CN102863028A - Method of preparing water-soluble iron oxide under room temperature condition - Google Patents
Method of preparing water-soluble iron oxide under room temperature condition Download PDFInfo
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- CN102863028A CN102863028A CN2012103347857A CN201210334785A CN102863028A CN 102863028 A CN102863028 A CN 102863028A CN 2012103347857 A CN2012103347857 A CN 2012103347857A CN 201210334785 A CN201210334785 A CN 201210334785A CN 102863028 A CN102863028 A CN 102863028A
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- iron salt
- iron oxide
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Abstract
The invention discloses a method of preparing a water-soluble iron oxide under a room temperature condition, belonging to the technical field of chemical industry. The method comprises the following steps of; grinding divalent iron salt, trivalent iron salt and a surfactant into a mortar, wherein a molar ratio of the divalent iron salt to the trivalent iron salt is 1: 2, and a molar ratio of the adding amount of the surfactant to the adding amount of the divalent iron salt is 2.5-5: 1; after fully grinding the components in the step 1, adding strong base, and fully grinding, wherein a molar ratio of the adding amount of the strong base to the adding amount of the divalent iron salt is 8: 1; after complete reaction, ultrasonically cleaning for 5-10 minutes by deionized water, centrifuging at 12000 r/min for 20 minutes, dropping solution, and repeating a process of ultrasonically cleaning for 5-10 minutes by the deionized water and dropping the solution for three times so as to obtain the water-soluble iron oxide. The method, provided by the invention, has the advantages that simple operation of the prepared water-soluble iron oxide, easiness in controlling the process, short preparation period, low production cost, small energy consumption, no environmental pollution, and easiness in popularization.
Description
Technical field
The invention belongs to chemical technology field, be specifically related to prepare under a kind of room temperature condition the method for water-soluble iron oxide compound.
Background technology
The water-soluble iron oxide compound is with water miscible tensio-active agent particle surface to be modified as a kind of special functional materials, is evenly dispersed in a kind of uniform and stable colloidal solution that forms in the aqueous solution.Generally with iron and its oxi etc. as magnetic-particle, as tensio-active agent, magnetic-particle is carried out finishing with water soluble molecules.Because water-soluble magnetic nanoparticle has water-soluble and magnetic solid so that magnetic nano-particle in a lot of fields, as magnetic separate, there is important application in the fields such as the target transportation of medicine, magnetic resonance imaging.
Ferriferous oxide common are iron protoxide (FeO), ferric oxide (Fe
2O
3) and Z 250 (Fe
3O
4) etc., be dissolved in acid, the organic solvent such as water insoluble, alkali and ethanol, ether.Ferriferous oxide is the magneticsubstance of commonly using.
The chemical preparation process of water-soluble iron oxide compound comprises that coprecipitation method, pyrolytic decomposition add aftertreatment, hydrothermal method etc. at present.Aforesaid method all must be through reaction or heat treated under the high temperature, and energy consumption is larger, and method is complicated.
Summary of the invention
The object of the present invention is to provide that a kind of energy consumption is low, technique is simple, prepare the method for water-soluble iron oxide compound under the room temperature condition.
Prepare the method for water-soluble iron oxide compound under the room temperature condition of the present invention, comprise the following steps:
1. divalent iron salt, trivalent iron salt and tensio-active agent are ground in mortar, wherein: the mol ratio of divalent iron salt and trivalent iron salt is 1: 2; The mol ratio of tensio-active agent and divalent iron salt add-on is 2.5-5: 1;
2. add highly basic after the component of step 1 is ground fully, fully grind, wherein: the mol ratio of highly basic and divalent iron salt add-on is 8: 1;
Question response fully after, with deionized water ultrasonic cleaning 5-10 minute, the centrifugal 30min of 12000r/min outwelled solution again, the process of extremely solution being outwelled in 5-10 minute with the deionized water ultrasonic cleaning will repeat three times, namely gets the water-soluble iron oxide compound.
The described divalent iron salt of step 1 is a kind of in Iron nitrate, ferrous ammonium sulphate and the ferrous sulfate.
The described tensio-active agent of step 1 is Trisodium Citrate.
The described trivalent iron salt of step 1 is a kind of in iron trichloride and the iron nitrate.
The described highly basic of step 2 is the sodium hydroxide quasi-alkali.
All EDS spectrum peaks of the water-soluble iron oxide powder of the present invention's preparation can contrast according to standard model:
By comparing with national standard, can obtain the kind of element in the sample:
The present invention compared with prior art has following advantage:
1. water-soluble iron Preparation method of the present invention is reacted and is at room temperature carried out, and has overcome the last handling process of complexity in the chemosynthesis, and the highly energy-consuming problem.
2. the chemical equation that carries out in the preparation process of the present invention is:
Fe
+2+2Fe
+3+8NaOH→Fe(OH)
2+4Fe(OH)
3 (1)
And then Fe (OH)
2And Fe (OH)
3Dehydration reaction generates FeFe simultaneously
2O
4:
Fe(OH)
2+2Fe(OH)
3→FeFe
2O
4+4H
2O (2)
3. adopt raw material simple among the preparation method of the present invention, and be the primary chemical raw material all, thereby preparation cost is low.
In a word, adopt the present invention to prepare the water-soluble iron oxide compound simple to operate, technique is easy to control, and preparation cycle is short, and production cost is low, and energy consumption is little, and non-environmental-pollution, is easy to promote.
