CN117125819A - Anaerobic ammonia oxidation gel particles and method for preparing and enhancing denitrification performance of anaerobic ammonia oxidation process under high total nitrogen load condition - Google Patents
Anaerobic ammonia oxidation gel particles and method for preparing and enhancing denitrification performance of anaerobic ammonia oxidation process under high total nitrogen load condition Download PDFInfo
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- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 title claims abstract description 184
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 title claims abstract description 152
- 230000003647 oxidation Effects 0.000 title claims abstract description 97
- 238000007254 oxidation reaction Methods 0.000 title claims abstract description 97
- 229910021529 ammonia Inorganic materials 0.000 title claims abstract description 92
- 238000000034 method Methods 0.000 title claims abstract description 79
- 229910052757 nitrogen Inorganic materials 0.000 title claims abstract description 76
- 239000007863 gel particle Substances 0.000 title claims abstract description 66
- 230000008569 process Effects 0.000 title claims abstract description 54
- 230000002708 enhancing effect Effects 0.000 title claims description 11
- 239000010802 sludge Substances 0.000 claims abstract description 54
- 229920001661 Chitosan Polymers 0.000 claims abstract description 32
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical class O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 30
- 239000002245 particle Substances 0.000 claims abstract description 21
- 238000002360 preparation method Methods 0.000 claims abstract description 16
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 53
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 34
- 238000003756 stirring Methods 0.000 claims description 31
- 239000007864 aqueous solution Substances 0.000 claims description 29
- 238000002156 mixing Methods 0.000 claims description 22
- 239000000243 solution Substances 0.000 claims description 19
- 238000004132 cross linking Methods 0.000 claims description 16
- 239000000203 mixture Substances 0.000 claims description 15
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 14
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 14
- 229910052742 iron Inorganic materials 0.000 claims description 11
- 239000011259 mixed solution Substances 0.000 claims description 11
- 238000011068 loading method Methods 0.000 claims description 10
- 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 9
- 239000012153 distilled water Substances 0.000 claims description 9
- 235000010413 sodium alginate Nutrition 0.000 claims description 9
- 239000000661 sodium alginate Substances 0.000 claims description 9
- 229940005550 sodium alginate Drugs 0.000 claims description 9
- 239000003638 chemical reducing agent Substances 0.000 claims description 8
- 239000008188 pellet Substances 0.000 claims description 8
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 6
- 238000001291 vacuum drying Methods 0.000 claims description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 5
- 239000001301 oxygen Substances 0.000 claims description 5
- 229910052760 oxygen Inorganic materials 0.000 claims description 5
- 239000012279 sodium borohydride Substances 0.000 claims description 5
- 229910000033 sodium borohydride Inorganic materials 0.000 claims description 5
- 238000000967 suction filtration Methods 0.000 claims description 5
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims description 4
- 239000001110 calcium chloride Substances 0.000 claims description 4
- 229910001628 calcium chloride Inorganic materials 0.000 claims description 4
- 229910000402 monopotassium phosphate Inorganic materials 0.000 claims description 4
- 235000019796 monopotassium phosphate Nutrition 0.000 claims description 4
- PJNZPQUBCPKICU-UHFFFAOYSA-N phosphoric acid;potassium Chemical compound [K].OP(O)(O)=O PJNZPQUBCPKICU-UHFFFAOYSA-N 0.000 claims description 4
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 3
- 238000000227 grinding Methods 0.000 claims description 3
- 239000011148 porous material Substances 0.000 claims description 3
- 239000011591 potassium Substances 0.000 claims description 3
- 229910052700 potassium Inorganic materials 0.000 claims description 3
- 238000011010 flushing procedure Methods 0.000 claims description 2
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 2
- 238000010899 nucleation Methods 0.000 claims description 2
- GSWAOPJLTADLTN-UHFFFAOYSA-N oxidanimine Chemical compound [O-][NH3+] GSWAOPJLTADLTN-UHFFFAOYSA-N 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 5
- 239000003795 chemical substances by application Substances 0.000 abstract description 3
- 238000005728 strengthening Methods 0.000 abstract description 3
- 239000002351 wastewater Substances 0.000 abstract description 3
- 230000000694 effects Effects 0.000 description 11
- 238000006243 chemical reaction Methods 0.000 description 10
- 238000005516 engineering process Methods 0.000 description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 8
- 241000894006 Bacteria Species 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 6
- 238000012546 transfer Methods 0.000 description 6
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 5
- XKMRRTOUMJRJIA-UHFFFAOYSA-N ammonia nh3 Chemical compound N.N XKMRRTOUMJRJIA-UHFFFAOYSA-N 0.000 description 5
- 230000014759 maintenance of location Effects 0.000 description 5
- 239000000463 material Substances 0.000 description 4
- 230000002572 peristaltic effect Effects 0.000 description 4
- 230000009467 reduction Effects 0.000 description 4
- 238000001179 sorption measurement Methods 0.000 description 4
- 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 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 239000007791 liquid phase Substances 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- 239000002028 Biomass Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 description 2
- 230000009471 action Effects 0.000 description 2
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- 239000008367 deionised water Substances 0.000 description 2
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- 238000001035 drying Methods 0.000 description 2
- 235000019441 ethanol Nutrition 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 238000007667 floating Methods 0.000 description 2
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- 244000005700 microbiome Species 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
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- 230000001105 regulatory effect Effects 0.000 description 2
- 239000003440 toxic substance Substances 0.000 description 2
- 239000011573 trace mineral Substances 0.000 description 2
- 235000013619 trace mineral Nutrition 0.000 description 2
- 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
- 230000002159 abnormal effect Effects 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
