CN113856621B - Preparation and application of Fe-S co-doped biochar material for simultaneously removing Pb-As composite pollution - Google Patents
Preparation and application of Fe-S co-doped biochar material for simultaneously removing Pb-As composite pollution Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title abstract description 14
- MBMLMWLHJBBADN-UHFFFAOYSA-N Ferrous sulfide Chemical compound [Fe]=S MBMLMWLHJBBADN-UHFFFAOYSA-N 0.000 claims abstract description 37
- 102000005298 Iron-Sulfur Proteins Human genes 0.000 claims abstract description 35
- 108010081409 Iron-Sulfur Proteins Proteins 0.000 claims abstract description 35
- 229910052785 arsenic Inorganic materials 0.000 claims abstract description 26
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- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims abstract description 13
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- HUEBVZADHUOMHL-UHFFFAOYSA-N [As].[Pb] Chemical compound [As].[Pb] HUEBVZADHUOMHL-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000001354 calcination Methods 0.000 claims abstract description 6
- 239000007788 liquid Substances 0.000 claims abstract description 5
- 238000004108 freeze drying Methods 0.000 claims abstract description 4
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- 238000006243 chemical reaction Methods 0.000 claims description 5
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- 230000001681 protective effect Effects 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
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- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- 230000010355 oscillation Effects 0.000 claims description 2
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- 230000000630 rising effect Effects 0.000 claims 1
- 238000007873 sieving Methods 0.000 claims 1
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 abstract description 22
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- 238000005470 impregnation Methods 0.000 abstract 1
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- 238000000034 method Methods 0.000 description 12
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- 238000001179 sorption measurement Methods 0.000 description 8
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- 229910052717 sulfur Inorganic materials 0.000 description 5
- 239000011593 sulfur Substances 0.000 description 5
- 239000002351 wastewater Substances 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 4
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- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
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- 229910052793 cadmium Inorganic materials 0.000 description 1
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
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- -1 electrochemistry Substances 0.000 description 1
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- 229910052753 mercury Inorganic materials 0.000 description 1
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- 229910052979 sodium sulfide Inorganic materials 0.000 description 1
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical compound [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 description 1
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Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
-
- 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
-
- 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
- C02F2101/103—Arsenic compounds
-
- 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
Abstract
The invention relates to preparation and application of an iron-sulfur co-doped biochar material for simultaneously removing arsenic-lead composite pollution. The iron-sulfur co-doped biochar material is prepared by fully mixing straw powder and suspension containing ferrous sulfate and sodium thiosulfate in a solid-to-liquid ratio of (7-12) g to 100mL through magnetic stirring for 10-36 hours, and pyrolyzing at 250-450 ℃ for 1-3 hours after freeze drying. The molar ratio of ferrous sulfate to sodium thiosulfate in the suspension is (0.7-2): 1. the iron-sulfur co-doped biochar can efficiently adsorb arsenic and lead in a composite polluted water body, the optimal removal rate of As (III) in 24 hours is more than 96%, and the removal rate of Pb (II) is more than 93%; and the removal rate of As (III) and Pb (II) can be kept above 90% under the condition of pH of 3-6. The iron-sulfur co-doped biochar is obtained by primary calcination after raw material impregnation, is simple to operate, has remarkable arsenic-lead removal effect, and has practical significance for treating industrial wastewater polluted by arsenic-lead.
Description
Technical Field
The invention belongs to the technical field of heavy metal treatment, and relates to preparation and application of a modified biochar material for simultaneously removing lead and arsenic combined pollution.
