CN113912194B - Modified microbial flocculant and application thereof in retarding membrane pollution - Google Patents
Modified microbial flocculant and application thereof in retarding membrane pollution Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F3/00—Biological treatment of water, waste water, or sewage
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Abstract
The invention relates to the field of microbial flocculant, and discloses a modified microbial flocculant, wherein acrylamide and acryloyloxyethyl are grafted in the microbial flocculantTrimethyl ammonium chloride. A preparation method of a modified microbial flocculant comprises the following steps: step I: adding a microbial flocculant solution into pure water, and then sequentially adding acrylamide and acryloyloxyethyl trimethyl ammonium chloride monomer, and stirring by using a magnetic stirrer to generate emulsion; step II: regulating the solution, adding the initiator and then using pure N 2 Oxygen is removed; step III: after the oxygen expelling is completed, adding sodium bisulfate and heating in a water bath; step IV: after the graft copolymerization process is completed, curing the reactant, and then repeatedly washing and purifying the reactant by using acetone and absolute ethyl alcohol to remove unreacted monomers in the modified microbial flocculant; step V: the modified microbial flocculant is freeze-dried and stored. Practice proves that the membrane flux is increased by 79.4% and the total pollution resistance is reduced by 90.3% after the modified microbial flocculant is added.
Description
Technical Field
The invention relates to the field of microbial flocculant, in particular to a modified microbial flocculant and application thereof in slowing down membrane pollution.
Background
The aerobic granular sludge membrane bioreactor (AGMBR) can be used as a novel water treatment technology with wide prospects, and can effectively treat and recycle urban sewage. AGMBR uses aerobic granular sludge to replace activated sludge as a main body of biochemical reaction, so that pollutants and suspended matters in municipal sewage can be removed efficiently. However, membrane fouling is a barrier limiting the large-scale development and application of AGMBRs. Particles, microorganisms, inorganic ions, extracellular polymers, soluble microbial products, etc., can all be adsorbed or aggregated on the membrane to promote contamination of the membrane.
At present, the pre-coagulation can efficiently remove organic pollutants and particulate matters in sewage, reduce the running cost, and is one of the most effective and commonly used membrane pollution control technologies. Among these, the choice of flocculant is an important factor in determining the pre-coagulation effect. The combination of the inorganic flocculant and the organic flocculant can also form larger floccules, so that flocculation effect is improved. However, some researches indicate that the artificially synthesized organic polymeric flocculant such as polyacrylamide, polydimethyl diallyl ammonium chloride and the like is difficult to biodegrade, and has potential harm to the environment. Therefore, in order to reduce secondary pollution to water body and keep good flocculation effect, the microbial flocculant with the characteristics of biodegradability, no secondary pollution and the like is a green flocculant which can possibly replace the traditional organic polymer flocculant.
The microbial flocculant has a plurality of functional groups, and can treat various pollutants; however, the low charge density can increase the dosage of the microbial flocculant, which is an application obstacle affecting the microbial flocculant in pollutant removal and membrane pollution alleviation.
Disclosure of Invention
The invention aims to provide a modified microbial flocculant and application thereof in alleviating membrane pollution, so as to solve the problem of application obstacle of the existing microbial flocculant in pollutant removal and membrane pollution alleviation.
In order to achieve the above purpose, the invention adopts the following technical scheme: a modified microbial flocculant comprises a microbial flocculant, wherein acrylamide and acryloyloxyethyl trimethyl ammonium chloride are grafted in the microbial flocculant.
On the other hand, the technical scheme also provides a preparation method of the modified microbial flocculant, which comprises the following steps:
step I: adding a microbial flocculant into pure water, sequentially adding acrylamide and acryloyloxyethyl trimethyl ammonium chloride monomer, and stirring to generate emulsion;
step II: adjusting the pH value of the solution, adding an initiator and then driving oxygen;
step III: after the oxygen expelling is completed, adding sodium bisulfate and heating in a water bath;
step IV: after the graft copolymerization process is completed, curing the reactant, and then washing and purifying to remove unreacted monomers in the modified microbial flocculant;
step V: the modified microbial flocculant is freeze-dried and stored.
