CN111326302B - Core-shell structure magnetic material for industrial clean air and preparation method thereof - Google Patents
Core-shell structure magnetic material for industrial clean air and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of industrial purification, and particularly relates to a core-shell structure magnetic material for industrial clean air and a preparation method thereof. In the material provided by the invention, the polyacid modified zinc ferrite has high light utilization rate, good photocatalytic effect and structural stability, a formed core-shell structure has large specific surface area and large pollutant adsorption capacity, and meanwhile, the durability of the material is improved by utilizing the excellent performances of low refractive index, high chemical stability, acid-base corrosion resistance and the like of silicon dioxide.
Description
Technical Field
The invention relates to the technical field of industrial purification, in particular to a core-shell structure magnetic material for industrial clean air and a preparation method thereof.
Background
With the improvement of the living standard of people and the use of a large amount of chemical raw materials for indoor decoration, a large amount of organic pollutants enter indoors, which brings great threat to the living health of people, and with the development of social economy and the improvement of the living standard of people, the living environment which characterizes the living quality of people is increasingly emphasized, and a safe and healthy living space is urgently hoped to be provided. And thus, research on air purification materials is also gaining importance.
In recent years, research on novel porous materials such as rare earth mesoporous oxides, activated carbon fibers, carbonized micron wood fibers and the like provides a new direction for adsorption and separation of micro-nano particles, but the technology is often used for adsorbing harmful gases and cannot effectively degrade the harmful gases. The other is made of TiO2The photocatalyst type air purification material using the material as a catalyst is a commonly used air purification material at present.
The indoor air pollution source mainly comprises carbon monoxide, nitrogen oxides and strong carcinogens generated by cooking and frying in a kitchen; toxic and harmful substances emitted by interior decoration materials, cosmetics, new furniture and the like mainly comprise formaldehyde, benzene, ether esters, trichloroethylene, acrylonitrile and other volatile organic compounds; in addition, there are damp-breeding fungi and the like. The conventional purification mode is activated carbon adsorption at present, but harmful substances are difficult to eradicate due to limited adsorption quantity. The degradation is a better technical means for solving the problem of organic matter pollution in the air. The existing catalytic degradation is mainly adopted, and the efficiency of the existing catalytic degradation material is not high due to the limitation of catalytic materials and environment.
The Chinese patent application No. 201510843593.2 discloses a silicon oxide-doped air purification material, which comprises the following components in parts by weight: 50-90 parts of titanium alkoxide, 2-10 parts of nano silicon oxide, 20-40 parts of chitin nano fiber, 3-10 parts of polyethylene glycol, 200-500 parts of anhydrous ethanol and 10-50 parts of water; the invention avoids TiO by uniformly doping the silicon dioxide2The long-time stable photocatalytic activity is maintained due to the agglomeration phenomenon caused by high surface energy along with the time extension; by using polyethylene glycol in TiO2The compact surface of the titanium dioxide film forms uniform tiny micropores and also overcomes TiO to a certain extent2Surface agglomeration of (a); the pollutant concentration on the surface is increased by the adsorption of chitin nano-fiber, and the chitin nano-fiber is TiO2Provides a basis for the performance of the smooth photocatalysis. Chinese patent application No. 201810112315.3 discloses a composite photocatalytic material for air purifier, which is prepared from activated carbon and nano TiO2A photocatalyst material and a noble metal, the compositionThe photocatalytic material is prepared by loading nano TiO on active carbon2Photocatalyst material in nano TiO2Noble metal nano particles are loaded on the photocatalyst material, and the active carbon has a porous structure; the composite photocatalytic material is used for degrading harmful gas in a catalytic degradation module of an air purifier.
In order to improve the ability of the air purification material to adsorb and catalytically degrade pollutants in the air, it is necessary to provide a novel air purification material, so as to achieve the effect of efficiently purifying pollutants in the air.
Disclosure of Invention
Aiming at the problems of poor adsorption effect, poor air purification efficiency, low catalytic degradation efficiency and the like of the existing material for purifying indoor air, the invention provides the core-shell structure magnetic material for industrial clean air and the preparation method thereof, so that the air evolution efficiency is improved, and the durability is good.
