CN113694882B - Preparation method of bulk phase loaded zero-valent iron biochar material - Google Patents
Preparation method of bulk phase loaded zero-valent iron biochar material Download PDFInfo
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- CN113694882B CN113694882B CN202010445914.4A CN202010445914A CN113694882B CN 113694882 B CN113694882 B CN 113694882B CN 202010445914 A CN202010445914 A CN 202010445914A CN 113694882 B CN113694882 B CN 113694882B
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
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- B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character
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Abstract
The invention discloses a preparation method of bulk phase loaded zero-valent iron biochar material, which is characterized in that suitable crop plants are planted in red soil, the crop plants absorb iron components in the red soil, the crop plants are treated and then subjected to anaerobic pyrolysis at a suitable temperature to obtain the bulk phase loaded zero-valent iron biochar material, and iron is stably embedded and loaded in biochar and is more reliable and durable when being used as a repairing material.
Description
Technical Field
The invention relates to a novel environment-friendly material, in particular to a bulk phase loaded zero-valent iron biochar material and a preparation method thereof.
Background
Heretofore, environmental pollution such as water pollution, soil pollution and the like has received global attention. Researchers find that zero-valent metals such as magnesium, copper, iron and the like have great advantages in removing underground refractory organic pollutants. Compared with other zero-valent metals, the zero-valent iron has simple preparation process, complete reaction and no secondary pollution to environment, and has wide attention in engineering application due to low cost and easy acquisition.
Among them, the nanoscale zero-valent iron can induce special surface effect and quantum effect due to its large specific surface area and surface energy, and has been widely used as an efficient repair material.
However, the nano zero-valent iron is very easy to be oxidized in the air to form a passivation layer to reduce the activity, and the nano zero-valent iron is easy to agglomerate to greatly reduce the specific surface area and the reaction activity, so that the reduction capability is reduced, and the application of the nano zero-valent iron is greatly limited.
For this reason, researchers often improve the removal performance of the nano zero-valent iron to heavy metals by using a method of biochar modification. The existing method for modifying nano zero-valent iron by using biochar is mainly to prepare a biochar nano zero-valent iron-nickel compound by soaking biomass to adsorb iron salt and the like and then performing steps of pyrolysis and the like. Even further, researchers have further modified the nickel by using nickel salts and the like. The biochar nano zero-valent iron-nickel composite obtained by the method is a surface-supported composite, and the stability and the like of the biochar nano zero-valent iron-nickel composite are required to be improved.
Disclosure of Invention
In order to overcome the above problems, the present inventors have conducted intensive studies and, as a result, found that: planting proper crop plants in the red soil, absorbing iron components in the red soil by the crop plants, treating the crop plants, and then pyrolyzing the treated crop plants at a proper temperature in an anaerobic manner to obtain a bulk phase loaded zero-valent iron biochar material, wherein iron is stably loaded in the biochar, thereby completing the invention.
The object of the present invention is to provide the following:
1. a bulk phase loaded zero-valent iron biochar material, wherein an iron body phase is loaded in biochar.
2. Bulk phase zero-valent iron-loaded biochar material as described in 1 above, wherein the zero-valent iron loading increases from the biochar surface to the biochar interior.
3. The bulk-phase zero-valent iron-loaded biochar material as described in the above 1, wherein nano zero-valent iron particles are dispersedly embedded in the biochar.
4. The bulk phase zero-valent iron-loaded biochar material as in the above 1, wherein the biochar is obtained from red soil suitable crop plants, and the red soil suitable crop plants are selected from one or more of ramie, common dayflower herb, iris and canna.
5. The bulk-loaded zero-valent iron biochar material as described in 4 above, wherein the red soil suitable crop plants are selected from ramie.
6. A method for preparing bulk zero-valent iron-loaded biochar material, which is obtained by anaerobic pyrolysis of crop plants planted in red soil.
7. The method of claim 6, wherein the crop plants are planted in the red soil for more than 3 months.
8. A method as described in 7 above, wherein the crop plants are planted in red soil with a nutrient containing citric acid applied.
