CN116375157A - Poly silicon aluminum magnesium composite flocculant for removing dye wastewater - Google Patents
Poly silicon aluminum magnesium composite flocculant for removing dye wastewater Download PDFInfo
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- CN116375157A CN116375157A CN202310458423.7A CN202310458423A CN116375157A CN 116375157 A CN116375157 A CN 116375157A CN 202310458423 A CN202310458423 A CN 202310458423A CN 116375157 A CN116375157 A CN 116375157A
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- 239000002131 composite material Substances 0.000 title claims abstract description 45
- -1 silicon aluminum magnesium Chemical compound 0.000 title claims description 4
- 239000002351 wastewater Substances 0.000 title description 5
- 229910021420 polycrystalline silicon Inorganic materials 0.000 title description 2
- 229920005591 polysilicon Polymers 0.000 title description 2
- 229920002472 Starch Polymers 0.000 claims abstract description 63
- 239000008107 starch Substances 0.000 claims abstract description 63
- 230000005291 magnetic effect Effects 0.000 claims abstract description 61
- SNAAJJQQZSMGQD-UHFFFAOYSA-N aluminum magnesium Chemical compound [Mg].[Al] SNAAJJQQZSMGQD-UHFFFAOYSA-N 0.000 claims abstract description 51
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 48
- 238000003756 stirring Methods 0.000 claims abstract description 36
- 235000019698 starch Nutrition 0.000 claims abstract description 23
- 238000000034 method Methods 0.000 claims abstract description 19
- 239000002253 acid Substances 0.000 claims abstract description 18
- 238000002360 preparation method Methods 0.000 claims abstract description 17
- 239000004115 Sodium Silicate Substances 0.000 claims abstract description 12
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229910052911 sodium silicate Inorganic materials 0.000 claims abstract description 12
- 239000002122 magnetic nanoparticle Substances 0.000 claims abstract description 7
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical class [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 claims abstract description 3
- 159000000003 magnesium salts Chemical class 0.000 claims abstract description 3
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 26
- 239000000843 powder Substances 0.000 claims description 11
- 238000001994 activation Methods 0.000 claims description 7
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 6
- 230000004913 activation Effects 0.000 claims description 6
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- 238000000227 grinding Methods 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- 229910052782 aluminium Inorganic materials 0.000 claims description 4
- 239000011777 magnesium Substances 0.000 claims description 3
- 229910052749 magnesium Inorganic materials 0.000 claims description 3
- 230000008569 process Effects 0.000 claims description 3
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 2
- 239000000463 material Substances 0.000 claims description 2
- 230000001105 regulatory effect Effects 0.000 claims description 2
- JLVVSXFLKOJNIY-UHFFFAOYSA-N Magnesium ion Chemical compound [Mg+2] JLVVSXFLKOJNIY-UHFFFAOYSA-N 0.000 claims 2
- 229910001425 magnesium ion Inorganic materials 0.000 claims 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims 1
- 229910052710 silicon Inorganic materials 0.000 claims 1
- 239000010703 silicon Substances 0.000 claims 1
- 229910021642 ultra pure water Inorganic materials 0.000 claims 1
- 239000012498 ultrapure water Substances 0.000 claims 1
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 abstract description 10
- 238000000975 co-precipitation Methods 0.000 abstract description 2
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 abstract 3
- 238000010438 heat treatment Methods 0.000 abstract 2
- 230000003213 activating effect Effects 0.000 abstract 1
- 238000005189 flocculation Methods 0.000 description 30
- 230000016615 flocculation Effects 0.000 description 30
- 230000000694 effects Effects 0.000 description 23
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 18
- 238000005345 coagulation Methods 0.000 description 18
- 230000015271 coagulation Effects 0.000 description 18
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 15
- 229960000583 acetic acid Drugs 0.000 description 11
- 239000012362 glacial acetic acid Substances 0.000 description 10
- 238000004062 sedimentation Methods 0.000 description 10
- 239000006247 magnetic powder Substances 0.000 description 9
- IQFVPQOLBLOTPF-HKXUKFGYSA-L congo red Chemical compound [Na+].[Na+].C1=CC=CC2=C(N)C(/N=N/C3=CC=C(C=C3)C3=CC=C(C=C3)/N=N/C3=C(C4=CC=CC=C4C(=C3)S([O-])(=O)=O)N)=CC(S([O-])(=O)=O)=C21 IQFVPQOLBLOTPF-HKXUKFGYSA-L 0.000 description 8
- 238000002835 absorbance Methods 0.000 description 7
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 5
- 238000000926 separation method Methods 0.000 description 5
- 239000006228 supernatant Substances 0.000 description 5
- 229910021645 metal ion Inorganic materials 0.000 description 4
- 238000001179 sorption measurement Methods 0.000 description 4
- 238000005303 weighing Methods 0.000 description 4
