CN112320894A - Bismuth sulfide modified iron-carbon filler, preparation method thereof and application thereof in sewage treatment - Google Patents
Bismuth sulfide modified iron-carbon filler, preparation method thereof and application thereof in sewage treatment Download PDFInfo
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- CN112320894A CN112320894A CN201910715977.4A CN201910715977A CN112320894A CN 112320894 A CN112320894 A CN 112320894A CN 201910715977 A CN201910715977 A CN 201910715977A CN 112320894 A CN112320894 A CN 112320894A
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- iron
- bismuth
- carbon filler
- sulfide modified
- bismuth sulfide
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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
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
- C02F1/46104—Devices therefor; Their operating or servicing
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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
- C02F7/00—Aeration of stretches of water
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W10/00—Technologies for wastewater treatment
- Y02W10/10—Biological treatment of water, waste water, or sewage
Abstract
The invention discloses a bismuth sulfide modified iron-carbon filler and a preparation method thereof, wherein reducing iron powder, cerium powder, expanded graphite and bentonite are used as raw materials, an ammonium bicarbonate aqueous solution is added, the raw materials are uniformly mixed and pelletized, and after drying and calcining, iron-carbon microspheres are prepared; the invention also discloses application of the bismuth sulfide modified iron-carbon filler in photoelectrocatalysis treatment of wastewater. The preparation method is safe and controllable, and the prepared filler has stable property, good structural strength, good sewage treatment effect, long service life and no secondary pollution.
Description
Technical Field
The invention belongs to the technical field of water treatment materials, and particularly relates to a bismuth sulfide modified iron-carbon filler, a preparation method thereof, and application thereof in sewage treatment.
Background
At present, rural economy in China develops rapidly, the rural living standard is obviously improved, but the problem of rural water environment pollution is not optimistic. Because the social and economic development level of rural areas is relatively lagged behind, the environmental protection consciousness of residents is generally thin, the environmental protection facilities are incomplete, the management is not in place and the like, most of villages and towns do not have perfect sewage collection systems, so that untreated domestic sewage in vast village and town areas is randomly discharged, a series of problems such as surface water and underground water pollution, agricultural resource damage and ecological environment deterioration are caused, the crisis of water resource shortage in China is even aggravated, and the sustainable development of social and economic of the villages and towns is severely restricted.
At present, the method for treating villages and towns has a physical method, a biological method and a chemical method, and the advantages and the disadvantages of various methods are as follows: (1) the physical method includes membrane separation technology and adsorption technology. The membrane separation technology is to screen out macromolecular pollutants by utilizing the aperture size of a membrane, so that the composition of village and town wastewater is complex, the membrane treatment process is easy to block, the treatment efficiency is low, and the membrane separation technology is not suitable for large-scale industrial treatment; while the adsorption technique is influenced by the hardness, alkalinity and Cl of the wastewater-The influence of the factors is large, and the practical wastewater treatment is greatly limited. (2) The biological method is mainly an activated sludge technology. The activated sludge technology realizes the degradation and utilization of pollutants in sewage by utilizing the metabolism of abundant microorganisms in the sludge, but the activated sludge method only has better treatment effect on the wastewater with low organic matter content. (3) The chemical method comprises an ozone oxidation technology, a Fenton oxidation technology and a photocatalysis technology. Ozone is a clean strong oxidant, has the advantages of strong oxidizing ability, simple equipment, no secondary pollution and the like, but has higher energy consumption; the Fenton oxidation technology has the advantages of simple process, mild conditions and the like, but can obtain better effect only under the conditions of microwave reinforcement, UV assistance and electric assistance; the photocatalysis treatment effect is thorough, the required equipment and process are simple, and the defects are that the energy utilization rate of the photocatalyst is not high, only a few photocatalyst can directly use solar energy, and meanwhile, the photocatalyst is easy to generate light corrosion so as to influence the use effect.
In summary, the single physical, biological and chemical technologies adopted in the existing village and town sewage treatment method are complicated to install, large in engineering quantity, short in technical staff, high in requirements on staff and cost, and incapable of completely meeting the requirements of efficient treatment of wide-spread village and town sewage with large water quantity and water quality fluctuation. Therefore, research on a new process for efficiently treating sewage in villages and towns is urgent.
