CN109399848B - High-salt high-ammonia nitrogen wastewater treatment method - Google Patents
High-salt high-ammonia nitrogen wastewater treatment method Download PDFInfo
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- C02F9/00—Multistage treatment of water, waste water or sewage
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- C—CHEMISTRY; METALLURGY
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- C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
- C01C1/00—Ammonia; Compounds thereof
- C01C1/02—Preparation, purification or separation of ammonia
- C01C1/022—Preparation of aqueous ammonia solutions, i.e. ammonia water
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- 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
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- C02F1/66—Treatment of water, waste water, or sewage by neutralisation; pH adjustment
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- C02F2101/00—Nature of the contaminant
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Abstract
The invention discloses a high-salinity high-ammonia-nitrogen wastewater treatment method, which comprises the following steps: (1) adding sodium hydroxide solid into the wastewater, carrying out reflux reaction, absorbing tail gas by a cold trap to generate a low-boiling-point organic solvent, and absorbing generated ammonia gas by water or dilute ammonia water to obtain concentrated ammonia water; (2) after the reflux reaction is finished, cooling, carrying out heat preservation and negative pressure reaction, absorbing tail gas by a cold trap to generate a low-boiling-point organic solvent, and absorbing generated ammonia gas by water to obtain dilute ammonia water; (3) after the negative pressure reaction is finished, cooling to room temperature and filtering; (4) regulating the pH value of the filtrate by using hydrochloric acid, carrying out reduced pressure distillation to recover distilled water, filtering the residual solid-liquid mixture, recovering sodium potassium salt, mechanically applying the filtrate to the wastewater of the next batch, and finally treating the wastewater in a sewage system to realize standard discharge; the treatment method is simple and effective, convenient to operate, low in cost and high in resource utilization rate, well controls and reduces the total discharge amount of the wastewater, and components in the wastewater are separated and utilized, so that clean production is realized.
Description
Technical Field
The invention relates to a high-salinity high-ammonia nitrogen wastewater treatment method, and belongs to the technical field of wastewater treatment.
Background
With the continuous and rapid development of the chemical industry in China, the chemical industry becomes one of the prop industries for the economic development in China, and with the increasingly stricter environmental protection policy, the difficulty and cost of three-waste treatment increase, especially for chemical wastewater with complex components, so that how to effectively treat the chemical wastewater becomes a new environmental protection problem for enterprises.
At present, the treatment methods of the wastewater in the chemical industry mainly comprise a chemical precipitation method, an ion exchange method, a membrane separation method, an adsorption method, a direct evaporation concentration method, an industrial water dilution method, a biochemical treatment method and the like. From the practical application point of view, many manufacturers adopt the combination of the two methods to obtain certain effects, but still belong to the treatment of 'tail end'.
The chemical industry needs to change the treatment mode mainly based on 'tail end' treatment at present, continuously carries out technical innovation in each link of the production process, adjusts the treatment mode of the production process, implements energy conservation and emission reduction from the source, controls and continuously reduces the total emission, and simultaneously turns the treatment technology to the recycling treatment direction, so that the whole process finally achieves the aim of clean production.
Disclosure of Invention
The invention aims to solve the technical problem of overcoming the defects of the prior art and provides a method for treating high-salt high-ammonia nitrogen wastewater, which is simple and effective, convenient to operate, low in cost, high in resource utilization rate, well controls and reduces the total discharge amount of the wastewater, separates and utilizes components in the wastewater, and realizes clean production.
