CN116621330A - Biological filler for slowly releasing carbon source and preparation method and application thereof - Google Patents
Biological filler for slowly releasing carbon source and preparation method and application thereof Download PDFInfo
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- CN116621330A CN116621330A CN202310840158.9A CN202310840158A CN116621330A CN 116621330 A CN116621330 A CN 116621330A CN 202310840158 A CN202310840158 A CN 202310840158A CN 116621330 A CN116621330 A CN 116621330A
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- carbon source
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- release carbon
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- 239000000945 filler Substances 0.000 title claims abstract description 147
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 130
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 130
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- 239000004743 Polypropylene Substances 0.000 claims abstract description 110
- -1 polypropylene Polymers 0.000 claims abstract description 110
- 229920001155 polypropylene Polymers 0.000 claims abstract description 110
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 28
- 238000000034 method Methods 0.000 claims abstract description 21
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 claims abstract description 15
- 239000004372 Polyvinyl alcohol Substances 0.000 claims abstract description 14
- 229920002451 polyvinyl alcohol Polymers 0.000 claims abstract description 14
- 239000010865 sewage Substances 0.000 claims abstract description 13
- 238000001179 sorption measurement Methods 0.000 claims abstract description 8
- CKUAXEQHGKSLHN-UHFFFAOYSA-N [C].[N] Chemical compound [C].[N] CKUAXEQHGKSLHN-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000003486 chemical etching Methods 0.000 claims abstract description 6
- 229940040526 anhydrous sodium acetate Drugs 0.000 claims abstract description 4
- 239000011259 mixed solution Substances 0.000 claims abstract description 4
- 239000002351 wastewater Substances 0.000 claims abstract description 4
- 239000003607 modifier Substances 0.000 claims abstract description 3
- 238000009360 aquaculture Methods 0.000 claims abstract 2
- 244000144974 aquaculture Species 0.000 claims abstract 2
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 70
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 38
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 35
- 230000004048 modification Effects 0.000 claims description 24
- 238000012986 modification Methods 0.000 claims description 24
- 239000011347 resin Substances 0.000 claims description 23
- 229920005989 resin Polymers 0.000 claims description 23
- 239000001632 sodium acetate Substances 0.000 claims description 23
- 230000006911 nucleation Effects 0.000 claims description 21
- 238000010899 nucleation Methods 0.000 claims description 21
- 239000012752 auxiliary agent Substances 0.000 claims description 19
- 239000001569 carbon dioxide Substances 0.000 claims description 19
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 19
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 18
- 239000000203 mixture Substances 0.000 claims description 17
- 238000002156 mixing Methods 0.000 claims description 15
- 238000001035 drying Methods 0.000 claims description 14
- 235000017281 sodium acetate Nutrition 0.000 claims description 11
- 239000000243 solution Substances 0.000 claims description 11
- NWGKJDSIEKMTRX-AAZCQSIUSA-N Sorbitan monooleate Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)OC[C@@H](O)[C@H]1OC[C@H](O)[C@H]1O NWGKJDSIEKMTRX-AAZCQSIUSA-N 0.000 claims description 9
- 239000003153 chemical reaction reagent Substances 0.000 claims description 9
- 239000012530 fluid Substances 0.000 claims description 8
- 230000010355 oscillation Effects 0.000 claims description 7
- 238000002791 soaking Methods 0.000 claims description 7
- 239000012047 saturated solution Substances 0.000 claims description 5
- 238000003828 vacuum filtration Methods 0.000 claims description 5
- 238000002844 melting Methods 0.000 claims description 4
- 230000008018 melting Effects 0.000 claims description 4
- VUZPPFZMUPKLLV-UHFFFAOYSA-N methane;hydrate Chemical compound C.O VUZPPFZMUPKLLV-UHFFFAOYSA-N 0.000 claims description 4
- 238000006116 polymerization reaction Methods 0.000 claims description 4
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 4
- 239000012498 ultrapure water Substances 0.000 claims description 4
- 230000009471 action Effects 0.000 claims description 3
- 238000007789 sealing Methods 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 claims 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 abstract description 24
- 229910052757 nitrogen Inorganic materials 0.000 abstract description 13
- 229910052698 phosphorus Inorganic materials 0.000 abstract description 10
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 abstract description 9
- 239000011574 phosphorus Substances 0.000 abstract description 9
- 244000005700 microbiome Species 0.000 abstract description 7
- 239000003344 environmental pollutant Substances 0.000 abstract description 6
- 231100000719 pollutant Toxicity 0.000 abstract description 6
- 230000006872 improvement Effects 0.000 abstract description 5
- 238000000746 purification Methods 0.000 abstract description 4
- ZORQXIQZAOLNGE-UHFFFAOYSA-N 1,1-difluorocyclohexane Chemical compound FC1(F)CCCCC1 ZORQXIQZAOLNGE-UHFFFAOYSA-N 0.000 abstract description 2
- 239000001593 sorbitan monooleate Substances 0.000 abstract description 2
- 229940035049 sorbitan monooleate Drugs 0.000 abstract description 2
- 235000011069 sorbitan monooleate Nutrition 0.000 abstract description 2
