CN111389346B - Preparation of composite magnetic material modified fly ash and method for treating slime water - Google Patents

Preparation of composite magnetic material modified fly ash and method for treating slime water Download PDF

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CN111389346B
CN111389346B CN202010210972.9A CN202010210972A CN111389346B CN 111389346 B CN111389346 B CN 111389346B CN 202010210972 A CN202010210972 A CN 202010210972A CN 111389346 B CN111389346 B CN 111389346B
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fly ash
magnetic material
material modified
distilled water
composite magnetic
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CN111389346A (en
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颜冬青
李振
张墩稳
李毅红
王进
刘莉君
马科文
于伟
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Shaanxi Coal And Chemical And Coal Preparation Co ltd
Xian University of Science and Technology
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Shaanxi Coal And Chemical And Coal Preparation Co ltd
Xian University of Science and Technology
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/10Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
    • B01J20/103Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate comprising silica
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/28Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28002Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their physical properties
    • B01J20/28009Magnetic properties
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/28Treatment of water, waste water, or sewage by sorption
    • C02F1/281Treatment of water, waste water, or sewage by sorption using inorganic sorbents
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/52Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
    • C02F1/54Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using organic material
    • C02F1/56Macromolecular compounds
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02WCLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W30/00Technologies for solid waste management
    • Y02W30/50Reuse, recycling or recovery technologies
    • Y02W30/91Use of waste materials as fillers for mortars or concrete

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  • Life Sciences & Earth Sciences (AREA)
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  • Chemical Kinetics & Catalysis (AREA)
  • Separation Of Suspended Particles By Flocculating Agents (AREA)
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Abstract

The invention discloses a preparation method of composite magnetic material modified fly ash, which comprises the following steps: firstly, slowly adding ferrous chloride tetrahydrate, ferric chloride hexahydrate and anhydrous sodium sulfite into distilled water for dissolving while stirring, and adding sodium hydroxide after the temperature of a magnetic stirrer rises to 70 ℃; then ultrasonically dispersing for 30min, and cooling to room temperature; magnetic particles are obtained by adopting magnetic adsorption separation; secondly, adding the fly ash, acrylamide and magnetic particles into distilled water, heating under the stirring condition, adding potassium persulfate, reacting for a period of time, and cooling to room temperature; and after cooling, adopting a magnet to adsorb and separate to prepare the composite magnetic material modified fly ash. The invention also discloses a method for treating slime water by using the composite magnetic material modified fly ash. According to the invention, the magnetic particles are introduced in the process of modifying the fly ash, so that the sedimentation of the coal slime water is accelerated, and the problem of recycling the coal slime after flocculation is solved.

Description

Preparation of composite magnetic material modified fly ash and method for treating slime water
Technical Field
The invention belongs to the technical field of slime water treatment, and particularly relates to a preparation method of composite magnetic material modified fly ash and a method for treating slime water.
Background
Fly Ash (FA) is solid waste generated in the coal combustion process, and a large amount of stacking not only occupies land, but also causes harm to human health and ecological environment. The comprehensive development and utilization of the fly ash can solve the problem of environmental pollution, change the cost into valuable and provide a driving force for economic growth. The fly ash has wide source and low price, has porosity, large specific surface area and better adsorption performance, has the advantages of treating waste by waste, saving resources, being economical and efficient and the like in the field of sewage treatment, and has wide application prospect. However, due to the specific hydrophobic structure of the surface of the fly ash, the fly ash is difficult to effectively contact with water, and the self-adsorption performance is not exerted, so that the sewage purification effect is poor.
At the present stage, a plurality of methods are used for treating the slime water, wherein the addition of a flocculating agent is one of the simplest and the fastest methods. The commonly used flocculants are divided into two main categories, inorganic flocculants and organic flocculants. The methods have the advantages of high treatment cost, large using amount, long treatment time, large difference of treatment effects and common treatment effect.
