CN104909425A - 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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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 industry the most ancient in human history, and after the Industrial Revolution of 18th century, Iron And Steel Industry develops rapidly and 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 also on the increase; At present, the method removing ammonia nitrogen in waste water is a lot, as ion-exchange method is selected NH
4 +ion has the zeolite in return resin of very strong selectivity, thus reach the object removing ammonia nitrogen, although this method technique is simple, reduced investment clearance is high, be only applicable to the ammonia nitrogen waste water of middle lower concentration, the ammonia nitrogen waste water for high density can cause operational difficulty because resin regeneration is frequent; Break point chlorination is also had to be chlorine or clorox are passed into the chemical denitrification process in waste water, the NH3-N in waste water being oxidized to N2, comparatively economy, treatment effect is used to stablize, not by Water Temperature, but invest less, working cost is high, by product chloramines and chlorinated organics can cause secondary pollution, are only applicable to process Low Concentration Ammonia Containing Wastewater; Also such as publication number is CN102060399A, name is called " the removing ammonia nitrogen device of organic composite denitrfying agent process high-concentration ammonia nitrogenous wastewater ", this patent removes high-concentration ammonia nitrogen in waste water by adding organic Composite denitrification agent, although operation of the present invention is easy, nitric efficiency for high-concentration ammonia nitrogenous wastewater is high, but the present invention combines with blow-off method, there is ammonia emission and cause secondary pollution in wastewater treatment process; Efficient, economic, stable, that treatment technology that is that do not produce the process ammonia nitrogen in high density of secondary pollution is Future Development direction can be accomplished so a kind of.
Summary of the invention
The technical problem that the present invention mainly solves: there is ammonia emission in conjunction with blow-off method in high-concentration ammonia nitrogenous wastewater treating processes for current organic composite denitrfying agent, cause secondary environmental pollution problem, provide a kind of organic composite denitrfying agent modification magnesium-aluminum-iron hydrotalcite nano magnetic adsorptive material, absorption high-concentration ammonia nitrogen in waste water, and saturated after can aging sorbing material top layer, under externally-applied magnetic field and current scour effect, realize the renewal of sorbing material, without the need to regeneration; Save energy consumption, reduced cost, high-concentration ammonia nitrogen in waste water can have been removed efficiently.
For solving the problems of the technologies described above, the present invention adopts technical scheme as described below: organic composite denitrfying agent modification magnesium-aluminum-iron hydrotalcite magnetic nano adsorption material preparation process is:
(1) magnesium-aluminum-iron hydrotalcite preparation: take 4.8 ~ 10.3g magnesium nitrate, 4.2 ~ 7.5g aluminum nitrate respectively, 5.5 ~ 13.9g iron nitrate is dissolved in 220 ~ 380ml and contains in the ethanol solution of 3.6 ~ 7.2g urea, stirred at ambient temperature 1h, pour in hydrothermal reaction kettle and be heated to 140 DEG C, reaction 13 ~ 15h, be cooled to room temperature, with after ethanol and washed with de-ionized water three times at 60 DEG C dry 6h, obtain nano magnalium molten iron talcum;
(2) magnetize: be concentrated hydrochloric acid and the saturated potassium hydroxide solution immersion 8h of 36.5% successively by mass concentration by the nano magnalium molten iron talcum of above-mentioned preparation, be placed in retort furnace, dry at temperature is 105 DEG C, near magnetic field magnetisation;
(3) modification: the nano magnalium molten iron talc materials after pickling, alkali leaching and magnetization is immersed in 10 ~ 40g organic composite denitrfying agent, stirs 25 ~ 65min;
(4) dry: by modified nano magnalium molten iron talc materials washed with de-ionized water 3 times, dry under nitrogen protection condition;
(5) activate: at temperature is 800 DEG C ~ 900 DEG C, calcine 4 ~ 6h.
Described organic composite denitrfying agent is: oxaloacetic acid, potassium oxalate, octadecyl acrylate three kinds, by quality ratio: 10% ~ 30% oxaloacetic acid, 20% ~ 45% potassium oxalate, 15% ~ 70% octadecyl acrylate.
