CN106865936A - A kind of method for releasing ammonia suppression in feces of livestock and poultry anaerobic fermentation process - Google Patents
A kind of method for releasing ammonia suppression in feces of livestock and poultry anaerobic fermentation process Download PDFInfo
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- CN106865936A CN106865936A CN201710084388.1A CN201710084388A CN106865936A CN 106865936 A CN106865936 A CN 106865936A CN 201710084388 A CN201710084388 A CN 201710084388A CN 106865936 A CN106865936 A CN 106865936A
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- ammonia
- anaerobic fermentation
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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
- C02F11/00—Treatment of sludge; Devices therefor
- C02F11/02—Biological treatment
- C02F11/04—Anaerobic treatment; Production of methane by such processes
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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
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/20—Nature of the water, waste water, sewage or sludge to be treated from animal husbandry
Abstract
The invention provides a kind of method for releasing ammonia suppression in feces of livestock and poultry anaerobic fermentation process.The present invention utilizes struvite crystallization sedimentation, and in pH value 79, volatile fatty acid is less than in the case of 0.4 with the mass concentration ratio of TIC, NH in detection ammonia inhibition system4 +Concentration, by magnesium salts and microcosmic salt according to NH4 +：Mg2+:PO4 3‑The mol ratio of three is 1:1:1 is added in livestock manure fermented reaction system, the concentration value or so when making the concentration of ammonia nitrogen be reduced to the fermentation process that ammonia suppression does not occur.The present invention sets up the method for releasing ammonia suppression in feces of livestock and poultry anaerobic fermentation process by studying influence factor of the ammonium magnesium phosphate reaction in the interior environment of anaerobic fermentation tank and reacting itself limiting factor.Present invention process is simple, and the guanite precipitation of reaction generation is a kind of slow-release fertilizer, and can not only release ammonia inhibition can also reclaim the nutrients such as nitrogen phosphorus, so as to reduce operating cost.
Description
Technical field
The present invention relates to agricultural wastes recycling field, and in particular to a kind of to react what is carried out based on ammonium magnesium phosphate
The ammonia occurred in feces of livestock and poultry anaerobic fermentation process suppresses release method.
Background technology
With gradually improving and economic fast development for modern farming enterprise's industrial system, the mode of production of animal husbandry has been sent out
Raw great change, progressively from decentralized, it is extensive change to scale, intensive management, Amount of poultry excrements is therewith drastically
The environmental problem for increasing and producing becomes increasingly conspicuous.Producing methane through anaerobic fermentation technology possesses the environment dirt of control feces of livestock and poultry due to it
The dual-use function of dye and the alleviation growing demand pressure of rural energy, by common concern and soon in the range of world in recent years
Speed development.As the quickening of China's the Course of Urbanization and rural culture pattern are gradually raised scattered to intensive from original peasant household
Change cultivation transformation, country has put into effect a series of construction that policies increase the big-and-middle-sized biogas engineering of livestock and poultry farms in scale.Cut-off
Since the first half of the year in 2013, China rural area is completed 13,000,000 6-10m3The meeting of specification methane-generating pit, produces the m of biogas 300,000,000 per year3, greatly
About 1,000,000 people in the countryside have used biogas.
Scale biogas engineering is that substantial amounts of bioenergy is brought in plant and villages and small towns, increased economy and Environmental Effect
Benefit.But because China's biogas engineering generally uses single raw material, such as feces of livestock and poultry.Animal wastes have C/N relatively low, and N high contains
The characteristic of amount, in addition frequently with the operator scheme of biogas slurry backflow in production practices, with the carrying out that anaerobic digestion is reacted, ammonia exists
Constantly accumulated in digestive juice, the ammonia nitrogen in high density for gradually forming will have a strong impact on the activity of methanogen, so as to reduce reactor
Gas producing efficiency, or even ultimately result in fermentation process failure.Thus, control and releasing for ammonia suppression are that feces of livestock and poultry is detested
Oxygen digests the hot issue in field.
