CN104445500A - Technique for adsorption treatment of low-concentration ammonia-nitrogen wastewater - Google Patents
Technique for adsorption treatment of low-concentration ammonia-nitrogen wastewater Download PDFInfo
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- CN104445500A CN104445500A CN201410659687.XA CN201410659687A CN104445500A CN 104445500 A CN104445500 A CN 104445500A CN 201410659687 A CN201410659687 A CN 201410659687A CN 104445500 A CN104445500 A CN 104445500A
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/34—Regenerating or reactivating
- B01J20/3416—Regenerating or reactivating of sorbents or filter aids comprising free carbon, e.g. activated carbon
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/34—Regenerating or reactivating
- B01J20/345—Regenerating or reactivating using a particular desorbing compound or mixture
- B01J20/3475—Regenerating or reactivating using a particular desorbing compound or mixture in the liquid phase
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
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Abstract
The invention discloses a technique for adsorption treatment of low-concentration ammonia-nitrogen wastewater and belongs to the technical field of wastewater treatment. The technique disclosed by the invention comprises activation of an adsorbent, an application process of the adsorbent and regeneration of the adsorbent. According to the technique disclosed by the invention, the selected adsorbent is remarkably improved in adsorption capacity on ammonia and nitrogen in wastewater after being activated under a certain condition; the concentration of the wastewater treated by adopting the technique disclosed by the invention can be controlled at an extremely low level, and the adsorbent is free of obvious reduction of treatment effect after being regenerated. The technique has the advantages of good treatment effect, low adsorbent regeneration cost, simple activation method, good recyclability and wide application range.
Description
Technical field
The present invention relates to a kind of Low Concentration Ammonia Containing Wastewater adsorption treatment novel process, specifically a kind of process matched therewith method adopting sorbent treatment Low Concentration Ammonia Containing Wastewater, belongs to technical field of waste water processing.
Background technology
In recent years, along with developing rapidly of China's economic, pollution of waterhead is day by day serious, and drinking water source water quality declines gradually.Wherein ammonia nitrogen is a kind of important substance causing body eutrophication and environmental pollution, and in water, ammonia nitrogen concentration is too high, nature can be suppressed nitrated, cause water hypoxia, cause fish poisoning, reduces water body self-purification ability, serious harm human health.Therefore, China and in the world many countries in drinking water standard, have strict restriction to ammonia-nitrogen content.
Ammonia nitrogen enters water body, particularly to flow lake, bay more slowly, easily cause algae and other microorganism amount reproductions in water, form eutrophication pollution, except making water treatment plants operation difficulty, causing the peculiar smell of tap water, oxygen in water time serious, can be made to decline, fish kill, water quality degenerates, and forms red tide, even can cause the dry destruction in lake.Ammonia nitrogen also makes to increase chlorine dosage in water disinfection and industrial circulating water sterilisation process; To some metal, particularly to copper, there is corrodibility; When reusing sewage, in reuse water, ammonia nitrogen can promote the breeding of microorganism in water pipe and watering equipment, forms biofouling, blocking pipe and watering equipment, and affects heat exchange efficiency.
Usual industrial middle and high concentration ammonia nitrogen waste water can pass through the steam stripped mode of stripping, and make sewage qualified discharge, this mode efficiency is high, effective, and can, with the ammonia nitrogen in the form recycle-water of ammonia, ammonium sulfate, be a kind of common ammonia nitrogen waste water treatment method.But when the ammonia nitrogen waste water of its process lower concentration, especially during below 200ppm, the problems such as energy consumption is relatively large, uneconomical will be produced.For Low Concentration Ammonia Containing Wastewater, in industry, conventional sorbent material that is natural or synthesis adsorbs, and also can reach good treatment effect.
Absorption method has the features such as simple to operate, installation cost is low and aqueous concentration is stable, comparatively general in industrial application.Absorption method, by the specific adsorptive power of sorbent material to ammonia nitrogen in water, when ammonium radical ion contacts with adsorbent surface, will be adsorbed on its surface, thus reach the object removing ammonia nitrogen in waste water.But general ammonia nitrogen adsorbent, loading capacity is less, needs frequent regeneration, and after regeneration, adsorptive power declines, and causes running cost higher, and this just limits its industrial applications to a certain extent.
