CN112850836A - Preparation and application of chitosan stabilized ferrous sulfide composite charcoal material - Google Patents
Preparation and application of chitosan stabilized ferrous sulfide composite charcoal material Download PDFInfo
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- CN112850836A CN112850836A CN201911178224.0A CN201911178224A CN112850836A CN 112850836 A CN112850836 A CN 112850836A CN 201911178224 A CN201911178224 A CN 201911178224A CN 112850836 A CN112850836 A CN 112850836A
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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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Abstract
The invention relates to the field of environmental remediation, and particularly relates to preparation and application of a chitosan stabilized ferrous sulfide composite biochar material. According to the invention, highland barley crop straws in plateau areas are used as a biochar raw material, and chitosan is used as a stabilizer of ferrous sulfide, so that the stability of the ferrous sulfide is improved, the ferrous sulfide is more uniformly loaded on the biochar, and the treatment effect on hexavalent chromium is enhanced. The invention provides an efficient, green and environment-friendly repairing material, which not only overcomes the defect that nano ferrous sulfide is easy to agglomerate, but also realizes resource utilization, effectively improves the removal efficiency of pollutants, and does not cause secondary pollution.
Description
Technical Field
The invention relates to the field of environmental remediation, and particularly relates to preparation and application of a chitosan stabilized ferrous sulfide composite biochar material.
Background
Chromium is a common heavy metal in surface and ground water and is commonly derived from various industrial processes such as metallurgy, chromate manufacture, textile dyeing, tanning, wood preservation, metal plating, and the like. It may constitute a high risk to the ecosystem and public health due to its carcinogenicity, persistence and bioaccumulation. Generally, chromium exists in the natural environment in the form of trivalent chromium (Cr (iii)) and hexavalent chromium (Cr (vi)). Toxicity of Cr (III)Smaller, usually in the form of precipitates, i.e. Cr (OH)3And Cr2O3Compared with Cr (III), Cr (VI) is highly toxic, generally soluble, easily migratable and exists in the form of oxyanion (CrO)4 2-，HCrO4 -，Cr2O7 2-). In china, Cr (vi) is listed as the preferred hazardous contaminant. In view of the great harm of chromium pollution to the environment and human health, chromium pollution abatement has attracted public and governmental attention. Therefore, it is very important to develop practical active materials capable of adsorbing and reducing cr (vi) to cr (iii) to minimize the toxicity of cr (vi).
Iron-based materials are considered a promising option for removing Cr (vi) from contaminated wastewater because they are readily available and inexpensive. Iron sulfide (FeS) can effectively reduce Cr (vi) because it can provide fe (II) and S (-II), both of which are strong reducing species, promoting Cr (vi) reduction. Compared with FeS mineral, the FeS nano-particles have higher reduction effect on Cr (VI) due to small particle size and large specific surface area. However, FeS nanoparticles are easy to agglomerate, so that the reactive sites are reduced, the reduction efficiency of Cr (VI) is reduced, and certain use limitation of nano ferrous sulfide is caused.
Chitosan is a renewable, transformed polysaccharide derived from deacetylation of chitin, which is widely found in nature. Because of the advantages of a large amount of amino and hydroxyl, the chitosan has good affinity to Cr (VI), and chitosan has been used as a stabilizer to improve the stability of the nano zero-valent iron, thereby obviously improving the treatment effect of the nano zero-valent iron on organic matters and heavy metals in water.
Biochar is a carbonaceous material that is converted from biomass. The adsorbent is used as an adsorbent for removing organic and inorganic pollutants from the environment due to the characteristics of porosity, large specific surface area, abundant surface functional groups, high stability, extremely low solubility and the like. In recent years, it has been successfully used as a mechanical carrier for dispersing nanoparticles to facilitate its environmental application. Most of the biochar raw materials are crop straws, shells, vegetables, sawdust, sludge and the like. Currently, the most common method of producing biochar is thermal cracking, i.e., low temperature thermal decomposition of biomass material under oxygen limited or deficient conditions. The pyrolysis method has relatively good adaptability, but dioxin in the generated tail gas cannot reach the standard and is discharged, thereby causing great threat to the environment. The sulfuric acid carbonization is a method for dehydrating and carbonizing biomass at low temperature by utilizing the dehydration property and strong acidity of concentrated sulfuric acid to obtain biochar. The method has the advantages of low cost, simple operation, high efficiency and no secondary pollution.