At present, ammonia suppresses release method, mainly there is following several：One is to change ambient parameter, by pH, carbon-nitrogen ratio etc.
The regulation of factor is completed；Two be domestication methanogen population, fixed by filler, element addition etc. mode strengthen microorganism pair
The tolerance of ammonia nitrogen in high density, so that anaerobic digestion can be carried out in the case where ammonia nitrogen concentration is higher.3rd, physical chemistry side
Method such as dilutes, stripping, chemical precipitation.(i.e. ammonium magnesium phosphate reacts struvite crystallization sedimentation, and the chemical name of guanite is
Ammonium magnesium phosphate, chemical formula is MgNH4PO4·6H2O reaction equations：Mg2++NH4 ++PO4 3-=MgNH4PO4·6H2O) have reaction former
Reason is simple, the reaction time is short, speed is fast, ammonia nitrogen removal frank is high, the features such as be affected by the external environment small, while can also realize to ammonia
Effective recovery of nitrogen.At present, this technology is mainly used in the industrial high ammonia-nitrogen wastewater for the treatment of and the nutrient of nitrogen phosphorus is recycled, anti-
Answering carries out treatment biogas slurry outside tank, need to only consider how to increase organic efficiency, but suppress for the ammonia during anaerobic reaction
Releasing need to consider the influence to reaction system stability such as the pH changes of retort, foreign ion addition, while to ensure anaerobism
The normal even running of engineering, will realize that accurately regulating and controlling and release the ammonia in fermentation process suppresses to remain in technical difficulty.
The content of the invention
In order to solve problems of the prior art, the purpose of the present invention is set up a kind of based on ammonium magnesium phosphate reaction
Simply, the ammonia that ammonia minimizing technology quickly, suitable is used in feces of livestock and poultry anaerobic fermentation process suppresses to release.
The main chemical reactions that the principle of the invention is formed according to magnesium ammonium phosphate sediment, by magnesium salts and phosphorus by contrasting selection
Salt is added in reactor, makes itself and NH4 +React, the equilibrium relation further according to ammonia nitrogen in anaerobic fermented liquid, by it certainly
By ammonia density reduction, so as to quickly realize releasing the purpose that ammonia suppresses.The present invention probes into ammonium magnesium phosphate reaction (MAP reactions) and exists
Influence factor and itself limiting factor of reaction in the interior environment of anaerobic fermentation tank.By these factors, a set of being applied to is set up
The method that ammonia suppresses is released in feces of livestock and poultry anaerobic fermentation.
In order to realize the object of the invention, technical scheme is comprised the following steps：
(1) when obvious ammonia suppression is formed in feces of livestock and poultry anaerobic fermentation system, the pH value of anaerobic fermentation system is adjusted
And the mass concentration ratio that VFA/TIC, the VFA/TIC are volatile fatty acid and TIC；
(2) to magnesium salts and phosphate is added in reaction system, while adjusting pH value to maintain fermentation system normally to run.
In the above method, the pH value of the regulation anaerobic fermentation system described in step (1) is ＞ 7.
Preferably, the pH value of the regulation anaerobic fermentation system described in step (1) is 7-8.
Step (1) the VFA/TIC ＜ 0.4.
Step (2) is a small amount of repeatedly to add magnesium salts and phosphate, prevents disposably to add the magnesium salts and phosphate of aim parameter.This
The magnesium salts that inventive embodiment is used is MgCl2·6H2O, phosphate is Na2HPO4·12H2O or K2HPO4·12H2O。
In the above method, magnesium salts and phosphate that step (2) is added every time make NH4 +：Mg2+：PO43-Mol ratio be 1：
1：1.The NH4 +It is the NH for intending eliminating in fermentation system4 +
PH value is ＞ 7 in step (2).