Summary of the invention
Technical problem to be solved by this invention adopts absorption method modal shortcoming when processing ammonia nitrogen waste water in industry, and wherein comprise the bad outlet ammonia nitrogen concentration caused of adsorption effect higher, adsorbent reactivation weak effect, adsorbent reactivation cost is more high.
The invention provides a kind of Low Concentration Ammonia Containing Wastewater adsorption treatment process method, this technique comprises: renovation process three aspects of the activation method of sorbent material, the application of sorbent material and sorbent material.
(1) sorbent material and activation method thereof
Sorbent material and activation solution are carried out mixed and modified, obtains the sorbent material after activating through washing, drying.
The processing condition that above-mentioned activation method adopts are:
Sorbent material can adopt activated carbon fiber and zeolite, activated carbon fiber and activated alumina or activated carbon fiber and gac to carry out compositely obtaining composite sorbent material; Wherein activated carbon fiber can be the one in polyacrylonitrile based activated carbon fiber, viscose base activated carbon fiber and asphalt activity carbon fiber; Zeolite model can be the one of 4A, 5A or 13X type;
In composite sorbent material, the volumetric ratio that activated carbon fiber occupies is 65% ~ 95%;
Described activation solution is wherein one or more such as sulfuric acid, nitric acid, hydrochloric acid, sodium hydroxide, sodium-chlor and sodium carbonate;
The mass concentration scope of activation solution is 5% ~ 60%;
Activation temperature is 30 ~ 90 DEG C;
The priming reaction time is 1 ~ 12h;
Activation number of times is more than twice or twice.
(2) adsorption applications of sorbent material
Under certain temperature condition, the above-mentioned composite sorbent material through overactivation is packed in fixed-bed adsorber, adsorption treatment is carried out to Low Concentration Ammonia Containing Wastewater.
The processing condition that above-mentioned adsorption process adopts are:
Entering water ammonia nitrogen concentration is 15 ~ 500ppm, and the pH scope entering water is 2 ~ 10;
Ammonia nitrogen waste water temperature range is 0 ~ 50 DEG C;
The operation residence time of ammonia nitrogen waste water is 0.5 ~ 4h;
Adsorbent packing density is 0.1 ~ 2.5kg/dm
3.
(3) renovation process of sorbent material
After described composite sorbent material adopts the processing method process ammonia nitrogen waste water for some time described in above-mentioned steps, its water outlet ammonia nitrogen concentration gos up to (generally not higher than 15ppm) during finite concentration, stops and carries out adsorbent reactivation process.First spray a small amount of regenerated liquid, after then using water vapor purging for some time, when detecting in outlet water vapor condensation water containing ammonia nitrogen, regenerative process terminates, and lays equal stress on and relapses additive process.
The processing parameter that above-mentioned regenerative process adopts is:
Regenerated liquid can adopt one or more in sodium-chlor, sodium sulfate, sodium carbonate, sodium hydroxide or sodium bicarbonate;
Regenerated liquid mass concentration scope is 0.1 ~ 10%;
Regenerated liquid spray flux needed for every kilogram of sorbent material is 5 ~ 20L;
The water vapor purging recovery time is 1 ~ 6 hour;
Water vapor pressure scope can adopt 0.1 ~ 1Mpa.
Beneficial effect of the present invention:
1, to export water concentration after treatment extremely low and controlled for ammonia nitrogen waste water;
2, sorbent material repeatedly recycles, and effect stability after using regeneration;
3, the renovation process of sorbent material is simple, and regeneration cost is lower.
Embodiment
The present invention is further illustrated below by way of specific embodiment.But the detail of embodiment only for explaining the present invention, should not be construed as limited overall technical solution.
Embodiment 1:
The activation method of sorbent material: take certain mass viscose base activated carbon fiber sample and 4A zeolite sample carries out composite, make in the volumetric spaces shared by sorbent material, the volumetric ratio that activated carbon fiber occupies is about 70%.First the composite sorbent material of 1.0t is got at 2m
3massfraction is that in the NaOH solution of 5% after 80 DEG C of immersion 1h, washes clean, then through 2.3m
3mass concentration is the sodium chloride solution soaking at room temperature 12h of 9%, washing and drying.
