CN103922380B - A kind of recovery method of pyrazolone factory effluent - Google Patents
A kind of recovery method of pyrazolone factory effluent Download PDFInfo
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- CN103922380B CN103922380B CN201410188082.7A CN201410188082A CN103922380B CN 103922380 B CN103922380 B CN 103922380B CN 201410188082 A CN201410188082 A CN 201410188082A CN 103922380 B CN103922380 B CN 103922380B
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Abstract
The invention provides a kind of recovery method of pyrazolone factory effluent, comprise the following steps: 1), by pyrazolone factory effluent and calcium oxide carry out replacement(metathesis)reaction, obtain reaction soln; Described pyrazolone factory effluent comprises the ammonium sulfate of mass percent >=20%; 2), by described reaction soln carry out stripping process, obtain gas mixture and feed liquid; Described gas mixture comprises ammonia and water vapour, and described feed liquid comprises calcium sulfate.The recovery method of pyrazolone factory effluent provided by the invention can reclaim the gas mixture and the calcium sulfate that obtain ammonia and water vapour from pyrazolone factory effluent, ammonia and calcium sulfate have higher using value and economic benefit, compared with prior art, the recovery method of pyrazolone factory effluent provided by the invention has good economy.
Description
Technical field
The present invention relates to pyrazolone technical field, particularly relate to a kind of recovery method of pyrazolone factory effluent.
Background technology
Containing pyrazolone structure in the molecule of pyrazolone, and there is azo-group.Pyrazolone can be used for preparing azo dyes, such as the production of bordeaux dyestuff, acid red dye, orange dye, tracid light yellow dyestuff; Pyrazolone also can be used for pharmaceutical synthesis, such as the production of quinizine, pyramidon and Sulpyrine; Pyrazolone also can be used for organic synthesis, such as the preparation of 1-phenyl-3-methyl-5-pyrazolones ketone and 1-p-sulfonic acid phenyl-3-methyl-5-pyrazolone.In addition, pyrazolone can be used as the chemical reagent detecting CO, vitamin B12, Fe, Cu and Ni.
The production process of pyrazolone is for carrying out watering down reaction by water, hydrochloric acid, aniline and Sodium Nitrite, in the reaction product obtained, add sulfuric acid be hydrolyzed, in the product that hydrolysis obtains, pass into ammoniacal liquor carry out neutralization reaction, the neutralization reaction product obtained and Butanonamide are carried out condensation reaction, obtains pyrazolone product.In pyrazolone production process, need to add a large amount of ammoniacal liquor carry out neutralization reaction, but the ammoniacal liquor added finally is not introduced in the product of pyrazolone, but be all dissolved in the factory effluent of pyrazolone, make containing a large amount of ammonia, nitrogen in the factory effluent of pyrazolone, the ammonia in pyrazolone factory effluent, nitrogen cannot effectively utilize the waste causing resource; And the pH value of pyrazolone factory effluent lower being difficult to processes, if be directly discharged in environment by pyrazolone factory effluent, serious problem of environmental pollution can be caused.Therefore, how the concern receiving people is reclaimed to pyrazolone factory effluent.
General by carrying out straight run distillation to pyrazolone factory effluent to reclaim the ammonium sulfate in pyrazolone factory effluent at present.But the ammonium sulfate purity that this recovery method obtains is lower, be difficult to utilize; And the price of ammonium sulfate is cheap, compared to high cost recovery, this recovery method causes very large economical load to enterprise.The recovery method economy of the pyrazolone factory effluent that prior art provides is poor.
Summary of the invention
In view of this, the object of the present invention is to provide a kind of recovery method of pyrazolone factory effluent, the recovery method of pyrazolone factory effluent provided by the invention can reclaim the gas mixture and the calcium sulfate that obtain ammonia and water vapour from pyrazolone factory effluent, and this recovery method has good economy.
The invention provides a kind of recovery method of pyrazolone factory effluent, comprise the following steps:
1), by pyrazolone factory effluent and calcium oxide carry out replacement(metathesis)reaction, obtain reaction soln; Described pyrazolone factory effluent comprises the ammonium sulfate of mass percent >=20%;
2), by described reaction soln carry out stripping process, obtain gas mixture and feed liquid, described gas mixture comprises ammonia and water vapour, and described feed liquid comprises calcium sulfate.
