CN104341009A - Method for preparing nano mesoporous ferric oxide - Google Patents
Method for preparing nano mesoporous ferric oxide Download PDFInfo
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- CN104341009A CN104341009A CN201410552469.6A CN201410552469A CN104341009A CN 104341009 A CN104341009 A CN 104341009A CN 201410552469 A CN201410552469 A CN 201410552469A CN 104341009 A CN104341009 A CN 104341009A
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Abstract
The invention discloses a method for preparing nano mesoporous ferric oxide. The method comprises the steps of preparing a carboxylation modified nano-cellulose dispersion, adding a ferric salt solution into the carboxylation modified nano-cellulose dispersion, adjusting pH with ammonia water, and after ferric ions in the ferric salt are adsorbed nano-fibers to form a complex, dehydrating and firing, thereby obtaining a product, namely nano mesoporous ferric oxide with uniform pore size and good dispersity. Compared with the prior art, the method has the beneficial effects that carboxylation modified nano-cellulose has better adsorbability to the ferric ions, so that ferric oxide particles are not prone to agglomeration, the pore size is more uniform, and the dispersity is better.
Description
Technical field
The present invention relates to the preparation field of mesoporous iron oxide, particularly a kind of preparation method of mesoporous nano ferric oxide.
Background technology
Ferric oxide has alkaline-resisting, high temperature resistant (heat fusion joint reaches 1565 DEG C), salt spray resistance, nontoxic, easy acquisition, inexpensive advantage, the hardness also had and magnetic, it is a kind of important transition metal oxide, at present in catalysis, dyestuff, magneticsubstance, the aspect such as gas sensitive and lithium ion battery material is widely used.And mesoporous iron oxide is applied except these, can also as pharmaceutical carrier.The preparation method at present with the ferric oxide of nano aperture mainly contains sol-gel method, template, hydrothermal method, coprecipitation method etc.The ferric oxide pattern of the nano aperture that diverse ways prepares is different, and in preparation process, the reunion of ferric oxide particles is difficult to control.Compared to solid ferric oxide particles, the mesoporous iron oxide with nano aperture has the advantage that density is low, specific surface area is high, is conducive to the application of ferric oxide.But still lack at present and a kind ofly prepare good dispersity, there is nano aperture and the method for the mesoporous iron oxide of uniform pore diameter.
Summary of the invention
The present invention in order to the uneven problem in the mesoporous iron oxide bad dispersibility with nano aperture, the aperture that solve prior art and prepare, and provides a kind of preparation method of mesoporous nano ferric oxide.
The technical scheme that the present invention solves the problems of the technologies described above is as follows:
A preparation method for mesoporous nano ferric oxide, carries out according to the following steps:
1. prepare the nano-cellulose aqueous dispersions of carboxylated modification:
Take 1g Mierocrystalline cellulose, 0.15g TEMPO, 1.68g NaClO
2joining volume with the 8ml mass concentration NaClO solution that is 15% is in the buffer solution of sodium phosphate of 200ml pH6.5, stirring reaction 24 hours under 45 DEG C of conditions, add dehydrated alcohol termination reaction, solution is poured into stratification in Erlenmeyer flask, outwell supernatant liquid, respectively successively with volumetric concentration be 50% second alcohol and water displacement, obtain clean, dense gelatinous carboxylated modified-cellulose dispersion liquid, again high pressure homogenizer process is carried out to dense gelatinous carboxylated modified-cellulose dispersion liquid, obtain the carboxylated modified nanometer cellulose aqueous dispersions of over dry.
2. the preparation of mesoporous nano ferric oxide:
In the carboxylated modified nanometer cellulose dispersion liquid obtained containing 0.2g over dry step 1, add the ferric salt solution that 40 ~ 100ml concentration is 0.1 ~ 1.0mol/l, pH is regulated to be 7.0 ~ 11 with strong aqua, after the iron ion treating in trivalent iron salt is adsorbed on and nanofiber forms mixture, dehydration, by the calcination 2 ~ 8 hours under 400 DEG C ~ 650 DEG C conditions of gained mixture, products therefrom is the mesoporous iron oxide with nano aperture.
The invention has the beneficial effects as follows:
The present invention has better adsorptivity through the nano-cellulose of carboxylated modification to iron ion, and ferric oxide particles is not easily reunited, aperture evenly, dispersed better.
Embodiment
Below in conjunction with embodiment, the invention will be further described.
Embodiment 1
A preparation method for mesoporous nano ferric oxide, carries out according to the following steps:
1. prepare the nano-cellulose aqueous dispersions of carboxylated modification: take 1g Mierocrystalline cellulose, 0.15gTEMPO, 1.68g NaClO by quality
2joining volume with the 8ml mass concentration NaClO solution that is 15% is in the buffer solution of sodium phosphate of the pH6.5 of 200ml, stirring reaction 24 hours under 45 DEG C of conditions, add dehydrated alcohol termination reaction, solution is poured into stratification in Erlenmeyer flask, outwell supernatant liquid, successively respectively with volumetric concentration be 50% ethanol, water displacement, obtain clean, dense gelatinous carboxylated modified-cellulose dispersion liquid, again high-pressure homogeneous process is carried out to dense gelatinous carboxylated modified-cellulose dispersion liquid, obtain the carboxylated modified nanometer cellulose dispersion liquid of over dry;
2. the preparation of mesoporous nano ferric oxide:
In the above-mentioned dispersion liquid of the carboxylated modified nanometer cellulose of over dry obtained in 0.2g step 1, add the ferric salt solution that 40ml mass concentration is 0.1mol/l, pH to 7.0 is regulated with ammoniacal liquor, after the iron ion treating in trivalent iron salt is adsorbed on and nanofiber forms mixture, dehydration, by the calcination 2 hours under 400 DEG C of conditions of gained mixture, the aperture of gained mesoporous iron oxide reaches nano level, uniform pore diameter and good dispersity.
