CN115322008B - Porous biological filler for purifying polluted seawater and preparation method and application thereof - Google Patents
Porous biological filler for purifying polluted seawater and preparation method and application thereof Download PDFInfo
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- C02F3/00—Biological treatment of water, waste water, or sewage
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Abstract
The invention discloses a porous biological filler for purifying polluted seawater and a preparation method and application thereof, belonging to the technical field of sewage treatment. The biological filler consists of an external porous mineral sphere and an embedded carbon source organism, wherein the mass ratio of the porous mineral sphere to the embedded carbon source organism is as follows: 7.5-8.5:1.5-2.5, wherein the porous mineral sphere has a single-channel and porous skeleton structure, the embedded carbon source organisms form a slow-release organic carbon source, and the biological filler contains various minerals, has large surface area of mutually communicated gaps, has the advantages of slow-release carbon source, contribution to biological oxidation reduction and the like. The porous biological filler prepared by the invention has larger specific surface area, communicated pore structure, multi-mineral component, slow-release organic carbon source and substances for promoting electron transfer, is not easy to harden, can remarkably improve the problems of slow growth, difficult aggregation and the like of water treatment microorganisms caused by conditions of high seawater salinity and the like, can be used for removing pollutants in polluted seawater, and has ideal nitrogen removal effect in particular.
Description
Technical Field
The invention belongs to the technical field of sewage treatment, and in particular relates to a porous biological filler for purifying polluted seawater, a preparation method and application thereof, which can be widely used for treating seawater polluted by nitrogen and organic compounds so as to achieve higher treatment requirements.
Background
Marine industry such as marine aquaculture produces a large amount of polluted seawater containing various organic matters and nitrogen compounds; for example, the excretion products of organisms and the rest of the bait in the marine aquaculture process increase the concentration of nitrogen pollutants and organic matters in the marine environment, resulting in marine pollution; due to the adverse effects of seawater salinity and other factors, water treatment microorganisms cannot produce high removal rates of pollutants like those in fresh water environments, and a considerable part of pollutants are discharged into seawater without being sufficiently removed, so that the marine environment is polluted.
The reason that the degradation of pollutants in seawater is more difficult than that in fresh water is that the conditions such as high salinity of seawater are not beneficial to the growth and aggregation of microorganisms, biological fillers are adopted to improve the biomass in a sewage treatment system, but the problems of small specific surface area, few available carbon sources, unfavorable biological oxidation reduction and the like caused by single filler components and non-communication of pores can be caused, the problems of low biomass and aggregation of microorganisms in a polluted seawater biological treatment device, unsatisfactory treatment effect and the like can be caused, and the biological fillers and effects applied to seawater treatment still need to be further developed and improved.
Disclosure of Invention
Aiming at the problems existing in the prior art, the invention provides a porous biological filler for purifying polluted seawater, and a preparation method and application thereof.
The technical scheme of the invention is that the porous biological filler for purifying polluted seawater comprises an external porous mineral sphere and an embedded carbon source organism blend, wherein the mass ratio of the porous mineral sphere to the embedded carbon source organism blend is as follows: 7.5-8.5:1.5-2.5, wherein the porous mineral sphere is provided with a single channel penetrating through the porous mineral sphere and a porous framework structure inside the porous mineral sphere, and the embedded carbon source organism blend forms a slow-release organic carbon source. The biological filler contains various mineral substances, has large surface area of interconnected gaps, has the advantages of slow release of carbon sources, contribution to biological oxidation reduction and the like.
Further, the porous mineral sphere is formed by bonding a plurality of particles through an organic low-temperature binder, wherein the particles are provided with a pore structure, and the pores are communicated inside the porous mineral sphere; the embedded carbon source organism blend permeates 60-80% by volume of the pores among the porous mineral sphere particles; the diameter of the single channel is 10% -25% of the diameter of the porous mineral sphere.
Further, the particles comprise the following components in percentage by weight: 16 to 19 percent of reduced iron powder, 3 to 5.5 percent of activated carbon powder, 3 to 5.5 percent of graphite powder, 15 to 19 percent of quartz powder, 3 to 5.5 percent of tourmaline powder, 3 to 5.5 percent of diatomite, 7 to 10 percent of zeolite powder, 3 to 5.5 percent of volcanic powder, 3 to 5.5 percent of medical stone powder, 0.5 to 1 percent of pore-forming agent, 0.8 to 1.2 percent of graphene and 25 to 30 percent of inorganic binder; these inorganic minerals are mixed, fired, crushed, sieved, and bonded to form the particles.
