CN115155506B - Iron-manganese oxide and preparation method and application thereof - Google Patents
Iron-manganese oxide and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a ferro-manganese oxide and a preparation method and application thereof. The preparation method of the ferro-manganese oxide comprises the following steps: 1) Dispersing soluble permanganate and phosphate in water to prepare a mixed solution, and then adding a strong acid solution for acidification to obtain an acidified mixed solution; 2) Adding a ferrous salt solution into the acidified mixed solution for reaction to obtain a colloid solution; 3) Adding the alkali solution into the colloid solution to adjust the pH value of the system to 7-8, and reacting to obtain the iron-manganese oxide. The iron-manganese oxide has high adsorption efficiency and large adsorption capacity on metal cations, and has the advantages of simple preparation process, easy separation of products, low production cost, no secondary pollution to the environment and good application prospect in the field of heavy metal wastewater treatment.
Description
Technical Field
The invention relates to the technical field of adsorbents, in particular to a ferro-manganese oxide and a preparation method and application thereof.
Background
A large amount of heavy metal wastewater is inevitably generated in the industrial production process, and if the wastewater is directly discharged into natural water, serious harm is caused to natural environment and aquatic organisms, and finally the health of human beings is endangered. At present, the methods commonly used for removing heavy metals in water comprise an adsorption method, a precipitation method, an ion exchange method, an electrochemical method and the like, wherein the adsorption method is widely applied because of the advantages of low cost, quick response, simple operation and the like, and is considered as the treatment method of the heavy metal polluted wastewater with the best application prospect. The key point of the adsorption method is the adsorbent, but the existing adsorbent has the problems of smaller adsorption capacity, high preparation cost, harm to the environment and the like, and the actual application requirement is difficult to completely meet.
Therefore, the development of the heavy metal adsorbent with large adsorption capacity, simple preparation, low cost, safety and environmental protection has very important significance.
Disclosure of Invention
The invention aims to provide a ferro-manganese oxide and a preparation method and application thereof.
The technical scheme adopted by the invention is as follows:
the preparation method of the ferro-manganese oxide comprises the following steps:
1) Dispersing soluble permanganate and phosphate in water to prepare a mixed solution, and then adding a strong acid solution for acidification to obtain an acidified mixed solution;
2) Adding a ferrous salt solution into the acidified mixed solution for reaction to obtain a colloid solution;
3) Adding the alkali solution into the colloid solution to adjust the pH value of the system to 7-8, and reacting to obtain the iron-manganese oxide.
Preferably, the mole ratio of the soluble permanganate to the phosphate is 1:0.1-1.5.
Preferably, the molar ratio of ferrous salt in the soluble permanganate and ferrous salt solution is 1:1-5.
Preferably, the soluble permanganate in the step 1) is at least one of sodium permanganate, potassium permanganate and calcium permanganate.
Preferably, the phosphate in the step 1) is at least one of potassium dihydrogen phosphate, dipotassium hydrogen phosphate, disodium hydrogen phosphate and sodium dihydrogen phosphate.
Preferably, the strong acid solution in the step 1) is at least one of concentrated sulfuric acid, concentrated nitric acid and phosphoric acid.
Further preferably, the strong acid solution in step 1) is concentrated sulfuric acid (sulfuric acid aqueous solution with mass fraction not less than 70%).
Preferably, the volume ratio of the mixed solution and the strong acid solution in the step 1) is 1:0.001-0.020.
Preferably, the ferrous salt in the ferrous salt solution in the step 2) is at least one of ferrous sulfate, ferrous chloride and ferrous nitrate.
Preferably, the ferrous salt solution of step 2) is slowly added by dropwise addition.
Preferably, the reaction in the step 2) is carried out at 20-60 ℃ for 20-40 min.
Preferably, the alkali solution in the step 3) is at least one of sodium hydroxide solution, potassium hydroxide solution and ammonia water.
Preferably, the concentration of the alkali solution in the step 3) is 0.2mol/L to 5mol/L.
