CN107986408B - Liquid magnetic composite flocculant and preparation and application thereof - Google Patents

Liquid magnetic composite flocculant and preparation and application thereof Download PDF

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CN107986408B
CN107986408B CN201711271788.XA CN201711271788A CN107986408B CN 107986408 B CN107986408 B CN 107986408B CN 201711271788 A CN201711271788 A CN 201711271788A CN 107986408 B CN107986408 B CN 107986408B
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magnetic composite
composite flocculant
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CN107986408A (en
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彭映林
余旺
郑雅杰
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Hunan City University
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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
    • 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
    • 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
    • C02F1/5263—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using natural chemical compounds
    • 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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  • 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)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Separation Of Suspended Particles By Flocculating Agents (AREA)

Abstract

The invention relates to the field of water treatment materials, in particular to a liquid magnetic composite flocculant which is a suspension containing a polymeric ferric sulfate solution, ferroferric oxide powder and a stabilizer; the stabilizer is at least one of polydimethyldiallyl ammonium chloride, polyvinylpyrrolidone K30 and chitosan. In addition, the invention also provides a preparation method and application of the liquid magnetic composite flocculant. Through a large amount of researches, the inventor discovers that the liquid magnetic composite flocculant which can prevent magnetic species from agglomerating, obviously slow down sedimentation, has high stability and good magnetic species dispersibility can be obtained through the cooperation of the components.