Further, the pore-forming agent comprises ammonium bicarbonate or ammonium carbonate.
Further, the inorganic binder includes sodium bentonite or calcium bentonite.
Further, the graphene is single-layer or few-layer or multi-layer graphene prepared by a physical method or a chemical method.
Further, the organic low temperature binder includes a methyl methacrylate or unsaturated polyester resin based binder.
Further, the embedded carbon source organism blend comprises the following components in percentage by weight: 1-2% of dissolution auxiliary agent, 10-15% of agar powder, 20-30% of straw powder, 10-15% of walnut shell powder, 15-20% of starch, 12-15% of glycerol, 3-6% of xanthan gum, 3-6% of trehalose, 5-7% of emulsifying agent and 5-10% of chitosan.
Further, the dissolution aid comprises dextrin or starch syrup or glucose.
Further, the starch comprises common starch or cross-linked starch; its advantages are low cost, easy degradation and forming paste.
Further, the emulsifier comprises sorbitol glyceride, sorbitan monooleate or monoglyceride;
further, the chitosan is acid-soluble chitosan.
A method for preparing a porous biological filler for purifying polluted seawater, which comprises the following steps:
(1) Preparing porous mineral spheres:
1) Mixing reduced iron powder (200 meshes), activated carbon powder (100 meshes), graphite powder (200 meshes), quartz powder (200 meshes), tourmaline powder (200 meshes), diatomite (100 meshes), zeolite powder (200 meshes), volcanic powder (100 meshes), medical stone powder (200 meshes), pore-forming agent and binder (200 meshes) and stirring uniformly to obtain an inorganic mixture.
2) Dispersing graphene with a dispersing agent, wherein the mass ratio of the graphene to the dispersing agent is 1:0.06-0.1.
3) Spraying the dispersed graphene accounting for 0.8-1.2% of the weight of the inorganic mixture and chlorine-free water accounting for 27-31% of the weight of the inorganic mixture onto the inorganic mixture, adding the graphene and chlorine-free water for multiple times, stirring the mixture uniformly again, stopping stirring the mixture until the mixture can be plastic, preparing wet filler particles by using a granulator, drying the particles, and roasting the particles to obtain the dry filler of the mixed components.
4) And mechanically crushing the dry filling materials of the mixed components, screening out particles with the particle size of 7-28 meshes, transferring the particles into a container, slowly adding an organic low-temperature binder, continuously stirring, immediately stopping when the mixture is basically plastic, transferring into a mould for granulating and drying to obtain the porous mineral sphere with a single channel penetrating the porous mineral sphere and a porous skeleton structure inside the porous mineral sphere.
(2) Preparing an embedded carbon source organism blend:
uniformly mixing a dissolution auxiliary agent, agar powder, straw powder, walnut shell powder, starch, glycerol, trehalose and chlorine-free water, and sequentially adding an emulsifier, xanthan gum and chitosan, wherein the chlorine-free water is intermittently added for 4-5 times; stirring in one direction in a water bath at 90-100 ℃ until gelatinization, and standing for 1-2h to obtain a blend; the material contains different types of carbon sources, can be continuously and slowly released within a period of time, and can be used for supplying different microbial degradation pollutants.
(3) Preparing porous biological filler:
adding the porous mineral spheres into the organic blend of the embedded carbon source, stirring in one direction, enabling the organic blend of the embedded carbon source to permeate into 60-80% of the volume of the inter-particle pores of the porous mineral spheres, reserving part of the pores, fishing out, transferring into a low-temperature container at 0-minus 20 ℃ for shaping, and then placing into a low-temperature oven at 40-45 ℃ for drying to obtain the porous biological filler.
The biological filler contains various mineral substances, has large surface area of interconnected gaps, has the advantages of slow release of carbon sources, contribution to biological oxidation reduction and the like.