Preferably, the reaction in the step 3) is carried out at normal temperature (25 ℃ +/-5 ℃), and the reaction time is 1-5 hours.
An iron manganese oxide, which is prepared by the preparation method.
An adsorbent comprising the above iron manganese oxide.
The method for removing the heavy metal ions in the wastewater comprises the following steps: adding the ferro-manganese oxide into the wastewater, adsorbing heavy metal ions, and separating out the ferro-manganese oxide.
Preferably, the adding amount of the iron-manganese oxide in the wastewater is 0.05 g/L-1.00 g/L.
Preferably, the adsorption is carried out under the condition that the pH value of the wastewater is 1-6, and the adsorption time is 1-12 h.
Preferably, the adsorption is performed under the condition that the rotation speed of the stirring device is 100r/min to 200 r/min.
Preferably, the heavy metal ion is Pb 2+ 。
The beneficial effects of the invention are as follows: the iron-manganese oxide has high adsorption efficiency and large adsorption capacity on metal cations, and has the advantages of simple preparation process, easy separation of products, low production cost, no secondary pollution to the environment and good application prospect in the field of heavy metal wastewater treatment.
Specifically:
1) The iron-manganese oxide disclosed by the invention has high efficiency in treating heavy metal wastewater, and the removal capacity of the iron-manganese oxide on lead-containing wastewater is greatly improved by introducing phosphate groups in the preparation process of the iron-manganese oxide and regulating and controlling the active sites on the surface of the iron-manganese oxide, so that the adsorption rate is high and the adsorption capacity is large;
2) The preparation process of the iron-manganese oxide is simple, the product is easy to separate from the reaction solution, the efficiency is high, the production cost is low, and no secondary pollution is caused to the environment;
3) The active site on the surface of the ferro-manganese oxide is regulated and controlled through pre-oxidation and acidification of the strong acid solution, so that the hydroxyl content on the surface of the ferro-manganese oxide is increased;
4) According to the invention, phosphate radical is introduced into the ferro-manganese oxide, so that the adsorption site on the surface of the ferro-manganese oxide is increased, the adsorption capacity of the ferro-manganese oxide to heavy metal cations is enhanced, the oxygen defect content on the surface of the ferro-manganese oxide is increased through pre-oxidation and the enhanced oxidation-reduction reaction of the strong acid solution, the lattice oxygen content on the surface is reduced, the adsorbed oxygen content is increased, and the hydroxyl content on the surface of the ferro-manganese oxide is increased on the premise that no additional reaction element is added;
5) The method combines the strategy of active site regulation and phosphate group introduction into the ferro-manganese oxide to prepare the ferro-manganese oxide taking hydroxyl and phosphate groups as main adsorption sites.
Drawings
Fig. 1 is an SEM image of the iron-manganese oxide of example 1.
Fig. 2 is an XRD spectrum of the iron-manganese oxide of example 1.
Fig. 3 is an XPS spectrum of the iron manganese oxide of example 1.
Fig. 4 is an XPS spectrum of the ferro-manganese oxide of comparative example 2.
Fig. 5 is an XPS spectrum of the ferro-manganese oxide of comparative example 3.
FIG. 6 is a graph showing the comparison of the adsorption performance of iron-manganese oxides to lead ions in example 1 and comparative examples 1 to 3.
Detailed Description
The invention is further illustrated and described below in connection with specific examples.
Example 1:
the preparation method of the ferro-manganese oxide comprises the following steps:
1) Adding 1g of potassium permanganate and 0.4g of monopotassium phosphate into 50mL of deionized water, stirring to fully dissolve, and adding 0.05mL of concentrated sulfuric acid for acidification to obtain an acidified mixed solution;
2) Dripping 25mL of ferrous sulfate solution with the concentration of 0.75mol/L into the acidified mixed solution, generating brown colloid, and stirring to react for 30min to obtain a colloid solution;
3) Adding a sodium hydroxide solution with the concentration of 3mol/L into the colloid solution, regulating the pH value of the system to 7-8, stirring and reacting for 3 hours, carrying out suction filtration, and drying the filtered solid in an oven at 60 ℃ for 24 hours to obtain the ferro-manganese oxide.
