CN101607769A - A kind of treatment process of nitrogen-containing wastewater - Google Patents
A kind of treatment process of nitrogen-containing wastewater Download PDFInfo
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- CN101607769A CN101607769A CNA2009101157818A CN200910115781A CN101607769A CN 101607769 A CN101607769 A CN 101607769A CN A2009101157818 A CNA2009101157818 A CN A2009101157818A CN 200910115781 A CN200910115781 A CN 200910115781A CN 101607769 A CN101607769 A CN 101607769A
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Abstract
The present invention relates to the treatment process of the comprehensive recovery technology, particularly a kind of nitrogen-containing wastewater of the processing of all kinds of nitrogen-containing wastewaters in the industry and ammonia.Traditional ion exchange method is owing to leak effluent liquid and to wear a little and can't promptly and accurately judge, causes that ammonia nitrogen exceeds standard in the effluent liquid, can not recycle NH in the stripping liquid
4 +The low recycle value of concentration is not high, also need handle ammonia nitrogen, and processing cost is higher.Technical solution of the present invention: a kind of treatment process of nitrogen-containing wastewater, the steps include: that the waste water injection that will contain ammonia nitrogen is filled with first exchange column of Zeo-karb, feed liquid flows out from first exchange column outlet after cationic exchange resin adsorption, flow into then and be filled with second exchange column of Zeo-karb and further adsorb, flow out the feed liquid ammonia nitrogen concentration less than 15mg/L from second exchange column outlet.The present invention is with low cost, comprehensively reclaim ammonia, qualified discharge or recycle waste water continuously.
Description
Technical field
The present invention relates to the processing of all kinds of nitrogen-containing wastewaters in the industry and the comprehensive recovery technology of ammonia, particularly relate to the treatment process of a kind of nitrogen-containing wastewater in the hydrometallurgy of tungsten and rare earth.
Background technology
There is the discharging of ammonia at present in a large number in fields such as industrial or agricultural, especially the hydrometallurgy of tungsten and rare earth all uses the reagent that contains ammonia nitrogen in a large number, make in the technology that all kinds of nitrogen-containing wastewater amounts are big and concentration is high, cause most of waste water not only can not return and recycle, and need ability qualified discharge after expensive processing.
Nitrogen is the nutritive ingredient in the water body.Just can cause that when the ammonia nitrogen of being received in the water body is excessive body eutrophication pollutes, mass mortality again after causing waterplant such as algae etc. to grow fast, and oxygen is by the microbiological degradation mass consumption, oxygen in water is sharply reduced, and then make hydrobiont mass mortality, this eutrophication bring red tide and wawter bloom phenomenon to cause very big financial loss.Announce that according to national environmental protection portion China in 2008 red tide takes place altogether 68 times, 13738 square kilometres of areas take place in accumulative total, cause 206.05 hundred million yuan of direct economic losses, and estimate that contingent red tide phenomenon was 73 times more than in 2009, with havoc ecology, contaminate environment, governments at all levels all actively develop protection and control measures.
Traditional ion exchange method is owing to leak effluent liquid and to wear point and (must stop charging when ammonia nitrogen concentration reaches 15mg/L in the effluent liquid, otherwise can not qualified discharge) can't promptly and accurately judge, cause that ammonia nitrogen concentration exceeds standard in the effluent liquid, can not recycle, and because of the NH of exchange resin absorption
4 +NH in the stripping liquid when very little, causing desorb (regeneration)
4 +The too low recycle value of concentration is not high, also need further to handle, thereby processing cost is higher.
Summary of the invention
The object of the invention provide a kind of with low cost, comprehensively reclaim ammonia, continuous qualified discharge or recycle the treatment process of the nitrogen-containing wastewater of waste water.
