CN111268773A - Magnetic coagulant and preparation method thereof - Google Patents

Magnetic coagulant and preparation method thereof Download PDF

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Publication number
CN111268773A
CN111268773A CN202010197441.0A CN202010197441A CN111268773A CN 111268773 A CN111268773 A CN 111268773A CN 202010197441 A CN202010197441 A CN 202010197441A CN 111268773 A CN111268773 A CN 111268773A
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China
Prior art keywords
magnetic
fly ash
coagulant
acid
preparing
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CN202010197441.0A
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Inventor
齐立强
刘堃杨
王瑞涛
李晶欣
王旭
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North China Electric Power University
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North China Electric Power University
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Publication of CN111268773A publication Critical patent/CN111268773A/en
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    • 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
    • C02F1/48Treatment of water, waste water, or sewage with magnetic or electric fields
    • C02F1/488Treatment of water, waste water, or sewage with magnetic or electric fields for separation of magnetic materials, e.g. magnetic flocculation
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/30Organic compounds

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  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Engineering & Computer Science (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Organic Chemistry (AREA)
  • Separation Of Suspended Particles By Flocculating Agents (AREA)

Abstract

The invention belongs to the technical field of coagulants, and provides a magnetic coagulant and a preparation method thereof. The method for preparing the magnetic coagulant comprises the following steps: (1) sorting fly ash into magnetic fly ash and non-magnetic fly ash; (2) modifying the non-magnetic fly ash by using a modifier to obtain modified fly ash; (3) and mixing the magnetic fly ash and the modified fly ash to prepare the magnetic coagulant. The magnetic coagulant can remove substances such as colloids, suspended matters, organic pollutants and the like in sewage, thereby reducing the content of COD (chemical oxygen demand) in the water and simultaneously solving the problems of overhigh magnetic seed production cost, complex process flow and the like in the magnetic coagulation sedimentation technology.