On the other hand, the technical scheme prepares the application of the modified microbial flocculant as a membrane pollution slowing agent or a membrane pollution treatment agent.
The principle and the advantages of the scheme are as follows: in the technical scheme, the microbial flocculant has the characteristics of no toxicity, environmental protection and safety, and has wide application field. Acrylamide and acryloyloxyethyl trimethyl ammonium chloride monomer have certain flocculation capacity, and can be independently used as flocculant, but the flocculation effect is limited. The microbial flocculant is subjected to grafting modification, acrylamide and an acryloyloxyethyl trimethyl ammonium chloride monomer are grafted on a molecular chain of the microbial flocculant, and the acrylamide is used as a high-activity monomer for more effectively attacking the microbial flocculant, plays a role in bridging in graft copolymerization of the acryloyloxyethyl trimethyl ammonium chloride and the microbial flocculant, can greatly improve the graft modification effect, and can improve the dissolubility and flocculation efficiency of the microbial flocculant after grafting modification, so that the treatment effect on membrane pollution is improved, and the membrane flux is increased. In the research and development process of the subject, the preparation of the modified microbial flocculant has great technical difficulty, and the selection of an initiator, pH, washing and purification and the like can have important influence on the modification effect of the microbial flocculant. In the technical scheme, before an initiator is added to carry out grafting copolymerization, the pH of the system is regulated to ensure that the copolymerization is carried out under the optimal condition, and researches show that the pH value of the reaction system can influence the reaction kinetics, when the pH value is too low, acyl groups in acrylamide easily react in molecules to cause the polymer to crosslink, but the too high pH value can accelerate chain transfer. After the grafting copolymerization is finished, the components in the system can be fully reacted by curing treatment; acetone and absolute ethyl alcohol are used for removing unreacted monomers in the modified microbial flocculant, so that the purity of the modified microbial flocculant is improved. After the grafting copolymerization is finished, the purity of the modified microbial flocculant can be improved through purification, the adding amount of the unpurified modified microbial flocculant is larger than that of the purified modified microbial flocculant under the same membrane pollution slowing effect, namely, the flocculation effect and the membrane pollution control effect of the purified modified microbial flocculant are better under the same adding amount condition. In practical application, the modified microbial flocculant has good adsorption bridging capacity due to hydroxyl, amino and other groups, and the long-chain structure is also beneficial to the adsorption of pollutants. During the operation of AGMBR, the addition of the modified microbial flocculant significantly slows down the decay of the membrane flux and the accumulation of contaminants on the membrane surface.
Preferably, as a modification, the mass addition ratio of the microbial flocculant, the acrylamide and the acryloyloxyethyl trimethyl ammonium chloride is 1-3:4-12:2-6.
In the technical scheme, the addition ratio of the microbial flocculant, the acrylamide and the acryloyloxyethyl trimethyl ammonium chloride has an important influence on the modifying effect of the flocculant, and the modifying effect of the microbial flocculant can be reduced when the ratio is not used.
Preferably, as a modification, the mass addition ratio of the microbial flocculant, the acrylamide and the acryloyloxyethyl trimethyl ammonium chloride is 3:12:6.
in the technical scheme, the addition ratio is the optimal addition ratio verified by the test, and under the condition of the ratio, the microbial flocculant has good modification effect and good treatment effect on membrane pollution after modification.
Preferably, as a modification, the microbial flocculant is klebsiella pneumoniae fermentation broth.
In the technical scheme, the microbial flocculant is a polysaccharide substance extracted from klebsiella pneumoniae, and researches show that the functional groups of acyloxy and ammonium are grafted to glucan or carboxyl is grafted to chitosan, so that the microbial flocculant has the effect of synergistically strengthening flocculation effect. The modified microbial flocculant with more excellent flocculation effect can be prepared by introducing amino, ammonium and acyloxy groups into the molecular chain of the microbial flocculant through graft copolymerization of the microbial flocculant, acryloyloxyethyl trimethyl ammonium chloride and acrylamide.