Technical solution of the present invention: a kind of treatment process of nitrogen-containing wastewater, the steps include: that the waste water injection that will contain ammonia nitrogen is filled with first exchange column of Zeo-karb, feed liquid flows out from first exchange column outlet after cationic exchange resin adsorption, flow into then and be filled with second exchange column of Zeo-karb and further adsorb, flow out the feed liquid ammonia nitrogen concentration less than 15mg/L from second exchange column outlet;
Flow out material liquid pH value when the outlet of first exchange column and equal 7 or when reaching the certain volume amount, judge that promptly first exchange column finished absorption, stop to enter waste water this moment, using deionized water instead ejects nitrogen-containing wastewater in the post and enters second exchange column, the waste water that will contain ammonia nitrogen simultaneously enters from second exchange column import, second exchange column exports effusive feed liquid and enters and be filled with the 3rd exchange column of Zeo-karb, flows out the feed liquid ammonia nitrogen concentration less than 15mg/L from the 3rd exchange column outlet;
With first good exchange column of deionized water wash, be that the hydrochloric acid of 3～6mol/L is resolved with 0.8～1.5 times of resin bed volume, concentration, resolve first good exchange column and change stand-by state over to;
Flow out material liquid pH value when the outlet of second exchange column and equal 7 or when reaching the certain volume amount, judge that promptly second exchange column finished absorption, stop to enter waste water this moment, using deionized water instead ejects nitrogen-containing wastewater in the post and enters the 3rd exchange column, the waste water that will contain ammonia nitrogen simultaneously enters from the 3rd exchange column import, the 3rd exchange column exports effusive feed liquid and enters and be filled with first exchange column of Zeo-karb, flows out the feed liquid ammonia nitrogen concentration less than 15mg/L from first exchange column outlet;
With second good exchange column of deionized water wash, be that the hydrochloric acid of 3～6mol/L is resolved with 0.8～1.5 times of resin bed volume, concentration, resolve second good exchange column and change stand-by state over to;
Flow out material liquid pH value when the outlet of the 3rd exchange column and equal 7 or when reaching the certain volume amount, judge that promptly the 3rd exchange column finished absorption, stop to enter waste water this moment, using deionized water instead ejects nitrogen-containing wastewater in the post and enters first exchange column, the waste water that will contain ammonia nitrogen simultaneously enters from first exchange column import, first exchange column exports effusive feed liquid and enters and be filled with second exchange column of Zeo-karb, flows out the feed liquid ammonia nitrogen concentration less than 15mg/L from second exchange column outlet;
With the 3rd good exchange column of deionized water wash, be that the hydrochloric acid of 3～6mol/L is resolved with 0.8～1.5 times of resin bed volume, concentration, resolve the 3rd good exchange column and change stand-by state over to, so alternate cycles is used in three exchange columns in twos;
If positively charged ion only contains NH in the waste water
4 +, can obtain NH when then resolving
4Cl concentration is the purified solution of 120～150g/L, and this solution can directly return in the technical process, maybe this solution is carried out evaporative crystallization and can obtain refining ammonia chloride crystal;
If remove in the waste water and contain NH
4 +Also contain other positively charged ions outward, then desorbed solution can be alkalized promptly adds NaOH the pH value of solution value is reached about 12, carries out evaporation concentration, and the free ammonia that evaporates is reclaimed in condensation, obtains other cationic muriate crystal simultaneously.
Zeo-karb is 001 * 7 dried resin, i.e. strongly acidic styrene type cation exchange resin.
The present invention has reduced investment, and working cost is low, the time of judgement breakthrough point that can be promptly and accurately, reduce the monitoring amount, and 001 * 7 resin absorption amount is big, and regeneration times is few, and water outlet is qualified discharge directly, NH
4 +Can reclaim and come back in the explained hereafter, its polymeric adsorbent can reuse by desorption and regeneration; Adopt HCl solution as 001 * 7 regenerator, can solve pH to the influence of absorption ammonia nitrogen and make regenerated liquid recycling, the convenient and regeneration back loading capacity of desorb remains unchanged substantially; When adsorption column regeneration or maintenance, remaining adsorption column still can be handled ammonia nitrogen waste water, works continuously qualified discharge; Applied widely, can handle various ammonia nitrogen waste waters, be not subjected to cationic influence of other coexistences, even if still can obtain other cationic muriate crystal having under the coexistence positively charged ion condition.
