CN101701228A - pH controlling technology for converting municipal sludge into acetic acid - Google Patents
pH controlling technology for converting municipal sludge into acetic acid Download PDFInfo
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- CN101701228A CN101701228A CN200910223522A CN200910223522A CN101701228A CN 101701228 A CN101701228 A CN 101701228A CN 200910223522 A CN200910223522 A CN 200910223522A CN 200910223522 A CN200910223522 A CN 200910223522A CN 101701228 A CN101701228 A CN 101701228A
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Abstract
The invention provides a pH controlling technology for converting municipal sludge into acetic acid, belonging to the field of the recovery of waste. The technology performs different pH control modes to two phases in a coupling system of generating hydrogen and generating acid/consuming hydrogen and generating acetic acid. Before 12 days of fermenting generating hydrogen and generating acid phase (A phase), the pH is not controlled, and from 13 days, the pH is remained at 9-10; the pH is remained at 6.5 when fermenting consuming hydrogen and generating acetic acid (H phase); and the fermentation is stopped after 18 days. The concentration of A phase acetic acid is 7.53g/L, the concentration of H phase acetic acid is 1.45g/L, and the index of A phase SCOD is reduced by 56.7%. The technology solves the problem of the environment pollution caused by the municipal sludge, obtains the acetic acid with high additional value, discharges the polluted water which is easily processed (SCOD index is low), and has the advantages of convenient operation, low cost and obvious effect, etc.
Description
Technical field
A kind of municipal sludge is converted into the pH CONTROL PROCESS of acetate, belongs to the changing waste into resources field.
Background technology
Along with the quickening of Urbanization in China, treatment rate of domestic sewage improves year by year, and the mud generation of municipal wastewater treatment plant also sharply increases.At present, the municipal wastewater treatment plant that China has built up operation just has more than 1320, and a year treatment capacity is 9,725 ten thousand m3.It is estimated that the annual sludge discharged amount in China municipal sewage plant (dry weight) is approximately 5,320,000 tons at present, 2,662 ten thousand tons of weight in wet bases (water ratio 80%), and with annual speed increment more than 15%.Therefore, that municipal sludge is carried out cost-effective treatment and disposal technology is extremely urgent in development.At present China's recycling sludge and innoxious process for treating comprise material of construction such as agricultural, compost burning, system cement and landfill etc., and national according to a preliminary estimate mud is agricultural to account for 44.8%, landfill accounts for 31%, other disposal account for 10.5%, do not dispose about 13.7%.These so-called " processing " and " disposal " estimate under given conditions all that basically above strictly speaking numeral is very inaccurate.According to statistics, the investment that China is used for the sludge treatment disposal accounts for the 20-50% of sewage work's gross investment, and has data to show, the sludge treatment of developed country is disposed the 50-70% that investment accounts for sewage work's gross investment.As can be seen, China's sludge treatment is in serious hysteretic state.