In order to solve the problems, the invention adopts the following technical scheme:
the invention also provides a preparation method of the core-shell structure magnetic material for industrial clean air, the magnetic material is prepared by adding polyacid when zinc ferrite is prepared by taking zinc nitrate hexahydrate, ferric nitrate nonahydrate and urea as raw materials, obtaining polyacid-modified nano zinc ferrite, and then coating silicon dioxide on the surface to form a core-shell structure, and the preparation method specifically comprises the following steps:
(1) adding zinc nitrate hexahydrate, ferric nitrate nonahydrate and urea into a mixed solution consisting of isopropanol and glycerol, then adding polyacid, mixing and stirring uniformly, transferring the obtained reaction solution into a stainless steel high-pressure reaction kettle, and carrying out solvothermal reaction to obtain a zinc ferrite precursor;
(2) sequentially centrifuging, washing, drying and annealing the precursor obtained by the reaction to obtain polyacid-modified nano zinc ferrite;
(3) adding polyacid modified nano zinc ferrite into a solution containing ethanol and deionized water, then adding ammonia water and ethyl orthosilicate, stirring for reaction, filtering, washing and drying after the reaction is finished, so as to obtain the silicon dioxide/polyacid modified zinc ferrite magnetic material with the core-shell structure, namely the core-shell structure magnetic material for industrial clean air.
Preferably, the polyacid is one of dichromic acid, dodecamolybdophosphoric acid and dodecaphosphotungstic acid.
Preferably, in the step (1), the mass ratio of the isopropanol, the glycerol, the zinc nitrate hexahydrate, the ferric nitrate nonahydrate, the urea and the polyacid is 100:80-100:40-50:40-50:15-25: 10-20.
Preferably, the temperature of the solvothermal reaction in the step (1) is 170-180 ℃, and the reaction time is 8-10 h.
Preferably, the temperature of the annealing in the step (2) is 440-460 ℃, and the time is 5-10 min.
Preferably, the rotation speed of the stirring reaction in the step (3) is 300-400rpm, and the reaction lasts for 5-8 h.
Preferably, the drying in the step (3) adopts vacuum drying at the temperature of 70-80 ℃ for 12-15 h.
Preferably, in the step (3), the mass ratio of the deionized water, the ethanol, the polyacid-modified nano zinc ferrite, the ammonia water and the tetraethoxysilane is 100:40-50:60-80:10-20: 20-30.
In the existing industrial air purification, harmful gas is mostly adsorbed, and the problems of poor adsorption effect, poor air purification efficiency, low catalytic degradation efficiency and the like exist. In view of the above, the invention provides a core-shell structure magnetic material for industrial clean air and a preparation method thereof, zinc nitrate hexahydrate, ferric nitrate nonahydrate and urea are added into a mixed solution consisting of isopropanol and glycerol, then polyacid is added, after full stirring, reaction liquid is transferred into a stainless steel high-pressure reaction kettle for solvothermal reaction; centrifuging, washing, drying and annealing the precursor obtained by the reaction to obtain polyacid-modified nano zinc ferrite; and then adding the obtained polyacid-modified nano zinc ferrite into a solution containing ethanol and deionized water, adding ammonia water and tetraethoxysilane, stirring and mixing, reacting, filtering, washing and drying to obtain the silicon dioxide/polyacid-modified zinc ferrite magnetic material with the core-shell structure. In the core-shell structure air purification material provided by the invention, the polyacid modified zinc ferrite has high light utilization rate, good photocatalysis effect and structural stability, the formed core-shell structure has large specific surface area and large pollutant adsorption capacity, and meanwhile, the durability of the material is improved by utilizing the excellent properties of low refractive index, high chemical stability, acid-base corrosion resistance and the like of silicon dioxide.
Compared with the prior art, the invention provides the core-shell structure magnetic material for industrial clean air and the preparation method thereof, and the outstanding characteristics and excellent effects are as follows:
1. the polyacid introduced by the invention effectively enhances the absorption of zinc ferrite to light, improves the utilization rate of light, increases the specific surface area and the number of active sites of the catalyst, improves the adsorption capacity of zinc ferrite to pollutants in the air, and simultaneously, the formed interface electric field promotes the separation of photo-generated electron pairs, thereby effectively improving the photocatalytic effect and the structural stability of the zinc ferrite.