Description

Liquid magnetic composite flocculant and preparation and application thereof
Technical Field
The invention belongs to the field of wastewater treatment, and particularly relates to a liquid magnetic composite flocculant.
Background
Due to the complexity and stability of the sewage dispersion system, a single flocculating agent is difficult to obtain a good treatment effect when being used for treating the sewage system. Since the composite flocculant can overcome many defects of using a single flocculant, the flocculation performance can be improved, and the water treatment cost can be reduced, the research and development and the application of the composite flocculant become the main development direction of novel, efficient and economic flocculants.
The magnetic flocculation technology is one of the most widely applied technologies in the magnetic separation water treatment technology. The magnetic flocculation technology is called as loading flocculation magnetic separation water treatment technology, and is characterized by adding a flocculating agent into water and simultaneously adding magnetic seeds to combine the pollutants, the magnetic seeds and the flocculating agent into a whole to form a magnetic complex, and then realizing solid-liquid separation through a magnetic separation device or self rapid sedimentation so as to remove the pollutants. In the magnetic flocculation process, the used medicaments mainly comprise magnetic seeds and a flocculating agent. The existing magnetic flocculation process generally adopts magnetic seeds and a flocculating agent which are respectively added, and magnetite (Fe) is selected3O4) When the magnetic flocculation is carried out, the process has more influencing factors, harsh control conditions and difficult guarantee of the magnetic flocculation effect.
If the magnetic composite flocculant integrating magnetism and flocculation characteristics is prepared, the flocculation process can be greatly simplified, the cost is saved, and the flocculation effect is easier to control. In the prior art, some preparation methods of the magnetic composite flocculant are also reported; for example, it has been reported that magnetic Fe3O4Impregnation of nanofluid into synthetic Al13Sol, ultrasoundAging for a certain time after dispersion, and then soaking in Al13In the sol, Al is coated for several times13And calcining the carrier in a muffle furnace to obtain the magnetic nano-polymeric Al13A flocculant. It has also been reported that PAC sol is obtained by dissolving PAC in water and ultrasonically dispersing; then adding Fe3O4Dissolving the powder in PAC sol, performing ultrasonic dispersion, aging for a certain time, and drying to obtain the magnetic flocculant. For another example, with FeCl3And FeCl2·4H2Preparing modified Fe by taking O as an iron source, ammonia water as a precipitator and oleic acid as a surfactant by adopting a coprecipitation method3O4Microparticles; then preparing cross-linked modified chitosan magnetic particles by adopting a reversed-phase suspension cross-linking method, and stirring a certain amount of carboxymethyl chitosan and modified Fe3O4The aqueous solution is dripped into paraffin oil for emulsification, a cross-linking agent is added under stirring at normal temperature, and after reaction for a certain time, a modified chitosan magnetic particle product is obtained by magnetic separation, washing and drying and is used as a flocculating agent for treating pulping and papermaking wastewater. For another example, acrylamide monomer and 2-acrylamide-2-methylpropanesulfonic acid are dissolved in water, and then oleic acid modified Fe is added3O4And (3) introducing nitrogen into the particles under stirring, adding potassium persulfate and sodium bisulfite, stirring for a certain time in a water bath, and washing, drying and crushing to obtain the novel anionic magnetic composite flocculant.
And the research reports that the acid activation modification and the coating modification of the loaded iron ions are carried out on the surface of the magnetite powder to prepare the powdery magnetic coagulant, the selected magnetite powder is put into a ball milling reaction device, dilute sulfuric acid and glycolic acid solution are added to be stirred for a certain time, ferric trichloride solution is added to be stirred and reacted until the material is dried and crushed, and then the product is obtained through separation and crushing.
Chinese patent publication No. CN106630059A discloses a magnetic powder composite polymeric ferric sulfate flocculant, which is prepared from the following raw materials in parts by weight: fe3O42-4 parts of powder, FeSO4·7H225-30 parts of O, 1-2 parts of cyclodextrin, a proper amount of sulfuric acid waste liquid, 2-3 parts of thiobacillus ferrooxidans, 4-6 parts of hydrogen peroxide, 1-2 parts of lanthanum nitrate, 3-5 parts of silver nitrate, VN8353-5 parts of polyacrylamide, and attapulgite15-25 parts of soil, 25-35 parts of ethylene glycol and 25-30 parts of water; the mass fraction of the sulfuric acid waste liquid is not less than 60%. Chinese patent publication No. CN103508523A discloses a composite flocculant for water treatment, which is composed of a plurality of flocculants in a composite manner, and comprises the following components in percentage by weight: 70-89% of polyaluminum chloride; 10-30% of aluminum salt; 0.1-2% of iron salt.
The magnetic composite flocculant is a powder flocculant and needs to be dried, however, the drying process easily causes the oxidation inactivation of effective components, expensive production equipment is needed, the preparation process is complex, the cost is high, and the prepared solid magnetic composite flocculant needs to be dissolved for use; the prior art still has more technical problem.
Disclosure of Invention
In order to solve the technical problems of the existing magnetic composite flocculant, the invention aims to provide a liquid magnetic composite flocculant (also called composite flocculant for short) and aims to provide a liquid magnetic composite flocculant product which avoids agglomeration and has good stability.
The second purpose of the invention is to provide a preparation method of the liquid magnetic composite flocculant.
The third purpose of the invention is to provide an application method of the liquid magnetic composite flocculant.
The existing magnetic flocculation process mostly adopts the respective addition of magnetic seeds and a flocculating agent, and the double-agent system needs two agent adding devices, so that the cost of water treatment is increased, and the magnetic flocculation effect cannot be ensured due to the uneven dispersion of the magnetic seeds; in addition, the prior art also provides some magnetic composite flocculant materials, which are solid materials and need drying treatment, however, the drying process easily makes some effective components easily oxidized and inactivated; in order to avoid oxidation in the drying process, drying is needed under the vacuum condition, and the industrial investment is huge. In order to overcome the problems in the prior art, the invention aims to provide a liquid type magnetic composite flocculant which uniformly mixes magnetic seeds and a flocculant and can be directly used without drying treatment. However, providing a liquid type composite flocculant is not a simple transformation of the product form, and it is required to overcome a number of technical problems, for example, problems such as poor magnetic species dispersibility, easy agglomeration, easy sedimentation, and the like. Through a large number of researches, the inventor finally finds a liquid composite magnetic flocculant with good dispersibility and good stability, and the specific technical scheme is as follows:
a liquid magnetic composite flocculant is a suspension containing a polymeric ferric sulfate solution, ferroferric oxide powder and a stabilizer;
the stabilizer is at least one of polydimethyldiallylammonium chloride (PDMDAAC), polyvinylpyrrolidone K30(PVP) and Chitosan (CTS).
Through a large amount of researches, the inventor discovers that the liquid magnetic composite flocculant which can prevent magnetic species from agglomerating, obviously slow down sedimentation, has high stability and good magnetic species dispersibility can be obtained through the cooperation of the components.
The key point of the invention is to provide a liquid magnetic composite flocculant for the first time. The inventor finds that the liquid magnetic composite flocculant with good dispersibility, difficult agglomeration and good stability can be obtained by the synergy of the polymeric ferric sulfate solution and the stabilizer required by the invention and further by the control of the particle size of the ferroferric oxide.
Preferably, the polymeric ferric sulfate solution is 8-14% of total iron by mass and 6-18% of basicity.
Preferably, the particle size of the ferroferric oxide powder is 1.3-10 mu m, and the Fe3O4The mass fraction is more than or equal to 80 percent.
Research shows that the particle size of the ferroferric oxide has influence on the stability and the like of the liquid magnetic composite flocculant, the large-particle ferroferric oxide is easy to settle, and the small-particle ferroferric oxide is easy to agglomerate; within the preferable range of the invention, the obtained liquid composite flocculant has higher stability and ferroferric oxide is less prone to agglomeration.
Preferably, the content of the ferroferric oxide powder is 5-80 g.L-1(ii) a More preferably 5 to 10 g.L-1。
In the invention, the stabilizing agent is matched with the polymeric ferric sulfate solution, and the uniform suspension with good uniformity, difficult agglomeration of magnetic seeds and good stability can be obtained.
The stabilizer can be at least one of the three components; in the actual use process, the poly dimethyl diallyl ammonium chloride can be used in the form of an aqueous solution, and the mass concentration of the poly dimethyl diallyl ammonium chloride can be 30-40%; both polyvinylpyrrolidone K30 and chitosan can be used in solid form.
Preferably, the content of the poly-dimethyldiallylammonium chloride is less than or equal to 256 g.L-1(ii) a More preferably 25.6 to 256 g.L-1。
More preferably, the content of the poly-dimethyldiallylammonium chloride is 80 to 240 g.L-1. Under the preferable content, the polymer can be cooperated with polymeric ferric sulfate, so that the dispersibility and the stability are obviously improved; the flocculation effect of the obtained liquid magnetic flocculant can be unexpectedly improved, and the COD removal rate is improved.
Preferably, the content of polyvinylpyrrolidone K30 is not more than 320 g.L-1(ii) a Preferably 32 to 320 g.L-1。
More preferably, the content of polyvinylpyrrolidone K30 is 40-240 g.L-1. Under the preferable content, the polymer can be cooperated with polymeric ferric sulfate, so that the dispersibility and the stability are obviously improved; the flocculation effect of the obtained liquid magnetic flocculant can be unexpectedly improved, and the COD removal rate is improved.
Preferably, the content of chitosan is less than or equal to 70 g.L-1(ii) a Preferably 7 to 70 g.L-1。
More preferably, the content of chitosan is 30 to 50 g.L-1. Under the preferable content, the polymer can be cooperated with polymeric ferric sulfate, so that the dispersibility and the stability are obviously improved; the flocculation effect of the obtained liquid magnetic flocculant can be unexpectedly improved, and the COD removal rate is improved.
The invention also provides a preparation method of the liquid magnetic composite flocculant, which comprises the steps of adding ferroferric oxide powder into a polymeric ferric sulfate solution under stirring, adding a stabilizer after the ferroferric oxide powder is dispersed, and uniformly stirring to obtain the liquid magnetic composite flocculant. Through the mixing sequence, mutual incompatibility among materials can be further avoided, agglomeration can be further reduced, and the stability of the finally obtained liquid magnetic composite flocculant is improved.
Preferably, the temperature in the stirring process is 30-60 ℃ and the time is 1-2 h.
The liquid magnetic composite flocculant is applied as a flocculant for sewage treatment.
Has the advantages that:
(1) the invention provides the liquid-form magnetic composite magnetic flocculant for the first time, and the use is convenient; vacuum drying is not needed, the preparation method is simple, and the cost is low;
(2) through the synergy of the components, the magnetic composite magnetic flocculant has good stability; the particle size of the ferroferric oxide and the content of the stabilizer are further regulated and controlled, so that the stability of the ferroferric oxide can be further improved, agglomeration is further avoided, and the application effect is improved;
(3) the magnetic composite flocculant prepared by the method has a combined flocculation effect, can be used for treating domestic wastewater, petroleum wastewater, heavy metal wastewater and mineral processing wastewater, and is wide in application;
(4) the method for preparing the magnetic composite flocculant has the advantages of simple process and good environmental and economic benefits.
Detailed Description
Evaluation of Dispersion stability of composite magnetic flocculant
The invention adopts a sedimentation method to evaluate the dispersion stability of the composite magnetic flocculant. After the preparation of the composite magnetic flocculant is finished, immediately pouring the composite magnetic flocculant into a 10mL test tube, starting timing, and observing the sedimentation condition of the magnetic seeds; after standing and settling for a period of time, the suspension begins to stratify, the upper layer is clear liquid, the lower layer is magnetic powder suspension, and the volume of the lower layer is settling volume; the sedimentation volume is smaller and smaller, and when the sedimentation volume is stable and unchanged, the timing is stopped, and the sedimentation time is recorded. Longer settling times indicate better stability, and shorter settling times indicate poorer stability.
Example 1