NH in monitoring system at any time in step (2)4+Concentration, wait be down to not occur ammonia suppress when NH4+Concentration, stops adding
Enter magnesium salts and phosphate.
The invention provides application of the above method in feces of livestock and poultry anaerobic fermentation.
The invention provides application of the above method in bio anaerobic fermentation.
Compared with prior art, the beneficial effects of the present invention are：The present invention suppresses releasing technology for other ammonia may
There is the problems such as time-consuming, hardly possible is manipulated, quantity of alkali consumption is big, devise a kind of feces of livestock and poultry carried out based on ammonium magnesium phosphate reaction
Anaerobic fermentation ammonia suppress release method using batch test carry out reaction condition influence probe into draw it is organic in pH, temperature, tank
Acid concentration, influence of the initial ammonia nitrogen concentration to MAP reaction efficiencies in the experiment of semicontinuous anaerobic fermentation so that better profit from MAP
Method carries out releasing ammonia suppression.Because MAP reactions are interionic chemical precipitation reactions, it is swift in response, can reach quickly except ammonia
Effect.Alkaline reagent can be selected in terms of reagent selection greatly for blow-off method quantity of alkali consumption reduces the effect of alkali consumption so as to reach
Really.Electric power energy consumption aspect is also relatively fewer.Experiment manipulation aspect, can draw Suitable agents addition according to experimental result,
Quantitative removal is carried out, it is convenient and swift.
The present invention simulates interior boundary and the external environment and every physico of anaerobic fermentation reaction system by batch test
Index is learned, specify that MAP reactions have the preferable removal effect highest can in the case of the initial ammonia nitrogen concentration of pH9,930mg/L
Reach more than 80% ammonia nitrogen removal frank, and acetic acid in VFAs also can be to right because of its decomposition to struvite crystals
MAP reactions have certain influence, and temperature factor has no considerable influence to this reaction.For it is carried out in semicontinuous anaerobic fermentation process
There is provided foundation.Tested by semicontinuous anaerobic fermentation, each influence factor dynamic change situation in further confirmatory reaction device inside
Lower MAP reacts the releasing effect to ammonia inhibition, with reference to batch test result, it is considered to which influence factor influence carries out MAP reactions, right
This method is further optimized.Result proves that experiment can obtain regulatable ammonia nitrogen removal frank according to the difference of salt adding amount,
Reach as high as 80%.Operating procedure of the present invention is simple and MAP reacts the guanite precipitation for generating, and is a kind of slow-release fertilizer, not only may be used
Releasing ammonia inhibition can also reclaim the nutrients such as nitrogen phosphorus, so as to reduce operating cost.
Brief description of the drawings
Fig. 1 is the ammonia nitrogen removal frank of difference pH under the medium temperature condition of embodiment 1.
Fig. 2 is the ammonia nitrogen removal frank of difference pH under the hot conditions of embodiment 1.
Fig. 3 A be embodiment 1 in pH=7.5 when, the ammonia nitrogen removal frank under the conditions of different sodium acetate concentrations.Fig. 3 B are implementation
In example 1 during pH=8, the ammonia nitrogen removal frank under the conditions of different sodium acetate concentrations.
Fig. 4 is the ammonia nitrogen removal frank figure of different initial ammonia nitrogen concentrations.
The graph of a relation that Fig. 5 is changed over time for the middle temperature day methane production of embodiment 2 with ammonia nitrogen concentration change.
The graph of a relation that Fig. 6 is changed over time for the day with high temperature methane production of embodiment 2 with ammonia nitrogen concentration change.
Specific embodiment
The preferred embodiment of the present invention is described in detail below in conjunction with embodiment.It will be appreciated that following real
Being given merely to play descriptive purpose for example is applied, is not used to limit the scope of the present invention.The skill of this area
Art personnel can carry out various modifications and replacement in the case of without departing substantially from spirit of the invention and spirit to the present invention.