According to the invention, ferrous sulfide is synthesized by ferrous sulfate heptahydrate and sodium sulfide nonahydrate, chitosan is used as a stabilizer of the ferrous sulfide, highland barley straws are used as a biochar raw material, the ferrous sulfide stabilized by the chitosan is loaded on the biochar, effective active sites of ferrous sulfide nanoparticles are increased, and the treatment efficiency of Cr (VI) is improved. The novel composite repairing material prepared by the invention has the concept of green sustainable repairing, realizes waste utilization, and improves the application limit of ferrous sulfide nano-particles in the field of environmental repairing.
Disclosure of Invention
The invention aims to improve the application limit of FeS nano particles in the field of environmental remediation, provides a green and environment-friendly preparation method, improves the stability of the FeS nano particles, and finally prepares a novel iron-based composite material which has large specific surface area, uniform load and good stability and can effectively remove Cr (VI).
In order to achieve the purpose, the invention is realized by the following technical scheme:
1) pulverizing cleaned and dried highland barley straw, and sieving with 40 mesh standard sieve.
2) Weighing 50mL of 98% concentrated sulfuric acid into a 250mL round-bottom flask, adding 50-80g of highland barley straw powder, adding a certain amount of asphalt, raising the temperature to 100-.
3) Weighing a certain amount of chitosan, adding into acetic acid solution, stirring well, dispersing in ultrasonic cleaning instrument for 15min,adding a certain amount of FeSO4·7H2And O, stirring the mixture on a magnetic stirrer for 30min, adding the prepared biochar, continuing stirring for 30min, slowly dropwise adding the sodium sulfide nonahydrate solution in the separating funnel into the reaction system, and continuously stirring for 1h after dropwise adding is completed to ensure that the reaction system fully reacts, wherein the nitrogen atmosphere is kept in the whole reaction process.
4) Washing with absolute ethyl alcohol, centrifuging, freezing at-4 ℃ for 12h, and drying with a freeze dryer for 24h to obtain the novel iron-based modified material.
Preferably, the biochar raw material in the step 1) is highland barley crop straws in a plateau area.
Preferably, the weight of the added highland barley straw powder in the step 2) is 65g, which is 70% of the weight of the sulfuric acid.
Preferably, the mass of the added asphalt in the step 2) is 1.3g, which is 2% of the mass of the highland barley straw powder.
Preferably, the heating temperature in the step 2) is 200 ℃, and the temperature is kept for 2 hours.
Preferably, the vacuum drying temperature in step 2) is 150 ℃.
Preferably, the volume fraction of the acetic acid solution in the step 3) is 2%.
Preferably, the volume ratio of the chitosan to the acetic acid solution in the step 3) is 1g:50 mL.
Preferably, the optimal mass ratio of the ferrous sulfide, the chitosan and the biochar in the step 3) is 2:2: 1.
Preferably, the freezing temperature of the freeze drying process in the step 4) is-50 ℃, and the pressure is 15 Pa.
The technical progress achieved by the invention is as follows:
the preparation of the biochar adopts a concentrated acid carbonization method, has low cost, simple operation and high yield, and does not cause secondary pollution to the environment.
The chitosan is used as a stabilizer, is a natural polysaccharide substance, has good stability, is biodegradable and nontoxic, and cannot pollute the environment.
Drawings
FIG. 1 is a comparison graph of 4 materials of biochar, FeS-chitosan and FeS-chitosan-biochar for removing Cr (VI).
