CN103252216B - Adsorbent, preparation process thereof and application of adsorbent to purification of ammonia-nitrogen wastewater with medium-low concentration - Google Patents
Adsorbent, preparation process thereof and application of adsorbent to purification of ammonia-nitrogen wastewater with medium-low concentration Download PDFInfo
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- CN103252216B CN103252216B CN201310214072.1A CN201310214072A CN103252216B CN 103252216 B CN103252216 B CN 103252216B CN 201310214072 A CN201310214072 A CN 201310214072A CN 103252216 B CN103252216 B CN 103252216B
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Abstract
The invention relates to a technology for purifying and treating ammonia-nitrogen wastewater by using an adsorption method and particularly relates to an adsorbent, a preparation process thereof and an application of the adsorbent to the purification of ammonia-nitrogen wastewater with medium-low concentration. An iron-plated woodchip adsorbent provided by the invention is composed of woodchips and Fe(OH)3. The preparation process comprises the following steps of: washing woodchips by using water for 1-3 times to remove impurities, drying, crushing and screening to ensure that the mass percentage of the woodchips with the particle sizes of 198-350mum is larger than or equal to 80%; subjecting a FeCl3 solution with the concentration of 0.15-0.25mol/L and a NaOH solution to reaction to generate a Fe(OH)3 suspension liquid; and then, sufficiently mixing the screened woodchips and the Fe(OH)3 suspension liquid according to the solid-to-liquid ratio of 0.6-1.0g/10mL, carrying out hydrothermal treatment at the temperature of 30-50 DEG C for 1.5-3h, washing a product by using water until the product is neutral, carrying out suction filtration, and drying the product. When the adsorbent is used for purifying the ammonia-nitrogen wastewater with medium-low concentration, the removal rate of NH4<+>-N is larger than or equal to 90%, and the removal rate of COD (Dissolved Organic Carbon) is larger than or equal to 75%.
Description
Technical field
The present invention relates to the technology of adsorption method for purifying process ammonia nitrogen waste water, especially a kind of adsorbent and preparation technology thereof are also applied to Low Concentration Ammonia Containing Wastewater in purification.
Background technology
Along with improving constantly of expanding economy and living standards of the people, wide material sources and the pollution that the ammonia nitrogen waste water that discharge capacity rises year by year causes has caused global concern.Except the industries such as oil, chemical industry, chemical fertilizer, iron and steel, food, pharmacy produce except a large amount of waste water, in the decomposition of itrogenous organic substance in sanitary sewage, animal excretion, percolate and agricultural production process, the use of nitrogenous fertilizer also can produce ammonia and nitrogen pollution.After ammonia nitrogen enters water body, be exactly the eutrophication causing water body the most significantly, make algae and planktonic rapid amount reproduction, dissolved oxygen declines, water quality severe exacerbation, and large number of biological is dead, causes black and odorous water.2010, China was useless, total amount of sewage discharge reaches 617.3 hundred million tons, and wherein discharged volume of industrial waste water is 237.5 hundred million tons, and in waste water, ammonia nitrogen discharge capacity reaches 120.3 ten thousand tons.As can be seen here, ammonia and nitrogen pollution has become one of serious pollution problem of China, and the ammonia nitrogen removed in waste water has become a focus and the difficult point of current environmental pollution improvement.
According to the difference of ammonia nitrogen concentration in waste water, waste water can be divided into 3 classes: high-concentration ammonia nitrogenous wastewater (NH
4 +-N >500 mg/L), intermediate concentration ammonia nitrogen waste water (NH
4 +-N is 50-500 mg/L), Low Concentration Ammonia Containing Wastewater (NH
4 +-N <50 mg/L).At present, the treatment technology relative maturity of high-concentration ammonia nitrogenous wastewater, but it is less for the research of middle Low Concentration Ammonia Containing Wastewater treatment technology, mainly contain biological denitrificaion method, break point chlorination, ion-exchange, soil irrigation method etc., these methods exist that operating cost is high mostly, complex treatment process, cause the shortcomings such as secondary pollution.