The application of activating adsorbent: be the composite sorbent material after loading activation in the ADSORPTION IN A FIXED BED tower of 1.2m at diameter, adsorbent packing density is 1.80kg/dm
3, concentration is that the nitrogen-containing wastewater of 40mg/L is with 0.8m
3the flow of/h, by adsorption tower, measures its water outlet ammonia nitrogen concentration.Result shows: be 35 DEG C in temperature, and pH is 6, and flow is 0.8m
3under/h, adopt GB 7479-87 Na Shi spectrophotometry, detect water outlet ammonia nitrogen concentration, detection display reaches national standard reference GB 8978-1996, namely aqueous concentration is less than 15mg/L, and denitrogenation filtrate processing efficiency is 340L/kg, and saturated treatment capacity is 740L/kg.
The renovation process of sorbent material: to the ADSORPTION IN A FIXED BED tower of saturated adsorption, spray mass concentration is the NaOH solution 4.2m of 5%
3(adsorbent mass is about 0.83t), after draining away the water, passes into 0.1Mpa hot steam regeneration 4h, penetrate adsorption efficiency after regeneration and be about 330L/kg, without obviously reducing.
Embodiment 2:
The activation method of sorbent material: the viscose base activated carbon fiber and the activated alumina ball that take certain mass carry out composite, and make in the volumetric spaces shared by sorbent material, the volumetric ratio that activated carbon fiber occupies is about 85%.First the composite sorbent material of 0.6t is got at 1.4m
3massfraction is the Na of 6%
2cO
3in solution after 60 DEG C of immersion 2h, washes clean, then through 2.2m
3mass concentration is the sodium chloride solution soaking at room temperature 6h of 5%, washing and drying.
The adsorption applications of activating adsorbent: be the sorbent material after loading activation in the ADSORPTION IN A FIXED BED tower of 0.9m at diameter, adsorbent packing density is 0.73kg/dm
3, concentration is that the nitrogen-containing wastewater of 100mg/L is with 0.8m
3the flow of/h, by adsorption tower, measures its water outlet ammonia nitrogen concentration.Result shows: be 40 DEG C in temperature, and pH be neutrality, and flow velocity is 1.2m
3under/h, adopt GB 7479-87 Na Shi spectrophotometry, detect water outlet ammonia nitrogen concentration, detection display reaches national standard reference GB 8978-1996, namely aqueous concentration is less than 15mg/L, and denitrogenation filtrate processing efficiency is 240L/kg, and saturated treatment capacity is 540L/kg.
The regeneration of sorbent material: to the ADSORPTION IN A FIXED BED tower of saturated adsorption, spray mass concentration is the NaOH solution 3.4m of 4%
3(adsorbent mass is about 0.54t), after draining away the water, passes into 0.9Mpa hot steam regeneration 2h, penetrate adsorption efficiency after regeneration and be about 250L/kg, have and slightly raise.
Embodiment 3:
The activation method of sorbent material: the asphalt activity carbon fiber sample and the cocoanut active charcoal sample that take certain mass are composite, and make in the volumetric spaces shared by sorbent material, the volumetric ratio that activated carbon fiber occupies is about 67%.First the composite sorbent material of 0.8t is got at 5.3m
3massfraction is that in the salpeter solution of 10% after 60 DEG C of immersion 4h, washes clean, then through 6.0m
3mass concentration is the sodium hydroxide solution 60 DEG C immersion 2h of 15%, washing and drying.
The adsorption applications of activating adsorbent: be the composite sorbent material after loading activation in the ADSORPTION IN A FIXED BED tower of 2.3m at diameter, adsorbent packing density is 1.04kg/dm
3, concentration is that the nitrogen-containing wastewater of 73mg/L is with 0.9m
3the flow of/h, by adsorption tower, measures its water outlet ammonia nitrogen concentration.Result shows: be 35 DEG C in temperature, and pH is 9, and flow is 0.9m
3under/h, adopt GB 7479-87 Na Shi spectrophotometry, detect water outlet ammonia nitrogen concentration, detection display reaches national standard reference GB 8978-1996, namely aqueous concentration is less than 15mg/L, and denitrogenation filtrate processing efficiency is 430L/kg, and saturated treatment capacity is 960L/kg.
The regeneration of sorbent material: to the adsorption column of saturated adsorption, spray mass concentration is the NaOH solution 4.8m of 10%
3(adsorbent mass is about 0.76t), drain away the water, pass into 0.4Mpa hot steam regeneration 1h from adsorption column top, penetrate adsorption efficiency after regeneration and be about 435L/kg, without considerable change.
