CN113105051A - Method for controlling liquid caustic soda addition in ammonia distillation process based on conductivity change - Google Patents
Method for controlling liquid caustic soda addition in ammonia distillation process based on conductivity change Download PDFInfo
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- CN113105051A CN113105051A CN202110345107.XA CN202110345107A CN113105051A CN 113105051 A CN113105051 A CN 113105051A CN 202110345107 A CN202110345107 A CN 202110345107A CN 113105051 A CN113105051 A CN 113105051A
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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
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/02—Treatment of water, waste water, or sewage by heating
- C02F1/04—Treatment of water, waste water, or sewage by heating by distillation or evaporation
- C02F1/048—Purification of waste water by evaporation
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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
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/66—Treatment of water, waste water, or sewage by neutralisation; pH adjustment
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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
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/16—Nitrogen compounds, e.g. ammonia
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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
- C02F2209/00—Controlling or monitoring parameters in water treatment
- C02F2209/05—Conductivity or salinity
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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
- C02F2209/00—Controlling or monitoring parameters in water treatment
- C02F2209/06—Controlling or monitoring parameters in water treatment pH
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Abstract
The invention relates to the technical field of ammonia distillation processes, in particular to a method for controlling the addition of liquid caustic soda in an ammonia distillation process based on conductivity change, which solves the problem of controlling the addition of the liquid caustic soda in the ammonia distillation process. A method for controlling the liquid caustic soda addition in an ammonia distillation process based on conductivity change comprises the following steps: the first step is as follows: gradually dripping liquid alkali into the ammonium sulfate solution, and measuring and recording the pH value change of the solution, the conductivity change of the solution and the liquid alkali input amount in the whole process of adding the liquid alkali; the second step is that: after the ammonium sulfate solution and the liquid caustic soda are mixed to reach a reaction equivalence point, the liquid caustic soda is continuously added into the mixed solution, and the pH value of the solution, the conductivity of the solution and the addition amount of the liquid caustic soda are continuously measured. The invention discloses a method for controlling the liquid caustic soda addition in the ammonia distillation process based on the change of the conductivity, which is provided by adopting two ammonium sulfate solutions with different concentrations and a sodium hydroxide solution to carry out a variable control experiment and according to the change relationship between the solution conductivity and the liquid caustic soda addition in the ammonia distillation process.
Description
Technical Field
The invention relates to the technical field of ammonia distillation processes, in particular to a method for controlling the addition of liquid caustic soda in an ammonia distillation process based on conductivity change.
Background
Coal produces a certain amount of residual ammonia water with higher ammonia nitrogen, cyanide, sulfide, phenol and COD concentration in the coking process, the residual ammonia water generally needs to be treated by oil removal, ammonia distillation, dephenolization and other treatment processes, the ammonia distillation can remove the cyanide and sulfide in the residual ammonia water while removing the ammonia nitrogen in the residual ammonia water, so that the ammonia distillation wastewater can meet the water quality requirement of biological dephenolization inlet water, and common ammonia distillation technologies comprise the following six types: the ammonia distillation technology is implemented by adding alkali liquor into raw material wastewater, wherein the sodium hydroxide solution is the most common alkali liquor, and the essence of the reaction of the alkali liquor and the wastewater is that fixed ammonium salt reacts with the sodium hydroxide solution to form ammonium hydroxide and sodium salt, even if the fixed ammonia is changed into volatile ammonia, because the addition of the liquid alkali in the ammonia distillation process directly affects the content of ammonia at the bottom of a tower and the ammonia distillation efficiency, and the removal rate of ammonia is insufficient due to too small alkali addition, the ammonia distillation efficiency is low, and the excessive cold liquid alkali wastes liquid alkali, and the excessive cold liquid alkali also needs to consume more steam for heating, so that the control of the liquid alkali needs to be realized by monitoring related data of the solution in the ammonia distillation process, aiming at the requirement, a method for controlling the liquid caustic soda addition in the ammonia distillation process based on the conductivity change can be provided.
