CN108996647B - Preparation method of magnetic composite flocculant, product and application thereof - Google Patents
Preparation method of magnetic composite flocculant, product and application thereof Download PDFInfo
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- CN108996647B CN108996647B CN201810792565.6A CN201810792565A CN108996647B CN 108996647 B CN108996647 B CN 108996647B CN 201810792565 A CN201810792565 A CN 201810792565A CN 108996647 B CN108996647 B CN 108996647B
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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
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/54—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using organic material
- C02F1/56—Macromolecular compounds
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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
- C02F1/48—Treatment of water, waste water, or sewage with magnetic or electric fields
- C02F1/488—Treatment of water, waste water, or sewage with magnetic or electric fields for separation of magnetic materials, e.g. magnetic flocculation
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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
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/5236—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents
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Abstract
The invention relates to a preparation method of a magnetic composite flocculant, a product and an application thereof, wherein chitosan and acrylamide are subjected to polymerization reaction to form a copolymer composite flocculant, and ferroferric oxide is compounded on a copolymer through a gel reaction. The product obtained by the method of the invention utilizes the magnetic separation effect of ferroferric oxide to accelerate the sedimentation speed of the flocculating constituent, integrates the adsorption capacity of chitosan to heavy metal ions in wastewater and the adsorption capacity of polyacrylamide to refractory organic matters, overcomes many defects of a single flocculating constituent, has wide application range, can adsorb heavy metal ions and refractory organic matters in wastewater simultaneously, adds medicine once, reduces secondary pollution, can accelerate the sedimentation speed of the flocculating constituent in the presence of a magnetic field, and has the advantages of good flocculation effect, high sedimentation speed, simple preparation, safety, environmental protection and the like.
Description
Technical Field
The invention relates to the field of wastewater treatment, in particular to a preparation method of a magnetic composite flocculant, a product and application thereof.
Background
At present, the problem of water pollution is becoming more serious, the problem of water treatment is becoming more and more serious, and various methods for water treatment, such as adsorption, chemical oxidation, electrodialysis, biochemistry, ion exchange and the like, but the flocculation precipitation method is still a more effective and lower-cost pretreatment method.
Polyacrylamide is a macromolecular compound with relatively active chemical properties, and has long molecular chains, and the long chains with large magnitude orders have huge adsorption surface area in water, so the polyacrylamide has good flocculation effect, can bridge among particles by utilizing the long chains to form large-particle floccules, and has high settling speed.
The chitosan is a linear molecule, and the molecular chain contains a reactive group-NH2OH, which in acidic solution forms a cationic polymer with a high charge densityElectrolyte, which shows good complexing and flocculating properties, can react with many metal ions (such as Hg)2+、Ni2+、Cu2+、Pb2+、Ca2+、Ag+Etc.) to form stable chelate, so that the chitosan has unique advantages of using as heavy metal ion complexing agent in waste water treatment, no toxicity, no secondary pollution and good biodegradability. However, chitosan has the disadvantages of small molecular weight, poor bridging capability and particularly high cost. The chitosan and acrylamide are grafted and copolymerized to be used as the flocculating agent, so that the cost is reduced, and the defects of small molecular weight and poor bridging capability of single chitosan are overcome. Meanwhile, the magnetic separation of ferroferric oxide can be utilized to quickly separate flocculate from water, thereby accelerating the speed of wastewater treatment.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a preparation method of a magnetic composite flocculant.
Yet another object of the present invention is to: provides a magnetic composite flocculant product prepared by the method.
Yet another object of the present invention is to: provides an application of the product.
