CN111871410B - Magnetocaloric-pyroelectric composite material and preparation method and application thereof - Google Patents
Magnetocaloric-pyroelectric composite material and preparation method and application thereof Download PDFInfo
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- CN111871410B CN111871410B CN202010802009.XA CN202010802009A CN111871410B CN 111871410 B CN111871410 B CN 111871410B CN 202010802009 A CN202010802009 A CN 202010802009A CN 111871410 B CN111871410 B CN 111871410B
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- 239000002131 composite material Substances 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title abstract description 13
- 239000000463 material Substances 0.000 claims abstract description 83
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- 238000000034 method Methods 0.000 claims abstract description 24
- 239000002957 persistent organic pollutant Substances 0.000 claims abstract description 13
- 238000006731 degradation reaction Methods 0.000 claims abstract description 8
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 8
- 238000003980 solgel method Methods 0.000 claims abstract description 7
- 230000015556 catabolic process Effects 0.000 claims abstract description 6
- 238000011282 treatment Methods 0.000 claims abstract description 6
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 22
- 239000011258 core-shell material Substances 0.000 claims description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- DHEQXMRUPNDRPG-UHFFFAOYSA-N strontium nitrate Chemical compound [Sr+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O DHEQXMRUPNDRPG-UHFFFAOYSA-N 0.000 claims description 14
- 238000001035 drying Methods 0.000 claims description 13
- 238000003756 stirring Methods 0.000 claims description 12
- 239000002105 nanoparticle Substances 0.000 claims description 11
- IWOUKMZUPDVPGQ-UHFFFAOYSA-N barium nitrate Chemical compound [Ba+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O IWOUKMZUPDVPGQ-UHFFFAOYSA-N 0.000 claims description 10
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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 6
- 238000013329 compounding Methods 0.000 claims description 6
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical group [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 claims description 6
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 19
- 229910002182 La0.7Sr0.3MnO3 Inorganic materials 0.000 description 19
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- FYDKNKUEBJQCCN-UHFFFAOYSA-N lanthanum(3+);trinitrate Chemical compound [La+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O FYDKNKUEBJQCCN-UHFFFAOYSA-N 0.000 description 3
- 239000011572 manganese Substances 0.000 description 3
- MIVBAHRSNUNMPP-UHFFFAOYSA-N manganese(2+);dinitrate Chemical compound [Mn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MIVBAHRSNUNMPP-UHFFFAOYSA-N 0.000 description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical compound NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 description 2
- XNWFRZJHXBZDAG-UHFFFAOYSA-N 2-METHOXYETHANOL Chemical compound COCCO XNWFRZJHXBZDAG-UHFFFAOYSA-N 0.000 description 2
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- 239000002033 PVDF binder Substances 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
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- RLJMLMKIBZAXJO-UHFFFAOYSA-N lead nitrate Chemical compound [O-][N+](=O)O[Pb]O[N+]([O-])=O RLJMLMKIBZAXJO-UHFFFAOYSA-N 0.000 description 2
- 229910021645 metal ion Inorganic materials 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 239000005416 organic matter Substances 0.000 description 2
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- 229920002981 polyvinylidene fluoride Polymers 0.000 description 2
- 229910052761 rare earth metal Inorganic materials 0.000 description 2
- 238000006479 redox reaction Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229910001030 Iron–nickel alloy Inorganic materials 0.000 description 1
- 229910013641 LiNbO 3 Inorganic materials 0.000 description 1
- 229910052779 Neodymium Inorganic materials 0.000 description 1
- 229920002582 Polyethylene Glycol 600 Polymers 0.000 description 1
- OUUQCZGPVNCOIJ-UHFFFAOYSA-M Superoxide Chemical compound [O-][O] OUUQCZGPVNCOIJ-UHFFFAOYSA-M 0.000 description 1
- WGLPBDUCMAPZCE-UHFFFAOYSA-N Trioxochromium Chemical compound O=[Cr](=O)=O WGLPBDUCMAPZCE-UHFFFAOYSA-N 0.000 description 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- 229910007717 ZnSnO Inorganic materials 0.000 description 1
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- 230000009471 action Effects 0.000 description 1
- 238000009303 advanced oxidation process reaction Methods 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006065 biodegradation reaction Methods 0.000 description 1
