CN109626577A - A kind of graphene oxide strengthened anaerobic ammoxidation particle and preparation method thereof - Google Patents
A kind of graphene oxide strengthened anaerobic ammoxidation particle and preparation method thereof Download PDFInfo
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- CN109626577A CN109626577A CN201910119449.2A CN201910119449A CN109626577A CN 109626577 A CN109626577 A CN 109626577A CN 201910119449 A CN201910119449 A CN 201910119449A CN 109626577 A CN109626577 A CN 109626577A
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- graphene oxide
- anaerobic
- particle
- oxidizing bacteria
- mixed liquor
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- 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
-
- 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
- C02F2003/003—Biological treatment of water, waste water, or sewage using granular carriers or supports for the microorganisms using activated carbon or the like
Abstract
The invention belongs to technical field of sewage, it is related to a kind of graphene oxide strengthened anaerobic ammoxidation particle and preparation method thereof, powdered graphene oxide is uniformly mixed with the liquid containing anaerobic ammonia oxidizing bacteria, make anaerobic ammonia oxidizing bacteria be oxidized graphene powder to be adsorbed, form the graphene oxide molecule containing anaerobic ammonia oxidizing bacteria, then Waterborne Polyurethane Prepolymer mixing is added into mixed solution, it adds polymerization initiator and carries out polymerization reaction, it is set to be frozen into the ester shape hydrosol, then machine cuts are carried out again obtains graphene oxide strengthened anaerobic ammoxidation particle, its manufacture craft is simple, it is easy to operate, it is cheap, the embedded immobilization anaerobic ammonium oxidation granular specificity of production is high, stability is good, it is suitble to industrialized production, desirable good economic and environmental benefit.
Description
Technical field:
The invention belongs to technical field of sewage, it is related to a kind of graphene oxide strengthened anaerobic ammoxidation particle and its system
Preparation Method.
Background technique:
In recent years, a kind of effective side is increasingly regarded as using anaerobic ammonia oxidation processing nitrogen-containing wastewater
Method.In this course, ammonium oxidation is nitrogen using nitrite as electron acceptor by anaerobic ammonia oxidizing bacteria.It is taken off with traditional
Nitrogen system is compared, and Anaerobic ammonium oxidation system has oxygen demand few, does not need additional organic carbon source, the surplus sludge volume of generation is few
Advantage, these all greatly reduce operating cost.But since the following four characteristic of anaerobic ammonia oxidizing bacteria makes in a reality
Maintain sufficient amount of anaerobic ammonium oxidation sludge extremely difficult in the reactor of border operation: first is that anaerobic ammonia oxidizing bacteria belongs to autotrophy
Type microorganism, rate of rise are very slow；Second is that the biomass of anaerobic ammonia oxidizing bacteria is low in reactor, this detests starting one
Anaerobic ammonium oxidation reactor is very slow, generally requires three months or more time；Third is that being generated in anaerobic ammonia oxidation reactor big
The nitrogen of amount can make microbial suspension in reactor, being easy to be lost biomass with water flow；Fourth is that nitrogenous organic when handling
When waste water, the presence of organic matter can promote the growth of heterotroph, and the anaerobic ammonia oxidizing bacteria of autotrophic type is in due to slow growth
Disadvantage in competition is easy to be eliminated.Therefore it is active and anti-to improve anaerobic ammonia oxidizing bacteria for the application for anaerobic ammonia oxidation process
Only thallus loss is crucial.
Graphene oxide (Graphene oxide, GO) is a kind of new carbon haveing excellent performance, and is graphite
(Graphite) product of the powder after strong acid aoxidizes and removes, research shows that GO has biggish specific surface area, good glue
Bulk properties, surface have oxygen-containing functional group abundant (such as carboxyl, hydroxyl, alkoxy) and low cytotoxicity, and have preferable
Biocompatibility can be used to promote microbial activity due to these characteristics of graphene oxide.Such as document is " no
The comparison of low abundance Anammox flora with reinforced by additive " is to derive from integral part nitrosation-anaerobic ammoxidation sequence
The activated sludge of batch reactor technique compares Fe2 by anaerobism batch test for object+, graphene oxide, Fe3+After adding
Influence to the denitrification effect of anaerobic ammonia oxidizing bacteria, activity, key function gene dosage, community structure and function abundance, experiment
The result shows that it is best to the promotion effect of microbial metabolism function to add graphene oxide；Document " Anammox reinforcement technique
Progress " from the enrichment of Anammox bacterium (including accelerate granulating, using biomembrane, using membrane bioreactor etc.), add
Add chemical substance (manganese dioxide, graphene oxide, iron ion, Anammox intermediate product etc.), apply physical field (ultrasonic wave, magnetic
Field, electric field etc.) and biological reinforced and strain stream add etc., describe at present both at home and abroad about Anammox process strengthening
Progress analyzes technical essential, has parsed strengthening mechanism, finally points out that following research direction should concentrate on and strengthens parameter
Optimization, the different comprehensive function for strengthening strategy, the long term effect of reinforcing and to the side such as further investigation of strengthening mechanism
Face.