The purpose of the invention is realized by the following scheme: a preparation method of a magnetic composite flocculant comprises the steps of performing polymerization reaction on chitosan and acrylamide to form a copolymer composite flocculant, simultaneously compounding ferroferric oxide on a copolymer through a gel reaction, and accelerating the sedimentation speed of a flocculating constituent by utilizing the magnetic separation effect of the ferroferric oxide, and at least comprises the following preparation steps:
(1) preparation of chitosan and acrylamide copolymer
Weighing chitosan, putting the chitosan into a three-neck flask, and adding acetic acid aqueous solution for dissolving; then adding acrylamide under stirring, wherein the mass ratio of ammonium persulfate to chitosan to acrylamide is 1: (4-10): (30-50), continuously stirring until the chitosan and the acrylamide are completely dissolved, heating to a certain temperature of 70-90 ℃, adding ammonium persulfate, and reacting to obtain a chitosan and acrylamide copolymer solution;
(2) preparation of ferroferric oxide nanoparticles
Weighing ferric chloride and ferrous chloride, dissolving in water to prepare a mixed solution, wherein the mass ratio of the ferric chloride to the ferrous chloride to the distilled water is 1: (2-5): (50-80), slowly dropping ammonia water into the mixed solution under stirring, adjusting the pH to 6-7, starting to generate a large amount of black ferroferric oxide nanoparticles, continuously dropping ammonia water until the hydrolysis is complete, aging, separating the prepared particles from the solution, and washing with distilled water to obtain the ferroferric oxide nanoparticles;
(3) composition of copolymer and ferroferric oxide nano-particles
Dispersing ferroferric oxide nanoparticles into a copolymer solution, wherein the molar concentration ratio of the copolymer to the ferroferric oxide to the sodium tripolyphosphate is (20-30): (20-30): 1; adjusting the pH value of the solution, adding sodium tripolyphosphate while stirring to perform a gel reaction, and obtaining the copolymer and ferroferric oxide nanoparticle composite flocculant.
The invention utilizes the magnetic separation effect of ferroferric oxide to accelerate the sedimentation speed of the flocculating constituent, and integrates the adsorption capacity of chitosan to heavy metal ions in wastewater and the adsorption capacity of polyacrylamide to refractory organic matters.
On the basis of the scheme, in the step (1): the mass fractions of the chitosan and the acetic acid are both (3% -5%); the time of the copolymerization reaction is as follows: 3-5 h.
In the step (2): the technological conditions of the aging reaction are as follows: aging for 1-2 h at 50-90 ℃.
In the step (3): the pH range is 6-7.
The invention provides a magnetic composite flocculant obtained by any one of the preparation methods.
The invention also provides an application of the magnetic composite flocculant in wastewater treatment.
Compared with the prior art, the composite flocculant overcomes many defects of a single flocculant, has a wide application range, can adsorb heavy metal ions and refractory organic matters in wastewater simultaneously, can be added with drugs once, reduces secondary pollution, can accelerate the sedimentation speed of a flocculating body in the presence of a magnetic field, and has the advantages of good flocculation effect, high sedimentation speed, simplicity in preparation, safety, environmental protection and the like.
Detailed Description
The present invention will be described in detail with reference to specific examples.
Example 1
Preparing a mixed solution from ferric chloride, ferrous chloride and distilled water according to the mass ratio of 1:2:50, slowly dropwise adding ammonia water into the mixed solution under stirring, starting to generate a large amount of black ferroferric oxide nano-particles when the pH value reaches 6, and continuously dropwise adding ammonia water until the hydrolysis is nearly complete; aging at 50 deg.C for 2 hr, separating the obtained particles from the solution, and washing with distilled water to obtain ferroferric oxide nanoparticles;
weighing chitosan, adding acetic acid water solution into a three-neck flask for dissolving, wherein the mass fractions of the chitosan and the acetic acid in the water are both 3%; then adding acrylamide under stirring, continuously stirring until the acrylamide is completely dissolved, heating to 70 ℃, and adding ammonium persulfate, wherein the mass ratio of the ammonium persulfate to the chitosan to the acrylamide is 1:4: 30, reacting for 5 hours to obtain a chitosan and acrylamide copolymer;
dispersing ferroferric oxide nano particles into a copolymer solution, adjusting the pH value of the solution to 6, stirring, and then adding sodium tripolyphosphate, wherein the molar concentration ratio of the copolymer to the ferroferric oxide to the sodium tripolyphosphate is 20: 20: 1, obtaining a flocculant compounded by a copolymer and ferroferric oxide nano particles after a gel reaction;
the prepared ozone catalyst is used for treating the wastewater of a certain steel plant, the initial COD value of the steel wastewater is 530 mg/L, and the removal rate of the COD is 57.1 percent after 5 minutes of flocculation and precipitation.