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- 238000003912 environmental pollution Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 239000005431 greenhouse gas Substances 0.000 description 1
- 230000003100 immobilizing effect Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 239000002054 inoculum Substances 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
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- 238000006116 polymerization reaction Methods 0.000 description 1
- 150000003077 polyols Chemical group 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
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- 238000011105 stabilization Methods 0.000 description 1
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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
-
- 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
- C02F3/30—Aerobic and anaerobic processes
- C02F3/302—Nitrification and denitrification treatment
- C02F3/307—Nitrification and denitrification treatment characterised by direct conversion of nitrite to molecular nitrogen, e.g. by using the Anammox process
-
- 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
- C02F2003/001—Biological treatment of water, waste water, or sewage using granular carriers or supports for the microorganisms
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- Life Sciences & Earth Sciences (AREA)
- Microbiology (AREA)
- Biodiversity & Conservation Biology (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Purification Treatments By Anaerobic Or Anaerobic And Aerobic Bacteria Or Animals (AREA)
Abstract
The invention belongs to the field of biological denitrification treatment of wastewater, and discloses anaerobic ammonia oxidation gel particles and a method for preparing and strengthening denitrification performance of an anaerobic ammonia oxidation process under a high total nitrogen load condition. The preparation method of the anaerobic ammonia oxidation gel particles comprises the following steps: preparing chitosan modified diatomite, preparing a gel agent and preparing anaerobic ammonia oxidation gel particles. According to the invention, the ANAMMOX gel particles and the ANAMMOX particle sludge with low total nitrogen load are mixed and added into the anaerobic ammonia oxidation process reactor with high total nitrogen load, so that the problems of remarkably reduced denitrification efficiency and unstable operation of the ANAMMOX process under the condition of higher total nitrogen load in the prior art are solved.
Description
Technical Field
The invention belongs to the field of biological denitrification treatment of wastewater, and in particular relates to anaerobic ammonia oxidation gel particles and a method for preparing and strengthening denitrification performance of an anaerobic ammonia oxidation process under the condition of high total nitrogen load.
Background
The anaerobic ammonia oxidation (ANAMMOX) process belongs to a novel biological denitrification technology, and has the obvious advantages of no need of aeration, no need of additional carbon source, high reaction rate and the like compared with the traditional biological denitrification technology. It is reported that compared with the traditional nitrification and denitrification process, the method for treating the nitrogen-containing wastewater by using the ANAMMOX process can eliminate the need of adding a carbon source and an aeration system and related power equipment, so that the operation and maintenance cost is greatly reduced; meanwhile, the output of the excess sludge is obviously reduced, a sludge treatment unit is omitted, and the occupied area of a process structure is obviously reduced; in addition, as the gas generated by the ANAMMOX reaction is mainly nitrogen, the emission of greenhouse gases is obviously reduced; therefore, the ANAMMOX process is regarded as a novel biological denitrification technology which is economical, energy-saving, efficient and low-carbon and has popularization and application values.
However, the existing large-scale popularization and application of the ANAMMOX process also face some non-negligible problems. For example, ANAMMOX bacteria grow slowly and at a high temperature; in addition, when the total nitrogen load of the inflow water is higher, the ANAMMOX denitrification process often faces the problems that the sludge floats up and runs off, biomass is difficult to maintain, the denitrification capacity of the reaction device is greatly reduced, and the treatment effect is obviously deteriorated. How to improve the operational stability and denitrification efficiency of the ANAMMOX denitrification process at high total nitrogen loading has been a challenging problem. And realizing good operation stability and higher denitrification efficiency of the ANAMMOX process under high total nitrogen load greatly promotes the practical application of the ANAMMOX process technology.
At present, related researchers have also continuously tried and explored to improve the treatment performance of the ANAMMOX process under high total nitrogen load, mainly comprising the steps of improving the structure of a reaction device, controlling proper hydraulic conditions, crushing floating sludge aggregates after being collected and then re-adding the sludge aggregates into a reactor, regulating and controlling the sedimentation performance of the sludge by utilizing an exogenous addition group induction signal, and the like.
However, the above-mentioned methods still suffer from various limitations in practical applications, such as improvement of the construction of the reaction apparatus, complicated implementation, and high cost; the control of proper hydraulic conditions is only suitable for specific conditions with slower water inflow velocity, and the exogenous addition of quorum sensing signals also faces the problems of signal cost and the like.
Therefore, it is currently needed to propose an anaerobic ammonia oxidation gel particle and a preparation method thereof, and apply the same to enhance the denitrification performance of the anaerobic ammonia oxidation process under the condition of high total nitrogen load.
Disclosure of Invention
The invention aims at overcoming the defects of the prior art, and provides anaerobic ammonia oxidation gel particles and a method for preparing and strengthening denitrification performance of an anaerobic ammonia oxidation process under the condition of high total nitrogen load. According to the invention, the ANAMMOX gel particles and the ANAMMOX particle sludge with low total nitrogen load are mixed and added into the anaerobic ammonia oxidation process reactor with high total nitrogen load, so that the problems of remarkably reduced denitrification efficiency and unstable operation of the ANAMMOX process under the condition of higher total nitrogen load in the prior art are solved.