Background
Lead and arsenic are widely present in nature as the second "five toxic elements" (cadmium, mercury, arsenic, lead, chromium), and their impact on environmental and human health safety is of great concern. The arsenic-lead composite pollution in the water body is mainly generated in the industrial processes of smelting, mining, electroplating and the like. Trivalent arsenic As (III) in water has higher toxicity, mobility and solubility. Lead is usually present in the wastewater in the form of Pb (II). The arsenic-lead composite pollution is not easy to be degraded chemically or biologically, can be enriched in human body through ingestion, and has great harm to organs such as stomach, intestinal tract, liver, kidney and the like of human body. In order to mitigate the effect of co-contamination of arsenic and lead on human health, world Health Organization (WHO) established an international maximum level of contamination of arsenic in drinking water of 10 ppb and lead of 10 ppb. Therefore, it is important to repair arsenic and lead contamination in aqueous solutions.
At present, a plurality of purification technologies such As chemical precipitation, electrochemical treatment, membrane separation, ion exchange, adsorption and the like are adopted to treat As (III) and Pb (II) in wastewater. Compared with chemical precipitation method, the method has the limitations of high cost and the like, such as a large amount of sludge, electrochemistry, membrane separation and the like, and adsorption is considered as one of the most promising technologies because of the special advantages of simple operation, high cost efficiency, no sludge treatment and the like.
The biochar prepared from agricultural wastes such as straw has the advantages of developed pore structure, stable fat chain structure, wide sources and the like, and has been widely used as an economic adsorbent. Compared with unmodified biochar, the iron-based and sulfur-based modified biochar has better adsorption capacity for As (III) and Pb (II). Studies have now demonstrated the feasibility of biochar co-supported iron and sulfur: (1) The Chinese patent application (publication number CN 111229160A) proposes a preparation method of biochar for simultaneously immobilizing ferrous sulfide and zero-valent iron, namely, the calcined corn stalk biochar is prepared by continuously stirring the calcined corn stalk biochar with ferrous sulfate and sodium sulfide in anaerobic conditions after hydrophilic treatment, so that the material has good adsorption performance on lead in wastewater. However, the method only considers the removal of lead by the material, and the complex pollution of various heavy metals usually exists in the actual wastewater, so the application range is quite limited. (2) The Chinese patent application (publication number CN 111925806A) proposes a preparation method of a sulfur-doped nano ferroferric oxide/biochar composite material, which combines the loading of ferroferric oxide and the modification of sulfur, so that the material has high-efficiency adsorption performance on arsenic and lead, but the preparation process needs multiple high-temperature calcination and the modification process of sulfur needs continuous stirring in an anaerobic environment, so that the preparation method is complex in procedure, high in cost and strict in preparation condition requirement, and is unfavorable for mass production in practical application.
Disclosure of Invention
As the most of iron-sulfur co-doped materials at present, the problems of easy oxidation, agglomeration and the like exist in the zero-valent iron sulfide, the nano-iron sulfide and the like, nitrogen is introduced and calcined for many times in the preparation process, the generated materials are extremely easy to oxidize and need anaerobic storage, the preparation conditions are harsh, the cost is high, and only removal of single heavy metal is generally considered. In order to overcome the problems, the invention provides a preparation method and an application method of the Fe-S co-doped biochar, wherein the Fe-based functional groups and the S-based functional groups are simultaneously loaded on the biochar through one-time calcination, and the Fe-S co-doped biochar can simultaneously and efficiently remove the As-Pb pollution. Through repeated experimental researches, the invention creatively utilizes ferrous sulfate and sodium thiosulfate to react with biomass in the soaking process, so that iron oxide and iron sulfide can be loaded on biochar through calcination, and the final product is stable and easy to store and has the capability of efficiently removing arsenic and lead.
The invention provides a preparation method of a modified biochar material for simultaneously removing lead and arsenic combined pollution, which comprises the following steps: the modified biochar material is iron-sulfur co-doped biochar formed by pyrolysis of ferrous sulfate and sodium thiosulfate and biomass. And fully mixing straw powder, ferrous sulfate and suspension of sodium thiosulfate through magnetic stirring, then freeze-drying, calcining at 250-450 ℃ in a protective atmosphere, and maintaining the temperature for 1-3 hours to obtain a pyrolysis product, namely the iron-sulfur co-doped biochar.