Free anaerobic ammonia oxidizing bacteria is fixed on carrier by microorganism embedded immobilization technology by chemically or physically means,
It can effectively overcome the problems, such as that biomass is lost, but the occlusion vehicle of existing embedded immobilization technology production, as alginate embeds
That there are still mass-transfer performances is poor for carrier, sodium carboxymethylcellulose occlusion vehicle, polyvinyl alcohol embedding carrier etc., after influencing immobilization
The bioactivity and longtime running stability of anaerobic ammonia oxidizing bacteria are poor, breakable problem.
Summary of the invention:
It is an object of the invention to overcome disadvantage of the existing technology, existing microorganism embedded immobilization technology is solved
Deficiency, design provides a kind of graphene oxide strengthened anaerobic ammoxidation particle and preparation method thereof, for improving anaerobic ammoniation bacterium
Activity.
To achieve the goals above, graphene oxide strengthened anaerobic ammoxidation particle of the present invention is by containing graphite oxide
The mixture of alkene and anaerobic ammonia oxidizing bacteria is made by the Polyurethane carrier embedding fixation with duct, wherein the matter of graphene oxide
Amount concentration is 0.1%-0.5%, the biological denitrificaion for waste water.
When graphene oxide strengthened anaerobic ammoxidation particle preparation of the present invention, by powdered graphene oxide with contain
There is the liquid of anaerobic ammonia oxidizing bacteria uniformly to mix, so that anaerobic ammonia oxidizing bacteria is oxidized graphene powder and adsorbed, is formed to contain and be detested
Then the graphene oxide molecule of anaerobic ammonium oxidation bacterium Waterborne Polyurethane Prepolymer is added into mixed solution and mixes, then plus
Enter polymerization initiator and carry out polymerization reaction, so that it is frozen into the ester shape hydrosol, then carry out machine cuts again, specifically include following
Step:
(1) being deployed into mixed liquor volatile suspended solid, MLVSS concentration (MLVSS) with anaerobic ammonium oxidation sludge and tap water is
The mixed liquor A of 2500-10000mg/L；
(2) graphene oxide powder of gross mass 0.1%~0.5% is added in solution A, and is mixed
Liquid B；
(3) Waterborne Polyurethane Prepolymer of gross mass 10-15% is added in mixed liquid B, and is mixed
Liquid C；
(4) initiator potassium persulfate (KPS) of gross mass 1-2% and urging for 0.2-0.5% are successively added into mixed liquor C
Agent tetramethylethylenediamine (TEMED), and stir evenly, mixed liquor D is made；
(5) after mixed liquor D standing being obtained water-soluble gelled solids in 5-30 minutes, water-soluble gelled solids, which are cut into side length, is
Graphene oxide strengthened anaerobic ammoxidation particle is prepared in the cubic granules of 2-8mm.
The additive amount of graphene oxide powder of the present invention has an important influence the performance of embedded particles obtained, GO
Amount it is too low, cannot play the role of effective strengthened anaerobic ammoxidation bacterium activity and reinforce embedded particles intensity；The amount of GO is excessively high,
The duct inside embedded particles can be blocked, mass-transfer performance is reduced, influences nitrogen removal performance, while excessively high GO can be to anaerobism ammonia oxygen
Change bacterium and generate bio-toxicity, GO concentration control in embedding medium aqueous solution is not only played into support embedded particles in 0.1%-0.5%
Inner space skeleton, enhances the effect of mechanical performance, while making more loose inside embedded particles, increases the mass transfer of embedded particles
Property, strengthen Anammox performance.