In order to achieve the above object, a first aspect of the present invention provides a method for preparing anaerobic ammonium oxidation gel particles, the method comprising the steps of:
s1: preparation of chitosan modified diatomite
Mixing chitosan with water to obtain chitosan water solution; mixing the chitosan aqueous solution with diatomite, and sequentially carrying out stirring, vacuum suction filtration, roasting and grinding treatment to obtain the chitosan modified diatomite;
s2: preparation of gel
Mixing polyvinyl alcohol, sodium alginate and high-temperature distilled water, and stirring to obtain a gelatinous mixture; mixing and stirring the gelatinous mixture and the chitosan modified diatomite uniformly, and cooling to obtain the gel;
s3: preparation of anammox gel particles
Uniformly mixing anaerobic ammonia oxidation sludge with the gel and nano zero-valent iron to obtain a mixed solution; mixing the mixed solution with a calcium chloride aqueous solution and performing first crosslinking to obtain an ammonia oxide primary gel pellet; mixing the ammonia oxidation initial gel pellets with a potassium dihydrogen phosphate aqueous solution and performing secondary crosslinking to obtain the anaerobic ammonia oxidation gel particles.
According to the present invention, preferably, in step S1:
the stirring treatment equipment comprises a temperature-controlled magnetic stirrer; the temperature of the stirring treatment is 30-35 ℃, the time is 3-5h, and the stirring speed is 120-130r/min;
the roasting treatment equipment comprises a muffle furnace; the temperature of the roasting treatment is 450-550 ℃ and the time is 3-4h;
the chitosan modified diatomite is obtained by using a 120-150 mesh screen mesh, the grain diameter range of the chitosan modified diatomite is 100-125 mu m, and the specific surface area is 90-100m 2 And/g, the pore diameter is 19-136nm.
According to the present invention, preferably, in step S2:
the high-temperature distilled water is distilled water with the temperature of more than or equal to 90 ℃;
the content of polyvinyl alcohol is 11-15wt% and the content of sodium alginate is 1-2wt% based on the total weight of the gelatinous mixture;
the concentration of the chitosan modified diatomite in the gel is 2-6g/L;
the cooling is to cool the gel to 45-55 ℃.
In the invention, as a preferable scheme, in the step S2, polyvinyl alcohol, sodium alginate and high-temperature distilled water are mixed and continuously stirred to obtain a uniform gelatinous mixture; and mixing and stirring the gelatinous mixture and the chitosan modified diatomite within 5-15min from the beginning of stirring, enhancing the stirring strength to ensure uniform stirring, and cooling to obtain the gel.
According to the present invention, preferably, in step S3:
the mass fraction of the calcium chloride aqueous solution is 7-9wt%;
the time of the first crosslinking is 12-24 hours, and the temperature is 30-35 ℃;
the molar concentration of the potassium dihydrogen phosphate aqueous solution is 0.7-1.0mol/L;
the second crosslinking time is 1-5h, and the temperature is 30-35 ℃;
the anaerobic ammonia oxidation sludge has total nitrogen load lower than 0.4 kg-TN/(m) 3 Anaerobic ammoxidation sludge under d);
the volume ratio of the gel to the anaerobic ammonia oxidation sludge is (10-5): (3-4);
the concentration of the nano zero-valent iron in the mixed solution is 1.1-2.3g/L, and the particle size of the nano zero-valent iron is 100-150nm.
In the invention, in the step S3, the mixed solution of anaerobic ammoxidation sludge, the gel and the nano zero-valent iron is slowly stirred to prevent the nano zero-valent iron from being oxidized. Preferably, the above mixture is added dropwise to 7-9wt% CaCl by peristaltic pump 2 Crosslinking in aqueous solution for 12-24 hours at room temperature to complete a first crosslinking process, wherein the process can form anaerobic ammonia oxidation primary gel pellets after completion; thereafter, the oxidized primary gel pellets are added to KH of 0.7-1.0mol/L 2 PO 4 And (3) crosslinking in the aqueous solution for 1-5h at room temperature to complete a second crosslinking process, so that the anaerobic ammonia oxidation gel particles with stable structure and higher activity can be obtained, and the anaerobic ammonia oxidation gel particles are washed by deionized water and then stored at the temperature of 4 ℃ for standby.
According to the present invention, preferably, the preparation method of the nano zero-valent iron is a liquid phase reduction method, including: mixing the high-valence molten iron solution with citric acid and a strong reducing agent aqueous solution, uniformly mixing and stirring under nitrogen atmosphere, and carrying out vacuum suction filtration, flushing and vacuum drying to obtain the nano zero-valent iron.
According to the present invention, preferably, the molar concentration of the high-valent molten iron solution is 1.1 to 1.3mol/L; the high-valence molten iron solution is Fe 3+ Aqueous solution and/or Fe 2+ An aqueous solution.
According to the present invention, preferably, the molar concentration of the strong reducing agent aqueous solution is 0.8 to 1.2mol/L; the strong reducing agent is sodium borohydride and/or potassium borohydride.
According to the present invention, preferably, the vacuum drying is performed at a temperature of 55 to 65 ℃ for 15 to 25 hours.
