CN104909425B - Method used for treating high concentration ammonia nitrogen in metallurgical waste water - Google Patents
Method used for treating high concentration ammonia nitrogen in metallurgical waste water Download PDFInfo
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- CN104909425B CN104909425B CN201510272156.XA CN201510272156A CN104909425B CN 104909425 B CN104909425 B CN 104909425B CN 201510272156 A CN201510272156 A CN 201510272156A CN 104909425 B CN104909425 B CN 104909425B
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Abstract
The invention discloses a method used for treating high concentration ammonia nitrogen in metallurgical waste water, and belongs to the field of metallurgical waste water treatment. According to the method, an organic composite denitrification agent modified magnesium aluminum iron hydrotalcite magnetic nano adsorptive material is prepared via magnetization, modification, drying, and activation, and then adsorption rods are prepared and are arranged in an adsorption tower to treat high concentration ammonia nitrogen in metallurgical waste water. In removing processes, high concentration ammonia nitrogen in waste water is absorbed, after saturation, aging of the surface layer of the adsorption material is realized, and updating of the adsorption material is realized under the action of an applied magnetic field and flow scour, and regeneration is not needed. After shedding, an obtained residue is waterless, and is small in volume; no ammonia gas is generated or released into the atmosphere; no precipitate is obtained; and no environmental secondary pollution is caused. Separation can be realized under the action of the applied magnetic field; ammonia nitrogen concentration is reduce to 0.45mg/L from 2000-6000mg/L; ammonia nitrogen removing ratio is higher than 99.99%; and the method can be used for treating waste water with high concentration ammonia nitrogen, and possesses a promising prospect.
Description
Technical field
The present invention relates to a kind of method of ammonia nitrogen in high density, especially metallurgy waste water treatment technical field.
Background technology
Metallurgical industry is one of the most ancient industry in human history, and after the Industrial Revolution of 18th century, steel and iron industry is sent out rapidly
Exhibition causes serious pollution, and after entering for 20th century, metallurgical production scale increases rapidly, and the content of high-concentration ammonia nitrogen in waste water is not yet
Break and increase；At present, the method removing ammonia nitrogen in waste water is a lot, and such as ion exchange method is to nh4 +Ion has very strong selectivity
Zeolite as exchanger resin, thus reaching the purpose removing ammonia nitrogen, although this method process is simple, reduced investment clearance
Height, but it is only applicable to the ammonia nitrogen waste water of middle low concentration, the ammonia nitrogen waste water for high concentration frequently can cause to grasp because of resin regeneration
Make difficult；Break point chlorination is also had to be that chlorine or sodium hypochlorite are passed through the change that the nh3-n in waste water is oxidized in waste water n2
Learn denitrification process, stable using relatively inexpensive, treatment effect, it is not subject to Water Temperature, but investment is less, operating cost is high, by-product
Thing chloramines and chlorinated organics can cause secondary pollution, be only applicable to process Low Concentration Ammonia Containing Wastewater；Also such as Publication No.
Cn102060399a, entitled " organic composite denitrifier process high-concentration ammonia nitrogenous wastewater except ammonia nitrogen device ", this patent is passed through
Add organic Composite denitrification agent and remove high-concentration ammonia nitrogen in waste water although present invention operation is easy and simple to handle, for ammonia nitrogen in high density
The nitric efficiency of waste water is high, but the present invention is to combine with blow-off method, there is ammonia emission and cause in wastewater treatment process
Secondary pollution；So a kind of process skill that can accomplish process ammonia nitrogen in high density that is efficient, economic, stable, not producing secondary pollution
Art is the direction of Future Development.
Content of the invention
Present invention mainly solves technical problem: for current organic composite denitrifier combine blow-off method in ammonia nitrogen in high density
There is ammonia emission in wastewater treatment process, cause secondary environmental pollution problem, there is provided a kind of organic composite denitrifier is modified
Magnesium-aluminum-iron hydrotalcite nano magnetic adsorptive material, the aging adsorbing material top layer of energy after absorption high-concentration ammonia nitrogen in waste water, and saturation,
Under externally-applied magnetic field and current scour act on, realize the renewal of adsorbing material, need not regenerate；Save energy consumption, reduce cost,
High-concentration ammonia nitrogen in waste water can efficiently be removed.
