CN101708423B - Preparation method for spherical nanometre magnesium ferrite desulfurizer - Google Patents
Preparation method for spherical nanometre magnesium ferrite desulfurizer Download PDFInfo
- Publication number
- CN101708423B CN101708423B CN2009103111626A CN200910311162A CN101708423B CN 101708423 B CN101708423 B CN 101708423B CN 2009103111626 A CN2009103111626 A CN 2009103111626A CN 200910311162 A CN200910311162 A CN 200910311162A CN 101708423 B CN101708423 B CN 101708423B
- Authority
- CN
- China
- Prior art keywords
- preparation
- spherical
- mgfe2o4
- nanometre
- microemulsion
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Images
Landscapes
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The present invention discloses a preparation method for a spherical nanometre magnesium ferrite desulfurizer, which belongs to the field of pollution control and technology. The method comprises the following steps of: dissolving a ferric nitrate and a magnesium nitrate in a glycol; adding an ammonium acetate into the mixture under the condition of violent stirring; putting the microemulsion in a high-pressure reactor to perform crystallization at 108 to 200 DEG C for 24 to 48h; and after filtering, washing and drying, calcining in a muffle furnace at 500 DEG C for 2h, thus obtaining the spherical nanometre MgFe2O4. The obtained MgFe2O4 is tested by an absorption test and the obtained MgFe2O4 has SO2 adsorbability. The method not only broadens a good MgFe2O4 shape changing and synthesizing method, but also has good SO2 adsorbability. The preparation method has good application value and application prospect in the field of absorption catalysis.
Description
Technical field
The invention belongs to gas purification desulfurizing agent preparation field, relate to a kind of preparation method of nanometer fume desulfurizing agent, specifically relate to the preparation method of nanometer magnesium ferrite (MgFe204) desulfurizing agent with spherical pattern.
Background technology
Acid rain is one of main Environmental Problems of face of mankind nowadays, and acid rain not only destroys natural environments such as water body, soil, forest, also human body, animal and plant has been caused harm.In China, it mainly is that main component is SO in the flue gas owing to the discharging of flue gases in a large number that acid rain forms
2China is coal-fired big country, as not taking effective control measure, SO
2Discharging certainly will cause severe contamination to environment.At present, generally believe that flue gas desulfurization (FGD) technology is control SO
2One of the most effective means.
In various dry desulfurizing process, the more carbon based material adsorbing and removing SO that utilizes is used in research
2But carbon based material coking problem such as subside will occur at higher temperature and cause adsorption capacity to descend rapidly, thereby can't carry out high temperature desulfurizing.Metal oxide has high-temperature stability, can be used for sulfur removal material.Simultaneously, metal oxide does not need the high energy electron generating means, does not have the trouble that solid waste is handled again compared with charged dry powder injection desulfurization, the adsorbable regenerability of also integrated carbon based material absorption method and the catalytic performance of self, thereby in dry desulfurization, be a dark horse, enjoy people to attract attention.Removal methods also develops into composite metal oxide from single metal oxide, unites from the general catalytic oxidation absorption that is adsorbed onto, and develops into nanometer technology combining from simple support type, and growth momentum is swift and violent, and prospect is unlimited.In recent years, people such as Lee (Lee, S.J; Jung, S.Y; Lee, S.C; Jun, H.K; Ryu, C.K; Kim, J.C.Ind.Eng.Chem.Res.2009,48,2691? 696) utilize coprecipitation to prepare Ce-Fe-MgO sorbent-loaded Ti, Al, Zr studies its nature of devulcanization.People such as Cheng (Cheng, W.P; Yu, X.Y; Wang, W.J; Liu, L; Yang, J.G.; He, M.Y.CatalysisCommunications.2008,9,1505? 509) on the MgAlFe hydrotalcite, flood Cu, study its desulphurizing ability.People such as Yu (Yu, Q.C; Zhang, S.C; Wang, X.D; Zhang, J; Lu, Z.M.Materials.2008,15,500-504) utilize CuO/? Al
2O
3Carry out various transformations as the sulfur dioxide adsorbent and to it.Mostly present various research is to improve SO by the load different metal
2The removal ability, and increase its surface area, thereby improve SO by the pattern that changes desulfurizing agent
2Adsorption capacity yet there are no play-by-play.
Summary of the invention
The technical problem to be solved in the present invention provide a kind of simple to operate, pollution-free, cost is low, the method for the nanometer magnesium ferrite of the spherical pattern of Hydrothermal Preparation of good product dispersibility (MgFe2O4) desulfurizing agent.The special appearance of this material increases its surface area, absorption SO
2Ability strengthens.
Preparation of catalysts method of the present invention is as follows:
1) preparation of microemulsion: claim 0.5-4gFe (NO
3)
39H
2O and 0.5-3gMg (NO
3)
26H
2O is dissolved in the 50-300ml ethylene glycol, put into water-bath magnetic agitation pot and at room temperature stir and clarify fully up to solution, then under intense stirring condition again with 30-150mmolNH
4Ac joins in the above-mentioned solution, obtains microemulsion.
