CN102674472A - Rod-shaped nanometer ferric oxide and method for preparing same - Google Patents
Rod-shaped nanometer ferric oxide and method for preparing same Download PDFInfo
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- CN102674472A CN102674472A CN2012101673391A CN201210167339A CN102674472A CN 102674472 A CN102674472 A CN 102674472A CN 2012101673391 A CN2012101673391 A CN 2012101673391A CN 201210167339 A CN201210167339 A CN 201210167339A CN 102674472 A CN102674472 A CN 102674472A
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- red stone
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Abstract
The invention relates to a method for preparing rod-shaped nanometer ferric oxide. The method particularly includes using rod-shaped nanometer cellulous, which is prepared by natural cellulous, as a template; dissolving FeCl3*6H2O in nanometer cellulous aqueous solution with a certain concentration; adding a proper quantity of urea, performing hydrothermal synthesis reaction for 2 to 24 hours at the temperature ranging from 110 DEG C to 150 DEG C; centrifugally separating and washing the prepared rod-shaped nanometer ferric oxide after the reaction is completed, and drying the prepared rod-shaped nanometer ferric oxide to obtain brick-red ferric oxide powder. The nanometer cellulous is used as the template to prepare the nanometer ferric oxide, the method is simple in process, the size of a product is uniform, and dispersibility is good.
Description
Technical field:
The present invention relates to a kind of rod-like nano red stone (α-Fe
2O
3) the preparation method, this method especially with the clubbed nano-cellulose of natural cellulose preparation as template.
Background technology:
Nano material and nanostructure be the most dynamic in the current investigation of materials field, the future economy and social development are had the very research object of material impact, also be the most active in the nanosecond science and technology, near the important component part of using.Nano-sized iron oxide has good chemical stability, light stability and photocatalytic, is widely used in fields such as luster coating, printing ink, leather, automobile finish, the high magnetic recording material of electronics, catalyzer and biomedical engineering.
Common nano-sized iron oxide compound method has the precipitator method, sol-gel method, freeze-drying, the hot method of hydrothermal/solvent etc.And use petroleum base tensio-active agents and macromolecule complex agent in the preparation process to play control action kou to red stone size and pattern more.Li Ling (number of patent application: 01130089.2) invented a kind of with tensio-active agents such as X 2073, Triple Pressed Stearic Acid oxygen Vinyl Ether, fatty acid loss water sorbit esters; The agent of macromolecule complex such as Z 150PH, SEPIGEL 305 prepares the method for nano oxidized iron powder as stablizer.(number of patent application: 02137552.6) invented a kind of is the method that stablizer prepares nano-sized iron oxide with TX10 (OP-10) to Shi Liyi etc.Brave grade is gathered by Sui, and (number of patent application: 03111879.8) having invented a kind of is the method that stablizer prepares nano-sized iron oxide with the octadecyl sodium sulfonate.(number of patent application: 200510023582.6) invented a kind of is stablizer with Z 150PH (PVA) to Li Zhen etc., and the control particle diameter prepares the method for nano-sized iron oxide.Mostly the stablizer that uses in the above-mentioned patent is petroleum chemicals, and the red stone pattern of preparation is random nanoparticle.
Summary of the invention:
The present invention proposes a kind of rod-like nano red stone and preparation method thereof; This method especially with the clubbed nano-cellulose of natural cellulose preparation as template, purpose is to be used for the biomass-based material substitution petroleum-based products of natural reproducible the preparation of nano material.
Technical scheme of the present invention is: a kind of preparation method of rod-like nano red stone, with Hydrothermal Preparation, the preparation method comprises the steps:
, mass concentration adds FeCl respectively in being 0.5%～5% clubbed nano-cellulose dispersion liquid
36H
2O and urea mix, and wherein, the ratio of the corresponding every gram clubbed nano-cellulose of the amount of substance of Fe is 2.5 * 10
-4～1.0 * 10
-2Mol/g; Under 110～150 ℃, reacted 2～24 hours at last, with the brick-red product spinning washing that obtains, lyophilize obtains the rod-like nano croci.