Anaerobic sludge digestion is a biological procedures by the collaborative complexity of finishing of multiple flora.General experience hydrolysed ferment bacterium, the horizontal conversion of vertically taking over conversion and consumption hydrogen acetogen group of producing hydrogen acetogen and methanogen three class floras.Many studies show that, heat treated can be killed asporulate methanogen, thereby has suppressed the product methane reaction, has avoided the conversion of acetate to methane.After methanogen is suppressed, cause reactor head hydrogen dividing potential drop to raise.Under the higher hydrogen partial pressure condition, producing hydrogen product acetic acidreaction can not carry out on thermodynamics, and consumption hydrogen acetogen requires to depress and could effectively change into acetate to hydrogen and carbonic acid gas at the hydrogen branch of trying one's best high, based on this principle, Liu and, people such as Chen Jian propose a kind of two anaerobic fermentation acetate systems that are coupled.It constantly vacuumizes from producing hydrogen product acetate phase (A phase) by vacuum pump, provide lower hydrogen dividing potential drop for producing the hydrogen acetogen, the gas that vacuumizes constantly enters consumption hydrogen and produces acetate phase (H phase), make H keep higher hydrogen dividing potential drop mutually, the amount (application number 200610041457) that the total system operation can obviously be carried high acid and produce acetate.To produce hydrogen product acetate phase and consume hydrogen product acetate two coupled system acid producing abilities mutually in order to improve, Liu and, people such as Chen Jian adopt the forced ventilation measure at the two alternate vacuum pumps that are provided with, to produce hydrogen by the forced ventilation measure produces the hydrogen that acetate produces mutually and consumes hydrogen product acetate with carbonic acid gas as substrate, coupled system acetate productive rate reaches 0.46g acetate/g glucose, and the acetate productive rate during than system's natural ventilation improves, 16%-28% (application number 200710134829); Liu and, people such as Chen Jian adopt fed-batch process not only to reduce product hydrogen and produce the impact of acetate phase organic loading, and reduced product hydrogen velocity peak values, homogenizing the product hydrogen speed in the whole fermentation process, help reaching with consumption hydrogen and produce the balance that acetate consumes hydrogen speed mutually, improve two alternate acid yields (application number 200710134828).
PH is an important envrionment conditions of microorganism existence, not only influences the physiologically active of microorganism, the more important thing is decision mud acidogenic fermentation type.The optimum pH of relevant sludge anaerobic fermentation and acid production, the conclusion that different investigators draw is also inconsistent.Most of investigator thinks that pH is in slightly acidic or near relatively being fit to sludge anaerobic fermentation and acid production under the neutrallty condition.As (Banerjee A such as Banerjee, Elefsiniotis P, Tuhtar D, The effect of addition of potato-processing wastewateron the acidogenesis of primary sludge under varied hydraulic retention time and temperature.JBiotechnol, 1999,72 (3): 203-212.) discover when sludge fermentation pH value is 4.5 left and right sides, can obtain higher volatilization organic acid (VFAs) output, this moment, its value was 1181mg/L.(Lin C Y such as Lin, Effect of heavy metals on volatilefatty acid degradation in anaerobic digestion.Water Res, 1992,26:177-183.) think and will improve high-molecular weight VFAs constituent ratio that then Shi Yi pH condition is between 5.8-6.2; If pH to moving, then causes low-molecular-weight VFAs ratio to increase towards acidic side.Yet the domestic part Study person of having but draws the conclusion that alkaline condition more helps sludge anaerobic fermentation and acid production.As, (Xiao Benyi such as Xiao Benyi, Liu Junxin, pH is to the influence of alkaline purification sludge anaerobic fermentation to produce hydrogen, Science Bulletin, 2005,50 (24): 2734-2738) and Yuan Hongying etc. (Yuan Hongying, based on the excess sludge acidication and the mechanism research thereof of acid-alkali accommodation, Tongji University's Ph D dissertation, 2006) investigated the pH value in the 4.0-11.0 scope, pH is to the influence of residual active sludge anaerobic fermentation and acid production.Found that, anaerobically fermenting 8 days, the pH value is 9.0 and 10.0 o'clock, the productive rate of total VFAs will be apparently higher than acidity and neutrallty condition; It is under 10.0 conditions that the total acid maximum yield appears at the pH value, is 256.2mgVFAs/g-VS (VS, volatile solid content).She (he) think that the VFAs productive rate is better than acidity and neutrallty condition under strong alkaline condition, reason is attributable to two aspects: (1) is organic melts rate and significantly improved under alkaline condition; (2) VFAs consumes approach and promptly produces the methane process and be blocked under strong alkaline condition.As seen, there is obviously dispute in the home and abroad investigator on the optimum pH of sludge anaerobic fermentation and acid production.Qiu Jian etc. discover that pH is bigger to the reactor influence, pH is controlled at 9-10, though acetic acid content increases (Qiu Jian, regulation and control pH promotes mud to produce sour usefulness and the directed acetate that produces of two-phase coupled system, China's water supply and drainage, 2009.25 (13)), but SCOD degradation capability deficiency, the SCOD index is very high in the waste water that reactor is discharged, and causes the later stage cost for wastewater treatment to improve.