In the invention, the preparation method of the nano zero-valent iron comprises the following steps: weighing 12.5-14.2g FeCl 3 ·6H 2 O is prepared into 1.1 to 1.3mol/LFECl 3 ·6H 2 And (3) uniformly stirring the O solution by using a precise quantitative electric stirrer, and introducing nitrogen in the stirring process to remove oxygen. Then 105-115ml of 0.2mol/L sodium borohydride (NaBH) 4 ) The aqueous solution is stirred electrically to stir NaBH by peristaltic pump 4 Dropwise adding the aqueous solution into the FeCl 3 ·6H 2 In the O solution, the solution gradually turns black and NaBH 4 After the completion of the dropwise addition, the reaction was continued for about 30 minutes under stirring. And then carrying out vacuum suction filtration on the black mixed solution to obtain stable black nano iron particles, washing the black nano iron particles by using 20% -30% ethanol aqueous solution, and washing again by using absolute ethanol. Finally, the washed black nano particles are placed in a vacuum drying oven at 60 ℃ for drying for 20 hours to obtain nano zero-valent iron (nZVI, 100-150 nm), and the nano zero-valent iron is taken out to a vacuum dryer for preservation. The reaction equation for preparing nZVI is shown below:
4Fe 3+ +3BH 4 - +9H 2 O→4Fe 0 ↓+3H 2 BO 3 - +12H + +6H 2 ↑；
the principle of preparing nano zero-valent iron by liquid phase reduction is that the nano zero-valent iron is prepared in high-valent iron solution, such as Fe 3+ And/or Fe 2+ The solution is added with a strong reducing agent (sodium borohydride, potassium borohydride and the like), and stable black nano zero-valent iron particles can be formed under the dispersion and stabilization actions of the strong reducing agent. The method is simple and feasible, has low cost and the obtained nano zero-valent iron has high reactivity.
According to the present invention, preferably, the particle diameter of the anammox gel particles is 3 to 8mm.
The invention also provides the anaerobic ammonia oxidation gel particles prepared by the preparation method of the anaerobic ammonia oxidation gel particles.
In a third aspect, the present invention provides a method for enhancing denitrification performance of an anaerobic ammonia oxidation process under high total nitrogen loading conditions, said method comprising seeding an anaerobic ammonia oxidation process reactor with anaerobic ammonia oxidation granular sludge and said anaerobic ammonia oxidation gel particles.
According to the present invention, preferably, the high total nitrogen load condition includes a total nitrogen load of 26.3 to 35.5 kg-TN/(m) 3 D) the pH of the reactor feed water is 7.0-8.0, the dissolved oxygen concentration of the reactor feed water is below 0.4mg/L, and the operating temperature of the reactor is 33-38 ℃.
According to the invention, the reactor is preferably an upward flow sludge bed reactor (UASB), and the upward flow sludge bed reactor preferably has a height of 80-100cm and an inner diameter of 8-12cm.
According to the present invention, preferably, the anaerobic ammonium oxidation granular sludge is obtained by taking a total nitrogen load of less than 0.4 kg-TN/(m) from 2 years of operation 3 The reactor of d), the particle size of the anaerobic ammonia oxidation granular sludge is 0.8-2.5mm.
According to the present invention, preferably, the volume ratio of the anaerobic ammonia oxidation gel particles to the anaerobic ammonia oxidation granular sludge is (1-2): (2-1).
According to the present invention, preferably, the ratio of the total volume of the anaerobic ammonia oxidation gel particles and anaerobic ammonia oxidation particulate sludge to the effective volume of the reactor is 1: (5-20).
The invention has the action principle that:
the denitrification performance and the operation stability of the ANAMMOX process are severely deteriorated under the condition of high total nitrogen load. This is mainly due to abnormal secretion of extracellular polymer in the ANAMMOX granular sludge caused by high total nitrogen load, and further causes loosening of the granular structure and reduction of the density, so that floating and loss of the granules occur. The invention embeds and immobilizes the ANAMMOX sludge to form ANAMMOX gel particles, and compared with the ANAMMOX granular sludge, the ANAMMOX gel particles have obviously improved particle stability and mechanical strength. Thus, at high total nitrogen loading, the retention of microorganisms in the reaction apparatus can be effectively increased by using the ANAMMOX gel particles. In addition, the ANAMMOX gel particles have strong resistance to the changes of different nitrogen concentrations, temperatures, toxic substance concentrations, organic load and the like of inflow water. The invention develops an embedding material which is economical, easy to maintain biological attachment and activity, excellent in mass transfer performance and high in mechanical strength, and successfully adopts an embedding immobilization technology to strengthen denitrification performance and operation stability of the ANAMMOX process under the condition of high total nitrogen load.