Description

Magnetic coagulant and preparation method thereof
Technical Field
The invention relates to the technical field of coagulants, in particular to a magnetic coagulant and a preparation method thereof.
Background
China is a country with water resource shortage, and the water resource problem restricts the development of the country to a certain extent. In recent years, with the progress of industrialization and urbanization in China, the phenomenon of water pollution is increasingly prominent, and the cost of sewage treatment is increasingly increased. The fly ash is a byproduct generated by a coal-fired power plant, China is a big country for producing and using coal, and billions of tons of fly ash can be produced by coal-fired power generation of China every year. At present, fly ash becomes one of the current industrial waste residues with large discharge capacity in China, and a large amount of untreated fly ash can cause great damage and influence on the environment. The fly ash particles are in a porous honeycomb structure, have large specific surface area and high adsorption activity, and can be used for treating sewage.
Currently, most studies on fly ash are used to modify fly ash, so as to increase the surface area, increase active sites and enhance the adsorption capacity. There have also been studies on the preparation of fly ash into a coagulant for use in the treatment of sewage. However, no research has been made on fly ash as a magnetic coagulant. The magnetic coagulation sedimentation technology in the prior art also has the defects of overhigh production cost of magnetic seeds, complex process flow and the like.
Disclosure of Invention
The invention aims to provide a magnetic coagulant which integrates magnetism and coagulation characteristics, thereby achieving the effect of removing COD in water with high efficiency.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a preparation method of a magnetic coagulant, which comprises the following steps:
(1) sorting fly ash into magnetic fly ash and non-magnetic fly ash;
(2) modifying the non-magnetic fly ash by using a modifier to obtain modified fly ash;
(3) and mixing the magnetic fly ash and the modified fly ash to prepare the magnetic coagulant.
Preferably, the non-magnetic fly ash is refined and then modified.
Preferably, the grain diameter of the refined non-magnetic fly ash is less than 75 microns.
Preferably, the solid-to-liquid ratio of the non-magnetic fly ash to the modifier is 1g: (0.5-1.5) ml.
Preferably, the modifier comprises salt and acid, and the solid-to-liquid ratio of the salt to the acid is 1g (10-30) ml.
Preferably, the acid comprises hydrochloric acid and sulfuric acid, the volume ratio of the hydrochloric acid to the sulfuric acid is 1 (2-4), the concentration of the hydrochloric acid is 37%, and the concentration of the sulfuric acid is 98%.
Preferably, the salt is sodium chloride or ammonium fluoride.
Preferably, the modified fly ash is prepared by sequentially drying and refining the modified fly ash after the modification treatment.
The invention also provides a magnetic coagulant prepared by the method.
The magnetic coagulant provided by the invention is obtained by screening out a part of coal ash with magnetism, modifying the other part of coal ash to prepare modified coal ash, and mixing the modified coal ash and the modified coal ash. The method changes the fly ash into valuable, and achieves the purpose of treating wastes with processes of wastes against one another. The magnetic coagulant can remove substances such as colloids, suspended matters, organic pollutants and the like in sewage, thereby reducing the content of COD (chemical oxygen demand) in the water and simultaneously solving the problems of overhigh magnetic seed production cost, complex process flow and the like in the magnetic coagulation sedimentation technology.
Detailed Description
The invention provides a preparation method of a magnetic coagulant, which comprises the following steps:
(1) sorting fly ash into magnetic fly ash and non-magnetic fly ash;
(2) modifying the non-magnetic fly ash by using a modifier to obtain modified fly ash;
(3) and mixing the magnetic fly ash and the modified fly ash to prepare the magnetic coagulant.
The fly ash is from a byproduct generated by a coal-fired power plant, and is separated into magnetic fly ash and non-magnetic fly ash.
In the present invention, the method of sorting fly ash is preferably magnetic separation.
The invention uses a modifier to modify the non-magnetic fly ash to obtain the modified fly ash.
The non-magnetic fly ash of the present invention is preferably refined before the modification treatment.
In the present invention, the particle size after the thinning is preferably less than 75 micrometers, and more preferably less than 50 micrometers.
In the present invention, the method of refinement is preferably grinding.
The invention also preferably screens the non-magnetic fly ash before thinning.
In the present invention, the mesh number of the screen for sieving is preferably 200 meshes, and the sieved part is taken out.
In the invention, the solid-to-liquid ratio of the non-magnetic fly ash to the modifier is preferably 1g: (0.5 to 1.5) ml, more preferably 1g: (0.75 to 1.25) ml, more preferably 1g: 1 ml.
In the invention, the modifier comprises salt and acid, and the solid-to-liquid ratio of the salt to the acid is preferably 1g (10-30) ml, more preferably 1g (15-25) ml, and still more preferably 1g (20 ml).
In the invention, the acid is preferably hydrochloric acid and sulfuric acid, and the volume ratio of the hydrochloric acid to the sulfuric acid is preferably 1: 2-4, and more preferably 1: 3.
In the present invention, the concentration of the hydrochloric acid is preferably 37%, and the concentration of the sulfuric acid is preferably 98%.
In the present invention, the salt is preferably sodium chloride or ammonium fluoride, and more preferably sodium chloride.
The invention utilizes acid and salt to modify the fly ash, which is beneficial to coarsening the surface of the fly ash, increasing the specific surface area of the fly ash, opening the closed pore channel, removing impurities in the channel, increasing the porosity of the fly ash, having stronger adsorption effect on pollutants in wastewater, and simultaneously salt modifier ions adsorbed on the surface of the fly ash can exchange ions with the pollutants in the wastewater, thereby further improving the adsorption effect.
In the present invention, the modification treatment is preferably performed under shaking and stirring conditions.
In the present invention, the time for the modification treatment is preferably 0.5 to 1.5 hours, and more preferably 1 hour.
The modification treatment of the present invention is preferably carried out by microwave treatment after shaking and stirring.