In one embodiment, the selected straw is rice straw.
In a specific embodiment, the solid-to-liquid ratio of the rice straw powder to the suspension is 5-15 g/100 mL, preferably 7-12 g/100 mL.
In a specific embodiment, the molar ratio of ferrous sulfate to sodium thiosulfate in the suspension is controlled to be 0.5-2.5: 1, preferably 0.7 to 2:1.
preferably, the suspension is stirred by magnetic force for 10-36 hours and then freeze-dried.
Preferably, the heating rate is controlled to be 5-10 ℃/min during pyrolysis.
Preferably, the pyrolysis is carried out at the temperature of 250-450 ℃ and the temperature is kept for 1-3 hours.
Preferably, the pyrolysis product is dried after washing impurities with deionized water.
The invention also provides application of the iron-sulfur co-doped biochar material in an arsenic-lead composite polluted water body. Further, adding 1-3 g/L of the modified biochar into the wastewater polluted by the combination of As (III) and Pb (II) for oscillation reaction, performing adsorption treatment, and taking the solutions before and after the reaction to measure the concentrations of As (III) and Pb (II).
Preferably, the material is applied to a composite solution of As (III) and Pb (II), and the initial pH value of the material is adjusted to be 2-7, preferably 3-6.
Compared with the prior art, the invention has the following advantages: the invention can obtain the Fe-S co-doped biochar by fully soaking and mixing the straw powder and the suspension mixed by the ferrous sulfate and the sodium thiosulfate and then calcining for one time, has simple operation and lower cost, and is beneficial to large-scale production and practical application. The prepared iron-sulfur co-doped biochar can simultaneously and efficiently remove As (III) and Pb (II) in a water body, and has better anti-interference capability on pH. Experiments prove that: the optimal removal rate of the material to As (III) within 24 hours is more than 96%, and the removal rate to Pb (II) is more than 93%; and the removal rate of the iron-sulfur co-doped biochar to As (III) Pb (II) is maintained above 90% within the pH range of 3-6.
Drawings
FIG. 1 is an XPS picture of the material of example 1
FIG. 2 shows the effect of different initial pH values on adsorption of As (III) and Pb (II) in example 2.
Detailed Description
The following further illustrates the invention in connection with specific examples, but is not to be construed as limiting the invention. The technical means used in the examples are conventional means well known to those skilled in the art unless otherwise indicated. Unless specifically stated otherwise, the reagents, methods and apparatus employed in the present invention are those conventional in the art.
Example 1
Preparing the iron-sulfur co-doped biochar: 10g of rice straw powder is taken and added into 100mL of rice straw powder with the molar ratio of 1:1 and sodium thiosulfate, magnetically stirring for 10 hr, and freeze drying. And (3) placing the dried solid in a nitrogen atmosphere, pyrolyzing at 300 ℃ for 2 hours at a heating rate of 5 ℃/min, cooling, and flushing with deionized water for three times to obtain the Fe-S-BC. Comparison was performed using unmodified biochar.
Preparation of unmodified biochar: and (3) putting the rice straw powder into a nitrogen atmosphere, pyrolyzing at 300 ℃ for 2 hours at a heating rate of 5 ℃/min, cooling, and flushing with deionized water for three times to obtain the unmodified Biochar (BC).
The BET test results are shown in Table 1, and the XPS results are shown in FIG. 1.
TABLE 1 BET test results of iron-sulfur Co-doped biochar and unmodified biochar
| Absorbent | Specific surface area (m) 2 /g) | Pore volume (cm) 2 /g) | Aperture (nm) |
| BC | 20.18 | 0.013 | 21.31 |
| Fe/S-BC | 121.90 | 0.058 | 17.85 |
As can be seen from table 1 and fig. 1, the iron-sulfur co-doped biochar has a larger specific surface area and pore volume by immobilizing iron and sulfur, and the iron-sulfur compound loaded on the biochar can further promote the removal of As and Pb.
