CN113019326A - Iron-based-carboxyl modified biochar and preparation method and application thereof - Google Patents
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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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- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0225—Compounds of Fe, Ru, Os, Co, Rh, Ir, Ni, Pd, Pt
- B01J20/0229—Compounds of Fe
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- B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
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- B09C1/00—Reclamation of contaminated soil
- B09C1/08—Reclamation of contaminated soil chemically
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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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- B01J2220/4875—Sorbents characterised by the starting material used for their preparation the starting material being a waste, residue or of undefined composition
- B01J2220/4887—Residues, wastes, e.g. garbage, municipal or industrial sludges, compost, animal manure; fly-ashes
Abstract
The invention relates to the technical field of remediation of heavy metal pollution in non-ferrous smelting sites, and particularly relates to iron-based-carboxyl modified biochar and a preparation method and application thereof. The preparation method specifically comprises the following steps: pretreating a biomass raw material and then pyrolyzing to obtain biochar; mixing biochar with a hydrogen peroxide solution in a solid-to-liquid ratio of 1:10-20, stirring for reaction, filtering to obtain filter residue, and drying to obtain modified biochar; mixing the high-iron red mud and a sulfuric acid solution in a solid-to-liquid ratio of 1-3:1-2, reacting, centrifuging and filtering to obtain a filtrate, and obtaining an iron-based impregnation solution; adding the modified biochar into the iron-based impregnation liquid for ultrasonic impregnation, filtering to obtain filter residues, and cleaning and drying to obtain the iron-based-carboxyl modified biochar composite material. The preparation method is simple in process and mild in condition, and the obtained modified composite material can effectively reduce the biological effectiveness of heavy metals such as antimony, cadmium and the like in an antimony smelting site and improve the soil survival rate of the site.
Description
Technical Field
The invention relates to the technical field of remediation of heavy metal pollution in non-ferrous smelting sites, and particularly relates to iron-based-carboxyl modified biochar and a preparation method and application thereof.
Background
A large amount of antimony-containing waste is generated in the antimony smelting process and migrates in different environment media, so that soil and water pollution is easily caused, and the human health is threatened. In recent years, antimony levels have been found to exceed corresponding environmental standards in various environmental media around the world. In the antimony smelting field, heavy metals such as antimony in the field soil seriously exceed the standard due to smelting process, atmospheric settlement and the like, so that the attention of researchers is attracted.
Antimony in antimony smelting site is mainly pentavalent antimony (Sb (OH)6 -) The form of (A) is present, and accounts for almost more than 90% of the total antimony content. The pentavalent antimony is an oxyanion, and the higher the pH value in the soil system, the stronger the antimony migration in the soil. The biochar is cheap and easy to obtain, environment-friendly, large in specific surface area and good in adsorption and passivation effects on cationic heavy metals such as lead and cadmium in soil. However, the currently used biochar is generally alkaline and has no obvious effect on antimony, and the activity and the migration capacity of the biochar in soil can be even increased, so that the soil antimony pollution is caused. In addition, the heavy metal types in the soil of the antimony smelting site are various, the pollution degree difference is large, and the charcoal material is not beneficial to the application of the charcoal material in the remediation of the heavy metal in the soil of the nonferrous smelting site because the adsorption sites are not enough and the capacity of fixing the heavy metal is limited; red mud is a typical bulk industrial solid waste, and resource utilization of the red mud becomes a hotspot and difficulty of current research.
Disclosure of Invention
Aiming at the problems in the prior art, the invention develops an iron-based-carboxyl modified biochar composite material based on the adsorption and passivation selectivity of different types of heavy metals on corresponding groups in an antimony smelting site through industrial and agricultural solid wastes such as biomass, red mud and the like so as to realize the synchronous passivation of the multiple metals in the antimony smelting site.
In order to achieve the above object, the present invention provides a preparation method of iron-based-carboxyl modified biochar, which specifically comprises:
s1: pretreating a biomass raw material and then pyrolyzing to obtain biochar; the biomass raw material is one or more of birch, hickory shell, pine needle and vinegar residue;
s2: mixing the biochar with a hydrogen peroxide solution in a solid-to-liquid ratio of 1:10-20, stirring for reaction, filtering to obtain filter residue, and drying to obtain modified biochar;
s3: mixing the high-iron red mud and a sulfuric acid solution in a solid-to-liquid ratio of 1-3:1-2, reacting, centrifuging and filtering to obtain a filtrate, and obtaining an iron-based impregnation solution;
s4: and adding the modified biochar into the iron-based impregnation liquid for ultrasonic impregnation, filtering to obtain filter residues, and cleaning and drying to obtain the iron-based-carboxyl modified biochar composite material.
