CN105693056B - A method of with zeroth order Nanoscale Iron reinforcement sludge anaerobic digestion methane phase - Google Patents
A method of with zeroth order Nanoscale Iron reinforcement sludge anaerobic digestion methane phase Download PDFInfo
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- CN105693056B CN105693056B CN201610146298.6A CN201610146298A CN105693056B CN 105693056 B CN105693056 B CN 105693056B CN 201610146298 A CN201610146298 A CN 201610146298A CN 105693056 B CN105693056 B CN 105693056B
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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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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E50/00—Technologies for the production of fuel of non-fossil origin
- Y02E50/30—Fuel from waste, e.g. synthetic alcohol or diesel
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Abstract
A method of with zeroth order Nanoscale Iron reinforcement sludge anaerobic digestion methane phase, belonging to solid waste resource recovery technical field.Anaerobically digested sludge pH is first adjusted to 6.8 7.2；In N2Protection under by sludge be packed into anaerobic reaction bottle, lead to N2It is less than 300mV to ORP, it adds simultaneously into zeroth order Nanoscale Iron, make a concentration of 100 1000mg/L of zeroth order Nanoscale Iron, anaerobic reaction bottle is placed in shaking table and carries out anaerobic digestion, shaking speed is set as 150 180rpm, anaerobic digestion is reacted 15 20 days, and gas chromatography is selected to measure the concentration of methane in gas phase along journey, methane yield is measured using gas-liquid equilibrium method, to which methane volumetric be obtained by calculation.The present invention does not need the input of additional energy source, and dosage is few compared with common iron powder, and there is higher cost-effectiveness, this method to be suitable for anaerobically digested sludge and excess sludge.
Description
Technical field
The present invention relates to a kind of methods with zeroth order Nanoscale Iron reinforcement sludge anaerobic digestion methane phase.Belong to solid waste
Resource technology field.
Background technology
Along with the implementation that China's urbanization is in progress, the sludge quantity that sewage disposal generates sharply increases.According to statistics, China city
The annual emissions of the current dewatered sludge of sewage treatment plant of city are about 1,500,000 tons, and annual growth is more than 10%, and it is useless to account for China's total solid
The 3.2% of gurry.However, " the light mud of heavy water " idea makes the sludge direct emission of a large amount of non-complete stabilities, sludge direct emission
The secondary pollution for not only causing environment also creates a large amount of energy waste.
Anaerobic sludge digestion process is a complicated organic matter degradation process, in being total to for methanogen and non-methanogen
Biodegradable organic is decomposed into carbon dioxide, methane under same-action, is sludge reduction, innoxious, recycling has
One of effect means.The process includes hydrolysed ferment section, hydrogenesis and acetogenesis section and methane phase section three parts, is connected each other, common shadow
Ring anaerobic digestion effect.However that there are reaction speeds is slow, residence time length (20-30 days), produces first for traditional anaerobic digestion techniques
The disadvantages such as alkane efficiency is low, and degradation effect of organic compound is low, to limit the promotion and application of the technology.In three ranks of anaerobic digestion
Duan Zhong, hydrolysis acidification section and methane phase section are main rate-limiting steps in anaerobic digestion process.Hydrolysis stage, which refers to macromolecular, to be had
Machine compound, such as protein, carbohydrate, fat are converted into amino acid, monosaccharide, aliphatic acid, sweet under the action of hydrolysed ferment bacterium
The process of the small molecular organic compounds such as oil.The abundant degree of hydrolysis directly determines maximum energy recovery rate.Due to hydrolyzing not
Fully, still remain the organic matters such as a large amount of protein and cellulose after digestion in sludge, while causing energy waste also not
Conducive to the volume reduction of sludge.The methanation stage is the final step of anaerobic digestion, is the committed step for realizing recycling.According to reaction
The difference of matrix, there are three types of pathway of methane production altogether, respectively with acetic acid, H2/CO2And methyl compound is substrate, and it is anti-with first two
Answer approach most commonly seen.Studies have shown that in anaerobic digester system about 70% CH4Acetic acid is originated from, a large amount of CO is supervened2,
To reduce CH in biogas4Concentration.
Currently, the method for common reinforcement sludge anaerobic digestion methane phase is sludge strenuous primary treatment mode, the sludge is strong
Changing pretreatment mode has the physico-chemical process such as ultrasonic wave, heat treatment, ozone, soda acid, these methods can carry to a certain extent
The hydrolysis acidification rate of organic matter when high anaerobic digestion, is conducive to the progress of follow-up methane phase process.However, above-mentioned sludge is strengthened
Pretreatment mode belongs to preconditioning technique, the step of not only having increased Treatment of Sludge, but also lacks there are high energy consumption is inefficient
Point.For example, most common heat treatment technics, although the degradation rate to sludge is promoted, promotion effect is simultaneously little, and highest is only
It is 20% or so, moreover, even if to the excess sludge progress anaerobic digestion after heat treatment, organic matter is residual in postdigestive sludge
Allowance is according to just close to 50%.