Arsenic and lead removal experiment:
1. comparison of removal rates of different addition amounts of iron-sulfur co-doped biochar
The prepared iron-sulfur co-doped biochar is applied to a composite solution of As (III) and Pb (II) with initial concentration of 50mg/L, the initial pH value of the solution is adjusted to 5, the iron-sulfur co-doped biochar is added according to 1g/L, 2g/L and 3g/L, the solution is horizontally oscillated in a constant temperature water bath oscillator at 25 ℃ for 24 hours, the concentration of arsenic and lead in the treated solution is measured according to the method described in documents such As GB 7475-87, HJ 694-2014 and the like, the result is recorded, and the removal rate is calculated. The results are shown in Table 2,
TABLE 2 influence of different concentration addition amounts on As (III) and Pb (II) removal rates in composite solutions
| Biochar addition amount (g/L) | As (III) content after treatment (ppm) | As (III) removal rate (%) | Pb (II) content (ppm) after treatment | Pb (II) removal Rate (%) |
| 1 | 2.145 | 95.71 | 3.265 | 93.47 |
| 2 | 1.610 | 96.78 | 0.730 | 98.54 |
| 3 | 0.810 | 98.38 | 0.655 | 98.69 |
The results show that: the removal rate of the prepared biochar material to As (III) and Pb (II) is kept above 90%, and the removal rate is increased along with the increase of the addition amount. But the removal rate of arsenic and lead is higher by adding 1g/L of the Fe-S co-doped biochar, which respectively reaches 95.71 percent and 93.47 percent.
2. Comparison of removal Rate at different initial pH conditions
Meanwhile, the composite solution of As (III) and Pb (II) is subjected to adsorption experiments by adjusting the initial pH to 3,4,5 and 6 respectively and adding iron-sulfur co-doped biochar according to 1 g/L. After the end of the experiment, the results were measured. The results are shown in FIG. 1.
The prepared iron-sulfur co-doped biochar has the advantages that the removal rate of arsenic and lead reaches over 90% under different pH values, so that the iron-sulfur co-doped biochar has good anti-interference capability and application range on pH.
Example 2
Preparing the iron-sulfur co-doped biochar:
reference is made to example 1, which differs in that: the solid-liquid ratio of the rice straw powder to the suspension is 7g:100mL, the protective atmosphere is argon, and the heating rate is 10 ℃/min.
Arsenic and lead removal experiment: the procedure of example 1 was followed, wherein the pH of the composite solution of iron-sulfur co-doped biochar 1g/L, as (III) and Pb (II) was 5. After the end of the experiment, the percentage of arsenic and lead removed was determined. The results show that: the removal rate of As (III) is 93.66 percent, the removal rate of Pb (II) is 91.93 percent,
example 3
Preparing the iron-sulfur co-doped biochar: reference is made to example 1, which differs in that: the molar ratio of ferrous sulfate to sodium thiosulfate in the suspension is 2:1, the pyrolysis time is 3h, the rest is the same as in example 1.
Arsenic and lead removal experiment: the procedure of example 1 was followed, wherein the pH of the composite solution of iron-sulfur co-doped biochar 1g/L, as (III) and Pb (II) was 5. After the end of the experiment, the percentage of arsenic and lead removed was determined. The results show that: the removal rate of As (III) at the reaction equilibrium was 94.21%, and the removal rate of Pb (II) was 95.68%.
Example 4
Preparing the iron-sulfur co-doped biochar: reference is made to example 1, which differs in that: the pyrolysis temperature was 350 ℃, the pyrolysis time was 3 hours, and the rest was the same as in example 1.
Arsenic and lead removal experiment: the procedure of example 1 was followed, wherein the pH of the composite solution of iron-sulfur co-doped biochar 1g/L, as (III) and Pb (II) was 5. After the end of the experiment, the percentage of arsenic and lead removed was determined. The results show that: the removal rate of As (III) at the reaction equilibrium was 96.95%, and the removal rate of Pb (II) was 91.27%.