For solving above-mentioned technical problem, the present invention adopts technical scheme as described below: organic composite denitrifier modification magnesium
Ferro-aluminum brucite magnetic nano adsorption material preparation process is:
(1) magnesium-aluminum-iron brucite preparation: weigh 4.8～10.3g magnesium nitrate, 4.2～7.5g aluminum nitrate respectively, 5.5～
13.9g ferric nitrate is dissolved in the ethanol solution that 220～380ml contains 3.6～7.2g carbamide, stirs 1h, under room temperature
Enter to be heated to 140 DEG C in hydrothermal reaction kettle, react 13～15h, be cooled to room temperature, cleaned with ethanol and deionized water after three times
6h is dried at 60 DEG C, obtains nano magnalium molten iron Talcum；
(2) magnetize: by the nano magnalium molten iron Talcum of above-mentioned preparation be 36.5% with mass concentration successively concentrated hydrochloric acid and
Saturation potassium hydroxide solution soaks 8h, is placed in Muffle furnace, dries at temperature is 105 DEG C, near magnetic field magnetization；
(3) modified: the nano magnalium molten iron talc materials after pickling, alkali leaching and magnetization to be immersed 10～40g organic multiple
Close in denitrifier, stir 25～65min；
(4) dry: modified nano magnalium molten iron talc materials deionized water is cleaned 3 times, in nitrogen ceiling
Dry under part；
(5) activate: at temperature is 800 DEG C～900 DEG C, calcine 4～6h, you can.
Described organic composite denitrifier is: oxaloacetic acid, potassium oxalate, three kinds of octadecyl acrylate, by quality ratio:
10%～30% oxaloacetic acid, 20%～45% potassium oxalate, 15%～70% octadecyl acrylate.
A kind of concrete application method processing Metallurgical Waste Water middle and high concentration ammonia nitrogen:
(1) by the organic composite preparing denitrifier modification magnesium-aluminum-iron brucite magnetic nano adsorption material and adhesive
5:1 is made into viscous fluid in mass ratio, and by viscous fluid uniformly in plastic hollow microsphere top layer, coating layer thickness is 4～7cm；
(2) the plastic hollow microsphere of coated viscous fluid is dried after 9～17min under ventilation state, is placed in adsorption tower,
Every layer of setting height(from bottom) is 15～60cm, and space height is 40～85cm, allows the metallurgy that ammonia nitrogen concentration is 2000～6000mg/l to give up
Water flows through in adsorption tower, flow speed control 7～18m3/ h, stops 25～60min in adsorption tower, and organic composite denitrifier adsorbs not
Break and tend to saturation, magnesium-aluminum-iron brucite magnetic nano adsorption material top layer is constantly aging；
(3) Metallurgical Waste Water current wash away with externally-applied magnetic field in the presence of, aging adsorbing material top layer comes off layer by layer；
(4) finally measure ammonia-nitrogen content in water outlet waste water.
Described adhesive proportioning by weight is: 35 parts of glycerol, 15 parts of Polyethylene Glycol, 30 parts of citric acids and 20 parts
Boric acid.
The principle of the present invention: magnesium-aluminum-iron hydrotalcite material has specific surface area greatly, belongs to mesoporous material material, through organic multiple
Close denitrifier modified to ammonia nitrogen in waste water, there is absorption property it is often more important that, the addition of organic composite denitrifier, can make
Obtain after adsorbing material absorption ammonia nitrogen reaches saturation and can voluntarily come off layer by layer, realize the renewal on adsorbing material surface, again adsorb useless
Ammonia nitrogen in high density in water, and the residue after coming off separates in current scour and externally-applied magnetic field effect.
Compared with additive method, Advantageous Effects are the present invention:
(1) in the organic composite denitrifier modification magnesium-aluminum-iron brucite magnetic nano adsorption material absorption waste water preparing
The aging adsorbing material top layer of energy after ammonia nitrogen in high density, and saturation, under externally-applied magnetic field and current scour act on, realizes adsorbing material
Renewal, need not regenerate；
(2) residue no moisture, small volume after coming off, separable under externally-applied magnetic field, adsorbing material need not regenerate, and removes
Rate is high, low cost；
(3) it is directed to Metallurgical Waste Water water quality situation, that has selected that oxaloacetic acid, potassium oxalate, octadecyl acrylate make is organic
Composite denitrification agent, its addition enables to voluntarily come off layer by layer after adsorbing material absorption ammonia nitrogen reaches saturation, with strong points；
(4) also no precipitation generates, is not result in secondary environmental pollution will not to produce ammonia entrance air.
