CN103755109B - Storage and reactivation methods of anaerobic ammonia oxidation granule sludge - Google Patents
Storage and reactivation methods of anaerobic ammonia oxidation granule sludge Download PDFInfo
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- CN103755109B CN103755109B CN201310743603.6A CN201310743603A CN103755109B CN 103755109 B CN103755109 B CN 103755109B CN 201310743603 A CN201310743603 A CN 201310743603A CN 103755109 B CN103755109 B CN 103755109B
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- dimethyl sulfoxide
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- 239000010802 sludge Substances 0.000 title claims abstract description 44
- 238000000034 method Methods 0.000 title claims abstract description 38
- 230000003647 oxidation Effects 0.000 title claims abstract description 33
- 238000007254 oxidation reaction Methods 0.000 title claims abstract description 33
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 title claims abstract description 32
- 239000008187 granular material Substances 0.000 title claims abstract description 20
- 229910021529 ammonia Inorganic materials 0.000 title claims abstract description 16
- 230000007420 reactivation Effects 0.000 title claims abstract description 13
- 238000003860 storage Methods 0.000 title claims abstract description 10
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims abstract description 82
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000004140 cleaning Methods 0.000 claims abstract description 15
- 230000006978 adaptation Effects 0.000 claims abstract description 13
- 229910017053 inorganic salt Inorganic materials 0.000 claims abstract description 13
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000007853 buffer solution Substances 0.000 claims abstract description 8
- 229910052786 argon Inorganic materials 0.000 claims abstract description 5
- 239000004033 plastic Substances 0.000 claims abstract description 5
- 229920003023 plastic Polymers 0.000 claims abstract description 5
- 238000011084 recovery Methods 0.000 claims abstract description 4
- 238000004321 preservation Methods 0.000 claims description 28
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 18
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 17
- 229910052757 nitrogen Inorganic materials 0.000 claims description 9
- 230000004913 activation Effects 0.000 claims description 6
- XKMRRTOUMJRJIA-UHFFFAOYSA-N ammonia nh3 Chemical compound N.N XKMRRTOUMJRJIA-UHFFFAOYSA-N 0.000 claims description 5
- 238000013016 damping Methods 0.000 claims description 5
- 239000012530 fluid Substances 0.000 claims description 5
- 239000010801 sewage sludge Substances 0.000 claims description 5
- JVMRPSJZNHXORP-UHFFFAOYSA-N ON=O.ON=O.ON=O.N Chemical compound ON=O.ON=O.ON=O.N JVMRPSJZNHXORP-UHFFFAOYSA-N 0.000 claims description 4
- 238000005273 aeration Methods 0.000 claims description 4
- 239000007789 gas Substances 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 4
- 238000012261 overproduction Methods 0.000 claims description 4
- 238000005057 refrigeration Methods 0.000 claims description 3
- 238000000151 deposition Methods 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 claims description 2
- 239000000758 substrate Substances 0.000 claims description 2
- 230000000694 effects Effects 0.000 abstract description 7
- 238000005406 washing Methods 0.000 abstract 1
- 241000894006 Bacteria Species 0.000 description 3
- 241001453382 Nitrosomonadales Species 0.000 description 2
- 230000001580 bacterial effect Effects 0.000 description 2
- 239000012153 distilled water Substances 0.000 description 2
- 230000008030 elimination Effects 0.000 description 2
- 238000003379 elimination reaction Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005779 cell damage Effects 0.000 description 1
- 208000037887 cell injury Diseases 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000005138 cryopreservation Methods 0.000 description 1
- 239000002577 cryoprotective agent Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000004108 freeze drying Methods 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
Classifications
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- Y02W10/12—
Landscapes
- Treatment Of Sludge (AREA)
- Purification Treatments By Anaerobic Or Anaerobic And Aerobic Bacteria Or Animals (AREA)
Abstract
The invention provides a storage method of anaerobic ammonia oxidation granule sludge. The storage method comprises the steps of collecting anaerobic ammonia oxidation granule sludge to be stored; firstly, washing the anaerobic ammonia oxidation granule sludge for 3-5 times by using an inorganic salt buffer solution before storage; selecting a clean organic plastic bottle with good air tightness as a storage container; firstly, adding clean water and dimethyl sulfoxide to the storage container, and putting the storage container into an environment at 0-4 DEG C for refrigerating for 3-6 hours, so as to transfer the cleaned sludge to the refrigerated sealed container; placing the sealed container in the environment at 0-4 DEG C to store after aerating for 20-30 minutes by argon. The invention also provides a reactivation method of stored anaerobic ammonia oxidation granule sludge. The reactivation method comprises the steps of taking out the storage container; firstly, carrying out a temperature adaptation test before activity recovery; cleaning the stored granule sludge for 6-10 times by using the inorganic salt buffer solution after temperature adaptation, and then transferring to an anaerobic reactor to be started to carry out activity recovery. By adopting the methods, the anaerobic ammonia oxidation granule sludge can be successfully stored, and the activity of the granule sludge is quick to recover, so that the subsequent use is convenient.