- 238000010170 biological method Methods 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 229910000423 chromium oxide Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 229910000428 cobalt oxide Inorganic materials 0.000 description 1
- IVMYJDGYRUAWML-UHFFFAOYSA-N cobalt(ii) oxide Chemical compound [Co]=O IVMYJDGYRUAWML-UHFFFAOYSA-N 0.000 description 1
- 230000001808 coupling effect Effects 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000004042 decolorization Methods 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
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- 238000006056 electrooxidation reaction Methods 0.000 description 1
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- 239000012362 glacial acetic acid Substances 0.000 description 1
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- 239000000696 magnetic material Substances 0.000 description 1
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- 239000002114 nanocomposite Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
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- 239000010815 organic waste Substances 0.000 description 1
- 235000006408 oxalic acid Nutrition 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- ZBSCCQXBYNSKPV-UHFFFAOYSA-N oxolead;oxomagnesium;2,4,5-trioxa-1$l^{5},3$l^{5}-diniobabicyclo[1.1.1]pentane 1,3-dioxide Chemical compound [Mg]=O.[Pb]=O.[Pb]=O.[Pb]=O.O1[Nb]2(=O)O[Nb]1(=O)O2 ZBSCCQXBYNSKPV-UHFFFAOYSA-N 0.000 description 1
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 description 1
- DCKVFVYPWDKYDN-UHFFFAOYSA-L oxygen(2-);titanium(4+);sulfate Chemical compound [O-2].[Ti+4].[O-]S([O-])(=O)=O DCKVFVYPWDKYDN-UHFFFAOYSA-L 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/32—Manganese, technetium or rhenium
- B01J23/34—Manganese
-
- 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
- B01J23/002—Mixed oxides other than spinels, e.g. perovskite
-
- 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
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/835—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with germanium, tin or lead
-
- 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
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/84—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/843—Arsenic, antimony or bismuth
- B01J23/8437—Bismuth
-
- B01J35/40—
-
- 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
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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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/10—Heat treatment in the presence of water, e.g. steam
-
- 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
- B01J37/34—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation
- B01J37/341—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation
- B01J37/344—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation of electromagnetic wave energy
- B01J37/346—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation of electromagnetic wave energy of microwave energy
-
- 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
- B01J37/34—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation
- B01J37/348—Electrochemical processes, e.g. electrochemical deposition or anodisation
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/725—Treatment of water, waste water, or sewage by oxidation by catalytic oxidation
-
- 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
- B01J2523/00—Constitutive chemical elements of heterogeneous catalysts
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W10/00—Technologies for wastewater treatment
- Y02W10/30—Wastewater or sewage treatment systems using renewable energies
- Y02W10/37—Wastewater or sewage treatment systems using renewable energies using solar energy
Abstract
The invention provides a magnetocaloric-pyroelectric composite material, and a preparation method and application thereof, and belongs to the technical field of sewage treatment. The magnetocaloric-pyroelectric composite material is obtained by adopting a sol-gel method, a hydrothermal method and a microwave sintering method for the magnetocaloric material and the pyroelectric material. The magnetocaloric-pyroelectric composite material obtained by the invention has good stability, and the prepared material contains magnetocaloric materials, so that the magnetocaloric-pyroelectric composite material can be recycled by using a magnet, and therefore, the powder sample has small loss, can be repeatedly used for a plurality of times, and has high recycling rate. The magnetocaloric-pyroelectric composite material can be used in organic pollutant degradation applications.
Description
Technical Field
The invention belongs to the technical field of sewage treatment, and particularly relates to a magnetocaloric-pyroelectric composite material and a preparation method and application thereof.
