CN108996647A - Preparation method of magnetic coupling flocculant and products thereof and application - Google Patents

Preparation method of magnetic coupling flocculant and products thereof and application Download PDF

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Publication number
CN108996647A
CN108996647A CN201810792565.6A CN201810792565A CN108996647A CN 108996647 A CN108996647 A CN 108996647A CN 201810792565 A CN201810792565 A CN 201810792565A CN 108996647 A CN108996647 A CN 108996647A
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preparation
copolymer
chitosan
flocculant
oxide nano
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CN108996647B (en
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何丹农
代卫国
童琴
邓洁
赵昆峰
金彩虹
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Shanghai National Engineering Research Center for Nanotechnology Co Ltd
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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
    • C02F1/52Treatment 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
    • 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
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/52Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
    • C02F1/5236Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents

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  • Chemical & Material Sciences (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)
  • Inorganic Chemistry (AREA)
  • Analytical Chemistry (AREA)
  • Separation Of Suspended Particles By Flocculating Agents (AREA)

Abstract

The present invention relates to preparation methods of a kind of magnetic coupling flocculant and products thereof and application, it reacts chitosan to form copolymer composite flocculation agent with acrylamide polymerization, ferroso-ferric oxide is combined on copolymer by gel reaction simultaneously, preparation and copolymer and ferroferric oxide nano granules including at least the preparation of ferroferric oxide nano granules, chitosan and acrylamide copolymer it is compound.The product that the method for the present invention obtains, accelerate the sinking speed of floccule body using the magnetic separation effect of ferroso-ferric oxide, adsorption capacity and polyacrylamide of the chitosan to heavy metal ions in wastewater roll into one to the adsorption capacity of hardly degraded organic substance, overcome many deficiencies of single flocculant, wide adaptation range, heavy metal ions in wastewater and hardly degraded organic substance can be adsorbed simultaneously, disposable dosing, reduce secondary pollution, it can accelerate floc settlement speed in the presence of magnetic field, have flocculating effect good, sinking speed is fast, the advantages that preparation is simple, safety and environmental protection.