Description
Technical field
The present invention relates to a kind of preservation and reactivation method of anaerobic ammonium oxidation granular sludge.
Background technology
Anaerobic ammonia oxidation process receives much concern because it is energy-efficient.The core carrier that anaerobic ammonia oxidizing bacteria reacts as Anammox, from last century the nineties find that it is present in industrialized waste water treatment plant and theoretical investigation is crossed in practical application further.But the anaerobic ammonia oxidizing bacteria doubling time is long, increasess slowly, be thus applied to actual waste water process more difficult.Enrichment culture also effective preservation Anammox bacterial classification is the effective measure breaking through application bottleneck.
Common preiservative methods has whiteruss method, liquid nitrogen method, cold method, lyophilization and gel embedding method etc.Though these technology can effectively retain bacteria be active to a certain extent, if but be applied to the preservation process of anaerobic ammonium oxidation granular sludge, then inevitably there is certain drawback, as affected granule sludge form, causes that sludge structure makes a variation, operating process is complicated and operative technique requires high.
Summary of the invention
The object of the present invention is to provide a kind of preservation and reactivation method of anaerobic ammonium oxidation granular sludge.
The technical solution used in the present invention is:
A store method for anaerobic ammonium oxidation granular sludge, described store method is:
By the granule sludge of anaerobic ammonia oxidation reactor overproduction and/or go out sewage sludge collect, for needing the mud preserved, using the clean and organic plastics bottle of good leak tightness as preservation container, the sludge volume preserved is needed to be the preferred 1:3 of 1:2 ~ 4(with the volumetric ratio of preservation container), first in preservation container, add clean water and dimethyl sulfoxide (DMSO), the volume ratio of clean water and mud is the preferred 1:1 of 1:0.8 ~ 1.2(), the add-on of dimethyl sulfoxide (DMSO) is preservation system (the i.e. mud made after finally adding mud, crystal water, the preservation system of dimethyl sulfoxide (DMSO) mixing composition) in the volume fraction of dimethyl sulfoxide (DMSO) be 2% ~ 10%(preferably 4 ~ 5%), by be added with clean water and dimethyl sulfoxide (DMSO) preservation container closure after at 0 ~ 4 DEG C temp. keeping (usually refrigerating 3 ~ 6h), liquid in container temperature is made to be 0 ~ 4 DEG C, take out and obtain the container after refrigerating, inorganic salt buffer solution for cleaning is first used 3 ~ 5 times by needing the mud preserved, mud after cleaning loads the container after refrigeration, after argon gas aeration 20 ~ 30min, encloses container, make to be in anoxic condition in encloses container, finally the encloses container that above-mentioned mud, water and dimethyl sulfoxide (DMSO) are housed is placed in the environment of 0 ~ 4 DEG C and preserves.
The component of described inorganic salt damping fluid is composed as follows: KH
2pO
45 ~ 20mgL
-1, CaCl
22H
2o1 ~ 10mgL
-1, MgSO
42H
2o200 ~ 400mgL
-1, KHCO
3800 ~ 1500mgL
-1, preferred ingredient consists of: KH
2pO
410mgL
-1, CaCl
22H
2o7.4mgL
-1, MgSO
42H
2o300mgL
-1, KHCO
31250mgL
-1.