In order to solve the technical problems, the invention provides a method for treating high-salinity high-ammonia nitrogen wastewater, which comprises the following steps:
step (1): adding sodium hydroxide solid into the wastewater, carrying out reflux reaction, absorbing tail gas after the reflux reaction by a cold trap to generate a low-boiling-point organic solvent, and absorbing ammonia gas generated by the reaction by water or dilute ammonia water to prepare concentrated ammonia water;
step (2): after the reflux reaction is finished, cooling the reaction liquid to the required temperature, carrying out heat preservation and negative pressure reaction, absorbing tail gas after the negative pressure reaction by a cold trap to generate a low-boiling-point organic solvent, absorbing ammonia gas generated by the reaction by water to prepare dilute ammonia water, and applying the dilute ammonia water to the step (1) for absorbing the ammonia gas generated by the reaction;
and (3): after the negative pressure reaction is finished, cooling the reaction liquid to room temperature, filtering and washing to realize solid-liquid separation, wherein a filter cake is zinc-magnesium salt;
and (4): and (4) adjusting the pH value of the filtrate obtained in the step (3) to 6-7 by using hydrochloric acid, carrying out reduced pressure distillation to recover distilled water, cooling and filtering the residual solid-liquid mixture, recovering sodium potassium salt of a filter cake, mechanically applying the filtered filtrate to the wastewater of the next batch, and finally treating the wastewater in a sewage system to achieve standard discharge.
The technical scheme of the invention is further defined as follows:
further, in the method for treating the high-salt high-ammonia-nitrogen wastewater, the ammonia nitrogen content of the high-salt high-ammonia-nitrogen wastewater is 10000-100000 mg/L, the COD is 10000-100000 mg/L, and the pH value is 10-14.
In the method for treating the high-salt high-ammonia nitrogen wastewater, the weight ratio of the amount of the sodium hydroxide to the amount of the wastewater is 1 (10-100).
In the method for treating the high-salt high-ammonia nitrogen wastewater, the temperature of the reflux reaction in the step (1) is 80-110 ℃, and the time of the reflux reaction is 1-10 h.
In the method for treating the high-salt high-ammonia nitrogen wastewater, the temperature of the negative pressure reaction in the step (2) is 40-80 ℃, and the vacuum degree of the negative pressure reaction is-0.07-0.09 Mpa.
In the method for treating high-salt high-ammonia nitrogen wastewater, the ammonia nitrogen content in the reaction solution after the reflux reaction is 100-300 mg/L, and the COD is 500-1000 mg/L.
In the method for treating high-salt high-ammonia nitrogen wastewater, the content of ammonia nitrogen in reaction liquid after the negative pressure reaction is finished is 0-100 mg/L, and the COD is 0-500 mg/L.
The invention has the beneficial effects that:
firstly, through reflux reaction and negative pressure reaction under alkaline condition, ammonia nitrogen and COD are reduced, the process is simple and effective, the operation is convenient, and the cost is low; secondly, the low-boiling-point organic solvent is separated by tail gas absorption and cooling, and an ammonia water solution is prepared at the same time, so that resource utilization is realized; thirdly, separating zinc magnesium salt and sodium potassium salt, and further purifying and recycling; fourthly, the distilled water is recovered by reduced pressure distillation so as to realize recycling; controlling and reducing the total amount of discharged wastewater, separating and utilizing all components in the wastewater, and realizing clean production.
The high-salt high-ammonia nitrogen wastewater treatment method firstly reduces ammonia nitrogen and COD through alkali addition reflux reaction and negative pressure reaction, tail gas absorbs a generated low-boiling-point organic solvent through a cold trap, ammonia gas generated by the reaction is absorbed through water or dilute ammonia water to prepare concentrated ammonia water, recycling is realized, and the dilute ammonia water finally obtained by the negative pressure reaction can be applied to the reflux reaction for absorbing the ammonia gas, so that resources are saved, and the cost is reduced; then cooling and filtering the reaction liquid, and separating solid zinc magnesium salt, wherein the filtrate is sodium potassium salt solution; and (3) after the pH value of the filtrate is adjusted, carrying out reduced pressure distillation to recover distilled water, filtering the residual solid-liquid mixture, recovering sodium potassium salt, mechanically applying the filtrate to the wastewater of the next batch, and finally treating the wastewater in a sewage system to realize standard discharge.
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FIG. 1 is a process flow diagram of an embodiment of the present invention.