Description

Preparation method of magnetic coupling flocculant and products thereof and application
Technical field
The present invention relates to field of waste water treatment, its product of the preparation method of specifically a kind of magnetic coupling flocculant and answer With.
Background technique
There are many ways to water pollution problems is on the rise at present, and water treatment problems also become increasingly severeer, water process, Such as absorption, chemical oxidation, electrodialysis, biochemistry, ion exchange, but flocculent precipitation are still a kind of more effective and cost is relatively low Preprocess method.
Polyacrylamide is a kind of high-molecular compound that chemical property is more active, because it has very long strand, greatly The long-chain of the order of magnitude has huge adsorption surface area in water, therefore flocculation is good, can be built bridge between particles using long-chain, shape At the floccule body of bulky grain, sinking speed is fast.
Chitosan is a kind of linear molecule, contains reactive group-NH in strand2,-OH, in an acidic solution can shape At the cationic polyelectrolyte of high charge density, good complex performance and flocculating property are shown, it can be with many metal ions (such as Hg2+、Ni2+、Cu2+、Pb2+、Ca2+、Ag+Deng) stable chelate is formed, so chitosan is used as heavy metal in the treatment of waste water Ionic complexing agent has unique advantage, nontoxic, does not generate secondary pollution, biological degradability is good.But there are molecular weight for chitosan Small, bridge formation ability difference, particularly disadvantage at high cost.And it is reduced using chitosan and acrylic amide graft copolymerization as flocculant Cost solves that independent molecular weight of chitosan is small, disadvantage of bridge formation ability difference again.Made simultaneously using the magnetic separation of ferroso-ferric oxide With that flocculate can be made to be rapidly separated with water, accelerate the rate of wastewater treatment.
Summary of the invention
In view of the deficiencies of the prior art, it is an object of that present invention to provide a kind of preparation methods of magnetic coupling flocculant.
Another object of the present invention is: providing a kind of magnetic coupling flocculant product of above method preparation.
Another object of the present invention is to: a kind of application of the said goods is provided.
The object of the invention is realized by following proposal: a kind of preparation method of magnetic coupling flocculant, by chitosan and third Acrylamide polymerization reaction forms copolymer composite flocculation agent, while ferroso-ferric oxide is combined to copolymer by gel reaction On, accelerate the sinking speed of floccule body using the magnetic separation effect of ferroso-ferric oxide, include at least following preparation step:
(1) preparation of chitosan and acrylamide copolymer
Chitosan is weighed in three-necked flask, acetic acid aqueous solution dissolution is added;Then acrylamide, persulfuric acid are added under stiring The mass ratio of ammonium, chitosan and acrylamide is 1:(4 ~ 10): (30-50) is continued stirring until after being completely dissolved, it is warming up to 70 ~ Certain temperature at 90 DEG C, is added ammonium persulfate, and reaction obtains chitosan and acrylamide copolymer solution;
(2) preparation of ferroferric oxide nano granules
Weigh that iron chloride, frerrous chloride are soluble in water to be made into mixed solution, iron chloride, frerrous chloride, distilled water mass ratio be 1:(2 ~ 5): (50 ~ 80) are slowly dropped in mixed solution with ammonium hydroxide under stiring, are adjusted after pH reaches 6-7 and are started to generate largely Black ferroferric oxide nano particle, continue ammonium hydroxide to hydrolysis is added dropwise and tend to completely, after ageing, then by particle obtained from molten It separates, is washed with distilled water to get ferroferric oxide nano granules are arrived in liquid;
(3) copolymer and ferroferric oxide nano granules is compound
Disperse ferroferric oxide nano granules in copolymer solution, copolymer, ferroso-ferric oxide, sodium tripolyphosphate mole Concentration ratio is (20 ~ 30): (20 ~ 30): 1;PH value of solution is adjusted, sodium tripolyphosphate is added with stirring and gel reaction occurs to get arriving Copolymer and the compound flocculant of ferroferric oxide nano granules.
The present invention accelerates the sinking speed of floccule body using the magnetic separation effect of ferroso-ferric oxide, by chitosan to weight in waste water The adsorption capacity and polyacrylamide of metal ion roll into one to the adsorption capacity of hardly degraded organic substance.
