CN109576332B - Method for preparing magnetic nano ferroferric oxide by biological reduction - Google Patents

Method for preparing magnetic nano ferroferric oxide by biological reduction Download PDF

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CN109576332B
CN109576332B CN201811302970.1A CN201811302970A CN109576332B CN 109576332 B CN109576332 B CN 109576332B CN 201811302970 A CN201811302970 A CN 201811302970A CN 109576332 B CN109576332 B CN 109576332B
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蒋海明
李侠
兰建英
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Inner Mongolia University of Science and Technology
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Abstract

The invention discloses a method for preparing magnetic nano ferroferric oxide by biological reduction, which comprises the steps of using Fe (OH)3The nano colloid is used as an electron acceptor, the functional microbial flora is used as an inoculum, and H is used2One or more of methanol, sodium acetate and methane are taken as substrates, anaerobic culture is carried out at the temperature of 30-35 ℃, and electrons generated by the substrates metabolized by functional microbial flora directly react with Fe (OH)3Reduction of nano colloidal particles to Fe3O4. The invention utilizes electrons generated by the metabolism of substrates by the electroactive microorganisms to directly convert Fe (OH)3Reduction to Fe3O4The process is easy to control, the reaction condition is mild, and the method is environment-friendly. The substrate can be directly agricultural and urban hydrolysis fermentation products of organic solid wastes, so that the organic wastes are fully utilized, the treatment of the organic wastes is realized, and the substrate has the advantage of small environmental pollution and has important significance for energy conservation, emission reduction and environmental treatment.

