CN103359802A - Method and device for recovering ammonia from nitrochlorobenzene ammonolysis wastewater - Google Patents
Method and device for recovering ammonia from nitrochlorobenzene ammonolysis wastewater Download PDFInfo
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- CN103359802A CN103359802A CN2012100866170A CN201210086617A CN103359802A CN 103359802 A CN103359802 A CN 103359802A CN 2012100866170 A CN2012100866170 A CN 2012100866170A CN 201210086617 A CN201210086617 A CN 201210086617A CN 103359802 A CN103359802 A CN 103359802A
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- ammonia
- waste water
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- nitroxyl chloride
- phenylamino
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Abstract
The invention discloses a method and device for recovering ammonia from nitrochlorobenzene ammonolysis wastewater. According to the method, ammonolysis wastewater is evaporated by using ammonia distilling equipment so as to liberate free ammonia; or an alkaline substance is added firstly so as to convert ammonium ions in the ammonolysis wastewater into the free ammonia, and then, evaporation is carried out; the free ammonia in vapor is absorbed by water, then returns to a material proportioning process of nitrochlorobenzene ammonolysis and is cyclically reused in a manner of serving as an ammonolysis raw material; and then, the treated wastewater is subjected to electrolysis and catalytic oxidation treatment and ammonium chloride recovery. Compared with the prior art, the method and the device have the advantages that the free ammonia is recovered and utilized in a cycling manner, so that the consumption of ammonia is reduced; after the free ammonia is recovered, the consumption of neutralizing acid is reduced, the volume of the wastewater is reduced, and the load of the sewage treatment device is reduced; and by adopting the method and the device, the recovery ratio of ammonia and ammonium chloride can be adjusted randomly according to the market price of liquid ammonia and ammonium chloride.
Description
Technical field
The present invention relates to recovery method and the device of ammonia in a kind of nitroxyl chloride phenylamino solution waste water, belong to technical field of waste water processing.
Background technology
In nitroxyl chloride phenylamino solution, owing to used excess of ammonia, and after reaction, generated ammonium chloride.Therefore, after centrifugation and washing, contain free ammonia and the ammonium chloride of higher concentration in the waste water, and a small amount of nitro-chlorobenzene and N-methyl-p-nitroaniline.The treatment process of nitroxyl chloride phenylamino solution waste water is at present: adopt first the organism such as device for sewage treatment by electrolysis degraded nitro-chlorobenzene and N-methyl-p-nitroaniline; Retrieving arrangement with ammonium chloride reclaims ammonium chloride again.After adopting this method to process, but ammonia nitrogen qualified discharge in the waste water.But before entering electrolysis-catalytic oxidation device, waste water must be weakly acidic, and contains excessive free ammonia in the ammonia solution waste water, forms a buffer system with ammonium chloride, and therefore it is neutralized into slightly acidic need to consume a large amount of acid.
Summary of the invention
The object of the invention is to, recovery method and the device of ammonia in a kind of nitroxyl chloride phenylamino solution waste water is provided, to overcome the deficiency of present ammonia solution method of wastewater treatment, reduce consuming, improve the comprehensive utilization ratio of ammonia.
Technical scheme of the present invention: the recovery method of ammonia is in the nitroxyl chloride phenylamino solution waste water: ammonia solution waste water is evaporated with ammonia still process equipment, free ammonia is wherein overflowed; Perhaps add first after alkaline matter is converted into free ammonia with the ammonium ion in the ammonia solution waste water, evaporate again; After absorbing, free ammonia water in the steam returns the burden process of nitroxyl chloride phenylamino solution, as ammonia solution raw material cyclically utilizing.
In the preceding method, described evaporation is that waste water is heated to boiling, keeps boiling time 4～10h; Be preferably 8～10h.
In the preceding method, described alkaline matter is calcium oxide, calcium hydroxide or sodium hydroxide.
The retrieving arrangement of ammonia is in the nitroxyl chloride phenylamino solution waste water that the above method adopts: nitroxyl chloride phenylamino solution device is connected with ammonia still process equipment through waste pipe; Ammonia still process equipment links to each other with the water absorption tower through pipeline, and the water absorption tower links to each other with material-compound tank in the nitroxyl chloride phenylamino solution device.
In the aforementioned means, also be arranged in parallel the tank that responds between nitroxyl chloride phenylamino solution device and the ammonia still process equipment.
Ammonia still process equipment described in the aforementioned means is preferably vacuum-evaporator.
Compared with prior art, the present invention has the following advantages:
1, recycling free ammonia has reduced the consumption of ammonia, makes the ammonia consumption drop to 0.3 from original 0.6.