Invention content
The purpose of the present invention is disclose a kind of method with zeroth order Nanoscale Iron reinforcement sludge anaerobic digestion methane phase, this method
Organic matter degradation is not thorough during overcoming conventional anaerobic digestion, and methane phase efficiency is low and sludge strenuous primary treatment mode is deposited
High energy consumption, the low technological deficiency of efficiency.
In order to achieve the above object, the present invention has found zeroth order Nanoscale Iron (NZVI) as a kind of strong reduction by studying for a long period of time
Agent is widely used in environment remediation field, can handle a variety of Recalcitrant chemicals, so as to reinforced anaerobic digestion process.Zero
Valence Nanoscale Iron can gas-evolving electrodes under anaerobic, provide electronics for anaerobe, reduce oxidation-reduction potential, adjust
PH provides suitable growth conditions for methanogen, and the ferrous ion dissolved is the important substance that Institute of Micro-biology needs,
It is the important component of enzyme.In addition compared with common Zero-valent Iron, zeroth order Nanoscale Iron, can due to its higher reactivity
Larger molecular organics difficult to degrade are handled, to realize microorganism broken wall, are released effectively intracellular organic matter, reinforced anaerobic digested
The hydrolysis of journey, acidification efficiency, to improve methane phase efficiency, the final effective recycling for realizing the energy.The present invention is using adjusting zero
Dosing method (including throwing amount and add the time) reinforced anaerobic digestion process of valence Nanoscale Iron (NZVI), reaches overall and improves anaerobism
Digestion effect increases the purpose of energy recovery.
Concrete scheme is as follows：
A, is 14.00g/L-15.00g/L by total suspended solid concentration SS, and volatile suspended solids concentration VSS is 6.00g/
L-7.00g/L, COD SCOD are that the anaerobic digestion of sewage treatment plant's anaerobic digester of 2000mg/L-3000mg/L is dirty
The pH of mud is adjusted to 6.8-7.2.
B, in N2Protection under the anaerobically digested sludge of step A is packed into anaerobic reaction bottle, and add zeroth order Nanoscale Iron, make
N is led in a concentration of 100-1000mg/L of zeroth order Nanoscale Iron in anaerobically digested sludge, sealing2To oxidation-reduction potential (ORP) be less than-
300mV。
Anaerobic reaction bottle is placed in shaking table by C, sets shaking speed as 150-180rpm, is carried out anaerobic digestion and is reacted 15-
20 days, then, gas chromatography is selected to measure the concentration of methane in gas phase along journey, methane aerogenesis is measured using gas-liquid equilibrium method
Amount, to which methane volumetric be obtained by calculation.
The zeroth order Nanoscale Iron size of above-mentioned steps B is 80-100nm.
The zeroth order Nanoscale Iron of above-mentioned steps B can be prepared by liquid phase reduction, or directly purchase obtains.Liquid phase reduction
Reaction principle is as follows：
2Fe(H2O)6 3++6BH4 -+6H2O=2Fe0(s)+6B(OH)3+21H2(g)
Specific operation process is：At room temperature to the FeCl of certain volume3·6H2O (0.04M) is slowly added dropwise isometric
NaBH4(0.15M) makes to be uniformly mixed using churned mechanically mode, and reduction process is added dropwise and is completed in 30min, is added dropwise to complete
After continue to stand 1h after being stirred 20min, make generation NZVI stabilize after precipitate, discard supernatant liquid, absolute ethyl alcohol be used in combination
The NZVI of synthesis, is finally stored in absolute ethyl alcohol for use by the impurity on 3~4 times removal surfaces of cleaning.
The present invention compared with the existing technology, has the advantage that and advantageous effect：
1, the NZVI that the present invention adds can destroy the cell membrane of microorganism, discharge intracellular organic matter and each hydrolase, by
It is ancient bacterium in methanogen, there is special cell envelope structure, common micro- life is higher than to the resistance of the strong reducing property of NZVI
Object, therefore, the best NZVI throwings amount of the present invention can ensure that the activity of function bacterium (methanogen) is not destroyed, while maximum journey
The intracellular organic matter of the non-functional bacterium of recycling of degree；Suitable NZVI charging times can reduce easily biological-degradable organic matter to NZVI
Unnecessary consumption reduces the dosage of NZVI, therefore the present invention is at low cost.