Detailed Description
Example 1
The flow of the high-salinity high-ammonia-nitrogen wastewater treatment method provided by the embodiment is shown in fig. 1, and the method specifically comprises the following steps:
step (1): adding sodium hydroxide solid into the high-salt high-ammonia nitrogen wastewater, carrying out reflux reaction at the temperature of 90 ℃ for 4h, absorbing tail gas after the reflux reaction by a cold trap to generate a low-boiling-point organic solvent, and absorbing ammonia gas generated by the reaction by water or dilute ammonia water to prepare concentrated ammonia water;
the ammonia nitrogen content in the high-salt high-ammonia nitrogen wastewater is 58400mg/L, the COD is 19600mg/L, and the pH value is 12;
the weight ratio of the amount of sodium hydroxide to the amount of wastewater is 1: 30;
step (2): after the reflux reaction is finished, the ammonia nitrogen content in the reaction liquid is 200mg/L, the COD is 800mg/L, the reaction liquid is cooled to the required temperature, the temperature of the negative pressure reaction is 65-70 ℃, the vacuum degree of the negative pressure reaction is-0.07 to-0.09 Mpa, the tail gas after the negative pressure reaction is absorbed by a cold trap to generate a low-boiling-point organic solvent, then ammonia gas generated by the water absorption reaction is used for preparing dilute ammonia water, and the dilute ammonia water is applied to the step (1) to absorb the ammonia gas generated by the reaction;
cooling and separating the organic solvent by tail gas of the reflux reaction and the negative pressure reaction through a cold trap;
and (3): after the negative pressure reaction is finished, the content of ammonia nitrogen in the reaction liquid is 50mg/L, the COD is 350mg/L, the reaction liquid is cooled to room temperature, and the reaction liquid is filtered and washed to realize solid-liquid separation, wherein a filter cake is zinc magnesium salt, and a filtrate is mainly sodium potassium salt solution;
and (4): and (4) regulating the pH value of the filtrate obtained in the step (3) to 6-7 by using hydrochloric acid, carrying out reduced pressure distillation to recover distilled water, cooling and filtering the residual solid-liquid mixture, recovering sodium potassium salt of a filter cake, mechanically applying the filtered filtrate to next batch of high-salt high-ammonia nitrogen wastewater, treating according to the method provided by the invention, and finally, treating in a sewage system to realize standard discharge.
Example 2
The flow of the high-salinity high-ammonia-nitrogen wastewater treatment method provided by the embodiment is shown in fig. 1, and the method specifically comprises the following steps:
step (1): adding sodium hydroxide solid into the high-salt high-ammonia nitrogen wastewater, carrying out reflux reaction at the temperature of 100 ℃ for 6h, absorbing tail gas after the reflux reaction by a cold trap to generate a low-boiling-point organic solvent, and absorbing ammonia gas generated by the reaction by water or dilute ammonia water to prepare concentrated ammonia water;
the ammonia nitrogen content in the high-salt high-ammonia nitrogen wastewater is 58400mg/L, the COD is 19600mg/L, and the pH value is 12;
the weight ratio of the amount of sodium hydroxide to the amount of wastewater is 1: 25;
step (2): after the reflux reaction is finished, the content of ammonia nitrogen in reaction liquid is 150mg/L, the COD is 600mg/L, the reaction liquid is cooled to the required temperature, the temperature of the negative pressure reaction is 65-70 ℃, the vacuum degree of the negative pressure reaction is-0.07 to-0.09 Mpa, tail gas after the negative pressure reaction is absorbed by a cold trap to generate a low-boiling-point organic solvent, ammonia gas generated by the water absorption reaction is used for preparing dilute ammonia water, and the dilute ammonia water is applied to the step (1) to absorb the ammonia gas generated by the reaction;
cooling and separating the organic solvent by tail gas of the reflux reaction and the negative pressure reaction through a cold trap;
and (3): after the negative pressure reaction is finished, the content of ammonia nitrogen in the reaction liquid is 35mg/L, the COD is 250mg/L, the reaction liquid is cooled to room temperature, and is filtered and washed to realize solid-liquid separation, wherein the filter cake is zinc magnesium salt filtrate which is mainly sodium sylvite solution;
and (4): and (4) regulating the pH value of the filtrate obtained in the step (3) to 6-7 by using hydrochloric acid, carrying out reduced pressure distillation to recover distilled water, cooling and filtering the residual solid-liquid mixture, recovering sodium potassium salt of a filter cake, mechanically applying the filtered filtrate to next batch of high-salt high-ammonia nitrogen wastewater, treating according to the method provided by the invention, and finally, treating in a sewage system to realize standard discharge.