2, reclaim free ammonia in advance after, greatly reduced ammonia solution waste water be neutralized into weakly acidic sour consumption, reduced consumption.
3, reclaim free ammonia in advance after, wastewater flow rate reduces, and has alleviated the load of waste disposal plant.
4, adopt method provided by the invention and device, can adjust flexibly according to the market value of liquefied ammonia and ammonium chloride the recovery ratio of ammonia and ammonium chloride.
Description of drawings
Fig. 1 is the recovery process flow sheet of ammonia in the nitroxyl chloride phenylamino solution waste water of the present invention;
Fig. 2 is the retrieving arrangement synoptic diagram of ammonia in the nitroxyl chloride phenylamino solution waste water of the present invention; 1-nitroxyl chloride phenylamino solution device wherein, 2-retort, 3-ammonia still process equipment, 4-water absorption tower, 5-material-compound tank.
Embodiment
Embodiments of the invention 1: when needs improve the recovery ratio of ammonia, the recovery method of ammonia in the nitroxyl chloride phenylamino solution waste water: add sodium hydroxide in the waste water that produces after the nitroxyl chloride phenylamino solution, make ammonium ion wherein change into free ammonia, send into vacuum-evaporator, waste water is heated to boiling, keep boiling time 8～10h, free ammonia is wherein overflowed; After absorbing, free ammonia water in the steam returns the burden process of nitroxyl chloride phenylamino solution, as ammonia solution raw material cyclically utilizing.Ammonia nitrogen in waste water index after this processes can drop to 100ppm.
The retrieving arrangement of ammonia in the nitroxyl chloride phenylamino solution waste water that aforesaid method adopts: comprise retort 2, ammonia still process equipment 3 and water absorption tower 4, nitroxyl chloride phenylamino solution device 1 is connected with ammonia still process equipment 3 through waste pipe; Also be arranged in parallel the tank 2 that responds between nitroxyl chloride phenylamino solution device 1 and the ammonia still process equipment 3; Ammonia still process equipment 3 links to each other with water absorption tower 4 through pipeline, and water absorption tower 4 links to each other with material-compound tank 5 in the nitroxyl chloride phenylamino solution device 1.Ammonia still process equipment 3 can adopt vacuum-evaporator.
Embodiments of the invention 2: when needs improve the recovery ratio of ammonia, the recovery method of ammonia in the nitroxyl chloride phenylamino solution waste water: add calcium oxide or calcium hydroxide in the waste water that produces after the nitroxyl chloride phenylamino solution, make ammonium ion wherein change into free ammonia, send into vacuum-evaporator, waste water is heated to boiling, keep boiling time 6～8h, free ammonia is wherein overflowed; After absorbing, free ammonia water in the steam returns the burden process of nitroxyl chloride phenylamino solution, as ammonia solution raw material cyclically utilizing.Ammonia nitrogen in waste water index after this processes can drop to 400ppm.
The retrieving arrangement of ammonia is with embodiment 1 in the nitroxyl chloride phenylamino solution waste water that the method adopts.
In above-described embodiment, ammonium ion is changed into free ammonia, is not limited in and uses sodium hydroxide or calcium oxide, calcium hydroxide, with other alkaloids also can, be the cost difference.
Embodiments of the invention 3: when needs improve the recovery ratio of ammonium chloride, the recovery method of ammonia in the nitroxyl chloride phenylamino solution waste water: the waste water that produces after the nitroxyl chloride phenylamino solution is directly sent into ammonia still process equipment, waste water is heated to boiling, keeps boiling time 4～5h, free ammonia is wherein overflowed; After absorbing, free ammonia water in the steam returns the burden process of nitroxyl chloride phenylamino solution, as ammonia solution raw material cyclically utilizing.Ammonia nitrogen in waste water index after this processes can drop to 800ppm.
The retrieving arrangement of ammonia in the nitroxyl chloride phenylamino solution waste water that the method adopts: comprise ammonia still process equipment 3 and water absorption tower 4, nitroxyl chloride phenylamino solution device 1 is connected with ammonia still process equipment 3 through waste pipe; Ammonia still process equipment 3 links to each other with water absorption tower 4 through pipeline, and water absorption tower 4 links to each other with material-compound tank 5 in the nitroxyl chloride phenylamino solution device 1.Ammonia still process equipment 3 can adopt vacuum-evaporator.