Disclosure of Invention
The invention aims to provide a method for controlling the addition of liquid caustic soda in an ammonia distillation process based on conductivity change, which solves the problem of controlling the addition of the liquid caustic soda in the ammonia distillation process.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for controlling the liquid caustic soda addition in an ammonia distillation process based on conductivity change comprises the following steps:
the first step is as follows: gradually dripping liquid alkali into the ammonium sulfate solution, and measuring and recording the pH value change of the solution, the conductivity change of the solution and the liquid alkali input amount in the whole process of adding the liquid alkali;
the second step is that: after the ammonium sulfate solution and the liquid caustic soda are mixed to reach a reaction equivalence point, continuously adding the liquid caustic soda into the mixed solution and continuously measuring the pH value of the solution, the conductivity of the solution and the addition amount of the liquid caustic soda;
the third step: drawing a change graph of the pH value of the solution along with the addition of the liquid caustic soda and a change graph of the pH value of the solution along with the addition of the liquid caustic soda according to the recorded data of the addition of the liquid caustic soda and the change data of the pH value of the solution;
the fourth step: drawing a change graph of the solution conductivity along with the liquid caustic soda adding amount and a change graph of the solution conductivity variation along with the liquid caustic soda adding amount according to the recorded data of the liquid caustic soda adding amount and the recorded data of the solution conductivity variation;
the fifth step: and selecting ammonium sulfate solutions with different concentrations to repeat the first step to the fourth step.
Preferably, the liquid alkali used in the first step is a 30wt% sodium hydroxide solution.
Preferably, the concentration of the ammonium sulfate solution used in the first step is 0.3896 mol/L.
Preferably, the concentration of the ammonium sulfate solution used in the fifth step is 0.8008 mol/L.
Preferably, the ammonium sulphate solution used for the tests carried out in the first and fifth steps is of the same mass.
The invention has at least the following beneficial effects:
1. the experiment result shows that the pH value of the solution changes slowly before reaching the equivalent point of the reaction along with the continuous increase of the adding amount of the sodium hydroxide, the pH value is not very sensitive along with the change of the adding amount of the sodium hydroxide at the later stage, the increase of the pH value is obvious only when the equivalent point is reached, and compared with the pH value and the change trend thereof, except that the conductivity of the solution is increased due to the fact that the sodium hydroxide is added at the equivalent point just before the adding point, the conductivity of the solution is continuously reduced along with the adding of the sodium hydroxide until the equivalent point is crossed, the adding of the sodium hydroxide is continued, the conductivity of the solution starts to rise reversely, and the trend that the conductivity of the solution changes along with the increase of the adding amount of the sodium hydroxide is more obvious, so the sodium hydroxide solution is more suitable to be used as reference data for controlling.
2. The experimental result shows that the conductivity of the solution is greatly influenced by the concentration of the ammonium sulfate solution, and the change of the conductivity is slightly influenced by the concentration of the ammonium sulfate solution, so that when the addition of the liquid caustic soda is controlled according to the change of the conductivity of the solution, the difference of the variation ranges of the concentrations of the ammonium sulfate solutions with different concentrations in the process of putting the liquid caustic soda is small, and the monitoring is conveniently carried out by using a unified monitoring device.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the description of the embodiments are briefly introduced below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on these drawings without creative efforts.
