CN109908868B - Iron-based porous adsorption material, preparation method thereof and application thereof in wastewater treatment - Google Patents
Iron-based porous adsorption material, preparation method thereof and application thereof in wastewater treatment Download PDFInfo
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Abstract
The invention discloses an iron-based porous adsorption material, a preparation method thereof and application thereof in wastewater treatment2O3And carbon black as raw material, wherein the content of elementary substance iron is 50% -70%, and Fe2+With Fe3+The content of the carbon is 22-49 percent, and the content of simple substance carbon is 1-8 percent; the iron-based porous adsorption material is prepared by adopting a powder metallurgy method, and Fe is weighed according to a molar ratio during preparation2O3Adding carbon black and CaCl as pore-forming agent2Adding the mixture into a ball milling tank for grinding; adding absolute ethyl alcohol into the ground raw materials, pouring the mixture into an electric hydraulic sample making machine for sample making, and sintering the mixture in a vacuum atmosphere furnace; the method is convenient to use and simple to operate, pollutants in water can be adsorbed after the wastewater enters the water body, and the wastewater can be manually salvaged after the adsorption is completed.
Description
Technical Field
The invention relates to the technical field of materials, in particular to an iron-based porous adsorption material, a preparation method thereof and application thereof in wastewater treatment.
Background
The porous metal material is a novel engineering material with excellent physical properties and good mechanical properties developed in the later stage of the 80 th century, has excellent physical properties such as small density, high rigidity, large specific surface area, good noise reduction effect, high electromagnetic shielding performance and the like, is widely applied to the aspects of catalysts, catalyst carriers, high-temperature liquid filters, heat exchangers and other functional materials, and can also be used as a structural material in the fields of aviation, buildings and the like.
At present, the wastewater is mainly treated by a physical, chemical or biological method, so that the wastewater is purified, and the pollution is reduced, thereby achieving the purposes of recovering and reusing the wastewater and fully utilizing water resources. The waste water treatment by the adsorption method utilizes the porosity and high specific surface area of the adsorbent to adsorb partial substances in the waste water, thereby achieving the purpose of separating water. Adsorption processes are being studied more and more extensively in the field of wastewater treatment. However, the conventional activated carbon adsorption method has disadvantages such as high chemical cost and difficulty in regeneration, and thus, the development of a cheap adsorption material with good performance is increasingly important at home and abroad. The adsorbing material is required to be cheap and easy to obtain, have excellent treatment efficiency, and be simple to operate and low in running cost. Therefore, the research of the invention is important content in developing an iron-based porous adsorption material and a preparation method thereof and applying the iron-based porous adsorption material to wastewater treatment.
Disclosure of Invention
The invention aims to provide an iron-based porous adsorption material, a preparation method thereof and application thereof in wastewater treatment.
The invention is realized by the following technical scheme:
the invention relates to an iron-based porous adsorption material, which mainly comprises Fe2O3And carbon black as raw materials, wherein the content of simple substance iron in the iron-based porous adsorption material is 50% -70%, and Fe2+With Fe3+The content of the carbon is 22-49 percent, and the content of simple substance carbon is 1-8 percent.
Preferably, the iron-based porous adsorption material in the invention contains 62% of elementary iron and Fe2+With Fe3+The content of (2) is 34%, and the content of simple substance carbon is 4%.