Further, the step of pretreating the biomass raw material and then pyrolyzing the pretreated biomass raw material to obtain the biochar specifically comprises the following steps:
crushing, cleaning and drying a biomass raw material to obtain a dry biomass raw material;
and (2) putting the dried biomass raw material into an inert atmosphere for pyrolysis for 2-4h, wherein the pyrolysis temperature is 200-600 ℃, introducing inert gas after pyrolysis is finished, cooling to room temperature, cleaning, and drying at 60 ℃ for 12-24h to obtain the biochar.
Further, the specific process parameters in step S2 are as follows:
the concentration of the hydrogen peroxide solution is 25-35%;
the temperature of the stirring reaction is 40-60 ℃, and the reaction time is 6-12 h.
Further, the content of iron and aluminum oxides in the high-iron red mud is respectively 30-50% and 15-25%, and the concentration of the sulfuric acid solution is 1-3 mol/L.
Further, the solid-to-liquid ratio of the modified biochar to the iron-based impregnating solution is 1:20-60, and the ultrasonic impregnation time is 40-60 min.
Further, deionized water is adopted in the cleaning process in the step S4, the temperature in the drying process is 60 ℃, and the drying time is 12-24 hours.
Based on the same invention idea, the invention provides the iron-based-carboxyl modified biochar which is prepared according to the preparation method.
Based on the same inventive concept, the invention also provides application of the iron-based carboxyl modified biochar prepared by the preparation method in heavy metal contaminated soil remediation.
Further, the heavy metal pollution comprises single antimony, arsenic or lead pollution or composite heavy metal pollution containing antimony, arsenic and lead.
Further, the application method specifically comprises the following steps:
adding the iron-based-carboxyl modified biochar into heavy metal contaminated soil, wherein the addition amount accounts for 1.0-2.0% of the heavy metal contaminated soil, and carrying out soil culture at a constant temperature of 25 ℃ for 30 days under the conditions that the water holding capacity is 60%.
Has the advantages that:
(1) the invention adopts natural biomass material which has huge specific surface area, abundant functional groups and developed micropore structure and adopts H2O2The modification can greatly increase oxygen-containing functional groups of the biochar, and metal oxides can be more easily loaded on the biochar in the red mud modification process, so that a large number of adsorption sites are added to the biochar, and the soil polluted by antimony and other heavy metal elements has a good repairing effect.
(2) The iron-based-carboxyl modified biochar can fully generate water to load the function of iron and aluminum oxides on the biochar, so that the migration capacity of heavy metals in soil is reduced, the local polluted soil remediation is achieved, the selection requirement of a passivator for an antimony smelting site is met, the material does not contain heavy metals, and the idea is provided for realizing resource utilization of biomass and red mud.
(3) The preparation process of the iron-based-carboxyl modified biochar is simple, the conditions are mild, a large amount of organic solvent is not needed, the environment is friendly, and the industrialization is easy to realize.
Drawings
FIG. 1 is SEM images of the vinegar residue biochar before and after modification according to an embodiment of the present invention;
fig. 2 is an XRD spectrum before and after the vinegar residue biochar is modified, which is provided by the embodiment of the present invention.
Detailed Description
In order to make the technical problems, technical solutions and advantages of the present invention more apparent, the following detailed description is given with reference to specific embodiments, but the scope of the present invention is not limited to the following specific embodiments.
Unless otherwise defined, all terms of art used hereinafter have the same meaning as commonly understood by one of ordinary skill in the art. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to limit the scope of the present invention.
Unless otherwise specifically stated, various raw materials, reagents, instruments, equipment and the like used in the present invention are commercially available or can be prepared by existing methods.
Example 1
S1: grinding birch into small pieces, cleaning, oven drying, placing into a stainless steel container, placing the container in a muffle furnace under nitrogen atmosphere, heating at 300 deg.C for pyrolysis, carbonizing for 4 hr, cooling, and taking out biochar obtained by carbonizing birch, wherein the biochar is acidic biochar.
S2: adding the biochar into 30% of H according to the solid-to-liquid ratio of 1:102O2Modifying the solution, then placing the solution into a magnetic stirrer for stirring at 40 ℃ for 12 hours, then carrying out solid-liquid separation, washing the biochar with deionized water, and drying the biochar at 60 ℃ to constant weight to obtain the modified biochar.