FIG. 1 is a graph showing the change in pH of a solution with the amount of sodium hydroxide added;
FIG. 2 is a graph showing the change in pH of a solution with the amount of sodium hydroxide added;
FIG. 3 is a graph of solution conductivity as a function of sodium hydroxide addition;
FIG. 4 is a graph of the change in solution conductivity with sodium hydroxide addition.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The first embodiment is as follows:
referring to fig. 1-4, a method for controlling the amount of liquid caustic soda added in an ammonia distillation process based on conductivity change comprises the following steps:
the first step is as follows: gradually dropwise adding a 30wt% sodium hydroxide solution into an ammonium sulfate solution with the mass of m and the concentration of 0.3896mol/L, and measuring and recording the pH value change of the solution, the conductivity change of the solution and the input amount of the 30wt% sodium hydroxide solution in the whole process of adding the 30wt% sodium hydroxide solution;
the second step is that: after the ammonium sulfate solution with the concentration of 0.3896mol/L and the 30wt% sodium hydroxide solution are mixed to reach a reaction equivalence point, the 30wt% sodium hydroxide solution is continuously added into the mixed solution, and the pH value of the solution, the conductivity of the solution and the adding amount of the 30wt% sodium hydroxide solution are continuously measured;
the third step: because the ammonium sulfate solution with the concentration of 0.3896mol/L and the sodium hydroxide solution with the concentration of 30wt% can generate acid-base neutralization reaction, the pH value of the solution can change along with the increase of the adding amount of the sodium hydroxide solution with the concentration of 30wt%, and a change graph of the pH value of the solution along with the adding amount of the sodium hydroxide can be drawn according to the recorded data of the adding amount of the sodium hydroxide solution with the concentration of 30wt% and the change data of the pH value of the solution;
a comparative example of example one was performed according to example one:
the first step is as follows: gradually dropwise adding a 30wt% sodium hydroxide solution into an ammonium sulfate solution with the mass of m and the concentration of 0.8008mol/L, and measuring and recording the pH value change of the solution, the conductivity change of the solution and the input amount of the 30wt% sodium hydroxide solution in the whole process of adding the 30wt% sodium hydroxide solution;
the second step is that: after the ammonium sulfate solution with the concentration of 0.8008mol/L and the 30wt% sodium hydroxide solution are mixed to reach a reaction equivalence point, the 30wt% sodium hydroxide solution is continuously added into the mixed solution, and the pH value of the solution, the conductivity of the solution and the adding amount of the 30wt% sodium hydroxide solution are continuously measured;
the third step: because the ammonium sulfate solution with the concentration of 0.8008mol/L and the sodium hydroxide solution with the concentration of 30wt% can generate acid-base neutralization reaction, the pH value of the solution can change along with the increase of the adding amount of the sodium hydroxide solution with the concentration of 30wt%, and a change graph of the pH value of the solution along with the adding amount of the sodium hydroxide can be drawn according to the recorded data of the adding amount of the sodium hydroxide solution with the concentration of 30wt% and the change data of the pH value of the solution;
the combination of the first example and the comparative example of the first example shows that: from the plotted graph of the change of the pH value of the solution along with the adding amount of the sodium hydroxide and the graph of the change of the pH value of the solution along with the adding amount of the sodium hydroxide, it can be found that the pH value of the solution is continuously increased along with the adding amount of the 30wt% sodium hydroxide solution, the pH value of the solution shows a continuously increasing change trend, but the change trend is slower before the equivalent point of the reaction is reached, the pH value is obviously increased when the equivalent point is reached, and the change of the pH value along with the adding amount of the sodium hydroxide at the later stage is not very sensitive;
in summary, the following results can be obtained: the first derivative of the solution pH value change calculated by extracting the relevant data is a positive value, which is consistent with the change trend of the solution pH value continuously increasing, however, as can be found from fig. 1 and fig. 2, in the whole ammonia distillation process, although there is a certain correlation between the solution pH value and the adding amount of the 30wt% sodium hydroxide solution, the correlation is obvious only when the two reactions reach the local place of reaction, and in other stages of the reaction, the solution pH value changes more smoothly along with the increase of the adding amount of the sodium hydroxide, so that the method for controlling the liquid alkali adding amount in the ammonia distillation process according to the pH value change has certain disadvantages.