Adding Fe with the particle size of 1.6-6.5 mu m into 5L of polymeric ferric sulfate solution (Shenzhen Changlong science and technology Co., Ltd.) with the total iron mass fraction of 11% and the basicity of 13%3O450g of 94% ferroferric oxide powder by mass is stirred until the ferroferric oxide powder is uniformly dispersed, then polydimethyldiallyl ammonium chloride (aqueous solution with the mass concentration of 40%) is added to ensure that the concentrations of the polydimethyldiallyl ammonium chloride respectively reach 80g/L, 160g/L and 240g/L (PDMDAAC concentration), then the mixture is heated to 60 ℃, and the mixture is continuously stirred for 2 hours to obtain liquid magnetic composite flocculant which is respectively marked as A, B, C, wherein the measured stabilization time of the liquid magnetic composite flocculant is respectively 10 days (liquid magnetic composite flocculant A), 17.5 days (liquid magnetic composite flocculant A) and 28.5 days (liquid magnetic composite flocculant C). The blank stabilization time was only 4 h.
Preparation of 25 mg. L-1Butyl xanthate solution. Adopting a Fenton-magnetic flocculation method to treat Fe in the Fenton process stage2+The concentration is 10 mg.L-1、H2O2The concentration is 0.4 mL. L-1The initial pH value of the solution is 7.5, the reaction time is 1h, and in the magnetic flocculation process stage, liquid magnetic composite flocculant A, B, C is respectively used, the concentrations of the three are controlled to be the same, so that the COD removal effects of the three under the same concentration are compared; for example, the concentration of all three is controlled to 100 mg.L-1In the process, the COD removal rates of the liquid magnetic composite flocculant A, B, C are respectively 89.12%, 90.34% and 85.55%; the result shows that the removal effect of the liquid magnetic composite flocculant B is better under the same use concentration, and further research also finds that the concentration of the liquid magnetic composite flocculant B is controlled to be 160 mg.L-1The wastewater treatment effect is better, the removal rate of xanthate in the treated wastewater reaches up to 82.22 percent, and the removal rate of COD can reach up to 96.75 percent.
Example 2
Adding Fe with the particle size of 1.6-2.6 mu m into 1L of polymeric ferric sulfate solution (Shenzhen Changlong science and technology Co., Ltd.) with the total iron mass fraction of 12% and the basicity of 10%3O410g of ferroferric oxide powder with the mass fraction of 94 percent is stirred to form ferroferric oxide powderAfter the body is uniformly dispersed, adding polyvinylpyrrolidone K30 (solid, analytically pure), wherein the concentrations of polyvinylpyrrolidone K30 respectively reach 40g/L, 120g/L and 240g/L (PVP concentration), then heating to 50 ℃, continuously stirring for 1h to obtain liquid magnetic composite flocculant, respectively marking the liquid magnetic composite flocculant as D, E, F, and measuring the stabilization time of the liquid magnetic composite flocculant to be 15.5 days, 30 days and 43 days respectively.
Preparation of 25 mg. L-1Butyl xanthate solution. Adopting a Fenton-magnetic flocculation method to treat Fe in the Fenton process stage2+The concentration is 10 mg.L-1、H2O2The concentration is 0.4 mL. L-1The initial pH value of the solution is 7.5, the reaction time is 1h, and in the magnetic flocculation process stage, liquid magnetic composite flocculant D, E, F is respectively used, the concentrations of the three are controlled to be the same, so that the COD removal effects of the three under the same concentration are compared; for example, the concentration of all three is controlled to 100 mg.L-1In the process, the COD removal rates of the liquid magnetic composite flocculant D, E, F are respectively 80.16%, 85.17% and 79.06%; the results show that the removal effect of the liquid magnetic composite flocculant E is better under the same use concentration, and further research shows that the concentration of the liquid magnetic composite flocculant E composite magnetic flocculant is controlled to be 130 mg.L-1The wastewater treatment effect is better, the removal rate of xanthate in the treated wastewater is 70.81%, and the removal rate of COD is 94.31%.
Example 3
Adding Fe with the particle size of 1.3-1.6 mu m into 10L of polymeric ferric sulfate solution (Shenzhen Changlong science and technology Co., Ltd.) with the total iron mass fraction of 10% and the basicity of 12%3O450g of ferroferric oxide powder with the mass fraction of 90 percent is stirred until the ferroferric oxide powder is uniformly dispersed, chitosan (solid, biological reagent) is added until the concentration reaches 10g/L, 30g/L and 50g/L (CTS concentration), then the mixture is heated to 60 ℃, the mixture is continuously stirred for 2 hours to obtain liquid magnetic composite flocculant which is respectively marked as liquid magnetic composite flocculant G, H, I, and the measured stabilization time of the liquid magnetic composite flocculant is respectively 6.5 days, 17 days and 25 days.
Preparation of 25 mg. L-1Butyl xanthate solution. Adopting a Fenton-magnetic flocculation methodTreatment, Fenton Process stage Fe2+The concentration is 10 mg.L-1、H2O2The concentration is 0.4 mL. L-1The initial pH value of the solution is 7.5, the reaction time is 1h, and in the magnetic flocculation process stage, liquid magnetic composite flocculant G, H, I is respectively used, the concentrations of the three are controlled to be the same, so that the COD removal effects of the three under the same concentration are compared; for example, the concentration of all three is controlled to 100 mg.L-1In the process, the COD removal rates of the liquid magnetic composite flocculant G, H, I are 81.37%, 88.78% and 91.34% respectively; the result shows that the removal effect of the liquid magnetic composite flocculant I is better under the same use concentration, and further research shows that the concentration of the liquid magnetic composite flocculant I composite magnetic flocculant is controlled to be 140 mg.L-1The wastewater treatment effect is better, the removal rate of xanthate in the treated wastewater reaches 83.69%, and the removal rate of COD reaches 97.32%.
Comparative example 1:
compared to example 1, the only difference is that PDMDAAC is replaced by ferrous sulfate, soluble starch, PAM (polyacrylamide), APAM (anionic polyacrylamide) or CPAM (cationic polyacrylamide). The result shows that when ferrous sulfate is added, the obtained composite magnetic flocculant has small change of the sedimentation time, namely the dispersion stability of the product cannot be improved (the stability time is similar to that of a blank control); when soluble starch, PAM, APAM and CPAM are selected, the composite flocculant generated by the soluble starch, PAM, APAM and CPAM are not mutually soluble, and suspension liquid with good stability and dispersibility cannot be obtained.
The embodiment and the proportion show that when the PDMDAAC, the PVP and the CTS required by the invention are adopted, the composite magnetic flocculant product with greatly improved dispersion stability can be obtained by matching with the polymeric ferric sulfate solution and controlling the material concentration, the ferroferric oxide particle size and the like.

