CN103831022A - Device and method for recycling ammonia nitrogen from coking wastewater - Google Patents
Device and method for recycling ammonia nitrogen from coking wastewater Download PDFInfo
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- CN103831022A CN103831022A CN201410079769.7A CN201410079769A CN103831022A CN 103831022 A CN103831022 A CN 103831022A CN 201410079769 A CN201410079769 A CN 201410079769A CN 103831022 A CN103831022 A CN 103831022A
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- waste water
- concentration
- diffusion dialysis
- peg20000
- coking chemical
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Abstract
The invention provides a diffusion dialysis device for recycling NH4<+> from coking wastewater, and a method for treating the coking wastewater and other high-concentration ammonia nitrogen wastewater and recycling the NH4<+> by using the device. The economic feasibility and technical feasibility of the treatment method are fully considered, the high-concentration NH4<+> in the coking wastewater is subjected to the combined technology of membrane diffusion dialysis separation and sodium tetraphenylborate selective precipitation, the aim of removing and recycling NH4<+> from the coking wastewater containing high-concentration ammonia nitrogen and other high-concentration ammonia nitrogen wastewater is achieved, the removal rate of the NH4<+> can be over 95 percent, and the recycling rate of the NH4<+> can be over 90 percent.
Description
Technical field:
The present invention relates to wastewater treatment, specifically belong to a kind of and reclaim NH from the coking chemical waste water containing ammonia nitrogen in high density or chemical fertilizer factory's waste water
4 +apparatus and method.
Technical background:
Adopt the NH of traditional biochemical process Treatment of Wastewater in Coking middle and high concentration
4 +, existence investment is large, operational management is complicated and water outlet is difficult to the problems such as up to standard, and can not realize NH
4 +resource reclaim and utilize.
Ammonia still process method, because the consumption to steam is large, is processed 1m
3waste water needs l/4t steam, only as coking chemical waste water middle and high concentration NH
4 +pretreating process.
Chemical precipitation method is because precipitation reaction is carried out more than pH9.0, in processing, need to add the NaOH of some in waste water, cause processed waste water alkalescence to exceed standard and processing cost increase, and in waste water, need to introduce excessive chemical substance sodium hydrogen phosphate and magnesium dichloride, the concentration of phosphorus and magnesium in water is increased, cause the increase of secondary pollution and processing cost.
Absorption method, as traditional wastewater processing technology, adopts zeolite or resin all can effectively adsorb the NH in coking chemical waste water
4 +, but the subject matter existing is: adsorbent is to NH
4 +absorption selectivity poor, in complicated waste water system, chaff interference is many, organic efficiency is low.
Reverse osmosis membrane technology can be removed the NH in coking chemical waste water preferably
4 +, but pressure process energy consumption is high; To NH
4 +separation selectivity is poor; NH in the cleaning of film and cleaning fluid
4 +reclaim and wait the problem facing still more.
Ion-exchange diffusion dialysis film can reclaim the positive and negative ion in coking chemical waste water, but due to NH
4 +the reasons such as separation selectivity is poor, at present only for the recovery process of Coal Gas Washing Cycling Water acid, alkali.
Tetraphenylboron sodium can with coking chemical waste water in NH
4 +carry out high selectivity precipitation reaction (K
sP=5.71 × 10
-8), but the solution loss that need avoid tetraphenylboron sodium to cause due to other ion salt effect in waste water increases processing cost and causes the secondary pollution of waste water.The present invention has adopted membrane technology by the NH of waste water side
4 +be transferred in tetraphenylboron sodium-PEG20000 composite precipitation agent solution and complete precipitation reaction by the method for diffusion dialysis, take full advantage of energy-conservation diffusion dialysis mode, effectively realized NH
4 +the separating of precipitation reaction and waste water.
Summary of the invention:
The object of the present invention is to provide one to reclaim NH from coking chemical waste water or other high-concentration ammonia nitrogenous wastewater
4 +apparatus and method, this device is made simple, operational effect is good; Method is to NH
4 +process selective height, non-secondary pollution, can realize NH
4 +reclaim.