Background
In the industrial production process, a large part of dye is lost along with sewage discharge every year, the dye has complex components, difficult decolorization, high organic matter content, good stability in water, biological toxicity and cancerogenicity, and environmental and human health hazard if not treated, is recognized as refractory sewage, so a method capable of efficiently degrading organic pollutants in sewage and an important method are sought.
The existing methods for effectively degrading the organic pollutants in the sewage include a physical method, a chemical method, a biological method and the like, wherein the physical method has small investment, and the method is simple and easy to implement, but does not degrade the organic pollutants from the source, so that the method is suitable for treating the low-concentration dye sewage; the investment cost of the chemical method is high, and secondary pollution is easy to cause; the biodegradation method has low cost and simple operation, but has higher environmental requirements, such as pH value, temperature and the like of sewage, so the actual degradation effect is not ideal, and the limitations promote the development of advanced oxidation technology.
The advanced oxidation technology developed at present is semiconductor photocatalysis technology, mechanical catalysis technology, thermal catalysis technology and the like, and the common characteristic of the advanced oxidation technology is that active free radicals with strong oxidability, such as hydroxyl free radicals, superoxide free radicals and the like, can be generated, and can degrade organic matters in sewage and decompose the organic matters into small molecular substances, such as water and CO 2 Etc., thereby achieving the purpose of sewage treatment. However, the advanced oxidation process has the limitation that, taking the semiconductor photocatalysis technology as an example, the utilization rate of light energy is not high and can be influenced by the light transmittance in the sewage, besides, the recovery of the photocatalysis material is difficult, so that the search for a method for more effectively degrading the organic pollutants in the sewage is urgent, and a method for degrading the organic pollutants by using the magneto-thermal-pyroelectric material is provided.
The pyroelectric material has a pyroelectric effect, can convert heat energy into electric energy, can generate positive and negative charge output under external thermal excitation (such as room temperature difference change), and has catalytic potential when compared with the photocatalytic degradation of organic pollutants of semiconductors by using the alternating change of cold and heat. The absorption and release of the surface charge can lead the surface charge to have oxidation-reduction reaction with the surface receptor to generate active free radicals with strong oxidability for degrading organic matters in sewage.
However, in our daily life, the rate of change of temperature and the range of change of temperature are limited, and are greatly influenced by the environment, and if the temperature change of the natural environment is only relied on, the catalytic degradation rate of the pyroelectric material is limited, so that the practical application range of the pyroelectric material is greatly limited. Therefore, finding a heat source which can get rid of the constraint of external environment, can generate the needed alternating heat source and can realize the artificial regulation and control of the organic matter degradation process for the pyroelectric material is a problem to be solved urgently.
The magnetocaloric material can convert magnetic energy into heat energy under the action of an alternating magnetic field, and the temperature change can be obtained by only applying an alternating magnetic field to the material, which is a process of absorbing and converting magnetic energy into heat energy and radiating the heat energy, and the alternating magnetic field is ubiquitous in the environment, so that an adjustable heat source can be obtained by applying the alternating magnetic field to the magnetic material, and the change rate is high and the change range is large. The magnetocaloric material and the pyroelectric material are combined to prepare the magnetocaloric-pyroelectric nano material, so that the multi-physical field coupling of magnetocaloric-pyroelectric is realized, and the great challenges of degrading organic matters of the existing pyroelectric material are hopefully solved.
Disclosure of Invention
In order to solve the problems in the prior art, the applicant provides a preparation method and application of a magnetocaloric-pyroelectric composite material. The new method for degrading organic pollutant with nanometer material utilizes magnetic-thermal-electric multiple physical field coupling to realize the pyroelectric catalysis effect induced by magnetic field. The pyroelectric material prepared by the invention has good stability, and the prepared material contains the magnetocaloric material, so that the magnet can be used for recycling, the loss of a powder sample is small, the powder sample can be repeatedly used for many times, and the recycling rate is high.
