CN117339396B - Film pollution control method of hydrogel modified granular activated carbon coupling pattern film - Google Patents
Film pollution control method of hydrogel modified granular activated carbon coupling pattern film Download PDFInfo
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- CN117339396B CN117339396B CN202311585546.3A CN202311585546A CN117339396B CN 117339396 B CN117339396 B CN 117339396B CN 202311585546 A CN202311585546 A CN 202311585546A CN 117339396 B CN117339396 B CN 117339396B
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- 239000000017 hydrogel Substances 0.000 title claims abstract description 35
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 25
- 230000008878 coupling Effects 0.000 title claims abstract description 10
- 238000010168 coupling process Methods 0.000 title claims abstract description 10
- 238000005859 coupling reaction Methods 0.000 title claims abstract description 10
- 238000011954 pollution control method Methods 0.000 title claims abstract description 10
- 239000012528 membrane Substances 0.000 claims abstract description 93
- 239000002245 particle Substances 0.000 claims abstract description 82
- 238000000034 method Methods 0.000 claims abstract description 29
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 24
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 6
- IXPNQXFRVYWDDI-UHFFFAOYSA-N 1-methyl-2,4-dioxo-1,3-diazinane-5-carboximidamide Chemical compound CN1CC(C(N)=N)C(=O)NC1=O IXPNQXFRVYWDDI-UHFFFAOYSA-N 0.000 claims description 18
- 235000010413 sodium alginate Nutrition 0.000 claims description 18
- 239000000661 sodium alginate Substances 0.000 claims description 18
- 229940005550 sodium alginate Drugs 0.000 claims description 18
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims description 10
- 239000002033 PVDF binder Substances 0.000 claims description 9
- 229920002981 polyvinylidene fluoride Polymers 0.000 claims description 9
- 239000000463 material Substances 0.000 claims description 8
- 238000004140 cleaning Methods 0.000 claims description 7
- 238000007790 scraping Methods 0.000 claims description 7
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 239000000178 monomer Substances 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 5
- 239000001110 calcium chloride Substances 0.000 claims description 4
- 229910001628 calcium chloride Inorganic materials 0.000 claims description 4
- 238000004132 cross linking Methods 0.000 claims description 4
- WHNWPMSKXPGLAX-UHFFFAOYSA-N N-Vinyl-2-pyrrolidone Chemical compound C=CN1CCCC1=O WHNWPMSKXPGLAX-UHFFFAOYSA-N 0.000 claims description 3
- 239000004952 Polyamide Substances 0.000 claims description 3
- 239000004695 Polyether sulfone Substances 0.000 claims description 3
- 229920002582 Polyethylene Glycol 600 Polymers 0.000 claims description 3
- 229920003081 Povidone K 30 Polymers 0.000 claims description 3
- 238000005266 casting Methods 0.000 claims description 3
- 239000004745 nonwoven fabric Substances 0.000 claims description 3
- 238000005191 phase separation Methods 0.000 claims description 3
- 229920002492 poly(sulfone) Polymers 0.000 claims description 3
- 229920002647 polyamide Polymers 0.000 claims description 3
- 229920006393 polyether sulfone Polymers 0.000 claims description 3
- 239000003431 cross linking reagent Substances 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims description 2
- 230000001678 irradiating effect Effects 0.000 claims description 2
- 230000001105 regulatory effect Effects 0.000 claims description 2
- 238000002791 soaking Methods 0.000 claims description 2
- 238000003756 stirring Methods 0.000 claims description 2
- FXIVKZGDYRLHKF-UHFFFAOYSA-N C(C)OP(OC(C1=C(C=C(C=C1C)C)C)=O)(=O)C1=CC=CC=C1 Chemical compound C(C)OP(OC(C1=C(C=C(C=C1C)C)C)=O)(=O)C1=CC=CC=C1 FXIVKZGDYRLHKF-UHFFFAOYSA-N 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 15
- 230000008569 process Effects 0.000 abstract description 12
- 239000003344 environmental pollutant Substances 0.000 abstract description 7
- 231100000719 pollutant Toxicity 0.000 abstract description 7
- 230000007774 longterm Effects 0.000 abstract description 6
- 238000001471 micro-filtration Methods 0.000 abstract description 6
- 230000015572 biosynthetic process Effects 0.000 abstract description 5
- 230000002195 synergetic effect Effects 0.000 abstract description 5
- 238000011065 in-situ storage Methods 0.000 abstract description 4
- 238000000108 ultra-filtration Methods 0.000 abstract description 4
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 abstract 1
- 239000010410 layer Substances 0.000 description 6
- 230000008901 benefit Effects 0.000 description 5
- 238000005265 energy consumption Methods 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 4
- 230000009471 action Effects 0.000 description 3
- 238000005243 fluidization Methods 0.000 description 3
- 230000009467 reduction Effects 0.000 description 3
- 230000004907 flux Effects 0.000 description 2
- 238000005374 membrane filtration Methods 0.000 description 2
- 238000009285 membrane fouling Methods 0.000 description 2
- 230000032683 aging Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000000635 electron micrograph Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000012065 filter cake Substances 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 238000006748 scratching Methods 0.000 description 1
- 230000002393 scratching effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 238000012876 topography Methods 0.000 description 1