Embodiment
The present invention adopts Zeo-karb, and 2～3 (being with 3) exchange columns are the one group of waste water that can handle ammonia nitrogen concentration 30～30000mg/L.The waste water that will contain ammonia nitrogen enters from first exchange column top (or bottom); feed liquid (or top) outflow after exchange resin absorption from the bottom; flow into second exchange column then; wherein first exchange column is main adsorption column; second exchange column is guard column (guaranteeing that ammonia nitrogen concentration is less than 15mg/L in the effluent liquid), the 3rd stand-by column that exchange column is finished for regeneration.When first exchange column top (or bottom) effluent liquid pH value 〉=7 (or reaching the certain volume amount); judge that promptly first exchange column finished absorption; stop to enter waste water this moment; using deionized water instead ejects nitrogen-containing wastewater in the post; the waste water that will contain ammonia nitrogen simultaneously is from second exchange column top (or bottom) charging; effusive feed liquid enters the 3rd exchange column (this moment, second exchange column was main adsorption column, and the 3rd exchange column is guard column, prevents that ammonia nitrogen concentration exceeds standard in the effluent liquid).First exchange column finishing with deionized water wash is that hydrochloric acid about 3～6mol/L carries out desorb (regeneration) with 0.8～1.5 times of resin bed volume, concentration, and the exchange column after the regeneration changes stand-by state over to.Three posts circulate successively.
If positively charged ion only contains NH in the waste water
4 +(or free ammonia) can obtain NH during then desorb (regeneration)
4Cl concentration is the purified solution of 120～150g/L, and this solution can directly return in the wet method smelting process flow process of tungsten and rare earth, maybe this solution is carried out evaporative crystallization and can obtain refining ammonia chloride crystal.
If remove in the waste water and contain NH
4 +(or free ammonia) is outer also to contain other positively charged ions, and then desorb (regeneration) liquid can be alkalized (adding NaOH reaches about 12 the pH value of solution value) carries out evaporation concentration, and the free ammonia that evaporates is reclaimed in condensation, obtains other cationic muriate crystal simultaneously.
Embodiment 1: ion exchange column Φ 40 * 300mm, in adorn 001 * 7 (strongly acidic styrene type cation exchange resin) dried resin 275g, the waste water that with ammonia nitrogen concentration is 810mg/L enters from the exchange column top with the 50mL/min flow, detecting effluent liquid pH value when being fed to 14.1L is 7, promptly stop charging, using deionized water instead ejects surplus liquid, getting the effluent liquid cumulative volume is 15.6L, wherein the fore portion effluent volume is 5.2L, ammonia nitrogen concentration is 10mg/L (meeting 15mg/L one class emission standard) by analysis, qualified discharge.The rear section effluent volume is 10.2L, ammonia nitrogen concentration is that 87mg/L enters another exchange column with this effluent liquid by same flow (specification is similarly Φ 40 * 300mm by analysis, in adorn 001 * 7 dried resin 275g), after 10.2L solution had advanced, effluent liquid 10.2L ammonia nitrogen concentration by analysis was 8mg/L.Continue quantitatively to enter the waste water 16.5L that ammonia nitrogen concentration is 810mg/L, wherein the fore portion effluent volume is 6.0L, and ammonia nitrogen concentration is 25mg/L by analysis.This solution with after aforementioned effluent liquid 10.2L mixes by analysis ammonia nitrogen concentration be 14mg/L (meeting 15mg/L one class emission standard), it is 11L that rear section effluent liquid and water top liquid merge the back volume, and ammonia nitrogen concentration is 91mg/L, and this solution enters the 3rd exchange column, repeat above step, successively circulation.
