CN103831022B - A kind of apparatus and method reclaiming ammonia nitrogen from coking chemical waste water - Google Patents
A kind of apparatus and method reclaiming ammonia nitrogen from coking chemical waste water Download PDFInfo
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- CN103831022B CN103831022B CN201410079769.7A CN201410079769A CN103831022B CN 103831022 B CN103831022 B CN 103831022B CN 201410079769 A CN201410079769 A CN 201410079769A CN 103831022 B CN103831022 B CN 103831022B
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- waste water
- diffusion dialysis
- chemical waste
- coking chemical
- peg20000
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Abstract
The invention provides one and reclaim NH from coking chemical waste water
4 +diffusion dialysis device, and reclaim NH with this device Treatment of Wastewater in Coking and other high-concentration ammonia nitrogenous wastewater
4 +method, the present invention takes into full account economic feasibility and the technical feasibility of processing method, by the NH of coking chemical waste water middle and high concentration
4 +through the technical combinations of membrane diffusion dialysis separation and tetraphenylboron sodium selective precipitation, achieve from containing removing the coking chemical waste water of ammonia nitrogen in high density and other high-concentration ammonia nitrogenous wastewater and reclaiming NH
4 +target, NH
4 +removal efficiency can reach more than 95%, NH
4 +the rate of recovery can reach more than 90%.
Description
Technical field:
The present invention relates to wastewater treatment, specifically belong to a kind of and reclaim NH from containing the coking chemical waste water of 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, due to large to the consumption of steam, processes 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 carried out at more than pH9.0 due to precipitation reaction, the NaOH adding some in waste water is needed in process, processed waste water alkalescence is caused to exceed standard and processing cost increase, and need to introduce excessive chemical substance sodium hydrogen phosphate and magnesium dichloride in waste water, the concentration of phosphorus and magnesium in water is increased, causes the increase of secondary pollution and processing cost.
Absorption method is as traditional wastewater processing technology, and employing zeolite or resin all can adsorb the NH in coking chemical waste water effectively
4 +, but the subject matter existed is: adsorbent is to NH
4 +absorption selectivity poor, in the waste water system of complexity, chaff interference is many, and organic efficiency is low.
Reverse osmosis membrane technology can remove 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 +institute's problems faced such as recovery are 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 difference, at present only for the recovery process of Coal Gas Washing Cycling Water acid, alkali.
Tetraphenylboron sodium can with the NH in coking chemical waste water
4 +carry out high selectivity precipitation reaction (K
sP=5.71 × 10
-8), but the solution loss need avoiding tetraphenylboron sodium in waste water causing due to other ion salt effect makes processing cost increase and causes the secondary pollution of waste water.Present invention employs membrane technology by the NH of waste water side
4 +be transferred in tetraphenylboron sodium-PEG20000 composite precipitation agent solution by the method for diffusion dialysis and complete precipitation reaction, take full advantage of energy-conservation diffusion dialysis mode, effectively achieve NH
4 +being separated of precipitation reaction and waste water.
Summary of the invention:
One is the object of the present invention is to provide to reclaim NH from coking chemical waste water or other high-concentration ammonia nitrogenous wastewater
4 +apparatus and method, this device makes simple, and operational effect is good; Method is to NH
4 +process selective height, non-secondary pollution, can NH be realized
4 +reclaim.
One provided by the invention reclaims NH from coking chemical waste water
4 +diffusion dialysis device, the diffusion dialysis film adopted in this diffusion dialysis device prepares by the following method:
(1) compound concentration is 4 ~ 6%(W/V) cellulose diacetate acetone soln, with magnetic stirring apparatus airtight stirring, cellulose diacetate is fully dissolved;
(2) in above-mentioned lysate, adding PEG400 (A.R) makes its concentration be 4%(V/V), airtightly to stir, leave standstill, obtain 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, repeat after 5min once, make the diffusion dialysis film thickness 0.23-0.25mm after making, naturally dry and namely 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 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) drive antikinesis in the runner of coking chemical waste water and compound precipitants film both sides in above-mentioned diffusion dialysis device with peristaltic pump respectively, make the NH in coking chemical waste water
4 +reacted by diffusion dialysis film and compound precipitants, 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, and isolate tetraphenylboron ammonium-PEG20000 precipitation, supernatant recycles;
3) tetraphenylboron ammonium-PEG20000 precipitation acetone solution, incites somebody to action wherein NH
4 +be separated by cationic exchange resin adsorption, the NH in eluent
4 +the method of ammonium magnesium phosphate chemical precipitation is adopted to reclaim.