Description

Method for preparing magnetic nano ferroferric oxide by biological reduction
Technical Field
The invention belongs to the field of preparation of nano ferroferric oxide, and particularly relates to a method for preparing magnetic nano ferroferric oxide by biological reduction.
Background
The magnetic nano ferroferric oxide is a nano material with special functions and has the characteristics of superparamagnetism, small-size effect, quantum tunneling effect and the like. The nano ferroferric oxide is one of soft magnetic materials which are most widely applied, and shows good application prospect in the application fields of catalysts, recording materials, magnetic fluid materials, electronic materials, radiography imaging, targeted drug delivery, drug carriers, DNA detection and the like.
At present, the common preparation methods of the magnetic nano ferroferric oxide include a precipitation method, a thermal decomposition method, a hydrothermal method, a solvothermal method, a microemulsion method, an air oxidation method, an electrostatic spinning method and a microwave method. The pH value of the precipitation method is high, and the preparation process is not easy to control. The thermal decomposition method is a method in which an organic iron compound is dissolved in a solvent, the reaction temperature is controlled, and then the reaction product is decomposed and precipitated in a high-pressure reaction vessel or by condensation and reflux. Magnetic particles prepared by a thermal decomposition method generally have high crystallinity, but the magnetic particles have poor hydrophilic properties. The hydrothermal method and the solvothermal method are collectively called as a hydrothermal method, and refer to a method in which water or a solvent is used as a dispersion medium and reacts in a sealed reaction vessel under high temperature and high pressure to obtain magnetic particles. The microemulsion method is a good preparation method for preparing nano powder with narrow distribution, regular shape and good dispersion. The reaction is carried out in the space of microemulsion drops, and the preparation of the microemulsion is complex.
Therefore, the development of the preparation method of the magnetic nano ferroferric oxide, which is easy to control, mild in reaction conditions and environment-friendly, has very important significance.
Disclosure of Invention
The invention aims to provide a method for preparing magnetic nano ferroferric oxide by biological reduction, which has the advantages of easily controlled process, mild reaction conditions and environmental protection and overcomes the defects of the traditional preparation method of the magnetic nano ferroferric oxide.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for preparing magnetic nano ferroferric oxide by biological reduction comprises the following steps:
with Fe (OH)3The nano colloid is used as an electron acceptor, the functional microbial flora is used as an inoculum, and H is used2One or more of methanol, sodium acetate and methane are taken as substrates, anaerobic culture is carried out at the temperature of 30-35 ℃, and electrons generated by the substrates metabolized by functional microbial flora directly react with Fe (OH)3Reduction of nano colloidal particles to Fe3O4；
The functional microbial flora comprises electroactive methane anaerobic oxidizing bacteria, Methanosarcina barberi strain Fusaro (A), (B), (C) and C) a)
Figure BDA0001852844050000021
BAA-2329)、Methanosarcina mazei strain OCM88(
Figure BDA0001852844050000023
BAA-159)、Methanobacterium palustre(
Figure BDA0001852844050000022
BAA-1077), Methanosarcina barkeri 800(DSM 800), Methanosarcina barkeri (DSM 8687) and Methanosarcina mazei (DSM 10132).
When the biological reduction method is used for preparing the nano ferroferric oxide, the hydrolysis fermentation product of solid organic waste of agriculture and/or cities can be directly used as a substrate, and the environment can be managed while the nano ferroferric oxide is prepared.
In the invention, the nano ferroferric oxide with different magnetic susceptibilities can be obtained by controlling the reduction conditions.
In the invention, the screening and enriching conditions of the functional microorganism electroactive methane anaerobic oxidizing bacteria are as follows:
with Fe (OH)3Colloid is used as electron acceptor, anaerobic activated sludge and rice field sludge are used as inoculum, and H is used2One or more of methanol, sodium acetate and methane are used as electron donors, and the anaerobic culture is carried out at the temperature of 30-35 ℃, wherein the concentration of the electron donors is 20 millimole/liter.
A specific implementation method of a method for preparing magnetic nano ferroferric oxide by biological reduction comprises the following steps:
the first step, using the sludge of paddy field and anaerobic active sludge as inoculum, using Fe (OH)3Colloid as electron acceptor, with H2One or more of methanol, sodium acetate and methane are taken as substrates, and the electroactive methane anaerobic oxidizing bacteria are obtained by enrichment;
secondly, mixing the obtained electrically active anaerobic methane-oxidizing bacteria with Methanosarcina barocri strain Fusaro, Methanosarcina mazei strain OCM88, Methanosarcina barocri 800, Methanosarcina barocri and Methanosarcina mazei to obtain a functional microbial flora;
third, providing Fe (OH)3Nano colloidal particles;
the fourth step, taking functional microbial flora as inoculum and Fe (OH)3The nano colloidal particles are used as electron acceptors and H is used as a catalyst2One or more of methanol, sodium acetate and methane as substrate, mixing the substrate, electron acceptor and culture medium, sterilizing, adding inoculum, and anaerobically culturing when Fe (OH)3And (5) blackening the nano colloid, namely finishing the reduction of the magnetic nano ferroferric oxide.
In the third step, Fe (OH) is provided3The nano colloidal particles specifically comprise:
FeCl is added3Dissolving in deionized water to prepare FeCl3Adding NaOH solution into the water solution continuously under the condition of high-speed stirring to generate Fe (OH)3Precipitating, pouring out supernatant after centrifuging, adding deionized water into the centrifugal precipitate for dispersing, centrifuging again, pouring out the supernatant, and repeating the centrifuging operation until the pH value of the centrifugal supernatant is neutral; the resulting centrifugal precipitate is Fe (OH)3And diluting the nano colloidal particles with deionized water to obtain a suspension for later use.
Compared with the prior art, the invention has the following characteristics and beneficial effects:
(1) the invention utilizes electrons generated by the metabolism of substrates by the electroactive microorganisms to directly convert Fe (OH)3Reduction to Fe3O4The process is easy to control, the reaction condition is mild, and the method is environment-friendly.
(2) The hydrolysis fermentation product of agricultural and urban organic solid waste (such as granular straw, cow dung and the like) can be directly used as a substrate, so that the organic waste is fully utilized, the treatment of the organic waste is realized, and the hydrolysis fermentation product has the advantage of low environmental pollution and has important significance for energy conservation, emission reduction and environmental treatment.
(3) The magnetic nano ferroferric oxide materials with different magnetic susceptibilities can be obtained by controlling the biological reduction time.
Drawings
FIG. 1 shows magnetic nano-ferroferric oxide prepared by biological reduction with different substrates, from left to right, a magnetic nano-ferroferric oxide reference substance prepared by reduction with methane as a substrate, magnetic nano-ferroferric oxide prepared by reduction with sodium acetate as a substrate, magnetic nano-ferroferric oxide prepared by reduction with methanol as a substrate, and magnetic nano-ferroferric oxide prepared by reduction with hydrogen as a substrate.
Detailed Description
In order to more clearly illustrate the present invention and/or the technical solutions in the prior art, the following will describe embodiments of the present invention with reference to the accompanying drawings. It is obvious that the drawings in the following description are only some examples of the invention, and that for a person skilled in the art, other drawings and embodiments can be derived from them without inventive effort.
It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention. In addition, the technical features involved in the embodiments of the present invention described below may be combined with each other as long as they do not conflict with each other.
Examples
In this embodiment, the specific process for preparing magnetic nano ferroferric oxide is as follows:
step one, enriching the electroactive methane anaerobic oxidizing bacteria:
using rice field sludge and anaerobic active sludge as inoculum, using Fe (OH)3Colloid as electron acceptor, with H2And enriching the methane and the methanol as substrates to obtain the electroactive methane anaerobic oxidizing bacteria. 100ml of DSMZ _ medium 120a medium was added to a 250ml anaerobic flask, methanol and Fe (OH) were added3Colloid, wherein the final concentration of methanol is up to 20mmol/l, the final concentration of iron element is up to 20mmol/l, N2/CO2(v/v 80:20) aeration for 45 minutes, deoxygenated and sterilized at 121 ℃ for 30 minutes, and then cooled to room temperature. By CH4/H2The gas above the liquid in the anaerobic tube was removed by gas replacement with a mixed gas (v/v 20:80), aerated for 15min, added with 10ml of inoculum, and then cultured anaerobically at 35 ℃. When in useFe (OH) in anaerobic tubes3And (3) repeating the operation for 3-5 times by taking the suspension in the anaerobic tube as an inoculum after the nano colloid turns black, and enriching to obtain the electroactive anaerobic methane-oxidizing bacteria.
(2) Construction of functional microbial flora:
the electrically active anaerobic methane-oxidizing bacteria obtained by enrichment and Methanosarcina barberi strain Fusaro (A), (B), (C
Figure BDA0001852844050000045
BAA-2329)、Methanosarcina mazei strain OCM88(
Figure BDA0001852844050000046
BAA-159), Methanosarcina barkeri 800(DSM 800), Methanosarccina barkeri (DSM 8687) and Methanosarccina mazei (DSM 10132) to obtain a functional microorganism.
(3)Fe(OH)3Preparing nano colloidal particles:
adding a certain amount of FeCl3Dissolving in deionized water to prepare FeCl with certain concentration3Adding NaOH solution into the water solution continuously under the condition of high-speed stirring to generate Fe (OH)3Precipitating, centrifuging 5000g, pouring out supernatant, dispersing the centrifugal precipitate with deionized water, centrifuging 5000g, pouring out supernatant, and repeating the above centrifuging operation until the pH value of the centrifuged supernatant is neutral. Prepared Fe (OH)3And diluting the nano colloidal particles with deionized water to obtain a suspension with a certain concentration for later use.
(4) Biological reduction preparation of magnetic nano ferroferric oxide:
the obtained functional microbial flora is taken as an inoculum, the ferric hydroxide nano colloid is taken as an electron acceptor, and H2Methane and methanol as substrates. Adding 9ml of DSMZ _ medium 120a culture medium into a 27ml anaerobic tube, and adding methanol and 1ml of ferric hydroxide colloid suspension, wherein the final concentration of the methanol is 20 mmol/l; n is a radical of2/CO2(v/v 80:20) aeration for 10 minutes, deoxygenated and sterilized at 121 ℃ for 30 minutes, then cooled to room temperature, and treated with CH4/H2(v/v 20:80) removing the gas above the anaerobic tube liquid by replacement, and exposingAerating for 5min, adding 1ml of inoculum, and performing anaerobic culture at 35 ℃. And when the ferric hydroxide colloid in the anaerobic tube becomes black, finishing the biological reduction preparation of the magnetic nano ferroferric oxide.
The following reactions mainly occur in anaerobic bottles:
Figure BDA0001852844050000041
Figure BDA0001852844050000042
Figure BDA0001852844050000043
Figure BDA0001852844050000044
the invention can utilize H2Methane, sodium acetate and methanol as substrate, and small molecular H produced by hydrolysis and fermentation of agricultural and urban organic solid waste (such as granular straw, cow dung, etc.)2Sodium acetate, methanol and methane as substrates.
The specific embodiments described herein are merely illustrative of the patent spirit of the invention. Various modifications or additions may be made or substituted in a similar manner to the specific embodiments described herein by those skilled in the art without departing from the spirit of the invention or exceeding the scope thereof as defined in the appended claims.