The fly ash is fine ash collected from flue gas generated after coal combustion, is main solid waste discharged from a coal-fired power plant, and belongs to solid waste residues in coal chemical industry. The fly ash has adsorption capacity, and the coal slurry can be considered to be flocculated by the fly ash. However, in practice, the surface of the fly ash has strong hydrophobicity, and is difficult to disperse in the coal slurry water, namely in the water phase, so that the contact probability with coal particles in the coal slurry water is low, and the flocculation effect is poor. In addition, the flocculated flocculating agent is precipitated in coal slime, and if the flocculating agent cannot be recycled, the cost is high, and the economic value is low.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provide a preparation method of composite magnetic material modified fly ash, which not only accelerates the precipitation of coal slime water, but also solves the problem of recycling after coal slime flocculation by introducing magnetic particles in the process of modifying the fly ash.
In order to achieve the purpose, the invention adopts the technical scheme that: the preparation method of the composite magnetic material modified fly ash is characterized by comprising the following steps:
step one, measuring 250mL of distilled water, putting the measured distilled water into a 500mL beaker, slowly adding three reagents, namely 0.4g of ferrous chloride tetrahydrate, 1.08g of ferric chloride hexahydrate and 1g of anhydrous sodium sulfite, into the beaker in sequence while stirring by adopting a magnetic stirrer, and stirring until the reagents are dissolved in the distilled water; after the reagent is dissolved, the temperature of the magnetic stirrer starts to rise, and after the temperature of the magnetic stirrer rises to 70 ℃, 10g of sodium hydroxide is added and the reaction is continuously stirred for 40 min; then, placing the beaker in an ultrasonic instrument for ultrasonic dispersion for 30min, and then cooling to room temperature; after cooling, putting a magnet on the outer wall of the beaker, adsorbing the magnetic substance generated by the reaction on the inner wall of the beaker, pouring out the supernatant in the beaker, adding distilled water for washing, repeatedly pouring out the supernatant, adding distilled water for multiple times until the pH of the solution is neutral, and drying to obtain magnetic particles;
step two, adding the fly ash, the acrylamide and the magnetic particles prepared in the step one into a three-necked bottle filled with distilled water, heating to a certain temperature under the condition of stirring, adding an initiator potassium persulfate with the mass of 1% of that of the acrylamide, reacting for a period of time, and then cooling the reaction liquid to room temperature; and after cooling, putting a magnet on the outer wall of the three-necked bottle, adsorbing the modified fly ash substance generated by the reaction on the inner wall of the beaker, pouring out the supernatant, adding distilled water for washing, and drying for a certain time under a vacuum condition at a certain temperature to obtain the composite magnetic material modified fly ash.
The preparation method of the composite magnetic material modified fly ash is characterized in that in the second step, the amount of the fly ash is 0.8-1.2 g, the amount of acrylamide is 0.05-1.0 g, and the amount of the magnetic particles is 0.1-0.5 g.
The preparation method of the composite magnetic material modified fly ash is characterized in that in the second step, the use amount of the fly ash is 1g, the use amount of the acrylamide is 0.1g, and the use amount of the magnetic particles is 0.2 g.
The preparation method of the composite magnetic material modified fly ash is characterized in that the volume of distilled water in the three-necked bottle filled with distilled water in the step two is 10-60 mL.
The preparation method of the composite magnetic material modified fly ash is characterized in that the volume of distilled water in the three-necked bottle filled with distilled water in the step two is 30 mL.
The preparation method of the composite magnetic material modified fly ash is characterized in that the reaction time in the step two is 1-12 h, and the reaction temperature is 50-90 ℃.
The preparation method of the composite magnetic material modified fly ash is characterized in that the reaction time in the step two is 2 hours, and the reaction temperature is 70 ℃.
The preparation method of the composite magnetic material modified fly ash is characterized in that the drying time in the step two is 10-48 h, and the drying temperature is 20-60 ℃.
The preparation method of the composite magnetic material modified fly ash is characterized in that in the second step, the drying time is 24 hours, and the drying temperature is 30 ℃.
The preparation method of the composite magnetic material modified fly ash is characterized in that in the step one, the drying temperature of the magnetic substance is 20-60 ℃, and the drying time is 10-48 h.