The technical scheme of the invention is as follows:
the composite material is a magnetocaloric material and a pyroelectric material; the magnetocaloric material is at least one of iron, iron alloy, cobalt alloy, nickel alloy, iron oxide, cobalt oxide and nickel oxide, rare earth element, rare earth-Mn-based perovskite compound or giant magnetocaloric material; the pyroelectric material is Ba 0.7 Sr 0.3 TiO 3 、Bi 0.5 Na 0.5 TiO 3 、BaTiO 3 、LiTaO 3 、LiNbO 3 、KNbO 3 、NaNbO 3 、BiFeO 3 、Pb(Zr,Ti)O 3 、GaN、ZnSnO 3 、ZnO、PbTiO 3 At least one of lead magnesium niobate, polyvinylidene fluoride or polyvinylidene fluoride.
The mol ratio of the magnetocaloric material to the pyroelectric material is 1:1-1:6.
the iron alloy, cobalt alloy and nickel alloy are Fe 50 Co 50 、Fe 51 Rh 49 、Fe 93.57 Si 6.43 Or Ni 2 (Mn 90 V 10 ) At least one of Sn; the oxide of iron, cobalt and nickel is beta-Fe 2 O 3 、Fe 3 O 4 、MnFe 2 O 4 、ZnFe 2 O 4 、CoFe 2 O 4 Or NiFe 2 O 4 At least one of (a) and (b); the rare earth element and rare earth-Mn based perovskite compound is Nd, tb, dy, ho, er, tm, gd, la 1-x Sr x MnO 3 、(La 67 Ba 33 )MnO 3 、(La 90 Na 10 )MnO 3 Or (La) 65 Y 5 Sr 30 )MnO 3 At least one of (a) and (b); the giant magneto-caloric material is Gd 5 (Si 2 Ge 2 ) Or LaFe 11.2 Co 0.7 Si 1.1 At least one of them.
The La is 1-x Sr x MnO 3 Wherein x is in the range of 0<x<1。
The composite material is a core-shell, columnar, lamellar or composite nanotube array; wherein the core-shell-shaped middle core layer is made of a magneto-thermal material, and the shell layer is made of a pyroelectric material.
The composite material is compounded by adopting a sol-gel method, and the specific compounding method is as follows:
with magneto-caloric material La 1-x Sr x MnO 3 The pyroelectric material is Ba 0.7 Sr 0.3 TiO 3 Examples are:
la is subjected to 1-x Sr x MnO 3 Dispersing the nano particles in glycol, adding tetrabutyl titanate, fully stirring and uniformly mixing to obtain suspension, and drying at 60-90 ℃ to obtain powder; dissolving strontium nitrate and barium nitrate in water according to the element molar ratio of 0.7:0.3, adding the dried powder into the water, fully stirring the mixture, performing hydrothermal reaction at 150-180 ℃, washing, drying and calcining the mixture after the reaction is finished, namely preserving the heat for 3-4 hours at 750-800 ℃ to finally obtain La 1-x Sr x MnO 3 @Ba 0.7 Sr 0.3 TiO 3 A nano core-shell structure composite material.
The composite material can be compounded by adopting a sol-gel method, and the specific compounding method is as follows:
using magnetocaloric material as beta-Fe 2 O 3 The pyroelectric material is PbTiO 3 Examples are:
beta-Fe 2 O 3 Dispersing nano particles in glycol, adding tetrabutyl titanate, stirring and mixing to obtain suspension, drying at 60-90 ℃ to obtain powder, adding the dried powder into lead nitrate solution, stirring and performing hydrothermal reaction at 150-180 ℃, washing, drying and calcining after the reaction is finished, and preserving heat for 2-4 hours at 700-750 ℃ to obtain beta-Fe 2 O 3 @PbTiO 3 A nano core-shell structure composite material.