- 238000004134 energy conservation Methods 0.000 abstract 1
- 238000005265 energy consumption Methods 0.000 abstract 1
- 238000011065 in-situ storage Methods 0.000 abstract 1
- 230000000694 effects Effects 0.000 description 18
- 239000000463 material Substances 0.000 description 16
- XKMRRTOUMJRJIA-UHFFFAOYSA-N ammonia nh3 Chemical compound N.N XKMRRTOUMJRJIA-UHFFFAOYSA-N 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 6
- 239000003995 emulsifying agent Substances 0.000 description 6
- 239000002131 composite material Substances 0.000 description 5
- 238000012545 processing Methods 0.000 description 5
- 239000007787 solid Substances 0.000 description 5
- 150000001242 acetic acid derivatives Chemical class 0.000 description 4
- 239000011248 coating agent Substances 0.000 description 4
- 238000000576 coating method Methods 0.000 description 4
- 238000002474 experimental method Methods 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 238000000354 decomposition reaction Methods 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 238000000967 suction filtration Methods 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 230000002209 hydrophobic effect Effects 0.000 description 2
- 238000002386 leaching Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 230000014759 maintenance of location Effects 0.000 description 2
- 239000000693 micelle Substances 0.000 description 2
- 239000010902 straw Substances 0.000 description 2
- 235000017060 Arachis glabrata Nutrition 0.000 description 1
- 244000105624 Arachis hypogaea Species 0.000 description 1
- 235000010777 Arachis hypogaea Nutrition 0.000 description 1
- 235000018262 Arachis monticola Nutrition 0.000 description 1
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 1
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- JVMRPSJZNHXORP-UHFFFAOYSA-N ON=O.ON=O.ON=O.N Chemical compound ON=O.ON=O.ON=O.N JVMRPSJZNHXORP-UHFFFAOYSA-N 0.000 description 1
- 229920005372 Plexiglas® Polymers 0.000 description 1
- 241000209140 Triticum Species 0.000 description 1
- 235000021307 Triticum Nutrition 0.000 description 1
- MMDJDBSEMBIJBB-UHFFFAOYSA-N [O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[NH6+3] Chemical compound [O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[NH6+3] MMDJDBSEMBIJBB-UHFFFAOYSA-N 0.000 description 1
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 description 1
- 238000010170 biological method Methods 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000013270 controlled release Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000012851 eutrophication Methods 0.000 description 1
- 230000003203 everyday effect Effects 0.000 description 1
- 239000008103 glucose Substances 0.000 description 1
- 125000001165 hydrophobic group Chemical group 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 230000035800 maturation Effects 0.000 description 1
- 230000000813 microbial effect Effects 0.000 description 1
- 239000005445 natural material Substances 0.000 description 1
- 235000020232 peanut Nutrition 0.000 description 1
- 230000002572 peristaltic effect Effects 0.000 description 1
- 239000005014 poly(hydroxyalkanoate) Substances 0.000 description 1
- 229920001610 polycaprolactone Polymers 0.000 description 1
- 239000004632 polycaprolactone Substances 0.000 description 1
- 229920000903 polyhydroxyalkanoate Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 230000003381 solubilizing effect Effects 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229920001059 synthetic polymer Polymers 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F3/00—Biological treatment of water, waste water, or sewage
- C02F3/28—Anaerobic digestion processes
- C02F3/2806—Anaerobic processes using solid supports for microorganisms
-
- 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
- C02F2101/10—Inorganic compounds
- C02F2101/105—Phosphorus 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
- C02F2101/10—Inorganic compounds
- C02F2101/16—Nitrogen compounds, e.g. ammonia
-
- 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
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/007—Contaminated open waterways, rivers, lakes or ponds
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/06—Nutrients for stimulating the growth of microorganisms
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W10/00—Technologies for wastewater treatment
- Y02W10/10—Biological treatment of water, waste water, or sewage
Abstract
The invention discloses a slow-release carbon source biological filler, a preparation method and application thereof, belonging to the field of water quality purification biological fillers. The slow-release carbon source biological filler is prepared by adopting porous polypropylene as a carrier, anhydrous sodium acetate as a carbon source and a mixed solution of polyvinyl alcohol and sorbitan monooleate as a hydrophilic modifier through a chemical etching method and a vacuum negative pressure adsorption method. The filler prepared by the invention has a porous structure, can provide an adhesion carrier for microorganisms, has good biocompatibility, can realize slow and stable release of a carbon source, and provides a sufficient carbon source for sewage treatment. The slow-release carbon source filler can be recycled, so that energy conservation and consumption reduction can be realized. By constructing a slow-release carbon source biological filler treatment system, the method can realize the effective removal of nitrogen and phosphorus pollutants of domestic sewage and aquaculture wastewater with low carbon nitrogen ratio (C/N) and in-situ improvement of the water quality of river and lake.