Description of drawings
Fig. 1 can spectrogram (EDS) for the energy-dispersive spectroscopy that adopts gained water-soluble iron oxide compound of the present invention
Wherein: X-coordinate represents energy (keV), and ordinate zou represents intensity.
Fig. 2 is for adopting the infrared spectrogram of gained water-soluble iron oxide compound of the present invention
Wherein: X-coordinate represents wavelength (cm
-1), ordinate zou represents absorption intensity
Embodiment
Embodiment 1
The method for preparing the water-soluble iron oxide compound under a kind of room temperature condition: with 1 mmole divalent iron salt (in ferrous sulfate, ferrous sulfate, the ammonium Iron nitrate a kind of), 2 mmole trivalent iron salt (iron trichlorides, or iron nitrate) 2.5 mmole tensio-active agents (Trisodium Citrate) mix and add in the mortar fully grinding.Then add 8 mmole highly basic (sodium hydroxide, or potassium hydroxide) continue to grind, after question response is complete, with deionized water ultrasonic cleaning 5-10 minute, the centrifugal 30min of 12000r/min outwelled solution again, the process of extremely solution being outwelled in 5-10 minute with the deionized water ultrasonic cleaning will repeat three times, obtain the black magnetic powder, EDS is accredited as ferriferous oxide, and collection of illustrative plates as shown in Figure 1.Contain the elements such as C, O, Na, Si, Fe, Cu, Zn among the EDS, wherein Cu, Si, Zn are from substrate.The Fourier transform infrared spectroscopy figure of sample contrasts 1616,1385cm with the infrared spectra of pure citric acid as shown in Figure 2
-1COO in the corresponding Trisodium Citrate in the peak that the place occurs
-, the vibrations of C-O key, there is the existence of citrate on the surface of ferriferous oxide that preparation is described, so that product can be water-soluble.
Embodiment 2
The method for preparing the water-soluble iron oxide compound under a kind of room temperature condition: 1 mmole divalent iron salt (in ferrous sulfate, ferrous sulfate, the ammonium Iron nitrate a kind of), 2 mmole trivalent iron salt (iron trichlorides, or iron nitrate) 3.75 mmole tensio-active agents (Trisodium Citrate) mix and add in the mortar fully grinding.Then add 0.32g highly basic (sodium hydroxide, or potassium hydroxide) continue to grind, after question response is complete, with deionized water ultrasonic cleaning 5-10 minute, the centrifugal 30min of 12000r/min outwells solution again, and the process of extremely solution being outwelled in 5-10 minute with the deionized water ultrasonic cleaning will repeat three times, obtain the black magnetic powder, be accredited as ferriferous oxide through EDS.
Embodiment 3
The method for preparing the water-soluble iron oxide compound under a kind of room temperature condition: 1 mmole divalent iron salt (in ferrous sulfate, ferrous sulfate, the ammonium Iron nitrate a kind of), 2 mmole trivalent iron salt (iron trichlorides, or iron nitrate) 5 mmole tensio-active agents (Trisodium Citrate) mix and add in the mortar fully grinding.Then add 8 mmole highly basic (sodium hydroxide, or potassium hydroxide) continue to grind, after question response is complete, with deionized water ultrasonic cleaning 5-10 minute, the centrifugal 30min of 12000r/min again, solution is outwelled, and the process of extremely solution being outwelled in 5-10 minute with the deionized water ultrasonic cleaning will repeat three times, obtains the black magnetic powder.Be accredited as ferriferous oxide through EDS.
Claims (5)
1. prepare the method for water-soluble iron oxide compound under the room temperature condition, it is characterized in that comprising the following steps:
(1) divalent iron salt, trivalent iron salt and tensio-active agent are ground in mortar, wherein: the mol ratio of divalent iron salt and trivalent iron salt is 1: 2; The mol ratio of tensio-active agent and divalent iron salt add-on is 2.5-5: 1;
(2) add highly basic after the component of step (1) is ground fully, fully grind, wherein: the mol ratio of highly basic and divalent iron salt add-on is 8: 1;
(3) question response fully after, with deionized water ultrasonic cleaning 5-10 minute, the centrifugal 30min of 12000r/min outwelled solution again, the process of extremely solution being outwelled in 5-10 minute with the deionized water ultrasonic cleaning will repeat three times, namely gets the water-soluble iron oxide compound.
2. by the method for preparing the water-soluble iron oxide compound under the room temperature condition claimed in claim 1, it is characterized in that the described divalent iron salt of step (1) is a kind of in Iron nitrate, ferrous ammonium sulphate and the ferrous sulfate.
3. by the method for preparing the water-soluble iron oxide compound under the room temperature condition claimed in claim 1, it is characterized in that the described tensio-active agent of step (1) is Trisodium Citrate.
4. by the method for preparing the water-soluble iron oxide compound under the room temperature condition claimed in claim 1, it is characterized in that the described trivalent iron salt of step (1) is a kind of in iron trichloride and the iron nitrate.
5. by the method for preparing the water-soluble iron oxide compound under the room temperature condition claimed in claim 1, it is characterized in that the described highly basic of step (2) is the sodium hydroxide quasi-alkali.
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Citations (1)
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|---|---|---|---|---|
| CN101555042A (en) * | 2009-05-19 | 2009-10-14 | 李峰 | Method for preparing spinel type iron-containing oxide nano-materials by low heat solid state reaction |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101555042A (en) * | 2009-05-19 | 2009-10-14 | 李峰 | Method for preparing spinel type iron-containing oxide nano-materials by low heat solid state reaction |
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Application publication date: 20130109 |