Preferably, described step 1) in the mass ratio of pyrazolone factory effluent and calcium oxide be (45 ~ 55): 1.
Preferably, described step 1) in the temperature of replacement(metathesis)reaction be 20 DEG C ~ 30 DEG C.
Preferably, described step 1) in time of replacement(metathesis)reaction be 2 hours ~ 4 hours.
Preferably, described step 1) in the pH value of reaction soln be 11 ~ 14.
Preferably, described step 2) in the temperature of stripping process be 50 DEG C ~ 65 DEG C.
Preferably, described step 2) in the pressure >=2MPa of stripping process.
Preferably, described step 2) mass ratio of ammonia and water vapour is (20 ~ 25) in gas mixture: (75 ~ 80).
Preferably, also comprising described step 2) gas mixture that obtains carries out condensation process, obtains ammoniacal liquor.
The ammoniacal liquor that described in the gas mixture that method described in technique scheme obtains by the present invention or technique scheme, method obtains is for the preparation of pyrazolone.
The invention provides a kind of recovery method of pyrazolone factory effluent, comprise the following steps: 1), by pyrazolone factory effluent and calcium oxide carry out replacement(metathesis)reaction, obtain reaction soln; Described pyrazolone factory effluent comprises the ammonium sulfate of mass percent >=20%; 2), by described reaction soln carry out stripping process, obtain gas mixture and feed liquid, described gas mixture comprises ammonia and water vapour, and described feed liquid comprises calcium sulfate.The recovery method of pyrazolone factory effluent provided by the invention can reclaim the gas mixture and the calcium sulfate that obtain ammonia and water vapour from pyrazolone factory effluent, ammonia and calcium sulfate have higher using value and economic benefit, compared with prior art, the recovery method of pyrazolone factory effluent provided by the invention has good economy.
In addition, the recovery method of pyrazolone factory effluent provided by the invention, while reclaiming the gas mixture and calcium sulfate obtaining ammonia and water vapour, also processes pyrazolone factory effluent, reduces the pollution of pyrazolone factory effluent.Experimental result shows, the present invention reclaims from pyrazolone factory effluent that the pH value of remaining liquid after the gas mixture of ammonia and water vapour and calcium sulfate is 13 ~ 14, chemical oxygen demand (COD) is 4000 ~ 4700, the mass percent of nitrogen is 0.33% ~ 0.4%.
Embodiment
The invention provides a kind of recovery method of pyrazolone factory effluent, comprise the following steps:
1), by pyrazolone factory effluent and calcium oxide carry out replacement(metathesis)reaction, obtain reaction soln; Described pyrazolone factory effluent comprises the ammonium sulfate of mass percent >=20%;
2), by described reaction soln carry out stripping process, obtain gas mixture and feed liquid, described gas mixture comprises ammonia and water vapour, and described feed liquid comprises calcium sulfate.
The recovery method of pyrazolone factory effluent provided by the invention can reclaim the gas mixture and the calcium sulfate that obtain ammonia and water vapour from pyrazolone factory effluent, ammonia and calcium sulfate have higher using value and economic benefit, compared with prior art, the recovery method of pyrazolone factory effluent provided by the invention has good economy.In addition, the recovery method of pyrazolone factory effluent provided by the invention, while reclaiming the gas mixture and calcium sulfate obtaining ammonia and water vapour, also processes pyrazolone factory effluent, reduces the pollution of pyrazolone factory effluent.
Pyrazolone factory effluent and calcium oxide are carried out replacement(metathesis)reaction by the present invention, obtain reaction soln; Described pyrazolone factory effluent comprises the ammonium sulfate of mass percent >=20%.Calcium oxide preferably joins in pyrazolone factory effluent and carries out replacement(metathesis)reaction by the present invention, obtains reaction soln.The present invention preferably carries out described replacement(metathesis)reaction under the condition stirred.The method of the present invention to described stirring does not have special restriction, adopts stirring technique scheme well known to those skilled in the art.In the present invention, the temperature of described replacement(metathesis)reaction is preferably 20 DEG C ~ 30 DEG C, is more preferably 24 DEG C ~ 28 DEG C.In the present invention, the time of described replacement(metathesis)reaction is preferably 2 hours ~ 4 hours, is more preferably 2.5 hours ~ 3 hours.