Absorption method is subject to the favor of people always because it is simple to operation, removal effect is good.The adsorbents such as tradition absorption method many employings active carbon, NACF, treatment effect is good, but service life is short, and operating cost is high, and the regeneration cost of adsorbent is high, causes its application to be restricted.Therefore, in cheap, the efficient absorption of exploitation, low concentration ammonia nitrogen material has become the study hotspot of absorption method.
Summary of the invention
The object of the invention is to overcome above-mentioned defect, a kind of adsorbent and preparation technology thereof are provided and are applied to Low Concentration Ammonia Containing Wastewater in purification.
Technical scheme of the present invention: a kind of plating iron wood chip adsorbent, by wood chip, Fe (OH)
3composition, wherein wood chip mass percent Wei≤99%, Fe (OH)
3mass percent Wei≤1%.
A kind of plating iron wood chip adsorbent, wood pellet particle diameter 198 ~ 350 μm account for mass percent Wei≤80%.
A kind of plating iron wood chip absorbent preparation technique, comprises the following steps: wood chip is first washed to remove silt, mechanical admixture through 1-3 times, dries and pulverize, sieve, make wood pellet particle diameter account for quality hundred points of number≤80% at 198 ~ 350 μm; Be the FeCl of 0.15 ~ 0.25 mol/L afterwards by concentration
3solution and NaOH solution are reacted and are generated Fe (OH)
3suspension; To be sieved wood chip and Fe (OH) again
3suspension fully mixes with the ratio of solid-to-liquid ratio 0.6 ~ 1.0 g/10 mL, hydrothermal treatment consists 1.5 ~ 3 h at temperature 30 ~ 50 DEG C, and product is through being washed to neutrality, and suction filtration, dries.
A kind of plating iron wood chip absorbent preparation technique, optimum process condition is: wood pellet particle diameter accounts for quality Bai Fen Shuo≤85% at 198 ~ 350 μm, is the FeCl of 0.15 mol/L by concentration
3solution and NaOH solution are reacted and are generated Fe (OH)
3suspension, then by wood chip and Fe (OH)
3suspension fully mixes with the ratio of solid-to-liquid ratio 1.0 g/10 mL, hydrothermal treatment consists 2 h at temperature 40 DEG C, and product is through being washed to neutrality, and suction filtration, dries.
A kind of Low Concentration Ammonia Containing Wastewater method in purification, comprise the following steps: regulate ammonia nitrogen waste water pH to be 9 ~ 11, plating iron wood chip adsorbent amount 3 ~ 5 g/L, reaction temperature 25 ~ 35 DEG C, after ammonia nitrogen waste water and plating iron wood chip adsorbent hybrid reaction time 20 ~ 50 min, filter.
A kind of Low Concentration Ammonia Containing Wastewater method in purification, optimal parameter condition is: regulate ammonia nitrogen waste water pH to be 9, plating iron wood chip adsorbent amount is 3 g/L, and reaction temperature controls at 30 DEG C, after ammonia nitrogen waste water and plating iron wood chip adsorbent hybrid reaction time 30 min, filter.
The present invention adopts hydro-thermal method to prepare adsorbent, and hydro-thermal method is a kind of new technology, and the standby adsorbent of this legal system has fabulous performance: even particle distribution, reunion mild degree, can use more cheap raw material, eliminate high-temp combustion and ball milling etc.
The present invention adopts wood chip as the base material of adsorbent, have cellulose, poly-pentose based in this body structure of wood chip, and the acidic materials such as tannin, also have some aldehyde, ketone, alcohol, ester, wherein containing a large amount of hydroxyl, carboxyl, part free hydroxyl group, free amino acid and free wooden phenol, these functional groups can absorbed portion cationic species and organic matter; And Fe (OH)
3suspension has certain flocculating function.Therefore its sinking speed is fast, NH
4 +-N removal Shuai≤90%, COD removal Shuai≤75%, and the water outlet after purified treatment can meet the standard-required of " integrated wastewater discharge standard " (GB8978-1996).