In the invention, the selected embedding agent polyvinyl alcohol (PVA) has lower price, regular polyol structure and better stability. However, PVA has limited mass transfer properties, and how to improve the mass transfer properties and specific surface area of PVA becomes one of the technical cores of the present invention. Diatomite is biological siliceous rock composed of siliceous remains of diatom and other microorganisms, has the characteristics of large specific surface area and strong surface adsorption performance, and is wide in source and easy to obtain. In addition, diatomite can adsorb cations such as ammonia nitrogen under neutral or weak alkaline conditions. Therefore, the diatomite is modified by the chitosan, the original porous structure of the diatomite is damaged, a novel three-dimensional porous structure is formed, and the specific surface area and the adsorption performance of the chitosan modified diatomite are further improved compared with those of the unmodified diatomite. Therefore, the mass transfer performance and the specific surface area of the embedding agent PVA are greatly improved by adding the chitosan modified diatomite. This is an important reason for the good mass transfer properties and adsorption properties of the ANAMMOX gel particles prepared in the present invention. The addition of nano zero-valent iron (nZVI) effectively stimulates the activity of ANAMMOX bacteria in ANAMMOX gel particles.
However, the ANAMMOX activity of ANAMMOX gel particles added with nZVI and chitosan modified diatomaceous earth is still not as high as that of ANAMMOX particle sludge in a structurally stable period. In order to ensure that sufficient biomass can be maintained in the reactor and that the anaerobic ammonia oxidation process has high ANAMMOX activity, so that the anaerobic ammonia oxidation process achieves optimal overall denitrification performance under high total nitrogen load, the addition of ANAMMOX gel particles and ANAMMOX granular sludge to the reactor is selected.
The technical scheme of the invention has the following beneficial effects:
(1) The main material of the anaerobic ammonia oxidation gel particles prepared by the invention has low price and wide sources, and the process of preparing the anaerobic ammonia oxidation gel particles is simpler, so the implementation cost of the technology is lower.
(2) According to the invention, as the addition of the chitosan modified diatomite leads the prepared anaerobic ammonia oxidation gel particles to obviously improve the adsorption and mass transfer performance compared with the common gel particles, and the addition of the nano zero-valent iron (nZVI) also effectively stimulates the activity of the ANAMMOX bacteria, the biological retention quantity of the ANAMMOX bacteria in the reactor can be effectively improved by adopting the technology of the invention, the activity retention of the ANAMMOX bacteria is facilitated, and the anaerobic ammonia oxidation process reactor with high total nitrogen load can keep higher denitrification efficiency and operation stability;
(3) The technology is suitable for different types of reaction devices and different inflow water flow rates, has stronger resistance to toxic substances in inflow water or other water quality changes, and has wider application range;
(4) The PVA (polyvinyl alcohol), chitosan and diatomite used in the invention are all environment-friendly materials, so the invention does not cause the problem of secondary environmental pollution.
(5) According to the invention, the ANAMMOX gel particles are formed by embedding and immobilizing the ANAMMOX sludge, and the ANAMMOX gel particles and the ANAMMOX particle sludge with low total nitrogen load are mixed and added into an anaerobic ammonia oxidation process reactor with high total nitrogen load, so that the problems of remarkably reduced denitrification efficiency and unstable operation of the ANAMMOX process under the condition of higher total nitrogen load in the prior art are solved.
Additional features and advantages of the invention will be set forth in the detailed description which follows.
Drawings
The foregoing and other objects, features and advantages of the invention will be apparent from the following more particular descriptions of exemplary embodiments of the invention as illustrated in the accompanying drawings wherein like reference numbers generally represent like parts throughout the exemplary embodiments of the invention.
FIG. 1 is a schematic diagram showing the effect of different volume ratios of gel particles and granular sludge on total nitrogen removal rate at high total nitrogen load for a method of enhancing denitrification performance of an anaerobic ammonia oxidation process provided in examples 2-4 of the present invention.
FIG. 2 is a graph showing the effect of different inoculums of the anaerobic ammonia oxidation process at high total nitrogen loading provided by example 2 and comparative examples 1-2 of the present invention on total nitrogen removal at high total nitrogen loading.
Detailed Description
Preferred embodiments of the present invention will be described in more detail below. While the preferred embodiments of the present invention are described below, it should be understood that the present invention may be embodied in various forms and should not be limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the scope of the invention to those skilled in the art.
Example 1
The embodiment provides a preparation method of anaerobic ammonia oxidation gel particles, which comprises the following steps:
s1: preparation of chitosan modified diatomite
Firstly, placing chitosan into a conical flask, and adding a proper amount of distilled water to prepare a chitosan aqueous solution. Then the diatomite is weighed and added into the chitosan water solution, and stirred for 3 to 5 hours (room temperature, 120 to 130 r/min) by using a temperature-control magnetic stirrer. Vacuum filtering with vacuum filter, roasting in muffle furnace for 3-4 hr (500 deg.C), grinding, sieving with 120 mesh and 150 mesh sieve to obtain powder with particle diameter of 100-125 μm and specific surface area of 96m 2 And/g, chitosan modified diatomite with a pore diameter of 19-136nm.