In the present invention, described pyrazolone factory effluent is produce the waste water produced in pyrazolone process.In the present invention, described pyrazolone factory effluent comprises the ammonium sulfate of mass percent >=20%, preferably includes the ammonium sulfate of 20% ~ 25%.In the present invention, the pH value of described pyrazolone factory effluent is preferably 2 ~ 4, is more preferably 2.5 ~ 3.In the present invention, in described pyrazolone factory effluent, the mass percent of nitrogen is preferably 5% ~ 15%, is more preferably 8% ~ 10%.The source of the present invention to described pyrazolone factory effluent does not have special restriction, and can carry out press filtration to the pyrazolone crude product obtained in pyrazolone production process, the filtrate obtained after press filtration is pyrazolone factory effluent.The filter-pressing method of the present invention to described pyrazolone crude product does not have special restriction, and pressure filter can be adopted to carry out press filtration.
In order to accelerate the speed of above-mentioned replacement(metathesis)reaction, in the present invention, described calcium oxide is preferably Powdered calcium oxide.The source of the present invention to described calcium oxide does not have special restriction, can be bought obtain by market.
In the present invention, the mass ratio of described pyrazolone factory effluent and calcium oxide is preferably (45 ~ 55): 1, is more preferably (47 ~ 52): 1, most preferably is (48 ~ 50): 1.In the present invention, the pH value of described reaction soln is preferably 11 ~ 14, is more preferably 12 ~ 13.
After obtaining reaction soln, described reaction soln is carried out stripping process by the present invention, obtains gas mixture and feed liquid, and described gas mixture comprises ammonia and water vapour, and described feed liquid comprises calcium sulfate.The equipment of the present invention to described stripping process does not have special restriction, and in an embodiment of the present invention, the equipment of described stripping process can be ammonia still.In the present invention, the temperature of described stripping process is preferably 50 DEG C ~ 65 DEG C, is more preferably 55 DEG C ~ 60 DEG C.Replacement(metathesis)reaction liberated heat described in technique scheme preferably collects to carry out stripping process by the present invention, makes the temperature of described stripping process reach said temperature, makes the recovery method of pyrazolone factory effluent provided by the invention save the energy.In the present invention, the pressure of described stripping process preferably >=2MPa, be more preferably 3MPa ~ 8MPa, most preferably be 4MPa ~ 6MPa.In the present invention, in described gas mixture, the mass ratio of ammonia and water vapour is preferably (20 ~ 25): (75 ~ 80), are more preferably (22 ~ 24): (76 ~ 78).The present invention makes the mass ratio of ammonia and water vapour in described gas mixture meet above-mentioned requirements by regulating the intake of water vapour in above-mentioned stripping process.The present invention isolates ammonia by stripping process from above-mentioned reaction soln, described reaction soln after isolating ammonia remaining material be feed liquid.
After obtaining gas mixture, described gas mixture is preferably carried out condensation process by the present invention, obtains ammoniacal liquor.The equipment of the present invention to described condensation process does not have special restriction, in an embodiment of the present invention, pipe bundle condenser can be adopted to carry out described condensation process.In the present invention, the temperature of described condensation process is preferably 20 DEG C ~ 30 DEG C, is more preferably 22 DEG C ~ 26 DEG C.In the present invention, the mass concentration of described ammoniacal liquor is preferably 20% ~ 25%, is more preferably 22% ~ 24%.
The present invention can reclaim the gas mixture obtaining ammonia and water vapour from pyrazolone factory effluent, and the gas mixture of described ammonia and water vapour can be used for preparing pyrazolone.The ammoniacal liquor that technique scheme preferably prepares by the present invention as reaction raw materials in order to prepare pyrazolone.In the present invention, the ammoniacal liquor that technique scheme prepares also can be used as commodity selling.The recovery method of pyrazolone factory effluent provided by the invention has higher economy.
