CN102718190A - Potassium permanganate/silicon titanium pillared montmorillonite nanocomposite oxygen storage material and preparation method thereof - Google Patents
Potassium permanganate/silicon titanium pillared montmorillonite nanocomposite oxygen storage material and preparation method thereof Download PDFInfo
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- CN102718190A CN102718190A CN2012102291873A CN201210229187A CN102718190A CN 102718190 A CN102718190 A CN 102718190A CN 2012102291873 A CN2012102291873 A CN 2012102291873A CN 201210229187 A CN201210229187 A CN 201210229187A CN 102718190 A CN102718190 A CN 102718190A
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- pillared montmorillonite
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Abstract
The invention provides a potassium permanganate/silicon titanium pillared montmorillonite nanocomposite oxygen storage material, which is obtained through carrying out intercalation compounding on potassium permanganate and silicon titanium pillared montmorillonite. The oxygen released volume and the oxygen releasing rate of a potassium permanganate/silicon titanium pillared montmorillonite nanocomposite material are collected through a draining method, the condition that both the oxygen released volume and the oxygen releasing rate of the potassium permanganate/silicon titanium pillared montmorillonite nanocomposite oxygen storage material of the same mass are obviously less than those of potassium permanganate is indicated, and the condition that the composite oxygen storage material has a buffer action on oxygen release while the composite oxygen storage material has the function of oxygen storage is presented, so that the potassium permanganate/silicon titanium pillared montmorillonite nanocomposite oxygen storage material is the oxygen storage material with excellent performance. Furthermore, the potassium permanganate/silicon titanium pillared montmorillonite nanocomposite oxygen storage material has the advantages of simple preparation process, convenience in operation, mild reaction condition, low production cost and high production efficiency, so that the potassium permanganate/silicon titanium pillared montmorillonite nanocomposite oxygen storage material has excellent industrial production prospects.
Description
Technical field
The invention belongs to technical field of composite materials, relate to a kind of potassium permanganate/nano combined hydrogen-storing material of silicon titanium pillared montmorillonite and preparation method thereof.
Background technology
Hydrogen-storing material has the function of reversible absorption and release of oxygen; It can adsorb and release of oxygen under given conditions; Be mainly used in aerobic places such as hospital, office, dwelling house, market and health care place, can also be applied on the aerobic crowds such as plateau road vehicle, field worker, army's barracks and soldier.The hydrogen-storing material of document mainly contains cerium zirconium aluminium rare earth hydrogen-storing material at present, CeO2-ZrO2 is hydrogen-storing material, low cerium type Ce-Zr-Sn composite Nano hydrogen-storing material or the like, but these hydrogen-storing materials exist cost high, complicated process of preparation, defectives such as storage oxygen poor-performing.
Potassium permanganate is a kind of common strong oxidizer, claims the PP powder again, and normal temperature for the atropurpureus solid, discharges oxygen down easily under illumination or heating condition.But; The potassium permanganate solid is difficult for fixing; Manganse Dioxide in the time of reaction in the degradation production and potassium manganate can be surperficial at the potassium permanganate of unreacted with solid-state wrapped, thereby hindered the further reaction of residue potassium permanganate, greatly reduce its oxygenous efficient.
The pillared montmorillonite porous material is owing to have bigger interlamellar spacing and higher specific surface area, and as sorbent material and catalyzer, have vast potential for future development, but it is as the application of the carrier of hydrogen-storing material, and bibliographical information is not arranged at present as yet.
Summary of the invention
The objective of the invention is provides the higher potassium permanganate of a kind of reaction efficiency/silicon titanium pillared montmorillonite nanometer hydrogen-storing material to the problem that exists in the prior art;
Another object of the present invention provides the preparation method of a kind of potassium permanganate/nano combined hydrogen-storing material of silicon titanium pillared montmorillonite.
Potassium permanganate of the present invention/nano combined the hydrogen-storing material of silicon titanium pillared montmorillonite is potassium permanganate to be inserted evenly the silicon titanium is pillared to be taken off in the native lamella and get.
The mass ratio of said potassium permanganate and silicon titanium pillared montmorillonite is 1:1～1:2.