On the basis of above scheme, in step (1): the mass fraction of chitosan and acetic acid is (3% ~ 5%);Combined polymerization is anti- The time answered are as follows: 3 ~ 5h.
In step (2): being aged the process conditions of reaction are as follows: be aged 1 ~ 2h at 50 ~ 90 DEG C.
In step (3): pH range is 6 ~ 7.
The present invention provides a kind of magnetic coupling flocculant, is obtained according to any of the above-described preparation method.
The present invention also provides a kind of application of magnetic coupling flocculant in the treatment of waste water.
Compared with prior art, the present invention composite flocculation agent overcomes many deficiencies of single flocculant, wide adaptation range, Heavy metal ions in wastewater and hardly degraded organic substance can be adsorbed simultaneously, and disposable dosing reduces secondary pollution, in the presence of magnetic field It can accelerate the sinking speed of floccule body, have flocculating effect good, the advantages that sinking speed is fast, and preparation is simple, safety and environmental protection.
Specific embodiment
The present invention is described in detail combined with specific embodiments below.
Embodiment 1
It is in mass ratio that 1:2:50 is made into mixed solution by iron chloride, frerrous chloride and distilled water, it is under stiring that ammonium hydroxide is slow It is added drop-wise in mixed solution, starts to generate a large amount of black ferroferric oxide nano particle after pH reaches 6, continue that ammonium hydroxide is added dropwise Tend to be complete to hydrolysis;It is aged 2h at 50 DEG C, then particle obtained is separated from solution, is washed with distilled water, i.e., Obtain ferroferric oxide nano granules;
Chitosan is weighed in three-necked flask, acetic acid aqueous solution dissolution is added, the mass fraction of chitosan and acetic acid in water is equal It is 3%;Then acrylamide is added under stiring, continues stirring until after being completely dissolved, is warming up to 70 DEG C, ammonium persulfate, mistake is added The mass ratio of ammonium sulfate, chitosan and acrylamide is 1:4:30, is copolymerized after reacting 5h to get to chitosan and acrylamide Object;
It disperses ferroferric oxide nano granules in copolymer solution, adjustment pH value of solution to 6, then stirring is lower to be added trimerization phosphorus Sour sodium, copolymer, ferroso-ferric oxide, sodium tripolyphosphate molar concentration rate be 20:20:1, occur gel reaction after i.e. be total to Polymers and the compound flocculant of ferroferric oxide nano granules;
Prepared ozone catalyst handles certain steel plant wastewater, and the initial COD value of steel wastewater is 530 mg/L, warp 5 minutes flocculation sedimentations are crossed, the removal rate of COD is 57.1%.
Embodiment 2
It is in mass ratio that 1:3:60 is made into mixed solution by iron chloride, frerrous chloride and distilled water, it is under stiring that ammonium hydroxide is slow It is added drop-wise in mixed solution, starts to generate a large amount of black ferroferric oxide nano particle after pH reaches 7, continue that ammonium hydroxide is added dropwise Tend to be complete to hydrolysis;It is aged 1.5h at 60 DEG C, then particle obtained is separated from solution, is washed with distilled water, Obtain ferroferric oxide nano granules;
Chitosan is weighed in three-necked flask, acetic acid aqueous solution dissolution is added, the mass fraction of chitosan and acetic acid in water is equal It is 4%;Then acrylamide is added under stiring, continues stirring until after being completely dissolved, is warming up to 80 DEG C, ammonium persulfate, mistake is added The mass ratio of ammonium sulfate, chitosan and acrylamide is 1:5:35, is copolymerized after reacting 4h to get to chitosan and acrylamide Object;
It disperses ferroferric oxide nano granules in copolymer solution, adjustment pH value of solution to 7, then stirring is lower to be added trimerization phosphorus Sour sodium, copolymer, ferroso-ferric oxide, sodium tripolyphosphate substance withdrawl syndrome ratio be 25:25:1, occur gel reaction after to obtain the final product To copolymer and the compound flocculant of ferroferric oxide nano granules;
Prepared ozone catalyst handles certain steel plant wastewater, and the initial COD value of steel wastewater is 530 mg/L, warp 5 minutes flocculation sedimentations are crossed, the removal rate of COD is 54.5%.
Embodiment 3