Example 2
Preparing a mixed solution from ferric chloride, ferrous chloride and distilled water according to a mass ratio of 1:3:60, slowly dropwise adding ammonia water into the mixed solution under stirring, starting to generate a large amount of black ferroferric oxide nano-particles when the pH value reaches 7, and continuously dropwise adding ammonia water until the hydrolysis is nearly complete; aging at 60 deg.C for 1.5h, separating the obtained particles from the solution, and washing with distilled water to obtain ferroferric oxide nanoparticles;
weighing chitosan, putting the chitosan into a three-neck flask, adding an acetic acid aqueous solution for dissolving, wherein the mass fractions of the chitosan and the acetic acid in the water are both 4%; then adding acrylamide under stirring, continuously stirring until the acrylamide is completely dissolved, heating to 80 ℃, and adding ammonium persulfate, wherein the mass ratio of the ammonium persulfate to the chitosan to the acrylamide is 1:5: 35, reacting for 4 hours to obtain a chitosan and acrylamide copolymer;
dispersing ferroferric oxide nano particles into a copolymer solution, adjusting the pH value of the solution to 7, stirring, and then adding sodium tripolyphosphate, wherein the mass concentration ratio of the copolymer to the ferroferric oxide to the sodium tripolyphosphate is 25: 25: 1, obtaining a flocculant compounded by a copolymer and ferroferric oxide nano particles after a gel reaction;
the prepared ozone catalyst is used for treating the wastewater of a certain steel plant, the initial COD value of the steel wastewater is 530 mg/L, and the removal rate of the COD is 54.5 percent after 5 minutes of flocculation and precipitation.
Example 3
Preparing a mixed solution from ferric chloride, ferrous chloride and distilled water according to a mass ratio of 1:4:70, slowly dropwise adding ammonia water into the mixed solution under stirring, starting to generate a large amount of black ferroferric oxide nano-particles when the pH value reaches 6, and continuously dropwise adding ammonia water until the hydrolysis is nearly complete; aging at 70 deg.C for 1.5h, separating the obtained particles from the solution, and washing with distilled water to obtain ferroferric oxide nanoparticles;
weighing chitosan, adding acetic acid water solution into a three-neck flask for dissolving, wherein the mass fractions of the chitosan and the acetic acid in the water are both 5%; then adding acrylamide under stirring, continuously stirring until the acrylamide is completely dissolved, heating to 90 ℃, and adding ammonium persulfate, wherein the mass ratio of the ammonium persulfate to the chitosan to the acrylamide is 1: 6: 40, reacting for 3 hours to obtain a copolymer of chitosan and acrylamide;
dispersing ferroferric oxide nano particles into a copolymer solution, adjusting the pH value of the solution to 6, stirring, and then adding sodium tripolyphosphate, wherein the mass concentration ratio of the copolymer to the ferroferric oxide to the sodium tripolyphosphate is 30: 30: 1, obtaining a flocculant compounded by a copolymer and ferroferric oxide nano particles after a gel reaction;
the prepared ozone catalyst is used for treating the wastewater of a certain steel plant, the initial COD value of the steel wastewater is 530 mg/L, and the removal rate of the COD is 59.3 percent after 5 minutes of flocculation precipitation.