The preparation method of potassium permanganate of the present invention/nano combined hydrogen-storing material of silicon titanium pillared montmorillonite is silicon titanium pillared montmorillonite to be distributed to form silicon titanium pillared montmorillonite dispersion liquid in water or the acetic acid aqueous solution; The potassium permanganate solid is soluble in water, form potassium permanganate solution; Silicon titanium pillared montmorillonite dispersion liquid is mixed being placed in the ultrasonic dispersing appearance with potassium permanganate solution, ultra-sonic dispersion stirred after 1 ~ 2 hour 20 ~ 24 hours again; Suction filtration, washing, oven dry is ground into particle or grind into powder, obtains potassium permanganate/nano combined oxygen-making agent of silicon titanium pillared montmorillonite.
In the said silicon titanium pillared montmorillonite dispersion liquid, the mass percent of silicon titanium pillared montmorillonite is 5% ~ 15%.
In the said potassium permanganate solution, the mass percent of potassium permanganate is 12 % ~ 25%.
In the mixed system of said silicon titanium pillared montmorillonite dispersion liquid and potassium permanganate solution, the mass ratio of potassium permanganate and silicon titanium pillared montmorillonite is 1:1～1:2.
Below the volume through ir spectra map analysis, electron-microscope scanning picture and release of oxygen with put oxygen speed the performance of the potassium permanganate/nano combined hydrogen-storing material of silicon titanium pillared montmorillonite of invention preparation tested and characterized.
1, IR spectroscopy
Fig. 1 is the infrared spectrogram of potassium permanganate/nano combined hydrogen-storing material of silicon titanium pillared montmorillonite (a), modified montmorillonoid (b), potassium permanganate (c).Among the figure, at 1034cm
-1The strong absorption band at place is the charateristic avsorption band of modified montmorillonoid, mainly is the skeletal vibration of Si-O-Si; At 460 ~ 520cm
-1The peak of scope is the flexural vibration peak of Si-O and Al-O.Through finding that relatively modified montmorillonoid is at 1034cm
-1Blue shift has taken place in the charateristic avsorption band at place, and this mainly is because the small-size effect and the quantum size effect of nano flake cause.In the recombination process of potassium permanganate and silicon titanium pillared montmorillonite, the combination of chemical bond is arranged between them, can influence the vibrational frequency of bonded atom with it.Above-mentioned phenomenon shows that in the middle of the forming process of matrix material, silicon titanium pillared montmorillonite and potassium permanganate have produced certain physical and chemical interaction.In addition,, find that the color of potassium permanganate/silicon titanium pillared montmorillonite nano composite material is obviously deepened with respect to silicon titanium pillared montmorillonite, be dark coffee look through the color of contrast potassium permanganate/silicon titanium pillared montmorillonite nano composite material and silicon titanium pillared montmorillonite.Explanation thus, potassium permanganate and the compound success of silicon titanium pillared montmorillonite.
2, electron-microscope scanning analysis
Fig. 2 is the electron microscope photo scanning of modified montmorillonoid (a), potassium permanganate/nano combined hydrogen-storing material of silicon titanium pillared montmorillonite (b).Can find that from Fig. 2 inorganic materials two is alternate have been taken place compoundly, this shows and forms finely dispersed external phase between the inorganic phase, and two mutually compatible better.This is because formed chemical bond between the inorganics, because that the effect of chemical bond causes is two mutually compound, has promptly increased the biphase consistency, has stoped the generation of large-size particle, thereby has formed nano composite material.After modified montmorillonoid and potassium permanganate are compound, wrapped up one deck potassium permanganate on the modified montmorillonoid uniformly, formed laminate structure preferably, surface-area is very big, and lamella is thin, and modified montmorillonoid and inorganic body are combined closely.
3, put the oxygen amount and put the oxygen rate analysis
Collect the volume of potassium permanganate/nano combined hydrogen-storing material release of oxygen of silicon titanium pillared montmorillonite through drainage, and contrast with potassium permanganate.Respectively 1g potassium permanganate/nano combined hydrogen-storing material of silicon titanium pillared montmorillonite and 1g potassium permanganate are placed test tube, with test tube plug sealing back spirit lamp heating test tube, the oxygen of generation closes through air guide and is transferred to graduated cylinder.Collect and measure amount of oxygen in the graduated cylinder, and record begins to the time that finishes from putting oxygen at every turn.