The invention also provides a preparation method of the iron-based porous adsorption material, which comprises the following steps:
(1) preparing materials: mixing Fe2O3Weighing two raw materials according to the molar ratio of 1:0.225-0.325 with carbon black, and adding a pore-forming agent CaCl into the raw materials2The mass of the pore-forming agent is Fe2O31/30-1/20 by total weight of carbon black; adding the steel balls into the ball milling tank according to the material-ball ratio of 4-5:1Setting the running time to be 4-5h and the rotating speed to be 400-;
(2) preparing a sample: sieving the ground raw materials with a 80-mesh sieve, adding an adhesive, namely absolute ethyl alcohol into the powder after uniform mixing, uniformly mixing, pouring the mixture into a material tank of an electric hydraulic sample making machine, pressing the mixture into a sample with the diameter of phi 20 multiplied by 20mm, and setting the pressure to be 80 MPa;
(3) and (3) sintering: placing the pressed sample into a vacuum atmosphere furnace, and setting the sintering process parameters as follows: keeping the temperature at 220 ℃ for 30min, keeping the temperature at 600 ℃ for 30min, keeping the temperature at 1200 ℃ for 2h, opening a circulating water valve, starting a vacuum pump to vacuumize, and discharging when the furnace temperature is cooled to be below 100 ℃.
The invention also provides an application of the iron-based porous adsorption material in wastewater treatment.
Preferably, the wastewater in the present invention contains acid ions and basic ions.
Further, the acid ions in the present invention include SO4 2-、Cl-One or a mixture of two, the basic ion comprises OH-。
Preferably, the iron-based porous adsorption material is added in an amount of 1-58% of the total weight of the wastewater when the iron-based porous adsorption material treats acid ions and basic ions in the wastewater.
The calcium chloride is used as the pore-forming agent, can volatilize at high temperature and is beneficial to the formation of pores, and the anhydrous ethanol is used as the bonding agent, so that the raw material components can be effectively combined together to ensure that the contact area of the reaction raw materials is larger. In addition, the degree of reduction and the sintered shape of the sample can be controlled by controlling the temperature and the firing process. The iron-based porous adsorption material prepared by the invention can adsorb OH in wastewater-、SO4 2-And Cl-In which to OH-Has an adsorption rate of 56-58% to SO4 2-The adsorption rate of (B) is 60-65%, and the adsorption rate to Cl is 60-65%—The adsorption rate of (B) is 72-75%.
The iron-based porous adsorption material has a large number of pores inside, and can adsorb acid radical ions and alkaline particles in wastewaterHas the following effects. The adsorption principle is as follows: the iron-based porous adsorption material of the invention is used for treating OH in wastewater-、SO4 2-And Cl-There is both physical adsorption and chemical adsorption. The physical adsorption accounts for a large proportion, and the physical adsorption mainly utilizes the porous structure of the iron-based porous adsorption material to have a high adsorption specific surface area. During sample preparation, Fe2O3The CO generated by the reaction with the carbon black under the high-temperature condition can improve the porosity, and the reduced iron simple substance has pores. The chemical adsorption is the selective adsorption of groups on the surface of a microporous structure, and an iron simple substance reduced from an iron-based porous adsorption material in acidic or alkaline wastewater and acid radical ions or alkali ions in the wastewater are subjected to chemical reaction. Due to Fe2+And Fe3+Is a good flocculant, and particularly has higher adsorption-flocculation activity; meanwhile, the adsorbent can adjust the pH value of the wastewater to change iron ions into ferric hydroxide flocculent precipitates and adsorb suspended or colloidal micro particles and organic macromolecules in the wastewater; part of COD in the wastewater is removed, the pollutant load of an A/O system is reduced, and the addition proportion of dilution water can be reduced; the biochemical degradation efficiency of the A/O system can be obviously improved, and the microbial degradation efficiency of the A/O system can be stably improved; can remove volatile phenols toxic substances and effectively reduce the toxic action on microorganisms of an A/O system.
The iron-based porous adsorption material is used for treating acid radical ions or alkali ions in wastewater, and has the advantages of low cost, sustainability, easiness in operation and the like.
Compared with the prior art, the invention has the following advantages:
1. the preparation method is simple, and Fe is subjected to mechanical ball milling2O3And carbon black to prepare the iron-based porous absorbentAn additional material;
2. the invention reduces the iron oxide powder by a powder metallurgy method to fully exert mechanical property, the carbon black fully exerts chemical property and physical property, and the reduction degree and strength of the iron-based porous adsorption material can be controlled by controlling carbon blending coefficient and sintering temperature.