S3: mixing high-iron red mud and sulfuric acid solution in a solid-to-liquid ratio of 1:1, stirring for reaction, filtering to obtain filtrate, and obtaining iron-based impregnation liquid with reduced alkalinity and containing metal ions, wherein the high-iron red mud mainly contains metal oxides of iron and aluminum, the content of the metal oxides is 30.6% and 16.8%, and the metal ions in the obtained impregnation liquid are Fe3+And Al3+Mainly, richThe degrees are 1.3mol/L and 0.4mol/L respectively. The concentration of the sulfuric acid solution is 1mol/L, and the pH value of the obtained impregnation liquid is 6.7.
S4: mixing the modified biochar in a ratio of 1 g: adding 20ml of the solution into an iron-based impregnation solution, performing ultrasonic impregnation for 60min, filtering to obtain filter residue, cleaning, and drying at the temperature of 60 ℃ for 18h to obtain the iron-based-carboxyl modified biochar composite material.
Example 2
S1: grinding birch into small pieces, cleaning, oven drying, placing into a stainless steel container, placing the container in a muffle furnace under nitrogen atmosphere, heating at 375 deg.C for pyrolysis, carbonizing for 4 hr, cooling, and taking out biochar obtained by carbonizing birch, wherein the biochar is acidic biochar.
S2: adding the biochar into 30% of H according to the solid-liquid ratio of 1:152O2Modifying the solution, then placing the solution into a magnetic stirrer for stirring at the temperature of 50 ℃ for 10 hours, then carrying out solid-liquid separation, washing the biochar with deionized water, and drying the biochar at the temperature of 60 ℃ to constant weight to obtain the modified biochar.
S3: mixing high-iron red mud and sulfuric acid solution in a solid-to-liquid ratio of 1:1.5, stirring for reaction, filtering to obtain filtrate, and obtaining iron-based impregnation liquid with reduced alkalinity and containing metal ions, wherein the high-iron red mud mainly contains metal oxides of iron and aluminum, the content of the metal oxides is 35.6% and 20.8%, and the metal ions in the obtained impregnation liquid are Fe3+And Al3+Mainly, the concentration is 1.3mol/L and 0.4mol/L respectively. The concentration of the sulfuric acid solution is 2mol/L, and the pH value of the obtained impregnation liquid is 5.4.
S4: mixing the modified biochar in a ratio of 1 g: adding 30ml of the solution into an iron-based impregnation solution, carrying out ultrasonic impregnation for 60min, filtering to obtain filter residue, cleaning, and drying at the temperature of 60 ℃ for 18h to obtain the iron-based-carboxyl modified biochar composite material.
Example 3
S1: washing folium Pini, oven drying at 60 deg.C for 3 days, grinding, sieving with 1mm sieve, placing into stainless steel container, placing the container in muffle furnace under nitrogen atmosphere, pyrolyzing at 300 deg.C at a heating rate of 7 min/deg.C, carbonizing for 4 hr, cooling, and taking out the charcoal obtained by carbonizing folium Pini.
S2: adding the biochar into 30% of H according to the solid-liquid ratio of 1:202O2Modifying the solution, then placing the solution into a magnetic stirrer for stirring at the temperature of 60 ℃ for 8 hours, then carrying out solid-liquid separation, washing the biochar with deionized water, and drying the biochar at the temperature of 60 ℃ to constant weight to obtain the modified biochar.
S3: mixing high-iron red mud and sulfuric acid solution in a solid-to-liquid ratio of 1:2, stirring for reaction, filtering to obtain filtrate, and obtaining iron-based impregnation liquid with reduced alkalinity and containing metal ions, wherein the high-iron red mud mainly contains metal oxides of iron and aluminum, the content of the metal oxides is 31.6% and 18.8%, and the metal ions in the obtained impregnation liquid are Fe3+And Al3+Mainly, the concentration is 1.3mol/L and 0.4mol/L respectively. The concentration of the sulfuric acid solution is 3mol/L, and the pH value of the obtained impregnation liquid is 4.8.
S4: mixing the modified biochar in a ratio of 1 g: adding 40ml of the solution into an iron-based impregnation solution, carrying out ultrasonic impregnation for 60min, filtering to obtain filter residues, cleaning, and drying at the temperature of 60 ℃ for 18h to obtain the iron-based-carboxyl modified biochar composite material.