The experimental technique used in embodiment, if without specified otherwise, being conventional method.Material used in embodiment,
Reagent etc., if without specified otherwise, commercially obtaining.
Pig manure in the present embodiment is the pig manure after being dried purchased from pig peasant household of Fujian Province, using preceding dry by what is bought
Pig manure pulverizer crushes powdered, standby；Seed sludge takes from In Shunyi District of Beijing east Huashan methane station normal table fortune
Capable biogas engineering fermentation pool bottom sludge.
The detection method of the various parameters in embodiment is as follows：Gas production：Determined using row's saturated common salt water law, instrument is
Wet gas flow meter.Gas componant：Biogas analytical instrument Biogas5000 is determined.PH value, electrical conductivity：Joining using SG23 more
Number tester is determined.Ammonia nitrogen (NH4 +- N) concentration：Salicylic acid-hypochlorite photometry (UV-1000 ultraviolet specrophotometers).Wave
Hair property aliphatic acid (Volatile fatty acids, VFA) and TIC (Total inorganic carbon, TIC) are dense
Degree：Titration (ZDJ-5 thunder magnetic titrator).Amount of dry matter (Total solid, TS)：Determined using weight method, sample is placed on
Dried to constant weight in the baking oven of (105 ± 5) DEG C, then claim its quality.Volatile solid (Volatile solid, VS) is determined：It is dry
Material after dry 24h is put into Muffle furnace, the calcination 2h under 550 DEG C of high temperature, and quality is claimed after being put into drier cooling.Guanite is precipitated
Quantitative analysis：X-ray powder diffraction instrument is determined.
The batch-type of embodiment 1 is tested
Raw material is taken respectively from the fermentation pig manure of stable operation 200 days, and fermentation method is conventional method.Middle temperature R1 (37 DEG C) and
High temperature R2 (55 DEG C) CSTR reactors, are tested in 37,55 DEG C of shaking bath.It is front and rear to have carried out temperature, pH, organic acid
And initial 4 kinds of factors of ammonia nitrogen concentration are studied for the influence of MAP reaction removal ammonia nitrogen efficiency.Test specific disposition such as table
Shown in 1, following 4 conditions influences are probed into experiment, and VS is in the range of 65%~70% in total mixture.
14 condition influence factor inquiry experiments of table are set
Specific implementation：(as a example by inquiring into temperature variable and react influence in anaerobic fermented liquid to MAP) take 9ml biogas slurries in
In centrifuge tube, centrifugation (10min, 8000r/min) takes ammonia nitrogen concentration, PO during supernatant determines biogas slurry4 3-Concentration and Mg2+Concentration,
The biogas slurry that period will preserve is mixed, and is dispensed enter in Erlenmeyer flask, every bottle of 100ml.According to NH4 +：Mg2+:PO4 3-=1:1:1
Ratio is calculated and adds MgCl2·6H2O and Na2HPO4·12H2O is measured, and timing is started during addition.One is taken every 1,3,5,7 hours
Secondary sample (biogas slurry after 3ml mixings) determines ammonia nitrogen concentration in the same way, and pH, PO are determined simultaneously when last time is sampled4 3-Concentration and
Mg2+Concentration, records post analysis processing data.Its dependent variable experimentation is same as described above, wherein probe into pH reacting MAP
In influence experiment in anaerobic fermented liquid, MgCl is being added2·6H2O and Na2HPO4·12H20.5mol/L HCl are used before O
Or 0.5mol/L NaOH regulations pH.
Experimental result is as follows：
(1) pH carries out the influence of ammonia nitrogen removal to MAP reactions：It will be seen from figure 1 that in middle temperature (37 DEG C) and high temperature (55
DEG C) in the case of two kinds, the ammonia nitrogen removal frank highest all in pH 9 reaches 60%-70%.PH in 7.0-7.5, ammonia nitrogen removal frank
Reach 45%-55%.