200mL carries out desorb (regeneration) to first exchange column with 4mol/L HCl solution, gets desorption and regeneration liquid 220mL, contains Cl
-Ion 98g/L, this solution directly Returning process use; 200mL carries out desorb (regeneration) to second exchange column with 4mol/L HCl solution, gets desorption and regeneration liquid 220mL, contains Cl
-Ion 124g/L, this solution directly Returning process use, and also this solution can be carried out evaporative crystallization and can obtain refining ammonia chloride crystal.
Embodiment 2: ion exchange column is with example 1.Be that 31400mg/L waste water 0.4L enters from the exchange column top with 30mL/min with ammonia nitrogen concentration earlier, using deionized water after having advanced instead ejects surplus liquid, getting the effluent liquid cumulative volume is 0.7L, wherein the fore portion effluent volume is 100mL, ammonia nitrogen concentration is 12mg/L (meeting 15mg/L one class emission standard) by analysis, qualified discharge.The rear section effluent volume is 600mL, ammonia nitrogen concentration is that 105mg/L enters another exchange column with this effluent liquid by same flow (specification is similarly Φ 40 * 300mm by analysis, in adorn 001 * 7 dried resin 275g), after 600mL solution had advanced, effluent liquid (600mL) ammonia nitrogen concentration by analysis was 13mg/L.Continue quantitatively to enter the waste water 0.4L that ammonia nitrogen concentration is 31400mg/L, wherein the fore portion effluent volume is 150mL, and ammonia nitrogen concentration is 30mg/L by analysis.This solution with after aforementioned effluent liquid 750mL mixes by analysis ammonia nitrogen concentration be 15mg/L (meeting 15mg/L one class emission standard), it is 550mL that rear section effluent liquid and water top liquid merge the back volume, ammonia nitrogen concentration is 1050mg/L, this solution enters the 3rd exchange column, repeat above step, successively circulation.
200mL carries out desorb (regeneration) to first exchange column with 4mol/L HCl solution, gets desorption and regeneration liquid 220mL, contains Cl
-Ion 118g/L, this solution directly Returning process use; With 4mol/L HCl 200mL second exchange column carried out desorb (regeneration), get desorption and regeneration liquid 220mL, contain Cl
-Ion 103g/L, this solution directly Returning process use, and also this solution can be carried out evaporative crystallization and can obtain refining ammonia chloride crystal.
Embodiment 3: with embodiment 1.Different is that two exchange columns are together in series, continuously feeding, the waste water that is about to ammonia nitrogen concentration and is 810mg/L enters from first exchange column top with the 50mL/min flow, and effluent liquid directly enters second exchange column top and goes out from the post underflow after resin absorption.When first exchange column is fed to 15L, stop charging, use deionized water instead surplus liquid is headed into second exchange column.This moment, first exchange column changed desorb (regeneration) operation over to, and second exchange column continues to enter the waste water that ammonia nitrogen concentration is 810mg/L from the top with the 40mL/min flow.From the effluent liquid that second effusive fore portion volume of exchange column is 15L, ammonia nitrogen concentration is 13mg/L (meeting 15mg/L one class emission standard) by analysis, qualified discharge.When second exchange column when to begin to enter from the top ammonia nitrogen concentration be the waste water of 810mg/L its effluent liquid then be connected in series into the 3rd exchange column (or the regeneration of playing a reversed role back finished first exchange column).Circulation successively.
200mL carries out desorb (regeneration) to first exchange column with 4mol/L HCl solution, gets desorption and regeneration liquid 225mL, contains Cl
-Ion 115g/L, this solution directly Returning process use, and also this solution can be carried out evaporative crystallization and can obtain refining ammonia chloride crystal.
