CN101532169A - Method for hydrothermally synthesizing Alpha-iron oxide red nanocrystalline - Google Patents
Method for hydrothermally synthesizing Alpha-iron oxide red nanocrystalline Download PDFInfo
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- CN101532169A CN101532169A CN200910068132A CN200910068132A CN101532169A CN 101532169 A CN101532169 A CN 101532169A CN 200910068132 A CN200910068132 A CN 200910068132A CN 200910068132 A CN200910068132 A CN 200910068132A CN 101532169 A CN101532169 A CN 101532169A
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Abstract
The invention relates to a method for synthesizing Alpha-iron oxide red nanocrystalline of different shapes by hydrothermal control, belonging to the technical field of inorganic nano material preparation technology. In the invention, water is taken as a solvent, yellow potassium ferrocyanide is dissolved in water, and hydrogen peroxide is added as an oxidant, the ion concentration of hexacyanoferrate is controlled within the range of 0.01-1mol/L, the volume ratio between water and hydrogen peroxide is 0-10:1, and precursor solution is obtained. Then, the precursor is put in a hermetic reaction kettle lined with polytetrafluoroethylene for 0.5-48 hours of crystallization at the temperature of 100-180 DEG C to obtain the Alpha-iron oxide red nanocrystalline. The Alpha-iron oxide red synthesized by the method is uniform in size distribution, controllable in shape, low in cost, simple in equipment, safe and easy in operation, excellent in technique repetition and stable in product quality, and is suitable for industrial large scale production.
Description
Technical field
The invention belongs to the inorganic nano material preparation process technology field, relate to the preparation method of inorganic nano material, specifically the nanocrystalline synthetic method of alpha-ferric oxide.Can use material of construction, coating, plastics, rubber, pottery, glass, papermaking,
Cultivate, aspect such as linoleum, art painting, medicine, makeup, catalyzer, senior correct grinding material, magnetic pipe recording material, feed for pet additive.
Background technology
Alpha-ferric oxide is modal a kind of in the ferriferous oxide, also is a kind of semiconductor material, as a kind of important industrial raw material and product, obtains people about the performance of ferric oxide and preparation research always and gets extensive concern.In the ferric oxide of all consumption, have 80% to be chemosynthesis in the world, be called synthetic iron oxide.Have only 20% usefulness natural mineral to process, be called natural iron oxide.Purity height, particle diameter are evenly neat owing to having, size is easily done control for synthetic iron oxide, thereby form and aspect are good, and application performance is good.With respect to conventional block ferric oxide, nano-sized iron oxide has good weather resisteant, catalytic, photostabilization, magnetic and ultraviolet ray is had good absorption and shielding effect, and it is mainly used in aspects such as transparent pigment, gas sensitive, catalyzer symphysis thing medical material.
The present invention is to be raw material with the yellow prussiate of potash, prepares monodispersed spheric, cubical, netted and dendritic alpha-titanium dioxide two iron.For netted alpha-ferric oxide preparation of nano crystal, also bright at present for reporting.The present invention also provides a simple synthetic route for the netted nanocrystalline preparation of alpha-ferric oxide.
Summary of the invention
The synthetic method that provides a kind of alpha-ferric oxide nanocrystalline is provided meaning of the present invention, this method has synthetic alpha-ferric oxide uniform in size distribution, pattern and controlled amount, the degree of crystallinity height, operational safety, easy, good process repeatability, the advantage of constant product quality.
Characteristics of the present invention are to use the title complex yellow prussiate of potash as raw material, need not to add mineralizer simultaneously, make operation simpler, and cost is cheaper.