Embodiment 4:
The activation method of sorbent material: the viscose base activated carbon fiber and the 13X type zeolite that take certain mass are composite, and make in the volumetric spaces shared by sorbent material, the volumetric ratio that activated carbon fiber occupies is about 81%.First the composite sorbent material of 2.6t is got at 10m
3massfraction is 80 DEG C of immersion 4h in the salpeter solution of 20%, and washes clean, then through 8m
3massfraction is sodium hydroxide solution soaking at room temperature 2h, washing and drying.
The adsorption applications of activating adsorbent: be the composite sorbent material after loading activation in the ADSORPTION IN A FIXED BED tower of 0.8m at diameter, adsorbent packing density is 1.85kg/dm
3, concentration is that the nitrogen-containing wastewater of 140mg/L is with 0.8m
3the flow of/h, by adsorption tower, measures its water outlet ammonia nitrogen concentration.Result shows: be 20 DEG C in temperature, and pH is about 6, and flow is 0.8m
3under/h, adopt GB 7479-87 Na Shi spectrophotometry, detect water outlet ammonia nitrogen concentration, detection display reaches national standard reference GB 8978-1996, namely aqueous concentration is less than 15mg/L, and denitrogenation filtrate processing efficiency is 580L/kg, and saturated treatment capacity is 1360L/kg.
The renovation process of sorbent material: to the ADSORPTION IN A FIXED BED tower of saturated adsorption, spray mass concentration is the NaOH solution 10m of 10%
3(adsorbent mass is about 2.34t), after draining away the water, pass into 1.2Mpa hot steam regeneration 3h, penetrating adsorption efficiency after regeneration is 560L/kg, without considerable change.
Embodiment 5:
The activation method of sorbent material: the polyacrylonitrile based activated carbon fiber and the wood activated charcoal that take certain mass are composite, and make in the volumetric spaces shared by sorbent material, the volumetric ratio that activated carbon fiber occupies is about 87%.First the composite sorbent material of 1.6t is got at 8.0m
3massfraction is that in the salpeter solution of 10% after 60 DEG C of immersion 4h, washes clean, then through 6.0m
3massfraction is the sodium hydroxide solution 60 DEG C immersion 2h of 10%, washing and drying, then uses 5.0m
3, 5% sodium chloride solution soak at room temperature 6h, washing and drying.
The adsorption applications of activating adsorbent: be the composite sorbent material after loading activation in the ADSORPTION IN A FIXED BED tower of 1.8m at diameter, adsorbent packing density is 1.38kg/dm
3, concentration is that the nitrogen-containing wastewater of 40mg/L is with 1.2m
3the flow of/h, by adsorption tower, measures its water outlet ammonia nitrogen concentration.Result shows: be 28 DEG C in temperature, and pH is 8, and flow is 1.2m
3under/h, adopt GB 7479-87 Na Shi spectrophotometry, detect water outlet ammonia nitrogen concentration, detection display reaches national standard reference GB 8978-1996, namely aqueous concentration is less than 15mg/L, and denitrogenation filtrate processing efficiency is 650L/kg, and saturated treatment capacity is 1130L/kg.
The regeneration of sorbent material: to the adsorption tower of saturated adsorption, spray mass concentration is the NaOH solution 7.5m of 10%
3(adsorbent mass is about 1.48t), drain away the water, pass into 0.2Mpa hot steam regeneration 4h from adsorption column top, penetrating adsorption efficiency after regeneration is 638L/kg, without considerable change.
Embodiment 6:
The activation method of sorbent material: the polyacrylonitrile based activated carbon fiber and the 5A type zeolite that take certain mass are composite, and in the volumetric spaces shared by sorbent material, the volumetric ratio that activated carbon fiber occupies is about 72%.First the composite sorbent material of 1.5t is got at 4.2m
3massfraction is 60 DEG C of immersion 12h in the sulphuric acid soln of 40%, and washes clean, then through 6.0m
3massfraction is the sodium hydroxide solution soaking at room temperature 6h of 5%, washing and drying.