Claims (2)
1, a kind of treatment process of nitrogen-containing wastewater, the steps include: that the waste water injection that will contain ammonia nitrogen is filled with first exchange column of Zeo-karb, feed liquid flows out from first exchange column outlet after cationic exchange resin adsorption, flow into then and be filled with second exchange column of Zeo-karb and further adsorb, flow out the feed liquid ammonia nitrogen concentration less than 15mg/L from second exchange column outlet;
Flow out material liquid pH value when the outlet of first exchange column and equal 7 or when reaching the certain volume amount, judge that promptly first exchange column finished absorption, stop to enter waste water this moment, using deionized water instead ejects nitrogen-containing wastewater in the post and enters second exchange column, the waste water that will contain ammonia nitrogen simultaneously enters from second exchange column import, second exchange column exports effusive feed liquid and enters and be filled with the 3rd exchange column of Zeo-karb, flows out the feed liquid ammonia nitrogen concentration less than 15mg/L from the 3rd exchange column outlet;
With first good exchange column of deionized water wash, be that the hydrochloric acid of 3～6mol/L is resolved with 0.8～1.5 times of resin bed volume, concentration, resolve first good exchange column and change stand-by state over to;
Flow out material liquid pH value when the outlet of second exchange column and equal 7 or when reaching the certain volume amount, judge that promptly second exchange column finished absorption, stop to enter waste water this moment, using deionized water instead ejects nitrogen-containing wastewater in the post and enters the 3rd exchange column, the waste water that will contain ammonia nitrogen simultaneously enters from the 3rd exchange column import, the 3rd exchange column exports effusive feed liquid and enters and be filled with first exchange column of Zeo-karb, flows out the feed liquid ammonia nitrogen concentration less than 15mg/L from first exchange column outlet;
With second good exchange column of deionized water wash, be that the hydrochloric acid of 3～6mol/L is resolved with 0.8～1.5 times of resin bed volume, concentration, resolve second good exchange column and change stand-by state over to;
Flow out material liquid pH value when the outlet of the 3rd exchange column and equal 7 or when reaching the certain volume amount, judge that promptly the 3rd exchange column finished absorption, stop to enter waste water this moment, using deionized water instead ejects nitrogen-containing wastewater in the post and enters first exchange column, the waste water that will contain ammonia nitrogen simultaneously enters from first exchange column import, first exchange column exports effusive feed liquid and enters and be filled with second exchange column of Zeo-karb, flows out the feed liquid ammonia nitrogen concentration less than 15mg/L from second exchange column outlet;
With the 3rd good exchange column of deionized water wash, be that the hydrochloric acid of 3～6mol/L is resolved with 0.8～1.5 times of resin bed volume, concentration, resolve the 3rd good exchange column and change stand-by state over to, so alternate cycles is used in three exchange columns in twos;
If positively charged ion only contains NH in the waste water
4 +, can obtain NH when then resolving
4Cl concentration is the purified solution of 120～150g/L, and this solution can directly return in the technical process, maybe this solution is carried out evaporative crystallization and can obtain refining ammonia chloride crystal;
If remove in the waste water and contain NH
4 +Also contain other positively charged ions outward, then desorbed solution can be alkalized promptly adds NaOH the pH value of solution value is reached about 12, carries out evaporation concentration, and the free ammonia that evaporates is reclaimed in condensation, obtains other cationic muriate crystal simultaneously.
2, according to the treatment process of the described a kind of nitrogen-containing wastewater of claim 1, it is characterized in that: Zeo-karb is 001 * 7 dried resin, i.e. strongly acidic styrene type cation exchange resin.