In the invention, the power of the microwave modification treatment is preferably 500-800W, and more preferably 600W; the temperature of the microwave treatment is preferably 50-70 ℃, and further preferably 60 ℃; the time for the microwave treatment is preferably 5-20 min, and more preferably 10 min. The microwave treatment can accelerate the modification process of the modifier to the fly ash, and can also change the characteristics of the fly ash by utilizing the microwave to further modify the fly ash, thereby increasing the adsorption performance of the fly ash.
In the present invention, the microwave treatment is preferably performed in a microwave synthesizer.
In the invention, after the modification treatment, the modified fly ash is preferably dried and refined in sequence to obtain the modified fly ash.
The present invention also preferably performs suction filtration before drying.
In the invention, the drying temperature is preferably 100-110 ℃, and more preferably 105 ℃; the drying time is preferably 0.5-1.5 h, and more preferably 1 h.
In the present invention, the particle size after the thinning is preferably less than 75 micrometers, and more preferably less than 50 micrometers.
In the present invention, the method of refinement is preferably grinding. Grinding can increase the specific surface area of the modified fly ash, so that the reaction contact area becomes large.
The invention mixes the magnetic fly ash and the modified fly ash to prepare the magnetic coagulant.
In the invention, the magnetic fly ash and the modified fly ash are mixed and then preferably sieved by a 200-mesh sieve, and the part under the sieve is the magnetic coagulant.
The invention also provides the magnetic coagulant obtained by the method.
The magnetic coagulant and the preparation method thereof provided by the present invention will be described in detail with reference to the following examples, but they should not be construed as limiting the scope of the present invention.
Example 1
(1) Pretreatment of fly ash
Taking fly ash, putting a magnet block with the thickness of 15 multiplied by 20 multiplied by 2.5cm into the fly ash, stirring, carrying out magnetic separation, collecting the fly ash on the surface of the magnet, namely the magnetic fly ash, and weighing 20g for later use. And (3) sieving the fly ash remaining after magnetic separation with a 200-mesh sieve, weighing 20g of undersize, and grinding to obtain the non-magnetic fly ash with the particle size of less than 75 microns.
(2) Preparation of the modifier
Hydrochloric acid with the concentration of 37% and sulfuric acid with the concentration of 98% are taken and mixed according to the proportion of 1:3 to obtain mixed acid, and 1g of sodium chloride is mixed with 20ml of mixed acid to prepare the modifier.
(3) Modification treatment
And (3) adding the modifier prepared in the step (2) into the non-magnetic fly ash obtained in the step (1), and modifying the non-magnetic fly ash. And (3) oscillating and stirring at normal temperature for reaction for 1h, performing suction filtration after the reaction is finished, then placing the reaction product in an oven for drying at 105 ℃ for 1h, and crushing the dried product to obtain the modified fly ash. The particle size of the modified fly ash prepared in this example is 50 to 75 microns.
(4) Preparation of magnetic coagulant
And (3) mixing the modified fly ash prepared in the step (3) with the magnetic fly ash obtained in the step (1), sieving by a 200-mesh sieve, and taking undersize products to obtain the magnetic coagulant.
The magnetic coagulant prepared by the invention is used for treating sewage. The initial COD of the taken sewage is 319mg/L, the pH of the sewage is adjusted to 9, and a magnetic coagulant is added, wherein the dosage ratio of the sewage to the magnetic coagulant is 2g/100 ml. After the magnetic coagulant is added into the sewage for adsorption oscillation for 1 hour, a 6B-80 type water quality COD rapid determinator is adopted for determination, the COD of the treated sewage is 55.5mg/L, and the removal rate of the COD is 82.6 percent at the moment.
Example 2
(1) Pretreatment of fly ash
Taking fly ash, putting a magnet block with the thickness of 15 multiplied by 20 multiplied by 2.5cm into the fly ash, stirring, carrying out magnetic separation, collecting the fly ash on the surface of the magnet, namely the magnetic fly ash, and weighing 20g for later use. And (3) sieving the fly ash remaining after magnetic separation with a 200-mesh sieve, weighing 20g of undersize, and grinding to obtain the non-magnetic fly ash with the particle size of 75 microns.
(2) Preparation of the modifier
Hydrochloric acid and sulfuric acid with the concentrations of 37% and 98% respectively are taken and mixed according to the proportion of 1:3 to obtain mixed acid, and 1g of ammonium fluoride is mixed with 20ml of mixed acid to prepare the modifier.
(3) Modification treatment
And (3) adding the modifier prepared in the step (2) into the non-magnetic fly ash obtained in the step (1), and modifying the non-magnetic fly ash. Stirring and reacting for 1h at normal temperature, then placing into a microwave synthesizer, and carrying out microwave for 10min at 600W and 60 ℃. And after the reaction is finished, carrying out suction filtration, then placing the mixture in an oven to be dried for 1h at the temperature of 100 ℃, and crushing the dried mixture to obtain the modified fly ash. The particle size of the modified fly ash prepared in this example is 50 to 75 microns.
(4) Preparation of magnetic coagulant
And (3) mixing the modified fly ash prepared in the step (3) with the magnetic fly ash obtained in the step (1), sieving by a 200-mesh sieve, and taking undersize products to obtain the magnetic coagulant.
The magnetic coagulant prepared by the invention is used for treating sewage. The initial COD of the taken sewage is 319mg/L, the pH of the sewage is adjusted to 9, and a magnetic coagulant is added, wherein the dosage ratio of the sewage to the magnetic coagulant is 2g/100 ml. After the magnetic coagulant is added into the sewage for adsorption oscillation for 1 hour, a 6B-80 type water quality COD rapid determinator is adopted for determination, the COD of the treated sewage is 51.6mg/L, and the removal rate of the COD is 83.8 percent.
From the above embodiments, the present invention provides a magnetic coagulant and a preparation method thereof. The magnetic coagulant can remove substances such as colloids, suspended matters, organic pollutants and the like in sewage, thereby reducing the content of COD (chemical oxygen demand) in the water and simultaneously solving the problems of overhigh magnetic seed production cost, complex process flow and the like in the magnetic coagulation sedimentation technology.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.