Disclosure of Invention
Based on the defects of the prior art, the invention aims to provide the bismuth sulfide modified iron-carbon filler, and the micro-electrolysis catalytic activity of the iron-carbon filler is improved by modifying bismuth sulfide.
The invention also provides a preparation method of the bismuth sulfide modified iron-carbon filler and application of the bismuth sulfide modified iron-carbon filler in sewage treatment.
In order to achieve the purpose, the invention adopts the technical scheme that:
a preparation method of bismuth sulfide modified iron-carbon filler comprises the following steps:
(1) crushing and sieving reducing iron powder, cerium powder, expanded graphite and bentonite serving as raw materials, uniformly mixing, adding an ammonium bicarbonate aqueous solution, uniformly mixing, pelletizing, drying at 80-120 ℃ for 20-40 minutes, and calcining at 450-550 ℃ for 1.5-2.5 hours in a nitrogen atmosphere to obtain iron-carbon microspheres; the iron-carbon microsphere comprises the following raw materials in parts by weight: 40-60 parts of reducing iron powder, 5-10 parts of cerium powder, 20-40 parts of expanded graphite and 10-20 parts of bentonite;
(2) adding bismuth chloride into water, and fully stirring until the bismuth chloride is dissolved to obtain bismuth source reaction liquid; adding thiourea into an aqueous solution of N, N-dimethylformamide, and fully stirring until the thiourea is dissolved to obtain a sulfur source reaction solution; adding the sulfur source reaction solution into the zinc bismuth source reaction solution, and stirring for 0.5-1 hour to obtain a hydrothermal reaction solution; wherein the molar ratio of the bismuth chloride to the thiourea is 1: 2.5-5;
(3) and (3) placing the iron-carbon microspheres obtained in the step (1) into the hydrothermal reaction liquid obtained in the step (2), stirring for 0.5-1 hour, carrying out hydrothermal reaction for 5-10 hours at 150-200 ℃, cooling to room temperature, carrying out solid-liquid separation, taking out solids, washing, air-drying, and then carrying out heat preservation for 1.5-3 hours at 200-250 ℃ to obtain the iron-carbon microspheres.
Preferably, the mass fraction of ammonium bicarbonate in the aqueous solution of ammonium bicarbonate in the step (1) is 1-5%.
Further, the adding amount of the aqueous solution of ammonium bicarbonate is 20-40% of the total mass of the raw materials.
Preferably, the volume percentage of the N, N-dimethylformamide in the aqueous solution of the N, N-dimethylformamide in the step (2) is 30-50%.
Preferably, the molar concentrations of bismuth chloride in the bismuth source reaction liquid in the step (2) are respectively 0.015-0.035 mol/L; the molar concentration of thiourea in the sulfur source reaction liquid is 0.1-0.18 mol/L.
Preferably, the adding amount of the iron carbon microspheres in the hydrothermal reaction solution in the step (3) is 125-200 g/L.
The bismuth sulfide modified iron-carbon filler prepared by the method is adopted.
Preferably, the particle size of the bismuth sulfide modified iron-carbon filler is 20-40 mm.
The application of the bismuth sulfide modified iron-carbon filler in sewage treatment comprises the following steps: adding the bismuth sulfide modified iron-carbon filler into the sewage to be treated, stirring and aerating.
Preferably, the addition amount of the bismuth sulfide modified iron-carbon filler is 100-200 g/L.
The raw materials used in the preparation method are all common commercial products.
The preparation method is safe and controllable, and the prepared filler has stable property, good structural strength, good sewage treatment effect, long service life and no secondary pollution.
Detailed Description
In order to make the technical purpose, technical solutions and advantages of the present invention clearer, the technical solutions of the present invention are further described with reference to specific examples, which are intended to explain the present invention and are not to be construed as limiting the present invention, and those who do not specify a specific technique or condition in the examples follow the techniques or conditions described in the literature in the art or follow the product specification.
