CN102423684B - A kind of modified zeolite ammonia nitrogen adsorbent and use thereof and renovation process - Google Patents
A kind of modified zeolite ammonia nitrogen adsorbent and use thereof and renovation process Download PDFInfo
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- CN102423684B CN102423684B CN201110335138.3A CN201110335138A CN102423684B CN 102423684 B CN102423684 B CN 102423684B CN 201110335138 A CN201110335138 A CN 201110335138A CN 102423684 B CN102423684 B CN 102423684B
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Abstract
The invention discloses a kind of modified zeolite ammonia nitrogen adsorbent and use thereof and renovation process, the preparation process of this adsorbent is: by natural zeolite after broken, grinding, the process of acid bubble, with CuSO
45H
2o aqueous solution, through pyroreaction, cooling, cleans, is drying to obtain finished product.Use and the renovation process of this adsorbent are: select lucite to do adsorption column, add this adsorbent in post, and nitrogenous effluent is squeezed into adsorption column by peristaltic pump and carried out adsorption reaction after regulating PH to alkalescent.After absorption a period of time, carry out backwash to adsorption column, absorption completes, and clean this adsorbent with hydrochloric acid or sulfuric acid, recovery and rinsing liquid, evaporative crystallization obtains ammonium chloride or ammonia sulfate crystal; Adsorbent after cleaned can re-use.Modified zeolite ammonia nitrogen adsorbent adsorption capacity of the present invention is large, and advantages of good adsorption effect, regenerates simple and convenient, adopts this sorbent treatment nitrogenous effluent, and technique is simple, stable water outlet.
Description
Technical field
The invention belongs to technical field of sewage, specifically a kind of modified zeolite ammonia nitrogen adsorbent and use thereof and renovation process.
Background technology
Ammonia nitrogen can cause the eutrophication of water body, produces toxic action to aquatile, increases the difficulty of Water purification, thus affects human health.Ammonia and nitrogen pollution in current China surface water body and body of groundwater constantly increases, and destroys normal Nitrogen transformation in natural ecosystems, causes serious impact and potential harm to water environment and human health.At present, the processing method of conventional ammonia nitrogen waste water mainly contains blow-off method, break point chlorination method, chemical precipitation method, biological denitrificaion method and ion-exchange.
Blow-off method utilizes the difference existed between the actual concentrations of contained ammonia nitrogen in waste water and equilibrium concentration, uses air stripping in the basic conditions, the ammonia nitrogen in waste water is constantly transferred in gas phase by liquid phase, thus remove ammonia nitrogen.This kind of method cost is high, and processed waste water is difficult to completely up to standard, and the ammonia of effusion easily causes secondary pollution.
Break point chlorination is dropped in waste water chlorine or clorox, the ammonium oxidation in waste water become the chemical denitrification process of nitrogen.Break point chlorination is swift in response, and cost of equipment is low, but the safe handling of liquid chlorine and shelf appeal high, in operation, chlorine dosage is large, thus operational management cost is high.So method is not too applicable to the process of large discharge high concentration nitrogen-containing waste water, the wastewater treatment especially containing a large amount of organic nitrogen compound.
Chemical precipitation method makes it form sediment by adding chemical agent in waste water and remove the denitrogenation of waste water technology of ammonia nitrogen.This kind of method technique is simple, but there is the very high problem of cost, is difficult to realize engineer applied.
Biological denitrificaion approach generally comprises two stages of nitrification and denitrification, organic nitrogen compound completes denitrification process jointly through the assimilation of ammoniation, nitrification, denitrification and microorganism, relates generally to nitrococcus, nitrifier and denitrifying bacterium three quasi-microorganism.This class methods Problems existing is that nitrobacteria growth is slow, and the reaction time is long, higher to requirement for environmental conditions, and treatment facility is huge.