- 238000011481 absorbance measurement Methods 0.000 description 3
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 230000005294 ferromagnetic effect Effects 0.000 description 3
- 239000012530 fluid Substances 0.000 description 3
- 229910052943 magnesium sulfate Inorganic materials 0.000 description 3
- 235000019341 magnesium sulphate Nutrition 0.000 description 3
- 239000002105 nanoparticle Substances 0.000 description 3
- 231100000252 nontoxic Toxicity 0.000 description 3
- 230000003000 nontoxic effect Effects 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 229910002800 Si–O–Al Inorganic materials 0.000 description 2
- 229910002801 Si–O–Mg Inorganic materials 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 description 2
- 239000008394 flocculating agent Substances 0.000 description 2
- 238000007885 magnetic separation Methods 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000006386 neutralization reaction Methods 0.000 description 2
- 229910017135 Fe—O Inorganic materials 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 238000010170 biological method Methods 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 150000001735 carboxylic acids Chemical class 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 150000002500 ions Chemical group 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 238000006068 polycondensation reaction Methods 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 239000003440 toxic substance Substances 0.000 description 1
- 239000003403 water pollutant Substances 0.000 description 1
- 238000003911 water pollution Methods 0.000 description 1
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Classifications
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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
- C02F1/5245—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents using basic salts, e.g. of aluminium and iron
-
- 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
- C02F1/52—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
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/34—Organic compounds containing oxygen
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/38—Organic compounds containing nitrogen
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/40—Organic compounds containing sulfur
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/34—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/34—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32
- C02F2103/343—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32 from the pharmaceutical industry, e.g. containing antibiotics
Abstract
The invention discloses a preparation method of a magnetic magnesium aluminum polysilicate-starch composite flocculant, which comprises the following steps: in the first step, fe is synthesized by using a coprecipitation method 3 O 4 Magnetic nanoparticles for preparing Fe with concentration of 1100-1500mg/L 3 O 4 Solution of Fe 3 O 4 Stirring the solution in water bath to obtain brown Fe 3 O 4 Adding sodium silicate solution, stirring to dissolve, adjusting pH to optimal value with sulfuric acid and sodium hydroxide, heating in water bath, stirring, standing, etcThe step of obtaining the magnetic polysilicic acid solution. Adding proper amount of aluminum salt and magnesium salt into magnetic polysilicic acid solution, and activating to obtain magnetic polysilicic acid aluminum magnesium (Fe) 3 O 4 PSAM) solution, then adding a proper amount of starch solution into the obtained magnetic aluminum magnesium polysilicate solution, and carrying out water bath heating and other steps again, thus obtaining the magnetic aluminum magnesium polysilicate-starch composite flocculant.
Description
Technical Field
The invention belongs to the technical field of inorganic-natural organic composite flocculant, and particularly relates to a preparation method of a magnetic magnesium aluminum polysilicate-starch composite flocculant.
Background
With the development of various industries of society, water treatment in the aspect of environment faces serious examination, in order to reduce the water pollution condition and reduce the harm to human living environment, a plurality of water purifying methods have been developed, and the flocculant is more widely applied to water treatment due to simple and efficient operation and low cost, thereby having wide application prospect;
however, most flocculants are not degradable, and can also have certain influence on the environment, even some toxic substances are involved, and the normal physicochemical biological methods cannot meet the current requirements, so that the environment-friendly flocculants which are biodegradable, nontoxic and harmless and have good flocculation effect are researched;
the flocculation mechanism mainly comprises adsorption bridging, adsorption electric neutralization and the like, different flocculation mechanisms exist in different periods, and finally solid-liquid separation is carried out by a physical or chemical method, so that in order to improve the flocculation effect, a magnetic technology is introduced, and the flocculation effect is obviously improved.