The composite material can be compounded by adopting a hydrothermal method, and the specific compounding method is as follows:
the magnetic thermal material is cobalt powder, and the pyroelectric material is PbTiO 3 Examples are:
dispersing cobalt powder in polyethylene glycol-600 dissolved solution by ultrasonic wave, adding urea and titanium sulfate solution successively, stirring and mixing for 2-3 h at 60-80 ℃, washing with ethanol and water respectively, and drying to obtain Co@Ti (OH) 2 Coating the product, followed by Co@Ti (OH) 2 The coating product and lead nitrate are dissolved in deionized water, then transferred into a reaction kettle, washed and dried after hydrothermal reaction, and then kept at 600-650 ℃ for 2-3 hours to finally obtain Co@PbTiO 3 A nano core-shell structure composite material.
The composite material can be compounded by adopting a microwave sintering method, and the specific compounding method is as follows:
using pyroelectric material as BiFeO 3 The magnetocaloric material is CoFe 2 O 4 Examples are:
taking Bi as a raw material 2 O 3 ，Fe 2 O 3 ，C O3 O 4 Drying in 100-120 deg.c oven for 10-12 hr to obtain Bi 2 O 3 And Fe (Fe) 2 O 3 Taking out the raw materials, mixing, sieving, and then preserving heat in a muffle furnace at 700-750 ℃ for 10-12 h to obtain BiFeO 3 The powder is subjected to secondary ball milling and granulation to obtain BiFeO 3 Powder; drying Fe 2 O 3 And C O3 O 4 Mixing the raw materials in a mass ratio, sieving, then preserving heat for 4-5 hours in a muffle furnace at 950-1000 ℃, and then performing secondary ball milling and granulation to obtain CoFe 2 O 4 Powder according to BiFeO 3 、CoFe 2 O 4 With BiFeO 3 Sequentially placing into a round die with the diameter of 10mm, pressing into layers under 200-250 MPa, and preserving the temperature of the pressed composite material at 900-950 ℃ for 2-3 h to obtain (1-x) BiFeO 3 /xCoFe 2 O 4 Sandwich-like layered composite material, wherein x = 0.2,0.4,0.6 or 0.8.
The application of the composite material in degradation of organic pollutants.
The beneficial technical effects of the invention are as follows:
the heat source in the invention is stable, and is not from the heat energy of room temperature difference change, but from the temperature change generated by the magnetocaloric effect, and realizes the magnetic-thermal-electric multi-physical field coupling in the whole degradation process of the organic matters. Compared with the energy conversion efficiency of the photoelectric material used for photocatalysis, the energy conversion efficiency of the pyroelectric material is higher, and the catalysis efficiency is expected to be improved. Besides, the pyroelectric material has good stability, and the prepared material contains the magnetocaloric material, so that the magnet can be used for recycling, the loss of a powder sample is small, the powder sample can be repeatedly used for many times, and the recycling rate is high.
Magnetocaloric-pyroelectric materials can have various modes of communication, and can be broadly classified into the following categories, as shown in fig. 1: one is particle recombination, in which two phases are uniformly distributed in the form of particles of the order of microns, the coupling between the two phases taking place between macroscopic and microscopic phases; one is layered composite, two phases are alternately overlapped in a single layer form; one is nanocomposite, due to the large differences in properties and macroscopically exhibited in the nanoscale range; yet another is columnar compounding.
FIG. 2 is an illustration of a specific magneto-pyroelectric core-shell structured materialThe principle of degrading organic pollutants by the magnetocaloric-pyroelectric material is adopted. Wherein La is selected from 1-x Sr x MnO 3 (LSMO) nanoparticle as core material of core-shell structure, and pyroelectric material Ba 1-x SrxTiO 3 And (BST) is wrapped on the LSMO core to prepare the LSMO@BST nano core-shell structure with complete structure.