Feed liquid obtained above is preferably filtered by the present invention, obtains calcium sulfate.In the present invention, the method for described filtration is preferably press filtration.In the present invention, the time of described feed liquid press filtration is preferably 1 hour ~ 3 hours, is more preferably 1.5 hours ~ 2.5 hours, most preferably is 2 hours.In the present invention, the pressure of described feed liquid press filtration is preferably 4MPa ~ 7MPa, is more preferably 5MPa ~ 6.5MPa, most preferably is 6MPa.The equipment of the present invention to described feed liquid press filtration does not have special restriction, can carry out press filtration in pressure filter to described feed liquid.The filtrate that the present invention obtains after preferably above-mentioned feed liquid being filtered sends into sewage work's process.The present invention can reclaim and obtain calcium sulfate from pyrazolone factory effluent, and calcium sulfate has higher use value and economic benefit, can be applicable to building trade.The recovery method of pyrazolone factory effluent provided by the invention has higher economy.
The present invention does not have special restriction to the time sequence that the condensation process of above-mentioned gas mixture and feed liquid are filtered, described feed liquid is filtered and can be carried out before the condensation process of above-mentioned gas mixture, also can carry out after the condensation process of above-mentioned gas mixture, can also carry out with the condensation process of above-mentioned gas mixture simultaneously.
The present invention to above-mentioned pyrazolone factory effluent and reclaim the gas mixture of ammonia and water vapour and calcium sulfate from above-mentioned pyrazolone factory effluent after the pH value of remaining liquid, chemical oxygen demand (COD) (COD) and nitrogen content test.In the present invention, described pH value adopts acidometer to test; Described COD adopts dichromate titration to test; Described nitrogen content is tested according to the standard of HJ535-2009 " the mensuration Berthelot spectrophotometry of Water quality ammonia nitrogen ".Test result is, the pH value of above-mentioned pyrazolone factory effluent is 2 ~ 4, COD is 15000 ~ 20000, the mass percent of nitrogen is 5% ~ 15%; From above-mentioned pyrazolone factory effluent, reclaim that the pH value of remaining liquid after the gas mixture of ammonia and water vapour and calcium sulfate is 13 ~ 14, COD is 3000 ~ 5000, the mass percent of nitrogen is 0.2% ~ 0.4%.The present invention, while reclaim the gas mixture and calcium sulfate obtaining ammonia and water vapour from pyrazolone factory effluent, also processes pyrazolone factory effluent, reduces the pollution of pyrazolone factory effluent.
The invention provides a kind of recovery method of pyrazolone factory effluent, comprise the following steps: 1), by pyrazolone factory effluent and calcium oxide carry out replacement(metathesis)reaction, obtain reaction soln; Described pyrazolone factory effluent comprises the ammonium sulfate of mass percent >=20%; 2), by described reaction soln carry out stripping process, obtain gas mixture and feed liquid, described gas mixture comprises ammonia and water vapour, and described feed liquid comprises calcium sulfate; The recovery method of pyrazolone factory effluent provided by the invention can reclaim the gas mixture and the calcium sulfate that obtain ammonia and water vapour from pyrazolone factory effluent, ammonia and calcium sulfate have higher using value and economic benefit, compared with prior art, the recovery method of pyrazolone factory effluent provided by the invention has good economy.In addition, the recovery method of pyrazolone factory effluent provided by the invention, while reclaiming the gas mixture and calcium sulfate obtaining ammonia and water vapour, also processes pyrazolone factory effluent, reduces the pollution of pyrazolone factory effluent.
In order to understand the present invention further; be described in detail below in conjunction with the recovery method of embodiment to pyrazolone factory effluent provided by the invention; but be to be understood that; these describe just in order to further illustrate the features and advantages of the present invention, and they can not be interpreted as limiting the scope of the present invention.
Pyrazolone factory effluent in following examples of the present invention is the filtrate obtained after the pyrazolone crude product obtained in pyrazolone production process is carried out press filtration, and other reaction raw materials are commercial goods.