One provided by the invention reclaims NH from coking chemical waste water
4 +diffusion dialysis device, the diffusion dialysis film adopting in this diffusion dialysis device is to prepare by the following method:
(1) compound concentration is 4～6%(W/V) cellulose diacetate acetone soln, cellulose diacetate is fully dissolved with the airtight stirring of magnetic stirring apparatus;
(2) be 4%(V/V to adding PEG400 (A.R) to make its concentration in above-mentioned lysate), airtight stirring, leaves standstill, and obtains preparation liquid;
(3) select commercially available 100 orders, thickness be 0.15mm nylon cloth as carrier, put on glass plate, topple over a small amount of preparation liquid, at the uniform velocity push through with scraper plate, after 5min, repeat once, make the diffusion dialysis film thickness 0.23-0.25mm after making, naturally dry and obtain diffusion dialysis film; NH
4 +diffusion velocity U in this diffusion dialysis film
nH4 +=2.95 × 10
-7m/s.
Required diffusion dialysis membrane area S(m
2) calculating, can be according to formula lnC
t=lnC
0-U
nH4sT/V sets, wherein V(m
3) be the volume of pending waste water, C
0(g/L) be pending waste water NH
4 +concentration, C
t(g/L) be requirement processed waste water NH
4 +concentration, T(s) be the hydraulic detention time of waste water in diffusion dialysis device.
One provided by the invention reclaims NH from coking chemical waste water
4 +method, comprise the steps:
1) respectively with antikinesis in the runner of peristaltic pump driving coking chemical waste water and compound precipitants film both sides in above-mentioned diffusion dialysis device, make the NH in coking chemical waste water
4 +react with compound precipitants by diffusion dialysis film, the compound precipitants of consumption is added liquid with compound precipitants by fluid filling pump and is supplemented in cyclic process;
2) reactant liquor leaves standstill through settling tank, isolates tetraphenylboron ammonium-PEG20000 precipitation, and supernatant recycles;
3) tetraphenylboron ammonium-PEG20000 precipitation acetone solution, wherein NH
4 +separate the NH in eluent by cationic exchange resin adsorption
4 +adopt the method for ammonium magnesium phosphate chemical precipitation to reclaim.
The velocity ratio that described coking chemical waste water and compound precipitants move in the runner of diffusion dialysis film both sides is 1:2～3, and preferably 1:2, to ensure to form the timely output of precipitation;
Described compound precipitants is added the additional amount of liquid in cyclic process, with the contained tetraphenylboron sodium concentration of compound precipitants in service 0.5%～0.7%(W/V) be advisable;
Described compound precipitants is tetraphenylboron sodium and PEG20000 mixture aqueous solution, and wherein the concentration of tetraphenylboron sodium is 0.5%～0.7%, and the concentration of PEG20000 is 2 times of tetraphenylboron sodium concentration.To keep osmotic pressure and the waste water infiltration pressure of composite precipitation agent solution basic identical, in running, there is not water yield migration and be advisable in the concrete concentration that PEG20000 is selected.
It is tetraphenylboron sodium and PEG20000 mixture aqueous solution that described compound precipitants is added liquid, and wherein the concentration of tetraphenylboron sodium is 5～20%, and the concentration of PEG20000 is 2 times of tetraphenylboron sodium concentration.
Described coking chemical waste water can be also other ammonia nitrogen in high density (NH
4 +) waste water, as synthetic ammonia waste water, percolate etc.
By diffusion dialysis device of the present invention and recovery NH
4 +method Treatment of Wastewater in Coking and other high-concentration ammonia nitrogenous wastewater, NH
4 +removal efficiency can reach more than 95%, the rate of recovery can reach more than 90%.