Disclosure of Invention
Aiming at the problems, the invention provides the preparation method of the magnetic aluminum magnesium polysilicate-starch composite flocculant, which is simple to operate and obvious in flocculation effect, and the magnetic flocculant prepared by the method is obvious in flocculation effect, has no pollution to the environment, is biodegradable, and can be widely applied to sewage treatment, such as advanced treatment of chemical wastewater such as factory wastewater, pharmaceutical wastewater and the like.
In order to achieve the above effects, the present invention adopts the following scheme:
the preparation method of the magnetic magnesium aluminum polysilicate-starch composite flocculant comprises the following steps:
(1) Fe is synthesized by adopting a coprecipitation method 3 O 4 Washing, drying, grinding into powder to obtain Fe 3 O 4 Magnetic nanoparticles, followed by the preparation of Fe at a concentration of 1100-1500mg/L 3 O 4 A solution;
(2) At Fe 3 O 4 Adding sodium silicate into the solution, stirring until the sodium silicate is dissolved, adjusting the PH of the solution, and performing activation treatment to obtain a magnetic polysilicic acid solution;
(3) Adding aluminum salt and magnesium salt into the magnetic polysilicic acid solution, and performing activation treatment to prepare a magnetic polysilicic acid magnesium flocculant;
(4) The limited range of the concentration of the metal ions in the step (3) can enable flocculation reaction to be more complete, flocculation can achieve the optimal effect, if the concentration of the metal ions is lower than the minimum concentration value, good flocculation effect cannot be achieved, and if the concentration of the metal ions is higher than the maximum concentration value, the problems of metal ion residues and the like can be caused;
(5) Adding the pretreated starch solution into the prepared magnetic aluminum magnesium polysilicate flocculant, and performing water bath stirring, standing, curing and other steps to obtain the magnetic aluminum magnesium polysilicate-starch composite flocculant.
Further, in the preparation method of the magnetic magnesium aluminum polysilicate-starch composite flocculant, the pH of the sodium silicate solution is regulated to 2-4 by using an acid solution in the step (2).
The PH value is taken as an important factor influencing the flocculant effect, has great influence on the flocculant forming process, and under the state of stronger acidity, polysilicic acid is easy to generate polycondensation reaction, gel phenomenon occurs, the combination is influenced, the flocculation effect is reduced, if the alkalinity is stronger, the activation process is difficult to control, and the electric neutralization effect cannot be exerted to the greatest extent.
Further, in the preparation method of the magnetic magnesium aluminum polysilicate-starch composite flocculant, the activation treatment process in the step (2) is as follows: stirring in water bath at 35-45deg.C for 1.5-2.5 hr, standing and aging for 2-8 hr.
Further, in the preparation method of the magnetic aluminum magnesium polysilicate-starch composite flocculant, the water bath temperature in the step (3) is 30-50 ℃, the stirring time is 1.5-2.5h, and the standing and curing time is 3-8h.
Further, in the steps (2) - (3), the reaction temperature is an important factor affecting the reaction process, if the temperature is lower than the set temperature, the electrostatic effect is weak, and ineffective collision is generated, so that the flocculation effect is poor, if the temperature is higher than the set temperature, the polysilicic acid loses the original activity, the material structure is destroyed, the flocculation effect is also affected, the water bath stirring can make the reaction more sufficient, the electrostatic effect between molecules is enhanced, and the flocculation effect is optimal.
Standing and curing are carried out to complete the reaction, the curing time is determined to ensure that the floccules are more compact, the sedimentation speed is increased, and the removal rate is obviously improved.
In the preparation method of the magnetic magnesium aluminum polysilicate-starch composite flocculant, starch is pretreated by 0.5-1.5% glacial acetic acid in the step (4) to prepare starch solution.
The purpose of the pretreatment of starch with glacial acetic acid is to accelerate the dissolution rate of starch, a large amount of carboxylic acid is grafted with aluminum magnesium polysilicate, the adsorption net capturing capacity is enhanced, the flocculation effect is enhanced, and the concentration of acetic acid is too high or too low to influence the flocculation efficiency, thereby playing a role in blocking flocculation.
