CN111320265A - Anaerobic ammonium oxidation sludge activity evaluation method and application - Google Patents
Anaerobic ammonium oxidation sludge activity evaluation method and application Download PDFInfo
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- CN111320265A CN111320265A CN201811540224.6A CN201811540224A CN111320265A CN 111320265 A CN111320265 A CN 111320265A CN 201811540224 A CN201811540224 A CN 201811540224A CN 111320265 A CN111320265 A CN 111320265A
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- C02F2203/004—Apparatus and plants for the biological treatment of water, waste water or sewage comprising a selector reactor for promoting floc-forming or other bacteria
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- C02F2209/00—Controlling or monitoring parameters in water treatment
- C02F2209/03—Pressure
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Abstract
The invention provides an activity evaluation method of anaerobic ammonium oxidation sludge, which comprises the following steps: step S1, providing a sealable reaction container and a reaction solution; step S2, adding anaerobic ammonia oxidation sludge and reaction liquid into the sealable reaction container to enable the anaerobic ammonia oxidation sludge to be in contact with the reaction liquid; and step S3, testing the pressure of the closed reaction container at different time to obtain the pressure change rate, and representing the activity of the anaerobic ammonia oxidation sludge according to the pressure change rate. The method has the advantages of no need of building a device, low experiment cost, short experiment period, capability of rapidly providing qualitative and semi-quantitative data and obviously improved efficiency.
Description
Technical Field
The invention relates to an anaerobic ammonium oxidation sludge activity evaluation method and application.
Background
Nitrogen pollution is one of the important factors causing water eutrophication, and waste water denitrification is one of the main works of sewage treatment. Ammonia nitrogen removal in traditional wastewater treatment is generally realized through nitrification and denitrification processes, ammonia oxidizing bacteria oxidize ammonia nitrogen into nitrite in a nitrification stage, and nitrite oxidizing bacteria oxidize nitrite into nitrate; the heterotrophic denitrifying bacteria convert nitrified product nitrate into nitrogen gas in the denitrification stage, so that the denitrification treatment of the wastewater is realized. The conversion of ammonia nitrogen into nitrate nitrogen is realized by aeration, a large amount of electric energy is consumed, a sufficient carbon source is required in the denitrification process, carbon sources (organic matters) are often insufficient in urban sewage and certain special sewage, an additional carbon source is required, the operation cost is increased, and secondary pollution is possibly caused. In the anaerobic ammonia oxidation denitrification process, the anaerobic ammonia oxidation bacteria uses CO2As a carbon source, with NO2 -Is an electron acceptor, NH4 +Is an electron donor, generates nitrogen (trace nitrate nitrogen as a byproduct), directly realizes the denitrification of wastewater, greatly shortens the process of oxidizing and reducing ammonia nitrogen into nitrogen, and has high efficiency and material and energy saving. The research on the scientific research and the application of the anaerobic ammonia oxidation process has important value. The applicability of the anaerobic ammonia oxidation process under different water quality conditions is evaluated, and the treatment efficiency of the anaerobic ammonia oxidation process is important for the research of anaerobic ammonia oxidation application under different influence factors. In the prior art, the research is generally carried out by adopting a method of establishing an anaerobic ammonia oxidation small test process, changing operation conditions or changing the quality of inlet water. However, anaerobic nitrogen-oxygen bacteria are sensitive to light, oxygen and the like, and have strict requirements on the environment, so the research method has the problems of high construction cost of a test device, long test period, easy collapse of the process due to impact in the test process and the like.
Disclosure of Invention
The invention provides a method for evaluating the activity of anaerobic ammonia oxidation sludge by using pressure change on the basis of researching the anaerobic ammonia oxidation reaction process. The method can quickly evaluate the activity of the anaerobic ammonia oxidation sludge, reduces the work of assay and analysis and has low labor intensity.