Ion-exchange refers to the ion exchange process occurred on the interface of solid particle and liquid.Conventional clinoptilolite (Chinoptilolite) is as the ion exchanger except ammonia at present, and this material is to NH
4+selective penetrated property can higher than to other ions, therefore to NH
4+clearance can reach 90%-97%, but nitrate nitrogen, cultured water, organic nitrogen to be acted on without removal, and ion-exchanger consumption is large, needs frequent regeneration, is not suitable for the waste water processed containing a large amount of suspension and organic pollution.Therefore, study selective good, easily regeneration and the low water treatment absorbent of cost become focus both domestic and external.But up to now, there is not yet the zeolite-loaded burning copper of employing to prepare the relevant report of ammonia nitrogen removal agent.
Summary of the invention
Technical problem to be solved by this invention be to provide a kind of there is simple regeneration, the modified zeolite ammonia nitrogen adsorbent that can reduce cost for wastewater treatment and its use and renovation process.
The present invention solves the problems of the technologies described above with following technical scheme:
Invention one, modified zeolite ammonia nitrogen adsorbent, be made by carried metal cupric oxide on zeolite (Copper-Oxide-Coated-Zeolite is called for short COCZ), its preparation method is:
(1) first natural zeolite is carried out fragmentation, milled processed, then cross 20-40 mesh sieve, after soaking 24h with the sulfuric acid that volumetric concentration is 2%-10%, clean to pH be 6.5-7.5, at 120 DEG C of-150 DEG C of temperature, steam 16-24h, then be cooled to normal temperature after drying in 105 DEG C, for subsequent use;
(2) by CuSO
45H
2the weight proportion of the zeolite after O and above-mentioned process be 1: 3 ratio get CuSO
45H
2o is dissolved in ultra-pure water, mix with zeolite again, stir, 24h is reacted under 650 DEG C of hot conditions, wash away after being cooled to room temperature and do not have loaded surface particles, when to wash solution to pH being 6.5-7.5, drier under being placed in 100 DEG C of-150 DEG C of temperature, namely obtain modified zeolite ammonia nitrogen adsorbent finished product.
Invention two, the use of modified zeolite ammonia nitrogen adsorbent and renovation process:
Lucite is selected to do adsorption column, the modified zeolite ammonia nitrogen adsorbent that 3m is high is added in post, nitrogenous effluent is squeezed into adsorption column by peristaltic pump and is carried out adsorption reaction after regulating PH to 9, after absorption 5h, backwash 10min is carried out to adsorption column, then with hydrochloric acid or sulfuric acid cleaned 50min, recovery and rinsing liquid, evaporative crystallization obtains ammonium chloride or ammonia sulfate crystal, and the adsorbent after cleaned can re-use.
Described adsorption column adopts internal diameter to be 1.8m, highly to be the lucite post of 5.0m; The water inlet initial concentration of process waste water is 500-550mg/L, temperature 20-25 DEG C, and be 9 with NaOH adjust pH, flow control is at 6m/h, and treating capacity is 15m
3/ h, hydraulic detention time is 30min.
Product modified zeolite ammonia nitrogen adsorbent of the present invention has that adsorption capacity is large, advantages of good adsorption effect, regenerate advantage simply and easily.
Use product modified zeolite ammonia nitrogen adsorbent process nitrogenous effluent of the present invention, have the following advantages:
1. be carrier with zeolite, by cupric oxide load on the zeolite surface, form heteropolymer, and remain the structure of micropore, improve the Adsorption effect to ammonia nitrogen in sewage.
2. the preparation method of this adsorbent is simple, and recyclable regenerative utilizes.
3. equipment runs easy, and process stable effluent quality, can be used for the advanced nitrogen process to sewage.
4. zeolite rich reserves, cheap, and adsorbent that in actual use can be more expensive with some is used in conjunction with each other, and such complementation has higher economic benefit.
Accompanying drawing explanation
Fig. 1 is the process chart utilizing product modified zeolite ammonia nitrogen adsorbent process nitrogenous effluent of the present invention.