Embodiment
Organic composite denitrifier modification magnesium-aluminum-iron brucite magnetic nano adsorption material preparation of the present invention: weigh respectively first
4.8～10.3g magnesium nitrate, 4.2～7.5g aluminum nitrate, 5.5～13.9g ferric nitrate be dissolved in 220～380ml contain 3.6～
In the ethanol solution of 7.2g carbamide, under room temperature stir 1h, pour into and in hydrothermal reaction kettle, be heated to 140 DEG C, reaction 13～
15h, is cooled to room temperature, is cleaned with ethanol and deionized water after three times and 6h is dried at 60 DEG C, obtains nano magnalium molten iron Talcum；
By the nano magnalium molten iron Talcum of above-mentioned preparation be 36.5% with mass concentration successively concentrated hydrochloric acid and saturation potassium hydroxide solution
Soak 8h, be placed in Muffle furnace, dry at temperature is 105 DEG C, near magnetic field magnetization；By after pickling, alkali leaching and magnetization
In nano magnalium molten iron talc materials immersion 10～40g organic composite denitrifier, stir 25～65min；By modified nanometer
Magnesium-aluminum-iron hydrotalcite material deionized water is cleaned 3 times, dries under nitrogen protective condition；At temperature is 800 DEG C～900 DEG C
Calcining 4～6h, you can.
Described organic composite denitrifier is: oxaloacetic acid, potassium oxalate, three kinds of octadecyl acrylate, by quality ratio:
10%～30% oxaloacetic acid, 20%～45% potassium oxalate, 15%～70% octadecyl acrylate；
A kind of concrete application method processing Metallurgical Waste Water middle and high concentration ammonia nitrogen: first the organic composite preparing is taken off
Nitrogen agent modification magnesium-aluminum-iron brucite magnetic nano adsorption material is made into viscous fluid, by viscous fluid with adhesive 5:1 in mass ratio
In plastic hollow microsphere top layer, thickness degree is 4～7cm；By the tiny balloon of coated viscous fluid under ventilation state be dried 9～
After 17min, it is placed in adsorption tower, every layer of setting height(from bottom) is 15～60cm, space height is 40～85cm, allow the ammonia nitrogen concentration be
The Metallurgical Waste Water of 2000～6000mg/l flows through in adsorption tower, flow speed control 7～18m3/ h, in adsorption tower stop 25～
60min, the absorption of organic composite denitrifier constantly tends to saturation, and magnesium-aluminum-iron brucite magnetic nano adsorption material top layer is constantly old
Change；Metallurgical Waste Water current wash away with externally-applied magnetic field in the presence of, aging adsorbing material top layer comes off layer by layer；Finally measure
Ammonia-nitrogen content in water outlet waste water.
Described adhesive proportioning by weight is: 35 parts of glycerol, 15 parts of Polyethylene Glycol, 30 parts of citric acids and 20 parts
Boric acid.
Example 1
Weigh 4.8g magnesium nitrate, 4.2g aluminum nitrate first respectively, 5.5g ferric nitrate is dissolved in 220ml and contains 3.6g carbamide
In ethanol solution, stir 1h under room temperature, pour into and in hydrothermal reaction kettle, be heated to 140 DEG C, react 13h, be cooled to room temperature, use
Ethanol and deionized water are dried 6h after cleaning three times at 60 DEG C, obtain nano magnalium molten iron Talcum；Nanometer by above-mentioned preparation
The concentrated hydrochloric acid that magnesium-aluminum-iron brucite is 36.5% with mass concentration successively and saturation potassium hydroxide solution soak 8h, are placed in Muffle furnace
In, dry at temperature is 105 DEG C, near magnetic field magnetization；By the nano magnalium molten iron Talcum material after pickling, alkali leaching and magnetization
In material immersion 1g oxaloacetic acid, 2g potassium oxalate and 7g octadecyl acrylate, stir 25min；By modified nano magnalium molten iron
Talc materials deionized water is cleaned 3 times, dries under nitrogen protective condition；Calcine 4h at temperature is 800 DEG C；To be prepared into
To organic composite denitrifier modification magnesium-aluminum-iron brucite magnetic nano adsorption material and adhesive 5:1 in mass ratio be made into sticky
Liquid, by viscous fluid in tiny balloon top layer, coating layer thickness is 4cm；By the tiny balloon of coated viscous fluid under ventilation state
After 9min is dried, it is placed in adsorption tower, every layer of tiny balloon setting height(from bottom) is 15cm, space height is 40cm, allow ammonia nitrogen concentration
Metallurgical Waste Water for 2000mg/l flows through in adsorption tower, flow speed control 7m3/ h, stops 25min in adsorption tower, and organic composite takes off
Nitrogen agent absorption constantly tends to saturation, and magnesium-aluminum-iron brucite magnetic nano adsorption material top layer is constantly aging；In Metallurgical Waste Water current
Wash away with externally-applied magnetic field in the presence of, aging adsorbing material top layer comes off layer by layer；Finally measure ammonia nitrogen in water outlet waste water to contain
Amount is reduced to 0.15mg/l from 2000mg/l, and clearance reaches more than 99.99%.
