CN110548879A - Preparation method and application of green synthetic novel iron-carbon material - Google Patents
Preparation method and application of green synthetic novel iron-carbon material Download PDFInfo
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- CN110548879A CN110548879A CN201910480707.XA CN201910480707A CN110548879A CN 110548879 A CN110548879 A CN 110548879A CN 201910480707 A CN201910480707 A CN 201910480707A CN 110548879 A CN110548879 A CN 110548879A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/17—Metallic particles coated with metal
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/70—Treatment of water, waste water, or sewage by reduction
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
- C02F2101/22—Chromium or chromium compounds, e.g. chromates
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/38—Organic compounds containing nitrogen
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/40—Organic compounds containing sulfur
Abstract
The invention relates to the field of preparation and application of environment restoration materials, in particular to a preparation method of a green synthetic novel iron-carbon material, which is characterized in that red clover extract is used as a reducing agent to replace NaBH 4 to prepare zero-valent iron.
Description
Technical Field
The invention relates to the field of preparation of environment-friendly repairing materials, in particular to a preparation method of a green synthetic novel iron-carbon material.
Background
Since the 80 s in the 20 th century, zero-valent iron has gradually become the key point of research on environmental remediation materials by virtue of being non-toxic, abundant in content, cheap and easy to produce, and good in pollutant removal effect. But the outstanding problems that currently limit the application of zero-valent iron are: (1) the surface is easy to passivate in the using and storing processes, the storage and the service life of the material are limited, and the material occupies reactive sites on the surface of the material, so that the material is prevented from contacting with pollutants, the activity of the material is reduced, and the degradation rate is reduced; (2) in practical applications, due to magnetic forces and van der waals forces, particles attract each other and agglomerate into micro-scale or even larger particles, thereby affecting their reactivity and migratory diffusion capability.
the biochar has larger specific surface area and porosity, and in addition, contains a large amount of mineral components, such as aromatic structures, oxygen-containing functional groups and the like, wherein the aromatic structures enable the biochar to have stronger chemical and biological stability, be not easily decomposed and exist for a long time; due to the existence of the oxygen-containing functional group, the biochar has good adsorption capacity and can be used for treating organic matters, heavy metals and other pollutants in the environment. Therefore, the biochar is widely used as a carrier of the nano zero-valent iron. At present, most of biochar materials are crop straws, shells, vegetables, sawdust, sludge and the like, and aquatic plants have relatively few researches on making biochar. The duckweed is a water surface floating plant, is widely distributed, has short growth period and is easy to salvage.
Herba Trifolii Pratentis is a perennial herb of Leguminosae, also named as Trifolium Pratense L and Trifolium Pratense L. Herba Trifolii Pratentis contains flavonoids, proteins, amino acids, saccharides and vitamins. The method is one of a few plants which are unique in 4 kinds of abundant and balanced isoflavone substances in the world, the isoflavone has a polyphenol hydroxyl structure and has strong reducibility and oxidation resistance, and the method for reducing zero-valent iron by using the red clover extracting solution is a green and environment-friendly synthesis method and has good application prospect.
4In addition, the invention takes duckweed as a biomass raw material, and adds soluble starch on the basis of zero-valent iron loaded by biochar, the starch can be used as a good template or a dispersing agent, so that the nano material has better dispersing capacity, the zero-valent iron is more uniformly dispersed on the biochar, and simultaneously, the starch can effectively prevent the aggregation of nano particles and the inactivation of the material.
Disclosure of Invention
the invention aims to improve the application limit of nano zero-valent iron repairing materials in the field of environmental repair, and provides a preparation method of a green synthetic novel iron-carbon material.