Example 3
The flow of the high-salinity high-ammonia-nitrogen wastewater treatment method provided by the embodiment is shown in fig. 1, and the method specifically comprises the following steps:
step (1): respectively adding the filtrate and sodium hydroxide solid after the treatment in the step (4) in the embodiment 2 into the high-salt high-ammonia nitrogen wastewater, carrying out reflux reaction at the temperature of 100 ℃ for 6h, absorbing tail gas after the reflux reaction by a cold trap to generate a low-boiling-point organic solvent, and absorbing ammonia gas generated by the reaction by water or dilute ammonia water to prepare concentrated ammonia water;
the ammonia nitrogen content of the high-salt high ammonia nitrogen wastewater is 65200mg/L, the COD is 24800mg/L, and the pH value is 12;
the weight ratio of the amount of sodium hydroxide to the amount of wastewater is 1: 25;
step (2): after the reflux reaction is finished, the ammonia nitrogen content in the reaction liquid is 180mg/L, the COD is 720mg/L, the reaction liquid is cooled to the required temperature, the temperature of the negative pressure reaction is 65-70 ℃, the vacuum degree of the negative pressure reaction is-0.07 to-0.09 Mpa, the tail gas after the negative pressure reaction is absorbed by a cold trap to generate a low-boiling-point organic solvent, then ammonia gas generated by the water absorption reaction is used for preparing dilute ammonia water, and the dilute ammonia water is applied to the step (1) to absorb the ammonia gas generated by the reaction;
cooling and separating the organic solvent by tail gas of the reflux reaction and the negative pressure reaction through a cold trap;
and (3): after the negative pressure reaction is finished, the content of ammonia nitrogen in the reaction liquid is 40mg/L, the COD is 310mg/L, the reaction liquid is cooled to room temperature, and is filtered and washed to realize solid-liquid separation, wherein the filter cake is zinc magnesium salt filtrate which is mainly sodium potassium salt solution;
and (4): and (4) regulating the pH value of the filtrate obtained in the step (3) to 6-7 by using hydrochloric acid, carrying out reduced pressure distillation to recover distilled water, cooling and filtering the residual solid-liquid mixture, recovering sodium potassium salt of a filter cake, mechanically applying the filtered filtrate to next batch of high-salt high-ammonia nitrogen wastewater, treating according to the method provided by the invention, and finally, treating in a sewage system to realize standard discharge.
In addition to the above embodiments, the present invention may have other embodiments. All technical solutions formed by adopting equivalent substitutions or equivalent transformations fall within the protection scope of the claims of the present invention.
Claims (7)
1. A method for treating high-salt high-ammonia nitrogen wastewater is characterized by comprising the following steps: the method specifically comprises the following steps:
step (1): adding sodium hydroxide solid into the wastewater, carrying out reflux reaction, absorbing tail gas after the reflux reaction by a cold trap to generate a low-boiling-point organic solvent, and absorbing ammonia gas generated by the reaction by water or dilute ammonia water to prepare concentrated ammonia water;
step (2): after the reflux reaction is finished, cooling the reaction liquid to the required temperature, carrying out heat preservation and negative pressure reaction, absorbing tail gas after the negative pressure reaction by a cold trap to generate a low-boiling-point organic solvent, absorbing ammonia gas generated by the reaction by water to prepare dilute ammonia water, and applying the dilute ammonia water to the step (1) for absorbing the ammonia gas generated by the reaction;
and (3): after the negative pressure reaction is finished, cooling the reaction liquid to room temperature, filtering and washing to realize solid-liquid separation, wherein a filter cake is zinc-magnesium salt;
and (4): and (4) adjusting the pH value of the filtrate obtained in the step (3) to 6-7 by using hydrochloric acid, carrying out reduced pressure distillation to recover distilled water, cooling and filtering the residual solid-liquid mixture, recovering sodium potassium salt of a filter cake, mechanically applying the filtered filtrate to the wastewater of the next batch, and finally treating the wastewater in a sewage system to achieve standard discharge.