The present invention is different from active carbon absorption technology, not only inexpensive, be easy to get, and have the advantages that absorption coexists with ion-exchange, its outstanding advantages be plating iron wood chip as a kind of biological adsorption agent, can be used as fertilizer after the absorption of centering Low Concentration Ammonia Containing Wastewater is saturated and be applied to orchard and garden.
Determine to elaborate to each technological parameter below:
One, investigated the impact of Hydrothermal Synthesis temperature on ammonia nitrogen absorption effect, adsorption test condition is: FeCl
3solution concentration=0.15 mol/L, solid-to-liquid ratio=1.0 g/10 mL, ammonia nitrogen waste water pH=9, reaction time=30 min, reaction temperature=28 DEG C, adsorbent amount is 3 g/L.Fig. 1 is shown in the impact of Hydrothermal Synthesis temperature on ammonia nitrogen absorption effect.
Fig. 1 shows, and along with the rising of Hydrothermal Synthesis temperature, ammonia nitrogen removal effect is better.But too high synthesis temperature causes cost also higher.
Two, modifier FeCl has been investigated
3concentration is on the impact of ammonia nitrogen absorption effect, and adsorption test condition is: Hydrothermal Synthesis 2 h at 40 DEG C, solid-to-liquid ratio=1.0 g/10 mL, ammonia nitrogen waste water pH=9, reaction time=30 min, reaction temperature=31 DEG C, adsorbent amount is 3 g/L.Modifier FeCl
3fig. 2 is shown in the impact of concentration on ammonia nitrogen absorption effect.
As shown in Figure 2, with Fe (OH)
3suspension is compared, and the clearance of plating iron wood chip to ammonia nitrogen is higher.Along with Fe (OH)
3the increase of suspension concentration, the clearance of ammonia nitrogen also increases to some extent; Ammonia nitrogen removal frank also increases along with the increase of modifier iron concentration in plating iron wood chip.In addition, detect and to find after absorption ammonia nitrogen Fe in solution
3+concentration has a little increase, therefore infers that plating iron wood chip is removed in the process of ammonia nitrogen and may be there is cation exchange.
Three, wood chip and Fe (OH) has been investigated
3the ratio (solid-to-liquid ratio) of suspension is on the impact of ammonia nitrogen absorption effect, and adsorption test condition is: Hydrothermal Synthesis 2 h, FeCl at 40 DEG C
3solution concentration=0.15 mol/L, ammonia nitrogen waste water pH=9, reaction time=30 min, reaction temperature=33 DEG C, adsorbent amount is 3 g/L.Fig. 3 is shown in the impact of solid-to-liquid ratio on ammonia nitrogen absorption effect.
As can be seen from Figure 3, in the scope of 0.6 ~ 1.0 g/10 mL, along with wood chip and Fe (OH)
3the raising of suspension ratio, ammonia nitrogen removal frank slowly declines; But in the scope of 1.0 ~ 1.6 g/10 mL, ammonia nitrogen removal frank reduces fast.
Four, investigated the impact of pH value of solution on ammonia nitrogen absorption effect, adsorption test condition is: Hydrothermal Synthesis 2 h, FeCl at 40 DEG C
3solution concentration=0.15 mol/L, solid-to-liquid ratio=1.0 g/10 mL, reaction time=30 min, reaction temperature=32 DEG C, adsorbent amount is 3 g/L.Fig. 4 is shown in the impact of solution ph on ammonia nitrogen absorption effect.