The present invention also provides the reactivation method of the anaerobic ammonium oxidation granular sludge after preservation, described reactivation method is: taken out by the preservation container depositing anaerobic ammonium oxidation granular sludge, carry out thermal adaptation operation, 2 ~ 4 thermogrades are on average chosen between storage temperature and default recovery temperature, heating in water bath is incubated, preserve container and be incubated adaptation 12 ~ 36h at each temperature, after thermal adaptation, take out the anaerobic ammonium oxidation granular sludge after preserving, by the inorganic salt buffer solution for cleaning 6 ~ 10 times with identical component in store method, mud after cleaning adds in anaerobic reactor to be launched and carries out activation recovering: the operational conditions of anaerobic reactor is: run at normal temperature or middle temperature 30 ~ 38 DEG C, hydraulic detention time (HRT) is 2 ~ 6h, initial influent ammonia nitrogen and nitrite nitrogen concentration are respectively 42 ~ 98mgL
-1, increase water inlet substrate concn and shorten these two kinds of adjustable strategies of HRT and carry out respectively or intersect carrying out, until reactor total nitrogen removal efficiency more than 85%, obtain higher nitrogen removal performance and can steady in a long-termly run.
Further, when anaerobic reactor to be launched runs at normal temperatures, preferred described thermal adaptation step is: preserve container and first at 6 ~ 8 DEG C, adapt to 12 ~ 36h, then adapt to 12 ~ 36h at 12 ~ 14 DEG C, finally at 18 ~ 22 DEG C, adapt to 12 ~ 36h.
The present invention is gone out sewage sludge by the granule sludge or anaerobic ammonia oxidation reactor preserving anaerobic ammonia oxidation reactor overproduction and is maintained its anaerobic ammoxidation activity, solves a difficult problem for bacterium source scarcity in anaerobic ammonia oxidation process practical application.Embodiment of the present invention test proof this method can be good at preserving anaerobic ammonium oxidation granular sludge, and when dropping into application, activation recovering is very fast also can start anaerobic ammonia oxidation reactor fast, and reactor nitrogen removal performance promotes very fast within a short period of time.
Beneficial effect of the present invention is mainly reflected in: 1. cryopreservation bacterial classification avoids the impact of the excessive self-dissolving of bacterium under normal temperature and comparatively high temps; 2. the interpolation of cryoprotective agent dimethyl sulfoxide (DMSO) helps avoid cell injury; 3. the stability that any process ensure that Conservation environment is not done to encloses container between preservation period, easy and simple to handle; 4. the impact of temperature to granule sludge activity has effectively been contained in the thermal adaptation test before reactivation granule sludge; 5. the long period can preserve anaerobic ammonium oxidation granular sludge and can higher anaerobic ammoxidation activity be maintained.
Embodiment
Below in conjunction with specific embodiment, the present invention is described further, but protection scope of the present invention is not limited in this:
Embodiment 1:
Anaerobic ammonium oxidation granular sludge and the anaerobic ammonia oxidation reactor of collecting laboratory surplus go out sewage sludge, with inorganic salt damping fluid (composition: KH
2pO
410mgL
-1, CaCl
22H
2o7.4mgL
-1, MgSO
42H
2o300mgL
-1, KHCO
31250mgL
-1) clean 3 times, preserve in units of the mud after the cleaning of 0.5L.Save set is selected to customize the organic plastics bottle that volume is 1.5L osculum, and soaks 3d with after distilled water cleaning.After preparation work, to preserving the distilled water and the 50mL dimethyl sulfoxide (DMSO) that add 0.5L in container, put it into the refrigerator of 4 DEG C, guarantee to take out after in encloses container, solution temperature is 4 DEG C through 4h, granule sludge to be saved for 0.5L is gone in encloses container, and through argon gas aeration 30min, then cover tightly lid and form enclosed space, preserve in the refrigerator finally encloses container being placed 4 DEG C.