- 231100001234 toxic pollutant Toxicity 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D65/00—Accessories or auxiliary operations, in general, for separation processes or apparatus using semi-permeable membranes
- B01D65/02—Membrane cleaning or sterilisation ; Membrane regeneration
Abstract
The invention discloses a membrane pollution control method of a hydrogel modified granular active carbon coupling pattern membrane, which is used for ultrafiltration, microfiltration, membrane bioreactors and other various water treatment systems through the synergistic effect of modified active carbon granules and the pattern membrane. According to the invention, the hydrogel layer is synthesized on the surfaces of the GAC particles in situ, so that the control effect of the fluidized particles on large-particle membrane pollutants is improved, meanwhile, the damage to the membrane is greatly reduced or eliminated on the flexible surface of the hydrogel, and the carbon loss caused by direct collision of the GAC particles is reduced. Meanwhile, the pattern film is further coupled, and the formation of small particle film pollution is controlled. The synergistic effect of the two can simultaneously and comprehensively control membrane pollution caused by various different particle pollutants, and long-term stable operation of the process is realized.
Description
Technical Field
The invention relates to the technical field of water treatment, in particular to a membrane pollution control method of a hydrogel modified granular activated carbon coupling pattern membrane.
Background
Currently, the world population is continually increasing and the industry demand is continually increasing, resulting in a significant reduction in available water resources. The membrane technologies such as ultrafiltration/microfiltration and the like are widely applied to water treatment, and compared with the traditional method, the method has the advantages of high treatment efficiency, low energy consumption, small occupied area and the like. However, membrane fouling is still a key bottleneck restricting membrane application, resulting in a great reduction in membrane flux, resulting in an increase in operating pressure or a serious decrease in water flux, and when membrane fouling reaches a certain level, the operation needs to be stopped and the membrane is chemically cleaned to restore its permeability, but the chemical cleaning of the membrane accelerates the aging damage of the membrane, and generates a large amount of toxic pollutants, resulting in serious negative effects. In recent years, the particle fluidized bed membrane pollution control method is attracting more attention, and has the advantages of low energy consumption, simple operation, sustainable operation, environmental protection and the like. However, in long-term running operation, fluidized particles may cause serious damage to the membrane surface, so that the technology cannot be applied to the actual water treatment process, and in addition, the membrane pollution control effect on the formation of small particles is poor. The existing particle fluidized bed membrane pollution control method has the following defects: (1) In long-term operation, the scraping action of fluidized particles can cause serious damage to the surface of the membrane, weaken the interception action of the membrane, even lead to rupture of the membrane, and increase the replacement cost of the membrane; (2) The particle fluidized bed method is effective only for membrane pollution formed by large particles, but the control effect is still to be improved; (3) The fluidized particles have poor pollution control effect on the small particle membrane, and can not realize continuous and stable operation of the water treatment process.
Based on the above-mentioned current situation, there is a need to develop a novel membrane pollution control technology to comprehensively and effectively control membrane pollution formation while reducing damage to the membrane surface.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a membrane pollution control method of a hydrogel modified granular activated carbon coupling pattern membrane, which is used for various water treatment systems such as ultrafiltration, microfiltration, membrane bioreactors and the like. Firstly, a hydrogel layer with a certain thickness is synthesized on the surface of granular activated carbon in situ, so that the control effect of fluidized particles on large-particle membrane pollutants is improved, and meanwhile, the damage of the fluidization of the particles on the membrane surface and the release of powdered carbon caused by direct collision of the granular activated carbon are weakened or eliminated. On the basis, the pattern film is further coupled, and the formation of the pollution of the small particle film can be effectively controlled due to the large surface area and the rugged surface of the pattern film. The synergistic effect of the modified activated carbon particles and the pattern film can simultaneously and comprehensively control organic pollution, inorganic pollution, biological pollution and the like of the film caused by various scale pollutants, meanwhile, the damage to the film is greatly reduced or eliminated on the flexible surface of the hydrogel, and the long-term stable operation of the process can be realized.