Graphene oxide of the present invention be any graphene oxide pure powder of analysis with graphene oxide characteristic or
The pure powder of chemistry, or prepare as follows:
(1) it pre-oxidizes: taking 5 grams of high-grade pure graphite powders that the burning for being placed with the concentrated sulfuric acid () of 500 milliliters of mass concentrations 98% is added
In cup, mechanical stirring obtains mixed liquor A for 24 hours；
(2) it aoxidizes: the beaker equipped with mixed liquor A being moved in 4 DEG C of ice-water baths below, then by 25 grams of potassium permanganate
(KMnO4) it is slowly added in beaker, mechanical stirring moves back ice-water bath for 24 hours, and holding chamber middle benefit gas is slow added into 500 milliliters and goes
After ionized water, mechanical stirring obtains mixed liquid B for 24 hours；Then saturation hydrogenperoxide steam generator is slowly added in mixed liquid B, until mixed
It closes liquid color and becomes golden yellow, and without stirring 5h after color change in 1min；
(3) washing precipitating: will fill water, staticly settle in beaker, when upper solution and following precipitating have bright bed boundary,
Outwell supernatant, and according to volume ratio concentrated hydrochloric acid: deionized water=1:9 ratio prepares dilute hydrochloric acid solution 1000ml, with dilute salt
Acid solution in three times washes graphite oxide solution, obtains sediment；
(4) it is centrifuged: taking 50ml centrifuge tube, sediment made from step (3) is fitted into centrifuge tube in 4000r/min condition
Lower centrifugation 15min obtains sediment；
(5) it dialyses: the sediment after centrifugation being fitted into dialyse 3 days in bag filter obtains graphene oxide solution；
(6) be freeze-dried: graphene oxide solution is fitted into culture dish, be first put into household freezer freeze it is blocking,
It puts it into freeze drier be freeze-dried two days again and obtains the cotton-shaped graphene oxide of brown color.
Compared to the prior art the present invention, has the following advantages that and effect: first is that effectively improving anaerobic ammonia oxidizing bacteria activity:
GO is mixed with anaerobic ammonia oxidizing bacteria, is fabricated to embedded particles, can improve more attachment sites for anaerobic ammonia oxidizing bacteria, effectively
The increase of anaerobic ammonia oxidizing bacteria extracellular polymeric (EPS) is stimulated, and then improves anaerobic ammonia oxidizing bacteria activity, experiments have shown that addition GO
Embedded particles its anaerobic ammonia oxidizing bacteria activity increases about 10.26%；Second is that the embedding after aqueous energy polyurethane material immobilization
Particle high mechanical strength, swelling behavior are good: the mixed solution of GO and anaerobic ammonia oxidizing bacteria being made up of aqueous polyurethane water-soluble
Glue is cut into the cubic block particle of 2-8mm, and gained particle has good mechanical strength and swelling behavior, in long-term operation
Cash out good physicochemical stability；Third is that the manufacture craft of entire embedded immobilization process is simple, easy to operate, low cost
Honest and clean, the embedded immobilization anaerobic ammonium oxidation granular specificity of production is high, and stability is good, is suitble to industrialized production, desirable is good
Economic and environmental benefit.
Detailed description of the invention:
Fig. 1 is the picture of graphene oxide strengthened anaerobic ammoxidation particle of the present invention.
Fig. 2 is graphene oxide strengthened anaerobic ammoxidation particle inner scanning electromicroscopic photograph of the present invention, wherein 1 is to detest
Anaerobic ammonium oxidation bacterium, 2 be graphene oxide.
Specific embodiment:
The invention will be further described by way of example and in conjunction with the accompanying drawings.
Embodiment 1:
The liquid containing anaerobic ammonia oxidizing bacteria that the present embodiment is modulated by powdered graphene oxide and with tap water
(concentration is 5000mg/L (MLVSS)) is uniformly mixed to get mixed liquor, so that anaerobic ammonia oxidizing bacteria is oxidized graphene powder and is inhaled
It is attached, molecule is formed, by mass percentage, graphene oxide accounts for 0.3% in mixed liquor, adds 10% aqueous poly- ammonia
Then the mixing of ester performed polymer is added 1%KPS and 0.2%TEMED respectively as initiator and catalyst and carries out polymerization reaction, makes
It is frozen into the ester shape hydrosol, finally carries out machine cuts, and the cube embedded particles that side length is 5mm are made.