The velocity ratio that described coking chemical waste water and compound precipitants run in the runner of diffusion dialysis film both sides is 1:2 ~ 3, preferred 1:2, to ensure the timely output forming precipitation;
Described compound precipitants adds the additional amount of liquid in cyclic process, with tetraphenylboron sodium concentration 0.5% ~ 0.7%(W/V contained by compound precipitants in running) 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 the osmotic pressure of composite precipitation agent solution substantially identical with waste water infiltration pressure, in running, there is not water yield migration be advisable in the concrete concentration that PEG20000 is selected.
It is tetraphenylboron sodium and PEG20000 mixture aqueous solution that described compound precipitants adds 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 also can be 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 advantage that has of the present invention and effect:
(1) the diffusion dialysis film prepared 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 when reusing 6 times each 10 hours and service life.
(2) after coking chemical waste water and compound precipitants are separated by this film of employing, 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 +compound precipitants can be entered and tetraphenylboron sodium carries out efficient single-minded precipitation reaction by this film.
(3) film prepared by completely can not be penetrating to compound precipitants, and the tetraphenylboron acid group-PEG20000 compound therefore in compound precipitants can not enter waste water by this film, avoids 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 +when being entered in composite precipitation agent solution by diffusion dialysis film, 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 in compound precipitants and the Na of higher concentration of elution process accumulation
+have good permeability, thus the continuous circulation can protecting compound card precipitant solution uses, not outer row.
(5) tetraphenylboron sodium of certain proportioning and PEG20000 is adopted not to change tetraphenylboron sodium and NH as compound precipitants in inventive method
4 +reactivity, but the crystalline form of precipitation can be changed, thus effectively can stop the tetraphenylboron ammonium-deposition of PEG20000 sediment on film surface, make diffusion dialysis film to NH
4 +dialysis speed substantially do not change along with the carrying out of running.
(6) compound that in compound precipitants, tetraphenylboron sodium and PEG20000 are formed effectively can prevent tetraphenyl borate radical ion by film to exosmosing in coking chemical waste water, avoids 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 tetraphenylboron sodium chemical stability in aqueous, repeatedly can be recycled in processing procedure.
(9), in subsequent step, adopt the present invention to NH in waste water
4 +tetraphenylboron ammonium-PEG20000 precipitation the acetone solution be separated, incites somebody to action wherein NH
4 +reclaimed by the method for cationic ion-exchange resin and ammonium magnesium phosphate chemical precipitation.Acetone solvent, mother liquor of precipitation of ammonium and resin column regenerative elution liquid involved in process can be recycled, and whole processing procedure is without the discharge of waste water, waste gas and solid waste.
(10) said method Treatment of Wastewater in Coking is adopted, to wherein NH
4 +removal efficiency can reach more than 95%, the rate of recovery can reach more than 90%; Different according to the requirement of process waste water, select suitable membrane area process waste water, the concentration of ammonia nitrogen can realize≤15mg/L, 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 about 0.1% in acetone solution precipitation and removal process, not need in waste water or precipitating reagent, add other compound any; Compound precipitants can in running Reusability, consume and magnitude of recruitment few, 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 reclaimed also can be used as commodity selling and obtains corresponding economic benefit.
Accompanying drawing illustrates:
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 makes cellulose diacetate fully dissolve, and being mixed with concentration is 5%(W/V) cellulose diacetate acetone soln;
(2) drawing 20ml PEG400 with pipette adds in above-mentioned cellulose diacetate acetone soln, leaves standstill, obtain preparation liquid after airtight stirring 1h; Wherein the concentration of PEG400 is 4%(V/V);
(3) adopt that commercially available aperture is 100 orders, thickness is that the nylon cloth of 0.15mm is as carrier, be cut into that width is 75mm, length is the band of 800mm, put on glass plate and topple over 20ml preparation liquid, at the uniform velocity push through with scraper plate (select width is 100mm, middle 80mm has 0.25mm dark groove, corrosion resistant plate that thickness is 2mm produce), repeat after 5min 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 add the preparation of liquid
Prepared by compound precipitants:
(1) with the raw material that tetraphenylboron sodium (AR) and PEG20000 (AR, molecular weight 8800-11200) are prepared as compound precipitants.
(2) take 3g tetraphenylboron sodium and 6g PEG20000 is dissolved in 200ml deionized water respectively, be settled to 500ml by after two kinds of solution mixing, 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 adds liquid preparation:
Take 12.5g tetraphenylboron sodium and 25g PEG20000 is dissolved in 100ml deionized water respectively, be settled to 250ml by after two kinds of solution mixing, be mixed with compound precipitants and add liquid.The concentration that compound precipitants adds 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: diffusion dialysis film embodiment 1 made is cut into the film block that 7 pieces are of a size of 70mm × 100mm, being clipped on respectively by 8 pieces of thickness is the PE(polyethylene of 1cm) between the diffusion dialysis device unit made of plate, use bolt presses.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 from Taiyuan coke-oven plant, NH
4 +concentration 520mg/L, COD concentration 5103mg/L) the compound precipitants 500ml for preparing of 200ml and embodiment 2 uses BT00-300T Lange constant flow peristaltic pump with the flow of 50ml/min. and 100ml/min. respectively respectively by the respective sheet frame runner of diffusion dialysis device (as shown in Figure 1), be diffused dialyser between coking chemical waste water and compound precipitants to separate, two kinds of liquid flow with contrary direction in respective sheet frame runner.