Preserve after two months, thermal adaptation before first carrying out activation recovering under the water-bath gradient temperature of 6 DEG C-14 DEG C-20 DEG C after encloses container takes out, 24h is adapted to respectively at each temperature, after thermal adaptation, take out the granule sludge above-mentioned inorganic salt buffer solution for cleaning 7 times after preserving, then the mud after cleaning being proceeded to effective volume is that the upflow anaerobic sludge blanket reactor of 0.5L carries out activation recovering.Reactor runs at normal temperatures, and HRT is 3h, and influent ammonia nitrogen and nitrite nitrogen concentration are respectively since 70mgL
-1progressively increase, move to 10d, the ratio of the ammonia nitrogen that reactor is removed and nitrite nitrogen is 1:1.32, and the nitre nitrogen of generation is 0.21 with the ratio of the ammonia nitrogen of removal, closely the theoretical ratio of Anammox reaction, now shows that anaerobic ammonia oxidation reactor has started successfully.Continue to move to 32d, in reactor, total nitrogen elimination capacity reaches 4.38kgm
-3d
-1(granule sludge can make reactor total nitrogen elimination capacity be up to 6.41kgm before preserving in carried reactor
-3d
-1), move to 47d, water inlet total nitrogen concentration has reached to 508mgL
-1.Simultaneously during activation recovering, particle characteristics is also greatly improved.At 13d, level before the activity of granule sludge reaches and preserves is 0.14g Ng
-1vSSd
-1, total Extracellular polymers content is by the 2.12gg before preserving
-1vSS increases to 2.41gg
-1vSS, content of hemachrome is from 0.02 μm of olg
-1vSS increases sharply to 0.42 μm of olg
-1vSS.As can be seen here, anaerobic ammonium oxidation granular sludge is preserved and reactivation is connected proper, and after granule sludge reactivation, proterties is excellent, functional.
Claims (7)
1. a store method for anaerobic ammonium oxidation granular sludge, is characterized in that described store method is:
By the granule sludge of anaerobic ammonia oxidation reactor overproduction and/or go out sewage sludge collect, for needing the mud preserved, using the clean and organic plastics bottle of good leak tightness as preservation container, the sludge volume preserved is needed to be 1:2 ~ 4 with the volumetric ratio of preservation container, first in preservation container, add clean water and dimethyl sulfoxide (DMSO), the volume ratio of clean water and mud is 1:0.8 ~ 1.2, the add-on of dimethyl sulfoxide (DMSO) makes the volume fraction of dimethyl sulfoxide (DMSO) in the preservation system after finally adding mud be 2% ~ 10%, by be added with clean water and dimethyl sulfoxide (DMSO) preservation container closure after at 0 ~ 4 DEG C temp. keeping, liquid in container temperature is made to be 0 ~ 4 DEG C, take out and obtain the container after refrigerating, inorganic salt buffer solution for cleaning is first used 3 ~ 5 times by needing the mud preserved, mud after cleaning loads the container after refrigeration, after argon gas aeration 20 ~ 30min, encloses container, make to be in anoxic condition in encloses container, finally the encloses container that above-mentioned mud, water and dimethyl sulfoxide (DMSO) are housed is placed in the environment of 0 ~ 4 DEG C and preserves,
The component of described inorganic salt damping fluid is composed as follows: KH
2pO
45 ~ 20mgL
-1, CaCl
22H
2o 1 ~ 10mgL
-1, MgSO
42H
2o 200 ~ 400mgL
-1, KHCO
3800 ~ 1500mgL
-1.
2. the method for claim 1, is characterized in that the component of inorganic salt damping fluid is composed as follows: KH
2pO
410mgL
-1, CaCl
22H
2o 7.4mgL
-1, MgSO
42H
2o300mgL
-1, KHCO
31250mgL
-1.
3. the method for claim 1, is characterized in that the sludge volume that described needs are preserved is 1:3 with the volumetric ratio of preservation container.
4. the method for claim 1, is characterized in that the volume ratio of described clean water and mud is 1:1.
5. the method for claim 1, is characterized in that the add-on of described dimethyl sulfoxide (DMSO) makes the volume fraction of dimethyl sulfoxide (DMSO) in the preservation system after finally adding mud be 4 ~ 5%.