Preferably, as a modification, in the step II, the pH is adjusted to 2-4, the initiator is potassium persulfate, and the addition amount of the initiator is 0.01-0.03mol/L and N 2 The oxygen-expelling time is 30min.
In the technical scheme, the pH value of the reaction system can influence the reaction kinetics, when the pH value is too low, acyl in acrylamide is easy to react in molecules to cause the polymer to crosslink, but too high pH value can accelerate chain transfer, and the pH range is a proper range value verified by a test. The potassium persulfate is an oxidation initiator, the graft copolymerization process is influenced by different addition concentrations of the initiator, and further the modification effect is influenced, and the grafting copolymerization effect can be ensured by the concentration of the initiator. In addition, the purpose of oxygen displacement is to avoid the occurrence of side reactions, thereby ensuring an efficient graft copolymerization process.
Preferably, as a modification, the concentration of sodium bisulfate in the step III is 0.01-0.03mol/L, and the heating temperature in the water bath is 60 ℃.
In the technical scheme, sodium bisulfate is a reduction initiator, and is cooperated with potassium persulfate to initiate a grafting copolymerization process, the different addition concentrations of the initiator can influence the grafting copolymerization process of the sodium bisulfate, so that the modification effect is influenced, and the grafting copolymerization effect can be ensured by the concentration of the initiator. The initiation temperature is an important factor influencing the graft copolymerization process, the proper temperature is favorable for the graft copolymerization, and the high reaction temperature can destroy the functional group and the space structure of the microbial flocculant, so that the treatment efficiency is reduced. In addition, the high temperature increases the chance of radical and chain termination collisions, which are not experimentally verified as optimal.
Preferably, as a modification, in step IV, the curing time is 12-24 hours.
In the technical scheme, the components in the system can be fully reacted by curing, the curing time is too short, the components are not fully reacted, and the modification effect is affected; the curing time is too long and does not have a substantial positive effect on the reaction, but affects the efficiency, and is the optimal curing time verified by the test.
Preferably, as an improvement, the addition amount of the modified microbial flocculant is 5-30mg/L, and the modified microbial flocculant is used in combination with polyaluminium chloride.
In the technical scheme, the polyhydroxy cation complex generated by polyaluminium chloride coordination hydrolysis shows strong electric neutralization capacity, so that pollutants in raw sewage are aggregated and larger floccules are formed. The polyaluminium chloride and the modified microbial flocculant are used in a combined mode, pollutants can be aggregated to form larger floccules, so that the pollutants are difficult to enter membrane holes, a loose and porous filter cake layer is formed on the surface of the membrane, and membrane pollution is reduced. Through practical application detection, the polyaluminum oxide and the modified microbial flocculant show a synergistic reinforcing effect after being used cooperatively, the membrane flux is increased by 79.4%, and the total pollution resistance is reduced by 90.3%.
Drawings
FIG. 1 shows the effect of modified microbial flocculant addition on the membrane filtration normalization flux of an aerobic granular sludge membrane bioreactor.
FIG. 2 shows the effect of modified microbial flocculant dosage on the membrane fouling resistance of an aerobic granular sludge membrane bioreactor.
Detailed Description
The following is a further detailed description of the embodiments:
examples 1-7 and comparative examples 1-12 are examples and comparative examples, respectively, of the present invention, and the examples and comparative examples differ only in the amounts of raw materials added and the process parameters for the preparation, and are specifically shown in table 1. And (3) injection: in the washing purification, it is indicated whether washing purification is performed or not.
TABLE 1
A modified microbial flocculant comprises a microbial flocculant, wherein acrylamide and acryloyloxyethyl trimethyl ammonium chloride are grafted in the microbial flocculant.