Alpha-ferric oxide synthesis step is as follows:
Yellow prussiate of potash is dissolved in the distilled water, and controlling six cyanogen, to close iron concentration be 0.01-1mol/L, adds hydrogen peroxide as oxygenant, and the volume ratio of water and hydrogen peroxide is 3:1, obtains precursor solution.Above-mentioned precursor solution is loaded in the airtight reactor that is lined with tetrafluoroethylene 100-180 ℃ of heating crystallizations 0.5-48 hours, treat that the crystallization afterreaction still temperature that finishes reduces to room temperature, product water is washed till neutrality, and it is nanocrystalline to obtain alpha-ferric oxide in 3 hours 120 ℃ of vacuum-dryings then.
Description of drawings
Accompanying drawing 1 is the X-ray powder diffraction figure (by preparation in the embodiment 1) of synthetic alpha-ferric oxide.
Specific embodiments
Embodiment 1
In the 50mL beaker, add 15mL distilled water, under agitation add the 1.06g yellow prussiate of potash again, continue to be stirred to yellow prussiate of potash and dissolve fully, add the 5mL hydrogen peroxide then, continue to stir after 10 minutes, above-mentioned solution is changed in the 50mL reactor, 140 ℃ of crystallization 3 hours, the reaction afterreaction still that finishes naturally cooled to room temperature, the gained red precipitate with deionized water wash to neutral, products therefrom gets final product 120 ℃ of following vacuum-dryings 3 hours.
Embodiment 2
Crystallization time in the embodiment 1 is become 6 hours, and other condition is constant.
Embodiment 3
Crystallization time in the embodiment 1 is become 9 hours, and other condition is constant.
Embodiment 4
Crystallization time in the embodiment 1 is become 12 hours, and other condition is constant.
Embodiment 5
Crystallization time in the embodiment 1 is become 15 hours, and other condition is constant.
Embodiment 6
Crystallization time in the embodiment 1 is become 21 hours, and other condition is constant.
Embodiment 7
Crystallization time in the embodiment 1 is become 25 hours, and other condition is constant.
Embodiment 8
Crystallization time in the embodiment 1 is become 48 hours, and other condition is constant.
Embodiment 9
The quality of yellow prussiate of potash in the embodiment 1 is become 0.53g, and other condition is constant.
Embodiment 10
The quality of yellow prussiate of potash in the embodiment 1 is become 2.12g, and other condition is constant.
The present invention can describe in detail by embodiment, but the invention is not restricted to above embodiment.
Claims (4)
1. the nanocrystalline hydrothermal synthesis method of alpha-ferric oxide is characterized in that comprising the steps:
A. reacting precursor formulations prepared from solutions: yellow prussiate of potash is dissolved in distilled water, and controlling six cyanogen, to close iron concentration be 0.01-1mol/L, adds hydrogen peroxide as oxygenant, and the volume ratio of distilled water and hydrogen peroxide is 0-10:1, obtains precursor solution;
B. the synthetic alpha-ferric oxide of hydro-thermal is nanocrystalline: above-mentioned precursor is loaded on heating crystallization in the airtight reactor that is lined with tetrafluoroethylene, treat that the crystallization afterreaction still temperature that finishes reduces to room temperature, product water is washed till neutrality, and it is nanocrystalline to obtain alpha-ferric oxide in 3 hours 120 ℃ of vacuum-dryings then.Wherein, crystallization temperature is 100-180 ℃, and crystallization time is 0.5-48 hours.
2. the nanocrystalline hydrothermal synthesis method of alpha-ferric oxide that requires according to right 1 is characterized in that described molysite is a yellow prussiate of potash.
3. the nanocrystalline hydrothermal synthesis method of alpha-ferric oxide that requires according to right 1 is characterized in that described hydrogen peroxide concentration is 25-30%.
4. the nanocrystalline hydrothermal synthesis method of alpha-ferric oxide that requires according to right 1 is characterized in that described crystallization temperature preferentially is selected from 140 ℃.
