CN100554155C - Adopt the method for ultrasonic synthesizing manganese octahedron molecular screen - Google Patents
Adopt the method for ultrasonic synthesizing manganese octahedron molecular screen Download PDFInfo
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- CN100554155C CN100554155C CNB2007100317242A CN200710031724A CN100554155C CN 100554155 C CN100554155 C CN 100554155C CN B2007100317242 A CNB2007100317242 A CN B2007100317242A CN 200710031724 A CN200710031724 A CN 200710031724A CN 100554155 C CN100554155 C CN 100554155C
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Abstract
The invention discloses a kind of method that adopts ultrasonic synthesizing manganese octahedron molecular screen, this method is under 40～100 ℃ of temperature of reaction, potassium permanganate places ultrasonic water bath to react for some time with the acid liquid that mixes of manganous sulfate molar ratio between 0.5～1.5, products therefrom after filtration, wash and after drying, promptly obtain manganese octahedron molecular screen (OMS-2), this material can be used for electrode materials, the absorption of heavy metal ion in the sewage, phenol, methyl alcohol, formaldehyde, organic catalyzed oxidation such as hexanaphthene, the low-temperature catalytic oxidation catalyzer of CO, this method is simple, can synthesize the OMS-2 material fast.
Description
Technical field
The present invention relates to a kind of method that adopts ultrasonic synthesizing manganese octahedron molecular screen.
Background technology
As a kind of new-type functional material, manganese oxide octahedron molecular screen (OMS-2) is in the SCR of the reaction of the low-temperature oxidation of carbon monoxide, vehicle exhaust oxynitride reaction, electrochemical reaction, and the absorption of heavy metal ion etc. is used widely in organic pollutant (as phenol, methyl alcohol, formaldehyde, hexanaphthene etc.) DeR and the water source.OMS-2 has good hydrophobicity, thermostability, ion interchangeability and is rich in advantages such as lattice oxygen.The synthetic OMS-2 material of at present existing several different methods, as: circumfluence method, in acidic solution, use KMnO
4, K
2S
2O
8, perhaps KClO
3Oxidation Mn
2+, but this method needs the long reaction times, generally needs to reflux 24 hours at least, just can obtain complete crystal formation; Sol-gel method adopts KMnO
4With polyvalent alcohol (glucose), polycarboxylic acid (toxilic acid, fumaric acid) reaction, this method is easy to generate other crystal formations, and the material that causes preparing is mixed with dephasign.
Sonochemistry is meant and utilizes acoustic cavitation can quicken and control chemical reaction, improves a new cross discipline of the new chemical reaction of reaction yield and initiation.Ultrasonic wave can by liquid medium to around propagate, and in liquid medium, produce ultrasonic cavitation, the small complex in the liquid is activated under acoustic wave action, shows as a series of dynamic processes such as oscillating growth, contraction and even collapse of complex.At the utmost point of cavitation bubble collapse in the short period of time, can in little space around it, produce the high temperature of 1900～5200K and surpass the high pressure of 50MPa, the transient temperature velocity of variation is up to 109K/s and with intensive shockwave and the momentary velocity microjet up to 400km/h.These phenomenons can increase the surface-area of inhomogeneous reaction, improve the rate of mass transfer between the interface, promote the formation of cenotype, have been widely used in the preparation of powder body material.
Summary of the invention
The invention provides a kind of method that adopts ultrasonic quick synthesizing manganese octahedron molecular screen.This method is under 40～100 ℃ of temperature of reaction, is 0.5～1.5 to be made into mixing solutions with potassium permanganate and manganous sulfate according to molar ratio, add concentrated nitric acid and regulate the pH value less than 1, react for some time in the ultrasonic water bath and be placed on, products therefrom after filtration, the washing and after drying promptly obtains manganese octahedron molecular screen.
The above-mentioned ultrasonic reaction time is 1～12h.
Above-mentioned frequency of ultrasonic is 20～100KHZ, and hyperacoustic power is 120～800W.
The invention has the beneficial effects as follows: method provided by the invention can shorten preparation time greatly, raise the efficiency, and the OMS-2 of preparation has good crystal formation.
Description of drawings
Fig. 1 is the feature XRD figure of the OMS-2 of ultrasonic method preparation of the present invention.
Embodiment
Embodiment 1:
Potassium permanganate and manganous sulfate are that 0.76 proportioning is mixed into homogeneous solution according to molar ratio, add concentrated nitric acid and regulate the pH value less than 1, solution changes in 75 ℃ of ultrasonic water bath, ultrasonic frequency 40KHz, ultrasonic power 120w, ultrasonic reaction 12h, and after-filtration, deionized water and ethanol repetitive scrubbing, 90 ℃ of dry 12h can obtain the OMS-2 material.
Embodiment 2:
Potassium permanganate and manganous sulfate are that 0.76 proportioning is mixed into homogeneous solution according to molar ratio, add concentrated nitric acid and regulate the pH value less than 1, solution changes in 75 ℃ of ultrasonic water bath, ultrasonic frequency 40KHz, ultrasonic power 480w, ultrasonic reaction 6h, and after-filtration, deionized water and ethanol repetitive scrubbing, 90 ℃ of dry 12h can obtain the OMS-2 material.
Embodiment 3:
Potassium permanganate and manganous sulfate are that 0.76 proportioning is mixed into homogeneous solution according to molar ratio, add concentrated nitric acid and regulate the pH value less than 1, solution changes in 70 ℃ of ultrasonic water bath, ultrasonic frequency 60KHz, ultrasonic power 120w, ultrasonic reaction 4h, and after-filtration, deionized water and ethanol repetitive scrubbing, 90 ℃ of dry 12h can obtain the OMS-2 material.