The reduced iron powder in the following examples was purchased from Zhengzhou Hencui metallurgy welding materials Co., Ltd., particle size 200 mesh; the cerium powder is purchased from Yangzhou rare earth metal Co Ltd of Taizhou city, Jiangsu province, and has the granularity of 300 meshes; the expanded graphite is prepared from Hades and Xin graphiteThe product company Limited (the product is ultrafine expandable graphite), the expansion multiplying power is 10-20 mL/g; the bentonite is purchased from Sen perlite application Limited company in Xinyang city, has the granularity of 325 meshes, the montmorillonite content of more than or equal to 70 percent and the density of 2.5 g/cm3。
Example 1
A preparation method of bismuth sulfide modified iron-carbon filler comprises the following steps:
(1) taking 50 g of reducing iron powder, 8 g of cerium powder, 27 g of expanded graphite and 15 g of bentonite as raw materials, crushing and sieving the raw materials, uniformly mixing, adding 35 mL of ammonium bicarbonate aqueous solution with the mass fraction of 3%, uniformly mixing, pelletizing, baking for 30 minutes at 100 ℃, and calcining for 2 hours at 500 ℃ in a nitrogen atmosphere to obtain iron-carbon microspheres;
(2) adding 1.9 g of bismuth chloride (6 mmol) into 240 mL of deionized water, and fully stirring until the bismuth chloride is dissolved to obtain a bismuth source reaction solution; adding 1.8 g of thiourea (24 mmol) into 240 mL of aqueous solution of N, N-dimethylformamide (the volume percentage of the N, N-dimethylformamide is 40%), and fully stirring until the thiourea is dissolved to obtain a sulfur source reaction solution; adding the sulfur source reaction solution into the zinc-bismuth source reaction solution, and stirring for 30 minutes to obtain a hydrothermal reaction solution (the molar ratio of bismuth chloride to zinc chloride to thiourea is 1: 4);
(3) and (2) placing the iron-carbon microspheres obtained in the step (1) into the hydrothermal reaction liquid obtained in the step (2), stirring for 0.5 hour, carrying out hydrothermal reaction at 180 ℃ for 8 hours, cooling to room temperature, filtering to obtain a solid, alternately washing with ethanol and deionized water, naturally drying, and then carrying out heat preservation at 220 ℃ for 2 hours to obtain the iron-carbon microspheres.
Example 2
A preparation method of bismuth sulfide modified iron-carbon filler comprises the following steps:
(1) taking 60 g of reducing iron powder, 10 g of cerium powder, 20 g of expanded graphite and 10 g of bentonite as raw materials, crushing and sieving the raw materials, uniformly mixing, adding 35 mL of ammonium bicarbonate aqueous solution with the mass fraction of 3%, uniformly mixing, pelletizing, baking for 40 minutes at 80 ℃, and calcining for 1.5 hours at 550 ℃ in a nitrogen atmosphere to obtain iron-carbon microspheres;
(2) adding 1.9 g of bismuth chloride (6 mmol) into 240 mL of deionized water, and fully stirring until the bismuth chloride is dissolved to obtain a bismuth source reaction solution; adding 1.36 g of thiourea (18 mmol) into 240 mL of aqueous solution of N, N-dimethylformamide (the volume percentage of the N, N-dimethylformamide is 40%), and fully stirring until the thiourea is dissolved to obtain a sulfur source reaction solution; adding the sulfur source reaction solution into the zinc-bismuth source reaction solution, and stirring for 30 minutes to obtain a hydrothermal reaction solution (the molar ratio of bismuth chloride to zinc chloride to thiourea is 1: 3);
(3) and (2) placing the iron-carbon microspheres obtained in the step (1) into the hydrothermal reaction liquid obtained in the step (2), stirring for 0.5 hour, carrying out hydrothermal reaction at 150 ℃ for 10 hours, cooling to room temperature, filtering to obtain a solid, alternately washing with ethanol and deionized water, naturally drying, and then carrying out heat preservation at 200 ℃ for 3 hours to obtain the iron-carbon microspheres.