Compared with prior art, the present invention has advantage and effect:
(1) the diffusion dialysis film of preparing has good chemical stability, has the performance of resistance to chemical attack, resistance to oxidation, resistance to uniform temperature and hydrolysis, the chemical stability that still can keep in the situation that reusing 6 times each 10 hours and service life.
(2) after adopting this film that coking chemical waste water and compound precipitants are separated, diffusion dialysis film is to NH in waste water
4 +there is good permeability, to NH in waste water
4 +diffusion dialysis treatment effect be better than the selective cation-exchange membrane of commercially available DF-120.Therefore the NH in waste water
4 +can enter compound precipitants and tetraphenylboron sodium carries out efficient single-minded precipitation reaction by this film.
(3) prepared film completely can not be penetrating to compound precipitants, therefore acid group-the PEG20000 of the tetraphenylboron in compound precipitants compound can not enter waste water by this film, avoided the polluter of processing procedure to release new in waste water.
(4) according to the Donnan balance principle in diffusion dialysis, the NH in waste water
4 +in entering composite precipitation agent solution by diffusion dialysis film time, in order to keep the electroneutral of solution, the Na of the medium molal quantity of composite precipitation agent solution
+ion also can enter coking chemical waste water by diffusion dialysis film.Prepared diffusion dialysis film removes NH
4 +have outside good permeability, also can ensure the Na of the higher concentration to accumulating with elution process in compound precipitants
+there is good permeability, thereby can protect the continuous circulation use of compound card precipitant solution, outer row.
(5) in inventive method, adopt the tetraphenylboron sodium of certain proportioning and PEG20000 not to change tetraphenylboron sodium and NH as compound precipitants
4 +reactivity, but can change the crystalline form of precipitation, thereby can effectively stop the deposition of tetraphenylboron ammonium-PEG20000 sediment on film surface, make diffusion dialysis film to NH
4 +dialysis speed along with the carrying out of running do not change substantially.
(6) compound that in compound precipitants, tetraphenylboron sodium and PEG20000 form can effectively prevent tetraphenyl borate radical ion by film to exosmosing in coking chemical waste water, avoided the secondary pollution of tetraphenylboron sodium to waste water.
(7) in compound precipitants, certain density PEG20000 can make the water yield of diffusion dialysis film both sides substantially not change as osmotic pressure instrumentality.
(8) in compound precipitants, PEG20000 and tetraphenylboron sodium form compound and can increase the chemical stability of tetraphenylboron sodium in the aqueous solution, can in processing procedure, repeatedly be repeated to utilize.
(9), in subsequent step, adopt the present invention to NH in waste water
4 +tetraphenylboron ammonium-PEG20000 precipitation the acetone solution separating, wherein NH
4 +method by cationic ion-exchange resin and ammonium magnesium phosphate chemical precipitation reclaims.Acetone solvent, mother liquor of precipitation of ammonium and resin column regenerative elution liquid related in process can be recycled, and whole processing procedure is without the discharge of waste water, waste gas and solid waste.
(10) adopt said method Treatment of Wastewater in Coking, to NH wherein
4 +removal efficiency can reach more than 95%, the rate of recovery can reach more than 90%; According to the requirement difference of processing waste water, select suitable membrane area to process waste water, can realize≤15mg/L of the concentration of ammonia nitrogen, reaches national grade one discharge standard.
(11) in processing procedure, the regeneration of deionization exchange column needs to consume and reclaim NH
4 +deng the NaOH of molal quantity, and can cause outside the loss of acetone solvent approximately 0.1% in acetone solution precipitation and removal process, do not need to add any other compound in waste water or precipitating reagent; Compound precipitants can be in running Reusability, consume and magnitude of recruitment few, can determine by the chemical monitoring in running.Being processed into of whole processing procedure ton waste water should be managed the difference of influent waste water and draining water quality everywhere and change.In addition the ammonium magnesium phosphate reclaiming also can be used as commodity selling and obtains corresponding economic benefit.