Example two:
referring to fig. 1-4, a method for controlling the amount of liquid caustic soda added in an ammonia distillation process based on conductivity change comprises the following steps:
the first step is as follows: gradually dropwise adding a 30wt% sodium hydroxide solution into an ammonium sulfate solution with the mass of m and the concentration of 0.3896mol/L, and measuring and recording the pH value change of the solution, the conductivity change of the solution and the input amount of the 30wt% sodium hydroxide solution in the whole process of adding the 30wt% sodium hydroxide solution;
the second step is that: after the ammonium sulfate solution with the concentration of 0.3896mol/L and the 30wt% sodium hydroxide solution are mixed to reach a reaction equivalence point, the 30wt% sodium hydroxide solution is continuously added into the mixed solution, and the pH value of the solution, the conductivity of the solution and the adding amount of the 30wt% sodium hydroxide solution are continuously measured;
the third step: the ion equation of the acid-base neutralization reaction of the ammonium sulfate solution with the concentration of 0.3896mol/L and the sodium hydroxide solution with the concentration of 30wt% is as follows:
because the electric power capacities of chemical substances before and after the reaction are different and the 30wt% sodium hydroxide solution is also converted into ions, the conductivity of the solution can change along with the increase of the adding amount of the 30wt% sodium hydroxide solution, and a change graph of the solution conductivity along with the adding amount of the sodium hydroxide and a change graph of the solution conductivity change along with the adding amount of the sodium hydroxide can be drawn according to the recorded data of the adding amount of the 30wt% sodium hydroxide solution and the change data of the solution conductivity;
a comparative example of example two was performed according to example two:
the first step is as follows: gradually dropwise adding a 30wt% sodium hydroxide solution into an ammonium sulfate solution with the mass of m and the concentration of 0.8008mol/L, and measuring and recording the pH value change of the solution, the conductivity change of the solution and the input amount of the 30wt% sodium hydroxide solution in the whole process of adding the 30wt% sodium hydroxide solution;
the second step is that: after the ammonium sulfate solution with the concentration of 0.8008mol/L and the 30wt% sodium hydroxide solution are mixed to reach a reaction equivalence point, the 30wt% sodium hydroxide solution is continuously added into the mixed solution, and the pH value of the solution, the conductivity of the solution and the adding amount of the 30wt% sodium hydroxide solution are continuously measured;
the third step: the ion equation of the acid-base neutralization reaction of the ammonium sulfate solution with the concentration of 0.8008mol/L and the sodium hydroxide solution with the concentration of 30wt% is as follows:
since the chemical substances before and after the reaction have different electric power capacities and the 30wt% sodium hydroxide solution is converted into ions, the conductivity of the solution changes with the increase of the adding amount of the 30wt% sodium hydroxide solution, according to the recorded data of the adding amount of the 30wt% sodium hydroxide solution and the change of the conductivity of the solutionThe chemical data can be used for drawing a graph of the change of the solution conductivity along with the adding amount of the sodium hydroxide and a graph of the change of the solution conductivity along with the adding amount of the sodium hydroxide,
the comparative examples of example two and example two combine to show that: from the drawn change graph of the solution conductivity along with the sodium hydroxide adding amount and the change graph of the solution conductivity along with the sodium hydroxide adding amount, it can be found that, except that the solution conductivity is increased due to just adding a little sodium hydroxide, the solution conductivity is continuously reduced before an equivalence point along with the adding of the sodium hydroxide until the equivalence point is crossed, the sodium hydroxide is continuously added, the solution conductivity starts to reversely rise, in addition, the conductivity is greatly influenced by the concentration of the ammonium sulfate solution in the whole process, and the change of the conductivity is slightly influenced by the concentration of the ammonium sulfate solution;
in summary, the following results can be obtained: before the equivalence point, the addition of sodium hydroxide causes free ammonium cations to combine with sodium hydroxide to generate ammonium hydroxide (or ammonia monohydrate as understood) with poor ionization capacity, so that the overall ion level is reduced, and the solution conductivity is reduced; after the equivalence point, the sodium hydroxide is added to be converted into ions to enhance the conductivity, and the calculation is carried out according to experimental data, wherein before the equivalence point, the first derivative of the conductivity is negative, namely the conductivity is smaller and smaller, and after the equivalence point, the first derivative of the conductivity is positive, namely the conductivity is rapidly increased.