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| CNA2009101157818A CN101607769A (en) | 2009-07-26 | 2009-07-26 | A kind of treatment process of nitrogen-containing wastewater |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101838061A (en) * | 2010-05-17 | 2010-09-22 | 赣州华兴钨制品有限公司 | Method for treating ammonia-nitrogen wastewater and recovering the same into ammonium salt |
| CN102120658A (en) * | 2011-01-31 | 2011-07-13 | 中国环境科学研究院 | Treatment and recycling method of ammonia nitrogen in electrolytic manganese production end wastewater |
| CN102259039A (en) * | 2011-05-20 | 2011-11-30 | 中国水利水电科学研究院 | Method for quickly activating exchanger by using alkali and acid at different times and device used by same |
| CN103449568A (en) * | 2013-09-05 | 2013-12-18 | 南昌大学 | Method for treating wastewater with extremely low rare earth concentration by using coarse-grained clay in ionic rare-earth tailings |
| CN109052741A (en) * | 2016-01-19 | 2018-12-21 | 青岛大学 | A kind of synchronous decoloration of printing waste water and nitrogen recovery and treatment method |
| CN111003750A (en) * | 2019-12-16 | 2020-04-14 | 浙江工业大学 | Ultrasonic modified resin and application thereof in removing ammonia nitrogen in wastewater |
| CN112358009A (en) * | 2020-10-19 | 2021-02-12 | 深圳雅居乐环保科技有限公司 | Method for treating wastewater by using ion exchange column |
-
2009
- 2009-07-26 CN CNA2009101157818A patent/CN101607769A/en active Pending
Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101838061A (en) * | 2010-05-17 | 2010-09-22 | 赣州华兴钨制品有限公司 | Method for treating ammonia-nitrogen wastewater and recovering the same into ammonium salt |
| CN101838061B (en) * | 2010-05-17 | 2012-01-04 | 赣州华兴钨制品有限公司 | Method for treating ammonia-nitrogen wastewater and recovering the same into ammonium salt |
| CN102120658A (en) * | 2011-01-31 | 2011-07-13 | 中国环境科学研究院 | Treatment and recycling method of ammonia nitrogen in electrolytic manganese production end wastewater |
| CN102120658B (en) * | 2011-01-31 | 2013-02-27 | 中国环境科学研究院 | Treatment and recycling method of ammonia nitrogen in electrolytic manganese production end wastewater |
| CN102259039A (en) * | 2011-05-20 | 2011-11-30 | 中国水利水电科学研究院 | Method for quickly activating exchanger by using alkali and acid at different times and device used by same |
| CN103449568B (en) * | 2013-09-05 | 2014-11-26 | 南昌大学 | Method for treating wastewater with extremely low rare earth concentration by using coarse-grained clay in ionic rare-earth tailings |
| CN103449568A (en) * | 2013-09-05 | 2013-12-18 | 南昌大学 | Method for treating wastewater with extremely low rare earth concentration by using coarse-grained clay in ionic rare-earth tailings |
| CN109052741A (en) * | 2016-01-19 | 2018-12-21 | 青岛大学 | A kind of synchronous decoloration of printing waste water and nitrogen recovery and treatment method |
| CN109052742A (en) * | 2016-01-19 | 2018-12-21 | 青岛大学 | A kind of decoloration of printing waste water and nitrogen recovery method |
| CN109052741B (en) * | 2016-01-19 | 2021-08-03 | 青岛大学 | Synchronous decoloring and nitrogen recovery treatment method for printing wastewater |
| CN109052742B (en) * | 2016-01-19 | 2021-08-03 | 青岛大学 | Method for decoloring printing wastewater and recovering nitrogen |
| CN111003750A (en) * | 2019-12-16 | 2020-04-14 | 浙江工业大学 | Ultrasonic modified resin and application thereof in removing ammonia nitrogen in wastewater |
| CN111003750B (en) * | 2019-12-16 | 2022-10-11 | 浙江工业大学 | Ultrasonic modified resin and application thereof in removing ammonia nitrogen in wastewater |
| CN112358009A (en) * | 2020-10-19 | 2021-02-12 | 深圳雅居乐环保科技有限公司 | Method for treating wastewater by using ion exchange column |
| CN112358009B (en) * | 2020-10-19 | 2022-04-01 | 广州雅居乐固体废物处理有限公司 | Method for treating wastewater by using ion exchange column |
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Application publication date: 20091223 |