(2) temperature carries out the influence of ammonia nitrogen removal to MAP reactions：Show that temperature has no to MAP reactions by Fig. 1 and Fig. 2 bright
Development rings.
(3) influence of the organic acid to MAP reaction efficiencies：Different organic acids concentration is reacted MAP at two kinds at a temperature of
Do not make significant difference.See Fig. 3 A and Fig. 3 B.
(4) initial influence of the ammonia nitrogen concentration to MAP reaction efficiencies：All it is as seen from Figure 4 just under conditions of pH7-9
Beginning ammonia nitrogen concentration is higher, and ammonia nitrogen removal frank is bigger.
The semicontinuous anaerobic fermentation of embodiment 2 is tested
Take and crush standby pig manure, anaerobic fermentation 350 days, the first stage is startup stage, and R1, R2 are from OLR
1g.VS/L.d, 37 DEG C of startup optimizations.Just pyroreaction tank is heated up after being stablized according to the index observing such as aerogenesis, pH reactor
(37-55 DEG C) is while increasing productivity
(1-3g.vs/L.d).It is raised to after target temperature and load and reactor stabilization a period of time
(0-183 days) start plus ammonium salt (NH4Cl), make total ammonia nitrogen (TAN) concentration for 1000,2000,3000,4000mg/L
Until obvious ammonia occur suppressing.Index such as pH, VFA/TIC, methane production, biogas composition etc. are surveyed in observation decline or obvious
Change, adds magnesium salts (Mg2Cl·6H2O), microcosmic salt (Na2HPO4·12H2O、K2HPO4·12H2O MAP reactions) are carried out ammonia nitrogen is dense
Degree is released and arrives 1000mg/L or so, is released ammonia and is suppressed.As shown in Figure 5, at 182 days afterwards, the NH of artificial addition4 +Make TAN concentration
Rise, and day methane production is also from 7.5L CH4d- 1It is down to 6L CH4d- 1The scope of left and right, when TAN concentration rises to 5000mg L-1
When, there is the phenomenon that pH declines, day methane production is also gradually reduced because that can not bear in reactor.Carried out at the 301st day immediately
MAP reacts.After MAP reactions are carried out, ammonia nitrogen concentration is substantially reduced, while methane production gos up.Fig. 6 situations are similar to, but high
Warm fermentation tank is stablized relatively, and two secondary undulations only occur when being maintained at 1000mg/L after adding ammonium salt at 183 days.Lifting TAN's
During be down to 4.6L CH again from 6.4 to 5.44d- 1, retort occurs same existing after carrying out the reaction of first time MAP at 301 days
As.But it is noted that after first time MAP reactions (the 345th day), although TAN concentration declines but methane production is down to 0L therewith
CH4d- 1, pH is also down to 6 or so, has been not suitable for anaerobic fermentation reaction.But second situation is stablized relatively, with also along with product first
The decline of alkane amount and pH, but all in the buffering controlled range of anaerobic fermentation, again can be extensive through the buffer system adjustment in its system
It is multiple normal.
MAP precipitation reaction is carried out in anaerobic reaction-pot and should be noted following two conditions：(1)pH>7 and VFA/TIC<0.4
Shi Jinhang, otherwise easily causes retort to be acidified, and then causes influence anaerobic fermentation stability of becoming sour.(2) high-concentration ammonia-nitrogen is released
The magnesium salts and microcosmic salt that should be repeatedly added on a small quantity during the suppression for causing, will the reduction of ammonia nitrogen concentration gradient, rather than being disposably down to
Aimed concn.
Although above the present invention is described in detail with a general description of the specific embodiments,
On the basis of the present invention, it can be made some modifications or improvements, this will be apparent to those skilled in the art.Cause
This, these modifications or improvements, belong to the scope of protection of present invention without departing from theon the basis of the spirit of the present invention.