S2: preparation of gel
Mixing polyvinyl alcohol (polymerization degree 1830+ -20, saponification degree about 99%, analytical grade), sodium alginate (viscosity of Sodium Alginate (SA) about 162 mpa.s) with distilled water above 90 ℃ and continuously stirring to obtain a uniform colloidal mixture (the content of polyvinyl alcohol is 11wt% and the content of sodium alginate is 1.5wt% based on the total weight of the colloidal mixture); mixing and stirring the gelatinous mixture and the chitosan modified diatomite (the concentration of the chitosan modified diatomite in the gel is 2 g/L) within 5-15min from the beginning of stirring, enhancing the stirring strength to ensure uniform stirring, and cooling to 50 ℃ to obtain the gel;
s3: preparation of anammox gel particles
Anaerobic ammonium oxidation sludge (total nitrogen load lower than 0.4 kg-TN/(m) 3 Anaerobic ammonia oxidation sludge under d) is uniformly mixed with the gelling agent and nano zero-valent iron to obtain a mixed solution (the volume ratio of the gelling agent to the anaerobic ammonia oxidation sludge is 10:9, a step of performing the process; the concentration of the nano zero-valent iron in the mixed solution is 1.1g/L, and the particle size of the nano zero-valent iron is 100-150 nm);
the mixture was added drop-wise to 7% by weight CaCl using peristaltic pumps 2 Crosslinking in aqueous solution for 20 hours at room temperature to complete a first crosslinking process, wherein after the process is completed, anaerobic ammonia oxidation primary gel pellets can be formed; thereafter, the oxidized primary gel pellets were added to 0.7mol/L KH 2 PO 4 And (3) crosslinking for 3 hours at room temperature in an aqueous solution to finish a second crosslinking process, wherein anaerobic ammonia oxidation gel particles with stable structure and higher activity (the particle size of the anaerobic ammonia oxidation gel particles is 3-8 mm) can be obtained, and the anaerobic ammonia oxidation gel particles are washed by deionized water and then stored at the temperature of 4 ℃ for standby.
The preparation method of the nano zero-valent iron is a liquid phase reduction method and comprises the following steps: weigh 12.5g FeCl 3 ·6H 2 O, formulated as 1.1mol/LFECl 3 ·6H 2 And (3) uniformly stirring the O solution by using a precise quantitative electric stirrer, and introducing nitrogen in the stirring process to remove oxygen. Thereafter, 105mL of 0.2mol/L sodium borohydride (NaBH) 4 ) The aqueous solution is stirred electrically to stir NaBH by peristaltic pump 4 Dropwise adding the aqueous solution into the FeCl 3 ·6H 2 In the O solution, the solution gradually turns black and NaBH 4 After the completion of the dropwise addition, the reaction was continued for 30 minutes under stirring. Then vacuum filtering the black mixed solution to obtain stable black nano-iron particles, and firstly using 30% ethanol aqueous solution to make the black nano-iron particlesWashing, and then washing again by using absolute ethyl alcohol. Finally, the washed black nano particles are placed in a vacuum drying oven at 60 ℃ for drying for 20 hours to obtain nano zero-valent iron (nZVI, 100-150 nm), and the nano zero-valent iron is taken out to a vacuum dryer for preservation.
Example 2
The present example provides a method for enhancing denitrification performance of an anaerobic ammonia oxidation process under high total nitrogen loading conditions, the method comprising inoculating anaerobic ammonia oxidation granular sludge and the anaerobic ammonia oxidation gel particles (group a (V 2 Group)).
The high total nitrogen load condition is manually prepared by adopting:
in the operation stage I (1-10 d), the ammonia nitrogen concentration of the reactor inlet water is 350mg/L, the nitrate nitrogen concentration of the reactor inlet Shui Ya is 462mg/L, and the Hydraulic Retention Time (HRT) of the reactor is controlled to be 8h (the total nitrogen load is about 1.50 kg-TN/(m) 3 D)); the water inlet component of the reactor also comprises KH 2 PO 4 (78mg/L)，KHCO 3 (347mg/L)，MgSO 4 ·7H 2 O(370mg/L)，CaCl 2 ·2H 2 O(70mg/L)，NH 4 Cl and NaNO 2 400mg/L and 687mg/L, respectively, and 1mL/L of each of the trace element solutions I and II was added. The microelement solution I consists of 5.00g/L EDTA and 5.00g/L FeSO 4 Composition; the trace element II consists of 15.00g/L EDTA and 0.43g/L ZnSO 4 ·4H 2 O、0.99g/L MnCl 2 ·4H 2 O、0.014g/LH 3 BO 4 、0.25g/L CuSO 4 ·5H 2 O、0.22g/L Na 2 MoO 4 ·2H 2 O、0.21g/LNa 2 SeO 4 ·10H 2 O and 0.19g/L NiCl 2 ·6H 2 O composition.
In the operation stage II (11-40 d), the ammonia nitrogen concentration of the inlet water is maintained to be 284mg/L and the nitrite nitrogen concentration is maintained to be 369mg/L, and the HRT is reduced to 4h (the total nitrogen load is about 3.92 kg-TN/(m) 3 ·d))；
In the operation stage III (41-75 d), the ammonia nitrogen concentration of the inlet water is continuously increased to 400mg/L and the nitrite nitrogen concentration is continuously increased to 520mg/L, and the HRT is regulated to 3.5h (the total nitrogen load is about 6.45 kg-TN/(m) 3 ·d))；
Run stage IV (76-110 d) continueIncreasing ammonia nitrogen concentration of the inlet water to 450mg/L and nitrite nitrogen concentration to 585mg/L, and adjusting HRT to 3.0h (total nitrogen load is about 8.40 kg-TN/(m) 3 ·d))。
During the whole operation period, the pH value of the reactor inlet water is 7.2-8.0, the dissolved oxygen concentration of the reactor inlet water is below 0.1mg/L, and the operation temperature of the reactor is 33-35 ℃.