Embodiment 1
In the reactor of 50000L, add 30000kg pyrazolone factory effluent, the Powdered calcium oxide adding 660kg under the condition stirred in described pyrazolone factory effluent carries out replacement(metathesis)reaction, obtains reaction soln;
Described reaction soln pump is got in ammonia still, in described ammonia still, pass into water vapour, under 2MPa, the condition of 60 DEG C, stripping process is carried out to described reaction soln, control the air flow of water vapour in described stripping process, obtain gas mixture and feed liquid, in described gas mixture, the mass ratio of ammonia and water vapour is 20:80, and described feed liquid comprises calcium sulfate;
By the condensation in the pipe bundle condenser of 20 DEG C of described gas mixture, obtain the ammoniacal liquor that mass concentration is 20%; Using the ammoniacal liquor obtained as reaction raw materials in order to prepare pyrazolone;
By feed liquid obtained above press filtration 2 hours in the pressure filter of 6MPa, obtain calcium sulfate 1800kg, the filtrate obtained after described feed liquid press filtration is delivered to sewage work.
The pH value of the filtrate that the pyrazolone factory effluent that provides of the embodiment of the present invention 1 and embodiment 1 obtain, COD and nitrogen content is detected according to method described in technique scheme.The pH value of the pyrazolone factory effluent that detected result provides for the embodiment of the present invention 1 is 3, COD is 17000, the mass percent of nitrogen is 15.11%; The pH value of the filtrate that embodiment 1 obtains is 14, COD is 4000, the mass percent of nitrogen is 0.33%, the embodiment of the present invention 1 is while from pyrazolone factory effluent, recovery obtains ammoniacal liquor and calcium sulfate, also pyrazolone factory effluent is processed, reduce the pollution of pyrazolone factory effluent.
Embodiment 2
In the reactor of 50000L, add 30000kg pyrazolone factory effluent, the Powdered calcium oxide adding 640kg under the condition stirred in described pyrazolone factory effluent carries out replacement(metathesis)reaction, obtains reaction soln;
Described reaction soln pump is got in ammonia still, in described ammonia still, pass into water vapour, under 3MPa, the condition of 50 DEG C, stripping process is carried out to described reaction soln, control the air flow of water vapour in described stripping process, obtain gas mixture and feed liquid, in described gas mixture, the mass ratio of ammonia and water vapour is 22:78, and described feed liquid comprises calcium sulfate;
By the condensation in the pipe bundle condenser of 22 DEG C of described gas mixture, obtain the ammoniacal liquor that mass concentration is 22%; Using the ammoniacal liquor obtained as reaction raw materials in order to prepare pyrazolone;
By feed liquid obtained above press filtration 1 hour in the pressure filter of 4MPa, obtain calcium sulfate 1745kg, the filtrate obtained after described feed liquid press filtration is delivered to sewage work.
The pH value of the filtrate that the pyrazolone factory effluent that provides of the embodiment of the present invention 2 and embodiment 2 obtain, COD and nitrogen content is detected according to method described in technique scheme.The pH value of the pyrazolone factory effluent that detected result provides for the embodiment of the present invention 2 is 3, COD is 17000, the mass percent of nitrogen is 15.11%; The pH value of the filtrate that embodiment 2 obtains is 13.6, COD is 4200, the mass percent of nitrogen is 0.35%, the embodiment of the present invention 2 is while from pyrazolone factory effluent, recovery obtains ammoniacal liquor and calcium sulfate, also pyrazolone factory effluent is processed, reduce the pollution of pyrazolone factory effluent.
Embodiment 3
In the reactor of 50000L, add 30000kg pyrazolone factory effluent, the Powdered calcium oxide adding 600kg under the condition stirred in described pyrazolone factory effluent carries out replacement(metathesis)reaction, obtains reaction soln;
Described reaction soln pump is got in ammonia still, in described ammonia still, pass into water vapour, under 4MPa, the condition of 55 DEG C, stripping process is carried out to described reaction soln, control the air flow of water vapour in described stripping process, obtain gas mixture and feed liquid, in described gas mixture, the mass ratio of ammonia and water vapour is 24:76, and described feed liquid comprises calcium sulfate;
By the condensation in the pipe bundle condenser of 26 DEG C of described gas mixture, obtain the ammoniacal liquor that mass concentration is 24%; Using the ammoniacal liquor obtained as reaction raw materials in order to prepare pyrazolone;
By feed liquid obtained above press filtration 1.5 hours in the pressure filter of 5MPa, obtain calcium sulfate 1636kg, the filtrate obtained after described feed liquid press filtration is delivered to sewage work.