The preparation method of the green synthetic novel iron-carbon material comprises the following steps:
a. Pretreatment of biomass material: cleaning herba Spirodelae with deionized water, oven drying at 60-80 deg.C, and pulverizing to 20-50mm with pulverizer.
b. and (3) preparing the biochar, namely placing the pretreated biomass material in a porcelain boat, placing the porcelain boat in a tubular furnace, performing pyrolysis in the atmosphere of N 2, wherein the initial temperature is 40 ℃, heating to 400-plus-800 ℃ at the heating rate of 5 ℃/min, and keeping for 2h to prepare the biochar, grinding, and sieving with a 100-mesh sieve for later use.
c. Preparing red clover extract: weighing 6g of red clover powder, placing the red clover powder into a 250mL round-bottom flask, adding a certain amount of mixed solution (volume ratio V) of anhydrous ethanol and deionized waterWater (W)：VEthanol=4: 6), placing into an ultrasonic cleaner, carrying out reflux extraction in a water bath at 60 ℃, carrying out centrifugal filtration, and transferring into a sample bottle for standby.
d. The preparation method of the improved biochar loaded zero-valent iron comprises the steps of dissolving a certain amount of FeSO 4 & lt 7 & gt H 2 O in a mixed solution of ethanol and deionized water, magnetically stirring for 30min in a three-necked flask, adding a certain amount of soluble starch, continuously stirring for 30min, adding a certain amount of prepared biochar, continuously stirring for 30min, transferring the red clover extracting solution to a separating funnel, slowly dripping into a reaction system, continuously stirring for 30min after dripping is finished, enabling the reaction system to fully react, washing with deionized water and absolute ethyl alcohol, centrifuging, freezing for 12H at-4 ℃, and drying for 13H by using a freeze dryer, so that the green synthetic novel iron carbon material is prepared.
N 2 was continuously introduced during the preparation of the material in step d.
Preferably, the biomass pyrolysis temperature is 500-.
Preferably, the proportion of the ethanol and deionized water mixed solution in the preparation process of the novel iron-carbon material is VWater (W)：VEthanol=7:3。
preferably, the optimal ratio of the biochar, the starch and the zero-valent iron is 1:3: 3.
the invention has the following advantages:
(1) the synthetic method is green and pollution-free, the red clover is one of a few plants which are unique and have 4 abundant and balanced isoflavone substances in the world, the isoflavone has a polyphenol hydroxyl structure and has stronger reducibility and oxidation resistance, and compared with a chemical reducing agent NaBH 4, the plant extracting solution is safer and more environment-friendly.
(2) The dispersibility is good: the starch has better dispersing capacity on the nano material, so that the zero-valent iron is more uniformly dispersed on the biochar, and simultaneously, the starch can effectively prevent the agglomeration of nano particles and the inactivation of the material.
Drawings
FIG. 1 is a graph comparing FTIR with and without the addition of soluble starch.
FIG. 2 is a comparison graph of the effect of the novel iron-carbon material prepared by the present invention and pure biochar/zero-valent iron on Cr (VI) removal in water.
FIG. 3 is a comparison graph of the effect of the novel iron-carbon material prepared by the present invention and pure biochar/zero-valent iron on removing methylene blue from water.
FIG. 4 is a graph showing the change of the removal rate of Cr (VI) in soil with the increase of water-soil ratio of the novel iron-carbon material prepared by the invention.
FIG. 5 is a color comparison graph of the novel iron-carbon material prepared by the invention after reacting with pure biochar/zero-valent iron and Cr (VI) solution for 10 min.
FIG. 6 is a color comparison graph of the novel iron-carbon material prepared by the present invention after reacting with pure biochar/zero-valent iron and methylene blue solution for 10 min.
Detailed Description
The following embodiments describe the preparation of a green synthetic novel iron-carbon material and its application effect in detail. It should be noted that the following embodiments are only for illustrating the effects of the technical solutions of the present invention, and are not intended to limit the present invention.
example 1:
(1) Pretreatment of biomass material: cleaning herba Spirodelae with deionized water, oven drying at 60-80 deg.C, and pulverizing to 20-50mm with pulverizer.
(2) And (2) preparing the biochar, namely placing the biomass material in the step (1) in a porcelain boat, putting the porcelain boat in a tubular furnace, pyrolyzing the porcelain boat in the atmosphere of N 2, wherein the initial temperature is 40 ℃, the temperature is increased to 600 ℃ at the temperature increase rate of 5 ℃/min, and the temperature is kept for 2 hours to obtain the biochar, grinding the biochar, and sieving the biochar with a 100-mesh sieve for later use.