The reactor is an upward flow sludge bed reactor (UASB), the height is 95cm, the inner diameter is 9.5cm, the material is acrylic, the outermost layer is a water bath layer, and the internal reflux ratio of the effluent is set to be 2.5.
The anaerobic ammonia oxidation granular sludge is obtained from stable operation for more than 2 years, and the total nitrogen load is lower than 0.4 kg-TN/(m) 3 The reactor of d), the particle size of the anaerobic ammonia oxidation granular sludge is 0.8-2.5mm.
The volume ratio of the anaerobic ammonia oxidation gel particles to the anaerobic ammonia oxidation granular sludge is 1:1.
the ratio of the total volume of the anaerobic ammonia oxidation gel particles and anaerobic ammonia oxidation granular sludge to the effective volume of the reactor is 1:5.
example 3
The present embodiment provides a method for enhancing denitrification performance of anaerobic ammoxidation process under high total nitrogen load condition, and the difference between the present embodiment and embodiment 2 is that: the volume ratio of the anaerobic ammonia oxidation gel particles to the anaerobic ammonia oxidation granular sludge is 1:0.5 (V) 1 A group).
Example 4
The present embodiment provides a method for enhancing denitrification performance of anaerobic ammoxidation process under high total nitrogen load condition, and the difference between the present embodiment and embodiment 2 is that: the volume ratio of the anaerobic ammonia oxidation gel particles to the anaerobic ammonia oxidation granular sludge is 1:2 (V) 3 A group).
As shown in fig. 1, V during the whole operation 2 The total nitrogen removal rate of the group is highest, and in the operation stages I-IV, V 2 Total nitrogen removal rates of the groups were 91%, 85%, 90% and 82%, respectively; v (V) 1 The total nitrogen removal rates of the groups were 89%, 77%, 69% and 56%, respectively; and V is 3 The total nitrogen removal rate of the group is the lowest, and in the stages I-IV, the total nitrogen is removedThe rates were 92%, 69%, 61% and 48%, respectively.
Comparative example 1
This comparative example provides an anaerobic ammoxidation process under high total nitrogen loading conditions which differs from example 1 only in that: only the same anaerobic ammonium oxidation gel particles (group B) as in group a (example 2) were inoculated in the anaerobic ammonium oxidation process reactor.
The ratio of the volume of the anaerobic ammonia oxidation gel particles to the effective volume of the reactor is 1:5.
comparative example 2
This comparative example provides an anaerobic ammoxidation process under high total nitrogen loading conditions which differs from example 1 only in that: the anaerobic ammonia oxidation process reactor was inoculated with only the same anaerobic ammonia oxidation granular sludge (group C) as in group a (example 2).
The ratio of the volume of the anaerobic ammonia oxidation granular sludge to the effective volume of the reactor is 1:5.
as shown in fig. 2:
in run I, at a total nitrogen load of about 1.50 kg-TN/(m3.d), the total nitrogen removal from the reactor run to day 5, A, B and group C reactors remained high at 91%,90% and 93%, respectively;
in the operation stage II, the total nitrogen load is increased to 4.92 kg-TN/(m 3. D), and when the reactor is operated to 25 days, the total nitrogen removal rates of the A, B and C group reactors are reduced to 87%, 75% and 68%, respectively, but the total nitrogen removal rate of the A group is obviously higher than that of the B group and the C group;
in the operation stage III, the total nitrogen load is continuously increased to 6.51 kg-TN/(m 3. D), when the reactor is operated to 55 days, the total nitrogen removal rate of the group B reactor and the group C reactor is obviously reduced to 67% and 57% respectively, and the total nitrogen removal rate of the group A reactor is increased to 94%;
in the operation stage IV, the total nitrogen load is increased to 18.43 kg-TN/(m 3. D), the reactor is operated until 105 days, the denitrification performance of the group C reactor is seriously deteriorated, the total nitrogen removal rate is greatly reduced to 34%, the total nitrogen removal rate of the group B reactor is higher than that of the group C (60%), however, the total nitrogen removal rate of the group A reactor is obviously higher than that of the group B and the group C under the high total nitrogen load and is up to 84%.
Meanwhile, by monitoring, the surface of the anaerobic ammonia oxidation gel particles of the group A reactor is adsorbed with a considerable amount of anaerobic ammonia oxidation bacteria from disintegrated anaerobic ammonia oxidation particle sludge, so that the biological retention quantity of the group A reactor is not obviously reduced compared with that of the group B reactor, but the denitrification rate of the group A is obviously improved.
As can be seen from examples 2-4 and comparative examples 1-2, inoculating anaerobic ammonia oxidation granular sludge and the anaerobic ammonia oxidation gel particles of the invention in the anaerobic ammonia oxidation process reactor can effectively improve the denitrification performance and the operation stability of the ANAMMOX system under the condition of high total nitrogen load, and the optimal mixing ratio of the gel particles and the granular sludge is 1:1, so that the technology has great application potential.
The foregoing description of embodiments of the invention has been presented for purposes of illustration and description, and is not intended to be exhaustive or limited to the embodiments disclosed. Many modifications and variations will be apparent to those of ordinary skill in the art without departing from the scope and spirit of the various embodiments described.