Example 4
Preparing a mixed solution from ferric chloride, ferrous chloride and distilled water according to a mass ratio of 1:5:80, slowly dropwise adding ammonia water into the mixed solution under stirring, starting to generate a large amount of black ferroferric oxide nano-particles when the pH value reaches 7, and continuously dropwise adding ammonia water until the hydrolysis is nearly complete; aging at 80 deg.C for 1h, separating the obtained particles from the solution, and washing with distilled water to obtain ferroferric oxide nanoparticles;
weighing chitosan, adding acetic acid water solution into a three-neck flask for dissolving, wherein the mass fractions of the chitosan and the acetic acid in the water are both 3%; then adding acrylamide under stirring, continuously stirring until the acrylamide is completely dissolved, heating to 90 ℃, and adding ammonium persulfate, wherein the mass ratio of the ammonium persulfate to the chitosan to the acrylamide is 1: 8: 45, reacting for 3 hours to obtain a copolymer of chitosan and acrylamide;
dispersing ferroferric oxide nano particles into a copolymer solution, adjusting the pH value of the solution to 7, stirring, and then adding sodium tripolyphosphate, wherein the mass concentration ratio of the copolymer to the ferroferric oxide to the sodium tripolyphosphate is 20: 25: 1, obtaining a flocculant compounded by a copolymer and ferroferric oxide nano particles after a gel reaction;
the prepared ozone catalyst is used for treating the wastewater of a certain steel plant, the initial COD value of the steel wastewater is 530 mg/L, and the removal rate of the COD is 56.9 percent after 5 minutes of flocculation precipitation.
Example 5
Preparing a mixed solution from ferric chloride, ferrous chloride and distilled water according to a mass ratio of 1:3:80, slowly dropwise adding ammonia water into the mixed solution under stirring, starting to generate a large amount of black ferroferric oxide nano-particles when the pH value reaches 6, and continuously dropwise adding ammonia water until the hydrolysis is nearly complete; aging at 90 deg.C for 1h, separating the obtained particles from the solution, and washing with distilled water to obtain ferroferric oxide nanoparticles;
weighing chitosan, adding acetic acid water solution into a three-neck flask for dissolving, wherein the mass fractions of the chitosan and the acetic acid in the water are both 5%; then adding acrylamide under stirring, continuously stirring until the acrylamide is completely dissolved, heating to 70 ℃, and adding ammonium persulfate, wherein the mass ratio of the ammonium persulfate to the chitosan to the acrylamide is 1: 10: 50, reacting for 5 hours to obtain a chitosan and acrylamide copolymer;
dispersing ferroferric oxide nano particles into a copolymer solution, adjusting the pH value of the solution to 6, stirring, and then adding sodium tripolyphosphate, wherein the mass concentration ratio of the copolymer to the ferroferric oxide to the sodium tripolyphosphate is 25: 20: 1, obtaining a flocculant compounded by a copolymer and ferroferric oxide nano particles after a gel reaction;
the prepared ozone catalyst is used for treating the wastewater of a certain steel plant, the initial COD value of the steel wastewater is 530 mg/L, and the removal rate of the COD is 58.8 percent after 5 minutes of flocculation and precipitation.