6. the reactivation method of the anaerobic ammonium oxidation granular sludge after a preservation, the store method of described anaerobic ammonium oxidation granular sludge is: by the granule sludge of anaerobic ammonia oxidation reactor overproduction and/or go out sewage sludge collect, for needing the mud preserved, using the clean and organic plastics bottle of good leak tightness as preservation container, the sludge volume preserved is needed to be 1:2 ~ 4 with the volumetric ratio of preservation container, first in preservation container, add clean water and dimethyl sulfoxide (DMSO), the volume ratio of clean water and mud is 1:0.8 ~ 1.2, the add-on of dimethyl sulfoxide (DMSO) makes the volume fraction of dimethyl sulfoxide (DMSO) in the preservation system after finally adding mud be 2% ~ 10%, by be added with clean water and dimethyl sulfoxide (DMSO) preservation container closure after at 0 ~ 4 DEG C temp. keeping, liquid in container temperature is made to be 0 ~ 4 DEG C, take out and obtain the container after refrigerating, inorganic salt buffer solution for cleaning is first used 3 ~ 5 times by needing the mud preserved, mud after cleaning loads the container after refrigeration, after argon gas aeration 20 ~ 30min, encloses container, make to be in anoxic condition in encloses container, finally the encloses container that above-mentioned mud, water and dimethyl sulfoxide (DMSO) are housed is placed in the environment of 0 ~ 4 DEG C and preserves,
The component of described inorganic salt damping fluid is composed as follows: KH
2pO
45 ~ 20mgL
-1, CaCl
22H
2o 1 ~ 10mgL
-1, MgSO
42H
2o 200 ~ 400mgL
-1, KHCO
3800 ~ 1500mgL
-1;
It is characterized in that described reactivation method is: taken out by the preservation container depositing anaerobic ammonium oxidation granular sludge, carry out thermal adaptation operation, 2 ~ 4 thermogrades are on average chosen between storage temperature and default recovery temperature, heating in water bath is incubated, preserve container and be incubated adaptation 12 ~ 36h at each temperature, after thermal adaptation, take out the anaerobic ammonium oxidation granular sludge after preserving, by the inorganic salt buffer solution for cleaning 6 ~ 10 times with identical component in store method, mud after cleaning adds in anaerobic reactor to be launched and carries out activation recovering: the operational conditions of anaerobic reactor is: run at normal temperature or middle temperature 30 ~ 38 DEG C, hydraulic detention time is 2 ~ 6h, initial influent ammonia nitrogen and nitrite nitrogen concentration are respectively 42 ~ 98mgL
-1, increase water inlet substrate concn and shorten these two kinds of adjustable strategies of HRT and carry out respectively or intersect carrying out, until reactor total nitrogen removal efficiency reaches more than 85%, and can steady in a long-termly run.
7. method as claimed in claim 6, it is characterized in that described anaerobic reactor to be launched runs at normal temperatures, the operation steps of described thermal adaptation is: preserve container and first at 6 ~ 8 DEG C, adapt to 12 ~ 36h, at 12 ~ 14 DEG C, adapt to 12 ~ 36h again, finally at 18 ~ 22 DEG C, adapt to 12 ~ 36h.
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CN104085983A (en) * | 2014-06-13 | 2014-10-08 | 杭州师范大学 | Method for activating anaerobic ammonia oxidation sludge under low-temperature condition by using ultrasonic waves |
CN106635896B (en) * | 2016-12-01 | 2019-12-03 | 北京市环境保护科学研究院 | A method of industrialization anaerobic ammonia oxidizing bacteria being stored and utilizing again |
CN110902843B (en) * | 2018-09-18 | 2020-12-29 | 江南大学 | Method for determining optimal preservation temperature of anaerobic ammonia oxidation biomembrane for sewage treatment |
CN110129203B (en) * | 2019-04-23 | 2021-05-11 | 杭州师范大学 | Preservation and recovery method of anaerobic ammonium oxidation strain |
CN110407337B (en) * | 2019-08-08 | 2022-04-05 | 青岛思普润水处理股份有限公司 | MBBR-autotrophic denitrification-based suspension carrier water-containing preservation and activity recovery method |
CN110407336B (en) * | 2019-08-08 | 2022-04-08 | 青岛思普润水处理股份有限公司 | Wet storage and activity recovery method based on MBBR (moving bed biofilm reactor) autotrophic denitrification suspension carrier |
CN110759486A (en) * | 2019-09-18 | 2020-02-07 | 天津城建大学 | Method for quickly starting anaerobic ammonia oxidation in SBR reactor under low substrate concentration |
CN112678947B (en) * | 2019-10-17 | 2022-05-10 | 江南大学 | Method for determining optimum preservation temperature of anaerobic granular sludge |
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