Fig. 2 is that embodiment 1 utilizes water outlet ammonia nitrogen concentration curve map after modified zeolite ammonia nitrogen adsorbent process smeltery ammonia nitrogen waste water.
Fig. 3 is that embodiment 2 utilizes water outlet ammonia nitrogen concentration curve map after the ammonia nitrogen waste water of modified zeolite ammonia nitrogen adsorbent disposal of refuse field.
Fig. 4 is that embodiment 3 utilizes water outlet ammonia nitrogen concentration curve map after modified zeolite ammonia nitrogen adsorbent process plant ammonia nitrogen waste water.
Detailed description of the invention
Below in conjunction with accompanying drawing and specific embodiment, the invention will be further described, but the protection domain of application claims be not only confined to following examples.
The preparation method of modified zeolite ammonia nitrogen adsorbent of the present invention is undertaken by following operating procedure:
(1) first natural zeolite is carried out fragmentation, milled processed, then cross 20-40 mesh sieve, after soaking 24h with the sulfuric acid that volumetric concentration is 2%-10%, clean to pH be 6.5-7.5, at 120 DEG C of-150 DEG C of temperature, steam 16-24h, then be cooled to normal temperature after drying in 105 DEG C, for subsequent use;
(2) by CuSO
45H
2the weight proportion of the zeolite after O and above-mentioned process be 1: 3 ratio get CuSO
45H
2o is dissolved in ultra-pure water, mix with zeolite again, stir, 24h is reacted under 650 DEG C of hot conditions, wash away after being cooled to room temperature and do not have loaded surface particles, when to wash solution to pH being 6.5-7.5, drier under being placed in 100 DEG C of-150 DEG C of temperature, namely obtain modified zeolite ammonia nitrogen adsorbent finished product.
Use method and the regeneration technology flow process of product modified zeolite ammonia nitrogen adsorbent process ammonia nitrogen waste water of the present invention, as shown in Figure 1, its operating process is described below:
Lucite is selected to do adsorption column, in post, interpolation is highly the modified zeolite adsorbent 8 of 3m, and modified zeolite adsorbent is supported by grillage 9, and the top of adsorption column is provided with inspection socket 5, air outlet slit 6 and water inlet 4, bottom is provided with delivery port 10, has cowling panel 7 in adsorption column.
The water inlet initial concentration of nitrogen-containing wastewater is 500-550mg/L, temperature 20-25 DEG C, collecting-tank 2 is entered through grid 1, squeezed into the water inlet 4 of this adsorption column by peristaltic pump 3 after regulating PH to 9 with NaOH, flow out from delivery port 10 after flowing through modified zeolite adsorbent 8 and grillage 9 process, enter clear water reserviors 11, extract out finally by pump 12 and carry out reuse.Regulate flow velocity 6m/h in processes, often at regular intervals at 10 place's water samplings, cross filtering with microporous membrane post analysis and measure ammonia-nitrogen content.
After absorption 5h, carry out backwash 10min to adsorption column, table wash water enters cowling panel from A, and back washing water enters from delivery port 10, finally all flows out postprecipitation through water inlet 4 and filters reuse.Carry out cleaning 50min to this adsorbent, recovery and rinsing liquid with hydrochloric acid or sulfuric acid again, evaporative crystallization obtains ammonium chloride or ammonia sulfate crystal; Adsorbent after cleaned can re-use.The water inlet flow velocity of waste water is that (treating capacity is 15m to 6m/h
3/ h), hydraulic detention time is 30min.