A kind of embody rule method processing Metallurgical Waste Water middle and high concentration ammonia nitrogen:
(1) by the organic composite denitrfying agent modification magnesium-aluminum-iron hydrotalcite magnetic nano adsorption material prepared and tackiness agent in mass ratio 5:1 be made into viscous fluid, by even for viscous fluid Tu in plastic hollow microballoon top layer, coat-thickness is 4 ~ 7cm;
(2) by the plastic hollow microballoon of coated viscous fluid under ventilation state after dry 9 ~ 17min, be placed in adsorption tower, every layer of mounting height is 15 ~ 60cm, space height is 40 ~ 85cm, ammonia nitrogen concentration is allowed to be that the Metallurgical Waste Water of 2000 ~ 6000mg/L flows through in adsorption tower, flow rate control 7 ~ 18m
3/ h, stops 25 ~ 60min in adsorption tower, and the absorption of organic composite denitrfying agent is constantly tending towards saturated, and magnesium-aluminum-iron hydrotalcite magnetic nano adsorption material top layer is constantly aging;
(3) under the effect of washing away with externally-applied magnetic field of Metallurgical Waste Water current, aging sorbing material top layer comes off layer by layer;
(4) finally ammonia-nitrogen content in water outlet waste water is measured.
Described tackiness agent by weight proportioning is: 35 parts of glycerol, 15 parts of polyoxyethylene glycol, 30 parts of citric acids and 20 parts of boric acid.
Principle of the present invention: it is large that magnesium-aluminum-iron hydrotalcite material has specific surface area, belong to mesoporous material material, to ammonia nitrogen in waste water, there is absorption property through organic composite denitrfying agent is modified, the more important thing is, adding of organic composite denitrfying agent, can come off layer by layer voluntarily after sorbing material absorption ammonia nitrogen can be made to reach capacity, realize the renewal on sorbing material surface, again adsorb the ammonia nitrogen in high density in waste water, and the residue after coming off is separated with externally-applied magnetic field effect in current scour.
The present invention is compared with additive method, and Advantageous Effects is:
(1) the organic composite denitrfying agent modification magnesium-aluminum-iron hydrotalcite magnetic nano adsorption material absorption high-concentration ammonia nitrogen in waste water prepared, and saturated after can aging sorbing material top layer, under externally-applied magnetic field and current scour effect, realize the renewal of sorbing material, without the need to regeneration;
(2) after coming off, residue is little without moisture, volume, separable under externally-applied magnetic field, and sorbing material is without the need to regeneration, and clearance is high, cost is low;
(3) for Metallurgical Waste Water water quality situation, selected the organic composite denitrfying agent that oxaloacetic acid, potassium oxalate, octadecyl acrylate are made, it add can make sorbing material adsorb ammonia nitrogen reach capacity after can come off layer by layer voluntarily, with strong points;
(4) ammonia can not be produced and enter air also without precipitating generation, can not secondary environmental pollution being caused.
Embodiment
Organic composite denitrfying agent modification magnesium-aluminum-iron hydrotalcite magnetic nano adsorption material preparation of the present invention: take 4.8 ~ 10.3g magnesium nitrate, 4.2 ~ 7.5g aluminum nitrate first respectively, 5.5 ~ 13.9g iron nitrate is dissolved in 220 ~ 380ml and contains in the ethanol solution of 3.6 ~ 7.2g urea, stirred at ambient temperature 1h, pour in hydrothermal reaction kettle and be heated to 140 DEG C, reaction 13 ~ 15h, be cooled to room temperature, with after ethanol and washed with de-ionized water three times at 60 DEG C dry 6h, obtain nano magnalium molten iron talcum; Be concentrated hydrochloric acid and the saturated potassium hydroxide solution immersion 8h of 36.5% successively by mass concentration by the nano magnalium molten iron talcum of above-mentioned preparation, be placed in retort furnace, dry at temperature is 105 DEG C, near magnetic field magnetisation; Nano magnalium molten iron talc materials after pickling, alkali leaching and magnetization is immersed in 10 ~ 40g organic composite denitrfying agent, stirs 25 ~ 65min; By modified nano magnalium molten iron talc materials washed with de-ionized water 3 times, dry under nitrogen protection condition; 4 ~ 6h is calcined at temperature is 800 DEG C ~ 900 DEG C.