The invention also discloses a method for treating slime water by using the composite magnetic material modified fly ash, which is characterized by comprising the following steps of: measuring 5mL of slime water, adding 0.05-0.3 g of the prepared composite magnetic material modified fly ash, uniformly stirring, and standing for 20-50 min to flocculate the slime water.
The method for treating the slime water by using the composite magnetic material modified fly ash is characterized in that the adding amount of the composite magnetic material modified fly ash is 0.1g, and the standing time is 30 min.
Compared with the prior art, the invention has the following advantages:
1. the invention adopts the cheap solid waste in the coal chemical industry for treating the slime water, and can reduce the harm of the solid waste in the coal chemical industry to human existence and ecological environment. Aiming at the problems of flocculation adsorption of the fly ash, the hydrophilic monomer acrylamide is grafted, so that the dispersing capacity of the fly ash in a water phase is improved, the contact chance of the fly ash and coal particles can be improved, and the flocculation effect is improved.
2. In order to further improve the economic value, the magnetic particles are creatively introduced in the process of modifying the fly ash, so that the sedimentation of the coal slime water is accelerated, and the problem of recycling the coal slime after flocculation can be solved.
3. Through a large amount of researches in the experimental process, the research shows that the surface of the coal particles generally has negative charges, so that the monomer acrylamide with amino groups with positive charges is selected for grafting modification, and the surface of the modified fly ash after grafting the acrylamide can take positive charges, thereby being beneficial to adsorbing the coal particles, improving the adsorption capacity and promoting the flocculation effect.
4. According to the invention, coal chemical industry solid waste residue coal ash is adopted to treat coal slime water, and in order to improve the contact adsorption of coal ash and coal particles in the coal slime water and increase the flocculation effect, hydrophilic monomers are grafted on the surface of the coal ash, so that the dispersibility of modified coal ash in a water phase is improved, the coal particles can be adsorbed to the greatest extent, and the flocculation effect is increased (the using amount is reduced, the treatment time is short, and the effect is obvious).
The invention is described in further detail below with reference to the figures and examples.
Drawings
FIG. 1 is an infrared spectrum of the existing fly ash and the composite magnetic material modified fly ash prepared by the present invention.
FIG. 2 is a scanning electron microscope image of the existing fly ash and the composite magnetic material modified fly ash prepared by the invention.
FIG. 3 is a diagram of flocculated coal slurry water obtained by treating coal slurry water with the conventional coal ash and the composite magnetic material modified coal ash prepared by the method.
FIG. 4 is a comparison chart of the conventional fly ash flocculant and the composite magnetic material modified fly ash flocculated coal slime water prepared by the method.
Detailed Description
Example 1
The embodiment comprises the following steps:
step one, measuring 250mL of distilled water, placing the measured distilled water in a 500mL beaker, and sequentially adding 0.4g of ferrous chloride tetrahydrate (FeCl) three reagents while stirring by adopting a magnetic stirrer 2 ·4H 2 O), 1.08g of iron chloride hexahydrate (FeCl) 3 ·6H 2 O) and 1g of anhydrous sodium sulfite (Na) 2 SO 3 ) Slowly adding into a beaker, and stirring until the reagent is dissolved in distilled water; after the reagent is dissolved, the temperature of the magnetic stirrer starts to rise, and after the temperature of the magnetic stirrer rises to 70 ℃, 10g of sodium hydroxide is added and the reaction is continuously stirred for 40 min; then, placing the beaker in an ultrasonic instrument for ultrasonic dispersion for 30min, and then cooling to room temperature; and after cooling, putting a magnet on the outer wall of the beaker, adsorbing the magnetic substance generated by the reaction on the inner wall of the beaker, pouring the supernatant in the beaker, adding distilled water for washing, repeatedly pouring the supernatant, adding distilled water for multiple times until the pH of the solution is neutral, and drying to obtain the magnetic particles. The drying temperature of the magnetic substance is 20 ℃, and the drying time is 29 h.