The invention is realized by the following technical scheme:
an activity evaluation method of anaerobic ammonia oxidation sludge comprises the following steps:
step S1, providing a sealable reaction container and a reaction solution;
step S2, adding anaerobic ammonia oxidation sludge and reaction liquid into the sealable reaction container to enable the anaerobic ammonia oxidation sludge to be in contact with the reaction liquid;
and step S3, testing the pressure of the closed reaction container at different time to obtain the pressure change rate, and representing the activity of the anaerobic ammonia oxidation sludge according to the pressure change rate.
According to the preferred embodiment of the invention, in step S3, after testing the pressure of the sealable reaction vessel at different times, a pressure-time relation curve is made, and the activity of the anammox sludge is characterized by the slope of the pressure-time relation curve.
According to a preferred embodiment of the present invention, the amount of the anammox sludge and the reaction solution loaded in the sealable reaction vessel is 85% to 90% of the effective volume of the sealable reaction vessel, and may be, for example, 85%, 86%, 87%, 88%, 89%, 90% or any value therebetween.
According to a preferred embodiment of the invention, the solids concentration (MLSS) of the anammox sludge in the mixture of anammox sludge and reaction liquid is in the range of 1.0-5.0g/L, such as 1.0g/L, 1.5g/L, 2.0g/L, 2.5g/L, 3.0g/L, 3.5g/L, 4.0g/L, 4.5g/L, 5.0g/L and any value in between, preferably 2.0-4.0 g/L.
According to a preferred embodiment of the present invention, the reaction solution comprises ammonia nitrogen and nitrite nitrogen, and preferably, the reaction solution comprises NH4Cl and NaNO2。
According to a preferred embodiment of the present invention, the reaction solution further contains trace elements including one or more of Ca, Mg, Fe, Cu, Zn and Mn.
According to a preferred embodiment of the present invention, NH is present in the reaction solution4 +The concentration of (b) is 100-500 mg/L.
According to a preferred embodiment of the present invention, NO is present in the reaction solution2 -And NH4 +Is 1.0-1.4, such as 1.0, 1.1, 1.2, 1.3, 1.4 and any value in between.
According to a preferred embodiment of the present invention, a pressure testing device is connected to the sealable reaction vessel, and the pressure of the sealable reaction vessel is tested by the pressure testing device.
According to a preferred embodiment of the present invention, step S3 is performed at a constant temperature to avoid the influence of temperature variation on the pressure. A thermostated oscillation chamber is used to control the thermostated conditions.
The method for evaluating the activity of the anaerobic ammonia oxidation sludge provided by the invention can be used for optimizing the anaerobic ammonia oxidation process conditions. The method provided by the invention can be used for rapidly investigating the influence of different influencing factors such as temperature, pH and the like on the operation of the anaerobic ammonia oxidation process, thereby being used for optimizing the anaerobic ammonia oxidation process conditions.
The test principle of the evaluation method provided by the invention is based on the anaerobic ammonia oxidation reaction process, and the currently accepted total reaction equation of the anaerobic ammonia oxidation reaction is as follows:
1NH4 ++1.32NO2 -+0.066HCO3 -+0.13H+→1.02N2+0.26NO3 -+0.066CH2O0.5N0.15+2.03H2O
from the view of the reaction process, all reactants are ions in a solution, the product contains gas and water, the volume of water generated by the reaction under certain conditions can be ignored compared with the volume of the gas, according to an ideal gas state equation PV ═ nRT, if the reaction is carried out in a closed container and the temperature is kept constant, the pressure in the reactor is inevitably increased in the reaction process, and in a certain range, the speed and the degree of the pressure increase are positively correlated with the generation speed and the amount of nitrogen in the reaction process; the nitrogen generation quantity is positively correlated with the sludge activity, so that the change of the pressure in the reactor has a definite relation with the sludge activity. And the sludge activity can be quickly evaluated through pressure testing by selecting proper reactor volume, reaction liquid adding amount, sludge adding amount and testing time period. The purpose of the present invention is to rapidly evaluate the activity of anammox sludge, and to seek a method for avoiding long-term culture and acclimatization with a short time, and for facilitating the operation. Under the conditions of miniaturization of the device, less mud for evaluation and short evaluation time, the absolute gas production rate in the evaluation process is necessarily smaller, if the gas production rate is taken as a direct test index, the absolute gas production rate is required to be measured, and under the condition of small absolute gas production rate, the measurement error is larger, and the difficulty of implementation means is larger; the pressure is selected as a test index, the absolute gas production volume is not needed to be concerned, and the pressure change is obvious enough as long as the gas phase volume in the closed reaction space is small enough, so that the measurement is more accurate and is easy to measure. In addition, the pressure measurement of the closed space is not affected by the change of the ambient atmospheric pressure, but the accuracy of the volume measurement is affected.