FeCl
36H
2The ratio of the amount of substance of O and urea is between 1:5～1:50.
The rod-like nano red stone, size is between long 50～1000 nm, and in wide 5～50 nm scopes, crystal formation is α-Fe
2O
3
Size is between long 100～300 nm, wide 5～30 nm.
Beneficial effect:
The inventive method preparation technology is simple, need not to use petroleum base tensio-active agent and macromolecule complex agent, pollutes for a short time, is the rod-like nano red stone technology of preparing of a kind of green, low-carbon (LC).The nano-sized iron oxide purity of preparation is high, pattern is single, have good dispersiveness.Therefore be that template prepares the rod-like nano red stone with the nano-cellulose, extremely wide research and application prospect are arranged.
Description of drawings:
Fig. 1 is the rod-like nano red stone (α-Fe of embodiment 2 preparations
2O
3) the TEM figure of different resolution.
Fig. 2 is the XRD figure of the rod-like nano red stone of embodiment 2 preparations.
Embodiment:
For better implement the present invention, the spy illustrates it, but is not limitation of the present invention.
The used clubbed nano-cellulose of the present invention is to be ZL200910025794.6 according to the patent No., and the method that name is called among a kind of preparation method of clubbed nano-cellulose prepares.
A kind of rod-like nano red stone (α-Fe
2O
3) the preparation method, it is characterized in that the preparation method comprises the steps:
A. the certain amount of nano Mierocrystalline cellulose is joined in the deionized water, through ultra-sonic dispersion, the preparation mass concentration is 0.5%～5% nano-cellulose dispersion liquid.
B. in the dispersion liquid of nano-cellulose, add a certain amount of FeCl
36H
2O mixes, and makes that the cellulosic ratio of the corresponding every gram of Fe amount of substance is 2.5 * 10
-4～1.0 * 10
-2Mol/g.
C. at nano-cellulose and FeCl
36H
2Add certain amount of urea in the mixed solution of O, make FeCl
36H
2The amount of substance of O and urea is than between 1:5～1:50.
D. with the mixing solutions of above-mentioned three kinds of materials under 110～150 ℃ of conditions, reacted 2～24 hours, the brick-red sample spinning washing with preparation through lyophilize, obtains rod-like nano red stone (α-Fe
2O
3) powder.
Embodiment 1:In the beaker of 50 mL, add 0.50 g FeCl respectively
36H
2O and 2.25 g urea are that 1% nano-cellulose suspension-s mixes with 40 mL concentration, obtain saffron suspension liquid, and wherein the concentration of Fe is 4.6 * 10
-2Mol/L.Behind magnetic agitation 30 min, above-mentioned solution is joined in the reaction kettle that gathers the tetrafluoro liner of 50 mL reaction 12 h under 110 ℃ of conditions.After treating that temperature natural is reduced to room temperature, bolarious product is carried out spinning, and, after lyophilize, obtain nano oxidized iron powder with deionized water wash number time.
Embodiment 2:In the beaker of 50 mL, add 0.60 g FeCl respectively
36H
2O and 3.75 g urea are that 2% nano-cellulose suspension-s mixes with 30 mL concentration, obtain saffron suspension liquid, and wherein the concentration of Fe is 7.4 * 10
-2Mol/L.Behind magnetic agitation 30 min, above-mentioned solution is joined in the reaction kettle that gathers the tetrafluoro liner of 50 mL reaction 6 h under 130 ℃ of conditions.After treating that temperature natural is reduced to room temperature, bolarious product is carried out spinning, and, after lyophilize, obtain nano oxidized iron powder with deionized water wash number time.