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| CN200910068132A CN101532169A (en) | 2009-03-16 | 2009-03-16 | Method for hydrothermally synthesizing Alpha-iron oxide red nanocrystalline |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101913658A (en) * | 2010-09-16 | 2010-12-15 | 厦门大学 | Alpha type ferric oxide and preparation method thereof |
| CN101928043A (en) * | 2010-09-16 | 2010-12-29 | 厦门大学 | Alpha-type ferric oxide micron ball and preparation method thereof |
| CN103880091A (en) * | 2012-12-20 | 2014-06-25 | 中国科学院大连化学物理研究所 | Preparation method of hexagonal nano iron oxide |
| CN104844016A (en) * | 2015-04-03 | 2015-08-19 | 福州大学 | Production method for depositing iron oxide film on ITO conductive glass |
| CN105219345A (en) * | 2015-10-16 | 2016-01-06 | 上海纳米技术及应用国家工程研究中心有限公司 | A kind of preparation method of Z 250 iron nucleocapsid structure-Graphene composite wave-suction material |
| CN108128813A (en) * | 2018-03-08 | 2018-06-08 | 中国科学院青海盐湖研究所 | The preparation method of alpha-type ferric oxide |
| CN108190966A (en) * | 2018-03-08 | 2018-06-22 | 中国科学院青海盐湖研究所 | The preparation method of alpha-type ferric oxide |
| CN108217752A (en) * | 2018-03-08 | 2018-06-29 | 中国科学院青海盐湖研究所 | A kind of preparation method of alpha-type ferric oxide |
| CN108328660A (en) * | 2018-03-08 | 2018-07-27 | 中国科学院青海盐湖研究所 | A kind of preparation method of alpha-type ferric oxide |
| RU2752756C1 (en) * | 2020-08-19 | 2021-08-02 | федеральное государственное бюджетное образовательное учреждение высшего образования "Санкт-Петербургский горный университет" | Apparatus for producing nanodispersed metal oxides |
-
2009
- 2009-03-16 CN CN200910068132A patent/CN101532169A/en active Pending
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101913658A (en) * | 2010-09-16 | 2010-12-15 | 厦门大学 | Alpha type ferric oxide and preparation method thereof |
| CN101928043A (en) * | 2010-09-16 | 2010-12-29 | 厦门大学 | Alpha-type ferric oxide micron ball and preparation method thereof |
| CN103880091A (en) * | 2012-12-20 | 2014-06-25 | 中国科学院大连化学物理研究所 | Preparation method of hexagonal nano iron oxide |
| CN103880091B (en) * | 2012-12-20 | 2015-05-06 | 中国科学院大连化学物理研究所 | Preparation method of hexagonal nano iron oxide |
| CN104844016A (en) * | 2015-04-03 | 2015-08-19 | 福州大学 | Production method for depositing iron oxide film on ITO conductive glass |
| CN105219345A (en) * | 2015-10-16 | 2016-01-06 | 上海纳米技术及应用国家工程研究中心有限公司 | A kind of preparation method of Z 250 iron nucleocapsid structure-Graphene composite wave-suction material |
| CN108128813A (en) * | 2018-03-08 | 2018-06-08 | 中国科学院青海盐湖研究所 | The preparation method of alpha-type ferric oxide |
| CN108190966A (en) * | 2018-03-08 | 2018-06-22 | 中国科学院青海盐湖研究所 | The preparation method of alpha-type ferric oxide |
| CN108217752A (en) * | 2018-03-08 | 2018-06-29 | 中国科学院青海盐湖研究所 | A kind of preparation method of alpha-type ferric oxide |
| CN108328660A (en) * | 2018-03-08 | 2018-07-27 | 中国科学院青海盐湖研究所 | A kind of preparation method of alpha-type ferric oxide |
| RU2752756C1 (en) * | 2020-08-19 | 2021-08-02 | федеральное государственное бюджетное образовательное учреждение высшего образования "Санкт-Петербургский горный университет" | Apparatus for producing nanodispersed metal oxides |
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Open date: 20090916 |