Step two, adding the fly ash, the acrylamide and the magnetic particles prepared in the step one into a three-necked bottle filled with distilled water, heating to a certain temperature under the condition of stirring, adding an initiator potassium persulfate with the mass of 1% of that of the acrylamide, reacting for a period of time, and then cooling the reaction liquid to room temperature; and after cooling, putting a magnet on the outer wall of the three-necked bottle, adsorbing the modified fly ash substance generated by the reaction on the inner wall of the beaker, pouring out the supernatant, adding distilled water for washing, and drying for a certain time under a vacuum condition at a certain temperature to obtain the composite magnetic material modified fly ash. The using amount of the fly ash is 0.9g, the using amount of the acrylamide is 1.0g, and the using amount of the magnetic particles is 0.3 g. The volume of the distilled water in the three-necked bottle containing the distilled water is 10 mL. The reaction time was 6h and the reaction temperature was 70 ℃. The drying time is 24h, and the drying temperature is 60 ℃.
The method for treating the slime water by using the composite magnetic material modified fly ash prepared by the embodiment comprises the following steps: measuring 5mL of slime water, adding 0.2g of the prepared composite magnetic material modified fly ash, stirring and uniformly mixing, and standing for 40min to flocculate the slime water.
Example 2
The embodiment comprises the following steps:
step one, measuring 250mL of distilled water, putting the measured distilled water into a 500mL beaker, adopting a magnetic stirrer to stir, and sequentially and slowly adding 0.4g of ferrous chloride tetrahydrate, 1.08g of ferric chloride hexahydrate and 1g of anhydrous sodium sulfite into the beaker, and stirring until the reagents are dissolved in the distilled water; after the reagent is dissolved, the temperature of the magnetic stirrer starts to rise, and after the temperature of the magnetic stirrer rises to 70 ℃, 10g of sodium hydroxide is added and the reaction is continuously stirred for 40 min; then, placing the beaker in an ultrasonic instrument for ultrasonic dispersion for 30min, and then cooling to room temperature; and after cooling, putting a magnet on the outer wall of the beaker, adsorbing the magnetic substance generated by the reaction on the inner wall of the beaker, pouring the supernatant in the beaker, adding distilled water for washing, repeatedly pouring the supernatant, adding distilled water for multiple times until the pH of the solution is neutral, and drying to obtain the magnetic particles. The drying temperature of the magnetic substance is 30 ℃, and the drying time is 10 h.
Step two, adding the fly ash, the acrylamide and the magnetic particles prepared in the step one into a three-necked bottle filled with distilled water, heating to a certain temperature under the condition of stirring, adding an initiator potassium persulfate with the mass of 1% of that of the acrylamide, reacting for a period of time, and then cooling the reaction liquid to room temperature; and after cooling, putting a magnet on the outer wall of the three-necked bottle, adsorbing the modified fly ash substance generated by the reaction on the inner wall of the beaker, pouring out the supernatant, adding distilled water for washing, and drying for a certain time under a vacuum condition at a certain temperature to obtain the composite magnetic material modified fly ash. The using amount of the fly ash is 1.1g, the using amount of the acrylamide is 0.8g, and the using amount of the magnetic particles is 0.1 g. The volume of the distilled water in the three-necked bottle containing the distilled water is 50 mL. The reaction time is 1h, and the reaction temperature is 50 ℃. The drying time is 40h, and the drying temperature is 20 ℃.
The method for treating coal slime water by using the composite magnetic material modified fly ash prepared in the embodiment comprises the following steps: measuring 5mL of slime water, adding 0.3g of the composite magnetic material modified fly ash, uniformly stirring, and standing for 20min to flocculate the slime water.