Embodiment 1
(1) first natural zeolite is carried out fragmentation, grinding, then cross 30 mesh sieves, soak 24h with the sulfuric acid that volumetric concentration is 5%, cleaning to pH is 7.0, at 120 DEG C of temperature, steam 24h, then is cooled to 25 DEG C after drying in 105 DEG C, for subsequent use;
(2) 100gCuSO is taken
45H
2o is dissolved in ultra-pure water, mixes, stir with the zeolite for subsequent use of 300g after above-mentioned process, under 650 DEG C of conditions, react 24h, wash away after being cooled to 25 DEG C and do not have loaded surface particles, when being 7.0 to wash solution pH, dry at 150 DEG C of temperature again, obtain modified zeolite ammonia nitrogen adsorbent;
(3) select lucite to do adsorption column, in post, add the modified zeolite ammonia nitrogen adsorbent of 3m, the waste water fetched is entered collecting-tank through grid and adopts NaOH to regulate PH to be 9, squeeze in adsorption column through pump, after process, enter clear water reserviors reuse from smeltery.By monitoring, influent ammonium concentration is 530mg/L, and temperature is 20 DEG C, and flow control is at 6m/h, and treating capacity is 15m
3/ h, hydraulic detention time is 30min, every 1h water sampling, measures ammonia-nitrogen content through 0.45 μm of filtering with microporous membrane post analysis.Its experiment the results are shown in Figure shown in 2, indicates adsorbent and shows good absorption property to ammonia nitrogen.The effect processing ammonia nitrogen within contact 5h can reach 98.7%, and along with the increase of time, adsorbance declines to some extent, and this may be because adsorbent reaches adsorption equilibrium gradually until saturated.
(4) after having adsorbed, carry out backwash 10min to adsorption column, then be the hydrochloric acid cleaning 50min of 10% by volumetric concentration, recovery and rinsing liquid, evaporative crystallization obtains ammonium chloride or ammonia sulfate crystal, and the adsorbent after cleaned can re-use.
Embodiment 2
(1) first natural zeolite is carried out fragmentation, grinding, then cross 20 mesh sieves, soak 24h with the sulfuric acid that volumetric concentration is 10%, cleaning to pH is 6.5, at 150 DEG C of temperature, steam 16h, then is cooled to 25 DEG C after drying in 105 DEG C, for subsequent use;
(2) 100gCuSO is taken
45H
2o is dissolved in ultra-pure water, the zeolite for subsequent use of drying with the pre-treatment of 300g process mixes, stir, 24h is reacted under 650 DEG C of conditions, wash away after being cooled to room temperature 25 DEG C and do not have loaded surface particles, when being 7.0 to wash solution pH, drier at 120 DEG C of temperature, obtain modified zeolite ammonia nitrogen adsorbent.
(3) select lucite to do adsorption column, in post, add the modified zeolite ammonia nitrogen adsorbent of 3m, the waste water fetched is entered collecting-tank through grid and adopts NaOH to regulate PH to be 9, squeeze in adsorption column through pump, after process, enter clear water reserviors reuse from soot.By monitoring, influent ammonium concentration is 500mg/L, and temperature is 23 DEG C, and flow control is at 6m/h, and treating capacity is 15m
3/ h, hydraulic detention time is 30min, every 1h water sampling, measures ammonia-nitrogen content through 0.45 μm of filtering with microporous membrane post analysis.Its experiment the results are shown in Figure shown in 3, indicates adsorbent and shows good absorption property to ammonia nitrogen.The effect processing ammonia nitrogen within contact 5h can reach 98.9%, and along with the increase of time, adsorbance declines to some extent, and this may be because adsorbent reaches adsorption equilibrium gradually until saturated.
(4) after having adsorbed, carry out backwash 10min to adsorption column, then be the hydrochloric acid cleaning 50min of 10% by volumetric concentration, recovery and rinsing liquid, evaporative crystallization obtains ammonium chloride or ammonia sulfate crystal, and the adsorbent after cleaned can re-use.
Embodiment 3
(1) first natural zeolite is carried out fragmentation, grinding, then cross 40 mesh sieves, soak 24h with the sulfuric acid that volumetric concentration is 2%, cleaning to pH is 7.5, at 130 DEG C of temperature, steam 24h, then is cooled to 25 DEG C after drying in 105 DEG C, for subsequent use;
(2) 100gCuSO is taken
45H
2o is dissolved in ultra-pure water, the zeolite for subsequent use of drying with the pre-treatment of 300g process mixes, stir, 24h is reacted under 650 DEG C of conditions, wash away after being cooled to room temperature 25 DEG C and do not have loaded surface particles, when being 7.0 to wash solution pH, drier at 135 DEG C of temperature, obtain modified zeolite ammonia nitrogen adsorbent.