The technical scheme for realizing the invention is as follows:
a membrane pollution control method of hydrogel modified granular active carbon coupling pattern membrane, in the water treatment system, pattern membrane assembly is selected and filled with hydrogel modified GAC particles;
the hydrogel-modified GAC particles are prepared by the following method:
(1) Sodium Alginate (SA) is selected as a hydrogel monomer material, and calcium chloride is selected as a monomer cross-linking agent;
(2) Preparing sodium alginate solution with the concentration of 1.0-10.0 wt%, regulating the temperature to 20-90 ℃ and the pH value to 3-9, soaking and cleaning GAC particles until water is clear, drying the GAC particles, adding the GAC particles into the sodium alginate solution, and stirring for 6-12h to ensure that the surface of the GAC is completely wrapped by the sodium alginate solution;
(3) Adding GAC particles fully contacted with sodium alginate into a calcium chloride solution with the concentration of 0.2-5.0wt%, then adding a photoinitiator TPO-L with the concentration of 0.1-1.0wt% into the calcium chloride solution, standing for at least 1min, taking out, uniformly taking out the particles, and putting the particles into an ultraviolet cross-linking instrument for irradiation for 1-3min to form stable hydrogel-coated GAC particles.
Preferably, the patterned membrane is made of polysulfone, polyethersulfone, polyvinylidene fluoride or polyamide material.
Preferably, the pattern film is prepared from polyvinylidene fluoride, and the specific method comprises the following steps:
(1) 15-20 wt% of polyvinylidene fluoride, 5wt% of PEG600, 5wt% of PVP K30 and the balance of DMF are added into a 50mL round bottom flask, and stirred at room temperature until a uniform and transparent solution is obtained;
(2) Filtering the solution, defoaming for 24 hours in a vacuum oven at 40 ℃, casting and scraping the solution on non-woven fabrics by adopting a scraper with the amplitude height of 0.01-0.20 cm;
(3) Immersing in deionized water (20-50 ℃) for phase separation, and cleaning the membrane with deionized water for 3-5 times after 24 hours.
Preferably, the sodium alginate solution has a temperature of 70 ℃ and a pH of 5.
Preferably, the molar ratio of calcium chloride to sodium alginate is 0.1-1.0.
Preferably, the hydrogel-modified GAC particles are present in the patterned membrane assembly in an amount of 30-50%.
Preferably, the hydrogel-modified GAC particles are 50% loaded in the patterned membrane assembly.
Preferably, the film surface of the pattern film is provided with a wavy micropattern having an amplitude height of 0.10-0.20 cm.
Preferably, the GAC particles have a particle size of 1.20-3.00mm.
Preferably, the hydrogel is wrapped with a thickness of 0.50-1.50mm.
The beneficial effects of the invention are as follows: the invention wraps the hydrogel on the surface of the granular activated carbon by using an in-situ synthesis method, and the hydrogel is a three-dimensional net-shaped structure material with extremely affinity, so that the hydrogel is adopted as a modified material, the pollution control effect of the membrane is obviously improved, and the soft texture plays a good role in protecting the membrane. The modified granular active carbon is in a fluidized state, and a large-volume filter cake layer which is originally compact on the surface of the membrane is removed by utilizing the scraping action of hydrogel, so that the membrane pollution is weakened. The invention can cooperatively control the membrane pollution of various systems such as microfiltration, ultrafiltration, membrane bioreactors and the like by utilizing the advantages of the modified activated carbon and the pattern membrane, obviously improve the membrane pollution control effect, improve the operation period of the reactors and reduce the energy consumption and operation cost. In addition, the compact flexible hydrogel layer is attached to the surface of the granular activated carbon, so that the damage of fluidized particles to the surface of the membrane in long-term operation can be weakened, the membrane replacement period is reduced, the stable membrane interception effect is maintained, meanwhile, carbon powder released by fluidization collision of GAC particles is reduced, and compared with the prior art, the whole process can achieve a better membrane pollution control effect with lower energy consumption and lower cost.