2. The method for treating high-salinity high-ammonia-nitrogen wastewater according to claim 1, characterized by comprising the following steps: the ammonia nitrogen content of the high-salt high-ammonia nitrogen wastewater is 10000-100000 mg/L, the COD is 10000-100000 mg/L, and the pH value is 10-14.
3. The method for treating high-salinity high-ammonia-nitrogen wastewater according to claim 1, characterized by comprising the following steps: the weight ratio of the amount of the sodium hydroxide to the amount of the wastewater is 1 (10-100).
4. The method for treating high-salinity high-ammonia-nitrogen wastewater according to claim 1, characterized by comprising the following steps: the temperature of the reflux reaction in the step (1) is 80-110 ℃, and the time of the reflux reaction is 1-10 h.
5. The method for treating high-salinity high-ammonia-nitrogen wastewater according to claim 1, characterized by comprising the following steps: in the step (2), the temperature of the negative pressure reaction is 40-80 ℃, and the vacuum degree of the negative pressure reaction is-0.07 to-0.09 Mpa.
6. The method for treating high-salinity high-ammonia-nitrogen wastewater according to claim 1, characterized by comprising the following steps: the ammonia nitrogen content of the reaction liquid after the reflux reaction is 100-300 mg/L, and the COD is 500-1000 mg/L.
7. The method for treating high-salinity high-ammonia-nitrogen wastewater according to claim 1, characterized by comprising the following steps: the content of ammonia nitrogen in the reaction liquid after the negative pressure reaction is 0-100 mg/L, and the COD is 0-500 mg/L.
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| CN1721344A (en) * | 2004-07-15 | 2006-01-18 | 中国科学院成都有机化学有限公司 | Process for treating and recovering wastewater of coking |
| CN103382067A (en) * | 2013-04-15 | 2013-11-06 | 北京中亿孚佑科技有限公司 | Novel method of coking residual ammoniacal liquor deamination, dephenolization, denitrification and utilization |
| CN206635062U (en) * | 2017-02-24 | 2017-11-14 | 上海东硕环保科技股份有限公司 | A kind of phenol ammonia waste water low-temperature evaporation treatment combined device |
| CN207016620U (en) * | 2017-06-28 | 2018-02-16 | 苏州山水源环保科技有限公司 | A kind of ammonia nitrogen and high salinity waste water processing system |
| CN107758960A (en) * | 2017-10-18 | 2018-03-06 | 江苏理工学院 | A kind of processing method of ammonia waste water |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1721344A (en) * | 2004-07-15 | 2006-01-18 | 中国科学院成都有机化学有限公司 | Process for treating and recovering wastewater of coking |
| CN103382067A (en) * | 2013-04-15 | 2013-11-06 | 北京中亿孚佑科技有限公司 | Novel method of coking residual ammoniacal liquor deamination, dephenolization, denitrification and utilization |
| CN206635062U (en) * | 2017-02-24 | 2017-11-14 | 上海东硕环保科技股份有限公司 | A kind of phenol ammonia waste water low-temperature evaporation treatment combined device |
| CN207016620U (en) * | 2017-06-28 | 2018-02-16 | 苏州山水源环保科技有限公司 | A kind of ammonia nitrogen and high salinity waste water processing system |
| CN107758960A (en) * | 2017-10-18 | 2018-03-06 | 江苏理工学院 | A kind of processing method of ammonia waste water |
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