Description
Technical Field
The invention belongs to the field of water quality purification materials, and particularly relates to a slow-release carbon source biological filler, and a preparation method and application thereof.
Background
In recent years, with the continuous promotion of the urban process in China, the life style and habit of people are changed while the water consumption is increased, and the nitrogen content in urban domestic sewage is obviously improved. Under the big background of stricter emission standard, the denitrification by the traditional nitrification and denitrification process often faces the problem of reduced denitrification effect caused by insufficient carbon source, and the effluent nitrogen concentration is not up to the standard, so that the water quality of urban rivers and lakes in China presents the water quality characteristics of high nitrogen and low carbon, and the eutrophication problem of the water bodies in rivers and lakes is easily caused.
In actual engineering, when the carbon nitrogen ratio (C/N) is generally smaller than 3.7, a carbon source needs to be externally added to ensure that denitrification and denitrification are smoothly carried out. However, the conventional additional carbon source is usually some low molecular organic matters such as glucose, methanol, etc., and the addition of the carbon source causes an increase in sewage treatment cost, and has a problem that the addition amount is not easy to control. Such as: when the amount of the added carbon source is insufficient, the treated water quality is easy to be unqualified, and when the amount of the added carbon source is excessive, the COD of the effluent exceeds the standard, so that secondary pollution and waste of the carbon source are caused.
The novel solid slow-release carbon source has the characteristics of stable carbon release and difficult secondary pollution, and can effectively improve the denitrification effect. Solid slow-release carbon sources commonly used at present include natural materials and synthetic polymeric materials. The natural materials include straw, corncob, wheat straw, peanut shell, etc. The slow-release carbon source material has low carbon release efficiency and influences the denitrification effect. In addition, other substances such as N, P and the like can be released by the natural material in the carbon releasing process, so that secondary pollution is easy to cause. The artificially synthesized high molecular polymer, such as polyhydroxyalkanoate, polycaprolactone, polyvinyl alcohol and other materials, can be used as a slow-release carbon source. Although these materials are capable of releasing sufficient carbon sources, the carbon release period is short and cannot provide microbial growth as a stable carbon source. In addition, the materials have high cost and are not easy to mold, and the wide application of the materials in practical engineering is also hindered. Therefore, the exploration of the novel slow-release carbon source filler is an effective way for removing nitrate in water.
Disclosure of Invention
Aiming at the defects existing in the prior art, the invention aims to provide a preparation method and application of a biological filler of a denitrification slow-release carbon source, and the denitrification effect of a biological method in treating low-C/N sewage is enhanced by developing a solid slow-release carbon source with excellent performance. The carbon source is selected as the carbon source which is easy to be absorbed and utilized by microorganisms and is easy to obtain, namely anhydrous sodium acetate, porous polypropylene is taken as a framework, the carbon source is coupled to polypropylene filler by adopting a vacuum negative pressure adsorption method to prepare the slow-release carbon source, and the polyvinyl alcohol and SPAN80 mixed solution is used for coating and hydrophilic modification to enhance the carbon release effect.
2. Technical proposal
In order to achieve the above purpose, the present invention provides the following technical solutions:
the preparation method of the slow-release carbon source biological filler comprises the steps of taking polypropylene resin as a basic skeleton, taking anhydrous sodium acetate as a carbon source, taking a mixed solution of polyvinyl alcohol and SPAN80 (SPAN 80) as a hydrophilic modifier, and preparing the polypropylene-based slow-release carbon source biological filler by a surface adsorption method. The prepared filler has a porous structure, can realize slow release of carbon sources, provides an adhesion carrier for microorganisms, and provides sufficient and stable carbon sources for sewage treatment or river and lake water purification and improvement.
The invention provides a preparation method of a slow-release carbon source biological filler, which comprises the following steps:
(1) Preparation of porous polypropylene filler: preparing polypropylene resin and nucleation auxiliary agent calcium carbonate, and mixing to obtain a mixture; carrying out supercritical carbon dioxide treatment on the mixture to obtain porous polypropylene filler; removing calcium carbonate of the porous polypropylene filler by adopting a chemical etching mode;
(2) Preparation of porous polypropylene slow-release carbon source biological filler: soaking the porous polypropylene filler obtained in the step (1) in acetic acid solution for vacuum filtration treatment, and drying;
(3) Preparation of porous polypropylene slow-release carbon source biological filler hydrophilic modification: and (3) carrying out hydrophilic modification treatment on the porous polypropylene slow-release carbon source biological filler obtained in the step (2).