Coking chemical waste water and compound precipitants adopt the method circulated in diffusion dialysis device respectively to run; Wherein in compound precipitants, the magnitude of recruitment of tetraphenylboron sodium and PEG20000 presses run duration NH
4 +the even supply of removal molal quantity equivalent, add liquid adopt embodiment 2 prepare compound precipitants add liquid, make the concentration of tetraphenylboron sodium molal quantity in running contained by precipitating reagent remain on (ultraviolet spectrophotometry detection) in 0.5 ~ 0.7% scope.
NH in the coking chemical waste water processed 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 reason speed and processing horizontal calculating, ton Treatment of Coking Effluent amount needs the membrane area provided to be 122.5m
2
From reactant liquor standing sedimentation pond bottom part from tetraphenylboron ammonium-PEG20000 sediment, supernatant can be used as compound precipitants and repeatedly reuses, not outer row.
By the above-mentioned sediment acetone solution be separated, lysate crosses 001 × 7 sodium form 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 containing tetraphenylboron sodium and PEG20000.
Acetone soln decompression distillation under 40 DEG C of conditions of tetraphenylboron sodium and PEG20000 is gone out acetone recycling, the tetraphenylboron sodium of gained and PEG20000 mixture is returned in compound precipitants and carries out next round precipitation reaction.Repeat to return the tetraphenylboron sodium-PEG20000 of dissolving to NH in waste water
4 +reactivity still can remain on more than 98%, do not add in reusing at continuous 6 times change or arrange outward.
Adsorb saturated after the NaOH solution wash-out of sodium form cationic ion-exchange resin 1.0mol/L, the NH in eluent
4 +ammonium magnesium phosphate chemical precipitation method can be adopted to be reclaimed, and 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 (3)
1. one kind is reclaimed NH from coking chemical waste water
4 +diffusion dialysis device, it is characterized in that, the diffusion dialysis film adopted in this diffusion dialysis device prepares by the following method:
(1) the cellulose diacetate acetone soln that mass concentration is 4 ~ 6% is prepared;
(2) in above-mentioned lysate, adding PEG400 makes its volumetric concentration be 4%, airtightly stirs, and leaves standstill, 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, repeat after 5min once, make the diffusion dialysis film thickness 0.23-0.25mm after making, naturally dry and namely 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) drive antikinesis in the runner of coking chemical waste water and compound precipitants film both sides in diffusion dialysis device according to claim 1 with peristaltic pump respectively, make the NH in coking chemical waste water
4 +reacted by diffusion dialysis film and compound precipitants, 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, and isolate tetraphenylboron ammonium-PEG20000 precipitation, supernatant recycles;
3) tetraphenylboron ammonium-PEG20000 precipitation acetone solution, incites somebody to action wherein NH
4 +be separated by cationic exchange resin adsorption, the NH in eluent
4 +the method of ammonium magnesium phosphate chemical precipitation is adopted to reclaim;
The velocity ratio that described coking chemical waste water and compound precipitants run in the runner of diffusion dialysis film both sides is 1: 2 ~ 3;
Described compound precipitants adds the additional amount of liquid in cyclic process, determines by tetraphenylboron sodium mass concentration 0.5% ~ 0.7% contained by compound precipitants in operation;
Described compound precipitants is tetraphenylboron sodium and PEG20000 mixture aqueous solution, and wherein the mass concentration of tetraphenylboron sodium is 0.5% ~ 0.7%, and the concentration value of PEG20000 is 2 times of tetraphenylboron sodium concentration value.
It is tetraphenylboron sodium and PEG20000 mixture aqueous solution that described compound precipitants adds liquid, and wherein the mass concentration of tetraphenylboron sodium is 5 ~ 20%, and the concentration value of PEG20000 is 2 times of tetraphenylboron sodium concentration value.
3. a kind of method reclaiming ammonia nitrogen from coking chemical waste water as claimed in claim 2, it is characterized in that, the velocity ratio that described coking chemical waste water and compound precipitants run in the runner of diffusion dialysis film both sides is 1: 2.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| 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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| CN103831022B true CN103831022B (en) | 2015-09-30 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
| 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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| 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 |
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