(3) preparing red clover extract: weighing 6g of red clover powder, placing the red clover powder into a 250mL round-bottom flask, adding a certain amount of mixed solution (volume ratio V) of anhydrous ethanol and deionized waterWater (W)：VEthanol=4: 6), placing into an ultrasonic cleaner, carrying out reflux extraction in a water bath at 60 ℃, carrying out centrifugal filtration, and transferring into a sample bottle for standby.
(4) Preparation of iron salt solution: 4.47g of FeSO4﹒7H2dissolving O in the mixed solution of deionized water and ethanol at a ratio of VWater (W)：VEthanolAnd (4) =7:3, thus obtaining an iron salt solution.
(5) and (3) preparing the amyloferric salt solution, namely transferring the ferric salt solution into a three-neck flask, introducing N 2, adding 0.9g of starch after 10min, magnetically stirring for 30min to obtain the amyloferric salt solution, and continuously introducing N 2 in the preparation process.
(6) And (3) preparing a biological carbon amyloferric salt solution, namely adding 0.3g of the biological carbon obtained in the step (2) into the amyloferric salt solution, magnetically stirring for 30min to obtain the biological carbon amyloferric salt solution, and continuously introducing N 2 in the preparation process.
(7) And (3) slowly dripping the red clover extracting solution obtained in the step (3) into the biological carbon amyloferric salt solution, continuously stirring for 30min after dripping is finished, continuously introducing N 2 in the preparation process, washing and centrifuging by using deionized water and absolute ethyl alcohol, freezing for 12h at-4 ℃, and drying for 13h by using a freeze dryer to obtain the novel iron carbon material.
The novel iron carbon material was scanned using infrared light.
Example 2:
The prepared novel iron-carbon material is applied to the removal experiment of Cr (VI) in water. 0.10g of the novel iron-carbon material is added into 100mL of Cr (VI) solution with the concentration of 50mg/L, and the solution is put into a constant temperature oscillation box to oscillate for 3 hours at the room temperature at the rotating speed of 100 r/min. Sampling at 10min, 30min, 60 min, 90 min, 120 min and 180 min, filtering with a 0.45-micron filter, and measuring the Cr (VI) concentration in the sample by using an ultraviolet-wind-solar photometry to obtain a degradation curve of the novel iron-carbon material to Cr (VI).
Example 3:
The prepared novel iron-carbon material is applied to the removal experiment of methylene blue in water. 0.05g of the novel iron-carbon material is added into 60mL of methylene blue solution with the concentration of 0.1g/L, and the solution is put into a constant temperature oscillation box to oscillate for 1h at the room temperature at the rotating speed of 100 r/min. Sampling at 10min and 30min, filtering with a 0.45-micrometer filter, and measuring absorbance at the wavelength of 664nm by using a spectrophotometer to obtain the degradation curve of the novel iron-carbon material to methylene blue.
Example 4:
The prepared novel iron-carbon material is applied to the removal experiment of Cr (VI) in soil. Collecting 0.5kg of common soil, adding 500mL of Cr (VI) solution with the concentration of 200mg/L, stirring and mixing uniformly, standing in a ventilated place without direct sunlight, naturally airing for one month, and sieving by using a 2mm standard sieve to prepare the soil with the theoretical Cr (VI) concentration of 200 mg/kg. Respectively pouring 10g of sieved soil into a 250mL conical flask, adding 0.05g of novel iron-carbon material, respectively adding 20mL, 50mL and 100mL of deionized water, sealing, placing the conical flask into a constant-temperature shaking incubator at 25 ℃ for shaking for 5h at a speed of 150r/min, taking supernatant after shaking is finished, and measuring the concentration of Cr (VI) in the supernatant by a spectrophotometry method. Separating the residue in the conical flask by a centrifuge, drying in a vacuum freeze dryer, digesting the dried soil, and determining the concentration of Cr (VI) in the digested liquid. The effect of different water and soil ratios on the Cr (VI) removal effect in the soil is studied, and the result is shown in FIG. 4. The graph shows that the Cr (VI) removal rate is reduced with the increase of the water-soil ratio, and the removal rate is up to 90% at the water-soil ratio of 2: 1.