Based on the embodiment, the iron-sulfur co-doped biochar can simultaneously and efficiently remove arsenic and lead in water, wherein the iron-sulfur co-doped biochar material is added into an arsenic-lead composite solution according to 1g/L, and a higher removal rate can be achieved. The initial pH value of the arsenic-lead composite solution is within the range of 3-6, the pH value of the solution is regulated, and the removal rate of the prepared iron-sulfur co-doped biochar on As (III) and Pb (II) is maintained to be more than 90%. The solid-liquid ratio of the straw powder to the suspension is within the range of 5-15 g:100mL, and the removal rate of the iron-sulfur co-doped biochar prepared by adjusting the dosage of the rice straw powder and the suspension to As (III) and Pb (II) is kept above 90%. The molar ratio of ferrous sulfate to sodium thiosulfate in the suspension is 0.5-2.5: in the range of 1, the removal rate of the iron-sulfur co-doped biochar prepared by adjusting the dosage of ferrous sulfate and sodium thiosulfate to As (III) and Pb (II) is kept above 90 percent.
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 (4)
1. The application of the Fe-S co-doped biochar material for simultaneously removing the Pb-As composite pollution is characterized by comprising the following steps of:
(1) Adding straw powder into a suspension containing ferrous sulfate and sodium thiosulfate, wherein the solid-to-liquid ratio of the straw powder to the suspension is 7-12 g/100 mL; the molar ratio of ferrous sulfate to sodium thiosulfate in the suspension is 0.7-2: 1, a step of;
(2) Stirring the solution obtained in the step (1) by magnetic force for 10-36 hours, fully mixing and then freeze-drying;
(3) Placing the dried mixture in a protective atmosphere, calcining for 1-3 hours at the temperature rising rate of 5-10 ℃/min to 250-450 ℃ to obtain a carbonized product, and washing and drying to obtain the Fe-S co-doped biochar material; adding the obtained iron-sulfur co-doped biochar material into an arsenic-lead composite polluted water body according to the ratio of 1-3 g/L, adjusting the initial pH value of the arsenic-lead composite polluted water body to 2-7, and carrying out oscillation reaction.
2. The use of the iron-sulfur co-doped biochar material for simultaneously removing lead-arsenic composite pollution according to claim 1, wherein the use is characterized in that: the straw powder is obtained by cleaning, drying, crushing and sieving rice straw.
3. The use of the iron-sulfur co-doped biochar material for simultaneously removing lead-arsenic composite pollution according to claim 1, wherein the use is characterized in that: the protective atmosphere is nitrogen or argon.
4. The use of the iron-sulfur co-doped biochar material for simultaneously removing lead-arsenic composite pollution according to claim 1, wherein the use is characterized in that: and adjusting the initial pH value of the arsenic-lead composite polluted water body to 3-6.
Priority Applications (1)
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| CN109777425A (en) * | 2019-01-22 | 2019-05-21 | 袁艺宁 | A kind of preparation method and applications of phosphorus ferric sulfate polymer |
| CN111925806A (en) * | 2020-07-20 | 2020-11-13 | 华东理工大学 | Sulfur-doped nano ferroferric oxide/biochar composite material as well as preparation method and application thereof |
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| CN106268720A (en) * | 2016-09-09 | 2017-01-04 | 安徽工业大学 | A kind of preparation method of the biological carbon composite adsorbing material removing surface water body molybdate |
| CN109777425A (en) * | 2019-01-22 | 2019-05-21 | 袁艺宁 | A kind of preparation method and applications of phosphorus ferric sulfate polymer |
| CN111925806A (en) * | 2020-07-20 | 2020-11-13 | 华东理工大学 | Sulfur-doped nano ferroferric oxide/biochar composite material as well as preparation method and application thereof |
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