Claims (10)
1. A method for preparing anaerobic ammonia oxidation gel particles, which is characterized by comprising the following steps:
s1: preparation of chitosan modified diatomite
Mixing chitosan with water to obtain chitosan water solution; mixing the chitosan aqueous solution with diatomite, and sequentially carrying out stirring, vacuum suction filtration, roasting and grinding treatment to obtain the chitosan modified diatomite;
s2: preparation of gel
Mixing polyvinyl alcohol, sodium alginate and high-temperature distilled water, and stirring to obtain a gelatinous mixture; mixing and stirring the gelatinous mixture and the chitosan modified diatomite uniformly, and cooling to obtain the gel;
s3: preparation of anammox gel particles
Uniformly mixing anaerobic ammonia oxidation sludge with the gel and nano zero-valent iron to obtain a mixed solution; mixing the mixed solution with a calcium chloride aqueous solution and performing first crosslinking to obtain an ammonia oxide primary gel pellet; mixing the ammonia oxidation initial gel pellets with a potassium dihydrogen phosphate aqueous solution and performing secondary crosslinking to obtain the anaerobic ammonia oxidation gel particles.
2. The method for producing anammox gel particles as claimed in claim 1, wherein, in step S1:
the stirring treatment equipment comprises a temperature-controlled magnetic stirrer; the temperature of the stirring treatment is 30-35 ℃, the time is 3-5h, and the stirring speed is 120-130r/min;
the roasting treatment equipment comprises a muffle furnace; the temperature of the roasting treatment is 450-550 ℃ and the time is 3-4h;
the particle size range of the chitosan modified diatomite is 100-125 mu m, and the specific surface area is 90-100m 2 And/g, the pore diameter is 19-136nm.
3. The method for producing anammox gel particles as claimed in claim 1, wherein, in step S2:
the high-temperature distilled water is distilled water with the temperature of more than or equal to 90 ℃;
the content of polyvinyl alcohol is 11-15wt% and the content of sodium alginate is 1-2wt% based on the total weight of the gelatinous mixture;
the concentration of the chitosan modified diatomite in the gel is 2-6g/L;
the cooling is to cool the gel to 45-55 ℃.
4. The method for producing anammox gel particles as claimed in claim 1, wherein, in step S3:
the mass fraction of the calcium chloride aqueous solution is 7-9wt%;
the time of the first crosslinking is 12-24 hours, and the temperature is 30-35 ℃;
the molar concentration of the potassium dihydrogen phosphate aqueous solution is 0.7-1.0mol/L;
the second crosslinking time is 1-5h, and the temperature is 30-35 ℃;
the anaerobic ammonia oxidation sludge has total nitrogen load lower than 0.4 kg-TN/(m) 3 Anaerobic ammoxidation sludge under d);
the volume ratio of the gel to the anaerobic ammonia oxidation sludge is (10-5): (3-4);
the concentration of the nano zero-valent iron in the mixed solution is 1.1-2.3g/L, and the particle size of the nano zero-valent iron is 100-150nm.
5. The method for preparing anammox gel particles as claimed in claim 1 or 4, wherein the method for preparing nano zero-valent iron comprises: mixing the high-valence molten iron solution with citric acid and a strong reducing agent aqueous solution, uniformly mixing and stirring under nitrogen atmosphere, and carrying out vacuum suction filtration, flushing and vacuum drying to obtain the nano zero-valent iron.
6. The method for producing anammox gel particles according to claim 5, wherein,
the molar concentration of the high-valence molten iron solution is 1.1-1.3mol/L; the high-valence molten iron solution is Fe 3+ Aqueous solution and/or Fe 2+ An aqueous solution;
the molar concentration of the strong reducing agent aqueous solution is 0.8-1.2mol/L; the strong reducing agent is sodium borohydride and/or potassium borohydride;
the temperature of the vacuum drying is 55-65 ℃ and the time is 15-25h.
7. The method for producing anammox gel particles according to claim 1, wherein the anammox gel particles have a particle diameter of 3 to 8mm.
8. An anammox gel particle produced by the process for producing an anammox gel particle as defined in any one of claims 1 to 7.
9. A method of enhancing denitrification performance of an anaerobic ammonia oxidation process under high total nitrogen loading conditions, the method comprising seeding an anaerobic ammonia oxidation process reactor with an anaerobic ammonia oxidation granular sludge and the anaerobic ammonia oxidation gel particles of claim 8.
10. The method for enhancing denitrification performance of an anaerobic ammonia oxidation process under high total nitrogen loading conditions according to claim 9, wherein,
the high total nitrogen load condition includes a total nitrogen load of 26.3-35.5 kg-TN/(m) 3 D), the pH of the reactor inlet water is 7.0-8.0, the dissolved oxygen concentration of the reactor inlet water is below 0.4mg/L, and the running temperature of the reactor is 33-38 ℃;
the reactor is an upward flow sludge bed reactor;
the anaerobic ammonia oxidation granular sludge is obtained from the operation for more than 2 years, and the total nitrogen load is lower than 0.4 kg-TN/(m) 3 The reactor of d), the particle size of the anaerobic ammonia oxidation granular sludge is 0.8-2.5mm;
the volume ratio of the anaerobic ammonia oxidation gel particles to the anaerobic ammonia oxidation granular sludge is (1-2): (2-1);
the ratio of the total volume of the anaerobic ammonia oxidation gel particles and anaerobic ammonia oxidation granular sludge to the effective volume of the reactor is 1: (5-20).
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