The result sees the following form.
| ? | Quality/g | Putting oxysome amasss/ml | Put oxygen time/s | Put oxygen speed/mls - -1 |
| Compound oxygen-making agent | 1 | 40 | 48 | 0.83 |
| Potassium permanganate | 1 | 90 | 29 | 3.10 |
From the data of last table; We can find out; The long-pending oxysome of putting less than potassium permanganate of oxysome of putting of the potassium permanganate of homogenous quantities/nano combined hydrogen-storing material of silicon titanium pillared montmorillonite amasss; The potassium permanganate of homogenous quantities/nano combined hydrogen-storing material of silicon titanium pillared montmorillonite put that oxygen speed is significantly less than potassium permanganate put oxygen speed, explain when compound hydrogen-storing material of the present invention has storage oxygen function that emitting of oxygen had shock absorption.
The relative prior art of the present invention has following characteristics:
1, to adopt potassium permanganate and silicon titanium pillared montmorillonite to carry out intercalation compound in the present invention; The matrix material that obtains has system oxygen and storage oxygen buffering dual function; Overcome potassium permanganate simultaneously and be difficult for fixing and the low shortcoming of reaction efficiency, thereby be a kind of hydrogen-storing material of excellent property.
2, preparation technology of the present invention is simple, and is easy to operate, and reaction conditions is gentle, and production cost is low, and production efficiency is high, has the favorable industrial prospect of production.
Description of drawings
Fig. 1 is the infrared spectrogram of potassium permanganate of the present invention/silicon titanium pillared montmorillonite nano composite material;
Fig. 2 is the electron-microscope scanning figure of potassium permanganate of the present invention/silicon titanium pillared montmorillonite nano composite material.
Embodiment
Embodiment 1
1. the preparation of organo montmorillonite: with polynite 0.5g and an amount of 150ml Shui ﹑ 1.5g cetyl trimethylammonium bromide at 80 ℃ of following high-speed stirring 2h; Anti-after backwashing Di ﹑ Chen Dian ﹑ suction filtration; Wash excessive cetyl trimethylammonium bromide off, under 80 ℃ of conditions, dry, grind; 200 orders sieve, and obtain organo montmorillonite.
2. the preparation of silicon titanium pillared montmorillonite poromerics: tetraethoxy 20ml ﹑ ethanol 20ml ﹑ Glacial acetic acid min. 99.5 10ml ﹑ zero(ppm) water 50ml is mixed; Add organo montmorillonite 0.643g; Slowly drip an amount of titanium tetrachloride 2ml, stirring at room 2h, oil bath Heating temperature then is elevated to 60 ℃; Observe when gelatin phenomenon occurring, move to 60 ℃ of oven dry in the watch-glass.Be ground into particle or grind into powder, obtain silicon titanium pillared montmorillonite 12.994g.
3. the preparation of potassium permanganate/silicon titanium pillared montmorillonite matrix material: silicon titanium pillared montmorillonite (12.994g) is evenly spread in the 130ml aqueous solution, form the modified montmorillonoid dispersion liquid; Potassium permanganate solid 13g is dissolved in the 52ml water, forms potassium permanganate solution; The modified montmorillonoid dispersion liquid mixed being placed in the ultrasonic dispersing appearance with potassium permanganate solution, ultra-sonic dispersion stirred 24 hours after 2 hours.Suction filtration, washing, oven dry is ground into particle or grind into powder, obtains potassium permanganate/silicon titanium pillared montmorillonite nano composite material 12.331g, productive rate 47.4%.
Embodiment 2
1. the preparation of organo montmorillonite: with embodiment 1.
2. the preparation of silicon titanium pillared montmorillonite poromerics: with embodiment 1.
3. the preparation of potassium permanganate/silicon titanium pillared montmorillonite matrix material: silicon titanium pillared montmorillonite (12.994g) is evenly spread in the 130ml aqueous solution, form the modified montmorillonoid dispersion liquid; Potassium permanganate solid 8.67g is dissolved in the 35ml water, forms potassium permanganate solution.The modified montmorillonoid dispersion liquid mixed being placed in the ultrasonic dispersing appearance with potassium permanganate solution, ultra-sonic dispersion stirred 20 hours after 2 hours.Suction filtration, washing, oven dry is ground into particle or grind into powder, obtains potassium permanganate/silicon titanium pillared montmorillonite nano composite material 12.280g, productive rate 56.7%.