2) crystallization: above gained microemulsion is placed autoclave 180-200 ℃ of following crystallization 24h-48h.
3) washing: the sample washing, the alcohol that obtain are washed, separated, dry under 60 ℃ the condition in the vacuum drying chamber, obtain MgFe
2O
4The nanosphere presoma.
4) calcining: with dried sample put into Muffle furnace with 1 ℃/min speed from room temperature temperature programming to 500 ℃, under 500 ℃ condition, calcine 2h again, finally obtain spherical pattern MgFe
2O
4
The invention has the beneficial effects as follows that this kind method not only widened MgFe
2O
4Pattern changes synthetic method, and to SO
2The good adsorption performance is arranged, and the present invention has excellent application value and application prospect in the adsoption catalysis field.
Description of drawings
Fig. 1 is prepared MgFe
2O
4The x-ray diffraction pattern of nanosphere desulfurizing agent (XRD).Abscissa is the angle of diffraction (2 θ) of twice, and ordinate is the intensity (cps) of diffraction maximum.
Fig. 2 is the MgFe of preparation
2O
4The sem photograph of nanosphere (SEM).
Fig. 3 is the MgFe of preparation
2O
4The transmission electron microscope figure (TEM) of nanosphere.
Fig. 4 is the MgFe of preparation
2O
4The x-ray photoelectron spectroscopy figure (XPS) of nanosphere desulfurizing agent.Abscissa is binding energy (eV), and ordinate is relative intensity (cps).
Fig. 5 is MgFe
2O
4The nanosphere desulfurizing agent is to sulfur dioxide adsorption capacity schematic diagram.Abscissa is sulfur dioxide partial pressure (kPa), and ordinate is the adsorbance (mmol/g) of sulfur dioxide.
The specific embodiment
Be described in detail specific embodiments of the invention below in conjunction with technical scheme and accompanying drawing.
Embodiment 1
Weighing 0.808gFe (NO
3)
39H
2O and 0.512gMg (NO
3)
26H
2O is dissolved in the 60ml ethylene glycol, put into water bath with thermostatic control magnetic agitation pot and at room temperature stir and clarify fully up to solution, then under intense stirring condition again with 30mmolNH
4Ac joins in the above-mentioned solution, and above gained microemulsion is placed 180 ℃ of following crystallization 24h of autoclave.Sample washing/the alcohol that obtains is washed/separated, and dried overnight under 60 ℃ the condition obtains MgFe in the vacuum drying chamber
2O
4The nanosphere presoma.With dried sample put into Muffle furnace with 1 ℃/min speed from room temperature temperature programming to 500 ℃, under 500 ℃ condition, calcine 2h again, finally obtain spherical pattern MgFe
2O
4Desulfurizing agent.
According to the preparation method of the present invention of embodiment 1, with Fe (NO
3)
39H
2The O quality is increased to 2.4g, Mg (NO
3)
26H
2The O quality is increased to 1.5g, and the ethylene glycol volume is increased to 180ml, NH
4Ac is increased to 90mmol, and 200 ℃ of following crystallization 24h of reactor make spherical pattern MgFe
2O
4Desulfurizing agent.
Embodiment 3
Preparation method of the present invention according to embodiment 1 is increased to 100ml with the ethylene glycol volume, and hydro-thermal reaction makes spherical pattern MgFe at 200 ℃ of following hydro-thermal reaction 30h
2O
4Desulfurizing agent.
According to the preparation method of the present invention of embodiment 1, with Fe (NO
3)
39H
2The O quality is increased to 3.2g, Mg (NO
3)
26H
2The O quality is increased to 2g, and the ethylene glycol volume is increased to 250ml, NH
4Ac is increased to 120mmol, and 180 ℃ of following crystallization 48h of reactor make spherical pattern MgFe
2O
4Desulfurizing agent.