3. The iron-based porous adsorption material has the advantages of low cost, good adsorption performance and convenient use, greatly reduces the labor intensity and the treatment and recovery cost, and has good application prospect.
Drawings
FIG. 1 is an SEM image (200 times) of an iron-based porous adsorption material prepared in example 1 of the present invention;
fig. 2 is an SEM (1000 x) of the iron-based porous adsorbent material prepared in example 1 of the present invention.
Detailed Description
Example 1
The iron-based porous adsorption material of the embodiment is mainly composed of Fe2O3And carbon black as raw materials, wherein the iron-based porous adsorption material contains 62% of simple substance iron and Fe2+With Fe3+The content of (2) is 34%, and the content of simple substance carbon is 4%.
The preparation method of the iron-based porous adsorption material of the embodiment comprises the following steps:
(1) preparing materials: mixing Fe2O3Weighing two raw materials according to the molar ratio of 1:0.3 with carbon black, and adding a pore-forming agent CaCl into the raw materials2The mass of the pore-forming agent is Fe2O31/26 based on the total weight of carbon black; adding steel balls into a ball milling tank according to a material-ball ratio of 5:1, setting the running time to be 5h and the rotating speed to be 400r/h, and starting a planetary ball mill for grinding;
(2) preparing a sample: sieving the ground raw materials with a 80-mesh sieve, adding an adhesive, namely absolute ethyl alcohol into the powder after uniform mixing, uniformly mixing, pouring the mixture into a material tank of an electric hydraulic sample making machine, pressing the mixture into a sample with the diameter of phi 20 multiplied by 20mm, and setting the pressure to be 80 MPa;
(3) and (3) sintering: placing the pressed sample into a vacuum atmosphere furnace, and setting the sintering process parameters as follows: keeping the temperature at 220 ℃ for 30min, keeping the temperature at 600 ℃ for 30min, keeping the temperature at 1200 ℃ for 2h, opening a circulating water valve, starting a vacuum pump to vacuumize, and discharging when the furnace temperature is cooled to be below 100 ℃.
The embodiment also provides application of the iron-based porous adsorption material in wastewater treatment.
In order to verify the adsorption effect of the iron-based porous adsorption material prepared in the embodiment on acid radical ions and alkaline ions in wastewater, 100mL of wastewater is selected, wherein OH is contained in the wastewater-In a concentration of 5%, SO4 2-Concentration of (2%), Cl-The concentration of the iron-based porous adsorption material is 2 percent, the adsorption time is 30min, the water temperature is 25 ℃, and the input amount of the iron-based porous adsorption material is 30 g. After one adsorption, the adsorbent material was washed clean and then the next adsorption test was performed for a total of 3 times, and the test results are shown in tables 1-3.
TABLE 1 iron-based porous adsorbent vs. OH-Adsorption Capacity test
TABLE 2 iron-based porous adsorbent materials vs SO4 2-Adsorption Capacity test
TABLE 3 iron-based porous adsorbent vs. Cl-Adsorption Capacity test
From the experimental results in the above table 1-3, it can be seen that the iron-based porous adsorption material prepared in this example has a dose of 30g to OH when the adsorption time is 30min, the water temperature is 25 ℃, and the iron-based porous adsorption material is added-Has an average adsorption rate of 57.3% for SO4 2-Has an average adsorption rate of 63.3% to Cl-The average adsorption rate of (2) was 73.5%.
As can also be seen from the above tables 1-2, the iron-based porous adsorbing material prepared in this example has a larger adsorption rate in the second adsorption compared to the first adsorption. The adsorption capacity is improved because the acid radical ions or the hydroxyl ions have corrosion action on the surface of the material in the adsorption process, so that the adsorption specific surface area is increased, and meanwhile, some impurities in the adsorption material are dissolved in the process, so that the hole structure channels are dredged, and the adsorption sites are increased.