Further, the dispersant comprises sodium dodecyl sulfate; step 3) drying the dried product at a dark and dry place or at a temperature of 50-75 ℃; the roasting condition of the step 3) is that; gradually heating from room temperature to 300-350 ℃ at a speed of 5-10 ℃/min, continuously roasting for 55-65 min, then heating to 650-700 ℃ and roasting for 25-35 min, and finally heating to 900-950 ℃ and roasting for 55-65 min; the particle size of the wet filler particles in the step 3) is 10-50 mm.
Use of a porous biological filler in seawater or freshwater contaminated with organic compounds.
Further, the organic compound includes a nitrogen-containing compound and a non-nitrogen-containing compound; the nitrogen-containing compound comprises a protein, an amino acid, urea, an amine or a nitro compound; the non-nitrogen containing compounds include carbohydrates, fats, phenols, aldehydes, ketones, non-nitrogen containing organic acids, hydrocarbons or synthetic detergents.
The invention has the beneficial effects that:
the channels and pores in the single-channel porous biological filler have a communicated pore structure, so that the surface area of the filler is increased, the microbial attachment growth is facilitated, the microbial mass can be increased, and the contact area with a water body can be increased; the particles forming the filler are composed of multi-component substances, and the particle size of the biological filler is increased by forming the filler by a plurality of particles, so that the biological filler is not easy to harden after long-term operation, and meanwhile, the multi-mineral components are beneficial to different metabolic processes of microorganisms; the embedded carbon source organism forms a slow-release organic carbon source, which can supplement the carbon source shortage in the polluted seawater treatment reactor, strengthen the heterotrophic denitrification process and improve the denitrification effect; the iron oxide, graphite powder and graphene in the filler accelerate the direct electron transfer process of microorganisms, pollutants and minerals, are beneficial to the rapid progress of the oxidation-reduction process, and can improve the pollutant removal performance.
The porous biological filler prepared by the invention has larger specific surface area, communicated pore structure, multi-mineral component, slow-release organic carbon source and substances for promoting electron transfer, is not easy to harden, can remarkably improve the problems of slow growth, difficult aggregation and the like of water treatment microorganisms caused by conditions of high seawater salinity and the like, can be used for removing pollutants in polluted seawater, and has ideal nitrogen removal effect in particular.
Drawings
FIG. 1 is a schematic diagram of a porous bio-filler according to the present invention; (a) a plan view; (b) S '-S' profile; (c) a K '-K' cross-sectional view; 1. porous mineral spheres, 2, single channel, 3, embedded carbon source organism blends.
FIG. 2 is an SEM image of the porous bio-filler prepared in example 1; (a) pre-use filler; (b) post-use filler.
FIG. 3 is an EDS diagram of the porous bio-filler prepared in example 1; (a) pre-use filler; (b) post-use filler.
FIG. 4 is an XRD pattern of the porous bio-filler prepared in example 1; (a) pre-use filler; (b) post-use filler.
Detailed Description
The following non-limiting examples will enable those of ordinary skill in the art to more fully understand the invention and are not intended to limit the invention in any way.
Example 1
A method for preparing a porous biological filler for purifying polluted seawater, comprising the following steps:
step one: the preparation materials and the weight percentages are respectively as follows: 17.4% of reduced iron powder, 4.3% of activated carbon powder, 4.3% of graphite powder, 17.2% of quartz powder, 4.4% of tourmaline powder, 4.4% of diatomite, 8.6% of zeolite powder, 4.4% of volcanic powder, 4.4% of medical stone powder, 0.5% of ammonium bicarbonate and 30% of sodium bentonite; and mixing uniformly to obtain an inorganic mixture.
Step two: graphene, which is 1% by weight of the inorganic mixture, is dispersed with a dispersant (sodium dodecyl sulfate) (wherein 1g of graphene is put into 0.07g of dispersant, and when the dispersion is prepared, the concentration of the dispersant is not more than 2mg/mL, namely, 0.07g of dispersant is put into 35mL of distilled water) for later use.
Step three: spraying the dispersed graphene and tap water (chlorine-free water) which is placed for 2 days and is 30% of the weight of the inorganic mixture on the inorganic mixture obtained in the step one, adding the mixture for multiple times, stirring the mixture again uniformly, stopping stirring the mixture until the mixture can be plastic, preparing wet filler with the particle size of 10-25 mm by using a granulator, and then placing the wet filler at a dry ventilation place for drying at room temperature for 24 hours; then placing the mixture in a muffle furnace, gradually heating the furnace temperature from room temperature to 350 ℃ for roasting 1h at 8 ℃ per minute, then heating the mixture to 700 ℃ for roasting 0.5h, finally heating the mixture to 950 ℃ for roasting 1h, and naturally placing the mixture for cooling to obtain the mixed dry filler.
