Method for preparing porous nano ferroferric oxide

A technology of ferroferric oxide and porosity, which is applied in the chemical field, can solve the problems of increasing industrialization costs, increasing requirements for reaction equipment, unfavorable industrialization promotion, etc., and achieves low cost, convenient and easy-to-obtain raw material sources, and low threshold for industrialized production Effect

Active Publication Date: 2014-04-23
TAIYUAN UNIV OF TECH
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  • Abstract
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Problems solved by technology

[0004] The existing technology is mainly through the Fe 3 o 4 Coexist with other materials to prepare porous magnetic materials, and mainly in the atmosphere of inert gas, such as filling inert gas (such as nitrogen) or in the reaction environment of high temperature and high pressure in the autoclave, which will increase the reaction Equipment requirements increase the cost of industrialization, which is not conducive to the promotion of industrialization

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  • Method for preparing porous nano ferroferric oxide
  • Method for preparing porous nano ferroferric oxide
  • Method for preparing porous nano ferroferric oxide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 2

[0047] Step 201: Massage Erbi〔n(Fe 2+ ): n(Fe 3+ )] = 1~3 Weigh Fe 2+ (FeCl 2 ·4H 2 O, FeSO 4 ·7H 2 O) and Fe 3+ (FeCl 3 ·6H 2 O, Fe 2 (SO4) 3 ), dissolved in 50~300mL polyvinyl alcohol / ethanol / deionized water to prepare Fe 2+ With Fe 3+ mixture;

[0048] Step 202: configure 0.5~10mol / L of precipitation agent NaHCO 3 / Na 2 CO 3 / NH 4 HCO 3 Alkaline substances such as polyvinyl alcohol / ethanol / deionized aqueous solution that are prone to iron salt formation and precipitation.

[0049] Step 203: Add NaHCO to 100 mL of deionized water in a 500 mL three-necked flask 3 , Na 2 CO 3 , (NH 4 ) 2 CO 3 , NH 4 HCO 3 One of the inorganic compounds that can easily decompose and generate non-oxygen. Heat to 40°C and keep for 20 minutes. This step is to remove oxygen in the reaction vessel;

[0050] Step 204: Transfer 201 and 202 to a three-necked flask, and under the conditions of constant temperature of 70°C and rapid mechanical stirring of 200r / min, drop the liquid to a certain pH=8, keep it for ...

Embodiment 3

[0058] Step 301: Molar ratio [n(Fe 2+ ): n(Fe 3+ )] = 1~3 Weigh Fe 2+ (FeCl 2 ·4H 2 O, FeSO 4 ·7H 2 O) and Fe 3+ (FeCl 3 ·6H 2 O, Fe 2 (SO4) 3 ), dissolved in 100mL polyvinyl alcohol / ethanol / deionized water to prepare Fe 2+ With Fe 3+ mixture;

[0059] Step 302: configure 0.5~10mol / L NaHCO 3 / Na 2 CO 3 / NH 4 HCO 3 Alkaline substances such as polyvinyl alcohol / ethanol / deionized aqueous solution that are prone to iron salt formation and precipitation.

[0060] Step 303: Add NaHCO to 100 mL of deionized water in a 500 mL three-neck flask 3 , N 2 H 4 ·H 2 O, Na 2 CO 3 , (NH 4 ) 2 CO 3 , NH 4 HCO 3 One of the inorganic compounds that can easily decompose and generate non-oxygen, heat to 80°C and keep it for 20 minutes;

[0061] Step 304: Transfer 301 and 302 to a three-necked flask, and under the condition of temperature rising to 60°C and constant temperature, 500r / min rapid mechanical stirring, drop the liquid to a certain pH=10, keep it for 2h, and gradually reduce the temperature to 30...

Embodiment 4

[0064] Step 401: Molar ratio [n(Fe 2+ ): n(Fe 3+ )] = 1~3 Weigh Fe 2+ (FeCl 2 ·4H 2 O, FeSO 4 ·7H 2 O) and Fe 3+ (FeCl 3 ·6H 2 O, Fe 2 (SO4) 3 ), dissolved in 300mL polyvinyl alcohol / ethanol / deionized water to prepare Fe 2+ With Fe 3+ mixture;

[0065] Step 402: configure 10 mol / L precipitant NaHCO 3 / Na 2 CO 3 / NH 4 HCO 3 Alkaline substances such as polyvinyl alcohol / ethanol / deionized aqueous solution that are prone to iron salt formation and precipitation.

[0066] Step 403: Add NaHCO to 100mL deionized water in a 500mL three-neck flask 3 , N 2 H 4 ·H 2 O, Na 2 CO 3 , (NH 4 ) 2 CO 3 , NH 4 HCO 3 One of the inorganic compounds that can easily decompose and generate non-oxygen, heat to 80°C and keep it for 40 minutes;

[0067] Step 404: Transfer 401 and 402 to a three-necked flask, and under the condition of increasing the temperature to 80°C and constant temperature, 200r / min rapid mechanical stirring, drip the liquid to a certain pH=12, keep it for 3h, and gradually reduce the tempe...

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Abstract

The invention discloses a method for preparing porous nano ferroferric oxide. The method comprises the steps: dissolving two of FeCl2.4H2O, FeSO4.7H2O, FeCl3.6H2O and Fe2(SO4)3 in one of polyvinyl alcohol, ethanol and deionized water or a mixture thereof to obtain a mixed solution containing Fe<2+> and Fe<3+>; adding one of NaHCO3, N2H4.H2O, Na2CO3, (NH4)2CO3 and NH4HCO3 in one of polyvinyl alcohol, ethanol and deionized water or the mixture thereof to obtain an alkaline substance aqueous solution; mixing the mixed solution containing Fe<2+> and Fe<3+> with the alkaline substance aqueous solution in a reaction vessel, heating, and stirring; adjusting the pH of the stirred mixed liquid to 8-13, keeping for 0.5-3 h, gradually adjusting the temperature to 30-60 DEG C, keeping the constant temperature for 2-24 h, allowing the mixed liquid to fully undergo a reaction, and after finishing the reaction, cooling to the room temperature; and washing the precipitate product after reaction with one of anhydrous ethanol and deionized water or a mixture thereof until the pH is 7, and drying for 8-36 h. The reaction process has no need of inert gas protection, and the industrialized production doorsill is low.

Description

Technical field [0001] The invention belongs to the field of chemistry and relates to a method for preparing porous nano ferroferric oxide. Background technique [0002] Porous magnetic Fe 3 O 4 It has attracted great attention because of the magnetic properties of magnetic materials and the high specific surface area and large pore volume of porous materials. It has been widely used in immobilized enzymes, cell separation, targeted drug delivery, DNA separation and other biological Medical field, and industrial fields such as high-density magnetic storage, magnetic fluid, catalysis, etc. Therefore, the design and synthesis of magnetic porous Fe 3 O 4 It has significant scientific significance and application value. [0003] At present, there are many methods for preparing Fe3O4 nanoparticles, such as high-energy ball milling, chemical co-precipitation, redox, solvothermal, microemulsion, and pyrolysis. But preparing porous nano-Fe 3 O 4 There are few reports on effective methods...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G49/08B82Y30/00
Inventor 马建超董宪姝徐德龙李泓锐李晨王玲玲
Owner TAIYUAN UNIV OF TECH
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