Based on the anaerobic reaction and gas production characteristics of the anaerobic ammonia oxidation reaction, the relative activity of the anaerobic ammonia oxidation sludge under different conditions is represented by the pressure change in the closed container, the anaerobic ammonia oxidation reaction conditions can be conveniently and rapidly optimized, and the qualitative and semi-quantitative effects of different influencing factors on the anaerobic ammonia oxidation reaction are examined. The method for evaluating the activity of the anaerobic ammonia oxidation sludge does not need to build a device, and the experiment cost is low; the experimental period is short, and qualitative and semi-quantitative data can be given quickly; the assay analysis work is reduced, and the labor intensity is low; a plurality of parallel tests can be carried out simultaneously, and the efficiency can be obviously improved.
Drawings
FIG. 1 is a schematic view of the structure of an experimental apparatus used in example 1 of the present invention.
FIG. 2 is a schematic view of the structure of an experimental apparatus used in comparative example 2 of the present invention.
FIG. 3 is a graph showing the relationship between pH and activated sludge activity in example 1 of the present invention.
Detailed Description
The present invention will be described in detail with reference to examples, but the present invention is not limited to the examples.
Example 1 the pressure test method provided by the present invention was used to examine the effect of pH on the anammox process
Step S1:
the experimental apparatus used in this example is structured as shown in fig. 1, and includes a reaction flask 1, the reaction flask 1 is sealed by a sealing plug 2, the effective volume of the reaction flask 1 is 200mL, and the sealing plug 2 is connected with a precision pressure gauge 3 for measuring the pressure in the reaction flask 1. The reaction flask 1 is controlled to be in a constant temperature state through a water bath 4.
By NH4Cl and NaNO2Preparing a reaction solution containing NO2 -And NH4 +The concentrations are 130mg/L and 100mg/L respectively, and each liter of reaction solution is added with 1mL of the microelement nutrient solution I and II respectively. Putting into a constant temperature box or constant temperature water bath, and keeping the temperature to 33 ℃ for standby.
And (3) a trace element nutrient solution I: EDTA 5000mg/L, FeSO45000mg/L；
And (3) trace element nutrient solution II: EDTA 5000mg/L, MnCl2·4H2O 990mg/L，ZnSO4·7H2O 430mg/L，CoCl2·6H2O 240mg/L，CuSO4·5H2O 250mg/L，NaMoO4·2H2O 220mg/L，NiCl2·6H2O190mg/L，NaSeO4·10H2O 210mg/L，H3BO414mg/L。
Step S2:
seven sets of the reaction apparatus shown in FIG. 1 were taken for standby. 130mL of concentrated anaerobic ammonia oxidation sludge is taken from an existing anaerobic ammonia oxidation test device in a laboratory, added with the reaction liquid prepared in the step one and adjusted to 500mL, uniformly stirred and quickly divided into thirteen parts, wherein seven parts are respectively added into the six reaction bottles 1 with the effective volume of 200mL (the other six parts are used in a comparative example 2), then the reaction liquid is respectively added into each reaction bottle, the sum of the volumes of the reaction liquid and the sludge in each reaction bottle is equal to 175mL, then the pH values of the reaction liquid in the six reaction bottles are respectively adjusted to 7.0, 7.4, 7.8, 8.2, 8.6 and 9.0 by dilute hydrochloric acid or sodium bicarbonate solution, the pH value of the reaction liquid in the other reaction bottle is not adjusted to the sludge, and used as blank comparison, and MLSS is actually measured. Then, the sum of the volumes of the reaction liquid and the sludge in each reaction bottle is adjusted to be equal by using a small amount of reaction liquid, and the sum is 180 ml. Sealing the reaction bottle by a sealing plug connected with a precision pressure gauge, placing the reaction bottle into a constant-temperature oscillation box, adjusting the temperature to 33 ℃, and starting oscillation by selecting a proper oscillation rate, wherein the oscillation frequency is preferably 30-50 RPM. The actual measurement of the MLSS of the anaerobic ammonia oxidation sludge in the blank contrast reaction bottle is 2.3 g/L.