Further, step (1) uses FeCl 3 ·6H 2 O and FeCl 2 ·4H 2 O synthesizes Fe 3 O 4 ；FeCl 3 ·6H 2 O is prepared in the concentrated hydrochloric acid atmosphere, and the concentration is 0.25-0.32mol/L; feCl 2 ·4H 2 O, wherein the concentration of the O prepared under the atmosphere of concentrated hydrochloric acid and iron powder is 0.08-0.16mol/L; and the two are mixed in a ratio of 1:1, excessive ammonia water is added.
Taking into account Fe 2+ Is easy to hydrolyze, so FeCl with concentration of 0.08-0.16mol/L is prepared under the atmosphere of concentrated hydrochloric acid and iron powder 2 ·4H 2 O; in order to prevent hydrolysis, when the two are mixed, excessive ammonia water is added, after mixing, stirring is carried out for 2 hours, the mixture is uniformly reacted, and finally, the mixture is put into an oven for drying and is ground into powder.
In view of the fact that the ferroferric oxide has strong magnetism and chemical reaction inertia, is nontoxic and harmless to environmental influence, the magnetic material ferroferric oxide is compounded with the traditional flocculant to form the magnetic composite flocculant; the ferromagnetic nano particles have larger specific surface area and magnetic dipole attraction, the adsorption capacity of the ferromagnetic nano particles can be enhanced, so that the removal rate of water pollutants is improved, the mud-water separation time is shortened, the volume of a sedimentation tank is reduced, the investment cost and the occupied area are saved, and the flocculant with strong adaptability, good separation effect, wide application range and improved flocculation effect is developed.
The preparation method of the magnetic aluminum magnesium polysilicate-starch composite flocculant has the advantages of low cost, simple operation, high flocculation performance, and ferromagnetic nano particles, and the flocculation effect is obvious when the preparation method is used for treating Congo red water samples: the removal rate is over 94 percent, and the prepared flocculant is nontoxic and harmless, can be recycled and reused, and has wide application prospect.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings that are required to be used in the embodiments or the description of the prior art will be briefly described below, and it is obvious that the drawings in the following description are only embodiments of the present invention, and that other drawings can be obtained according to the provided drawings without inventive effort for a person skilled in the art.
FIG. 1 shows a magnetic magnesium aluminum polysilicate-starch composite flocculant (Fe) according to example 1 of the present invention 3 O 4 -PSAM-St) and comparative magnesium aluminum polysilicate-starch composite flocculation (PSAT-St);
FIG. 2 shows a magnetic magnesium aluminum polysilicate-starch composite flocculant (Fe) according to example 1 of the present invention 3 O 4 -PSAM-St) and the XRD patterns of the comparative magnesium aluminum polysilicate-starch composite flocculant (PSAM-St).
The specific embodiment is as follows:
the following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
The preparation method of the magnetic magnesium aluminum polysilicate-starch composite flocculant comprises the following specific steps:
preparing FeCl of 0.285mol/L under concentrated hydrochloric acid atmosphere 3 ·6H 2 O, feCl of 0.15mol/L is prepared under the atmosphere of concentrated hydrochloric acid and iron powder 2 ·4H 2 Mixing the two solutions at a ratio of 1:1, rapidly adding 30ml of 25% ammonia water, stirring for 2h, washing with absolute ethyl alcohol for three times, drying the solution, and grinding into powder to obtain magnetic powder;
dissolving 72.465mg of magnetic powder in 50ml of H 2 O, stirring in a water bath at 60 ℃ for 2 hours at the rotating speed of 700rpm, and dissolving magnetic powder; adding 2.0035g of sodium silicate powder, stirring and dissolving, slowly dripping 20% sulfuric acid to adjust the pH of the solution to 3.0, stirring in a water bath at 40 ℃ for 2 hours, standing and curing for 4 hours to obtain a magnetic polysilicic acid solution;
weighing 0.5g of starch, dissolving in 100ml of 1% glacial acetic acid, and stirring at 40 ℃ for 2 hours to obtain a starch solution;
taking 1.5ml of starch solution treated by 1% glacial acetic acid, adding a magnetic magnesium aluminum polysilicate solution, stirring in a water bath at 40 ℃ for 2 hours, standing and curing for 24 hours, and preparing the magnetic magnesium aluminum polysilicate-starch composite flocculant;
1ml of magnetic aluminum magnesium polysilicate-starch composite flocculant is taken and added into 1L of simulated water sample, wherein the simulated water sample is Congo red solution with the concentration of 150 mg/L;
and (3) taking the supernatant of the water sample after coagulation sedimentation, measuring the absorbance, wherein the measured removal rate is shown in table 1, sucking out the flocculate after the first coagulation sedimentation by using a magnet, putting the flocculate into 1L of new Congo red water sample again for second coagulation, and repeating the third coagulation by the method.