2. According to the invention, the core-shell structure is formed by coating silicon dioxide, so that the specific surface area is increased, the adsorption capacity to pollutants is increased, and meanwhile, the prepared magnetic material with the core-shell structure can be used for a long time by utilizing the excellent properties of low refractive index, high chemical stability, acid and alkali corrosion resistance and the like of the silicon dioxide material.
3. The preparation method and the process are simple and convenient, have low cost, are harmless to the environment, can be treated at normal temperature, are suitable for large-scale industrial production, and have wide application prospect.
Drawings
FIG. 1: schematic diagram of the device for testing the effect of purifying air.
Detailed Description
The present invention will be described in further detail with reference to specific embodiments, but it should not be construed that the scope of the present invention is limited to the following examples. Various substitutions and alterations can be made by those skilled in the art and by conventional means without departing from the spirit of the method of the invention described above.
Example 1
(1) Adding zinc nitrate hexahydrate, ferric nitrate nonahydrate and urea into a mixed solution consisting of isopropanol and glycerol, then adding polyacid, mixing and stirring uniformly, transferring the obtained reaction solution into a stainless steel high-pressure reaction kettle, and carrying out solvothermal reaction to obtain a zinc ferrite precursor; in the reaction liquid, the mass ratio of isopropanol, glycerol, zinc nitrate hexahydrate, ferric nitrate nonahydrate, urea and polyacid is 100:90:45:45:20: 15; the temperature of the solvothermal reaction is 175 ℃, and the reaction is carried out for 9 hours; the polyacid is dodecamolybdophosphoric acid;
(2) sequentially centrifuging, washing, drying and annealing the precursor obtained by the reaction to obtain polyacid-modified nano zinc ferrite; the annealing temperature is 450 ℃ and the annealing time is 8 min;
(3) adding polyacid modified nano zinc ferrite into a solution containing ethanol and deionized water, then adding ammonia water and ethyl orthosilicate, stirring for reaction, filtering, washing and drying after the reaction is finished to obtain a silicon dioxide/polyacid modified zinc ferrite magnetic material with a core-shell structure, namely the core-shell structure magnetic material for industrial clean air; the stirring reaction speed is 350rpm, and the reaction lasts for 6 hours; vacuum drying at 75 deg.C for 14 h; in the reaction raw materials, the mass ratio of deionized water, ethanol, polyacid-modified nano zinc ferrite, ammonia water and tetraethoxysilane is 100:45:70:15: 25.
The test method comprises the following steps:
the air purification performance of the air purification core-shell structure magnetic material prepared in the embodiment is tested, the test is carried out in a test box of 1m × 1m × 1m, as shown in figure 1, a 10W xenon lamp is arranged in the test box, the air purification material prepared by the invention is added, the test for removing formaldehyde and benzene is respectively carried out, and the initial concentration of introduced formaldehyde is 1.28mg/m3(ii) a The initial concentration of the introduced benzene was 0.6mg/m3(ii) a According to an initial concentration of A0Respectively adopting corresponding gas concentration testers to test the gas concentration in the test chamber, wherein the concentration after 4h is AiAnd according to the formula B = (A)0-Ai）/A0The gas purification rate was calculated, and the results are shown in table 1.
Example 2
(1) Adding zinc nitrate hexahydrate, ferric nitrate nonahydrate and urea into a mixed solution consisting of isopropanol and glycerol, then adding polyacid, mixing and stirring uniformly, transferring the obtained reaction solution into a stainless steel high-pressure reaction kettle, and carrying out solvothermal reaction to obtain a zinc ferrite precursor; in the reaction solution, the mass ratio of isopropanol, glycerol, zinc nitrate hexahydrate, ferric nitrate nonahydrate, urea and polyacid is 100:80:40:40:15: 10; the temperature of the solvothermal reaction is 170 ℃, and the reaction lasts for 10 hours; the polyacid is dodecaphosphotungstic acid;
(2) sequentially centrifuging, washing, drying and annealing the precursor obtained by the reaction to obtain polyacid-modified nano zinc ferrite; the annealing temperature is 440 ℃, and the annealing time is 10 min;
(3) adding polyacid modified nano zinc ferrite into a solution containing ethanol and deionized water, then adding ammonia water and ethyl orthosilicate, stirring for reaction, filtering, washing and drying after the reaction is finished to obtain a silicon dioxide/polyacid modified zinc ferrite magnetic material with a core-shell structure, namely the core-shell structure magnetic material for industrial clean air; the stirring reaction speed is 300rpm, and the reaction lasts 8 hours; the drying adopts vacuum drying at the temperature of 70 ℃ for 15 h; in the reaction raw materials, the mass ratio of deionized water, ethanol, polyacid modified nano zinc ferrite, ammonia water and tetraethoxysilane is 100:40:60:10: 20.