Example 4
S1: cleaning vinegar residue, drying at 60 deg.C for 3 days, grinding, sieving with 1mm sieve, placing into stainless steel container, placing the container in muffle furnace under nitrogen atmosphere, pyrolyzing at 250 deg.C at a heating rate of 7 min/deg.C, carbonizing for 2 hr, cooling, and taking out biochar obtained by carbonizing vinegar residue.
S2: adding the biochar into 30% of H according to the solid-liquid ratio of 1:202O2Modifying the solution, then placing the solution into a magnetic stirrer for stirring at the temperature of 60 ℃ for 8 hours, then carrying out solid-liquid separation, washing the biochar with deionized water, and drying the biochar at the temperature of 60 ℃ to constant weight to obtain the modified biochar.
S3: mixing the high-iron red mud and a sulfuric acid solution in a solid-to-liquid ratio of 1:2, stirring for reaction, filtering to obtain a filtrate, and obtaining an iron-based impregnation liquid containing metal ions with reduced alkalinity, wherein the iron-based impregnation liquid contains metal ionsThe content of the high-iron red mud is 31.6 percent and 18.8 percent respectively, the content of the metal oxides of iron and aluminum is the main content, and the metal ions in the obtained impregnation liquid are Fe3+And Al3+Mainly, the concentration is 1.3mol/L and 0.4mol/L respectively. The concentration of the sulfuric acid solution is 3mol/L, and the pH value of the obtained impregnation liquid is 4.8.
S4: mixing the modified biochar in a ratio of 1 g: adding 40ml of the solution into an iron-based impregnation solution, carrying out ultrasonic impregnation for 60min, filtering to obtain filter residues, cleaning, and drying at the temperature of 60 ℃ for 18h to obtain the iron-based-carboxyl modified biochar composite material.
Structural characterization
SEM scanning analysis and XRD analysis are carried out on the obtained biochar and the modified iron-based-carboxyl modified biochar composite material, and materials before and after the modification of the vinegar residue are taken as examples and are shown in the attached drawings 1 and 2 in detail.
As can be seen from SEM atlas, the attached drawings 1(a) and (b) are respectively the vinegar residue biochar before and after modification, the modified vinegar residue biochar obtained in the attached drawing 1(b) is coarser than the unmodified vinegar residue biochar in the attached drawing 1(a), the surface pores and folds are more, and a plurality of fine granular objects are formed, so that the specific surface area of the biochar is greatly increased, and analysis is probably due to H2O2The porous structure formed by oxidation is beneficial to the adsorption of heavy metal ions.
The attached figures 2(a) and (b) are respectively the vinegar residue biochar before and after modification, and the composition of the phase in the atlas before and after modification of the vinegar residue biochar is analyzed by XRD. As can be seen from the figure, the mineral composition of the unmodified vinegar residue biochar and the modified vinegar residue biochar is obviously different. Compared with the unmodified vinegar residue biochar, the modified vinegar residue biochar has more phases containing oxygen functional groups and more peaks containing iron-based phases, so that the surface biochar is further successfully modified.
Application example
The iron-based carboxyl modified biochar composite prepared in the embodiment 1 is used for passivating heavy metal contaminated soil, and specifically comprises the following steps:
the soil to be tested is collected from a Hunan cold water JiangSb smelting field, a soil sample at the position of 0-20cm is collected, and the soil sample is dried in the air and then is filtered through a 2mm sieve to be repeatedly and uniformly mixed for later use.
Adopting a soil culture experiment, taking 1kg of soil sample to be tested, firstly determining the physical and chemical properties of the soil, wherein the physical and chemical properties comprise pH, total Sb, total As and total Pb, and the pH of the soil is 1: 5, measuring the aqueous suspension by using a pH meter; after the content of each heavy metal in the soil is measured by a soil leaching experiment (the specific steps are operated according to HJ/T300-2007 standard), the ICP method is used for measuring, and the measured basic physicochemical properties of the soil to be tested are shown in Table 1.
TABLE 1 basic physicochemical Properties of the soil tested
1kg of soil to be tested is taken and put into a basin, the water holding capacity of the soil is kept at about 60 percent by spraying deionized water, then biochar with different addition amounts is applied into the experimental basin, 4 groups of experimental groups are arranged, wherein 1.0 percent and 2.0 percent of unmodified biochar BC and 1.0 percent of iron-based-carboxyl modified biochar composite material BC-G and 2.0 percent are respectively added; and no biochar material was added as a control experiment.