Claims (1)
1. the preparation method of a spherical nanometre magnesium ferrite desulfurizer is characterized in that:
1) preparation of microemulsion: claim 0.808gFe (NO3) 39H2O and 0.512gMg (NO3) 26H2O to be dissolved in the 60ml ethylene glycol, putting into water-bath magnetic agitation pot at room temperature stirs up to solution and clarifies fully, under intense stirring condition, again 30mmolNH4Ac is joined in the above-mentioned solution then, obtain microemulsion;
2) crystallization: above gained microemulsion is placed autoclave 180-200 ℃ of following crystallization 24h-48h;
3) washing: the sample washing, the alcohol that obtain are washed, separated, dry under 60 ℃ the condition in the vacuum drying chamber, obtain magnesium ferrite desulfurizing agent nanosphere presoma;
4) calcining: with dried sample put into Muffle furnace with 1 ℃/min speed from room temperature temperature programming to 500 ℃, under 500 ℃ condition, calcine 2h again, finally obtain spherical pattern MgFe2O4.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009103111626A CN101708423B (en) | 2009-12-10 | 2009-12-10 | Preparation method for spherical nanometre magnesium ferrite desulfurizer |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009103111626A CN101708423B (en) | 2009-12-10 | 2009-12-10 | Preparation method for spherical nanometre magnesium ferrite desulfurizer |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101708423A CN101708423A (en) | 2010-05-19 |
| CN101708423B true CN101708423B (en) | 2011-09-14 |
Family
ID=42401243
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2009103111626A Expired - Fee Related CN101708423B (en) | 2009-12-10 | 2009-12-10 | Preparation method for spherical nanometre magnesium ferrite desulfurizer |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101708423B (en) |
Families Citing this family (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101829539B (en) * | 2010-05-21 | 2012-01-25 | 大连理工大学 | Method for preparing NiAl composite oxide desulfurizing agent with flower-shaped appearance |
| CN102107910B (en) * | 2011-03-23 | 2012-07-11 | 上海理工大学 | Preparation method of nano magnesium ferrite |
| CN102836634B (en) * | 2012-09-11 | 2015-01-14 | 北京世能中晶能源科技有限公司 | Desulfurization denitration method |
| CN104353461B (en) * | 2014-04-30 | 2017-09-08 | 金陵科技学院 | A kind of preparation method of high-ratio surface nano magnesium ferrite catalyst material available for solid propellant |
| CN104587948A (en) * | 2015-01-23 | 2015-05-06 | 三峡大学 | Magnetism recyclable nano adsorbent, preparation method and application thereof |
| CN106848277B (en) * | 2017-01-22 | 2020-07-07 | 曲阜师范大学 | Magnesium-iron-oxygen/carbon composite material and preparation method thereof |
| CN109534406A (en) * | 2018-11-21 | 2019-03-29 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of electrode material ferrous acid europium and products thereof and application |
| CN111229154A (en) * | 2020-02-18 | 2020-06-05 | 辽宁大学 | MgFe2O4/Fe2O3Composite and preparation method and application thereof |
| CN112175020A (en) * | 2020-10-15 | 2021-01-05 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation of cyclopentadiene/magnesium ferrite/cyclopentadiene nano material, product and application |
| CN112266024A (en) * | 2020-10-15 | 2021-01-26 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of cactus-shaped magnesium ferrate nano material, product and application |
-
2009
- 2009-12-10 CN CN2009103111626A patent/CN101708423B/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| CN101708423A (en) | 2010-05-19 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101708423B (en) | Preparation method for spherical nanometre magnesium ferrite desulfurizer | |
| Ma et al. | Preparation of a morph-genetic CaO-based sorbent using paper fibre as a biotemplate for enhanced CO2 capture | |
| Dong et al. | Elemental mercury removal from coal-fired flue gas using recyclable magnetic Mn-Fe based attapulgite sorbent | |
| Xie et al. | Novel regenerable sorbent based on Zr–Mn binary metal oxides for flue gas mercury retention and recovery | |
| Zhang et al. | The behavior of the manganese-cerium loaded metal-organic framework in elemental mercury and NO removal from flue gas | |
| CN105727736B (en) | Method of the catalyst for scrubbing CO_2 is prepared with metal-organic framework materials | |
| CN107362807B (en) | Mn/Co-based low-temperature SCO catalyst and preparation method thereof | |
| Chang et al. | Fe 2 O 3@ SiTi core–shell catalyst for the selective catalytic reduction of NO x with NH 3: activity improvement and HCl tolerance | |
| CN103011264B (en) | Preparation method of one-dimensional metal titanate nanorods | |
| Wang et al. | Lignin templated synthesis of porous carbon–CeO2 composites and their application for the photocatalytic desulphuration | |
| CN109364940A (en) | Charcoal loads ferrimanganic bimetallic oxide light Fenton composite material and preparation method | |
| Ren et al. | Purification of yellow phosphorus tail gas for the removal of PH 3 on the spot with flower-shaped CuO/AC | |
| CN113772710B (en) | Preparation method and application of cerium dioxide nanowire | |
| CN106824090B (en) | Preparation method and application of novel magnetic metal organic framework composite material | |
| CN109718738A (en) | A kind of zirconium oxide spherical adsorbent and its preparation method and application | |
| CN111701612A (en) | Magnetic nano composite material and preparation method thereof | |
| CN112316902A (en) | Composite MgO adsorbent and preparation method and application thereof | |
| Zhang et al. | Co3O4 nanotubes embedded in the interlayer of GO nanosheets for efficient Hg0 removal from coal flue gas | |
| CN110482544A (en) | Active carbon and its preparation method and application | |
| CN114367271B (en) | Load type MnO X Preparation method of @ NiCo-MOF composite material | |
| CN101829539B (en) | Method for preparing NiAl composite oxide desulfurizing agent with flower-shaped appearance | |
| CN115318303A (en) | Catalyst for removing soot particles of diesel vehicle at low temperature and preparation method thereof | |
| CN112138654B (en) | Catalyst for hydromethanation of carbon dioxide and application thereof | |
| WANG et al. | Hg0 removal by palygorskite (PG) supported MnOx catalyst | |
| Liu et al. | Synthesis of mesoporous cerium compound for CO2 capture |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C17 | Cessation of patent right | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20110914 Termination date: 20131210 |