Step S3:
and reading the pressure data of the precise pressure agent every five minutes after ten minutes, actually testing for 30 minutes, reading 7 groups of data by each set of device, and respectively making pressure-time relation curves under different pH conditions according to the results shown in the table 1, wherein the slope of the pressure-time relation curves is used for representing the sludge activity. Comparing the measured sludge activity under different pH conditions.
TABLE 1
The unit of pressure is KPa.
Comparative example 1 establishment of a Small scale test for anammox Process to investigate the influence of pH on the operation of the anammox Process
The method comprises the following steps:
newly building a set of anaerobic ammonia oxidation small-scale test process device, taking part of sludge from the normally-operated anaerobic ammonia oxidation process device to inoculate the sludge to the newly-built anaerobic ammonia oxidation test device, adjusting the operation parameters such as retention time, temperature, pH and the like, continuously operating and culturing for about half a month, inoculating the process, and successfully starting.
Step two:
the same reaction solution as in example 1 was prepared. I.e. with NH4Cl and NaNO2Preparing a reaction solution containing NO2 -And NH4 +The concentrations are 130mg/L and 100mg/L respectively, and a proper amount of trace elements are added into the reaction liquid. The pH value of the system is controlled by adopting an automatic pH value adjusting modeMaking the reaction solution at about 7.0, controlling other parameters of the system such as temperature and residence time in the optimum operation range (test temperature is controlled at 33 deg.C, residence time is controlled at 6 hr), adding the prepared reaction solution, stably running for 3 days, sampling, and testing NO in water2 -And NH4 +Concentration; then keeping the parameters such as temperature, retention time and the like unchanged, sequentially adjusting the pH of the system to 7.4, 7.8, 8.2, 8.6 and 9.0, and sampling and analyzing the NO of the effluent after the system is stably operated for 3 days under each pH condition2 -And NH4 +。
Step three:
and comparing the effluent quality of the system under different pH conditions, and judging the optimal pH operation range. The test data are shown in table 2:
TABLE 2
| pH | NO of effluent2 -(mg/L) | Outlet water NH4 +(mg/L) |
| 7.0 | 5.6 | 9.1 |
| 7.4 | 2.5 | 1.9 |
| 7.8 | 5.3 | 7.2 |
| 8.2 | 10.5 | 12.6 |
| 8.6 | 25.3 | 53.4 |
| 9.0 | 90.5 | 123.2 |
Analysis of the experimental data revealed that the optimum operating range of pH was around 7.4, consistent with the conclusions of the examples. However, the actual use time of the test is more than one month, the construction cost of the test device is high in the period, and the workload of water sample analysis and test is large.
Comparative example 2 examination of the influence of pH on the operation of the anaerobic Ammonia Oxidation Process by plethysmography
Step A1:
the experimental device used in this comparative example has a structure as shown in fig. 2, and includes a reaction flask 5, a gas collecting flask 6, and a drainage measuring flask 7, and the reaction flask 5, the gas collecting flask 6, and the drainage measuring flask 7 are connected in sequence by a communicating tube 8. The reaction flask 5 and the gas collecting flask 6 are kept in a constant temperature state through a water bath 9.