2, the entire anaerobic digestion strengthening process of the present invention does not need the input of additional energy source, improves the energy to the full extent
Net output increases substantially energy recovery rate, is the effective means for realizing " carbon neutralization ".
3, compared with common iron powder, except providing electron donor (H for anaerobic System2) outside, zeroth order Nanoscale Iron is due to it
Strong reducing property and strong reactivity can in reinforced anaerobic digestion system refractory organic hydrolysis, while destroying microorganism
Wall film, discharges intracellular organic matter and a large amount of hydrolases, the rate of recovery of postdigestive methane improve about 30%.
4, although common iron powder cost is only the 1/180~1/220 of NZVI, respectively reach best anaerobic digestion effect
When, the dosage of common iron powder is about 50-30 times of zeroth order Nanoscale Iron, and the completeness of energy recovery is far above common iron powder, because
This, NZVI has higher cost-effectiveness.
Description of the drawings
Fig. 1 is the NZVI throwings amount of 1-6 of the embodiment of the present invention and the variation diagram of methane concentration and reaction time
Fig. 2 is the NZVI throwings amount of 1-6 of the embodiment of the present invention and the variation diagram of methane production and reaction time
Specific implementation mode
Embodiment 1-6, wherein the zeroth order Nanoscale Iron throwing amount of Examples 1 and 2 are 0, the zeroth order Nanoscale Iron of embodiment 3,4,5,6
Throwing amount is followed successively by 100 (mg/L), 300 (mg/L), 600 (mg/L) and 1000 (mg/L), and the throwing amount of ethyl alcohol is 0 in addition to embodiment 1
Outside, it is 1 (mL).Other techniques are identical with condition.
A, sludge are taken from the anaerobically digested sludge of Shanghai sewage treatment plant anaerobic digester.According to standard method, survey
The total suspended solid concentration (SS=14.683g/L) of the fixed anaerobic digestion mud, volatile suspended solids concentration (VSS=6.841g/
L), total COD (COD=2263mg/L).Adjust pH ≈ 7.
B leads to N2When being less than -300mV to oxidation-reduction potential (ORP) (usual 30min).Then, in N2Protection under
It is 500mL that the sludge of step A, which is respectively charged into specification used in embodiment 1,2,3,4,5,6, and swept volume is 300mL anaerobic reactions
Bottle, while the zeroth order Nanoscale Iron (NZVI) listed by table 1 is added in each anaerobic reaction bottle, it is respectively 0 to make NZVI concentration,
100,300,600,1000mg/L, it covers tightly bottle cap and seals up membrana oralis sealing.Since NZVI is stored in absolute ethyl alcohol, so implementing
Example 2 only adds the absolute ethyl alcohol of same dose but does not add zeroth order Nanoscale Iron as a control group.Concrete composition is shown in Table 1.
C, anaerobic digestion.Anaerobic reaction bottle is placed in shaking table and carries out anaerobic digestion.Shaking speed is set as 150rpm.Instead
It is 35 DEG C to answer temperature.It samples within 0th, 1,2,3,4,6,10,15,20 day.
The concentration of methane selects gas chromatography to be measured along journey in gas phase.Gas-chromatography selects TCD detectors, TCD detections
Device operating parameter：Injector temperature is 80 DEG C, and detector temperature is 100 DEG C, and post case temperature is 80 DEG C.
Methane yield is measured using gas-liquid equilibrium method.Total biogas body that gas-liquid equilibrium must generate is done to anaerobic reaction bottle
Product, to which methane volumetric be obtained by calculation.
The data of gained in step C are mapped to obtain the variation of the best feed rate and methane concentration and reaction time of NZVI
The best feed rate and methane production and the variation relation figure in reaction time (Fig. 2) of relational graph (Fig. 1) and NZVI.
Intensive treatment is carried out to sludge with NZVI, breaking up cell wall makes organic matter be transferred to liquid phase from solid phase.In addition, zeroth order
Nanoscale Iron can gas-evolving electrodes under anaerobic, provide electronics for anaerobe, reduce oxidation-reduction potential, adjust pH,
Suitable growth conditions is provided for methanogen.
By Fig. 1,2 it is found that the most suitable throwing amount of NZVI is 600mg/L, methane concentration and yield reach maximum value at this time, after
The continuous throwing amount for increasing NZVI is for CH4Yield do not have a significant impact, and methane concentration is reduced to 33% from 45%；This
Outside, when NZVI concentration is less than 300mg/L, methane concentration change curve does not occur second peak, illustrates under the concentration conditions
Gas-evolving electrodes only occur for NZVI, by microorganism adsorption, but are not enough to destroy cell envelope.