The invention provides a preparation method of a slow-release carbon source biological filler, which specifically comprises the following steps:
preparation of porous polypropylene filler:
(1) Drying polypropylene resin and nucleation auxiliary agent calcium carbonate at 80 ℃ for 3 hours respectively; the weight ratio of the treated polypropylene resin to the nucleation auxiliary agent calcium carbonate is (80-90): (10-20) uniformly mixing to obtain a mixture;
(2) Mixing the mixture, adding into an extruder, and injecting supercritical carbon dioxide, wherein the volume ratio of the supercritical fluid carbon dioxide to the mixture is (0.02-0.08): 100, the adding rate of supercritical fluid carbon dioxide is 0.002L/min-0.005L/min, the temperature of a melting section is controlled to be 200-220 ℃, and the pressure is 1-5 MPa, so as to prepare the porous polypropylene filler;
(3) Removing calcium carbonate by chemical etching, firstly soaking porous polypropylene filler in 66.5% acetic acid solution by mass fraction, simultaneously carrying out ultrasonic oscillation at 40-60 ℃ for 48 hours, taking out, and drying in air for 48 hours. Acetic acid can carry out double decomposition reaction with calcium carbonate in the filler under the ultrasonic condition to generate carbon dioxide and water; the removal of calcium carbonate can increase the porosity of the material.
Preparation of porous polypropylene slow-release carbon source biological filler:
(4) Placing the filler obtained in the step (3) into a vacuum suction filtration device filled with sodium acetate saturated solution, and adsorbing sodium acetate by the filler under vacuum negative pressure;
(5) And (3) drying the filler obtained in the step (4) in air to obtain the polypropylene slow-release carbon source biological filler.
Hydrophilic modification of polypropylene slow-release carbon source biological filler:
(6) Dissolving 10 parts of polyvinyl alcohol and 5 parts of SPAN80 in 85 parts of ultrapure water, transferring to a beaker, placing in a constant-temperature oil bath magnetic stirrer, setting the temperature to 98+/-2 ℃, and stirring at 1000-2000rpm to prepare a hydrophilic modification reagent, and cooling for later use;
(7) And (3) coating the hydrophilic modification reagent prepared in the step (6) on the surface of the porous polypropylene slow-release carbon source biological filler prepared in the step (5), and performing hydrophilic modification on the porous polypropylene slow-release carbon source biological filler to prepare the hydrophilic porous polypropylene slow-release carbon source biological filler. Wherein, the polyvinyl alcohol contains a large amount of hydrophilic groups, namely hydroxyl groups, so that the hydrophilic performance of the material can be improved. Sorbitan monooleate (SP AN 80) is used as AN emulsifier, one end of the emulsifier is a polar hydrophilic group, the other end of the emulsifier is a nonpolar hydrophobic group, the emulsifier can be used as a hydrophilic modification reagent, and the hydrophobic core of the micelle has the capability of solubilizing organic matters by acting with sodium acetate to increase the dispersibility of the emulsifier to form a micelle, so that the emulsifier is added in the hydrophilic modification process, and the diffusion of hydrophilic and lipophilic pollutants on the surface of the filler can be increased.
Preferably, the vacuum negative pressure in the step (4) is controlled to be between-0.05 MPa and-0.5 MPa, and the negative pressure adsorption time is 60-5 min.
Preferably, the degree of polymerization of the polyvinyl alcohol in step (6) is 1750.+ -.50.
The invention further discloses application of the porous polypropylene-sodium acetate slow-release carbon source biological filler prepared by the preparation method to nitrogen and phosphorus pollutants, and the porous polypropylene-sodium acetate slow-release carbon source biological filler has the characteristics of high carbon release stability and strong durability, and can be well used for treating domestic sewage with low carbon nitrogen ratio (C/N), cultivation wastewater and river and lake water quality improvement.
Advantageous effects
The biological filler of the porous polypropylene-sodium acetate slow-release carbon source has the retention time of 24 hours in water under the conditions that the COD of inflow water is 20mg/L, the ammonia nitrogen is 2.1mg/L, the total nitrogen is 15mg/L and the total phosphorus is 0.5mg/L, and the removal rates of the biological filler on the ammonia nitrogen, the total nitrogen and the total phosphorus are 98%, 93% and 58% respectively.