(3) select lucite to do adsorption column, in post, add the modified zeolite ammonia nitrogen adsorbent of 3m, the waste water fetched is entered collecting-tank through grid and adopts NaOH to regulate PH to be 9, squeeze in adsorption column through pump, after process, enter clear water reserviors reuse from plant.By monitoring, influent ammonium concentration is 550mg/L, and temperature is 25 DEG C, and flow control is at 6m/h, and treating capacity is 15m
3/ h, hydraulic detention time is 30min, every 1h water sampling, measures ammonia-nitrogen content through 0.45 μm of filtering with microporous membrane post analysis.Its experiment the results are shown in Figure shown in 4, indicates adsorbent and shows good absorption property to ammonia nitrogen.The effect processing ammonia nitrogen within contact 5h can reach 98.0%, and along with the increase of time, adsorbance declines to some extent, and this may be because adsorbent reaches adsorption equilibrium gradually until saturated.
(4) after having adsorbed, carry out backwash 10min to adsorption column, then be the hydrochloric acid cleaning 50min of 10% by volumetric concentration, recovery and rinsing liquid, evaporative crystallization obtains ammonium chloride or ammonia sulfate crystal, and the adsorbent after cleaned can re-use.
Claims (1)
1. a modified zeolite ammonia nitrogen adsorbent, is characterized in that, its preparation method is:
(1) first natural zeolite is carried out fragmentation, milled processed, then cross 20-40 mesh sieve, after soaking 24h with the sulfuric acid that volumetric concentration is 2%-10%, clean to pH be 6.5-7.5, at 120 DEG C of-150 DEG C of temperature, steam 16-24h, then be cooled to normal temperature after drying in 105 DEG C, for subsequent use;
(2) by CuSO
45H
2the weight proportion of the zeolite after O and above-mentioned process is that the ratio of 1:3 gets CuSO
45H
2o is dissolved in ultra-pure water, mix with zeolite again, stir, 24h is reacted under 650 DEG C of hot conditions, wash away after being cooled to room temperature and do not have loaded surface particles, when to wash solution to pH being 6.5-7.5, drier under being placed in 100 DEG C of-150 DEG C of temperature, namely obtain modified zeolite ammonia nitrogen adsorbent finished product;
Use and the renovation process of described modified zeolite ammonia nitrogen adsorbent are: select lucite to do adsorption column, the modified zeolite ammonia nitrogen adsorbent that 3m is high is added in post, nitrogenous effluent is squeezed into adsorption column by peristaltic pump and is carried out adsorption reaction after regulating pH to 9, after absorption 5h, backwash 10min is carried out to adsorption column, then with hydrochloric acid or sulfuric acid cleaned 50min, recovery and rinsing liquid, evaporative crystallization obtains ammonium chloride or ammonia sulfate crystal, and the adsorbent after cleaned can re-use; Described adsorption column adopts internal diameter to be 1.8m, highly to be the lucite post of 5.0m; The water inlet initial concentration of process waste water is 500-550mg/L, temperature 20-25 DEG C, and be 9 with NaOH adjust pH, flow control is at 6m/h, and treating capacity is 15m
3/ h, hydraulic detention time is 30min.
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| CN110170338A (en) * | 2019-05-30 | 2019-08-27 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of the modified difunctional zeolite ion exchanger of Zr-Cu/ zeolite and products thereof and application |
| CN112028164A (en) * | 2020-08-25 | 2020-12-04 | 广西桂林新大桂工环境科技中心(有限合伙) | Preparation method of zeolite liquid for sewage treatment |
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