Summary of the invention
The technical problem to be solved in the present invention provides and a kind of municipal sludge is converted into the pH CONTROL PROCESS of acetate, and this technology is intended to improve when municipal sludge is converted into the acetate ability and reduces SCOD index in the waste water, reduces subsequent treatment cost.
For solving the problems of the technologies described above, the present invention proposes following technical scheme:
With the municipal sludge pretreatment fluid as substrate, with through the anaerobic activated sludge of heat treated as inoculum, produce acetate and carry out anaerobically fermenting in mutually producing hydrogen, making major ingredient is that the organic acid content of acetate obtains accumulation; Simultaneously, the biogas (hydrogen and carbonic acid gas) that acidization produces consumption hydrogen produce acetate mutually in as the substrate through the anaerobic activated sludge inoculum of heat treated, generation acetate.
In the described method, the municipal sludge pretreatment process is: sludge concentration 100g/L, regulate pH to 12.5 with 8mol/L NaOH, 90 ℃ of heating in water bath also stir 2h, are cooled to room temperature, the centrifugal 20min of 3000rpm, discard residue, supernatant liquor is the mud pretreatment fluid, and 4 ℃ of refrigerator preservations are standby.
In the described method, plant the activation method of mud: it is air-dry to get the anaerobic digestion active sludge, grinds, and sieves, and heats 2h down at 105 ℃, kills non-sporeformer methanogen.The anaerobic activated sludge that the heat treated of learning from else's experience is crossed adds in the 3g/L glucose nutrient solution, transfers pH to 6.5, and 35 ℃ activate 24h down.
In the described method, the processing condition of producing hydrogen product acetate phase (A phase) are as follows: getting the pretreatment fluid of certain mud, is 9-10 with initial pH regulator, does not control pH, reactor operation 12 days; Since the 13rd day, will be adjusted to 9-10 on the pH value, after this, be adjusted into 9-10 with the pH value every day.The processing condition that consumption hydrogen produces acetate phase (H phase) are as follows: planting mud concentration is 2-8gVS/L (VS, volatile solid content), and wherein preferred concentration produces acetate to plant mud concentration mutually be 6gVS/L for producing hydrogen, and consumption hydrogen produces acetate, and to plant mud concentration mutually be 4gVS/L; Initial pH6.5, regulate pH once every day in the fermenting process, makes that the pH value maintains 6.5 all the time in the reactor; Its fermentation condition is as follows: inflated with nitrogen 10-40min before the reactor operation, and sealing, 30-40 ℃ of bottom fermentation planted mud and adopted magnetic agitation or alternate manner to mix with substrate.
In the described method, the measuring method of SCOD is: earlier with centrifugal, supernatant liquor is got filtrate being used to and is detected the COD index with the filtering with microporous membrane of 0.45 μ m, and COD measures the mensuration with reference to GB 11914-89 hydrochemistry oxygen requirement.
In the described method, the measuring method of acetic acid concentration is: the sample of gathering in the fermenting process is centrifugal 10min under 4 ℃ of 4800rpm, use the filtering with microporous membrane of 0.45 μ m then, get 1mL filtrate in centrifuge tube, adding is with the 4-methylvaleric acid solution (as interior mark) of the 0.83g/L of volume and the phosphoric acid solution of 3mol/L (the volatilization organic acid in the solution is vaporized at Sample Room), mixing, the air inlet chromatography detects then.Gas Chromatographic Determination condition: AOC-20i automatic sampler; Fid detector; PEG-20M capillary column (30m * 0.32mm * 0.5 μ m, Dalian Zhong Hui reaches scientific instrument company limited); Adopt the single order temperature programming, 80 ℃ of initial temperature keep 3min, and the back rises to 210 ℃ with the speed of 15 ℃/min, keeps 2min.The temperature of Sample Room and detector all is made as 250 ℃.