Claims (8)

1. The liquid magnetic composite flocculant is characterized by being a suspension containing a polymeric ferric sulfate solution, ferroferric oxide powder and a stabilizer;
the stabilizer is at least one of polydimethyldiallyl ammonium chloride, polyvinylpyrrolidone K30 and chitosan;
the particle size of the ferroferric oxide powder is 1.3-10   mu m; fe in ferroferric oxide powder3O4The mass fraction is more than or equal to 80 percent;
the content of the ferroferric oxide powder is 5-80 g.L-1；
The content of the poly dimethyl diallyl ammonium chloride is 25.6-256   g.L-1；
The content of polyvinylpyrrolidone K30 is 32-320 g.L-1；
The content of the chitosan is 7-70     g.L-1；
The adopted polymeric ferric sulfate solution has 8-14% of total iron mass fraction and 6-18% of basicity.
2. The liquid magnetic composite flocculant according to claim 1, wherein the content of ferroferric oxide powder is 5-10 g.L-1。
3. The liquid magnetic composite flocculant according to claim 1, wherein the content of poly (dimethyldiallylammonium chloride) is 80-240 g.L.-1。
4. The liquid magnetic composite flocculant according to claim 1, wherein the content of polyvinylpyrrolidone K30 is 40-240 g.84 g.L-1。
5. The liquid magnetic composite flocculant according to claim 1, wherein the content of chitosan is 30 to 50   g.L-1。
6. A preparation method of the liquid magnetic composite flocculant according to any one of claims 1 to 5, characterized by adding ferroferric oxide powder into a polymeric ferric sulfate solution under stirring, adding a stabilizer after the ferroferric oxide powder is dispersed, and uniformly stirring to obtain the liquid magnetic composite flocculant.
7. The preparation method of the liquid magnetic composite flocculant according to claim 6, wherein the temperature in the stirring process is 20-60 ℃; the time is 1-2 h.
8. Use of the liquid magnetic composite flocculant according to any one of claims 1 to 5 as a flocculant for sewage treatment.
CN201711271788.XA 2017-12-05 2017-12-05 Liquid magnetic composite flocculant and preparation and application thereof Active CN107986408B (en)

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