The preparation method of the modified microbial flocculant of the present invention will now be described in detail by taking example 6 as an example, comprising the steps of:
step I: adding 3wt% of microbial flocculant into pure water, wherein the microbial flocculant in the embodiment is klebsiella pneumoniae fermentation liquor (extracted polysaccharide substances), sequentially adding 12wt% of acrylamide and 6wt% of acryloyloxyethyl trimethyl ammonium chloride monomer, and stirring by using a magnetic stirrer to generate emulsion;
step II: adjusting the pH of the solution to 3, adding a potassium persulfate initiator with the concentration of 0.025mol/L, and then using pure N 2 Oxygen is removed for 30min;
step III: after the oxygen is removed, adding sodium bisulfate with the concentration of 0.025mol/L, and heating in a water bath at the temperature of 60 ℃;
step IV: after the graft copolymerization process is completed, curing the reactant for 12 hours, and then repeatedly washing and purifying the reactant by using acetone and absolute ethyl alcohol to remove unreacted monomers in the modified microbial flocculant;
step V: the modified microbial flocculant was placed in a vacuum freeze dryer for drying and stored in a drying dish.
Experimental example one: flocculation capability test of modified microbial flocculant
The modified microbial flocculants prepared in the above examples and comparative examples were subjected to cation degree measurement and molecular weight measurement by the following test methods, and the detection results are shown in table 2 (mean, n=3).
(one) cationicity measurement
The cationicity refers to the percentage of cationic structural units in a macromolecule to the total number of structural units, and is an important parameter for characterizing the charge property and charge density of the macromolecule. The experiment adopts silver nitrate precipitation titration method to measure the cationic degree of the polymer, so as to obtain AgNO 3 Solution as titrant, K 2 CrO 4 The solution served as an indicator. The measurement steps are as follows:
(1) Weigh about 0.3g of sample in beaker to the nearest 0.0002g;
(2) Adding 200mL of deionized water to dissolve, and adding 0.05mol/L K 2 CrO 4 0.5mL of the solution, and placing the solution on a magnetic stirrer for stirring;
(3) With 0.5mol/L AgNO 3 Slowly titrating the solution, and stopping titrating when brick red precipitation appears in the solution;
(4) AgNO for recording 3 Volume of solution. The cationicity is calculated according to the following formula:
x＝vc/[vc+(m-vcM 2 )/M 1 ]
wherein x is the sample cationicity,%; v is AgNO consumed 3 The volume of the solution; c is AgNO 3 The concentration of the solution; m is the mass of the weighed sample; m is M 1 Is the molecular weight of the acrylamide monomer; m is M 2 Molecular weight of cationic monomer.
(II) molecular weight measurement
The molecular weight of the flocculant may be calculated from the intrinsic viscosity. According to the national standard GB T12005.1-1989, the measurement steps are divided into four steps:
(1) Determination of the flow time t of the aqueous NaCl solution 0 : after pouring 1mol/L NaCl solution into a dry glass sand core funnel for filtration, transferring 10mL to a Ubbelohde viscometer by a pipette, vertically placing the solution in a constant-temperature water bath (30+/-0.05) DEG C for 10min, and measuring the flow-through time t of the NaCl solution. Measuring three times, controlling the error within 0.2s, calculating the average value t 0 The final measurement of the flow-through time of NaCl aqueous solution is obtained.
(2) Weighing 0.20-0.30g of flocculant product into a 250mL beaker, then adding 100mL of NaCl solution with the concentration of 2.00mol/L and 100mL of distilled water, fully stirring until the product is dissolved, and filtering the solution to obtain a sample solution.
(3) The flow-through time t of the sample solution was measured by the same measurement method as in step (1).
(4) And calculating the relative molecular mass, looking up a table by a result obtained by calculating the above formula, obtaining a corresponding [ eta ]. C value, dividing the value by the sample concentration c, and obtaining a result which is the intrinsic viscosity [ eta ] of the solution.
η r ＝t/t 0
c＝mS/V
Mr＝802·[η] 1.25
Wherein eta is r Is the relative viscosity; t is t 0 The flow-through time of the NaCl solution, s; t is the flowing time of the test solution, s; [ eta ]]Is the intrinsic viscosity, mL/g; s is the solid content of the sample,%; m is the mass of the sample and g; v is the volume of the test solution, mL; c is the concentration of the test solution, g/mL; mr is a relative moleculeQuality.