Claims (5)
1. A preparation method of a magnetic composite flocculant is characterized in that chitosan and acrylamide are subjected to polymerization reaction to form a copolymer composite flocculant, ferroferric oxide is compounded on the copolymer through a gel reaction, and the sedimentation speed of a flocculating body is accelerated by utilizing the magnetic separation effect of the ferroferric oxide, and the preparation method at least comprises the following preparation steps:
(1) preparation of chitosan and acrylamide copolymer:
weighing chitosan, putting the chitosan into a three-neck flask, and dissolving the chitosan in an acetic acid aqueous solution; then adding acrylamide under stirring, continuously stirring until the acrylamide is completely dissolved, heating to 70-90 ℃, and adding ammonium persulfate, wherein the mass ratio of the ammonium persulfate to the chitosan to the acrylamide is 1: (4-10): (30-50), carrying out copolymerization reaction to obtain a chitosan and acrylamide copolymer solution;
(2) preparing ferroferric oxide nanoparticles:
weighing ferric chloride and ferrous chloride, dissolving in water to prepare a mixed solution, wherein the mass ratio of the ferric chloride to the ferrous chloride to the distilled water is 1: (2-5): (50-80), slowly dropping ammonia water into the mixed solution under stirring, adjusting the pH to 6-7, starting to generate a large amount of black ferroferric oxide nanoparticles, continuously dropping ammonia water until the hydrolysis is complete, aging, separating the prepared particles from the solution, and washing with distilled water to obtain the ferroferric oxide nanoparticles;
(3) compounding the copolymer with ferroferric oxide nanoparticles:
dispersing ferroferric oxide nanoparticles into a copolymer solution, wherein the molar concentration ratio of the copolymer to the ferroferric oxide to the sodium tripolyphosphate is (20-30): (20-30): 1; adjusting the pH value of the solution, adding sodium tripolyphosphate while stirring to perform a gel reaction, and obtaining a flocculant compounded by the copolymer and the ferroferric oxide nanoparticles; wherein the content of the first and second substances,
in the step (1): the mass fractions of the chitosan and the acetic acid are both 3-5%, and the polymerization reaction is carried out for 3-5 h;
in the step (2): the technological conditions of the aging reaction are as follows: reacting at 50-90 deg.C for 1-2 h.
2. The method for preparing a magnetic composite flocculant according to claim 1, wherein in the step (2): the pH range is 6-7.
3. The method for preparing a magnetic composite flocculant according to claim 1, wherein in the step (3): the pH range is 6-7.
4. A magnetic composite flocculant, characterized by being obtained by the production method according to any one of claims 1 to 3.
5. Use of the magnetic composite flocculant according to claim 4 in wastewater treatment.
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| CN110294858B (en) * | 2019-06-25 | 2022-01-25 | 常州大学 | Hydrogel sensing membrane capable of sequentially detecting anions, metal cations and dye molecules and preparation method thereof |
| CN111533284A (en) * | 2020-06-23 | 2020-08-14 | 桂虎 | Method for microbial ecological restoration treatment |
| CN112724317A (en) * | 2020-12-29 | 2021-04-30 | 科之杰新材料集团有限公司 | Preparation method of modified chitosan, flocculant, preparation method of flocculant and testing method of flocculant |
| CN114195208A (en) * | 2021-12-09 | 2022-03-18 | 陕西关天易景科技有限公司 | Composite sewage treatment agent and preparation method thereof |
| CN114873705B (en) * | 2022-05-19 | 2023-09-01 | 中国计量大学 | Magnetic modified carboxymethyl chitosan compound flocculant, preparation method thereof and application thereof in synchronously removing heavy metal antimony and chromium in printing and dyeing wastewater |
| CN115340157B (en) * | 2022-09-02 | 2024-03-26 | 浙江华蓝环境科技有限公司 | Modified chitosan-based magnetic flocculant and preparation method and application thereof |
| CN116987526B (en) * | 2023-08-30 | 2024-01-26 | 石家庄环腾能源科技有限公司 | Method for reducing total metal content of industrial mixed oil by demulsification flocculant |
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| CN103566906A (en) * | 2013-11-05 | 2014-02-12 | 河海大学 | Magnetic chitosan nanoparticle adsorbent, and preparation method and application thereof |
| CN104448347A (en) * | 2014-12-01 | 2015-03-25 | 哈尔滨理工大学 | Method for constructing annular chitosan microgel |
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| CN103566906A (en) * | 2013-11-05 | 2014-02-12 | 河海大学 | Magnetic chitosan nanoparticle adsorbent, and preparation method and application thereof |
| CN104448347A (en) * | 2014-12-01 | 2015-03-25 | 哈尔滨理工大学 | Method for constructing annular chitosan microgel |
| CN105367715A (en) * | 2015-12-16 | 2016-03-02 | 杭州电子科技大学 | Preparing method for amphiphilic positive ion and chitosan based magnetic flocculating agent |
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