Embodiment 4:
Potassium permanganate and manganous sulfate are that 0.76 proportioning is mixed into homogeneous solution according to molar ratio, add concentrated nitric acid and regulate the pH value less than 1, solution changes in 70 ℃ of ultrasonic water bath, ultrasonic frequency 100KHz, ultrasonic power 120w, ultrasonic reaction 4h, and after-filtration, deionized water and ethanol repetitive scrubbing, 90 ℃ of dry 12h can obtain the OMS-2 material.
Embodiment 5:
Potassium permanganate and manganous sulfate are that 0.76 proportioning is mixed into homogeneous solution according to molar ratio, add concentrated nitric acid and regulate the pH value less than 1, solution changes in 90 ℃ of ultrasonic water bath, ultrasonic frequency 100KHz, ultrasonic power 120w, ultrasonic reaction 1h, and after-filtration, deionized water and ethanol repetitive scrubbing, 90 ℃ of dry 12h can obtain the OMS-2 material.
Embodiment 6:
Potassium permanganate and manganous sulfate are that 1.5 proportioning is mixed into homogeneous solution according to molar ratio, add concentrated nitric acid and regulate the pH value less than 1, solution changes in 40 ℃ of ultrasonic water bath, ultrasonic frequency 100KHz, ultrasonic power 800w, ultrasonic reaction 10h, and after-filtration, deionized water and ethanol repetitive scrubbing, 90 ℃ of dry 12h can obtain the OMS-2 material.
Embodiment 7:
Potassium permanganate and manganous sulfate are that 0.5 proportioning is mixed into homogeneous solution according to molar ratio, add concentrated nitric acid and regulate the pH value less than 1, solution changes in 80 ℃ of ultrasonic water bath, ultrasonic frequency 100KHz, ultrasonic power 800w, ultrasonic reaction 10h, and after-filtration, deionized water and ethanol repetitive scrubbing, 90 ℃ of dry 12h can obtain the OMS-2 material.
Embodiment 8:
Potassium permanganate and manganous sulfate are that 0.9 proportioning is mixed into homogeneous solution according to molar ratio, add concentrated nitric acid and regulate the pH value less than 1, solution changes in 60 ℃ of ultrasonic water bath, ultrasonic frequency 60KHz, ultrasonic power 240w, ultrasonic reaction 2h, and after-filtration, deionized water and ethanol repetitive scrubbing, 90 ℃ of dry 12h can obtain the OMS-2 material.
Claims (3)
1, a kind of method that adopts ultrasonic synthesizing manganese octahedron molecular screen, it is characterized in that: under 40～100 ℃ of temperature of reaction, is 0.5～1.5 to be made into mixing solutions with potassium permanganate and manganous sulfate according to molar ratio, add concentrated nitric acid and regulate the pH value less than 1, react for some time in the ultrasonic water bath and be placed on, products therefrom after filtration, the washing and after drying promptly obtains manganese octahedron molecular screen.
2, method according to claim 1 is characterized in that: the above-mentioned ultrasonic reaction time is 1～12h.
3, method according to claim 1 is characterized in that: above-mentioned frequency of ultrasonic is 20～100KHZ, and hyperacoustic power is 120～800W.
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| Application Number | Priority Date | Filing Date | Title |
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| CNB2007100317242A CN100554155C (en) | 2007-11-28 | 2007-11-28 | Adopt the method for ultrasonic synthesizing manganese octahedron molecular screen |
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| CNB2007100317242A CN100554155C (en) | 2007-11-28 | 2007-11-28 | Adopt the method for ultrasonic synthesizing manganese octahedron molecular screen |
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| CN101186309A CN101186309A (en) | 2008-05-28 |
| CN100554155C true CN100554155C (en) | 2009-10-28 |
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Families Citing this family (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102198404B (en) * | 2011-04-08 | 2013-04-17 | 复旦大学 | Silver-supported nano manganese dioxide catalyst and preparation method and application thereof |
| BR112015022310A2 (en) * | 2013-03-14 | 2017-07-18 | Johnson Matthey Plc | useful catalyst for selective catalytic reduction, process for selectively reducing a gas mixture, and article for treating a gas containing nitrogen oxides |
| CN104923281A (en) * | 2014-03-21 | 2015-09-23 | 中国科学院上海硅酸盐研究所 | Nano manganese oxide molecular sieve for room temperature efficient nitrogen oxide removal and preparation method thereof |
| CN103979664B (en) * | 2014-06-03 | 2016-01-06 | 武汉纺织大学 | A kind of OMS-2 activates the method for persulphate degradation of organic waste water |
| CN105036216B (en) * | 2015-08-17 | 2017-10-13 | 江苏金环环保设备有限公司 | A kind of sodium manganese water-purifying material and its preparation method and application |
| CN105886781B (en) * | 2016-06-29 | 2018-01-02 | 广西桂柳化工有限责任公司 | Method for recovering manganese dioxide from electrolytic manganese anode mud |
| CN108744953B (en) * | 2018-05-22 | 2020-06-30 | 中南大学 | Application method of OMS-2 and/or metal-doped OMS-2 catalytic flue gas denitration |
| CN110368930A (en) * | 2019-08-07 | 2019-10-25 | 山东卓高新材料有限公司 | A kind of nano manganese oxide catalysis material and preparation method thereof |
| CN111266129B (en) * | 2020-02-01 | 2021-04-23 | 浙江大学 | Solid-phase OMS-2 molecular sieve catalyst for room-temperature formaldehyde purification and preparation method thereof |
| CN114452974B (en) * | 2022-02-21 | 2023-05-23 | 中南大学 | MnO 2 Base formaldehyde removal material, ultrasonic-microwave auxiliary preparation method thereof and application thereof in formaldehyde catalytic oxidation |
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2007
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