Consider that higher pH can cause the effusion of ammonia, therefore, the scope of setting pH value of solution is 4 to 11.As shown in Figure 4, when pH changes in 4 ~ 11 scopes, the change of deduction pH value of solution causes with the minimizing of ammonium nitrogen amount, and log bits are up to 44% to the clean eliminating rate of absorption of ammonia nitrogen, and the clean eliminating rate of absorption of plating iron wood chip to ammonia nitrogen is up to 77%.The clearance of ammonia nitrogen in solution increases with the increase of pH value of solution, this is because when solution is acid, the iron oxide layer of plating iron wood chip adsorbent surface hydroxylating occurs in acid water environment and is electropositive; And when solution is alkalescence, adsorbent surface is then electronegative, with the ion state ammonium generation electrostatic attraction effect of positive charge.
Five, investigated the impact of reaction time on ammonia nitrogen absorption effect, adsorption test condition is: Hydrothermal Synthesis 2 h, FeCl at 40 DEG C
3solution concentration=0.15 mol/L, solid-to-liquid ratio=1.0 g/10 mL, ammonia nitrogen waste water pH=9, reaction temperature=32 DEG C, adsorbent amount is 3 g/L.Fig. 5 is shown in the impact of reaction time on ammonia nitrogen absorption effect.
Fig. 5 shows, and whole adsorption process is carried out very rapid in 20 min, just substantially reaches adsorption equilibrium state after 30 min.
Six, investigated the impact of adsorbent amount on ammonia nitrogen absorption effect, adsorption test condition is: Hydrothermal Synthesis 2 h, FeCl at 40 DEG C
3solution concentration=0.15 mol/L, solid-to-liquid ratio=1.0 g/10 mL, ammonia nitrogen waste water pH=9, reaction time=30 min, reaction temperature=34 DEG C.Fig. 6 is shown in the impact of adsorbent amount on ammonia nitrogen absorption effect.
As seen from Figure 6, along with the increase of adsorbent amount, the clearance of ammonia nitrogen also presents rising situation, and that is because the increase of adsorption site makes the clearance increase of ammonia nitrogen very fast; And the increase of adsorbent amount also shows the Fe of adsorbent surface
3+quantity increases, and therefore the possibility of its displacement ammonium ion improves.But after arriving 3 g/L, its ascendant trend is not obvious.
Accompanying drawing explanation
Fig. 1 be in the present invention Hydrothermal Synthesis temperature on the impact of ammonia nitrogen absorption effect.
Fig. 2 be in the present invention modifier iron concentration on the impact of ammonia nitrogen absorption effect.
Fig. 3 be in the present invention solid-to-liquid ratio on the impact of ammonia nitrogen absorption effect.
Fig. 4 be in the present invention pH value of solution on the impact of ammonia nitrogen absorption effect.
Fig. 5 be in the present invention the reaction time on the impact of ammonia nitrogen absorption effect.
Fig. 6 be in the present invention adsorbent amount on the impact of ammonia nitrogen absorption effect.
Detailed description of the invention
The middle Low Concentration Ammonia Containing Wastewater of indication of the present invention refers to the waste water of ammonia nitrogen concentration within the scope of 50 ~ 150 mg/L.
Embodiment one:
Wood chip mass percent is 99.7%, Fe (OH)
3mass percent is 0.3%.
Preparation plating iron wood chip: wood pellet particle diameter 198 ~ 350 μm of mass percents account for 81%, and concentration is the FeCl of 0.15 mol/L
3solution and NaOH solution react the Fe (OH) generated
3suspension, then by wood chip and Fe (OH)
3after suspension fully mixes with the ratio of solid-to-liquid ratio 1.0 g/10 mL, hydrothermal treatment consists 2 h at temperature 40 DEG C, product is through being washed to neutrality, and suction filtration, dries, obtain plating iron wood chip adsorbent.
Plating iron wood chip adsorbent purified treatment ammonia nitrogen waste water: initial NH in waste water
4 +-N, COD concentration are respectively 102 mg/L and 355 mg/L, and reaction temperature controls at 25 DEG C, and regulate wastewater pH 9, plating iron wood chip adsorbent amount 3 g/L, measures ammonia nitrogen concentration 10 mg/L, COD 83 mg/L, NH in filtrate after reacting 30 min
4 +-N clearance reaches 90.2%.