The test was carried out by the method of example 1, and the test results are shown in Table 1.
Example 3
(1) Adding zinc nitrate hexahydrate, ferric nitrate nonahydrate and urea into a mixed solution consisting of isopropanol and glycerol, then adding polyacid, mixing and stirring uniformly, transferring the obtained reaction solution into a stainless steel high-pressure reaction kettle, and carrying out solvothermal reaction to obtain a zinc ferrite precursor; in the reaction solution, the mass ratio of isopropanol, glycerol, zinc nitrate hexahydrate, ferric nitrate nonahydrate, urea and polyacid is 100: 100: 50: 50: 25: 20; the temperature of the solvothermal reaction is 180 ℃, and the reaction lasts for 8 hours; the polyacid is dodecamolybdophosphoric acid;
(2) sequentially centrifuging, washing, drying and annealing the precursor obtained by the reaction to obtain polyacid-modified nano zinc ferrite; the annealing temperature is 460 ℃ and the annealing time is 5 min;
(3) adding polyacid modified nano zinc ferrite into a solution containing ethanol and deionized water, then adding ammonia water and ethyl orthosilicate, stirring for reaction, filtering, washing and drying after the reaction is finished to obtain a silicon dioxide/polyacid modified zinc ferrite magnetic material with a core-shell structure, namely the core-shell structure magnetic material for industrial clean air; the stirring reaction speed is 400rpm, and the reaction lasts for 5 hours; vacuum drying at 80 deg.C for 12 hr; in the reaction raw materials, the mass ratio of deionized water, ethanol, polyacid modified nano zinc ferrite, ammonia water and tetraethoxysilane is 100: 50:80: 20: 30.
The test was carried out by the method of example 1, and the test results are shown in Table 1.
Example 4
(1) Adding zinc nitrate hexahydrate, ferric nitrate nonahydrate and urea into a mixed solution consisting of isopropanol and glycerol, then adding polyacid, mixing and stirring uniformly, transferring the obtained reaction solution into a stainless steel high-pressure reaction kettle, and carrying out solvothermal reaction to obtain a zinc ferrite precursor; in the reaction solution, the mass ratio of isopropanol, glycerol, zinc nitrate hexahydrate, ferric nitrate nonahydrate, urea and polyacid is 100:88:46:44:19: 16; the temperature of the solvothermal reaction is 176 ℃, and the reaction is carried out for 9 hours; the polyacid is dichromic acid;
(2) sequentially centrifuging, washing, drying and annealing the precursor obtained by the reaction to obtain polyacid-modified nano zinc ferrite; the annealing temperature is 448 ℃ and the time is 7 min;
(3) adding polyacid modified nano zinc ferrite into a solution containing ethanol and deionized water, then adding ammonia water and ethyl orthosilicate, stirring for reaction, filtering, washing and drying after the reaction is finished to obtain a silicon dioxide/polyacid modified zinc ferrite magnetic material with a core-shell structure, namely the core-shell structure magnetic material for industrial clean air; the rotating speed of stirring reaction is 360rpm, and the reaction lasts for 7 hours; vacuum drying at 76 deg.C for 13 hr; in the reaction raw materials, the mass ratio of deionized water, ethanol, polyacid-modified nano zinc ferrite, ammonia water and tetraethoxysilane is 100:46:68:16: 24.
The test was carried out by the method of example 1, and the test results are shown in Table 1.
Comparative example 1
Comparative example 1 compared with example 1, the air evolution magnetic material prepared without the addition of polyacid treatment was tested by the method of example 1, and the test results are shown in table 1.