Claims (9)

1. The preparation method of the magnetic coagulant is characterized by comprising the following steps:
(1) sorting fly ash into magnetic fly ash and non-magnetic fly ash;
(2) modifying the non-magnetic fly ash by using a modifier to obtain modified fly ash;
(3) and mixing the magnetic fly ash and the modified fly ash to prepare the magnetic coagulant.
2. The method for preparing a magnetic coagulant according to claim 1, wherein the nonmagnetic fly ash is refined and then subjected to modification treatment.
3. The method for preparing a magnetic coagulant according to claim 2 wherein the particle size of the non-magnetic fly ash after refining is less than 75 microns.
4. The method for preparing a magnetic coagulant according to claim 1, wherein the solid-to-liquid ratio of the non-magnetic fly ash to the modifier is 1g: (0.5-1.5) ml.
5. The method for preparing a magnetic coagulant according to claim 1 or 4, wherein the modifier comprises salt and acid, and the solid-to-liquid ratio of the salt to the acid is 1g (10-30) ml.
6. The method for preparing a magnetic coagulant according to claim 5, wherein the acid comprises hydrochloric acid and sulfuric acid, the volume ratio of the hydrochloric acid to the sulfuric acid is 1 (2-4), the concentration of the hydrochloric acid is 37%, and the concentration of the sulfuric acid is 98%.
7. A process for the preparation of a magnetic coagulant as claimed in claim 5 where the salt is sodium chloride or ammonium fluoride.
8. The method for preparing a magnetic coagulant according to claim 1, wherein the modified fly ash is prepared by sequentially drying and refining after the modification treatment.
9. A magnetic coagulant produced by the process of any one of claims 1 to 8.
CN202010197441.0A 2020-03-19 2020-03-19 Magnetic coagulant and preparation method thereof Pending CN111268773A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113735234A (en) * 2021-09-24 2021-12-03 华北电力大学(保定) Fly ash-based magnetic coagulant for treating chromium-containing wastewater, preparation method, application and regeneration method

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113735234A (en) * 2021-09-24 2021-12-03 华北电力大学(保定) Fly ash-based magnetic coagulant for treating chromium-containing wastewater, preparation method, application and regeneration method

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