Cube embedded particles obtained are handled nitrogenous effluent by the present embodiment under continuous condition of culture, and detailed process is such as
Under:
(1) target waste water is added in cube embedded particles obtained, is cultivated one week in 32 DEG C of isothermal vibration incubators,
Restore the activity of anaerobic ammonia oxidizing bacteria in embedded particles, the volume ratio of embedded particles and target waste water is 2:8 in activation process, with
Ammonia nitrogen is reduced to the 10% of initial concentration as an activity cycle, after each activity cycle, changes water, and it is useless to inject fresh target
Water, the embedded particles after being activated；
(2) embedded particles after above-mentioned activation are added in ASBR reactor by reactor volume filling rate 20%, instead
Answer device dischargeable capacity 10L, the reaction time is 40 hours, the sedimentation time 10 minutes, ammonia nitrogen and nitrite nitrogen initial concentration in waste water
Respectively 100mg/L and 120mg/L, the monitoring result of water outlet are as follows: ammonia nitrogen NH3- N concentration is 1.7mg/L, and removal rate reaches
98.3%, nitrite nitrogen NO2- N concentration is 1.83mg/L, and removal rate reaches 98.5%, and COD CODcr removal rate reaches
87%, illustrate that the embedded particles of preparation have extraordinary application prospect.
Embodiment 2:
The liquid containing anaerobic ammonia oxidizing bacteria that the present embodiment is modulated by powdered graphene oxide and with tap water
(concentration is 8000mg/L (MLVSS)) uniformly mixing, adsorbs anaerobic ammonia oxidizing bacteria by GO powder, forms molecule, press
Mass percent, GO accounts for 5% in mixed liquor, adds 15% Waterborne Polyurethane Prepolymer mixing, 2%KPS is then added
Polymerization reaction is carried out as initiator and catalyst with 0.5%TEMED, it is made to be frozen into the ester shape hydrosol, is finally carried out mechanical
The cube embedded particles that side length is 5mm are made in cutting.
Cube embedded particles obtained are handled nitrogenous effluent by the present embodiment under continuous condition of culture, and detailed process is such as
Under:
(1) embedded particles obtained are taken, target waste water is added, is cultivated 7 days in 32 DEG C of isothermal vibration incubators, restore packet
The activity of anaerobic ammonia oxidizing bacteria in particle is buried, activation method is same as Example 1；
(2) embedded particles after above-mentioned activation are added in UASB reactor by reactor volume filling rate 10% and are carried out
Continuous culture, reactor dischargeable capacity 20L, hydraulic detention time 8 hours, ammonia nitrogen loading and nitrite load point in waste water
It Wei not 0.43kg/m3And 0.21kg/m .d3.d, the monitoring result of water outlet is shown: ammonia nitrogen removal frank reaches 95.2%, nitrite
Nitrogen NO2- N removal rate reaches 96%, and COD CODcr removal rate reaches 88.5%, and embedded particles show good de-
Nitrogen performance.
Claims (3)
1. a kind of graphene oxide strengthened anaerobic ammoxidation particle, it is characterised in that by containing graphene oxide and Anammox
The mixture of bacterium is made by the Polyurethane carrier embedding fixation with duct, and wherein the mass concentration of graphene oxide is 0.1%-
0.5%, it can be used in the biological denitrificaion of waste water.
2. a kind of preparation method of graphene oxide strengthened anaerobic ammoxidation particle as described in claim 1, it is characterised in that will
Powdered graphene oxide is uniformly mixed with the liquid containing anaerobic ammonia oxidizing bacteria, and anaerobic ammonia oxidizing bacteria is made to be oxidized graphene
Powder is adsorbed, and is formed the graphene oxide molecule containing anaerobic ammonia oxidizing bacteria, is then added into mixed solution aqueous
Base polyurethane prepolymer for use as mixing adds polymerization initiator and carries out polymerization reaction, so that it is frozen into the ester shape hydrosol, then carry out again
Machine cuts, specifically includes the following steps:
(1) being deployed into mixed liquor volatile suspended solid, MLVSS concentration with anaerobic ammonium oxidation sludge and tap water is 2500-10000mg/L
Mixed liquor A；
(2) graphene oxide powder of gross mass 0.1%~0.5% is added in solution A, and is uniformly mixed and obtains mixed liquid B；
(3) Waterborne Polyurethane Prepolymer of gross mass 10-15% is added in mixed liquid B, and is uniformly mixed and obtains mixed liquor C；
(4) initiator potassium persulfate of gross mass 1-2% and the catalyst tetramethyl of 0.2-0.5% are successively added into mixed liquor C
Base ethylenediamine, and stir evenly, mixed liquor D is made；
(5) after mixed liquor D standing being obtained water-soluble gelled solids in 5-30 minutes, it is 2- that water-soluble gelled solids, which are cut into side length,
Graphene oxide strengthened anaerobic ammoxidation particle is prepared in the cubic granules of 8mm.