Example 3
The embodiment comprises the following steps:
step one, measuring 250mL of distilled water, putting the measured distilled water into a 500mL beaker, slowly adding three reagents, namely 0.4g of ferrous chloride tetrahydrate, 1.08g of ferric chloride hexahydrate and 1g of anhydrous sodium sulfite, into the beaker in sequence while stirring by adopting a magnetic stirrer, and stirring until the reagents are dissolved in the distilled water; after the reagent is dissolved, the temperature of the magnetic stirrer starts to rise, and after the temperature of the magnetic stirrer rises to 70 ℃, 10g of sodium hydroxide is added and the reaction is continuously stirred for 40 min; then, placing the beaker in an ultrasonic instrument for ultrasonic dispersion for 30min, and then cooling to room temperature; and after cooling, putting a magnet on the outer wall of the beaker, adsorbing the magnetic substance generated by the reaction on the inner wall of the beaker, pouring the supernatant in the beaker, adding distilled water for washing, repeatedly pouring the supernatant, adding distilled water for multiple times until the pH of the solution is neutral, and drying to obtain the magnetic particles. The drying temperature of the magnetic substance is 60 ℃, and the drying time is 20 h.
Step two, adding the fly ash, the acrylamide and the magnetic particles prepared in the step one into a three-necked bottle filled with distilled water, heating to a certain temperature under the condition of stirring, adding an initiator potassium persulfate with the mass of 1% of that of the acrylamide, reacting for a period of time, and then cooling the reaction liquid to room temperature; and after cooling, putting a magnet on the outer wall of the three-necked bottle, adsorbing the modified fly ash substance generated by the reaction on the inner wall of the beaker, pouring out the supernatant, adding distilled water for washing, and drying for a certain time under a vacuum condition at a certain temperature to obtain the composite magnetic material modified fly ash. The using amount of the fly ash is 0.8g, the using amount of the acrylamide is 0.5g, and the using amount of the magnetic particles is 0.2 g. The volume of the distilled water in the three-necked bottle containing the distilled water is 60 mL. The reaction time is 10h, and the reaction temperature is 60 ℃. The drying time is 48h, and the drying temperature is 50 ℃.
The method for treating the slime water by using the composite magnetic material modified fly ash prepared by the embodiment comprises the following steps: measuring 5mL of slime water, adding 0.1g of the composite magnetic material modified fly ash, uniformly stirring, and standing for 40min to flocculate the slime water.
Example 4
The embodiment comprises the following steps:
step one, measuring 250mL of distilled water, putting the measured distilled water into a 500mL beaker, slowly adding three reagents, namely 0.4g of ferrous chloride tetrahydrate, 1.08g of ferric chloride hexahydrate and 1g of anhydrous sodium sulfite, into the beaker in sequence while stirring by adopting a magnetic stirrer, and stirring until the reagents are dissolved in the distilled water; after the reagent is dissolved, the temperature of the magnetic stirrer starts to rise, and after the temperature of the magnetic stirrer rises to 70 ℃, 10g of sodium hydroxide is added and the reaction is continuously stirred for 40 min; then, placing the beaker in an ultrasonic instrument for ultrasonic dispersion for 30min, and then cooling to room temperature; and after cooling, putting a magnet on the outer wall of the beaker, adsorbing the magnetic substance generated by the reaction on the inner wall of the beaker, pouring the supernatant in the beaker, adding distilled water for washing, repeatedly pouring the supernatant, adding distilled water for multiple times until the pH of the solution is neutral, and drying to obtain the magnetic particles. The drying temperature of the magnetic substance is 50 ℃, and the drying time is 48 h.
Step two, adding the fly ash, the acrylamide and the magnetic particles prepared in the step one into a three-necked bottle containing distilled water, heating to a certain temperature under the condition of stirring, adding an initiator potassium persulfate with the mass being 1% of that of the acrylamide, reacting for a period of time, and then cooling the reaction liquid to room temperature; and after cooling, putting a magnet on the outer wall of the three-necked bottle, adsorbing the modified fly ash substance generated by the reaction on the inner wall of the beaker, pouring out the supernatant, adding distilled water for washing, and drying for a certain time under a vacuum condition at a certain temperature to obtain the composite magnetic material modified fly ash. The using amount of the fly ash is 1.0g, the using amount of the acrylamide is 0.1g, and the using amount of the magnetic particles is 0.5 g. The volume of the distilled water in the three-necked bottle containing the distilled water is 40 mL. The reaction time is 12h, and the reaction temperature is 90 ℃. The drying time is 29h, and the drying temperature is 40 ℃.