The invention solves the problem of easy degradation product environmental pollution in the municipal sludge, obtain the high added value acetic acid product simultaneously; The present invention passes through the pH value in the regulation and control fermenting process, has improved simultaneously and has produced hydrogen product acetate and consume the hydroacetic acid output of middle acetate mutually, and obviously reduced SCOD index in the waste water, has alleviated the difficulty of subsequent wastewater treatment greatly; This processing unit is simple, and is easy to operate, and cost is low, has higher economic value.
Description of drawings
The experimental installation that Fig. 1 the present invention adopts
1, thief hole; 2, injection port; 3, pipe connecting; A, product hydrogen produce the acetate phase; H, consumption hydrogen produce the acetate phase.
Acetic acid concentration changes relatively in Fig. 2 two cover systems
A A phase; B H phase
SCOD change curve between Fig. 3 two cover coupled system yeast phases
Embodiment
Embodiment 1:
Method 1: the coupled system of control process pH not
The discarded initial SCOD value of municipal sludge of the interior mutually substrate of A is 16000mg/L.
Produce hydrogen and produce acetate phase (A phase): plant mud, concentration is 4gVS/L (VS refers to volatile solid), the pretreatment fluid of mud, and initial pH is adjusted to 10, does not control pH in the fermenting process.
Consumption hydrogen produces acetate phase (H phase): plant mud, concentration is 6gVS/L, and initial pH6.5 does not control pH in the fermenting process.
Fermentation condition: inflated with nitrogen 10-40min, sealing, 30-40 ℃ of bottom fermentation planted mud and adopted magnetic agitation or alternate manner to mix with substrate.
The coupled system of method 2: control process pH
The discarded initial SCOD value of municipal sludge of the interior mutually substrate of A is 16000mg/L.
Produce hydrogen and produce acetate phase (A phase): plant mud, concentration is 4gVS/L, the pretreatment fluid of mud, and initial pH is adjusted to 10, and every day is transferred pH one time in the beginning in 13 days of fermenting, and pH is adjusted to 10.
Consumption hydrogen produces acetate phase (H phase): plant mud, concentration is 6gVS/L, initial pH6.5, and regulate pH once every day in the fermenting process, makes the pH value maintain 6.5 all the time.
Fermentation condition: inflated with nitrogen 10-40min, sealing, 30-40 ℃ of bottom fermentation planted mud and adopted magnetic agitation or alternate manner to mix with substrate.
Fig. 2 is seen in the variation of two kinds of method acetic acid concentrations.A phase acetic acid concentration reached at the 12nd day and is up to 5.13g/L in the method 1, basicly stable afterwards no longer rising.A phase acetic acid concentration reached 5.67g/L at the 12nd day in the method 2, and continued to rise to the 18th day, was up to 7.42g/L.Two kinds of method H phase acetic acid concentrations also increase in time and constantly increase, and tend towards stability substantially to the 12nd day, and H finally is 1.17g/L mutually in the method 1, and H finally is 1.46g/L mutually in the method 2.
The two kinds of middle mutually SCOD degraded of method A situations as shown in Figure 3.SCOD index in the method 1 (initial 16000mg/L) is at the preceding 12 days 7241mg/L that descended, the 13rd day to the 18th day 116mg/L that only descends, SCOD index co-falling low 46.0%.SCOD index in the method 2 is at the preceding 12 days 1620mg/L that descended, the 13rd day to the 18th day 1091mg/L that only descends, and SCOD index co-falling is low by 16.9%, and fall is far below method 1.
Fermented preceding 12 days, the output of two kinds of method acetate is very nearly the same, but SCOD index difference is very big.Conceive 12 days uncomfortable pH in early stage thus, later stage re-adjustment pH, this method had both helped suppressing the growth of methanogen, helped producing the accumulation of acetate again, also can reduce SCOD largely simultaneously, improved the utilization ratio of substrate.