Claims (7)
1. the recovery method of ammonia in the nitroxyl chloride phenylamino solution waste water is characterized in that: ammonia solution waste water is evaporated with ammonia still process equipment, free ammonia is wherein overflowed; Perhaps add first after alkaline matter is converted into free ammonia with the ammonium ion in the ammonia solution waste water, evaporate again; After absorbing, free ammonia water in the steam returns the burden process of nitroxyl chloride phenylamino solution.
2. the recovery method of ammonia in the described nitroxyl chloride phenylamino solution waste water according to claim 1, it is characterized in that: described evaporation is that waste water is heated to boiling, keeps boiling time 4～10h.
3. the recovery method of ammonia in the described nitroxyl chloride phenylamino solution waste water according to claim 2, it is characterized in that: keeping boiling time is 8～10h.
4. the recovery method of ammonia in the described nitroxyl chloride phenylamino solution waste water according to claim 1, it is characterized in that: described alkaline matter is calcium oxide, calcium hydroxide or sodium hydroxide.
5. the retrieving arrangement of ammonia in the nitroxyl chloride phenylamino solution waste water that each described method adopts among the claim 1-4, it is characterized in that: nitroxyl chloride phenylamino solution device (1) is connected with ammonia still process equipment (3) through waste pipe; Ammonia still process equipment (3) links to each other with water absorption tower (4) through pipeline, and water absorption tower (4) link to each other with material-compound tank (5) in the nitroxyl chloride phenylamino solution device (1).
6. the retrieving arrangement of ammonia in the nitroxyl chloride phenylamino solution waste water according to claim 5 is characterized in that: be arranged in parallel the tank that responds (2) between nitroxyl chloride phenylamino solution device (1) and the ammonia still process equipment (3).
7. the retrieving arrangement of ammonia according to claim 5 or in the 6 described nitroxyl chloride phenylamino solution waste water, it is characterized in that: described ammonia still process equipment (3) is vacuum-evaporator.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012100866170A CN103359802A (en) | 2012-03-28 | 2012-03-28 | Method and device for recovering ammonia from nitrochlorobenzene ammonolysis wastewater |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012100866170A CN103359802A (en) | 2012-03-28 | 2012-03-28 | Method and device for recovering ammonia from nitrochlorobenzene ammonolysis wastewater |
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| CN103359802A true CN103359802A (en) | 2013-10-23 |
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| CN2012100866170A Pending CN103359802A (en) | 2012-03-28 | 2012-03-28 | Method and device for recovering ammonia from nitrochlorobenzene ammonolysis wastewater |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103626251A (en) * | 2013-12-04 | 2014-03-12 | 彭传义 | Three-phase azeotropic ammonia removal method |
| CN109320031A (en) * | 2018-10-19 | 2019-02-12 | 天津渤化永利化工股份有限公司 | A kind of method of ammonia II mud processing in alkali production process |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4689156A (en) * | 1985-11-12 | 1987-08-25 | Amax Inc. | Removal of ammonia from wastewater |
| CN101259967A (en) * | 2008-03-06 | 2008-09-10 | 马永伟 | Vacuum ammonia distillation technique |
| CN201148353Y (en) * | 2007-11-06 | 2008-11-12 | 金川集团有限公司 | Apparatus for reclaiming ammonia from ammonia-containing waste water |
| CN101696062A (en) * | 2009-10-24 | 2010-04-21 | 刘向文 | Treatment process for waster water from preparation of ammonium paratungstate |
| CN101941720A (en) * | 2010-08-23 | 2011-01-12 | 天津市创举科技有限公司 | Tube furnace ammonia evaporation process and equipment |
-
2012
- 2012-03-28 CN CN2012100866170A patent/CN103359802A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4689156A (en) * | 1985-11-12 | 1987-08-25 | Amax Inc. | Removal of ammonia from wastewater |
| CN201148353Y (en) * | 2007-11-06 | 2008-11-12 | 金川集团有限公司 | Apparatus for reclaiming ammonia from ammonia-containing waste water |
| CN101259967A (en) * | 2008-03-06 | 2008-09-10 | 马永伟 | Vacuum ammonia distillation technique |
| CN101696062A (en) * | 2009-10-24 | 2010-04-21 | 刘向文 | Treatment process for waster water from preparation of ammonium paratungstate |
| CN101941720A (en) * | 2010-08-23 | 2011-01-12 | 天津市创举科技有限公司 | Tube furnace ammonia evaporation process and equipment |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103626251A (en) * | 2013-12-04 | 2014-03-12 | 彭传义 | Three-phase azeotropic ammonia removal method |
| CN109320031A (en) * | 2018-10-19 | 2019-02-12 | 天津渤化永利化工股份有限公司 | A kind of method of ammonia II mud processing in alkali production process |
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Application publication date: 20131023 |