Example 2
Weigh 8.1g magnesium nitrate, 5.8g aluminum nitrate first respectively, 9.7g ferric nitrate is dissolved in 310ml and contains 5.3g carbamide
In ethanol solution, stir 1h under room temperature, pour into and in hydrothermal reaction kettle, be heated to 140 DEG C, react 14h, be cooled to room temperature, use
Ethanol and deionized water are dried 6h after cleaning three times at 60 DEG C, obtain nano magnalium molten iron Talcum；Nanometer by above-mentioned preparation
The concentrated hydrochloric acid that magnesium-aluminum-iron brucite is 36.5% with mass concentration successively and saturation potassium hydroxide solution soak 8h, are placed in Muffle furnace
In, dry at temperature is 105 DEG C, near magnetic field magnetization；By the nano magnalium molten iron Talcum material after pickling, alkali leaching and magnetization
In material immersion 6g oxaloacetic acid, 8g potassium oxalate and 6g octadecyl acrylate, stir 40min；By modified nano magnalium molten iron
Talc materials deionized water is cleaned 3 times, dries under nitrogen protective condition；Calcine 5h at temperature is 850 DEG C；To be prepared into
To organic composite denitrifier modification magnesium-aluminum-iron brucite magnetic nano adsorption material and adhesive 5:1 in mass ratio be made into sticky
Liquid, by viscous fluid in tiny balloon top layer, coating layer thickness is 6cm；By the tiny balloon of coated viscous fluid under ventilation state
After 12min is dried, it is placed in adsorption tower, every layer of tiny balloon setting height(from bottom) is 40cm, space height is 60cm, allow ammonia nitrogen concentration
Metallurgical Waste Water for 4000mg/l flows through in adsorption tower, flow speed control 12m3/ h, stops 45min, organic composite in adsorption tower
Denitrifier absorption constantly tends to saturation, and magnesium-aluminum-iron brucite magnetic nano adsorption material top layer is constantly aging；In Metallurgical Waste Water water
Stream wash away with externally-applied magnetic field in the presence of, aging adsorbing material top layer comes off layer by layer；Finally measure ammonia nitrogen in water outlet waste water
Content is reduced to 0.25mg/l from 4000mg/l, and clearance reaches more than 99.99%.
Example 3
Weigh 10.3g magnesium nitrate, 7.5g aluminum nitrate first respectively, 13.9g ferric nitrate is dissolved in 380ml and contains 7.2g carbamide
Ethanol solution in, under room temperature stir 1h, pour into and in hydrothermal reaction kettle, be heated to 140 DEG C, react 15h, be cooled to room temperature,
Cleaned with ethanol and deionized water after three times and 6h is dried at 60 DEG C, obtain nano magnalium molten iron Talcum；By receiving of above-mentioned preparation
The concentrated hydrochloric acid that rice magnesium-aluminum-iron brucite is 36.5% with mass concentration successively and saturation potassium hydroxide solution soak 8h, are placed in Muffle
In stove, dry at temperature is 105 DEG C, near magnetic field magnetization；By the nano magnalium molten iron Talcum after pickling, alkali leaching and magnetization
In material immersion 12g oxaloacetic acid, 8g potassium oxalate and 20g octadecyl acrylate, stir 65min；By modified nano magnalium
Molten iron talc materials deionized water is cleaned 3 times, dries under nitrogen protective condition；Calcine 6h at temperature is 900 DEG C；To make
The standby organic composite denitrifier modification magnesium-aluminum-iron brucite magnetic nano adsorption material obtaining is made into adhesive 5:1 in mass ratio
Viscous fluid, by viscous fluid in tiny balloon top layer, coating layer thickness is 7cm；By the tiny balloon of coated viscous fluid in ventilation shape
After 17min being dried under state, it is placed in adsorption tower, every layer of tiny balloon setting height(from bottom) is 60cm, space height is 85cm, allow ammonia nitrogen
Concentration is that the Metallurgical Waste Water of 6000mg/l flows through in adsorption tower, flow speed control 18m3/ h, stops 60min in adsorption tower, organic
Composite denitrification agent absorption constantly tends to saturation, and magnesium-aluminum-iron brucite magnetic nano adsorption material top layer is constantly aging；Metallurgical useless
Water current wash away with externally-applied magnetic field in the presence of, aging adsorbing material top layer comes off layer by layer；Finally measure in water outlet waste water
Ammonia-nitrogen content is reduced to 0.45mg/l from 6000mg/l, and clearance reaches more than 99.99%.