The foregoing shows and describes the general principles, essential features, and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are merely illustrative of the principles of the invention, but that various changes and modifications may be made without departing from the spirit and scope of the invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (5)
1. A method for controlling the liquid caustic soda addition in an ammonia distillation process based on conductivity change comprises the following steps:
the first step is as follows: gradually dripping liquid alkali into the ammonium sulfate solution, and measuring and recording the pH value change of the solution, the conductivity change of the solution and the liquid alkali input amount in the whole process of adding the liquid alkali;
the second step is that: after the ammonium sulfate solution and the liquid caustic soda are mixed to reach a reaction equivalence point, continuously adding the liquid caustic soda into the mixed solution and continuously measuring the pH value of the solution, the conductivity of the solution and the addition amount of the liquid caustic soda;
the third step: drawing a change graph of the pH value of the solution along with the addition of the liquid caustic soda and a change graph of the pH value of the solution along with the addition of the liquid caustic soda according to the recorded data of the addition of the liquid caustic soda and the change data of the pH value of the solution;
the fourth step: drawing a change graph of the solution conductivity along with the liquid caustic soda adding amount and a change graph of the solution conductivity variation along with the liquid caustic soda adding amount according to the recorded data of the liquid caustic soda adding amount and the recorded data of the solution conductivity variation;
the fifth step: and selecting ammonium sulfate solutions with different concentrations to repeat the first step to the fourth step.
2. The method for controlling the addition of the liquid caustic soda in the ammonia distillation process based on the change of the conductivity according to claim 1, which is characterized in that: the liquid caustic used in the first step is a 30wt% sodium hydroxide solution.
3. The method for controlling the liquid caustic soda addition in the ammonia distillation process based on the conductivity change as claimed in claim 2, wherein the method comprises the following steps: the concentration of the ammonium sulfate solution adopted in the first step is 0.3896 mol/L.
4. The method for controlling the liquid caustic soda addition in the ammonia distillation process based on the conductivity change as claimed in claim 3, wherein the method comprises the following steps: the concentration of the ammonium sulfate solution adopted in the fifth step is 0.8008 mol/L.
5. The method for controlling the liquid caustic soda addition in the ammonia distillation process based on the conductivity change as claimed in claim 4, wherein the method comprises the following steps: the quality of the ammonium sulfate solution used for the tests in the first step and the fifth step is the same.
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Citations (6)
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| CN101475842A (en) * | 2008-12-11 | 2009-07-08 | 中冶焦耐工程技术有限公司 | Ammonia distillation process |
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| CN208087254U (en) * | 2018-03-13 | 2018-11-13 | 河北安米诺氨基酸科技股份有限公司 | Ammonia still mends alkali system automatically |
| CN109668941A (en) * | 2018-12-06 | 2019-04-23 | 普瑞斯伊诺康有限公司 | A kind of method of sulfuric acid and manganese sulfate concentration in measurement electrolyte aqueous solution |
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- 2021-03-31 CN CN202110345107.XA patent/CN113105051A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101475842A (en) * | 2008-12-11 | 2009-07-08 | 中冶焦耐工程技术有限公司 | Ammonia distillation process |
| TW201226310A (en) * | 2010-12-16 | 2012-07-01 | Univ Kun Shan | Ammonia gas recovery method, concentration measurement method of ammonium sulfate solution, and concentration control method of ammonium sulfate solution |
| CN106007145A (en) * | 2016-07-05 | 2016-10-12 | 武汉钢铁股份有限公司 | Residual ammonia water treatment method and system |
| JP6269866B1 (en) * | 2017-01-30 | 2018-01-31 | 栗田工業株式会社 | PH control method by electric conductivity |
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| CN109668941A (en) * | 2018-12-06 | 2019-04-23 | 普瑞斯伊诺康有限公司 | A kind of method of sulfuric acid and manganese sulfate concentration in measurement electrolyte aqueous solution |
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Application publication date: 20210713 |