Described organic composite denitrfying agent is: oxaloacetic acid, potassium oxalate, octadecyl acrylate three kinds, by quality ratio: 10% ~ 30% oxaloacetic acid, 20% ~ 45% potassium oxalate, 15% ~ 70% octadecyl acrylate;
A kind of embody rule method processing Metallurgical Waste Water middle and high concentration ammonia nitrogen: first by the organic composite denitrfying agent modification magnesium-aluminum-iron hydrotalcite magnetic nano adsorption material prepared and tackiness agent in mass ratio 5:1 be made into viscous fluid, by viscous fluid Tu in plastic hollow microballoon top layer, Tu layer thickness is 4 ~ 7cm; By the tiny balloon of coated viscous fluid under ventilation state after dry 9 ~ 17min, be placed in adsorption tower, every layer of mounting height is 15 ~ 60cm, and space height is 40 ~ 85cm, ammonia nitrogen concentration is allowed to be that the Metallurgical Waste Water of 2000 ~ 6000mg/L flows through in adsorption tower, flow rate control 7 ~ 18m
3/ h, stops 25 ~ 60min in adsorption tower, and the absorption of organic composite denitrfying agent is constantly tending towards saturated, and magnesium-aluminum-iron hydrotalcite magnetic nano adsorption material top layer is constantly aging; Under the effect of washing away with externally-applied magnetic field of Metallurgical Waste Water current, aging sorbing material top layer comes off layer by layer; Finally measure ammonia-nitrogen content in water outlet waste water.
Described tackiness agent by weight proportioning is: 35 parts of glycerol, 15 parts of polyoxyethylene glycol, 30 parts of citric acids and 20 parts of boric acid.
Example 1
First 4.8g magnesium nitrate, 4.2g aluminum nitrate is taken respectively, 5.5g iron nitrate is dissolved in 220ml and contains in the ethanol solution of 3.6g urea, stirred at ambient temperature 1h, pour in hydrothermal reaction kettle and be heated to 140 DEG C, reaction 13h, be cooled to room temperature, with after ethanol and washed with de-ionized water three times at 60 DEG C dry 6h, obtain nano magnalium molten iron talcum; Be concentrated hydrochloric acid and the saturated potassium hydroxide solution immersion 8h of 36.5% successively by mass concentration by the nano magnalium molten iron talcum of above-mentioned preparation, be placed in retort furnace, dry at temperature is 105 DEG C, near magnetic field magnetisation; Nano magnalium molten iron talc materials after pickling, alkali leaching and magnetization is immersed in 1g oxaloacetic acid, 2g potassium oxalate and 7g octadecyl acrylate, stirs 25min; By modified nano magnalium molten iron talc materials washed with de-ionized water 3 times, dry under nitrogen protection condition; 4h is calcined at temperature is 800 DEG C; By the organic composite denitrfying agent modification magnesium-aluminum-iron hydrotalcite magnetic nano adsorption material prepared and tackiness agent in mass ratio 5:1 be made into viscous fluid, by viscous fluid Tu in tiny balloon top layer, coat-thickness is 4cm; The tiny balloon of coated viscous fluid after dry 9min, is placed in adsorption tower under ventilation state, and every layer of tiny balloon mounting height is 15cm, and space height is 40cm, allows ammonia nitrogen concentration be that the Metallurgical Waste Water of 2000mg/L flows through in adsorption tower, flow rate control 7m
3/ h, stops 25min in adsorption tower, and the absorption of organic composite denitrfying agent is constantly tending towards saturated, and magnesium-aluminum-iron hydrotalcite magnetic nano adsorption material top layer is constantly aging; Under the effect of washing away with externally-applied magnetic field of Metallurgical Waste Water current, aging sorbing material top layer comes off layer by layer; Finally measure ammonia-nitrogen content in water outlet waste water and be reduced to 0.15mg/L from 2000mg/L, clearance reaches more than 99.99%.