Claims (1)
1. a kind of process Metallurgical Waste Water middle and high concentration ammonia nitrogen method it is characterised in that:
(1) magnesium-aluminum-iron brucite preparation: weigh 4.8～10.3g magnesium nitrate, 4.2～7.5g aluminum nitrate, 5.5～13.9g nitre respectively
Sour dissolved ferric iron contains in the ethanol solution of 3.6～7.2g carbamide in 220～380ml, stirs 1h, pour hydro-thermal into anti-under room temperature
Answer and in kettle, be heated to 140 DEG C, react 13～15h, be cooled to room temperature, cleaned with ethanol and deionized water dry at 60 DEG C after three times
Dry 6h, obtains nano magnalium molten iron Talcum；
(2) magnetize: by the nano magnalium molten iron Talcum of above-mentioned preparation be 36.5% with mass concentration successively concentrated hydrochloric acid and saturation
Potassium hydroxide solution soaks 8h, is placed in Muffle furnace, dries at temperature is 105 DEG C, near magnetic field magnetization；
(3) modified: the nano magnalium molten iron talc materials immersion 10～40g organic composite after pickling, alkali leaching and magnetization is taken off
In nitrogen agent, stir 25～65min；Described organic composite denitrifier is: oxaloacetic acid, potassium oxalate, three kinds of octadecyl acrylate,
By quality ratio: 10%～30% oxaloacetic acid, 20%～45% potassium oxalate, 15%～70% octadecyl acrylate；
(4) dry: modified nano magnalium molten iron talc materials deionized water is cleaned 3 times, under nitrogen protective condition
Dry；
(5) activate: at temperature is 800 DEG C～900 DEG C, calcine 4～6h, you can；
(6) by the organic composite preparing denitrifier modification magnesium-aluminum-iron brucite magnetic nano adsorption material and adhesive by matter
Amount is made into viscous fluid than 5:1, and by viscous fluid uniformly in plastic hollow microsphere top layer, coating layer thickness is 4～7cm；Described glue
Stick proportioning by weight is: 35 parts of glycerol, 15 parts of Polyethylene Glycol, 30 parts of citric acids and 20 parts of boric acid；
(7) the plastic hollow microsphere of coated viscous fluid is dried after 9～17min under ventilation state, is placed in adsorption tower, every layer
Setting height(from bottom) is 15～60cm, and space height is 40～85cm, allows the Metallurgical Waste Water stream that ammonia nitrogen concentration is 2000～6000mg/l
Through in adsorption tower, flow speed control 7～18m3/ h, stops 25～60min in adsorption tower, and the absorption of organic composite denitrifier constantly becomes
In saturation, magnesium-aluminum-iron brucite magnetic nano adsorption material top layer is constantly aging；
(8) Metallurgical Waste Water current wash away with externally-applied magnetic field in the presence of, aging adsorbing material top layer comes off layer by layer；
(9) finally measure ammonia-nitrogen content in water outlet waste water.
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| CN107938412A (en) * | 2017-11-21 | 2018-04-20 | 常州思宇环保材料科技有限公司 | A kind of efficiently Winestock machine and its application process |
| CN111644147A (en) * | 2019-11-04 | 2020-09-11 | 南京工业大学 | Zeolite for adsorbing ammonia nitrogen in wastewater |
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| JP2006075815A (en) * | 2004-09-13 | 2006-03-23 | Shimane Univ | Molding for denitrifying/dephosphorizing and method for denitrifying/dephosphorizing sewage or waste water |
| CN102060399B (en) * | 2010-11-30 | 2012-12-26 | 常州大学 | Ammonia nitrogen removing device assisting organic compound denitrifier in treating high concentration ammonia nitrogen wastewater |
| CN104261547B (en) * | 2014-10-10 | 2016-03-02 | 武汉工程大学 | Hydrotalcite magnetite compound material for water treatment |
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