The adsorption applications of activating adsorbent: be the composite sorbent material after loading activation in the ADSORPTION IN A FIXED BED post of 2.4m at diameter, adsorbent packing density is 0.98kg/dm
3, concentration is that the nitrogen-containing wastewater of 40mg/L is with 2.0m
3the flow of/h, by adsorption column, measures its water outlet ammonia nitrogen concentration.Result shows: be 30 DEG C in temperature, and pH is about 6.5, and flow is 4m
3under/h, adopt GB 7479-87 Na Shi spectrophotometry, detect water outlet ammonia nitrogen concentration, detection display reaches national standard reference GB 8978-1996, namely aqueous concentration is less than 15mg/L, and denitrogenation filtrate processing efficiency is 780L/kg, and saturated treatment capacity is 1820L/kg.
The renovation process of sorbent material: to the ADSORPTION IN A FIXED BED post of saturated adsorption, spray mass concentration is the NaOH solution 10m of 10%
3(adsorbent mass is about 1.42t), after draining away the water, passes into 1.0Mpa hot steam regeneration 3h, penetrate adsorption efficiency after regeneration and be about 760L/kg, without considerable change.
Claims (7)
1. a Low Concentration Ammonia Containing Wastewater adsorption treatment process method, is characterized in that, this technique comprises: renovation process three aspects of the activation method of sorbent material, the adsorption applications of sorbent material and sorbent material;
(1) sorbent material and activation method thereof
By sorbent material and activation solution mixed and modified by carrying out, through washing, drying obtain activate after sorbent material;
The processing condition that above-mentioned activation method adopts are:
Sorbent material adopts activated carbon fiber and zeolite, activated carbon fiber and activated alumina or activated carbon fiber and gac to carry out compositely obtaining composite sorbent material;
(2) adsorption applications of sorbent material
Under certain temperature condition, the above-mentioned composite sorbent material through overactivation is packed in fixed-bed adsorber, adsorption treatment is carried out to Low Concentration Ammonia Containing Wastewater;
(3) renovation process of sorbent material
After described composite sorbent material adopts the processing method process ammonia nitrogen waste water for some time described in above-mentioned steps, when its water outlet ammonia nitrogen concentration gos up to finite concentration, stop and carry out adsorbent reactivation process; First, with a small amount of regenerated liquid spray, after then using water vapor purging for some time, when detecting in outlet water vapor condensation water containing ammonia nitrogen, regenerative process terminates, and lays equal stress on and relapses additive process.
2. according to the method for claim 1, it is characterized in that, in step (1), activated carbon fiber is the one in polyacrylonitrile based activated carbon fiber, viscose base activated carbon fiber and asphalt activity carbon fiber; Zeolite model is the one of 4A, 5A or 13X type.
3. according to the method for claim 1, it is characterized in that, step (1) described activation solution is wherein one or more such as sulfuric acid, nitric acid, hydrochloric acid, sodium hydroxide, sodium-chlor and sodium carbonate;
The mass concentration scope of activation solution is 5% ~ 60%;
Activation temperature is 30 ~ 90 DEG C;
The priming reaction time is 1 ~ 12h;
Activation number of times is more than twice or twice.
4. according to the method for claim 1, it is characterized in that, in step (1) composite sorbent material, the volumetric ratio that activated carbon fiber occupies is 65% ~ 95%.
5. according to the method for claim 1, it is characterized in that, the processing condition that adsorption process adopts are:
Entering water ammonia nitrogen concentration is 15 ~ 500ppm, and the pH scope entering water is 2 ~ 10;
Ammonia nitrogen waste water temperature range is 0 ~ 50 DEG C;
The operation residence time of ammonia nitrogen waste water is 0.5 ~ 4h;
Adsorbent packing density is 0.1 ~ 2.5kg/dm
3.
6. according to the method for claim 1, it is characterized in that, the processing parameter that regenerative process adopts is:
Regenerated liquid adopts one or more in sodium-chlor, sodium sulfate, sodium carbonate, sodium hydroxide or sodium bicarbonate;
Regenerated liquid mass concentration scope is 0.1 ~ 10%;
Regenerated liquid spray flux needed for every kilogram of sorbent material is 5 ~ 20L;
The water vapor purging recovery time is 1 ~ 6 hour;
Water vapor pressure scope adopts 0.1 ~ 1Mpa.
7. according to the method for claim 1, it is characterized in that, its water outlet ammonia nitrogen concentration gos up to not higher than 15ppm, stops and carries out adsorbent reactivation process.
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| CN112820357A (en) * | 2019-11-22 | 2021-05-18 | 武汉科技大学 | Arsenic solidification rate measuring method based on combustion temperature and ash melting point temperature and application |
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