FIG. 2 is a graph showing Cr (VI) removal rate-reaction time of FeS-chitosan-biochar.
FIG. 3 is a Cr (VI) removal rate-pH curve of FeS-chitosan-biochar.
Detailed Description
Example 1: preparation of materials
1) Preparing biochar: pulverizing cleaned and dried highland barley straw, and sieving with 40 mesh standard sieve. Weighing 50mL of 98% concentrated sulfuric acid into a 250mL round-bottom flask, adding 65g of highland barley straw powder, adding 1.3g of asphalt, raising the temperature to 200 ℃, maintaining for 2h, cooling to room temperature, adding deionized water, stirring for 15min, filtering, repeatedly washing and filtering until the pH value of filter residue is 7, putting the filter residue into a vacuum drying oven, setting the temperature to 150 ℃, drying for 16h, and passing through a standard sieve mesh of 100 meshes to obtain the biochar.
2) Preparing FeS: weighing 3.1591gFeSO4·7H2Dissolving O in 50mL deionized water, stirring for 30min on a magnetic stirrer, and weighing 2.7273gNa2S·9H2Dissolving O in 30mL of deionized water, performing ultrasonic treatment for 15min by using an ultrasonic cleaner, completely dissolving the O, transferring the O into a separating funnel, slowly dropwise adding the O into a ferrous sulfate solution, stirring for 1h after dropwise adding is completed, keeping the nitrogen atmosphere in the whole preparation process, washing with absolute ethyl alcohol, centrifuging, freezing for 12h at-4 ℃, and drying for 24h by using a freeze dryer to obtain the FeS.
3) Preparing FeS-chitosan: weighing 1g of chitosan, dissolving in 50mL of 2% acetic acid, stirring uniformly, ultrasonically dispersing in an ultrasonic cleaner for 15min, adding 3.1591g of FeSO4·7H2O, magnetically stirring the mixture for 30min to obtain Fe2+Chitosan mixture, weighing 2.7273gNa2S·9H2Dissolving O in 30mL deionized water, ultrasonically treating for 15min with ultrasonic cleaner, transferring into separating funnel, slowly dropwise adding into the above reaction system, stirring for 1h after dropwise adding is completed, maintaining nitrogen atmosphere in the whole preparation process, washing with anhydrous ethanol, centrifuging, freezing at-4 deg.C for 12h, and cooling with waterDrying for 24h by a freeze dryer to obtain the FeS-chitosan.
4) Preparing FeS-chitosan-biochar: weighing 1g of chitosan, dissolving in 50mL of 2% acetic acid, stirring uniformly, ultrasonically dispersing for 15min in an ultrasonic cleaner, adding 3.1591g of FeSO4·7H2O, magnetically stirring the mixture for 30min, adding 1g of spare biochar, continuously stirring for 30min, and weighing 2.7273gNa2S·9H2Dissolving O in 30mL of deionized water, performing ultrasonic treatment for 15 minutes by using an ultrasonic cleaner, completely dissolving the O, transferring the O into a separating funnel, slowly dropwise adding the O into the reaction system, stirring for 1h after dropwise adding is completed, keeping the nitrogen atmosphere in the whole preparation process, washing by using absolute ethyl alcohol, centrifuging, freezing for 12h at-4 ℃, and drying for 24h by using a freeze dryer to obtain the FeS-chitosan-biochar.
Example 2: comparison experiment of Cr (VI) removing effect of different materials
Respectively weighing 0.1g of biochar, FeS-chitosan and FeS-chitosan-biochar, respectively adding the biochar, FeS-chitosan and FeS-chitosan-biochar into 50mL of simulated wastewater with the initial chromium concentration of 100mg/L, sealing the wastewater, putting the wastewater into a constant-temperature 25 ℃ water bath oscillator, reacting for 24 hours, sampling and analyzing, and setting parallel tests in experiments. The calculated removal rate pairs are analyzed as shown in fig. 1.