Drawings
In order to more clearly illustrate the embodiments of the invention or the technical solutions in the prior art, the drawings that are required in the embodiments or the description of the prior art will be briefly described, it being obvious that the drawings in the following description are only some embodiments of the invention, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIGS. 1 (a) and 1 (b) are topography diagrams of a conventional GAC particle and a hydrogel-coated GAC particle, respectively;
FIG. 2 is a schematic illustration of the application of the present invention in membrane water treatment;
FIG. 3 is a graph of TMP (kPa) at the same time for modified GAC particles and ordinary GAC particles at the same particle size;
FIGS. 4 (a) and 4 (b) are graphs of TMP (kPa) at the same time for a flat film and a patterned film, respectively, coupling modified GAC particles;
FIGS. 5 (a) and 5 (b) are electron microscopy images of the membrane surface after filtration of modified GAC particles with normal GAC particles for 15 h.
Detailed Description
The technical solutions of the present invention will be clearly and completely described in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments 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 any inventive effort, are intended to be within the scope of the invention.
The following examples exemplify the use of the invention in the treatment of water in a microfiltration system.
Cleaning GAC particles at 70 ℃ under the condition of pH=5, putting the cleaned GAC particles into a sodium alginate solution with the concentration of 2wt% for fully mixing for 24 hours, fully wrapping sodium alginate monomers on the surfaces of the GAC particles, putting the particles into a calcium chloride solution with the concentration of 1wt% for crosslinking, adding a photoinitiator TPO-L with the concentration of 0.2wt% into the calcium chloride solution, standing for 1min, taking out, putting into an ultraviolet crosslinking instrument, and irradiating for 2min, so that the sodium alginate monomers are more firmly adhered on the surfaces of the GAC particles, as shown in figure 1. The surface appearance of the GAC particles (figure 1 (b)) coated with the Hydrogel (HD) is obviously different from that of the common GAC particles (figure 1 (a)), the surface of the GAC particles containing the hydrogel is smoother, and a silvery white hydrogel is obviously coated. The combination of GAC and hydrogel plays a role of 1+1 > 2 to achieve better membrane pollution control effect.
In the membrane filtration process, organic pollutants in water can be adsorbed to the surface of the membrane, a layer of pollutants is formed on the surface of the membrane, GAC particles have the effect of scraping the surface of the membrane, and under the drive of water flow, the GAC is continuously utilized to scrape the surface of the membrane, so that the accumulated pollution layers on the membrane are reduced, the purpose of slowing down membrane pollution is realized, and the transmembrane pressure difference is reduced. And the GAC particles wrap the hydrogel, so that the scraping of the GAC particles on the membrane is slowed down in the fluidization process, the service life of the membrane is prolonged, and compared with the existing membrane pollution control technology, the membrane pollution control method has the advantage that a better membrane pollution control effect can be achieved with lower energy consumption.
The prepared hydrogel-modified GAC particles were used in a membrane process water treatment system as shown in fig. 2. In the above described microfiltration system, hydrogel-modified GAC particles were filled in a pattern membrane module at a loading level of 50%. The pattern film can be made of polysulfone, polyethersulfone, polyvinylidene fluoride, polyamide and other materials, and as a preferred implementation mode, the pattern film is prepared by using polyvinylidene fluoride, and the specific method is as follows: (1) Polyvinylidene fluoride (20 wt%), PEG600 (5 wt%), PVP K30 (5 wt%) and DMF (70 wt%) were added to a 50mL round bottom flask and stirred at room temperature until a homogeneous, clear solution was obtained; (2) Filtering the solution, defoaming for 24 hours in a vacuum oven at 40 ℃, casting and scraping the solution on a non-woven fabric by adopting a scraper with the amplitude height of 0.10 cm; (3) Immersing in deionized water (30 ℃) for phase separation, and cleaning the membrane with deionized water for 4 times after 24 hours. The film surface was provided with a wavy micropattern having an amplitude height of 0.10 cm.
The object of treatment is lake water, which is conveyed from a right beaker to a pattern membrane assembly through a pump, and then is circulated back to the right beaker from the upper end, the process lasts for 15 hours, membrane pollution is formed on the surface of the pattern membrane in the process, and the pollution situation gradually increases along with the time.
In this example, the film contamination control cases without any GAC particles, with addition of ordinary GAC particles of the same particle size, and modified GAC particles were compared, respectively, and the results are shown in fig. 3. As is evident from fig. 3, after 15h of filtration, the transmembrane pressure difference (TMP) curve of the original membrane filtration was the highest, followed by the addition of the normal GAC particle group, and the modified GAC particle group was the lowest. It was demonstrated that the addition of GAC significantly reduced the transmembrane pressure difference, and that the transmembrane pressure difference was again reduced after the surface of the GAC coated the hydrogel at the same particle size.