The magnetic separation can reduce the mud-water separation time, quicken the floc sedimentation speed, can separate the flocs through an external magnetic field in practical application, reduces the cost for later separation, can realize repeated use of the separated flocs, has obvious coagulation effect, increases the use efficiency, and provides great help for reducing the investment cost.
Example 2
The preparation method of the magnetic magnesium aluminum polysilicate-starch composite flocculant comprises the following specific steps:
preparing FeCl of 0.25mol/L under the atmosphere of concentrated hydrochloric acid 3 ·6H 2 O, feCl of 0.08mol/L is prepared under the atmosphere of concentrated hydrochloric acid and iron powder 2 ·4H 2 Mixing the two solutions at a ratio of 1:1, rapidly adding 30ml of 25% ammonia water, stirring for 1.5h, washing with absolute ethyl alcohol for three times, drying the solution, and grinding into powder to obtain magnetic powder;
dissolving 70mg of magnetic powder in 50ml of H 2 O, stirring in a water bath at 50 ℃ for 1h at a rotating speed of 500rpm, and dissolving magnetic powder; adding 1.7248g of sodium silicate powder, stirring and dissolving, slowly dripping 20% sulfuric acid to adjust the pH of the solution to 2, stirring in a 35 ℃ water bath for 2.5 hours, standing and curing for 6 hours to obtain a magnetic polysilicic acid solution;
adding 19.82ml of 0.4mol/L aluminum sulfate solution and 2.56ml of 0.5mol/L magnesium sulfate solution, stirring in a water bath at 30 ℃ for 2.5 hours, standing and curing for 8 hours to obtain a magnetic polysilicate aluminum magnesium solution;
weighing 0.5g of starch, dissolving in 100ml of 0.5% glacial acetic acid, and stirring at 45 ℃ for 2 hours to obtain a starch solution; taking 1.32ml of starch solution treated by 1% glacial acetic acid, adding the magnetic aluminum magnesium polysilicate solution, stirring in a water bath at 30 ℃ for 3 hours, standing and curing for 22 hours, and preparing the magnetic aluminum magnesium polysilicate-starch composite flocculant.
1ml of magnetic aluminum magnesium polysilicate-starch composite flocculant is taken and added into 1L of simulated water sample, the simulated water sample is Congo red solution with the concentration of 150mg/L, absorbance measurement is carried out on supernatant fluid of the water sample after coagulation sedimentation, the measured removal rate is shown in table 1, the flocculation after the first coagulation sedimentation is sucked out by a magnet, the flocculation is put into 1L of new Congo red solution again for second coagulation, and the method is repeated for third coagulation.