Comparative example 1:
In the preparation process of the material in the example 1, soluble starch is not added, and other steps are repeated in the example 1. As shown in figure 1, the C = C bond of the novel iron-carbon material prepared by the invention is reduced, CH 2 is correspondingly increased, and the saturation of the carbon is enhanced.
Comparative example 2:
the novel iron-carbon material prepared by the patent is changed into biological carbon/zero-valent iron material without adding starch, and other steps are repeated to obtain the product of example 2. As can be seen from FIG. 2, the novel iron-carbon material prepared by the method has a Cr (VI) removal rate which is obviously higher than that of a pure biochar/zero-valent iron material, and the removal rate reaches 75% in the first 10 min.
Comparative example 3:
The novel iron-carbon material prepared by the patent is changed into biological carbon/zero-valent iron material without adding starch, and other steps are repeated to obtain the product of example 3. As can be seen from FIG. 3, the removal rate of the novel iron-carbon material prepared by the invention to methylene blue is obviously higher than that of a pure biochar/zero-valent iron material, and the removal rate reaches 86% in the first 10 min.
Comparative example 4:
the novel iron-carbon material prepared by the patent is changed into biological carbon/zero-valent iron material without adding starch, and other steps are repeated to obtain the iron-carbon material of the example 4. As can be seen from FIG. 4, the removal rate of the novel iron-carbon material prepared by the method disclosed by the invention on Cr (VI) in soil is obviously higher than that of a pure biochar/zero-valent iron material, and the removal rate is as high as 83%.
Claims (5)
1. A preparation method of green synthetic novel iron-carbon material is characterized by comprising the following steps:
(1) Pretreatment of biomass material;
(2) Preparing biochar;
(3) And (3) preparing a novel iron-carbon material.
2. The method for preparing green synthesized novel iron-carbon material according to claim 1, wherein the biomass material in (1) is duckweed.
3. The method as claimed in claim 1, wherein the biochar preparation in step (2) is performed by pyrolysis in a tubular furnace at an initial temperature of 40 ℃, a heating rate of 5 ℃/min, a temperature of 400 ℃ and 800 ℃, and a calcination time of 2 h.
4. The method for preparing green synthetic novel iron carbon material as claimed in claim 1, wherein the reducing agent in step (3) is red clover extract.
5. the method for preparing green synthetic novel iron carbon material according to claim 1, characterized in that in the step (3), the biological carbon: starch: the theoretical mass ratio of the zero-valent iron is 1:3: 3.
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Cited By (4)
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| CN111054312A (en) * | 2020-01-15 | 2020-04-24 | 中新曜昂环境修复(江苏)有限公司 | Preparation method of duckweed charcoal loaded nano zero-valent iron and method for repairing Pb pollutant soil |
| CN111410305A (en) * | 2020-04-07 | 2020-07-14 | 佛山科学技术学院 | Chromium-polluted water body remediation method and application |
| CN112246848A (en) * | 2020-10-23 | 2021-01-22 | 麻崇明 | Application of clover to treatment of residual compound solution after potassium permanganate preparation of oxygen |
| CN114984911A (en) * | 2022-06-13 | 2022-09-02 | 陕西学前师范学院 | Preparation method of high-adsorption-performance biochar-nano zero-valent iron compound |
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| CN111410305A (en) * | 2020-04-07 | 2020-07-14 | 佛山科学技术学院 | Chromium-polluted water body remediation method and application |
| CN112246848A (en) * | 2020-10-23 | 2021-01-22 | 麻崇明 | Application of clover to treatment of residual compound solution after potassium permanganate preparation of oxygen |
| CN114984911A (en) * | 2022-06-13 | 2022-09-02 | 陕西学前师范学院 | Preparation method of high-adsorption-performance biochar-nano zero-valent iron compound |
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