The preparation of the magnetocaloric-pyroelectric material into the nano core-shell structure has many advantages, such as: the core-shell structure ensures the mutual isolation between the magnetocaloric materials and the communication between the pyroelectric materials, thereby ensuring the insulation performance of the whole sample, ensuring the relatively large interface area between the two phases, and generating large magneto-electric coupling effect by the large interface area.
As shown in FIG. 2, when an alternating magnetic field is applied, the temperature of the inner core LSMO changes with the change of the magnetic field strength due to the existence of the magnetocaloric effect, the change is transmitted to the external BST shell layer, and the pyroelectric material has the capability of converting heat energy into electric energy, so that positive charges and negative charges are generated on the BST surface, and the occurrence of the positive charges and the negative charges can induce certain oxidation-reduction reactions to generate active free radicals with strong oxidability, such as OH, O 2 - These highly oxidizing substances can degrade organic pollutants into small molecular substances, such as CO 2 Water, etc., thereby achieving the purpose of degrading sewage.
Drawings
FIG. 1 is a schematic diagram of several modes of communication of magnetocaloric-pyroelectric materials.
FIG. 2 is a schematic illustration of catalytic effect of a specific magnetocaloric-pyroelectric core-shell structured material.
Fig. 3 is a schematic diagram of the preparation of lsmo@bst core-shell structured nano-material.
FIG. 4 is a graph of the UV-visible absorption spectra of RhB solutions at different times.
Detailed Description
The present invention will be described in detail below with reference to the drawings and examples.
Materials, reagents and the like used in the examples described below are commercially available unless otherwise specified.
Example 1
In the embodiment, the magneto-thermal-pyroelectric nano core-shell structure material is taken as an example, la 0.7 Sr 0.3 MnO 3 (LSMO) nanoparticle as core material of core-shell structure, ba 0.7 Sr 0.3 TiO 3 (BST) is taken as a shell layer, a sol-gel method is adopted to synthesize the magnetocaloric material, then a hydrothermal method is adopted to wrap the magnetocaloric material with a pyroelectric material shell layer, and the preparation schematic diagram is shown in figure 3.
La 0.7 Sr 0.3 MnO 3 Preparation of (LSMO): lanthanum nitrate, strontium nitrate and manganese nitrate are taken as raw materials and are dissolved in deionized water according to the molar ratio of 0.7:0.3:1, and metal ions are used as follows: citric acid: adding citric acid and ethylene glycol in the ratio of ethylene glycol=1:1.5:1.5, vigorously stirring, adding ammonia water to adjust the pH value to 9, presintering for 30min at 300 ℃, annealing for 4h at 950 ℃, and growing LSMO particles with good crystallization performance and obvious magnetocaloric effect.
Preparation of LSMO@BST nano core-shell structure material: dispersing LSMO nano particles in glycol by ultrasonic, adding tetrabutyl titanate into glycol, fully stirring, drying the obtained suspension at 90 ℃, dissolving strontium nitrate and barium nitrate in deionized water according to the element molar ratio of 0.7:0.3, adding the dried powder into the deionized water, fully stirring, transferring to a reaction kettle for hydrothermal reaction at 180 ℃, and performing heat treatment to obtain a sample. Core-shell structures with different shell thicknesses can be obtained by adjusting the molar ratio of the magnetocaloric material and the pyroelectric material.
Example 2
In the embodiment, taking a magnetocaloric-pyroelectric nano tube material as an example, preparing a porous alumina template (AAO template) by adopting an anodic oxidation method, and synthesizing La in nano holes of the AAO template by adopting a sol-gel method 0.7 Sr 0.3 MnO 3 @Ba 0.7 Sr 0.3 TiO 3 An array of nanotubes.
Preparation of AAO templates: the aluminum foil with the mass fraction higher than 99.999% is adopted, and the pretreated aluminum foil is obtained through cutting, annealing, polishing and other treatments in sequence. The method comprises the steps of taking oxalic acid solution with the concentration of 0.3mol/L as electrolyte, taking aluminum foil as an anode, taking a carbon rod as a cathode, carrying out electrochemical oxidation for 2-10h each time, removing a formed aluminum oxide film by using a mixed solution of phosphoric acid and chromium oxide after the first oxidation, carrying out the second oxidation after washing with distilled water, and finally obtaining the transparent AAO template under the same oxidation conditions as the first step.