Step four: mechanically crushing the dry filling, screening particles by a 7-28 mesh sieve, transferring the particles into a large beaker, slowly adding a methyl methacrylate binder, continuously stirring until the mixture is basically plastic, immediately stopping the stirring, transferring the mixture into a mould for granulating to form a single-channel and porous skeleton structure, and drying and qualifying the mixture to obtain the porous mineral spheres.
Step five: uniformly mixing 1.5% of maltodextrin, 12% of agar powder, 24% of straw powder, 12% of walnut shell powder, 17% of crosslinked starch, 13% of glycerol, 4.5% of trehalose and chlorine-free water according to the weight percentage, and sequentially adding 5.5% of monoglyceride fatty glyceride, 3.5% of xanthan gum and 7% of acid-soluble chitosan, wherein chlorine-free water is intermittently added for 4 times; and (3) stirring in one direction in a water bath at 95 ℃ until the mixture is gelatinized, and standing for 1.5h to obtain the embedded carbon source organism blend.
Step six: adding the porous mineral spheres obtained in the step four into the embedded carbon source organism blend obtained in the step five, stirring in one direction, enabling the embedded carbon source organism blend to permeate into 70% of the pore volume of the porous mineral spheres, reserving 30% of the pore volume, fishing out, transferring into a low-temperature container at-20 ℃ for shaping, and then placing into a low-temperature oven at 40 ℃ for drying, thus obtaining the porous biological filler.
The filler physical properties were tested: the porous bio-filler was tested for one hour water absorption, apparent density, porosity, filler density and carbon source content, and had a small density compared to the commercially available normal filler, with greater porosity, carbon source content and water absorption at the same mass (table 1).
TABLE 1 physical Properties of porous biological fillers
Example 2
The porous bio-filler prepared in example 1 was filled into a cylindrical organic glass column (diameter 10cm, height 70cm; the reactor was completely covered with tinfoil paper), the lowermost layer of the cylindrical column was filled with gravel filler about 5cm as a supporting layer, and then 50cm of porous bio-filler was filled; a water distribution tank with a working volume of 10L is used, the temperature of the water distribution tank is controlled by an electric heater at the temperature of 25 ℃, inlet water is pumped into simulated aquaculture seawater waste water with the water quality shown in table 2 by controlling the same flow rate by a peristaltic pump, the water level is adjusted to be 5cm above the surface of a filler, and after the cylindrical reactor is continuously operated for 2 months at the temperature of 25 ℃ to a stable hanging period, a pollutant removal experiment is started.
Further, glucose, potassium nitrate, ammonium chloride and monopotassium phosphate are added into the tap water from which chlorine has been removed, simulated polluted seawater is prepared as the inlet water of the reactor, and the inlet water concentration of each pollutant is shown in table 2.
TABLE 2 Water quality parameters of influent during the film formation of a reactor containing porous biological fillers
The pollutant water inlet concentration (three repeated samples in each group) of the treatment system is determined by taking 200mL of water sample from a water inlet, the pollutant water outlet concentration (three repeated samples in each group) of the treated water sample is determined by taking 200mL of water out of a water outlet after the sewage flow passes through a column (the hydraulic retention time is 12 h), and the temperature, the pH, the DO and the NO of the water sample are respectively tested 3 - -N、NO 2 - -N、NH 4 + N, TN and TOC.
NO 3 - -N、NO 2 - -N、NH 4 + N, TN removal rate of toc= (inlet water concentration-outlet water concentration)/inlet water concentration; each contaminant concentration was averaged over 3 removal rates as the final removal rate for that contaminant.
Reactor pair NO 3 - -N、NO 2 - -N、NH 4 + The removal rates of N, TN and TOC were 91.5%, 92.0%, 70.2%, 83.2% and 84.9%, respectively (Table 3).