Brief description of the drawings:
Fig. 1 diffusion dialysis device schematic diagram
Detailed description of the invention:
The preparation of embodiment 1 diffusion dialysis film
Be material of preparing with cellulose diacetate (L.R, acetic acid binding capacity 54.5～56%, moisture≤5.0%), PEG400 (A.R, molecular weight 370-460) and acetone (C.P).
Preparation method:
(1) take cellulose diacetate 25g, add 500ml acetone, on magnetic stirring apparatus, airtight stirring 24h fully dissolves cellulose diacetate, and being mixed with concentration is 5%(W/V) cellulose diacetate acetone soln;
(2) draw 20ml PEG400 with pipette and add in above-mentioned cellulose diacetate acetone soln, after airtight stirring 1h, leave standstill, obtain preparation liquid; Wherein the concentration of PEG400 is 4%(V/V);
(3) adopting commercially available aperture is that 100 orders, the thickness nylon cloth that is 0.15mm is as carrier, being cut into width is the band that 75mm, length are 800mm, put and on glass plate, topple over 20ml preparation liquid, at the uniform velocity push through with scraper plate (selecting width is that 100mm, middle 80mm have the groove that 0.25mm is dark, the corrosion resistant plate that thickness is 2mm to produce), after 5min, repeat once, naturally dry.Diffusion dialysis film thickness after making is 0.24mm.Through the known NH of experiment
4 +diffusion velocity U in this diffusion dialysis film
nH4 +=2.95 × 10
-7m/s.
Embodiment 2 tetraphenylboron sodiums-PEG20000 compound precipitants and compound precipitants are added the preparation of liquid
Compound precipitants preparation:
(1) raw material of preparing as compound precipitants with tetraphenylboron sodium (AR) and PEG20000 (AR, molecular weight 8800-11200).
(2) take 3g tetraphenylboron sodium and 6g PEG20000 and be dissolved in respectively in 200ml deionized water, after two kinds of solution are mixed, be settled to 500ml, be mixed with compound precipitants.In compound precipitants, the concentration of tetraphenylboron sodium is 0.6%(W/V), the concentration of PEG20000 is 1.2%(W/V).
Compound precipitants is added liquid preparation:
Take 12.5g tetraphenylboron sodium and 25g PEG20000 and be dissolved in respectively in 100ml deionized water, after two kinds of solution are mixed, be settled to 250ml, be mixed with compound precipitants and add liquid.The concentration that compound precipitants is added tetraphenylboron sodium in liquid is 5%(W/V), the concentration of PEG20000 is 10%(W/V).
Embodiment 3 reclaims ammonia nitrogen from coking chemical waste water
Assembling diffusion dialysis device: the diffusion dialysis film that embodiment 1 is made is cut into 7 film pieces that are of a size of 70mm × 100mm, the PE(polyethylene that to be clipped on respectively by 8 thickness be 1cm) between the diffusion dialysis device unit made of plate, compress with bolt.In device, the water-holding quantity of coking chemical waste water and the compound precipitants aqueous solution is respectively 140ml, and total effectively permeable membrane area is 245cm
2.
Coking chemical waste water (is taken to Taiyuan coke-oven plant, NH
4 +concentration 520mg/L, COD concentration 5103mg/L) the compound precipitants 500ml for preparing of 200ml and embodiment 2 use respectively BT00-300T Lange constant flow peristaltic pump with the flow of 50ml/min. and 100ml/min. respectively by diffusion dialysis device (as shown in Figure 1) sheet frame runner separately, between coking chemical waste water and compound precipitants, be diffused dialyser and separate, two kinds of liquid flow with contrary direction in sheet frame runner separately.
Coking chemical waste water and compound precipitants adopt the method operation circulating in diffusion dialysis device respectively; Wherein in compound precipitants, the magnitude of recruitment of tetraphenylboron sodium and PEG20000 is pressed run duration NH
4 +the even supply of removal molal quantity equivalent, add liquid and adopt the compound precipitants prepared of embodiment 2 to add liquid, make the concentration of the contained tetraphenylboron sodium molal quantity of precipitating reagent in running remain on (ultraviolet spectrophotometry detection) in 0.5～0.7% scope.