Embodiment 2: the coupled system (the initial mutually pH9.0 of A) that adopts the pH CONTROL PROCESS
The discarded initial SCOD value of municipal sludge of the interior mutually substrate of A is 16000mg/L.
Produce hydrogen and produce acetate phase (A phase): plant mud, concentration is 4gVS/L, the pretreatment fluid of mud, and initial pH is adjusted to 9, and every day is transferred pH one time in the beginning in 13 days of fermenting, and pH is adjusted to 9.
Consumption hydrogen produces acetate phase (H phase): plant mud, concentration is 6gVS/L, initial pH6.5, and regulate pH once every day in the fermenting process, makes the pH value maintain 6.5 all the time.
Fermentation condition: inflated with nitrogen 10-40min, sealing, 30-40 ℃ of bottom fermentation planted mud and adopted magnetic agitation or alternate manner to mix with substrate.
Table 1 adopts the coupled system (the initial mutually pH9.0 of A) of pH CONTROL PROCESS
| Time (d) | A phase acetic acid concentration (g/L) | H phase acetic acid concentration (g/L) | A phase SCOD index (mg/L) |
| ??12 | ??5.67 | ??1.07 | ??8833 |
| ??15 | ??6.60 | ??1.19 | ??7915 |
| ??18 | ??7.43 | ??1.32 | ??7113 |
Embodiment 3: the coupled system (the initial mutually pH10.0 of A) that adopts the pH CONTROL PROCESS
The discarded initial SCOD value of municipal sludge of the interior mutually substrate of A is 16000mg/L.
Produce hydrogen and produce acetate phase (A phase): planting mud concentration is 4gVS/L, and initial pH is adjusted to 10, and every day is transferred pH one time in the beginning in 13 days of fermenting, and pH is adjusted to 10.
Consumption hydrogen produces acetate phase (H phase): planting mud concentration is 6gVS/L, initial pH6.5, and regulate pH once every day in the fermenting process, makes the pH value maintain 6.5 all the time.
Fermentation condition: inflated with nitrogen 10-40min, sealing, 30-40 ℃ of bottom fermentation planted mud and adopted magnetic agitation or alternate manner to mix with substrate.
Table 2 adopts the coupled system (the initial mutually pH10.0 of A) of pH CONTROL PROCESS
| Time (d) | A phase acetic acid concentration (g/L) | H phase acetic acid concentration (g/L) | A phase SCOD index (mg/L) |
| ??12 | ??5.73 | ??1.13 | ??8521 |
| ??15 | ??6.71 | ??1.32 | ??7655 |
| ??18 | ??7.53 | ??1.45 | ??6931 |
The comparative example:
The discarded initial SCOD value of municipal sludge of the interior mutually substrate of A is 16000mg/L.
Produce hydrogen and produce acetate phase (A phase): plant mud, concentration 4gVS/L, the pretreatment fluid of mud, initial pH is 8.0, does not control pH in the process.
Consumption hydrogen produces acetate phase (H phase): plant mud, concentration is 6gVS/L, and initial pH is 6.5, does not control pH in the process.
Fermentation condition: inflated with nitrogen 10-40min, sealing, 30-40 ℃ of bottom fermentation planted mud and adopted magnetic agitation or alternate manner to mix with substrate.
| Time (d) | A phase acetic acid concentration (g/L) | H phase acetic acid concentration (g/L) | A phase SCOD index (mg/L) |
| ??12 | ??5.02 | ??1.45 | ??7677 |
| ??15 | ??4.65 | ??1.43 | ??6573 |
| ??18 | ??4.51 | ??1.37 | ??6564 |
Be understandable that, for those of ordinary skills, can be equal to replacement or change according to technical scheme of the present invention and inventive concept thereof, and all these changes or replacement all should belong to the protection domain of the appended claim of the present invention.