According to the invention, from the perspective of composite materials, a carbon source is loaded on the porous polypropylene filler to prepare the porous polypropylene slow-release carbon source biological filler, and the porous polypropylene slow-release carbon source biological filler is subjected to hydrophilic modification to increase the contact with pollutants in water. The adsorbed carbon source is slowly released by utilizing the loose and porous characteristics of the porous polypropylene filler, so that the durability and stability of carbon release are improved, the utilization rate of pollutant degradation to the carbon source is effectively improved, meanwhile, the polypropylene serving as a biological filler also provides an adhesion carrier for microorganism growth, and the utilization efficiency of microorganisms to the carbon source is further promoted. The filler prepared by the invention is easy to prepare, can be recycled, and has good expression and application prospects for sewage treatment, especially for purification and improvement of water quality of rivers and lakes.
Drawings
Fig. 1: scanning Electron Microscope (SEM) images of the internal porous structure of the porous polypropylene filler prepared in this example;
fig. 2: the porous polypropylene slow-release carbon source biological filler material object diagram prepared in the embodiment is shown;
fig. 3: solid-liquid contact angle measurement for polypropylene, porous polypropylene and hydrophilic modified porous polypropylene filler;
fig. 4: the carbon release effect of the porous polypropylene slow release carbon source filler prepared by different polypropylene and calcium carbonate proportions in the embodiment of the invention is compared with that of the porous polypropylene slow release carbon source filler prepared by different proportions in the comparative example;
fig. 5: the carbon release effect of the fillers with different material sources is compared;
fig. 6: the comparative graph shows the ammonia nitrogen removal effect of the porous polypropylene slow-release carbon source filler and the porous polypropylene filler in the embodiment of the invention;
fig. 7: the method is a comparison chart of the removal effect of the porous polypropylene slow-release carbon source filler and the porous polypropylene filler on total nitrogen;
fig. 8: the comparative graph shows the effect of the porous polypropylene slow-release carbon source filler and the porous polypropylene filler on removing total phosphorus.
Detailed Description
The following describes the technical solutions in the embodiments of the present invention in detail, and the described embodiments are only some of the embodiments of the present invention. All other embodiments, which are derived by a person skilled in the art based on the embodiments of the invention, fall within the scope of protection of the invention. The invention is further described below in connection with specific embodiments.
Example 1
The embodiment provides a preparation method of a porous polypropylene slow-release carbon source biological filler, which comprises the following steps:
preparation of porous Polypropylene filler
(1) Drying polypropylene resin and nucleation auxiliary agent calcium carbonate at 80 ℃ for 3 hours respectively; uniformly mixing the treated polypropylene resin and the nucleation auxiliary agent calcium carbonate according to the mass ratio of 90:10 to obtain mixed fillers with different proportions;
(2) Mixing the mixture, adding into an extruder, and injecting supercritical carbon dioxide, wherein the volume ratio of the supercritical fluid carbon dioxide to the mixture is (0.02-0.08): 100, the adding rate of supercritical fluid carbon dioxide is 0.002L/min-0.005L/min, the temperature of a melting section is controlled to be 200-220 ℃, the pressure is 1-5 MPa, and the porous polypropylene filler is prepared, wherein SEM (scanning electron microscope) in the porous polypropylene filler is shown in figure 1;
(3) Removing calcium carbonate by chemical etching, firstly soaking porous polypropylene filler in 66.5% saturated acetic acid solution by mass fraction, simultaneously carrying out ultrasonic oscillation at 40-60 ℃, carrying out double decomposition reaction on the saturated acetic acid solution and calcium carbonate in the polypropylene filler under the action of ultrasonic oscillation to generate carbon dioxide and water, taking out after 48h, and drying in air for 48h, wherein the removal of the calcium carbonate can increase the porosity of the material.
Preparation of porous polypropylene slow-release carbon source biological filler
(4) And (3) placing the filler obtained in the step (3) into a vacuum suction filtration device filled with 66.5% sodium acetate saturated solution, adsorbing sodium acetate by the filler under vacuum negative pressure, wherein the vacuum negative pressure is controlled to be-0.05 MPa to-0.5 MPa, and the negative pressure adsorption time is 60-5 min.
(5) And (3) drying the filler obtained in the step (4) in air to obtain the porous polypropylene slow-release carbon source biological filler.
Hydrophilic modification of porous polypropylene slow-release carbon biological filler
(6) 10 parts of polyvinyl alcohol with the polymerization degree of 1750+/-50 and 5 parts of SPAN80 are dissolved in 85 parts of ultrapure water, then transferred into a beaker, placed in a constant-temperature oil bath magnetic stirrer, set at the temperature of 98+/-2 ℃ and stirred at the rotation speed of 1000-2000rp m, and prepared into a hydrophilic modified reagent, and cooled for later use;
(7) And (3) coating the hydrophilic modification reagent prepared in the step (6) on the surface of the porous polypropylene slow-release carbon source biological filler prepared in the step (5), and performing hydrophilic modification on the porous polypropylene slow-release carbon source biological filler to prepare the hydrophilic porous polypropylene slow-release carbon source biological filler, as shown in figure 2.