Example 2
The iron-based porous adsorption material of the embodiment is mainly composed of Fe2O3And carbon black as raw materials, wherein the iron-based porous adsorption material contains 51% of simple substance iron and Fe2+With Fe3+The content of (2) is 48%, and the content of simple substance carbon is 1%.
The preparation method of the iron-based porous adsorption material of the embodiment comprises the following steps:
(1) preparing materials: mixing Fe2O3Weighing two raw materials according to the molar ratio of 1:0.225 with carbon black, and adding a pore-forming agent CaCl into the raw materials2The mass of the pore-forming agent is Fe2O31/30 based on the total weight of carbon black; adding steel balls into a ball milling tank according to a material-ball ratio of 4:1, setting the running time to be 4 hours and the rotating speed to be 500r/h, and starting a planetary ball mill for grinding;
(2) preparing a sample: sieving the ground raw materials with a 80-mesh sieve, adding an adhesive, namely absolute ethyl alcohol into the powder after uniform mixing, uniformly mixing, pouring the mixture into a material tank of an electric hydraulic sample making machine, pressing the mixture into a sample with the diameter of phi 20 multiplied by 20mm, and setting the pressure to be 80 MPa;
(3) and (3) sintering: placing the pressed sample into a vacuum atmosphere furnace, and setting the sintering process parameters as follows: keeping the temperature at 220 ℃ for 30min, keeping the temperature at 600 ℃ for 30min, keeping the temperature at 1200 ℃ for 2h, opening a circulating water valve, starting a vacuum pump to vacuumize, and discharging when the furnace temperature is cooled to be below 100 ℃.
The iron-based porous adsorption material prepared in the embodiment is applied to treatment of wastewater, wherein the wastewater contains acid radical ions and basic ions, and the acid radical ions comprise SO4 2-、Cl-One or a mixture of two, the basic ion comprises OH-. When the iron-based porous adsorption material of the embodiment is used for treating acid radical ions and alkaline ions in wastewater, the input amount can be selected according to the ion concentration in the wastewater, and the input amount is generally 1-58% of the total weight of the wastewater. When the method is used, the iron-based porous adsorption material can be made into a plastic shape and then placed into a cage-shaped bag to be thrown into water, the method is convenient to use and simple to operate, pollutants in water can be adsorbed after entering water, and the pollutants can be manually fished after adsorption is completed.
Example 3
The iron-based porous adsorption material of the embodiment is mainly composed of Fe2O3And carbon black as raw materials, wherein the iron-based porous adsorption material contains 68% of simple substance iron and Fe2+With Fe3+25% of (A), the content of elemental carbon is 7%.
The preparation method of the iron-based porous adsorption material of the embodiment comprises the following steps:
(1) preparing materials: mixing Fe2O3Weighing two raw materials according to the molar ratio of 1: 0.325 with carbon black, and adding a pore-forming agent CaCl into the raw materials2The mass of the pore-forming agent is Fe2O31/20 based on the total weight of carbon black; adding the steel balls into a ball milling tank according to a material-ball ratio of 4:1, setting the running time to be 5h and the rotating speed to be 500r/h, and starting a planetary ball mill for grinding;
(2) preparing a sample: sieving the ground raw materials with a 80-mesh sieve, adding an adhesive, namely absolute ethyl alcohol into the powder after uniform mixing, uniformly mixing, pouring the mixture into a material tank of an electric hydraulic sample making machine, pressing the mixture into a sample with the diameter of phi 20 multiplied by 20mm, and setting the pressure to be 80 MPa;
(3) and (3) sintering: placing the pressed sample into a vacuum atmosphere furnace, and setting the sintering process parameters as follows: keeping the temperature at 220 ℃ for 30min, keeping the temperature at 600 ℃ for 30min, keeping the temperature at 1200 ℃ for 2h, opening a circulating water valve, starting a vacuum pump to vacuumize, and discharging when the furnace temperature is cooled to be below 100 ℃.