Fig. 4 (a) and 4 (b) show TMP (kPa) graphs of the planar film and the patterned film under exactly the same conditions and particle filling rate, respectively. As can be seen from the figure, the transmembrane pressure difference after coupling the patterned membrane is lower, which reveals the advantages of the patterned membrane, which can bring about better membrane pollution control effect under the synergistic effect with the modified GAC.
Figure 5 shows the reduction of membrane surface damage by modified GAC. Conventional GAC particles fluidize in the membrane module without damaging the membrane for a short period of time, but scratch the membrane surface for a long period of time (15 h) with significant scratching occurring on the membrane surface, as shown in fig. 5 (b). The modified GAC surface layer is wrapped by hydrogel, and the impact force of the membrane contacted with the GAC is obviously reduced in the process of mutual friction, so that the damage degree of the surface is greatly reduced, as shown in fig. 5 (a).
In conclusion, according to the invention, the hydrogel layer is synthesized on the surface of the GAC particles in situ, so that the control effect of fluidized particles on large-particle membrane pollutants is improved, and meanwhile, the damage to the membrane is greatly reduced or eliminated on the flexible surface of the hydrogel. Further coupling the pattern film to control the formation of small particle film pollution. The synergistic effect of the two can simultaneously and comprehensively control membrane organic pollution, membrane inorganic pollution, membrane biological pollution and the like caused by various scale pollutants, and realize long-term stable operation of the process.
The foregoing description of the preferred embodiments of the invention is not intended to be limiting, but rather is intended to cover all modifications, equivalents, alternatives, and improvements that fall within the spirit and scope of the invention.
Claims (10)
1. A membrane pollution control method of a hydrogel modified granular active carbon coupling pattern membrane is characterized in that a pattern membrane component is selected and filled with hydrogel modified GAC particles in a water treatment system;
the hydrogel-modified GAC particles are prepared by the following method:
(1) Sodium Alginate (SA) is selected as a hydrogel monomer material, and calcium chloride is selected as a monomer cross-linking agent;
(2) Preparing sodium alginate solution with the concentration of 1.0% -10.0wt%, regulating the temperature to 20-90 ℃ and the pH value to 3-9, soaking and cleaning GAC particles until water is clear, drying the GAC particles, adding the GAC particles into the sodium alginate solution, and stirring for 6-12h to ensure that the surface of the GAC is completely wrapped by the sodium alginate solution;
(3) Adding GAC particles fully contacted with sodium alginate into a calcium chloride solution with the concentration of 0.2-5.0wt%, then adding a photoinitiator 2,4, 6-trimethylbenzoyl ethyl phenylphosphonate (TPO-L) with the concentration of 0.1-1.0wt% into the calcium chloride solution, standing for at least 1min, taking out the particles, uniformly putting the particles into an ultraviolet crosslinking instrument, and irradiating for 1-3min to form stable hydrogel-coated GAC particles.
2. The method of claim 1, wherein the patterned membrane is made of polysulfone, polyvinylidene fluoride, or polyamide material.
3. The method of claim 2, wherein the patterned film is prepared from a polyethersulfone material.
4. The method according to claim 2, wherein the patterned film is made of polyvinylidene fluoride, and the specific method is as follows:
(1) 15wt% -20wt% polyvinylidene fluoride, 5wt% PEG600, 5wt% PVP K30 and the balance DMF are added to a 50mL round bottom flask and stirred at room temperature until a homogeneous transparent solution is obtained;
(2) Filtering the solution, defoaming 24h in a vacuum oven at 40 ℃, casting and scraping the solution on a non-woven fabric by adopting a scraper with the amplitude height of 0.01-0.20 cm;
(3) Immersing in deionized water at 20-50 ℃ for phase separation, and cleaning the membrane with deionized water for 3-5 times after 24-h.
5. The method according to claim 1, wherein the molar ratio of calcium chloride to sodium alginate is 0.1-1.0.
6. The method of claim 1, wherein the hydrogel-modified GAC particles are present in an amount of 30-50% of the patterned membrane assembly.
7. The method of claim 6, wherein the hydrogel-modified GAC particles are present in an amount of 50% of the patterned membrane assembly.
8. The method of claim 4, wherein the patterned film has a film surface provided with a wavy micropattern having an amplitude height of 0.10-0.20 cm.
9. The method of claim 1, wherein the GAC particles have a particle size of 1.20 to 3.00 a mm.
10. The method of claim 1, wherein the hydrogel has a package thickness of 0.50-1.50mm.
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