Example 2:
the preparation method of the ferro-manganese oxide comprises the following steps:
1) Adding 0.8g of potassium permanganate and 0.8g of monopotassium phosphate into 50mL of deionized water, stirring for full dissolution, and adding 0.2mL of concentrated sulfuric acid for acidification to obtain an acidified mixed solution;
2) Dripping 25mL of ferrous sulfate solution with the concentration of 0.75mol/L into the acidified mixed solution, generating brown colloid, and stirring to react for 30min to obtain a colloid solution;
3) Adding a sodium hydroxide solution with the concentration of 3mol/L into the colloid solution, regulating the pH value of the system to 7-8, stirring and reacting for 3 hours, carrying out suction filtration, and drying the filtered solid in an oven at 60 ℃ for 24 hours to obtain the ferro-manganese oxide.
Example 3:
the preparation method of the ferro-manganese oxide comprises the following steps:
1) Adding 0.6g of potassium permanganate and 0.4g of monopotassium phosphate into 50mL of deionized water, stirring for full dissolution, and adding 0.15mL of concentrated sulfuric acid for acidification to obtain an acidified mixed solution;
2) Dripping 25mL of ferrous sulfate solution with the concentration of 0.75mol/L into the acidified mixed solution, generating brown colloid, and stirring to react for 30min to obtain a colloid solution;
3) Adding a sodium hydroxide solution with the concentration of 3mol/L into the colloid solution, regulating the pH value of the system to 7-8, stirring and reacting for 3 hours, carrying out suction filtration, and drying the filtered solid in an oven at 60 ℃ for 24 hours to obtain the ferro-manganese oxide.
Comparative example 1:
the preparation method of the ferro-manganese oxide comprises the following steps:
adding 1g of potassium permanganate into 50mL of deionized water, stirring for full dissolution, then dropwise adding 25mL of ferrous sulfate solution with the concentration of 0.75mol/L, simultaneously adding sodium hydroxide solution with the concentration of 3mol/L to adjust the pH value of the system to 7-8, stirring for reaction for 3h, carrying out suction filtration, and drying the filtered solid in an oven at 60 ℃ for 24h to obtain the ferro-manganese oxide.
Comparative example 2:
the preparation method of the ferro-manganese oxide comprises the following steps:
adding 1g of potassium permanganate and 0.4g of monopotassium phosphate into 50mL of deionized water, stirring for full dissolution, then dropwise adding 25mL of ferrous sulfate solution with the concentration of 0.75mol/L, simultaneously adding sodium hydroxide solution with the concentration of 3mol/L to adjust the pH value of the system to 7-8, stirring for reaction for 3 hours, carrying out suction filtration, and drying the filtered solid in an oven at 60 ℃ for 24 hours to obtain the iron-manganese oxide.
Comparative example 3:
the preparation method of the ferro-manganese oxide comprises the following steps:
adding 1g of potassium permanganate and 0.4g of monopotassium phosphate into 50mL of deionized water, stirring for full dissolution, then dropwise adding 25mL of ferrous sulfate solution with the concentration of 0.75mol/L, stirring for 30min, then adding sodium hydroxide solution with the concentration of 3mol/L to adjust the pH value of the system to 7-8, stirring for reaction for 3h, carrying out suction filtration, and drying the filtered solid in an oven at 60 ℃ for 24h to obtain the ferro-manganese oxide.
Performance test:
1) The Scanning Electron Microscope (SEM) image of the iron-manganese oxide of example 1 is shown in fig. 1, and the X-ray diffraction (XRD) image is shown in fig. 2.
As can be seen from fig. 1: the iron manganese oxide of example 1 has a uniform spherical structure that facilitates dispersion of the material in the liquid phase and contact with contaminants.
As shown in fig. 2: the crystalline structure of the iron-manganese oxide of example 1 is weak, mainly amorphous, and weak characteristic peaks at 32.7 °, 35.1 ° and 41.2 ° respectively represent ferric oxide and manganese dioxide.