Example 2
The embodiment provides a preparation method of a porous polypropylene slow-release carbon source biological filler, which comprises the following steps:
preparation of porous Polypropylene filler
(1) Drying polypropylene resin and nucleation auxiliary agent calcium carbonate at 80 ℃ for 3 hours respectively; uniformly mixing the treated polypropylene resin and the nucleation auxiliary agent calcium carbonate according to the mass ratio of 85:15 to obtain mixed fillers with different proportions;
(2) Mixing the mixture, adding into an extruder, and injecting supercritical carbon dioxide, wherein the volume ratio of the supercritical fluid carbon dioxide to the mixture is (0.02-0.08): 100, the adding rate of supercritical fluid carbon dioxide is 0.002L/min-0.005L/min, the temperature of a melting section is controlled to be 200-220 ℃, the pressure is 1-5 MPa, and the porous polypropylene filler is prepared, wherein SEM (scanning electron microscope) in the porous polypropylene filler is shown in figure 1;
(3) Removing calcium carbonate by chemical etching, firstly soaking porous polypropylene filler in 66.5% saturated acetic acid solution by mass fraction, simultaneously carrying out ultrasonic oscillation at 40-60 ℃, carrying out double decomposition reaction on the saturated acetic acid solution and calcium carbonate in the polypropylene filler under the action of ultrasonic oscillation to generate carbon dioxide and water, taking out after 48h, and drying in air for 48h, wherein the removal of the calcium carbonate can increase the porosity of the material.
Preparation of porous polypropylene slow-release carbon source biological filler
(4) And (3) placing the filler obtained in the step (3) into a vacuum suction filtration device filled with sodium acetate saturated solution, adsorbing sodium acetate by the filler under vacuum negative pressure, wherein the vacuum negative pressure is controlled to be-0.05 MPa to-0.5 MPa, and the negative pressure adsorption time is 60-5 min.
(5) And (3) drying the filler obtained in the step (4) in air to obtain the porous polypropylene slow-release carbon source biological filler.
Hydrophilic modification of porous polypropylene slow-release carbon biological filler
(6) 10 parts of polyvinyl alcohol with the polymerization degree of 1750+/-50 and 5 parts of SPAN80 are dissolved in 85 parts of ultrapure water, then transferred into a beaker, placed in a constant-temperature oil bath magnetic stirrer, set at the temperature of 98+/-2 ℃ and stirred at the rotation speed of 1000-2000rp m, and prepared into a hydrophilic modified reagent, and cooled for later use;
(7) And (3) coating the hydrophilic modification reagent prepared in the step (6) on the surface of the porous polypropylene slow-release carbon source biological filler prepared in the step (5), and performing hydrophilic modification on the porous polypropylene slow-release carbon source biological filler to prepare the hydrophilic porous polypropylene slow-release carbon source biological filler.
Example 3
In the step (1) of the embodiment, the polypropylene resin and the nucleation auxiliary agent calcium carbonate are respectively dried for 3 hours at 80 ℃; uniformly mixing the treated polypropylene resin and the nucleation auxiliary agent calcium carbonate according to the mass ratio of 80:20 to obtain mixed fillers with different proportions; other processing conditions were the same as in example 1.
Example 4
In the step (1) of the embodiment, the polypropylene resin and the nucleation auxiliary agent calcium carbonate are respectively dried for 3 hours at 80 ℃; uniformly mixing the treated polypropylene resin and the nucleation auxiliary agent calcium carbonate according to the mass ratio of 80:10 to obtain mixed fillers with different proportions; other processing conditions were the same as in example 1.
Example 5
Drying polypropylene resin and nucleation auxiliary agent calcium carbonate at 80 ℃ for 3 hours respectively; uniformly mixing the treated polypropylene resin and the nucleation auxiliary agent calcium carbonate according to the mass ratio of 90:20 to obtain mixed fillers with different proportions; other processing conditions were the same as in example 1.
Comparative example 1
In the step (1) of the embodiment, the polypropylene resin and the nucleation auxiliary agent calcium carbonate are respectively dried for 3 hours at 80 ℃; uniformly mixing the treated polypropylene resin and the nucleation auxiliary agent calcium carbonate according to the mass ratio of 95:5 to obtain mixed fillers with different proportions; other processing conditions were the same as in example 1.
Comparative example 2
In the step (1) of the embodiment, the polypropylene resin and the nucleation auxiliary agent calcium carbonate are respectively dried for 3 hours at 80 ℃; uniformly mixing the treated polypropylene resin and the nucleation auxiliary agent calcium carbonate according to the mass ratio of 75:25 to obtain mixed fillers with different proportions; other processing conditions were the same as in example 1.