As can be seen from the data in Table 2, the cationic degree and molecular weight of examples 1-7 of the present invention are both good, the addition of too high and too low of the microbial flocculant results in a decrease in cationic degree and molecular weight, while the addition of too high and too low of the acrylamide adversely affects the flocculant, and in the adjustment of the pH in step II, too high or too low of the pH adversely affects the flocculant, resulting in a decrease in cationic quarter and molecular weight. The absence of washing purification results in a decrease in the cationic degree, whereas the absence of graft modification of the flocculant adversely affects both cationic degree and molecular weight, particularly a significant decrease in molecular weight.
TABLE 2
| Group of | Degree of cation (%) | Molecular weight (kDa) |
| Example 1 | 42 | 3500 |
| Example 2 | 31 | 3800 |
| Example 3 | 57 | 4500 |
| Example 4 | 48 | 4600 |
| Example 5 | 43 | 4200 |
| Example 6 | 75 | 5800 |
| Example 7 | 62 | 5100 |
| Comparative example 1 | 26 | 3100 |
| Comparative example 2 | 17 | 4000 |
| Comparative example 3 | 44 | 3900 |
| Comparative example 4 | 29 | 3600 |
| Comparative example 5 | 41 | 4600 |
| Comparative example 6 | 72 | 4100 |
| Comparative example 7 | 14 | 2500 |
| Comparative example 8 | 20 | 3000 |
| Comparative example 9 | 52 | 4700 |
| Comparative example 10 | 64 | 5200 |
| Comparative example 11 | 32 | 4600 |
| Comparative example 12 | 34 | 1200 |
Experimental example two: flocculation capability test of modified microbial flocculant and polyaluminium chloride combined
And (3) test design: the aerobic granular sludge is cultivated in a sequencing batch reactor with the height and the inner diameter of 1.0m and 0.14m respectively and the hydraulic retention time of 4h, and the sludge concentration is 3735-4291mg/L. After biochemical treatment of the aerobic granular sludge, a part of the synthetic municipal sewage enters a beaker test device and a membrane filter element to be further treated.
The pre-coagulation experiment is carried out in a beaker test device, and the coagulation process is as follows: raw water is firstly uniformly mixed in a beaker test device; at the rotating speed of 200rpm, adding polyaluminium chloride with the concentration of 50mg/L and rapidly stirring for 1min; then adding a certain concentration of modified microbial flocculant (flocculant prepared in example 6) at the same rotation speed, and stirring for 4min. Followed by stirring at 40rpm for 10min and then standing for 10min.
Filtration experiment: the membrane filter component has pore diameter of 0.1um and effective area of 43.0cm 2 The effective volume of the PTFE membrane was 300ml and the water inlet volume was 200ml. During membrane filtration, a nitrogen cylinder was connected to the filtration module to maintain a transmembrane pressure (TMP) of 0.05 MPa. In addition, in order to prevent rapid precipitation of suspended solids and flocks, the rotation speed of the magnetic stirrer was constant at 150rpm.
And respectively adding modified microbial flocculant with different concentrations into the system, and detecting and analyzing the membrane flux and the total pollution resistance after adding. The experimental design and results of each experimental group are shown in table 3 below and fig. 1 and 2. And (3) injection: in FIG. 2, raw water is a control group without flocculant, and the addition concentration of the rest of the components of polyaluminum chloride is 50mg/L; MMF is an English abbreviation of modified microbial flocculant, and the adding concentration of the MMF is (0, 5, 10, 20 and 30 mg/L) respectively. The four columns from left to right for each set of data in fig. 2 are: r is R m 、R t 、R r 、R ir 。
The formula:
1) Membrane flux:
wherein: j is membrane flux, L/(m) 2 H); v is the filtration volume, L; t is the filtering time, h; a is the effective filtration area of the membrane, m 2 .