The same reaction solution as in example 1 was prepared and placed in a thermostat to a constant temperature of 33 ℃ for use.
Step A2:
six sets of reaction devices as shown in FIG. 2 were taken for use. Six portions of the anammox sludge-water mixed solution prepared in example 1 were taken and put into six 200ml reaction flasks, and then the reaction solution was added to each reaction flask so that the sum of the volumes of the reaction solution and the sludge in each reaction flask was equal to 175ml, and then the pH of the reaction solution in each reaction flask was adjusted to 7.0, 7.4, 7.8, 8.2, 8.6 and 9.0 with dilute hydrochloric acid or sodium bicarbonate solution, and then the sum of the volumes of the reaction solution and the sludge in each reaction flask was adjusted to 180ml with a small amount of the reaction solution. The reaction bottle is sealed by a bottle cap, a communicating pipe on the bottle cap connects the reaction bottle with a gas collecting bottle filled with water, and the gas production volume is indirectly measured by the water discharge volume of the gas collecting bottle. Putting the reaction bottle and the gas collection bottle into a constant-temperature water bath, and adjusting the temperature to 33 ℃.
Step A3:
the volume of water displaced was read at intervals after ten minutes and the actual test data is shown in table 3. The sludge activity is characterized by the slope of the volume-time curve. Comparing the measured sludge activity under different pH conditions.
TABLE 3
As can be seen from the data of table 3, the sensitivity in comparative example 2 is significantly reduced.
It should be noted that the above-mentioned embodiments are only for explaining the present invention, and do not constitute any limitation to the present invention. The present invention has been described with reference to exemplary embodiments, but the words which have been used herein are words of description and illustration, rather than words of limitation. The invention can be modified, as prescribed, within the scope of the claims and without departing from the scope and spirit of the invention. Although the invention has been described herein with reference to particular means, materials and embodiments, the invention is not intended to be limited to the particulars disclosed herein, but rather extends to all other methods and applications having the same functionality.
Claims (10)
1. An anammox sludge activity evaluation method, comprising:
step S1, providing a sealable reaction container and a reaction solution;
step S2, adding anaerobic ammonia oxidation sludge and reaction liquid into the sealable reaction container to enable the anaerobic ammonia oxidation sludge to contact and react with the reaction liquid;
and step S3, testing the pressure of the closed reaction container at different time, obtaining the pressure change rate, and representing the activity of the anaerobic ammonia oxidation sludge according to the pressure change rate.
2. The method of claim 1, wherein in step S3, after testing the pressure of the sealable reaction vessel at different times, a pressure-time curve is generated to characterize anammox sludge activity as the slope of the pressure-time curve.
3. The method according to claim 1 or 2, wherein the anaerobic ammonia oxidation sludge and the reaction solution are loaded in the sealable reaction vessel in an amount of 85 to 90% of the effective volume of the sealable reaction vessel.
4. A method according to any one of claims 1 to 3, wherein the anammox sludge solids concentration in the mixture of anammox sludge and reaction liquid is in the range of 1.0 to 5.0g/L, preferably 2.0 to 4.0 g/L.
5. Method according to any one of claims 1-4, characterized in that ammonia nitrogen and nitrite nitrogen are included in the reaction solution, preferably NH is included in the reaction solution4Cl and NaNO2。
6. The method according to any one of claims 1 to 5, wherein NH is present in the reaction solution4 +The concentration of (b) is 100-500 mg/L.
7. The method according to claim 5 or 6, wherein NO is present in the reaction solution2 -And NH4 +The mass concentration ratio of (A) is 1.0-1.4.
8. The method according to any one of claims 1 to 7, wherein a pressure testing device is connected to the closable reaction vessel, by which the pressure of the closable reaction vessel is tested.
9. The method according to any one of claims 1 to 8, wherein step S3 is performed at a constant temperature.
10. Use of the method of any one of claims 1-9 to optimize anammox process conditions.
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