Embodiment two:
Wood chip mass percent is 99.4%, Fe (OH)
3mass percent is 0.6%.
Preparation plating iron wood chip: wood pellet particle diameter 198 ~ 350 μm of mass percents account for 85%, and concentration is the FeCl of 0.20 mol/L
3solution and NaOH solution react the Fe (OH) generated
3suspension, then by wood chip and Fe (OH)
3after suspension fully mixes with the ratio of solid-to-liquid ratio 0.8 g/10 mL, hydrothermal treatment consists 3 h at temperature 30 DEG C, product is through being washed to neutrality, and suction filtration, dries, obtain plating iron wood chip adsorbent.
Plating iron wood chip adsorbent purified treatment ammonia nitrogen waste water: initial NH in waste water
4 +-N, Zn
2+concentration is respectively 94 mg/L and 4.5 mg/L, and reaction temperature controls at 35 DEG C, and regulate wastewater pH 10, adsorbent amount 3.5 g/L, measures ammonia nitrogen concentration 9 mg/L, Zn in filtrate after reacting 40 min
2+1.2 mg/L, NH
4 +-N clearance reaches 90.4%.
Embodiment three:
Wood chip mass percent is 99.4%, Fe (OH)
3mass percent is 0.6%.
Preparation plating iron wood chip: wood pellet particle diameter 198 ~ 350 μm of mass percents account for 85%, and concentration is the FeCl of 0.20 mol/L
3solution and NaOH solution react the Fe (OH) generated
3suspension, then by wood chip and Fe (OH)
3after suspension fully mixes with the ratio of solid-to-liquid ratio 0.8 g/10 mL, hydrothermal treatment consists 1.5 h at temperature 50 DEG C, product is through being washed to neutrality, and suction filtration, dries, obtain plating iron wood chip adsorbent.
Plating iron wood chip adsorbent purified treatment ammonia nitrogen waste water: initial NH in waste water
4 +-N, AsO
4 3-concentration is respectively 147 mg/L and 0.9 mg/L, and reaction temperature controls at 28 DEG C, and regulate wastewater pH 9, adsorbent amount 4.8 g/L, measures ammonia nitrogen concentration 13 mg/L, AsO in filtrate after reacting 30 min
4 3-0.3 mg/L, NH
4 +-N clearance reaches 91.2%.
Embodiment four:
Wood chip mass percent is 99.0%, Fe (OH)
3mass percent is 1.0%.
Preparation plating iron wood chip: wood pellet particle diameter 198 ~ 350 μm of mass percents account for 83%, and concentration is the FeCl of 0.25 mol/L
3solution and NaOH solution react the Fe (OH) generated
3suspension, then by wood chip and Fe (OH)
3after suspension fully mixes with the ratio of solid-to-liquid ratio 0.6 g/10 mL, hydrothermal treatment consists 2 h at temperature 45 DEG C, product is through being washed to neutrality, and suction filtration, dries, obtain plating iron wood chip adsorbent.
Plating iron wood chip adsorbent purified treatment ammonia nitrogen waste water: initial NH in waste water
4 +-N, COD, AsO
4 3-concentration is respectively 55 mg/L, 253 mg/L and 0.7 mg/L, and reaction temperature controls at 32 DEG C, and regulate wastewater pH 11, adsorbent amount 4 g/L, measures ammonia nitrogen concentration 5 mg/L, COD 69 mg/L, AsO in filtrate after reacting 50 min
4 3-0.3 mg/L, NH
4 +-N clearance reaches 90.9%.