Preparation of LSMO@BST nanotube array: lanthanum nitrate, strontium nitrate, manganese nitrate, barium nitrate and tetrabutyl titanate are taken as raw materials, the raw materials are dissolved in ethylene glycol methyl ether according to corresponding stoichiometric ratio, glacial acetic acid is added, the mixture is fully stirred to be completely dissolved, then a proper amount of acetic anhydride is added for dehydration, the solution is continuously stirred until the solution is cooled, a proper amount of ethanolamine is added to adjust the viscosity of the solution, and finally a proper amount of ethylene glycol methyl ether is added to adjust the concentration of the solution to 0.3mol/L. And (3) pouring the prepared gel into the prepared AAO template by adopting a vacuum negative pressure pouring method, repeating for several times, and finally annealing the AAO template poured with the gel for 10 hours at 600 ℃ to obtain the LSMO@BST nanotube array.
Example 3
In the embodiment, the pyroelectric nano particles are uniformly dispersed in the magnetocaloric material, the magnetocaloric material nano particles with good dispersibility are synthesized by adopting a sol-gel method, then the magnetocaloric material nano particles are dispersed in the gel of the pyroelectric material, and the magnetocaloric material is La 0.7 Sr 0.3 MnO 3 (LSMO) nanoparticle, and pyroelectric material selected from Ba 0.7 Sr 0.3 TiO 3 (BST) nanoparticles.
Lanthanum nitrate, strontium nitrate and manganese nitrate are taken as raw materials and are dissolved in deionized water according to the molar ratio of 0.7:0.3:1, and metal ions are used as follows: citric acid: adding citric acid and ethylene glycol in the ratio of ethylene glycol=1:1.5:1.5, vigorously stirring, adding ammonia water to adjust the pH value to 9, presintering for 30min at 300 ℃, annealing for 4h at 950 ℃, and growing LSMO particles with good crystallization performance and obvious magnetocaloric effect. Strontium nitrate, barium nitrate and tetrabutyl titanate are used as raw materials, gel is prepared, prepared LSMO particles are added into the prepared BST gel, continuous stirring is carried out in a water bath at 80 ℃ to enable mixed sol to form xerogel, the xerogel is dried in an oven at 140 ℃, then annealed at 400 ℃ for 2 hours, calcined at 700 ℃ for 2 hours, the powder is pressed into a wafer, and then annealed at 700 ℃ for 5 hours, so that a magnetocaloric-pyroelectric powder sample is obtained, and the pyroelectric particles are uniformly dispersed in the magnetocaloric particles.
Example 4
In the embodiment, the magnetocaloric material and the pyroelectric material are sandwich-like and have a layered structure, and the pyroelectric material is BiFeO 3 (BFO), the magnetocaloric material is CoFe 2 O 4 (CFO) a layered magneto-electric composite (1-x) BFO/xCFO was synthesized using a microwave sintering process, where x= 0.2,0.4,0.6,0.8.
Preparation of raw material Bi 2 O 3 ，Fe 2 O 3 ，C O3 O 4 Precisely weighing the raw materials according to the required stoichiometric ratio, and drying in an oven at 120 ℃ for 12 hours. Drying Bi 2 O 3 And Fe (Fe) 2 O 3 Taking out the raw materials, mixing, sieving, and pre-sintering (i.e. maintaining the temperature in a muffle furnace at 750deg.C for 12 h) to obtain BiFeO 3 The powder is subjected to secondary ball milling and granulation to obtain BiFeO 3 The powder is ready for use. Likewise, fe after drying 2 O 3 And C O3 O 4 Mixing the raw materials, sieving, presintering (i.e. preserving heat in a muffle furnace at 1000 ℃ for 5 h), performing secondary ball milling and granulating to obtain CoFe 2 O 4 The powder is ready for use. The BFO powder and the CFO powder are weighed according to a proportion, the BFO powder, the CFO powder and the CFO powder are placed into a round die with the diameter of 10mm according to the sequence, pressed into layers under 250MPa, and the pressed composite material is preserved for 3 hours at 950 ℃ to obtain the sandwich-shaped layered composite material.