2) X-ray photoelectron spectroscopy (XPS) full spectrum scan results of the iron manganese oxides of example 1 and comparative examples 1 to 3 are shown in Table 1, XPS O1 s fine scan results of the iron manganese oxides of example 1, comparative example 2 and comparative example 3 are shown in Table 2, and XPS spectra of the iron manganese oxides of example 1, comparative example 2 and comparative example 3 are shown in FIGS. 3 to 5, respectively.
TABLE 1 XPS Spectrum scanning results of iron manganese oxides of example 1 and comparative examples 1-3
TABLE 2 XPS O1 s Fine scanning results of the iron manganese oxides of example 1, comparative example 2 and comparative example 3
Note that: o (O) lat : lattice oxygen; o (O) ads : the surface adsorbs oxygen.
As can be seen from tables 1 to 2 and fig. 3 to 5:
a) The presence of the P element in the iron manganese oxides of comparative example 2, comparative example 3 and example 1, as compared with the iron manganese oxide of comparative example 1, confirms that a phosphate group has been introduced in the iron manganese oxide;
b) The increase in the surface adsorbed oxygen content of the iron-manganese oxides of example 1 was significant compared to the iron-manganese oxides of comparative examples 2 and 3, and the surface adsorbed oxygen was generally present on the iron-manganese oxide surface in the form of hydroxyl groups, confirming that the method of promoting the synthesis reaction with a strong acid solution and the oxidation front effectively increased the hydroxyl group content of the iron-manganese oxide surface (hydroxyl group content: example 1> comparative example 3> comparative example 2), increasing active sites for adsorbing lead ions, shows that the iron manganese oxide of the present invention effectively increases the adsorption capacity of iron manganese oxide to heavy metals by controlling the hydroxyl content of the material surface and introducing phosphate groups.
3) Taking 4 beakers, adding 100mL of lead nitrate solution with the concentration of 50mg/L, pH =5, respectively adding 0.01g of the iron-manganese oxide of the example 1 and the iron-manganese oxides of the comparative examples 1-3, placing the beakers in a constant-temperature shaking table with the temperature of 30 ℃ for shaking, taking the concentration of the supernatant liquid at intervals, and reacting until the adsorption reaches equilibrium, wherein the adsorption performance comparison graph of the iron-manganese oxide of the example 1 and the iron-manganese oxide of the comparative examples 1-3 on lead ions is shown in figure 6.
As can be seen from fig. 6:
a) The iron manganese oxides of example 1, comparative example 2 and comparative example 3 all have significantly enhanced lead adsorption properties after the introduction of phosphate groups as compared with the conventional iron manganese oxide (comparative example 1);
b) Compared with the directly synthesized iron manganese phosphate (comparative example 2), the adsorption capacity and the treatment efficiency of the iron manganese phosphate (comparative example 3) which adopts the pre-oxidation reprecipitation are obviously improved;
c) After adding a strong acid solution to the reaction system of the pre-oxidation to strengthen the active site of the ferro-manganese oxide (example 1), the adsorption capacity of the ferro-manganese oxide to lead is further improved;
d) Compared with 3 comparative examples, the adsorption capacity of the example 1 is respectively improved by 44.8%, 66.89% and 85.7% after 240min, the adsorption rate is obviously improved, the adsorption capacity of the example 1 can reach 190mg/g after 5min, compared with the system without acid solution (comparative example 3), the method has the advantages of 40 percent improvement, 81 percent improvement compared with the directly synthesized iron manganese oxide phosphate and 153 percent improvement compared with the traditional iron manganese oxide.
