the polymerization of styrene on the surface of TiO2, resulting in the reduction of the photochemical reaction site. But when the amount of styrene monomer is reduced, the structure of the composite material can not be supported well. The results show that when the dosage of styrene is 0.8 mL, the photocatalytic performance is well and the structure can be insured.
The foregoing is to be considered as preferred embodiments of the invention and is not intended to limit the invention, and any modifications, equivalents, and alternatives falling within the spirit and principles of the invention are intended to be included within the scope of the invention.
Claims (10)
1. A method for preparing magnetic porous material is characterized by comprising:
A magnetic, modified hydrophobic NiFe204 and hydrophilic TiO2 are used as stabilizers, NiFe204 is prepared by solvent thermal method, TiO2 is prepared by sol gel method, then W/O/W multiple Pickering emulsion is prepared by sol-gel method;
A composite magnetic catalyst TiO2/PS/NiFe2O4 is prepared by multiple Pickering emulsion polymerization
2. The method for preparing magnetic porous material according to claim 1, is characterized in that the preparation of NiFe204 by solvent thermal method comprises:
Dissolve 0.5g-g Ni (N03) 2 - 6 H20 and 1.5g~2.5g Fe(N03) 3 - 9 H20 in about mL anhydrous alcohol, stir and transfer it to PTFE autoclave to react at 200 °C for 8 hours~10 hours, form red-brown precipitation, centrifugally separate and obtain NiFe204 solid powder.
1.5g~2.5g NiFe204 is dispersed into a proper amount of water, 50% sodium pyrophosphate is added and dispersed at 75 °C for 30 minutes, the pH is adjusted to 7 ~ 8, then 6% CTAB is added to continue stirring for 1.5 h, centrifugally separate, and the deionized water is used for washing for three times, and the surface modified NiFe204 is obtained after being dried.
3. The method for preparing magnetic porous material, according to in claim 1 is characterized in that the preparation of TiO2 by sol-gel method comprises:
The 18 ml~25 ml anhydrous alcohol and a certain amount of tetrabutyl titanate are dispersed by ultrasonic for 30 min, and then 2~3 ml H20, 0.1~05 ml concentrated HCl and 18~25 mL anhydrous alcohol are added to form sol, aging to get wet gel; drying, grinding, and roasting the wet gel to obtain TiO2.
4. The method for preparing magnetic porous material according to claim 1 is characterized in that the preparation of W/O/W multiple Pickering emulsion comprises the following steps:
50 mg-100 mg modified NiFe204 is dispersed by ultrasonic in 5 mL~10 mL toluene, and 3 mL~6 mL distilled water is added and stirred fully to obtain the W/O colostrum 10 minutes later.
100-150mg TiO2 is dispersed in 8~10mL water and continually dispersed by ultrasonic for 10min. 6~9mL W/O colostrum is added to the TiO2 solution dispersed by ultrasonic and W/O/W Pickering emulsion is obtained after being stirred.
5. The method for preparing magnetic porous material according to claim 1 is characterized in that the preparation of TiO2/PS/NiFe2O4 composite magnetic catalyst by multiple Pickering emulsion polymerization comprises:
280~320 mg TiO2 is dispersed in 10 mg-15 mL water, and continually dispersed by ultrasonic for 5 minutes, marked as dispersed phase.
3mL~5mL W/O colostrum is taken, and then added 0.5mL~1mL styrene; the solution is stirred evenly to add into the dispersed phase; the dispersed phase is stirred to obtain the emulsion whose oil phase is the W//W Pickering emulsion containing styrene monomer; the emulsion is polymerized at room temperature for 12h, centrifugally separated, and then washed by deionized water and anhydrous alcohol separately with each for three times to obtain the TiO2/PS/NiFe2O4 composite porous magnetic catalyst.
6. A nano-sized hybrid superstructure microsphere material prepared by any of the methods for preparing magnetic porous material described in claim 1 to 5.
7. A micron-sized hybrid superstructure microsphere material prepared by any of the methods for preparing magnetic porous material described in claim 1 to 5.
8. An optical and chemical instrument parts prepared by any of the methods for preparing magnetic porous material described in claim 1 to 5.
9. A transparent film prepared by any of the methods for preparing magnetic porous material described in claim 1 to 5.
10. A dielectric layer for capacitors prepared by any of the methods for preparing magnetic porous material described in claim 1 to 5.
-1/3- 04 Dec 2020
A magnetic, modified hydrophobic NiFe2O4 and hydrophilic TiO2 are used as stabilizers, NiFe2O4 is prepared by solvent thermal method, TiO2 is prepared by sol-gel method, then W/O/W multiple Pickering emulsion is prepared by sol-gel method.
Preparation of TiO2/PS/ NiFe2O4 composite magnetic catalyst by multiple 2020103898
Pickering emulsion polymerization
Figure 1
Magnetic moment/emu ꞏ g-1
Figure 2 -2/3-
Coercive force/Oe
Figure 3 -3/3-
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