Comparative example 2
Compared with example 1, no silica coating treatment is adopted, so that the adsorption performance is influenced, and the test results are shown in table 1.
Table 1:
Claims (8)
1. a preparation method of a core-shell structure magnetic material for industrial clean air is characterized by comprising the following steps:
(1) adding zinc nitrate hexahydrate, ferric nitrate nonahydrate and urea into a mixed solution consisting of isopropanol and glycerol, then adding polyacid, mixing and stirring uniformly, transferring the obtained reaction solution into a stainless steel high-pressure reaction kettle, and carrying out solvothermal reaction to obtain a zinc ferrite precursor;
(2) sequentially centrifuging, washing, drying and annealing the precursor obtained by the reaction to obtain polyacid-modified nano zinc ferrite;
(3) adding polyacid modified nano zinc ferrite into a solution containing ethanol and deionized water, then adding ammonia water and ethyl orthosilicate, stirring for reaction, filtering, washing and drying after the reaction is finished to obtain a silicon dioxide/polyacid modified zinc ferrite magnetic material with a core-shell structure, namely the core-shell structure magnetic material for industrial clean air; the mass ratio of the deionized water, the ethanol, the polyacid modified nano zinc ferrite, the ammonia water and the tetraethoxysilane is 100:40-50:60-80:10-20: 20-30.
2. The method for preparing a magnetic material with a core-shell structure for industrial clean air according to claim 1, wherein the polyacid is one of dichromic acid, dodecamolybdophosphoric acid and dodecaphosphotungstic acid.
3. The preparation method of the core-shell structure magnetic material for industrial clean air according to claim 1, characterized in that in the step (1), the mass ratio of isopropanol, glycerol, zinc nitrate hexahydrate, ferric nitrate nonahydrate, urea and polyacid is 100:80-100:40-50:40-50:15-25: 10-20.
4. The method for preparing the magnetic material with the core-shell structure for industrial clean air as claimed in claim 1, wherein the temperature of the solvothermal reaction in the step (1) is 170-180 ℃, and the reaction time is 8-10 h.
5. The method for preparing a magnetic material with a core-shell structure for industrial clean air as claimed in claim 1, wherein the annealing temperature in step (2) is 440-460 ℃ and the annealing time is 5-10 min.
6. The method for preparing a magnetic material with a core-shell structure for industrial clean air as claimed in claim 1, wherein the rotation speed of the stirring reaction in step (3) is 300-400rpm, and the reaction time is 5-8 h.
7. The preparation method of the core-shell structure magnetic material for industrial clean air according to claim 1, characterized in that the drying in the step (3) is vacuum drying at 70-80 ℃ for 12-15 h.
8. A magnetic material with a core-shell structure for industrial clean air, which is prepared by the preparation method of any one of claims 1 to 7.
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| CN101229517A (en) * | 2007-01-25 | 2008-07-30 | 北京化工大学 | Method of preparing nanometer magnetic heteropoly acid |
| CN103418371A (en) * | 2012-05-17 | 2013-12-04 | 华东理工大学 | Preparation method of MOx@SiO2 shell-core structure catalyst |
| CN108336343A (en) * | 2018-03-14 | 2018-07-27 | 吉林大学 | A kind of preparation method and application of zinc ferrite/manganese dioxide composite material |
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| CN101229517A (en) * | 2007-01-25 | 2008-07-30 | 北京化工大学 | Method of preparing nanometer magnetic heteropoly acid |
| CN103418371A (en) * | 2012-05-17 | 2013-12-04 | 华东理工大学 | Preparation method of MOx@SiO2 shell-core structure catalyst |
| CN108336343A (en) * | 2018-03-14 | 2018-07-27 | 吉林大学 | A kind of preparation method and application of zinc ferrite/manganese dioxide composite material |
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Effective date of registration: 20211013 Address after: 226600 room 1, No.118, group 5, dongmiao village, Hai'an town, Hai'an City, Nantong City, Jiangsu Province Applicant after: Nantong Sanyou Jia Magnetic Industry Co.,Ltd. Address before: 610091, Sichuan, Chengdu province Qingyang dragon industrial port, East Sea 4 Applicant before: CHENDU NEW KELI CHEMICAL SCIENCE Co.,Ltd. CHINA |
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