Embodiment 3
1. the preparation of organo montmorillonite: with embodiment 1.
2. the preparation of silicon titanium pillared montmorillonite poromerics: with embodiment 1.
3. the preparation of potassium permanganate/silicon titanium pillared montmorillonite matrix material material: silicon titanium pillared montmorillonite (12.994g) is evenly spread in the 130ml aqueous solution, form the modified montmorillonoid dispersion liquid; Potassium permanganate solid 6.50g is dissolved in the 26ml water, forms potassium permanganate solution.Above-mentioned modified montmorillonoid dispersion liquid mixed being placed in the ultrasonic dispersing appearance with potassium permanganate solution, ultra-sonic dispersion stirred 22 hours after 1.5 hours.Suction filtration, washing, oven dry is ground into particle or grind into powder, obtains potassium permanganate/silicon titanium pillared montmorillonite nano composite material 10.056g, productive rate 51.6%.
Claims (6)
1. potassium permanganate/nano combined hydrogen-storing material of silicon titanium pillared montmorillonite is potassium permanganate to be inserted evenly the silicon titanium is pillared to be taken off in the native lamella and get.
2. potassium permanganate/nano combined hydrogen-storing material of silicon titanium pillared montmorillonite according to claim 1, it is characterized in that: the mass ratio of said potassium permanganate and silicon titanium pillared montmorillonite is 1:1～1:2.
3. like the preparation method of the said potassium permanganate of claim 1/nano combined hydrogen-storing material of silicon titanium pillared montmorillonite, be silicon titanium pillared montmorillonite to be distributed to form silicon titanium pillared montmorillonite dispersion liquid in water or the acetic acid aqueous solution; The potassium permanganate solid is soluble in water, form potassium permanganate solution; Silicon titanium pillared montmorillonite dispersion liquid is mixed being placed in the ultrasonic dispersing appearance with potassium permanganate solution, ultra-sonic dispersion stirred after 1 ~ 2 hour 20 ~ 24 hours again; Suction filtration, washing, oven dry is ground into particle or grind into powder, obtains potassium permanganate/nano combined oxygen-making agent of silicon titanium pillared montmorillonite.
4. like the preparation method of the said potassium permanganate of claim 3/nano combined hydrogen-storing material of silicon titanium pillared montmorillonite, it is characterized in that: in the said silicon titanium pillared montmorillonite dispersion liquid, the mass percent of silicon titanium pillared montmorillonite is 5% ~ 15%.
5. like the preparation method of the said potassium permanganate of claim 3/nano combined oxygen-making agent of silicon titanium pillared montmorillonite, it is characterized in that: in the said potassium permanganate solution, the mass percent of potassium permanganate is 12% ~ 25%.
6. like the preparation method of the said potassium permanganate of claim 3/nano combined hydrogen-storing material of silicon titanium pillared montmorillonite; It is characterized in that: in the mixed system of said silicon titanium pillared montmorillonite dispersion liquid and potassium permanganate solution, the mass ratio of potassium permanganate and silicon titanium pillared montmorillonite is 1:1～1:2.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107159191A (en) * | 2017-05-26 | 2017-09-15 | 四川大学 | Support type denitrating catalyst based on column clay and preparation method thereof |
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| CN101837278A (en) * | 2009-03-18 | 2010-09-22 | 中国科学院大连化学物理研究所 | Oxygen adsorbent, preparation method and application thereof |
| US20110082031A1 (en) * | 2009-10-05 | 2011-04-07 | Gm Global Technology Operations, Inc. | Method and system for monitoring a hydrocarbon adsorber |
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| CN101837278A (en) * | 2009-03-18 | 2010-09-22 | 中国科学院大连化学物理研究所 | Oxygen adsorbent, preparation method and application thereof |
| US20110082031A1 (en) * | 2009-10-05 | 2011-04-07 | Gm Global Technology Operations, Inc. | Method and system for monitoring a hydrocarbon adsorber |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107159191A (en) * | 2017-05-26 | 2017-09-15 | 四川大学 | Support type denitrating catalyst based on column clay and preparation method thereof |
| CN107159191B (en) * | 2017-05-26 | 2020-01-24 | 四川大学 | Supported denitration catalyst based on pillared clay and preparation method thereof |
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Application publication date: 20121010 |