Example 3
A preparation method of bismuth sulfide modified iron-carbon filler comprises the following steps:
(1) taking 40 g of reducing iron powder, 5 g of cerium powder, 40 g of expanded graphite and 15 g of bentonite as raw materials, crushing and sieving the raw materials, uniformly mixing, adding 35 mL of ammonium bicarbonate aqueous solution with the mass fraction of 3%, uniformly mixing, pelletizing, baking for 40 minutes at 80 ℃, and calcining for 1.5 hours at 550 ℃ in a nitrogen atmosphere to obtain iron-carbon microspheres;
(2) adding 1.9 g of bismuth chloride (6 mmol) into 240 mL of deionized water, and fully stirring until the bismuth chloride is dissolved to obtain a bismuth source reaction solution; adding 2.28 g of thiourea (30 mmol) into 240 mL of aqueous solution of N, N-dimethylformamide (the volume percentage of the N, N-dimethylformamide is 40%), and fully stirring until the thiourea is dissolved to obtain a sulfur source reaction solution; adding the sulfur source reaction solution into the zinc-bismuth source reaction solution, and stirring for 30 minutes to obtain a hydrothermal reaction solution (the molar ratio of bismuth chloride to zinc chloride to thiourea is 1: 5);
(3) and (2) placing the iron-carbon microspheres obtained in the step (1) into the hydrothermal reaction liquid obtained in the step (2), stirring for 0.5 hour, carrying out hydrothermal reaction at 200 ℃ for 5 hours, cooling to room temperature, filtering to obtain a solid, alternately washing with ethanol and deionized water, naturally drying, and then carrying out heat preservation at 250 ℃ for 1.5 hours to obtain the iron-carbon microspheres.
Comparative example 1
A bismuth sulfide modified iron-carbon filler, prepared according to the method of example 1, except that no cerium powder was added in step (1).
The performance of the bismuth sulfide modified iron-carbon filler prepared in examples 1 to 3 and comparative example 1 and the iron-carbon microsphere prepared in example 1 was tested. The method comprises the following steps: simulating organic sewage by using a phenol solution, wherein the concentration of phenol is 15 mg/L; the test is carried out in a transparent bottle (sealable) with the specification of 100 mL, and 100 mL of organic sewage is used in each test; the bismuth sulfide modified iron-carbon filler prepared in examples 1-3 and comparative example 1 and the iron-carbon microsphere prepared in example 1 are respectively used as treating agents, and the adding amount of the treating agents is 100 g/L.
The method comprises the following steps: after the addition of the adsorbent, shaking was continued for 2 minutes, and sampling and testing were performed.
The phenol adsorption amounts of the treatment agents of examples 1 to 3 and comparative example 1 were 0.39 mg, 0.38 mg, 0.39 mg and 0.30 mg, respectively, i.e., the phenol adsorption rates were 26%, 25%, 26% and 20%, respectively.
Step two: shaking was continued for 30 minutes and sampling was performed.
The phenol removal amounts of the adsorbents of examples 1 to 3 and comparative example 1 were 1.05 mg, 0.97 mg, 0.95 mg and 0.59 mg, respectively.
Step three: the pH was adjusted to 4, shaking was continued for 30 minutes, and sampling and testing were performed.
The phenol adsorption amounts of the adsorbents in examples 1 to 3 and comparative example 1 were 1.39 mg, 1.26 mg, 1.25 mg and 0.66 mg, respectively. The pH of the solution is adjusted to be acidic, which is helpful for the treating agent to further degrade organic matters.
Step four: then adding H2O2Solution (H in solution)2O2Was 1.5 mmol/L), was stirred open for 30 minutes, and was sampled for testing.
Due to the addition of H to the system2O2The iron-carbon filler is mixed with H2O2Generating heterogeneous Fenton-like reaction, generating superoxide radical and hydroxyl radical, and oxidatively degrading phenol. The phenol removal rates of examples 1-3 and comparative example 1 were 100%, 99%, and 75%, respectively.