Claims (6)
1. pH CONTROL PROCESS that municipal sludge is converted into acetate, it is characterized in that, in producing hydrogen product acetate/consumption hydrogen product acetate coupled system, to pass through pretreated municipal sludge as raw material, in two-phase, plant mud after the activation of access different concns respectively, adopt different pH control methods to control respectively to produce hydrogen to produce acetate and the consumption hydrogen product acetate pH value in the fermenting process mutually, concrete grammar is as follows:
(1) produce hydrogen and produce the acetate phase: initial pH is adjusted to 9-10, and earlier fermentation is not controlled the pH value, transfers pH one time every day from the beginning in the 13rd day of fermenting, and pH is adjusted to 9-10;
(2) consumption hydrogen produces the acetate phase: regulate pH once every day in the fermenting process, makes the pH value maintain 6.5 all the time.
2. method according to claim 1 is characterized in that, produces hydrogen product acetate and produces acetate, hydrogen and carbonic acid gas mutually, and consumption hydrogen produces acetate and utilizes product hydrogen to produce hydrogen and the carbon dioxide generating acetate that acetate produces mutually mutually.
3. method according to claim 1, it is characterized in that, the municipal sludge pretreatment process is: sludge concentration 100g/L, regulate pH to 12.5 with 8mol/L NaOH, 90 ℃ of heating in water bath also stir 2h, are cooled to room temperature, the centrifugal 20min of 3000rpm, discard residue, supernatant liquor is the mud pretreatment fluid, and 4 ℃ of refrigerator preservations are standby.
4. method according to claim 1, it is characterized in that, the activation method of planting mud is: it is air-dry to get the anaerobic digestion active sludge, grind, sieve, heat 2h down at 105 ℃, kill non-sporeformer methanogen, the anaerobic activated sludge that the heat treated of learning from else's experience is crossed adds in the 3g/L glucose nutrient solution, transfers pH to 6.5, and 35 ℃ activate 24h down.
5. method according to claim 1 is characterized in that, it is every liter of 6g volatile solid that product hydrogen product acetate is planted mud concentration mutually, and it is every liter of 4g volatile solid that consumption hydrogen product acetate is planted mud concentration mutually.
6. method according to claim 1 is characterized in that fermenting process is as follows: inflated with nitrogen 10-40min before the reactor operation, and sealing, 30-40 ℃ of bottom fermentation planted mud and adopted magnetic agitation or alternate manner to mix with substrate.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102994578A (en) * | 2012-12-13 | 2013-03-27 | 江南大学 | Method for producing volatile fatty acid by promoting anaerobic fermentation of urban excess sludge |
| CN103642856A (en) * | 2013-12-10 | 2014-03-19 | 中国环境科学研究院 | Method for promoting production of acetic acid by anaerobic fermentation of excess sludge |
| CN112979119A (en) * | 2021-02-25 | 2021-06-18 | 同济大学 | High-value treatment system or method for wet garbage in cities and towns |
-
2009
- 2009-11-23 CN CN200910223522A patent/CN101701228A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102994578A (en) * | 2012-12-13 | 2013-03-27 | 江南大学 | Method for producing volatile fatty acid by promoting anaerobic fermentation of urban excess sludge |
| CN103642856A (en) * | 2013-12-10 | 2014-03-19 | 中国环境科学研究院 | Method for promoting production of acetic acid by anaerobic fermentation of excess sludge |
| CN112979119A (en) * | 2021-02-25 | 2021-06-18 | 同济大学 | High-value treatment system or method for wet garbage in cities and towns |
| CN112979119B (en) * | 2021-02-25 | 2022-07-12 | 同济大学 | High-value treatment system or method for wet garbage in cities and towns |
| WO2022178960A1 (en) * | 2021-02-25 | 2022-09-01 | 同济大学 | High-value treatment system or method for urban wet waste |
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Application publication date: 20100505 |