NH in the coking chemical waste water of processing under above-mentioned treatment conditions
4 +clearance be changed to shown in following table:
Note: 1, processed waste water COD is 4329mg/L, and clearance is 15%, adopts high pressure liquid chromatography not in waste water
Detect tetraphenylboron sodium
2, Click here and manage speed and processing horizontal calculating, the membrane area that ton Treatment of Coking Effluent amount need to provide is 122.5m
2
Separate tetraphenylboron ammonium-PEG20000 sediment from bottom, reactant liquor standing sedimentation pond, supernatant can be used as compound precipitants and repeatedly reuses, not outer row.
By the above-mentioned sediment acetone solution separating, lysate is crossed 001 × 7 sodium type cation exchange resin column by NH wherein
4 +with the Na in post
+carry out ion-exchange, maximum saturation adsorbance can reach 69mg NH
4 +/ gram resin, efflux is the acetone soln that contains tetraphenylboron sodium and PEG20000.
The decompression distillation under 40 DEG C of conditions of the acetone soln of tetraphenylboron sodium and PEG20000 is gone out to acetone recycling, the tetraphenylboron sodium of gained and PEG20000 mixture are returned and in compound precipitants, carry out next round precipitation reaction.Tetraphenylboron sodium-the PEG20000 that repeats to return to dissolving is to NH in waste water
4 +reactivity still can remain on more than 98%, in continuous 6 times are reused, do not add change or outward row.
Adsorb the NaOH eluant solution of the sodium type cationic ion-exchange resin 1.0mol/L after saturated, the NH in eluent
4 +can adopt ammonium magnesium phosphate chemical precipitation method to be reclaimed, the rate of recovery reaches 92.5%.Eluent can reuse, not outer row.
The treatment effect of coking chemical waste water: NH
4 +clearance reach 95.3%, with ammonium magnesium phosphate form reclaim NH
4 +the rate of recovery reach 92.5%.
Claims (4)
1. one kind is reclaimed NH from coking chemical waste water
4 +diffusion dialysis device, it is characterized in that, the diffusion dialysis film adopting in this diffusion dialysis device is to prepare by the following method:
(1) the cellulose diacetate acetone soln that compound concentration is 4～6%;
(2) be 4% to adding PEG400 to make its concentration in above-mentioned lysate, airtight stirring, leaves standstill, and obtains preparation liquid;
(3) select 100 orders, thickness be 0.15mm nylon cloth as carrier, put on glass plate, topple over a small amount of preparation liquid, at the uniform velocity push through with scraper plate, after 5min, repeat once, make the diffusion dialysis film thickness 0.23-0.25mm after making, naturally dry and obtain diffusion dialysis film.
2. one kind is reclaimed NH from coking chemical waste water
4 +method, it is characterized in that, comprise the steps:
(1) respectively with antikinesis in the runner of peristaltic pump driving coking chemical waste water and compound precipitants film both sides in diffusion dialysis device claimed in claim 1, make the NH in coking chemical waste water
4 +react with compound precipitants by diffusion dialysis film, the compound precipitants of consumption is added liquid with compound precipitants by fluid filling pump and is supplemented in cyclic process;
(2) reactant liquor leaves standstill through settling tank, isolates tetraphenylboron ammonium-PEG20000 precipitation, and supernatant recycles;
3) tetraphenylboron ammonium-PEG20000 precipitation acetone solution, wherein NH
4 +separate the NH in eluent by cationic exchange resin adsorption
4 +adopt the method for ammonium magnesium phosphate chemical precipitation to reclaim;
The velocity ratio that described coking chemical waste water and compound precipitants move in the runner of diffusion dialysis film both sides is 1: 2～3;
Described compound precipitants is added the additional amount of liquid in cyclic process, determines by the contained tetraphenylboron sodium concentration 0.5%～0.7% of compound precipitants in service;
Described compound precipitants is tetraphenylboron sodium and PEG20000 mixture aqueous solution, and wherein the concentration of tetraphenylboron sodium is 0.5%～0.7%, and the concentration of PEG20000 is 2 times of tetraphenylboron sodium concentration.