J/J 0 : contaminant transmembrane flux/initial flux
2) Membrane resistance
Wherein: j (J) 0 Membrane flux when filtering pure water; j (J) 1 Membrane flux during sewage filtration; j (J) 2 For filtering pure water after cleaning the contaminated membraneMembrane flux; TMP is transmembrane pressure difference, pa; mu is the viscosity of the permeate, pa.s; r is R m Is the inherent resistance of the membrane; r is R t Is the total resistance of the membrane; r is R r Is a membrane reversible pollution resistance; r is R ir Is the irreversible pollution resistance of the membrane.
TABLE 3 Table 3
As can be seen from the data in Table 3, the combination effect of the modified microbial flocculant and the polyaluminum chloride is far from that the modified microbial flocculant and the polyaluminum chloride are used independently, and when the modified microbial flocculant and the polyaluminum chloride are combined, the synergistic effect of the modified microbial flocculant and the polyaluminum chloride is in a nonlinear relation, so that the addition amount of the modified flocculant is as follows: the addition amount of polyaluminum chloride is 1:5, and the best effect is achieved.
The foregoing is merely exemplary of the present invention, and specific technical solutions and/or features that are well known in the art have not been described in detail herein. It should be noted that, for those skilled in the art, several variations and modifications can be made without departing from the technical solution of the present invention, and these should also be regarded as the protection scope of the present invention, which does not affect the effect of the implementation of the present invention and the practical applicability of the patent. The protection scope of the present application shall be subject to the content of the claims, and the description of the specific embodiments and the like in the specification can be used for explaining the content of the claims.
Claims (6)
1. An application of a modified microbial flocculant as a membrane pollution reducing agent or a membrane pollution treating agent is characterized in that: the modified microbial flocculant comprises a microbial flocculant, wherein acrylamide and acryloyloxyethyl trimethyl ammonium chloride are grafted in the microbial flocculant; the mass addition ratio of the microbial flocculant to the acrylamide to the acryloyloxyethyl trimethyl ammonium chloride is 1-3:4-12:2-6; when the modified microbial flocculant is used, the modified microbial flocculant is combined with polyaluminium chloride, and the adding amount of the modified microbial flocculant is 5-30 mg/L;
the preparation method of the modified microbial flocculant comprises the following steps:
step I: adding a microbial flocculant into pure water, sequentially adding acrylamide and acryloyloxyethyl trimethyl ammonium chloride monomer, and stirring to generate emulsion;
step II: adjusting the pH value of the solution, adding an initiator and then driving oxygen;
step III: after the oxygen expelling is completed, adding sodium bisulfate and heating in a water bath;
step IV: after the graft copolymerization process is completed, curing the reactant, and then washing and purifying to remove unreacted monomers in the modified microbial flocculant;
step V: the modified microbial flocculant is freeze-dried and stored.
2. The use of a modified microbial flocculant according to claim 1 as a membrane pollution abatement agent or a membrane pollution abatement agent, characterized in that: the mass addition ratio of the microbial flocculant to the acrylamide to the acryloyloxyethyl trimethyl ammonium chloride is 3:12:6.
3. the use of a modified microbial flocculant according to claim 2 as a membrane pollution abatement agent or a membrane pollution abatement agent, characterized in that: the microbial flocculant is klebsiella pneumoniae fermentation liquor.
4. The use of a modified microbial flocculant as claimed in claim 3 as a membrane pollution abatement agent or a membrane pollution abatement agent, wherein: in the step II, the pH is regulated to 2-4, the initiator is potassium persulfate, the addition amount of the initiator is 0.01-0.03mol/L, and N 2 The oxygen-expelling time is 30min.
5. The use of a modified microbial flocculant as claimed in claim 4 as a membrane pollution abatement agent or a membrane pollution abatement agent, wherein: the concentration of sodium bisulfate in the step III is 0.01-0.03mol/L, and the water bath heating temperature is 60 ℃.
6. The use of a modified microbial flocculant as claimed in claim 5 as a membrane pollution abatement agent or a membrane pollution abatement agent, wherein: in the step IV, the curing time is 12-24 hours.
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