Example 6 Filler hydrophilicity comparison
The liquid-solid interface contact angle measurement experiment (figure 3) is carried out on the polypropylene, the porous polypropylene and the hydrophilic modified porous polypropylene filler in the example 1, and the result shows that the contact angle of the polypropylene filler exceeds 90.00 degrees, which indicates that the filler is hydrophobic and is not beneficial to the adhesion and film formation of microorganisms; the contact angle of the porous polypropylene filler is 79.00 degrees, which indicates that the hydrophilicity of the filler is improved by filler pore-forming; after hydrophilic modification of the filler surface by using polyvinyl alcohol, the contact angle of a liquid-solid interface is reduced to 53.50 degrees, which indicates that the hydrophilicity of the filler after hydrophilic modification is further enhanced, and the adhesion of microorganisms is very beneficial, so that the maturation of a biological film can be accelerated, and the removal efficiency of pollutants in water is improved.
Example 7 comparison of carbon Release Effect of controlled-release carbon Source biological Filler
The carbon release effect of the porous slow-release carbon source filler prepared by the polypropylene and the nucleation auxiliary agent calcium carbonate according to the mass ratio of the examples 1-5 and the comparative examples 1-2 is compared. And respectively cleaning the prepared porous polypropylene slow-release carbon source fillers with different proportions for one time to remove the residual sodium acetate on the surface, respectively soaking the fillers in 500mL of deionized water, and sealing the conical bottle mouth by using a sealing film of the sterile culture container. The flask was placed on a constant temperature shaking incubator and the temperature was controlled at 25.+ -. 1 ℃ and the shaking frequency was 80rpm. Taking COD as a carbon release index, sampling and measuring the carbon release amount of each group of carbon sources every day, and replacing the leaching liquid with 500mL of pure water after the measurement is completed. The leaching experiments were carried out continuously for 15 days. As shown in FIG. 4, 90:10 has a higher carbon release effect, and the porous polypropylene filler prepared by 90:10 (i.e. example 1) is adopted in the subsequent experiments.
EXAMPLE 8 comparison of carbon release effects of fillers of different Material sources
The slow-release carbon source prepared by common synthetic polymers of polyvinyl alcohol and sodium acetate is used as a control group, the porous polypropylene-sodium acetate composite slow-release carbon source (example 1) is used as an experimental group, and the carbon release amount of the slow-release carbon source filler is compared. The procedure of carbon release experiment was the same as in example 7. As shown in fig. 5, the carbon release amount of the biological filler of the polyvinyl alcohol-sodium acetate composite slow-release carbon source is close to 0 at the 8 th day, and the carbon release capacity is almost lost. The porous polypropylene-sodium acetate composite slow-release carbon source biological filler has higher initial carbon release amount, and the carbon release amount is always stabilized at about 44mg/L from the 5 th day. The porous polypropylene-sodium acetate composite slow-release carbon source biological filler prepared by the invention has good and stable carbon release effect.
Example 9: the denitrification and dephosphorization effects of the porous polypropylene-sodium acetate slow-release carbon biological filler on sewage with low carbon nitrogen ratio are compared with each other:
the porous polypropylene filler is used as a control, and the treatment effect of the hydrophilically modified porous polypropylene-sodium acetate slow-release carbon source biological filler on sewage with low carbon nitrogen ratio is compared. The experimental apparatus was a plexiglass reactor with an effective volume of 750ml. The reactor was filled with polypropylene and modified porous polypropylene-sodium acetate slow release carbon source filler (example 1), respectively, and peristaltic pump was used to feed water, discharge water, and carry out film formation. The COD of the inflow water is 20mg/L, the ammonia nitrogen is 2.1mg/L, the total nitrogen is 15mg/L, the total phosphorus is 0.5mg/L, and the hydraulic retention time is 24 hours. And measuring the COD, ammonia nitrogen, nitrate nitrogen, nitrite nitrogen, total nitrogen and total phosphorus concentration of the water. As shown in fig. 6-8, the removal rates of the porous polypropylene-sodium acetate slow-release carbon source biological filler on ammonia nitrogen, total nitrogen and total phosphorus are respectively 98%, 93% and 58%, and the removal rates of the porous polypropylene filler on the ammonia nitrogen, total nitrogen and total phosphorus are respectively 60%, 45% and 44%, which are obviously different.
In conclusion, the porous polypropylene-sodium acetate slow-release carbon source biological filler has the characteristics of high carbon release stability and strong durability, and can be well used for treating domestic sewage with low carbon nitrogen ratio (C/N), cultivation wastewater and river and lake water quality improvement.