9. The method as described in 6 above, wherein the pyrolysis is performed at a temperature of 500-900 ℃.
10. The method as described in 6 above, wherein the pyrolysis is performed at a temperature of 700-850 degrees celsius.
The invention has the following advantages:
(1) According to the bulk phase load zero-valent iron biochar material provided by the invention, zero-valent iron is stably loaded in biochar, zero-valent iron particles are not agglomerated and are dispersedly and stably loaded in the biochar in an embedding manner, so that the bulk phase load zero-valent iron biochar material is more reliable when being used as a repairing material;
(2) According to the bulk phase load zero-valent iron biochar material provided by the invention, the bulk phase load of zero-valent iron is gradually increased from the biochar surface to the inner layer, so that the reliability and durability of the biochar material as a repair material are further improved;
(3) The bulk phase load zero-valent iron biochar material provided by the invention comprises an iron-carbon compound formed by iron and carbon, so that the reliability and durability of the material used as a repair material are further improved;
(4) According to the preparation method of the bulk phase zero-valent iron-loaded charcoal material, common crop plants are planted in the red soil to serve as raw materials of the bulk phase zero-valent iron-loaded charcoal material, so that the cost is low, the operation is convenient, and the implementation is easy;
(5) The preparation method of the bulk phase zero-valent iron-loaded biochar material provided by the invention selects a proper temperature to ensure that the prepared bulk phase zero-valent iron-loaded biochar material has use reliability and durability.
Drawings
Fig. 1 shows an XRD spectrum of the bulk phase zero-valent iron-loaded biochar material 11 obtained in example 1 of the present invention.
Fig. 2 shows a TEM photograph of the bulk phase zero-valent iron-loaded biocarbon material 11 obtained in example 1 of the present invention.
Detailed Description
The present invention will be described in further detail below with reference to preferred embodiments and examples. The features and advantages of the present invention will become more apparent from the description.
The word "exemplary" is used exclusively herein to mean "serving as an example, embodiment, or illustration. Any embodiment described herein as "exemplary" is not necessarily to be construed as preferred or advantageous over other embodiments.
According to the bulk-phase zero-valent iron-loaded biochar material provided by the invention, plant crops are planted in red soil rich in (ferrous) iron, iron ions are absorbed by the crop plants and are transmitted to various organ tissues such as roots, stems and leaves, and the like, the iron ions are enriched in the crop plants through long-term growth and accumulation, and after anaerobic pyrolysis, the bulk phase of the zero-valent iron formed by reduction is loaded in the biochar.
As a raw material for forming the biochar, it has been found that crop plants suitable for red soil, such as ramie, dayflower, iris, canna, and the like, can be used. The inventor finds that the plants can be well enriched with iron, particularly ramie, and the enrichment effect is better through a large number of experiments.
As a biochar raw material, the carbon fiber content in the ramie is high, the bulk phase loaded zero-valent iron biochar material obtained from the ramie has a large specific surface area, and the ramie is planted once as perennial root crops, can be harvested for multiple times, is convenient to operate and has high utilization efficiency.
In practice, the crop plants are grown for as long a period as possible in order to ensure iron enrichment. The present inventors found that a planting period of 3 months or more is necessary to ensure the iron enrichment effect, and a planting period of 4 months or more is more advantageous, and a planting period of 6 months or more is more preferable.
The present inventors have found that the application of aqueous citric acid as a nutrient helps to improve iron enrichment in the biomass when growing crop plants. Preferably, the concentration of the aqueous citric acid solution is not higher than 1g/L, more preferably not higher than 500mg/L, and still more preferably in the range of 185 to 450 mg/L.
In the present invention, as a crop plant, the whole can be used as a raw material for obtaining biochar by pyrolysis. The present inventors have found that roots of crop plants, after pyrolysis, have a higher iron loading relative to the stems and leaves of the crop plants and are therefore more preferred.
Before pyrolysis, it is generally necessary to dry, pulverize and subject the crop plant parts to be pyrolyzed to a pyrolysis treatment.
The inventor finds that the influence of the pyrolysis temperature on the bulk zero-valent iron-loaded biochar material is remarkable. Under the temperature of 500-900 ℃, the stable bulk phase loaded zero-valent iron biochar material can be obtained.
In a preferred embodiment, the thermal pyrolysis of the dried and crushed particles of the crop plants is carried out at a temperature of 700-850 ℃, when part of zero-valent iron is stably supported in the biochar in the form of gamma-Fe, and iron carbon compounds are generated, so that the use reliability and durability of the bulk zero-valent iron-supported biochar material are further improved.
The pyrolysis reaction time is preferably 1 to 3 hours, preferably 1 to 1.5 hours. If the reaction time is too short, the content of zero-valent iron in the obtained phase zero-valent iron-loaded biochar material is relatively low, and if the reaction time is too long, the activity of the obtained phase zero-valent iron-loaded biochar material is deteriorated.
Examples
The present invention is further described below by way of specific examples, which are merely exemplary and do not limit the scope of the present invention in any way.
Example 1
Example 1
The ramie is planted in the red soil for 130 days, and 200mg/L of citric acid aqueous solution is sprayed every week. After 130 days, the hemp stalks were cut. Washing with deionized water, soaking in 0.01M dilute hydrochloric acid for 1 hr, oven drying at 70.0 deg.C, and pulverizing into 2mm granules. And pyrolyzing the crushed particles in a tubular muffle furnace at the temperature of 700 ℃ for 90 minutes to prepare the bulk phase loaded zero-valent iron biochar material.