Example 3
The preparation method of the magnetic magnesium aluminum polysilicate-starch composite flocculant comprises the following specific steps:
in a concentrated statePreparing FeCl of 0.32mol/L under hydrochloric acid atmosphere 3 ·6H 2 O, feCl of 0.16mol/L is prepared under the atmosphere of concentrated hydrochloric acid and iron powder 2 ·4H 2 Mixing the two solutions at a ratio of 1:1, rapidly adding 30ml of 25% ammonia water, stirring for 2.5h, washing with absolute ethyl alcohol for three times, drying the solution, and grinding into powder to obtain magnetic powder;
dissolving 80mg of magnetic powder in 50ml of H 2 O, stirring in a water bath at 60 ℃ for 3 hours at the rotating speed of 1100rpm, and dissolving magnetic powder; adding 2.1360g of sodium silicate powder, stirring and dissolving, slowly dripping 20% sulfuric acid to adjust the pH of the solution to 4.0, stirring in a 45 ℃ water bath for 1.5h, standing and curing for 8h to obtain a magnetic polysilicic acid solution;
adding 5.8ml of 0.427mol/L aluminum sulfate solution and 2.4ml of 0.854mol/L magnesium sulfate solution, stirring in a water bath at 50 ℃ for 1.5h, standing and curing for 3h to obtain a magnetic aluminum magnesium polysilicate solution;
weighing 0.5g of starch, dissolving in 100ml of 1.5% glacial acetic acid, and stirring at 60 ℃ for 1h to obtain a starch solution; taking 1.7ml of starch solution treated by 1% glacial acetic acid, adding the magnetic aluminum magnesium polysilicate solution, stirring in a water bath at 50 ℃ for 1h, standing and curing for 26h, and preparing the magnetic aluminum magnesium polysilicate-starch composite flocculant.
1ml of magnetic aluminum magnesium polysilicate-starch composite flocculant is taken and added into 1L of simulated water sample, the simulated water sample is Congo red solution with the concentration of 150mg/L, absorbance measurement is carried out on supernatant fluid of the water sample after coagulation sedimentation, the measured removal rate is shown in table 1, the flocculation after the first coagulation sedimentation is sucked out by a magnet, the flocculation is put into 1L of new Congo red solution again for second coagulation, and the method is repeated for third coagulation.
Comparative example 1
Preparing a sodium silicate solution with the concentration of 0.141mol/L, dropwise adding a sulfuric acid solution with the concentration of 20% until the pH value of the sodium silicate solution is 4.0, stirring in a water bath at the temperature of 40 ℃ for 2 hours, standing and curing for 2 hours to obtain a polysilicic acid solution; adding 13.208ml of 0.427mol/L aluminum sulfate solution and 1.65ml of 0.854mol/L magnesium sulfate solution, stirring in a water bath at 40 ℃ for 2 hours, standing and curing for 4 hours to obtain a polysilicate aluminum magnesium solution; weighing 0.5g of starch, dissolving in 100ml of 1.5% glacial acetic acid, and stirring at 60 ℃ for 1h to obtain a starch solution; taking 1.5ml of starch solution treated by 1% glacial acetic acid, adding a magnesium aluminum polysilicate solution, stirring in a water bath at 40 ℃ for 2 hours, standing and curing for 12 hours, and obtaining the magnesium aluminum polysilicate-starch composite flocculant.
1ml of the magnetic magnesium aluminum polysilicate-starch composite flocculant is taken and added into 1L of a simulated water sample, the simulated water sample is Congo red solution with the concentration of 150mg/L, the absorbance measurement is carried out on supernatant fluid of the water sample after coagulation sedimentation, and the measured removal rate is shown in a table 1.
Absorbance = C 1 /λ 1 =C 2 /λ 2
Wherein: lambda (lambda) 1 Simulated absorbance of water sample prior to flocculation experiment
λ 2 Absorbance of water sample supernatant after flocculation precipitation
The removal rate is calculated by measuring the absorbance of the water sample before and after coagulation:
removal rate = (1-lambda) 2 /λ 1 )×100％
λ 1 Absorbance before flocculation experiment
λ 2 Absorbance after flocculation experiment
| Comparative example 1 | Example 1 | Example 2 | Example 3 | |
| First removal rate | 92.16% | 94.56% | 93.87% | 93.45% |
| Second removal rate | 88.32% | 87.45% | 87.60% | |
| Third removal rate | 78.82% | 78.60% | 77.98% |
As can be seen from Table 1, the composite flocculant with magnetic nano particles added on the traditional flocculant can realize magnetic separation under the action of an external magnetic field, the removal rate is also increased, the coagulation effect is improved compared with that of the traditional flocculant, the second and third coagulation can be carried out on the simulated water sample after the first coagulation of the composite flocculant is recovered, and the removal rate is reduced but still can reach more than 50%.