Claims (4)
1. a plating iron wood chip adsorbent, is characterized in that: by wood chip, Fe (OH)
3composition, wherein wood chip mass percent Wei≤99%, Fe (OH)
3mass percent Wei≤1%;
The preparation technology of the wood chip of plating iron simultaneously adsorbent carries out according to the following steps: wood chip is first washed through 1-3 times to remove silt, mechanical admixture, dries and pulverizes, sieve, make wood pellet particle diameter account for quality hundred points of number≤80% at 198 ~ 350 μm; Be the FeCl of 0.15 ~ 0.25mol/L by concentration afterwards
3solution and NaOH solution are reacted and are generated Fe (OH)
3suspension; To be sieved wood chip and Fe (OH) again
3suspension fully mixes with the ratio of solid-to-liquid ratio 0.6 ~ 1.0g/10mL, hydrothermal treatment consists 1.5 ~ 3h at temperature 30 ~ 50 DEG C, and product is through being washed to neutrality, and suction filtration, dries.
2. a plating iron wood chip absorbent preparation technique, is characterized in that: comprise the following steps: wood chip is first washed through 1-3 times to remove silt, mechanical admixture, dries and pulverizes, sieve, make wood pellet particle diameter account for quality hundred points of number≤80% at 198 ~ 350 μm; Be the FeCl of 0.15 ~ 0.25mol/L by concentration afterwards
3solution and NaOH solution are reacted and are generated Fe (OH)
3suspension; To be sieved wood chip and Fe (OH) again
3suspension fully mixes with the ratio of solid-to-liquid ratio 0.6 ~ 1.0g/10mL, hydrothermal treatment consists 1.5 ~ 3h at temperature 30 ~ 50 DEG C, and product is through being washed to neutrality, and suction filtration, dries.
3. a kind of plating iron wood chip absorbent preparation technique according to claim 2, it is characterized in that: optimum process condition is: wood pellet particle diameter accounts for quality Bai Fen Shuo≤85% at 198 ~ 350 μm, is the FeCl of 0.15mol/L by concentration
3solution and NaOH solution are reacted and are generated Fe (OH)
3suspension, then by wood chip and Fe (OH)
3suspension fully mixes with the ratio of solid-to-liquid ratio 1.0g/10mL, hydrothermal treatment consists 2h at temperature 40 DEG C, and product is through being washed to neutrality, and suction filtration, dries.
4. Low Concentration Ammonia Containing Wastewater method in a purification, it is characterized in that: comprise the following steps: regulate ammonia nitrogen waste water pH to be 9 ~ 11, plating iron wood chip adsorbent amount 3 ~ 5g/L, reaction temperature 25 ~ 35 DEG C, after ammonia nitrogen waste water and plating iron wood chip adsorbent hybrid reaction time 20 ~ 50min, filter.
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| CN104138748A (en) * | 2014-08-07 | 2014-11-12 | 黄山学院 | Compound biosorbent capable of greatly improving capability of adsorbing heavy metal by waste biomasses and preparation method thereof |
| CN104573273B (en) * | 2015-01-27 | 2017-05-24 | 江西理工大学 | Building method of modified bioadsorbent structure-activity relationship model and application thereof |
| CN106146758B (en) * | 2016-07-08 | 2019-01-15 | 中国地质大学（武汉） | A kind of method that ultraviolet light-initiated sawdust surface grafting functional polymer prepares cation adsorbing material |
| CN108212086A (en) * | 2018-01-19 | 2018-06-29 | 北京师范大学 | For the modified activated carbon absorbent and its preparation process of Adsorption ammonia nitrogen |
| CN109364926B (en) * | 2018-12-14 | 2021-05-28 | 国网山东省电力公司电力科学研究院 | Preparation method of catalyst for removing ammonia nitrogen in desulfurization wastewater through Fenton-like reaction |
| CN113003770A (en) * | 2021-03-04 | 2021-06-22 | 江西理工大学 | Method for stably, circularly and efficiently treating salt-containing ammonia nitrogen wastewater by using ligand exchange adsorbent |
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