The method for treating coal slime water by using the composite magnetic material modified fly ash prepared in the embodiment comprises the following steps: measuring 5mL of slime water, adding 0.1g of the composite magnetic material modified fly ash, uniformly stirring, and standing for 50min to flocculate the slime water.
Example 5
The embodiment comprises the following steps:
step one, measuring 250mL of distilled water, putting the measured distilled water into a 500mL beaker, slowly adding three reagents, namely 0.4g of ferrous chloride tetrahydrate, 1.08g of ferric chloride hexahydrate and 1g of anhydrous sodium sulfite, into the beaker in sequence while stirring by adopting a magnetic stirrer, and stirring until the reagents are dissolved in the distilled water; after the reagent is dissolved, the temperature of the magnetic stirrer starts to rise, and after the temperature of the magnetic stirrer rises to 70 ℃, 10g of sodium hydroxide is added and the reaction is continuously stirred for 40 min; then, placing the beaker in an ultrasonic instrument for ultrasonic dispersion for 30min, and then cooling to room temperature; and after cooling, putting a magnet on the outer wall of the beaker, adsorbing the magnetic substance generated by the reaction on the inner wall of the beaker, pouring the supernatant in the beaker, adding distilled water for washing, repeatedly pouring the supernatant, adding distilled water for multiple times until the pH of the solution is neutral, and drying to obtain the magnetic particles. The drying temperature of the magnetic substance is 40 ℃, and the drying time is 40 h.
Step two, adding the fly ash, the acrylamide and the magnetic particles prepared in the step one into a three-necked bottle filled with distilled water, heating to a certain temperature under the condition of stirring, adding an initiator potassium persulfate with the mass of 1% of that of the acrylamide, reacting for a period of time, and then cooling the reaction liquid to room temperature; and after cooling, putting a magnet on the outer wall of the three-necked bottle, adsorbing the modified fly ash substance generated by the reaction on the inner wall of the beaker, pouring out the supernatant, adding distilled water for washing, and drying for a certain time under a vacuum condition at a certain temperature to obtain the composite magnetic material modified fly ash. The using amount of the fly ash is 1.2g, the using amount of the acrylamide is 0.05g, and the using amount of the magnetic particles is 0.4 g. The volume of the distilled water in the three-necked bottle containing the distilled water is 30 mL. The reaction time is 2h, and the reaction temperature is 80 ℃. The drying time is 10h, and the drying temperature is 30 ℃.
The method for treating the slime water by using the composite magnetic material modified fly ash prepared by the embodiment comprises the following steps: measuring 5mL of slime water, adding 0.05g of the prepared composite magnetic material modified fly ash, stirring and uniformly mixing, and standing for 30min to flocculate the slime water.
The composite magnetic material modified fly ash prepared in any one of the embodiments 1 to 5 is applied to flocculation of coal slime water, and the application method specifically comprises the following steps: 5mL of slime water is weighed, 0.1g of the composite magnetic material modified fly ash prepared by the method is added, and after uniform mixing, standing is carried out for 30min, so that flocculation can be carried out on the slime water, and the slime water can be purified.
Fig. 1 to 4 show the performance analysis of the composite magnetic material modified fly ash prepared in example 4, and the rest of the examples are basically the same as example 4.
FIG. 1 is an infrared spectrum of the existing fly ash and the composite magnetic material modified fly ash prepared by the present invention. Compared with the existing fly ash, the infrared spectrum of the composite magnetic material modified fly ash (the modified fly ash of the invention in figure 1) prepared by the invention is 2800cm -1 、1600cm -1 The peaks are respectively the peaks of C-H and carbonyl in the grafted polyacrylamide, which can show that the acrylamide monomer is grafted and polymerized on the fly ash.