TABLE 3 removal rate of contaminants from simulated seawater by a reactor filled with porous biological filler
The surface properties of the filler were observed, and the filler was characterized by Scanning Electron Microscope (SEM) analysis (fig. 2), X-ray spectroscopy analysis (EDS) (fig. 3), and X-ray diffractometer (XRD) analysis (fig. 4).
As can be seen from FIG. 2 (a) before the SEM analysis of the porous biological filler is used, the surface structure of the filler is loose and porous, and the wastewater is very favorable for fully contacting and mixing the filler and the wastewater in the flowing process, so that the efficiency of the micro-electrolysis reaction is improved, the internal structure of the filler is not a compact structure, and the internal structure is in a small sphere shape, and relatively large pores exist between the internal structure and the filler, so that the filler has a large water absorption rate. After use, as can be seen in fig. 2 (b), the surface is porous, and has a distinct microbial coverage, and the surface of the filler has been significantly changed after the reaction.
EDS analysis results show that the mass fraction of the surface of the filler particles changes before and after use as shown in FIG. 3 (a) and FIG. 3 (b). After the filler is used, the surface mass fraction of oxygen and iron is increased, the surface mass fraction of carbon is reduced, the elements are uniformly distributed, and the silicon and oxygen contents are far higher than those of other elements in FIG. 3 (b).
XRD analysis results show that after high-temperature roasting, in FIG. 4 (a), metallic iron in the filler exists in the form of simple substance and also exists in the form of oxide, and the ferric oxide covered on the surface of the filler mainly comprises Fe 3 O 4 、Fe 2 O 3 And FeO, the iron-containing filler oxide is increased after use compared with that before use, and the valence state of iron is mainly formed by Fe 0 Change to Fe 2+ Fe (b) 3+ Fig. 4 (b).
Research results show that the porous biological filler has a communicated pore structure, a larger specific surface area is favorable for microorganism adhesion and mass growth and reproduction, the particles have multicomponent minerals and are favorable for microorganism metabolism and pollutant conversion, meanwhile, the particle size of the filler is increased, hardening is not easy, an embedded carbon source provides a carbon source for denitrification, and the existence of graphite, iron oxide and graphene strengthens an electron transfer process, so that the filler has a good effect of removing pollutants, especially nitrogen.
The embodiments described herein are merely illustrative of the invention, and modifications and additions may be made to the specific embodiments by those skilled in the art without departing from the spirit of the invention.
Claims (5)
1. A porous bio-filler for purification of polluted seawater, characterized in that the porous bio-filler comprises an external porous mineral sphere and an embedded carbon source organism blend, the mass ratio of the porous mineral sphere and the embedded carbon source organism blend being: 7.5-8.5:1.5-2.5, wherein the porous mineral sphere is provided with a single channel penetrating through the porous mineral sphere and a porous skeleton structure inside the porous mineral sphere, and the embedded carbon source organism blend forms a slow-release organic carbon source;
the porous mineral sphere is formed by bonding a plurality of particles through an organic low-temperature binder, wherein the particles are provided with pore structures, and the pores are communicated inside the porous mineral sphere; the embedded carbon source organism blend permeates 60-80% of the volume of the pores among the porous mineral sphere particles; the diameter of the single channel is 10% -25% of the diameter of the porous mineral sphere;
the particles comprise the following components in percentage by weight: 16 to 19 percent of reduced iron powder, 3 to 5.5 percent of activated carbon powder, 3 to 5.5 percent of graphite powder, 15 to 19 percent of quartz powder, 3 to 5.5 percent of tourmaline powder, 3 to 5.5 percent of diatomite, 7 to 10 percent of zeolite powder, 3 to 5.5 percent of volcanic powder, 3 to 5.5 percent of medical stone powder, 0.5 to 1 percent of pore-forming agent, 0.8 to 1.2 percent of graphene and 25 to 30 percent of inorganic binder;
the pore-forming agent is ammonium bicarbonate or ammonium carbonate; the inorganic binder is sodium bentonite or calcium bentonite; the graphene is single-layer or few-layer or multi-layer graphene prepared by a physical method or a chemical method; the organic low-temperature binder is methyl methacrylate or unsaturated polyester resin binder;
the embedded carbon source organism blend comprises the following components in percentage by weight: 1-2% of dissolution auxiliary agent, 10-15% of agar powder, 20-30% of straw powder, 10-15% of walnut shell powder, 15-20% of starch, 12-15% of glycerol, 3-6% of xanthan gum, 3-6% of trehalose, 5-7% of emulsifying agent and 5-10% of chitosan;
the dissolution aid is dextrin or starch syrup or glucose; the starch is common starch or crosslinked starch; the emulsifier is sorbitol glyceride, sorbitan monooleate or monoglyceride; the chitosan is acid-soluble chitosan.