Embodiment 3:In the beaker of 100 mL, add 1.00 g FeCl respectively
36H
2O and 8 g urea are that 4% nano-cellulose suspension-s mixes with 50 mL concentration, obtain saffron suspension liquid, and wherein the concentration of Fe is 7.41 * 10
-2Mol/L.Behind magnetic agitation 30 min, above-mentioned solution is joined in the reaction kettle that gathers the tetrafluoro liner of 100 mL reaction 2 h under 140 ℃ of conditions.After treating that temperature natural is reduced to room temperature, bolarious product is carried out spinning, and, after lyophilize, obtain nano oxidized iron powder with deionized water wash number time.
Claims (4)
1. the preparation method of a rod-like nano red stone, is characterized in that the preparation method comprises the steps: with Hydrothermal Preparation
, mass concentration adds FeCl respectively in being 0.5%～5% clubbed nano-cellulose dispersion liquid
36H
2O and urea mix, and wherein, the ratio of the corresponding every gram clubbed nano-cellulose of the amount of substance of Fe is 2.5 * 10
-4～1.0 * 10
-2Mol/g; Under 110～150 ℃, reacted 2～24 hours at last, with the brick-red product spinning washing that obtains, lyophilize obtains the rod-like nano croci.
2. the preparation method of rod-like nano red stone according to claim 1 is characterized in that, FeCl
36H
2The ratio of the amount of substance of O and urea is between 1:5～1:50.
3. the rod-like nano red stone that the preparation method of rod-like nano red stone according to claim 1 obtains is characterized in that, size is between long 50～1000 nm, and in wide 5～50 nm scopes, crystal formation is α-Fe
2O
3
4. the rod-like nano red stone that the preparation method of rod-like nano red stone according to claim 1 obtains is characterized in that, size is between long 100～300 nm, wide 5～30 nm.
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|---|---|---|---|
| CN2012101673391A CN102674472A (en) | 2012-05-28 | 2012-05-28 | Rod-shaped nanometer ferric oxide and method for preparing same |
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| CN2012101673391A CN102674472A (en) | 2012-05-28 | 2012-05-28 | Rod-shaped nanometer ferric oxide and method for preparing same |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106745306A (en) * | 2016-12-09 | 2017-05-31 | 江苏大学 | A kind of α Fe2O3The preparation method of magnetic Nano rod |
| CN107162062A (en) * | 2017-06-19 | 2017-09-15 | 华南理工大学 | A kind of rod-like nano iron oxide and preparation method thereof |
| CN113663737A (en) * | 2021-08-19 | 2021-11-19 | 南京医科大学康达学院 | CMC-Fe-based microsphere and preparation method and application thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101509209A (en) * | 2009-03-10 | 2009-08-19 | 中国林业科学研究院林产化学工业研究所 | Method of preparing clubbed nano-cellulose |
-
2012
- 2012-05-28 CN CN2012101673391A patent/CN102674472A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101509209A (en) * | 2009-03-10 | 2009-08-19 | 中国林业科学研究院林产化学工业研究所 | Method of preparing clubbed nano-cellulose |
Non-Patent Citations (1)
| Title |
|---|
| 刘鹤: "纤维素纳米晶体及其复合物的制备与应用研究", 《中国博士学位论文全文数据库 工程科技Ⅰ辑》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106745306A (en) * | 2016-12-09 | 2017-05-31 | 江苏大学 | A kind of α Fe2O3The preparation method of magnetic Nano rod |
| CN106745306B (en) * | 2016-12-09 | 2018-12-14 | 江苏大学 | A kind of α-Fe2O3The preparation method of magnetic Nano stick |
| CN107162062A (en) * | 2017-06-19 | 2017-09-15 | 华南理工大学 | A kind of rod-like nano iron oxide and preparation method thereof |
| CN113663737A (en) * | 2021-08-19 | 2021-11-19 | 南京医科大学康达学院 | CMC-Fe-based microsphere and preparation method and application thereof |
| CN113663737B (en) * | 2021-08-19 | 2023-08-15 | 南京医科大学康达学院 | CMC-Fe-based microsphere, and preparation method and application thereof |
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Application publication date: 20120919 |