Embodiment 2
A preparation method for mesoporous nano ferric oxide, carries out according to the following steps:
1. prepare the nano-cellulose aqueous dispersions of carboxylated modification:
Identical with the step 1 of embodiment 1.
2. the preparation of mesoporous nano ferric oxide:
In the above-mentioned dispersion liquid of the carboxylated modified nanometer cellulose of over dry obtained in 0.2g step 1, add the iron salt solutions that 70ml mass concentration is 0.5mol/l, pH to 9.0 is regulated with ammoniacal liquor, after the iron ion treating in molysite is adsorbed on and nanofiber forms mixture, dehydration, by the calcination 5 hours under 525 DEG C of conditions of gained mixture, the aperture of gained mesoporous iron oxide reaches nano level, uniform pore diameter and good dispersity.
Embodiment 3
A preparation method for mesoporous nano ferric oxide, carries out according to the following steps:
1. prepare the nano-cellulose aqueous dispersions of carboxylated modification:
Identical with the step 1 of embodiment 1.
2. the preparation of mesoporous nano ferric oxide:
In the above-mentioned dispersion liquid of the carboxylated modified nanometer cellulose of over dry obtained in 0.2g step 1, add the iron salt solutions that 100ml mass concentration is 1.0mol/l, pH to 11 is regulated with ammoniacal liquor, after the iron ion treating in molysite is adsorbed on and nanofiber forms mixture, dehydration, by the calcination 8 hours under 650 DEG C of conditions of gained mixture, the aperture of gained mesoporous iron oxide reaches nano level, uniform pore diameter and good dispersity.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (1)
1. a preparation method for mesoporous nano ferric oxide, is characterized in that, method is carried out according to the following steps:
(1) the nano-cellulose aqueous dispersions of carboxylated modification is prepared:
Take 1g Mierocrystalline cellulose, 0.15g TEMPO, 1.68g NaClO
2joining volume with the 8ml mass concentration NaClO solution that is 15% is in the buffer solution of sodium phosphate of 200ml pH6.5, stirring reaction 24 hours under 45 DEG C of conditions, add dehydrated alcohol termination reaction, solution is poured into stratification in Erlenmeyer flask, outwell supernatant liquid, respectively successively with volumetric concentration be 50% second alcohol and water displacement, obtain clean, dense gelatinous carboxylated modified-cellulose dispersion liquid, again high pressure homogenizer process is carried out to dense gelatinous carboxylated modified-cellulose dispersion liquid, obtain carboxylated modified nanometer cellulose aqueous dispersions;
(2) preparation of mesoporous nano ferric oxide:
In the carboxylated modified nanometer cellulose aqueous dispersions obtained containing 0.2g over dry step (1), add the ferric salt solution that 40 ~ 100ml concentration is 0.1 ~ 1.0mol/l, pH is regulated to be 7.0 ~ 11 with strong aqua, after the iron ion treating in trivalent iron salt is adsorbed on and nanofiber forms mixture, dehydration, by the calcination 2 ~ 8 hours under 400 DEG C ~ 650 DEG C conditions of gained mixture, products therefrom is the mesoporous iron oxide with nano aperture.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105235090A (en) * | 2015-09-28 | 2016-01-13 | 湖北华强科技有限责任公司 | Red butyl rubber mixing technology |
| CN110040709A (en) * | 2019-04-08 | 2019-07-23 | 中科(马鞍山)新材科创园有限公司 | A method of regeneration prepares LiFePO4 from waste lithium iron phosphate battery |
| CN111992191A (en) * | 2020-08-26 | 2020-11-27 | 广西大学 | Rapid high-capacity intelligent cellulose-based oil absorption material and preparation method and application thereof |
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| CN101143733A (en) * | 2007-08-28 | 2008-03-19 | 武汉大学 | Method for preparing magnetic ferric oxide nano particles |
| CN103157515A (en) * | 2013-02-01 | 2013-06-19 | 北京大学深圳研究院 | Catalyst and method for performing carboxyl reaction on C6 of bacterial cellulose |
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| CN101143733A (en) * | 2007-08-28 | 2008-03-19 | 武汉大学 | Method for preparing magnetic ferric oxide nano particles |
| CN103157515A (en) * | 2013-02-01 | 2013-06-19 | 北京大学深圳研究院 | Catalyst and method for performing carboxyl reaction on C6 of bacterial cellulose |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105235090A (en) * | 2015-09-28 | 2016-01-13 | 湖北华强科技有限责任公司 | Red butyl rubber mixing technology |
| CN110040709A (en) * | 2019-04-08 | 2019-07-23 | 中科(马鞍山)新材科创园有限公司 | A method of regeneration prepares LiFePO4 from waste lithium iron phosphate battery |
| CN111992191A (en) * | 2020-08-26 | 2020-11-27 | 广西大学 | Rapid high-capacity intelligent cellulose-based oil absorption material and preparation method and application thereof |
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| CN104341009B (en) | 2016-05-04 |
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