Example 3: experiment of Cr (VI) removal rate of FeS-chitosan-biochar along with time change
Weighing 0.1g of FeS-chitosan-biochar, adding the FeS-chitosan-biochar into 50mL of simulated wastewater with the initial chromium concentration of 100mg/L, sealing the wastewater, putting the wastewater into a constant-temperature 25 ℃ water bath oscillator, respectively carrying out sampling analysis after reaction for 10, 20, 30, 60, 90, 120, 180, 360, 540, 720 and 1440min, and carrying out parallel test. The removal rate calculated by analysis is shown in fig. 2 as a function of time.
Example 4: experiment of Cr (VI) removal rate of FeS-chitosan-biochar along with pH change
Preparing 50mL of simulated wastewater with initial chromium concentration of 100mg/L, respectively adjusting the pH values to 2, 4, 6, 7, 8, 10 and 12, respectively adding 0.1g of FeS-chitosan-biochar, sealing, putting into a water bath oscillator with constant temperature of 25 ℃, reacting for 24h, sampling and analyzing, and setting up parallel tests in experiments. Analytically calculated removal rates as a function of pH are shown in fig. 3.
Claims (10)
1. The preparation and application of the chitosan stable ferrous sulfide composite biochar material are characterized by comprising the steps of biochar preparation, ferrous sulfide preparation, modification and the like.
2. The method for preparing a chitosan stabilized ferrous sulfide composite biochar material as claimed in claim 1, wherein the biochar raw material is highland barley crop straw in plateau areas.
3. The method for preparing the chitosan stabilized ferrous sulfide composite biochar material as claimed in claim 1, wherein the mass of the biochar raw material is 65g which is 70% of the mass of sulfuric acid.
4. The method for preparing the chitosan-stabilized ferrous sulfide composite biochar material according to claim 1, wherein the mass of the catalyst asphalt is 1.3g which is 2% of the mass of the biochar raw material.
5. The method for preparing the chitosan-stabilized ferrous sulfide composite biochar material as claimed in claim 1, wherein the biochar preparation condition is heating at 200 ℃ for 2 h.
6. The method for preparing the chitosan-stabilized ferrous sulfide composite biochar material according to claim 1, wherein the vacuum drying temperature of the biochar is 150 ℃.
7. The method for preparing the chitosan-stabilized ferrous sulfide composite biochar material as claimed in claim 1, wherein the volume fraction of the acetic acid solution is 2%.
8. The method for preparing the chitosan-stabilized ferrous sulfide composite biochar material as claimed in claim 1, wherein the volume ratio of the mass of the chitosan to the volume of the acetic acid solution is 1g:50 mL.
9. The method for preparing the chitosan stabilized ferrous sulfide composite biochar material as claimed in claim 1, wherein the optimal ratio of ferrous sulfide to chitosan to biochar is 2:2: 1.
10. The method for preparing a chitosan-stabilized ferrous sulfide composite biochar material as claimed in claim 1, wherein the freezing temperature in the freeze drying process in the processes of preparing and modifying the ferrous sulfide is below-50 ℃, and the drying pressure is below 15 pa.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113648972A (en) * | 2021-09-10 | 2021-11-16 | 南京万德斯环保科技股份有限公司 | Preparation method of novel iron-based biochar material |
| CN113860468A (en) * | 2021-08-26 | 2021-12-31 | 广东工业大学 | Composite material for efficiently treating hexavalent chromium pollution in environment and preparation method and application thereof |
| CN114849749A (en) * | 2022-05-30 | 2022-08-05 | 浙大宁波理工学院 | Preparation method, product and application of supported high-dispersion pyrite Fenton catalyst |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114849749B (en) * | 2022-05-30 | 2023-11-03 | 浙大宁波理工学院 | Preparation method, product and application of supported high-dispersion pyrite Fenton catalyst |
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Application publication date: 20210528 |