It is tetraphenylboron sodium and PEG20000 mixture aqueous solution that described compound precipitants is added liquid, and wherein the concentration of tetraphenylboron sodium is 5～20%, and the concentration of PEG20000 is 2 times of tetraphenylboron sodium concentration.
3. a kind of method that reclaims ammonia nitrogen from coking chemical waste water as claimed in claim 2, is characterized in that, the velocity ratio that described coking chemical waste water and compound precipitants move in the runner of diffusion dialysis film both sides is 1: 2.
4. a kind of method that reclaims ammonia nitrogen from coking chemical waste water as claimed in claim 2, is characterized in that, described coking chemical waste water substitutes with other high-concentration ammonia nitrogenous wastewater.
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|---|---|---|---|
| CN201410079769.7A CN103831022B (en) | 2014-03-06 | 2014-03-06 | A kind of apparatus and method reclaiming ammonia nitrogen from coking chemical waste water |
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|---|---|---|---|
| CN201410079769.7A CN103831022B (en) | 2014-03-06 | 2014-03-06 | A kind of apparatus and method reclaiming ammonia nitrogen from coking chemical waste water |
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|---|---|
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| CN103831022B CN103831022B (en) | 2015-09-30 |
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|---|---|---|---|
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105384225A (en) * | 2015-11-23 | 2016-03-09 | 天津工业大学 | Device removing inorganic icon type pollutant in water |
| CZ307446B6 (en) * | 2017-07-01 | 2018-08-29 | Asio, Spol. S R.O. | A deamonification device for wastewater treatment with high ammoniacal nitrogen concentration |
| CN111892224A (en) * | 2020-08-07 | 2020-11-06 | 重庆大学 | Ammonia nitrogen wastewater treatment system and method based on south of road dialysis and osmotic distillation coupling |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6495047B1 (en) * | 2001-03-21 | 2002-12-17 | Arup K. Sengupta | Process for selective coagulant recovery from water treatment plant sludge |
| CN1911988A (en) * | 2006-08-31 | 2007-02-14 | 陕西师范大学 | Preparation method of biodegradable cellulose acetate film |
| CN1943845A (en) * | 2006-09-08 | 2007-04-11 | 浙江工商大学 | Process for preparing poly acrylic acid-poly glycol/cellulose acetate composite film |
-
2014
- 2014-03-06 CN CN201410079769.7A patent/CN103831022B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6495047B1 (en) * | 2001-03-21 | 2002-12-17 | Arup K. Sengupta | Process for selective coagulant recovery from water treatment plant sludge |
| CN1911988A (en) * | 2006-08-31 | 2007-02-14 | 陕西师范大学 | Preparation method of biodegradable cellulose acetate film |
| CN1943845A (en) * | 2006-09-08 | 2007-04-11 | 浙江工商大学 | Process for preparing poly acrylic acid-poly glycol/cellulose acetate composite film |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105384225A (en) * | 2015-11-23 | 2016-03-09 | 天津工业大学 | Device removing inorganic icon type pollutant in water |
| CZ307446B6 (en) * | 2017-07-01 | 2018-08-29 | Asio, Spol. S R.O. | A deamonification device for wastewater treatment with high ammoniacal nitrogen concentration |
| CN111892224A (en) * | 2020-08-07 | 2020-11-06 | 重庆大学 | Ammonia nitrogen wastewater treatment system and method based on south of road dialysis and osmotic distillation coupling |
| CN111892224B (en) * | 2020-08-07 | 2023-02-07 | 重庆大学 | Ammonia-nitrogen wastewater treatment system and method based on south crossing dialysis and osmotic distillation coupling |
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