3. the preparation method of graphene oxide strengthened anaerobic ammoxidation particle according to claim 1, it is characterised in that described
Graphene oxide is that any graphene oxide with graphene oxide characteristic analyzes pure powder or the pure powder of chemistry, or presses as follows
Step preparation:
(1) it pre-oxidizes: 5 grams of high-grade pure graphite powders being taken to be added in the beaker for the concentrated sulfuric acid () for being placed with 500 milliliters of mass concentrations 98%,
Mechanical stirring obtains mixed liquor A for 24 hours；
(2) it aoxidizes: the beaker equipped with mixed liquor A being moved in 4 DEG C of ice-water baths below, is then slowly added 25 grams of potassium permanganate
Enter in beaker, mechanical stirring moves back ice-water bath for 24 hours, and holding chamber middle benefit gas is mechanical after being slow added into 500 ml deionized waters
Stirring obtains mixed liquid B for 24 hours；Then saturation hydrogenperoxide steam generator is slowly added in mixed liquid B, until mixed liquor color becomes gold
Yellow, and without stirring 5h after color change in 1min；
(3) washing precipitating: will fill water, staticly settle in beaker, when upper solution and following precipitating have bright bed boundary, outwell
Supernatant, and according to volume ratio concentrated hydrochloric acid: deionized water=1:9 ratio prepares dilute hydrochloric acid solution 1000ml, molten with dilute hydrochloric acid
Liquid in three times washes graphite oxide solution, obtains sediment；
(4) be centrifuged: take 50ml centrifuge tube, by sediment made from step (3) be fitted into centrifuge tube under the conditions of 4000r/min from
Heart 15min obtains sediment；
(5) it dialyses: the sediment after centrifugation being fitted into dialyse 3 days in bag filter obtains graphene oxide solution；
(6) be freeze-dried: graphene oxide solution is fitted into culture dish, be first put into household freezer freeze it is blocking, then general
It, which is put into freeze drier be freeze-dried two days, obtains the cotton-shaped graphene oxide of brown color.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111137985A (en) * | 2020-01-08 | 2020-05-12 | 西南科技大学 | Preparation method of microbial degradation material for treating ammonia nitrogen in sewage |
| CN114307880A (en) * | 2022-01-05 | 2022-04-12 | 深圳职业技术学院 | Preparation method of graphene carrier and reactor based on graphene carrier |
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| CN103898085A (en) * | 2014-03-26 | 2014-07-02 | 北京工业大学 | Diatomite adsorption anaerobic ammonium oxidation bacteria particles and preparation method thereof |
| KR20140103205A (en) * | 2013-02-14 | 2014-08-26 | 한국기계연구원 | Graphene-tio2 composite, and the preparation method thereof |
| CN108342099A (en) * | 2018-02-08 | 2018-07-31 | 青岛大学 | A kind of method of surface of graphene oxide chemical modification and application |
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2019
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| KR20140103205A (en) * | 2013-02-14 | 2014-08-26 | 한국기계연구원 | Graphene-tio2 composite, and the preparation method thereof |
| CN103898085A (en) * | 2014-03-26 | 2014-07-02 | 北京工业大学 | Diatomite adsorption anaerobic ammonium oxidation bacteria particles and preparation method thereof |
| CN108342099A (en) * | 2018-02-08 | 2018-07-31 | 青岛大学 | A kind of method of surface of graphene oxide chemical modification and application |
Non-Patent Citations (1)
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| DONG WANG ET AL: "Using graphene oxide to enhance the activity of anammox bacteria for nitrogen removal", 《BIORESOURCE TECHNOLOGY》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111137985A (en) * | 2020-01-08 | 2020-05-12 | 西南科技大学 | Preparation method of microbial degradation material for treating ammonia nitrogen in sewage |
| CN114307880A (en) * | 2022-01-05 | 2022-04-12 | 深圳职业技术学院 | Preparation method of graphene carrier and reactor based on graphene carrier |
| CN114307880B (en) * | 2022-01-05 | 2023-03-28 | 深圳职业技术学院 | Preparation method of graphene carrier and reactor based on graphene carrier |
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