The XRD spectrogram of the bulk phase zero-valent iron-loaded biochar material is shown in figure 1, wherein the diffraction peaks of zero-valent iron are 44.8 degrees, 65.1 degrees and 82.2 degrees, and the diffraction peaks of iron-carbon compounds CFe are 43.1 degrees, 50.4 degrees and 73.9 degrees 15.1 Diffraction peaks.
TEM of bulk phase loaded zero-valent iron biochar materials revealed that the zero-valent iron particles were dispersedly embedded in the biochar bulk phase.
XPS of bulk zero-valent iron-loaded biochar material revealed that the zero-valent iron content at the surface, at the depth of 40nm and at the depth of 80nm was 1.41%, 9.02% and 18.35, respectively.
Example 2
Planting ramie in red soil for 150 days, and cutting ramie stalks after 150 days. Washing with deionized water, soaking in 0.01M dilute hydrochloric acid for 1 hr, oven drying at 70.0 deg.C, and pulverizing into 2mm granule. And pyrolyzing the crushed particles in a tubular muffle furnace at the temperature of 600 ℃ to prepare the bulk phase loaded zero-valent iron biochar material.
The XRD and TEM results of the bulk zero-valent iron-loaded biochar material are similar to those in example 1.
Its XPS revealed that the zero valent iron content at its surface, at a depth of 40nm and at a depth of 80nm was 1.38%, 8.98% and 18.32, respectively.
Example 3
The ramie is planted in the red soil for 150 days, and 100mg/L citric acid aqueous solution is sprayed every week. Cutting hemp stalk after 150 days. Washing with deionized water, soaking in 0.01M dilute hydrochloric acid for 1 hr, oven drying at 70.0 deg.C, and pulverizing into 2mm granules. And pyrolyzing the crushed particles in a tubular muffle furnace at 800 ℃ to prepare the bulk phase zero-valent iron-loaded biochar material.
The XRD and TEM results of the bulk zero-valent iron-loaded biochar material are similar to those in example 1.
Its XPS revealed that the zero valent iron content at its surface, at a depth of 40nm and at a depth of 80nm was 1.43%, 9.06% and 18.44, respectively.
Experimental example 1
100ml of water and 5mg of dichlorodiphenyl trichloroethane were put into a 200ml Erlenmeyer flask, 20mg of the bulk phase zero-valent iron-supporting biochar material obtained in example 1 and 3ml of a potassium persulfate solution having a concentration of 3g/L were put into the flask, the mixture was shaken up, 1ml of the mixture was sampled every 30 minutes, the concentration of ferrous ions in the solution was measured by UV spectroscopy, and the dichlorodiphenyl trichloroethane concentration was measured by gas chromatography.
The concentration of ferrous ions in the solution is basically kept at 0.0049mg/ml, the concentration of the dichlorodiphenyl trichloroethane after 7 hours is 0.0015mg/ml, the concentration of the dichlorodiphenyl trichloroethane after 8 hours is 0.0007mg/ml, and the concentration of the dichlorodiphenyl trichloroethane after 9 hours is 0.0001mg/ml.
And taking out the bulk phase loaded with the zero-valent iron biochar material after 10 hours, washing with methanol for three times, and drying, wherein an XRD spectrogram is shown in figure 1.
The invention has been described in detail with reference to specific embodiments and illustrative examples, but the description is not intended to be construed in a limiting sense. Those skilled in the art will appreciate that various equivalent substitutions, modifications or improvements may be made to the embodiments and implementations of the invention without departing from the spirit and scope of the invention, and are within the scope of the invention.
Claims (1)
1. A method for preparing a bulk zero-valent iron-loaded biochar material by anaerobic pyrolysis of crop plants grown in red soil, as follows:
planting ramie in red soil for 130 days, and spraying 200mg/L citric acid aqueous solution every week; cutting hemp stalk after 130 days; washing with deionized water, soaking in 0.01M dilute hydrochloric acid for 1 hr, oven drying at 70.0 deg.C, and pulverizing into 2mm granule; pyrolyzing the crushed particles in a tubular muffle furnace at 700 ℃ for 90 minutes to prepare a bulk phase zero-valent iron-loaded biochar material;
in XRD spectrogram of bulk phase zero-valent iron-loaded biochar material, zero-valent iron diffraction peaks at 44.8 degrees, 65.1 degrees and 82.2 degrees and iron-carbon compound CFe at 43.1 degrees, 50.4 degrees and 73.9 degrees 15.1 Diffraction peaks.
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