The invention and its embodiments have been described above by way of illustration and not limitation, and the actual construction is not limited to this. Therefore, if one of ordinary skill in the art is informed by this disclosure, the structural mode and the embodiments similar to the technical scheme are not creatively designed without departing from the gist of the present invention.
Claims (10)
1. The biological filler of the slow-release carbon source is characterized in that the biological filler is prepared by a surface adsorption method by taking polypropylene resin as a basic skeleton, anhydrous sodium acetate as a carbon source and a mixed solution of polyvinyl alcohol and SPAN80 (SPAN 80) as a hydrophilic modifier.
2. A preparation method of a slow-release carbon source biological filler is characterized in that,
the method comprises the following steps:
(1) Preparation of porous polypropylene filler: preparing polypropylene resin and nucleation auxiliary agent calcium carbonate, and mixing to obtain a mixture; carrying out supercritical carbon dioxide treatment on the mixture to obtain porous polypropylene filler; removing calcium carbonate in the porous polypropylene filler;
(2) Preparation of porous polypropylene slow-release carbon source biological filler: soaking the porous polypropylene filler obtained in the step (1) in acetic acid solution for vacuum filtration treatment, and drying;
(3) Preparation of hydrophilic modification of biological filler of porous polypropylene slow-release carbon source: and (3) carrying out hydrophilic modification treatment on the porous polypropylene slow-release carbon source biological filler obtained in the step (2).
3. The method for preparing the slow-release carbon source biological filler according to claim 2, wherein,
the preparation of the mixture in the step (1): drying polypropylene resin and nucleation auxiliary calcium carbonate at 80 ℃ for 3 hours respectively, and uniformly mixing the treated polypropylene resin and the nucleation auxiliary calcium carbonate according to the weight ratio of 80-90:10-20 to obtain the polypropylene resin;
the supercritical carbon dioxide treatment of the mixture in the step (1) is as follows: mixing the mixture, putting the mixture into an extruder, and injecting the mixture into supercritical carbon dioxide equipment, wherein the volume ratio of supercritical fluid carbon dioxide to the mixture is (0.02-0.08): 100, the adding rate of supercritical fluid carbon dioxide is 0.002L/min-0.005L/min, the temperature of the melting section is controlled to be 200-220 ℃, and the pressure is 1-5 MPa.
4. The method for preparing the slow-release carbon source biological filler according to claim 2, wherein,
and (3) removing calcium carbonate in the porous polypropylene filler by adopting a chemical etching method in the step (1): soaking the porous polypropylene filler in 66.5% acetic acid solution by mass fraction, simultaneously carrying out ultrasonic oscillation at 40-60 ℃, generating carbon dioxide and water under the ultrasonic oscillation action of the 66.5% acetic acid solution and calcium carbonate in the polypropylene filler, taking out after 48 hours, and drying in air for 48 hours.
5. The method for preparing the slow-release carbon source biological filler according to claim 2, wherein,
the vacuum filtration treatment in the step (2) is operated as follows: and (3) placing the porous hydrophilic polypropylene filler into a vacuum filtration device filled with a sodium acetate saturated solution with the mass fraction of 66.5%, keeping sealing, starting the vacuum filtration device, enabling the filler to adsorb the sodium acetate saturated solution under vacuum negative pressure, enabling the single filtration time to be 5min, and repeating the operation for 2-3 times.
6. The method for preparing the slow-release carbon source biological filler according to claim 2, wherein,
the operation method of the hydrophilic modification treatment in the step (3) is as follows: the mass ratios are respectively 10:5:85 polyvinyl alcohol, SPAN80 and ultrapure water are transferred into a beaker, placed in a constant-temperature oil bath magnetic stirrer, set at 98+/-2 ℃ and stirred at 1000-2000rpm to prepare a hydrophilic modification reagent, and cooled for later use; and then, the prepared hydrophilic modification reagent is smeared on the surface of the prepared porous polypropylene slow-release carbon source biological filler, and the porous polypropylene slow-release carbon source biological filler is subjected to hydrophilic modification.
7. The method for preparing the biological filler of the slow-release carbon source according to claim 5, wherein the vacuum negative pressure is controlled to be between-0.05 MPa and-0.5 MPa, and the adsorption time of the vacuum negative pressure is between 60min and 5min.
8. The method for preparing a slow release carbon source biological stuffing according to claim 6, wherein the polymerization degree of the polyvinyl alcohol is 1750+ -50.
9. A slow-release carbon source bio-filler obtained by the production process according to any one of claims 2 to 8.
10. Use of the slow-release carbon source biological filler according to claim 9 in sewage treatment, preferably low carbon nitrogen ratio domestic sewage, aquaculture wastewater and river and lake water.
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