The soil after the experimental pots are respectively cultured for 30 days is subjected to leaching experiment, the content of each effective heavy metal in each group of experiments is measured by an ICP method, and the passivation effect is shown in Table 2.
TABLE 2 passivation conditions and passivation effects of heavy metal ions in antimony smelting site soil
From the experimental results, the metal-based biochar composite material (example 1) prepared by the invention is applied to the soil of an antimony smelting site, compared with the control, the effective state contents of Sb in the soil treated by 1.0% of BC, 2.0% of BC, 1.0% of BC-G and 2.0% of BC-G are respectively reduced by 20%, 32.7%, 47% and 58.5%, the effective state contents of As are respectively reduced by 21%, 41.2%, 44.7% and 63%, the effective state contents of Pb are respectively reduced by 10%, 31%, 37.8% and 67.6%, and the contents of various metal ions in the effective state of the soil of the antimony smelting site treated by the metal-based biochar composite material are obviously reduced, and the passivation effect is better than that of unmodified biochar.
The above-mentioned embodiments are only preferred embodiments of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered as the technical scope of the present invention, and equivalents and modifications of the technical solutions and concepts of the present invention should be covered by the scope of the present invention.
Claims (10)
1. The preparation method of the iron-based carboxyl modified biochar is characterized by specifically comprising the following steps of:
s1: pretreating a biomass raw material and then pyrolyzing to obtain biochar; the biomass raw material is one or more of birch, hickory shell, pine needle and vinegar residue;
s2: mixing the biochar with a hydrogen peroxide solution in a solid-to-liquid ratio of 1:10-20, stirring for reaction, filtering to obtain filter residue, and drying to obtain modified biochar;
s3: mixing the high-iron red mud and a sulfuric acid solution in a solid-to-liquid ratio of 1-3:1-2, reacting, centrifuging and filtering to obtain a filtrate, and obtaining an iron-based impregnation solution;
s4: and adding the modified biochar into the iron-based impregnation liquid for ultrasonic impregnation, filtering to obtain filter residues, and cleaning and drying to obtain the iron-based-carboxyl modified biochar composite material.
2. The method for preparing the iron-based-carboxyl modified biochar according to claim 1, wherein the step of pretreating the biomass raw material and then pyrolyzing the pretreated biomass raw material to obtain the biochar specifically comprises the following steps:
crushing, cleaning and drying a biomass raw material to obtain a dry biomass raw material;
and (2) putting the dried biomass raw material into an inert atmosphere for pyrolysis for 2-4h, wherein the pyrolysis temperature is 200-600 ℃, introducing inert gas after pyrolysis is finished, cooling to room temperature, cleaning, and drying at 60 ℃ for 12-24h to obtain the biochar.
3. The method for preparing iron-based-carboxyl modified biochar according to claim 1, wherein the specific process parameters in the step S2 are as follows:
the concentration of the hydrogen peroxide solution is 25-35%;
the temperature of the stirring reaction is 40-60 ℃, and the reaction time is 6-12 h.
4. The method for preparing the iron-based carboxyl modified biochar according to claim 1, wherein the contents of iron and aluminum oxides in the high-iron red mud are respectively 30-50% and 15-25%, and the concentration of the sulfuric acid solution is 1-3 mol/L.
5. The method for preparing the iron-based-carboxyl modified biochar according to claim 1, wherein the solid-to-liquid ratio of the modified biochar to the iron-based impregnating solution is 1:20-60, and the ultrasonic impregnation time is 40-60 min.
6. The method for preparing iron-based-carboxyl modified biochar according to claim 1, wherein deionized water is used in the cleaning process in the step S4, the temperature of the drying process is 60 ℃, and the drying time is 12-24 h.
7. An iron-based carboxyl-modified biocarbon produced by the production method according to any one of claims 1 to 6.
8. The application of the iron-based carboxyl modified biochar obtained by the preparation method of any one of claims 1-6 in remediation of heavy metal contaminated soil.
9. The use according to claim 8, wherein the heavy metal contamination comprises antimony, arsenic or lead contamination alone or in combination with antimony, arsenic or lead.
10. The use according to claims 8-9, characterized in that the application method comprises in particular the steps of:
adding the iron-based-carboxyl modified biochar into heavy metal contaminated soil, wherein the addition amount accounts for 1.0-2.0% of the heavy metal contaminated soil, and carrying out soil culture at a constant temperature of 25 ℃ for 30 days under the conditions that the water holding capacity is 60%.
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