FIG. 2 is a scanning electron microscope image of the existing fly ash and the composite magnetic material modified fly ash prepared by the present invention. A. B, C are scanning electron micrographs of the existing fly ash at different angles, and D, E, F are scanning electron micrographs of the composite magnetic material modified fly ash prepared by the invention at different angles. From a scanning electron microscope picture, the difference between the existing fly ash and the composite magnetic material modified fly ash prepared by the invention is shown, and the combination of infrared peak-off of infrared spectrum data indicates that the hydrophilic monomer acrylamide is successfully grafted and polymerized on the surface of the fly ash.
FIG. 3 is a diagram of flocculated coal slurry water obtained by treating coal slurry water with the conventional coal ash and the composite magnetic material modified coal ash prepared by the method. And sequentially carrying out flocculation for 10min, 20min and 30min on a slime water bottle treated by the composite magnetic material modified fly ash prepared by the invention and a slime water bottle treated by the existing fly ash from left to right, and then comparing flocculation effects to obtain the good flocculation effect of the modified composite magnetic material modified fly ash on the slime water.
Fig. 4 is a comparison diagram of coal slurry flocculated by the existing fly ash flocculant (fly ash flocculant without magnetic particles) and the composite magnetic material modified fly ash prepared by the invention (modified fly ash with magnetic particles). As can be seen from the figure, the effect of the composite magnetic material modified fly ash prepared by the invention on flocculating the coal slime is superior to that of the existing fly ash flocculating agent on flocculating the coal slime, and the effect is very obvious. Because the difference of effects cannot be obvious when the mobile phone is used, the solid contents in supernatant of the coal slime after flocculation for a certain time, the coal slime after flocculation by adopting the conventional coal ash flocculating agent (without adding magnetic particles) and the coal slime after flocculation by adopting the modified coal ash (with adding magnetic particles) are measured, and the measurement results are respectively shown in the following table 1.
TABLE 1 supernatant solids content
Figure BDA0002422799450000101
V represents the volume of supernatant taken;
m 1 represents the mass of the filter paper;
m 2 representing the total mass of the dried filter paper and the supernatant liquid solid;
m 2 -m 1 representing the total solid mass of the supernatant of the dried sample;
w represents the solid content of the supernatant of fly ash (m) 2 -m 1 )/V。
As can be seen from Table 1, the modified fly ash (with magnetic particles) of the invention can accelerate the sedimentation of the coal slime water, and the data clearly shows that the magnetic particles have obvious influence on the flocculation effect, and the modified fly ash (with magnetic particles) of the invention has good flocculation effect on the coal slime water.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and all simple modifications, changes and equivalent structural changes made to the above embodiment according to the technical spirit of the present invention still fall within the protection scope of the technical solution of the present invention.

Claims (9)

1. The preparation method of the composite magnetic material modified fly ash is characterized by comprising the following steps:
step one, measuring 250mL of distilled water, putting the measured distilled water into a 500mL beaker, slowly adding 0.4g of ferrous chloride tetrahydrate, 1.08g of ferric chloride hexahydrate and 1g of anhydrous sodium sulfite of three reagents into the beaker while stirring by a magnetic stirrer, and stirring until the reagents are dissolved in the distilled water; after the reagent is dissolved, the temperature of the magnetic stirrer starts to rise, and after the temperature of the magnetic stirrer rises to 70 ℃, 10g of sodium hydroxide is added and the reaction is continuously stirred for 40 min; then, placing the beaker in an ultrasonic instrument for ultrasonic dispersion for 30min, and then cooling to room temperature; after cooling, putting a magnet on the outer wall of the beaker, adsorbing the magnetic substance generated by the reaction on the inner wall of the beaker, pouring out the supernatant in the beaker, adding distilled water for washing, repeatedly pouring out the supernatant, adding distilled water for multiple times until the pH of the solution is neutral, and drying to obtain magnetic particles; the drying temperature of the magnetic substance is 20-60 ℃, and the drying time is 10-48 h;
step two, adding the fly ash, the acrylamide and the magnetic particles prepared in the step one into a three-necked bottle filled with distilled water, heating to a certain temperature under the condition of stirring, adding an initiator potassium persulfate with the mass of 1% of that of the acrylamide, reacting for a period of time, and then cooling the reaction liquid to room temperature; after cooling, putting a magnet on the outer wall of the three-necked bottle, adsorbing the modified fly ash substance generated by the reaction on the inner wall of the beaker, pouring out the supernatant, adding distilled water for washing, and drying for a certain time under a vacuum condition at a certain temperature to obtain the composite magnetic material modified fly ash;
the usage amount of the fly ash is 0.8-1.2 g, the usage amount of the acrylamide is 0.05-1.0 g, and the usage amount of the magnetic particles is 0.1-0.5 g.