Test example 1
Research on degradation of organic pollutants is carried out by taking the LSMO@BST nano core-shell structure material obtained in the example 1: 50mg of the prepared nano core-shell structure material is placed in 50mL of rhodamine B (5 mg/L) RhB solution, a beaker is placed in the center of a high-frequency magnetic field generator, the size and frequency of a magnetic field are regulated, the temperature of the liquid solution is recorded once every other minute until the temperature is stable, the magnetic field is closed until the temperature of the solution naturally drops to room temperature, then the magnetic field is opened again, the solution is sampled once every 5 cycles, the absorption intensity of the sample solution at 554nm is tested by using an ultraviolet spectrophotometer, and as a result, as shown in fig. 4, the maximum absorption peak intensity of the rhodamine B solution at 554nm is smaller and smaller along with the time, so that the LSMO@BST nano core-shell structure material prepared by us can degrade the RhB solution. The materials prepared in examples 2-4 have similar properties for degrading organic waste, and are not described in detail herein.
Claims (2)
1. The composite material is characterized by being a magnetocaloric material and a pyroelectric material; the magneto-caloric material is La 1-x Sr x MnO 3 The method comprises the steps of carrying out a first treatment on the surface of the The pyroelectric material is Ba 0.7 Sr 0.3 TiO 3 The method comprises the steps of carrying out a first treatment on the surface of the The La is 1-x Sr x MnO 3 Wherein x is in the range of 0<x<1；
The mol ratio of the magnetocaloric material to the pyroelectric material is 1:1-1:6, preparing a base material;
the composite material is in a core-shell shape; wherein the core-shell-shaped middle core layer is made of a magneto-thermal material, and the shell layer is made of a pyroelectric material;
the composite material is compounded by adopting a sol-gel method, and the compounding method comprises the following steps:
la is subjected to 1-x Sr x MnO 3 Dispersing the nano particles in glycol, adding tetrabutyl titanate, fully stirring and uniformly mixing to obtain suspension, and drying at 60-90 ℃ to obtain powder; dissolving strontium nitrate and barium nitrate in water according to the element molar ratio of 0.7:0.3, adding the dried powder into the water, fully stirring the mixture, performing hydrothermal reaction at 150-180 ℃, washing, drying and calcining the mixture after the reaction is finished, namely preserving the heat for 3-4 hours at 750-800 ℃ to finally obtain La 1-x Sr x MnO 3 @Ba 0.7 Sr 0.3 TiO 3 A nano core-shell structure composite material.
2. Use of the composite material according to claim 1 for degradation of organic contaminants, characterized in that the specific operations of the use are: the organic pollutant is rhodamine B solution, 50mg La is taken 1-x Sr x MnO 3 @Ba 0.7 Sr 0.3 TiO 3 The nano core-shell structure composite material is placed in 50mL of rhodamine B solution, wherein the concentration of rhodamine B is 5mg/L, a beaker is placed in the center of a high-frequency magnetic field generator, the size and frequency of a magnetic field are adjusted, the temperature of a liquid solution is recorded every other minute until the temperature is stable, the magnetic field is closed until the temperature of the solution naturally drops to room temperature, then the magnetic field is opened again, the solution is sampled once every 5 cycles, the absorption intensity of the sample solution at 554nm is tested by using an ultraviolet spectrophotometer, and the maximum absorption peak intensity of the rhodamine B solution at 554nm is smaller and smaller along with the increase of time.
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