It is in mass ratio that 1:4:70 is made into mixed solution by iron chloride, frerrous chloride and distilled water, it is under stiring that ammonium hydroxide is slow It is added drop-wise in mixed solution, starts to generate a large amount of black ferroferric oxide nano particle after pH reaches 6, continue that ammonium hydroxide is added dropwise Tend to be complete to hydrolysis;It is aged 1.5h at 70 DEG C, then particle obtained is separated from solution, is washed with distilled water, Obtain ferroferric oxide nano granules;
Chitosan is weighed in three-necked flask, acetic acid aqueous solution dissolution is added, the mass fraction of chitosan and acetic acid in water is equal It is 5%;Then acrylamide is added under stiring, continues stirring until after being completely dissolved, is warming up to 90 DEG C, ammonium persulfate, mistake is added The mass ratio of ammonium sulfate, chitosan and acrylamide is 1:6:40, is copolymerized after reacting 3h to get to chitosan and acrylamide Object;
It disperses ferroferric oxide nano granules in copolymer solution, adjustment pH value of solution to 6, then stirring is lower to be added trimerization phosphorus Sour sodium, copolymer, ferroso-ferric oxide, sodium tripolyphosphate substance withdrawl syndrome ratio be 30:30:1, occur gel reaction after to obtain the final product To copolymer and the compound flocculant of ferroferric oxide nano granules;
Prepared ozone catalyst handles certain steel plant wastewater, and the initial COD value of steel wastewater is 530 mg/L, warp 5 minutes flocculation sedimentations are crossed, the removal rate of COD is 59.3%.
Embodiment 4
It is in mass ratio that 1:5:80 is made into mixed solution by iron chloride, frerrous chloride and distilled water, it is under stiring that ammonium hydroxide is slow It is added drop-wise in mixed solution, starts to generate a large amount of black ferroferric oxide nano particle after pH reaches 7, continue that ammonium hydroxide is added dropwise Tend to be complete to hydrolysis;It is aged 1h at 80 DEG C, then particle obtained is separated from solution, is washed with distilled water, i.e., Obtain ferroferric oxide nano granules;
Chitosan is weighed in three-necked flask, acetic acid aqueous solution dissolution is added, the mass fraction of chitosan and acetic acid in water is equal It is 3%;Then acrylamide is added under stiring, continues stirring until after being completely dissolved, is warming up to 90 DEG C, ammonium persulfate, mistake is added The mass ratio of ammonium sulfate, chitosan and acrylamide is 1:8:45, is copolymerized after reacting 3h to get to chitosan and acrylamide Object;
It disperses ferroferric oxide nano granules in copolymer solution, adjustment pH value of solution to 7, then stirring is lower to be added trimerization phosphorus Sour sodium, copolymer, ferroso-ferric oxide, sodium tripolyphosphate substance withdrawl syndrome ratio be 20:25:1, occur gel reaction after to obtain the final product To copolymer and the compound flocculant of ferroferric oxide nano granules;
Prepared ozone catalyst handles certain steel plant wastewater, and the initial COD value of steel wastewater is 530 mg/L, warp 5 minutes flocculation sedimentations are crossed, the removal rate of COD is 56.9%.
Embodiment 5
It is in mass ratio that 1:3:80 is made into mixed solution by iron chloride, frerrous chloride and distilled water, it is under stiring that ammonium hydroxide is slow It is added drop-wise in mixed solution, starts to generate a large amount of black ferroferric oxide nano particle after pH reaches 6, continue that ammonium hydroxide is added dropwise Tend to be complete to hydrolysis;It is aged 1h at 90 DEG C, then particle obtained is separated from solution, is washed with distilled water, i.e., Obtain ferroferric oxide nano granules;
Chitosan is weighed in three-necked flask, acetic acid aqueous solution dissolution is added, the mass fraction of chitosan and acetic acid in water is equal It is 5%;Then acrylamide is added under stiring, continues stirring until after being completely dissolved, is warming up to 70 DEG C, ammonium persulfate, mistake is added The mass ratio of ammonium sulfate, chitosan and acrylamide is 1:10:50, is copolymerized after reacting 5h to get to chitosan and acrylamide Object;
It disperses ferroferric oxide nano granules in copolymer solution, adjustment pH value of solution to 6, then stirring is lower to be added trimerization phosphorus Sour sodium, copolymer, ferroso-ferric oxide, sodium tripolyphosphate substance withdrawl syndrome ratio be 25:20:1, occur gel reaction after to obtain the final product To copolymer and the compound flocculant of ferroferric oxide nano granules;
Prepared ozone catalyst handles certain steel plant wastewater, and the initial COD value of steel wastewater is 530 mg/L, warp 5 minutes flocculation sedimentations are crossed, the removal rate of COD is 58.8%.