The iron-based porous adsorption material prepared in this example can be used for wastewater treatment in the same manner as in examples 1 and 2.
Claims (6)
1. An iron-based porous adsorption material mainly comprising Fe2O3And carbon black as raw materials, which is characterized in that: the content of simple substance iron in the iron-based porous adsorption material is 50% -70%, and Fe2+With Fe3+The content of the carbon is 22-49 percent, and the content of simple substance carbon is 1-8 percent; the preparation method comprises the following steps:
(1) preparing materials: mixing Fe2O3Weighing two raw materials according to the molar ratio of 1:0.225-0.325 with carbon black, and adding a pore-forming agent CaCl into the raw materials2The mass of the pore-forming agent is Fe2O31/30-1/20 by total weight of carbon black; adding the steel balls into a ball milling tank according to the material-ball ratio of 4-5:1, setting the running time to be 4-5h and the rotating speed to be 400-;
(2) preparing a sample: sieving the ground raw materials with a 80-mesh sieve, adding an adhesive, namely absolute ethyl alcohol into the powder after uniform mixing, uniformly mixing, pouring the mixture into a material tank of an electric hydraulic sample making machine, pressing the mixture into a sample with the diameter of phi 20 multiplied by 20mm, and setting the pressure to be 80 MPa;
(3) and (3) sintering: placing the pressed sample into a vacuum atmosphere furnace, and setting the sintering process parameters as follows: keeping the temperature at 220 ℃ for 30min, keeping the temperature at 600 ℃ for 30min, keeping the temperature at 1200 ℃ for 2h, opening a circulating water valve, starting a vacuum pump to vacuumize, and discharging when the furnace temperature is cooled to be below 100 ℃.
2. An iron-based porous adsorbent material according to claim 1, characterized in that: the content of simple substance iron in the iron-based porous adsorption material is 62%, and Fe2+With Fe3+The content of (2) is 34%, and the content of simple substance carbon is 4%.
3. Use of an iron-based porous adsorbent material according to claim 1 or 2 in wastewater treatment.
4. Use of an iron-based porous adsorbent material according to claim 3 in wastewater treatment, characterized in that: the wastewater contains acid radical ions and alkaline ions.
5. Use of an iron-based porous adsorbent material according to claim 4 in wastewater treatment, characterized in that: the acid radical ions comprise SO4 2-、Cl-One or a mixture of two, the basic ion comprises OH-。
6. Use of an iron-based porous adsorbent material according to claim 4 in wastewater treatment, characterized in that: the input amount of the iron-based porous adsorption material is 1-58% of the total weight of the wastewater.
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| CN101816916A (en) * | 2010-04-26 | 2010-09-01 | 山东大学 | Technology for preparing phosphorus adsorbent |
| CN102838105A (en) * | 2012-09-11 | 2012-12-26 | 安徽工业大学 | Preparation method of grading porous carbon material |
| CN106076256A (en) * | 2016-07-06 | 2016-11-09 | 中山大学 | A kind of preparation method and applications of nanometer Fe (0) porous mud material with carbon element |
| CN108821285A (en) * | 2018-02-12 | 2018-11-16 | 哈尔滨工业大学 | A kind of method that ferrous metals salt melting infiltration prepares coal Quito hole active carbon material |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101816916A (en) * | 2010-04-26 | 2010-09-01 | 山东大学 | Technology for preparing phosphorus adsorbent |
| CN102838105A (en) * | 2012-09-11 | 2012-12-26 | 安徽工业大学 | Preparation method of grading porous carbon material |
| CN106076256A (en) * | 2016-07-06 | 2016-11-09 | 中山大学 | A kind of preparation method and applications of nanometer Fe (0) porous mud material with carbon element |
| CN108821285A (en) * | 2018-02-12 | 2018-11-16 | 哈尔滨工业大学 | A kind of method that ferrous metals salt melting infiltration prepares coal Quito hole active carbon material |
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