The above embodiments are merely intended to illustrate the technical solution of the present invention and not to limit the same, and although the present invention has been described with reference to preferred embodiments thereof, it will be understood by those of ordinary skill in the art that various changes in form and details may be made therein without departing from the spirit and scope of the present invention as defined by the following claims.
Claims (10)
1. The preparation method of the bismuth sulfide modified iron-carbon filler is characterized by comprising the following steps of:
(1) crushing and sieving reducing iron powder, cerium powder, expanded graphite and bentonite serving as raw materials, uniformly mixing, adding an ammonium bicarbonate aqueous solution, uniformly mixing, pelletizing, drying at 80-120 ℃ for 20-40 minutes, and calcining at 450-550 ℃ for 1.5-2.5 hours in a nitrogen atmosphere to obtain iron-carbon microspheres; the iron-carbon microsphere comprises the following raw materials in parts by weight: 40-60 parts of reducing iron powder, 5-10 parts of cerium powder, 20-40 parts of expanded graphite and 10-20 parts of bentonite;
(2) adding bismuth chloride into water, and fully stirring until the bismuth chloride is dissolved to obtain bismuth source reaction liquid; adding thiourea into an aqueous solution of N, N-dimethylformamide, and fully stirring until the thiourea is dissolved to obtain a sulfur source reaction solution; adding the sulfur source reaction solution into the zinc bismuth source reaction solution, and stirring for 0.5-1 hour to obtain a hydrothermal reaction solution; wherein the molar ratio of the bismuth chloride to the thiourea is 1: 2.5-5;
(3) and (3) placing the iron-carbon microspheres obtained in the step (1) into the hydrothermal reaction liquid obtained in the step (2), stirring for 0.5-1 hour, carrying out hydrothermal reaction for 5-10 hours at 150-200 ℃, cooling to room temperature, carrying out solid-liquid separation, taking out solids, washing, air-drying, and then carrying out heat preservation for 1.5-3 hours at 200-250 ℃ to obtain the iron-carbon microspheres.
2. The method of preparing a bismuth sulfide modified iron-carbon filler according to claim 1, wherein: in the step (1), the mass fraction of ammonium bicarbonate in the ammonium bicarbonate water solution is 1-5%.
3. The method of preparing a bismuth sulfide modified iron-carbon filler according to claim 2, wherein: the adding amount of the ammonium bicarbonate water solution is 20-40% of the total mass of the raw materials.
4. The method of preparing a bismuth sulfide modified iron-carbon filler according to claim 1, wherein: the volume percentage of the N, N-dimethylformamide in the aqueous solution of the N, N-dimethylformamide in the step (2) is 30-50%.
5. The method of preparing a bismuth sulfide modified iron-carbon filler according to claim 1, wherein: the molar concentrations of bismuth chloride in the bismuth source reaction liquid in the step (2) are respectively 0.015-0.035 mol/L; the molar concentration of thiourea in the sulfur source reaction liquid is 0.1-0.18 mol/L.
6. The method of preparing a bismuth sulfide modified iron-carbon filler according to claim 1, wherein: the adding amount of the iron carbon microspheres in the hydrothermal reaction liquid in the step (3) is 125-200 g/L.
7. The bismuth sulfide modified iron-carbon filler prepared by the method of any one of claims 1 to 6.
8. The bismuth sulfide modified iron-carbon filler of claim 7, wherein: the particle size of the bismuth sulfide modified iron-carbon filler is 20-40 mm.
9. The use of the bismuth sulfide modified iron carbon filler of claim 8 in sewage treatment, wherein: adding the bismuth sulfide modified iron-carbon filler into the sewage to be treated, stirring and aerating.
10. The use of the bismuth sulfide modified iron-carbon filler of claim 9 in sewage treatment, wherein: the addition amount of the bismuth sulfide modified iron-carbon filler is 100-200 g/L.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113121124A (en) * | 2021-03-29 | 2021-07-16 | 桂林理工大学 | Preparation method of cerium-doped bismuth sulfide/ferric oxide nano heterojunction |
| CN114349125A (en) * | 2021-11-23 | 2022-04-15 | 中车唐山机车车辆有限公司 | Iron-carbon filler for urine treatment and preparation method thereof |
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