Example 1 magnetic magnesium aluminum polysilicate-starch composite flocculation (Fe 3 O 4 -PSAM-St) and the comparative magnesium aluminum polysilicate-starch composite flocculant (PSAM-St) are shown in FIG. 1.
From FIG. 2 at 1644.84cm -1 Characteristic absorption peak at-c=o, at 605.14cm -1 The peak at the position is the bending vibration absorption peak of the newly generated Si-O-Al and Si-O-Mg bond, which shows that PSi (polysilicic acid) is bridged with aluminum and magnesium hydroxyl groups to generate new Si-O-Al and Si-O-Mg bond, and the position of 1151cm < -1 > is the 2 times frequency peak of Fe-O, which shows that the magnetic nano particles are successfully compounded with the polysilicate aluminum magnesium-starch and are connected by chemical bonds to generate the magnetic compound flocculant.
To further illustrate the successful compounding of the magnetic nanoparticles with the magnesium aluminum polysilicate-starch composite flocculant, PSASST and Fe, respectively 3 O 4- PSAM-St was powder diffraction tested and the results are shown in FIG. 2.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (9)
1. The preparation method of the magnetic magnesium aluminum polysilicate-starch composite flocculant is characterized by comprising the following steps of:
first, fe is prepared 3 O 4 Washing the magnetic nano particles with absolute ethyl alcohol and ultrapure water, drying, and finally grinding into powder to obtain Fe 3 O 4 Magnetic nano particles are stirred in water bath to obtain Fe 3 0 4 Solution, after that in Fe 3 0 4 Adding sodium silicate into the solution, stirring until the sodium silicate is dissolved, regulating the PH of the solution, and performing activation treatment to obtain a magnetic polysilicic acid solution, wherein the amount of added sodium silicate powder is 36.0324-48.0432g; then adding 0.4-0.7mol/L of magnesium salt of aluminum salt 0.5-1.1mol/L into the magnetic polysilicic acid solution, and performing activation treatment to prepare the magnetic polysilicic acid magnesium flocculant; and finally, adding a proper amount of starch solution into the obtained magnetic aluminum magnesium polysilicate solution, and finally obtaining the magnetic aluminum magnesium polysilicate-starch composite flocculant through water bath and other processes.
2. The method for preparing a magnetic magnesium aluminum polysilicate-starch composite flocculant according to claim 1, wherein the step (1) uses FeCl 3 ·6H 2 O and FeCl 2 ·4H 2 O synthesizes Fe 3 O 4 ；FeCl 3 ·6H 2 The concentration range of O preparation is approximately 0.25-0.32mol/L; feCl 2 ·4H 2 The concentration range of O preparation is approximately 0.08-0.16mol/L; mixing the two materials, and adding ammonia water during mixing.
3. The method for preparing the magnetic magnesium aluminum polysilicate-starch composite flocculant according to claim 1, wherein the activation treatment in the step (2) is carried out by stirring in a water bath at 35-45 ℃ for 1.5-2.5h, and standing and curing for 2-8h.
4. The method for preparing the magnetic magnesium aluminum polysilicate-starch composite flocculant according to claim 1, wherein the water bath temperature in the step (3) is 30-50 ℃, the stirring time is 1.5-2.5h, and the standing and curing time is 3-8h.
5. The method for preparing the magnetic magnesium aluminum polysilicate-starch composite flocculant according to claim 1, wherein in the step (4), starch is pretreated with 0.5-1.5% acetic acid to prepare a starch solution.
6. The method for preparing a magnetic magnesium aluminum polysilicate-starch composite flocculant according to claim 1, wherein the concentration of starch in the step (4) is 6% -9%.
7. The method for preparing the magnetic magnesium aluminum polysilicate-starch composite flocculant according to claim 1, wherein the molar ratio of aluminum ions to magnesium ions is 8:2.
8. the method for preparing a magnetic magnesium aluminum polysilicate-starch composite flocculant according to claim 1, wherein in the step (3), the molar ratio of aluminum ions to magnesium ions is (5-9): (1-5).
9. The method for preparing the magnetic magnesium aluminum polysilicate-starch composite flocculant according to claim 1, wherein the mass ratio of starch to silicon element in polysilicic acid is 0.03-0.06.
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