2. The method for preparing the porous biological filler according to claim 1, comprising the steps of:
(1) Preparing porous mineral spheres:
1) Mixing reduced iron powder, activated carbon powder, graphite powder, quartz powder, tourmaline powder, diatomite, zeolite powder, volcanic powder, medical stone powder, pore-forming agent and inorganic binder, and stirring uniformly to obtain an inorganic mixture;
2) Dispersing graphene with a dispersing agent, wherein the mass ratio of the graphene to the dispersing agent is 1:0.06-0.1;
3) Spraying the dispersed graphene accounting for 0.8-1.2% of the weight of the inorganic mixture and chlorine-free water accounting for 27-31% of the weight of the inorganic mixture onto the inorganic mixture, adding the graphene and chlorine-free water for multiple times, stirring the mixture uniformly again, stopping stirring the mixture until the mixture can be molded, preparing wet filler particles, drying the particles, and roasting the particles to obtain dry filler of mixed components;
4) Crushing the dry filling materials of the mixed components, screening out particles with the particle size of 7-28 meshes, slowly adding an organic low-temperature binder, continuously stirring, immediately stopping when the mixture is plastic, transferring into a mould for granulating and drying to obtain a porous mineral sphere with a single channel penetrating the porous mineral sphere and a porous skeleton structure inside the porous mineral sphere;
(2) Preparing an embedded carbon source organism blend:
uniformly mixing a dissolution auxiliary agent, agar powder, straw powder, walnut shell powder, starch, glycerol, trehalose and chlorine-free water, and sequentially adding an emulsifier, xanthan gum and chitosan, wherein the chlorine-free water is intermittently added for 4-5 times; stirring in one direction in a water bath at 90-100 ℃ until gelatinization, and standing for 1-2h to obtain a blend;
(3) Preparing porous biological filler:
adding the porous mineral spheres into the organic blend of the embedded carbon source, stirring in one direction, enabling the organic blend of the embedded carbon source to permeate into 60-80% of the volume of the pores among particles of the porous mineral spheres, reserving part of the pores, fishing out, transferring into a low-temperature container at 0-minus 20 ℃ for shaping, and then placing into a low-temperature oven at 40-45 ℃ for drying, thus obtaining the porous biological filler.
3. The method of claim 2, wherein the dispersant is sodium dodecyl sulfate; step 3), drying at a dark and dry place or at a temperature of 50-75 ℃; the roasting conditions in the step 3) are as follows: gradually heating from room temperature to 300-350 ℃ at a speed of 5-10 ℃/min, continuously roasting for 55-65 min, then heating to 650-700 ℃ and roasting for 25-35 min, and finally heating to 900-950 ℃ and roasting for 55-65 min; the particle size of the wet filler particles in the step 3) is 10-50 mm.
4. The use of a porous biological filler according to claim 1, in seawater or fresh water contaminated with organic compounds.
5. The use according to claim 4, wherein the organic compound comprises a nitrogen-containing compound and a non-nitrogen-containing compound; the nitrogen-containing compound is a protein, an amino acid, urea, an amine or a nitro compound; the non-nitrogen containing compound is a carbohydrate, fat, phenol, aldehyde, ketone, non-nitrogen containing organic acid, hydrocarbon or synthetic detergent.
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| CN202210999944.9A Active CN115322008B (en) | 2022-03-30 | 2022-08-19 | Porous biological filler for purifying polluted seawater and preparation method and application thereof |
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| CN115477396A (en) * | 2022-10-19 | 2022-12-16 | 苏州方舟环保科技有限公司 | Denitrification filler and method for treating sewage by using same |
| CN116375301B (en) * | 2023-06-05 | 2023-08-18 | 山东国宏生物科技有限公司 | Soybean oil wastewater treatment method |
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| CN114835507A (en) | 2022-08-02 |
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