Claims (7)

1. a kind of preparation method of magnetic coupling flocculant, which is characterized in that react chitosan with acrylamide polymerization to be formed Copolymer composite flocculation agent, while ferroso-ferric oxide being combined on copolymer by gel reaction, utilize ferroso-ferric oxide The sinking speed of floccule body is accelerated in magnetic separation effect, includes at least following preparation step:
(1) preparation of chitosan and acrylamide copolymer:
Chitosan is weighed in three-necked flask, is dissolved with acetic acid aqueous solution;Then acrylamide is added under stiring, it is lasting to stir To after being completely dissolved, 70 ~ 90 DEG C are warming up to, ammonium persulfate, the mass ratio of the ammonium persulfate, chitosan and acrylamide is added For 1:(4 ~ 10): (30-50), copolyreaction obtain chitosan and acrylamide copolymer solution;
(2) preparation of ferroferric oxide nano granules:
Weigh that iron chloride, frerrous chloride are soluble in water to be made into mixed solution, iron chloride, frerrous chloride, distilled water mass ratio be 1:(2 ~ 5): (50 ~ 80) are slowly dropped in mixed solution with ammonium hydroxide under stiring, are adjusted after pH reaches 6-7 and are started to generate largely Black ferroferric oxide nano particle, continue ammonium hydroxide to hydrolysis is added dropwise and tend to completely, after ageing, then by particle obtained from molten It separates, is washed with distilled water to get ferroferric oxide nano granules are arrived in liquid;
(3) copolymer and ferroferric oxide nano granules is compound:
Disperse ferroferric oxide nano granules in copolymer solution, copolymer, ferroso-ferric oxide, sodium tripolyphosphate mole Concentration ratio is (20 ~ 30): (20 ~ 30): 1;PH value of solution is adjusted, sodium tripolyphosphate is added with stirring and gel reaction occurs to get arriving Copolymer and the compound flocculant of ferroferric oxide nano granules.
2. the preparation method of magnetic coupling flocculant according to claim 1, it is characterised in that in step (1): chitosan and The mass fraction of acetic acid is 3% ~ 5%;3 ~ 5h of polymerization reaction.
3. the preparation method of magnetic coupling flocculant according to claim 1, it is characterised in that in step (2): pH range is 6 ~7。
4. according to claim 1 or the preparation method of the 3 magnetic coupling flocculants, it is characterised in that in step (2): ageing is anti- The process conditions answered are as follows: (1 ~ 2) h is reacted at (50 ~ 90) DEG C.
5. the preparation method of magnetic coupling flocculant according to claim 1, it is characterised in that in step (3): pH range is 6~7。
6. a kind of magnetic coupling flocculant, it is characterised in that -5 any preparation methods obtain according to claim 1.
7. a kind of application of magnetic coupling flocculant in the treatment of waste water according to claim 6.
CN201810792565.6A 2018-07-18 2018-07-18 Preparation method of magnetic composite flocculant, product and application thereof Active CN108996647B (en)

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Cited By (7)

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CN110294858A (en) * 2019-06-25 2019-10-01 常州大学 It is a kind of can sequence detection anion, metal cation and dye molecule hydrogel sensing membrane 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
CN114873705A (en) * 2022-05-19 2022-08-09 中国计量大学 Magnetically-modified carboxymethyl chitosan compound flocculant, preparation method thereof and application thereof in synchronous removal of heavy metals of antimony and chromium in printing and dyeing wastewater
CN115340157A (en) * 2022-09-02 2022-11-15 浙江华蓝环境科技有限公司 Modified chitosan-based magnetic flocculant and preparation method and application thereof
CN116987526A (en) * 2023-08-30 2023-11-03 石家庄环腾能源科技有限公司 Demulsification flocculant and method for reducing total metal content of industrial mixed oil

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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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Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110294858A (en) * 2019-06-25 2019-10-01 常州大学 It is a kind of can sequence detection anion, metal cation and dye molecule hydrogel sensing membrane and preparation method thereof
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
CN114873705A (en) * 2022-05-19 2022-08-09 中国计量大学 Magnetically-modified carboxymethyl chitosan compound flocculant, preparation method thereof and application thereof in synchronous removal of heavy metals of antimony and chromium in printing and dyeing wastewater
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
CN115340157A (en) * 2022-09-02 2022-11-15 浙江华蓝环境科技有限公司 Modified chitosan-based magnetic flocculant and preparation method and application thereof
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
CN116987526A (en) * 2023-08-30 2023-11-03 石家庄环腾能源科技有限公司 Demulsification flocculant and method for reducing total metal content of industrial mixed oil
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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