The pH value of the filtrate that the pyrazolone factory effluent that provides of the embodiment of the present invention 3 and embodiment 3 obtain, COD and nitrogen content is detected according to method described in technique scheme.The pH value of the pyrazolone factory effluent that detected result provides for the embodiment of the present invention 3 is 3, COD is 17000, the mass percent of nitrogen is 15.11%; The pH value of the filtrate that embodiment 3 obtains is 13.2, COD is 4300, the mass percent of nitrogen is 0.38%, the embodiment of the present invention 3 is while from pyrazolone factory effluent, recovery obtains ammoniacal liquor and calcium sulfate, also pyrazolone factory effluent is processed, reduce the pollution of pyrazolone factory effluent.
Embodiment 4
In the reactor of 50000L, add 30000kg pyrazolone factory effluent, the Powdered calcium oxide adding 580kg under the condition stirred in described pyrazolone factory effluent carries out replacement(metathesis)reaction, obtains reaction soln;
Described reaction soln pump is got in ammonia still, in described ammonia still, pass into water vapour, under 6MPa, the condition of 60 DEG C, stripping process is carried out to described reaction soln, control the air flow of water vapour in described stripping process, obtain gas mixture and feed liquid, in described gas mixture, the mass ratio of ammonia and water vapour is 20:80, and described feed liquid comprises calcium sulfate;
By the condensation in the pipe bundle condenser of 30 DEG C of described gas mixture, obtain the ammoniacal liquor that mass concentration is 20%; Using the ammoniacal liquor obtained as reaction raw materials in order to prepare pyrazolone;
By feed liquid obtained above press filtration 2.5 hours in the pressure filter of 6.5MPa, obtain calcium sulfate 1582kg, the filtrate obtained after described feed liquid press filtration is delivered to sewage work.
The pH value of the filtrate that the pyrazolone factory effluent that provides of the embodiment of the present invention 4 and embodiment 4 obtain, COD and nitrogen content is detected according to method described in technique scheme.The pH value of the pyrazolone factory effluent that detected result provides for the embodiment of the present invention 4 is 3, COD is 17000, the mass percent of nitrogen is 15.11%; The pH value of the filtrate that embodiment 4 obtains is 13.1, COD is 4500, the mass percent of nitrogen is 0.39%, the embodiment of the present invention 4 is while from pyrazolone factory effluent, recovery obtains ammoniacal liquor and calcium sulfate, also pyrazolone factory effluent is processed, reduce the pollution of pyrazolone factory effluent.
Embodiment 5
In the reactor of 50000L, add 30000kg pyrazolone factory effluent, the Powdered calcium oxide adding 545kg under the condition stirred in described pyrazolone factory effluent carries out replacement(metathesis)reaction, obtains reaction soln;
Described reaction soln pump is got in ammonia still, in described ammonia still, pass into water vapour, under 8MPa, the condition of 65 DEG C, stripping process is carried out to described reaction soln, control the air flow of water vapour in described stripping process, obtain gas mixture and feed liquid, in described gas mixture, the mass ratio of ammonia and water vapour is 25:75, and described feed liquid comprises calcium sulfate;
By the condensation in the pipe bundle condenser of 28 DEG C of described gas mixture, obtain the ammoniacal liquor that mass concentration is 25%; Using the ammoniacal liquor obtained as reaction raw materials in order to prepare pyrazolone;
By feed liquid obtained above press filtration 3 hours in the pressure filter of 7MPa, obtain calcium sulfate 1486kg, the filtrate obtained after described feed liquid press filtration is delivered to sewage work.
The pH value of the filtrate that the pyrazolone factory effluent that provides of the embodiment of the present invention 5 and embodiment 5 obtain, COD and nitrogen content is detected according to method described in technique scheme.The pH value of the pyrazolone factory effluent that detected result provides for the embodiment of the present invention 5 is 3, COD is 17000, the mass percent of nitrogen is 15.11%; The pH value of the filtrate that embodiment 5 obtains is 13, COD is 4700, the mass percent of nitrogen is 0.4%, the embodiment of the present invention 5 is while from pyrazolone factory effluent, recovery obtains ammoniacal liquor and calcium sulfate, also pyrazolone factory effluent is processed, reduce the pollution of pyrazolone factory effluent.