Most suitable front and back on day 4, the digestion time corresponding to first peak value of namely for methane concentration that adds the time, at this time body
The small organic molecule of easy biological utilisation is consumed completely substantially in system, and refractory organic is also in hydrolysis speed limit rank
Section.The anaerobic System for having added NZVI occurred second peak at the 10th day, and than first peak delays 6 days, was difficult to degrade
Organic matter further hydrolysis acidification required time under the action of NZVI and the hydrolase of release.
Table 1, the NZVI concentration gradients setting of embodiment 1-6
Claims (2)
1. a kind of method with zeroth order Nanoscale Iron reinforcement sludge anaerobic digestion methane phase, it is characterised in that：
A, is 14.00g/L-15.00g/L by total suspended solid concentration SS, and volatile suspended solids concentration VSS is 6.00g/L-
7.00g/L, COD SCOD are the anaerobically digested sludge of sewage treatment plant's anaerobic digester of 2000mg/L-3000mg/L
PH be adjusted to 6.8-7.2；
B, in N2Protection under the anaerobically digested sludge of step A is packed into anaerobic reaction bottle, and add zeroth order Nanoscale Iron, make anaerobism
N is led in a concentration of 100-1000mg/L of zeroth order Nanoscale Iron in digested sludge, sealing2It is less than -300mV to oxidation-reduction potential；
Anaerobic reaction bottle is placed in shaking table by C, sets shaking speed as 150-180rpm, is carried out anaerobic digestion and is reacted 15-20
Then it selects gas chromatography to measure the concentration of methane in gas phase along journey, methane yield is measured using gas-liquid equilibrium method,
To which methane volumetric be obtained by calculation；
The zeroth order Nanoscale Iron size of above-mentioned steps B is 80-100nm.
2. a kind of method with zeroth order Nanoscale Iron reinforcement sludge anaerobic digestion methane phase according to claim 1, feature
It is：The zeroth order Nanoscale Iron of step B is the commodity of market purchase or is prepared by liquid phase reduction, the behaviour of liquid phase reduction
It is as follows to make process：At room temperature to the FeCl of certain volume3·6H2Isometric NaBH is slowly added dropwise in O4, use is churned mechanically
Mode makes to be uniformly mixed, and reduction process is added dropwise and is completed in 30min, continues to stand 1h after being stirred 20min after being added dropwise to complete,
It is precipitated after so that the NZVI of generation is stabilized, discards supernatant liquid, be used in combination washes of absolute alcohol 3-4 all over the impurity on removal surface, finally
The NZVI of synthesis is stored in absolute ethyl alcohol for use；
Above-mentioned FeCl3·6H2A concentration of 0.04M of O；
Above-mentioned NaBH4A concentration of 0.15M.
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| CN106047941B (en) * | 2016-06-24 | 2019-12-27 | 太原理工大学 | Method for enhancing anaerobic digestion efficiency of excess sludge by modifying brewing wastes |
| CN106745717A (en) * | 2016-11-28 | 2017-05-31 | 江南大学 | A kind of method for strengthening molasses alcohol waste water Anaerobic Digestion |
| CN107522375A (en) * | 2017-08-22 | 2017-12-29 | 华南理工大学 | A kind of method that Zero-valent Iron and activated carbon strengthen excess sludge anaerobic digestion methane phase |
| CN108341571A (en) * | 2018-01-30 | 2018-07-31 | 上海交通大学 | The single step heating startup method of sludge high temperature anaerobic digestion reaction |
| CN109209268A (en) * | 2018-10-19 | 2019-01-15 | 中国石油集团渤海钻探工程有限公司 | The method that drain is returned in acidification is handled using reproducibility iron powder |
| CN110127972B (en) * | 2019-03-06 | 2020-12-29 | 同济大学 | Method for improving anaerobic digestion efficiency of sludge and simultaneously reducing heavy metal ecotoxicity |
| CN111099802A (en) * | 2020-01-02 | 2020-05-05 | 广州大学 | Method for producing methane by promoting anaerobic digestion of high-solid-content municipal sludge through zero-valent iron |
| CN114291989A (en) * | 2021-12-10 | 2022-04-08 | 同济大学 | Method for improving methane production amount of sludge anaerobic digestion by using iron/carbon/biological enzyme coupling technology |
| CN115521035A (en) * | 2022-10-11 | 2022-12-27 | 湖南大学 | Method for improving methane production by anaerobic digestion of sludge |
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