Claims (2)

1. A method for preparing magnetic nano ferroferric oxide by biological reduction is characterized by comprising the following steps:
the first step, using the sludge of paddy field and anaerobic active sludge as inoculum, using Fe (OH)3Colloid as electron acceptor, with H2One or more of methanol, sodium acetate and methane are taken as substrates,anaerobic culture is carried out at the temperature of 30-35 ℃, and the electrically active methane anaerobic oxidizing bacteria are obtained by enrichment;
secondly, mixing the obtained electrically active anaerobic methane-oxidizing bacteria with Methanosarcina barocri strain Fusaro, Methanosarcina mazei strain OCM88, Methanosarcina barocri DSM 800, Methanosarcina barocri DSM 8687 and Methanosarcona mazei DSM 10132 to obtain a functional microbial flora;
third, providing Fe (OH)3Nano colloidal particles;
the fourth step, taking functional microbial flora as inoculum and Fe (OH)3The nano colloidal particles are used as electron acceptors and H is used as a catalyst2One or more of methanol, sodium acetate and methane as substrate, mixing the substrate, electron acceptor and culture medium, sterilizing, adding inoculum, and anaerobically culturing at 30-35 deg.C while Fe (OH)3And (5) blackening the nano colloid, namely finishing the reduction of the magnetic nano ferroferric oxide.
2. The method for preparing magnetic nano ferroferric oxide by biological reduction according to claim 1, which is characterized in that:
in the third step, Fe (OH) is provided3The nano colloidal particles specifically comprise:
FeCl is added3Dissolving in deionized water to prepare FeCl3Adding NaOH solution into the water solution continuously under the condition of high-speed stirring to generate Fe (OH)3Precipitating, pouring out supernatant after centrifuging, adding deionized water into the centrifugal precipitate for dispersing, centrifuging again, pouring out the supernatant, and repeating the centrifuging operation until the pH value of the centrifugal supernatant is neutral; the resulting centrifugal precipitate is Fe (OH)3And diluting the nano colloidal particles with deionized water to obtain a suspension for later use.
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