As seen from the above embodiment, the invention provides a kind of recovery method of pyrazolone factory effluent, comprise the following steps: 1), by pyrazolone factory effluent and calcium oxide carry out replacement(metathesis)reaction, obtain reaction soln; Described pyrazolone factory effluent comprises the ammonium sulfate of mass percent >=20%; 2), by described reaction soln carry out stripping process, obtain gas mixture and feed liquid, described gas mixture comprises ammonia and water vapour, and described feed liquid comprises calcium sulfate.The recovery method of pyrazolone factory effluent provided by the invention can reclaim the gas mixture and the calcium sulfate that obtain ammonia and water vapour from pyrazolone factory effluent, ammonia and calcium sulfate have higher using value and economic benefit, compared with prior art, the recovery method of pyrazolone factory effluent provided by the invention has good economy.In addition, the recovery method of pyrazolone factory effluent provided by the invention, while reclaiming the gas mixture and calcium sulfate obtaining ammonia and water vapour, also processes pyrazolone factory effluent, reduces the pollution of pyrazolone factory effluent.
The explanation of above embodiment just understands method of the present invention and core concept thereof for helping.It should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention, can also carry out some improvement and modification to the present invention, these improve and modify and also fall in the protection domain of the claims in the present invention.Be apparent for those skilled in the art to the multiple amendment of these embodiments, General Principle as defined herein can realize without departing from the spirit or scope of the present invention in other embodiments.Therefore, the present invention can not be restricted to these embodiments shown in this article, but will meet the widest scope consistent with principle disclosed herein and features of novelty.
Claims (6)
1. a recovery method for pyrazolone factory effluent, comprises the following steps:
1), by pyrazolone factory effluent and calcium oxide carry out replacement(metathesis)reaction, obtain reaction soln; Described pyrazolone factory effluent comprises the ammonium sulfate of mass percent 20% ~ 25%; The mass ratio of described pyrazolone factory effluent and calcium oxide is (45 ~ 55): 1;
2), by described reaction soln carry out stripping process, obtain gas mixture and feed liquid, described gas mixture comprises ammonia and water vapour, and described feed liquid comprises calcium sulfate; The temperature of described stripping process is 50 DEG C ~ 65 DEG C; Pressure >=the 2MPa of described stripping process; In described gas mixture, the mass ratio of ammonia and water vapour is (20 ~ 25): (75 ~ 80).
2. method according to claim 1, is characterized in that, described step 1) in the temperature of replacement(metathesis)reaction be 20 DEG C ~ 30 DEG C.
3. method according to claim 1, is characterized in that, described step 1) in time of replacement(metathesis)reaction be 2 hours ~ 4 hours.
4. method according to claim 1, is characterized in that, described step 1) in the pH value of reaction soln be 11 ~ 14.
5. method according to claim 1, is characterized in that, also comprises described step 2) gas mixture that obtains carries out condensation process, obtains ammoniacal liquor.
6. the ammoniacal liquor that described in the gas mixture that the method in Claims 1 to 4 described in any one obtains or claim 5, method obtains is for the preparation of pyrazolone.
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| US20130004400A1 (en) * | 2011-07-01 | 2013-01-03 | Alstom Technology Ltd. | Chilled ammonia based co2 capture system with ammonia recovery and processes of use |
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| CN101243017A (en) * | 2005-08-11 | 2008-08-13 | 卡斯生有限公司 | Ammonium/ammonia removal from a stream |
| CN1884100A (en) * | 2006-07-06 | 2006-12-27 | 黄平峰 | Method for regeneration and cyclic utilization of ammonia |
| US20130004400A1 (en) * | 2011-07-01 | 2013-01-03 | Alstom Technology Ltd. | Chilled ammonia based co2 capture system with ammonia recovery and processes of use |
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| 吡唑酮母液废水预处理工艺研究;程高峰等;《广州化工》;20120830;第179页左栏第1-2段 * |
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