Claims (10)
1. a kind of method that ammonia suppresses in releasing feces of livestock and poultry anaerobic fermentation process, it is characterised in that comprise the following steps：
(1) when obvious ammonia is formed in feces of livestock and poultry anaerobic fermentation system suppressing, adjust anaerobic fermentation system pH value and
VFA/TIC, the VFA/TIC are the mass concentration ratio of volatile fatty acid and TIC；
(2) to magnesium salts and phosphate is added in reaction system, while adjusting pH value to maintain fermentation system normally to run.
2. the method for claim 1, it is characterised in that the pH value of the regulation anaerobic fermentation system described in step (1) is
＞ 7.
3. method as claimed in claim 2, it is characterised in that the pH value of the regulation anaerobic fermentation system described in step (1) is
7-8。
4. the method for claim 1, it is characterised in that step (1) the VFA/TIC ＜ 0.4.
5. the method as described in claim 1-4 is any, it is characterised in that step (2) is a small amount of repeatedly to add magnesium salts and phosphate,
Prevent disposably to add the magnesium salts and phosphate of aim parameter.
6. method as claimed in claim 5, it is characterised in that magnesium salts and phosphate that step (2) is added every time, makes NH4 +：
Mg2+：PO4 3-Mol ratio be 1：1：1；The NH4 +It is the NH for intending eliminating in fermentation system4 +。
7. method as claimed in claim 5, it is characterised in that pH value maintains ＞ 7 all the time in step (2).
8. method as claimed in claim 5, it is characterised in that NH in monitoring system at any time in step (2)4 +Concentration, wait to drop
When there is no ammonia nitrogen concentration when ammonia suppresses, stop adding magnesium salts and phosphate.
9. application of the method as described in claim 6-8 is any in feces of livestock and poultry anaerobic fermentation.
10. application of the method as described in claim 6-8 is any in bio anaerobic fermentation.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108751572A (en) * | 2018-05-17 | 2018-11-06 | 沈阳建筑大学 | A kind of wastewater treatment equipment and method of intensified denitrification and dephosphorization |
| CN110776226A (en) * | 2019-09-23 | 2020-02-11 | 农业部沼气科学研究所 | Method for treating excrement in pig farm |
| CN110981137A (en) * | 2019-11-27 | 2020-04-10 | 黄细香 | Novel rod liquid stirring type biogas slurry backflow slitting manure-pollution anaerobic fermentation machine |
| CN111072244A (en) * | 2019-12-23 | 2020-04-28 | 江苏裕创环境科技有限公司 | Comprehensive utilization method of large-scale dairy farm waste |
-
2017
- 2017-02-16 CN CN201710084388.1A patent/CN106865936A/en active Pending
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| Title |
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| M.S.ROMERO-GÜIZA: "Feasibility of coupling anaerobic digestion and struvite precipitation in the same reactor: Evaluation of different magnesium sources", 《CHEMICAL ENGINEERING JOURNAL》 * |
| S.ULUDAG-DEMIRER: "Anaerobic digestion of dairy manure with enhanced ammonia removal", 《JOURNAL OF ENVIRONMENTAL MANAGEMENT》 * |
| 于秋生 译: "《食品加工过程用水和用能管理手册》", 31 March 2013, 中国轻工业出版社 * |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108751572A (en) * | 2018-05-17 | 2018-11-06 | 沈阳建筑大学 | A kind of wastewater treatment equipment and method of intensified denitrification and dephosphorization |
| CN110776226A (en) * | 2019-09-23 | 2020-02-11 | 农业部沼气科学研究所 | Method for treating excrement in pig farm |
| CN110981137A (en) * | 2019-11-27 | 2020-04-10 | 黄细香 | Novel rod liquid stirring type biogas slurry backflow slitting manure-pollution anaerobic fermentation machine |
| CN111072244A (en) * | 2019-12-23 | 2020-04-28 | 江苏裕创环境科技有限公司 | Comprehensive utilization method of large-scale dairy farm waste |
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Application publication date: 20170620 |