4) Taking 3 beakers, adding 100mL of lead nitrate solution with the concentration of 50mg/L, pH =5 into each beaker, adding 0.03g of the iron-manganese oxide of the examples 1-3 respectively, placing the beakers into a constant-temperature shaking table with the temperature of 25 ℃ for shaking, taking supernatant at intervals to test the concentration of the solution, and reacting for 2 hours, wherein the test results of the removal rate of lead ions by the iron-manganese oxide of the examples 1-3 are shown in the following table:
TABLE 3 results of test for lead ion removal rate of iron-manganese oxides of examples 1 to 3
As can be seen from table 3: the removal rates of the iron-manganese oxides of examples 1 to 3 for lead ions were 100%, 100% and 97.42%, respectively, indicating that the iron-manganese oxides of the present invention have excellent lead ion removal effects.
The above examples are preferred embodiments of the present invention, but the embodiments of the present invention are not limited to the above examples, and any other changes, modifications, substitutions, combinations, and simplifications that do not depart from the spirit and principle of the present invention should be made in the equivalent manner, and the embodiments are included in the protection scope of the present invention.
Claims (5)
1. The preparation method of the ferro-manganese oxide is characterized by comprising the following steps:
1) Dispersing soluble permanganate and phosphate in water to prepare a mixed solution, and then adding a strong acid solution for acidification to obtain an acidified mixed solution;
2) Adding a ferrous salt solution into the acidified mixed solution for reaction to obtain a colloid solution;
3) Adding an alkali solution into the colloid solution, adjusting the pH value of the system to 7-8, and reacting to obtain the iron-manganese oxide;
the mole ratio of the soluble permanganate and the phosphate is 1:0.1-1.5;
the molar ratio of ferrous salt in the soluble permanganate and ferrous salt solution is 1:1-5;
the soluble permanganate in the step 1) is at least one of sodium permanganate, potassium permanganate and calcium permanganate;
the phosphate in the step 1) is at least one of potassium dihydrogen phosphate, dipotassium hydrogen phosphate, disodium hydrogen phosphate and sodium dihydrogen phosphate;
the strong acid solution in the step 1) is sulfuric acid aqueous solution with the mass fraction of more than or equal to 70%;
the volume ratio of the mixed solution to the strong acid solution in the step 1) is 1:0.001-0.020;
the ferrous salt in the ferrous salt solution in the step 2) is at least one of ferrous sulfate, ferrous chloride and ferrous nitrate;
the reaction in the step 2) is carried out at 20-60 ℃ for 20-40 min;
the reaction in the step 3) is carried out at normal temperature, and the reaction time is 1-5 h.
2. The method for producing iron-manganese oxide according to claim 1, wherein: the alkali solution in the step 3) is at least one of sodium hydroxide solution, potassium hydroxide solution and ammonia water.
3. Iron manganese oxide, characterized in that it is produced by the production method according to claim 1 or 2.
4. An adsorbent comprising the iron manganese oxide of claim 3.
5. A method for removing heavy metal ions in wastewater, which is characterized by comprising the following steps: adding the iron-manganese oxide according to claim 3 into the wastewater, adsorbing heavy metal ions, and separating out the iron-manganese oxide.
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| CN104815609A (en) * | 2015-05-06 | 2015-08-05 | 山东师范大学 | Fe/Mn composite oxide, preparation method and application thereof |
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| CN112934177A (en) * | 2021-02-03 | 2021-06-11 | 广东工业大学 | Manganese sulfide-phosphoric acid modified biochar composite material and preparation method and application thereof |
| CN114105210A (en) * | 2021-10-19 | 2022-03-01 | 中南大学 | Amorphous iron-manganese oxide and preparation and application thereof |
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| CN104815609A (en) * | 2015-05-06 | 2015-08-05 | 山东师范大学 | Fe/Mn composite oxide, preparation method and application thereof |
| CN106044734A (en) * | 2016-06-23 | 2016-10-26 | 宝钢发展有限公司 | Method for preparing nano-hydroxyapatite |
| CN108176362A (en) * | 2017-11-13 | 2018-06-19 | 汝城县三鑫电化有限公司 | A kind of iron and manganese oxides preparation method of stabilization |
| CN112934177A (en) * | 2021-02-03 | 2021-06-11 | 广东工业大学 | Manganese sulfide-phosphoric acid modified biochar composite material and preparation method and application thereof |
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