2. The method for preparing the composite magnetic material modified fly ash according to claim 1, wherein in the second step, the amount of the fly ash is 1g, the amount of the acrylamide is 0.1g, and the amount of the magnetic particles is 0.2 g.
3. The method for preparing the composite magnetic material modified fly ash according to claim 1, wherein the volume of the distilled water in the three-necked bottle containing the distilled water in the second step is 10 mL-60 mL.
4. The method for preparing composite magnetic material modified fly ash according to claim 3, wherein the volume of distilled water in the three-necked bottle containing distilled water in the second step is 30 mL.
5. The method for preparing the composite magnetic material modified fly ash according to claim 1, wherein the reaction time in the second step is 1-12 h, and the reaction temperature is 50-90 ℃.
6. The method for preparing the composite magnetic material modified fly ash according to claim 5, wherein the reaction time in the second step is 2 hours, and the reaction temperature is 70 ℃.
7. The method for preparing the composite magnetic material modified fly ash according to claim 1, wherein the drying time in the second step is 10-48 h, and the drying temperature is 20-60 ℃.
8. The method for treating the coal slime water by using the composite magnetic material modified fly ash as claimed in claim 1, is characterized by comprising the following steps of: measuring 5mL of slime water, adding 0.05-0.3 g of the prepared composite magnetic material modified fly ash, uniformly stirring, and standing for 20-50 min to flocculate the slime water.
9. The method for treating the coal slime water by using the composite magnetic material modified fly ash as claimed in claim 8, wherein the addition amount of the composite magnetic material modified fly ash is 0.1g, and the standing time is 30 min.
CN202010210972.9A 2020-03-24 2020-03-24 Preparation of composite magnetic material modified fly ash and method for treating slime water Active CN111389346B (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2003053860A1 (en) * 2001-12-11 2003-07-03 Henkel Kommanditgesellschaft Auf Aktien Method for purifying waste water and magnetic adsorbents suited therefor
CN101665280A (en) * 2009-10-19 2010-03-10 大连理工大学 Method for waste water treatment and preparing magnetic flocculant by reclaimed floc
CN103991940A (en) * 2011-03-29 2014-08-20 济宁医学院 Process for preparing hybrid flocculant from fly ash
CN104276643A (en) * 2014-10-10 2015-01-14 安徽理工大学 Method for preparing magnetic flocculating agent by compounding coal ash magnetic bead and polyacrylamide
CN108031453A (en) * 2017-12-13 2018-05-15 太原理工大学 Microwave radiation technology magnetism fly ash loading p-nitrophenol molecular engram solid phase extraction material

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2003053860A1 (en) * 2001-12-11 2003-07-03 Henkel Kommanditgesellschaft Auf Aktien Method for purifying waste water and magnetic adsorbents suited therefor
CN101665280A (en) * 2009-10-19 2010-03-10 大连理工大学 Method for waste water treatment and preparing magnetic flocculant by reclaimed floc
CN103991940A (en) * 2011-03-29 2014-08-20 济宁医学院 Process for preparing hybrid flocculant from fly ash
CN104276643A (en) * 2014-10-10 2015-01-14 安徽理工大学 Method for preparing magnetic flocculating agent by compounding coal ash magnetic bead and polyacrylamide
CN108031453A (en) * 2017-12-13 2018-05-15 太原理工大学 Microwave radiation technology magnetism fly ash loading p-nitrophenol molecular engram solid phase extraction material

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
聚丙烯酰胺改性粉煤灰对印染废水的处理效果;潘高峰等;《毛纺科技》;20170610;第45卷(第06期);第44-47页 *

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