Example 2
First 8.1g magnesium nitrate, 5.8g aluminum nitrate is taken respectively, 9.7g iron nitrate is dissolved in 310ml and contains in the ethanol solution of 5.3g urea, stirred at ambient temperature 1h, pour in hydrothermal reaction kettle and be heated to 140 DEG C, reaction 14h, be cooled to room temperature, with after ethanol and washed with de-ionized water three times at 60 DEG C dry 6h, obtain nano magnalium molten iron talcum; Be concentrated hydrochloric acid and the saturated potassium hydroxide solution immersion 8h of 36.5% successively by mass concentration by the nano magnalium molten iron talcum of above-mentioned preparation, be placed in retort furnace, dry at temperature is 105 DEG C, near magnetic field magnetisation; Nano magnalium molten iron talc materials after pickling, alkali leaching and magnetization is immersed in 6g oxaloacetic acid, 8g potassium oxalate and 6g octadecyl acrylate, stirs 40min; By modified nano magnalium molten iron talc materials washed with de-ionized water 3 times, dry under nitrogen protection condition; 5h is calcined at temperature is 850 DEG C; By the organic composite denitrfying agent modification magnesium-aluminum-iron hydrotalcite magnetic nano adsorption material prepared and tackiness agent in mass ratio 5:1 be made into viscous fluid, by viscous fluid Tu in tiny balloon top layer, coat-thickness is 6cm; The tiny balloon of coated viscous fluid after dry 12min, is placed in adsorption tower under ventilation state, and every layer of tiny balloon mounting height is 40cm, and space height is 60cm, allows ammonia nitrogen concentration be that the Metallurgical Waste Water of 4000mg/L flows through in adsorption tower, flow rate control 12m
3/ h, stops 45min in adsorption tower, and the absorption of organic composite denitrfying agent is constantly tending towards saturated, and magnesium-aluminum-iron hydrotalcite magnetic nano adsorption material top layer is constantly aging; Under the effect of washing away with externally-applied magnetic field of Metallurgical Waste Water current, aging sorbing material top layer comes off layer by layer; Finally measure ammonia-nitrogen content in water outlet waste water and be reduced to 0.25mg/L from 4000mg/L, clearance reaches more than 99.99%.
Example 3
First 10.3g magnesium nitrate, 7.5g aluminum nitrate is taken respectively, 13.9g iron nitrate is dissolved in 380ml and contains in the ethanol solution of 7.2g urea, stirred at ambient temperature 1h, pour in hydrothermal reaction kettle and be heated to 140 DEG C, reaction 15h, be cooled to room temperature, with after ethanol and washed with de-ionized water three times at 60 DEG C dry 6h, obtain nano magnalium molten iron talcum; Be concentrated hydrochloric acid and the saturated potassium hydroxide solution immersion 8h of 36.5% successively by mass concentration by the nano magnalium molten iron talcum of above-mentioned preparation, be placed in retort furnace, dry at temperature is 105 DEG C, near magnetic field magnetisation; Nano magnalium molten iron talc materials after pickling, alkali leaching and magnetization is immersed in 12g oxaloacetic acid, 8g potassium oxalate and 20g octadecyl acrylate, stirs 65min; By modified nano magnalium molten iron talc materials washed with de-ionized water 3 times, dry under nitrogen protection condition; 6h is calcined at temperature is 900 DEG C; By the organic composite denitrfying agent modification magnesium-aluminum-iron hydrotalcite magnetic nano adsorption material prepared and tackiness agent in mass ratio 5:1 be made into viscous fluid, by viscous fluid Tu in tiny balloon top layer, coat-thickness is 7cm; The tiny balloon of coated viscous fluid after dry 17min, is placed in adsorption tower under ventilation state, and every layer of tiny balloon mounting height is 60cm, and space height is 85cm, allows ammonia nitrogen concentration be that the Metallurgical Waste Water of 6000mg/L flows through in adsorption tower, flow rate control 18m
3/ h, stops 60min in adsorption tower, and the absorption of organic composite denitrfying agent is constantly tending towards saturated, and magnesium-aluminum-iron hydrotalcite magnetic nano adsorption material top layer is constantly aging; Under the effect of washing away with externally-applied magnetic field of Metallurgical Waste Water current, aging sorbing material top layer comes off layer by layer; Finally measure ammonia-nitrogen content in water outlet waste water and be reduced to 0.45mg/L from 6000mg/L, clearance reaches more than 99.99%.
Claims (4)
1. process a method for Metallurgical Waste Water middle and high concentration ammonia nitrogen, it is characterized in that organic composite denitrfying agent modification magnesium-aluminum-iron hydrotalcite magnetic nano adsorption material preparation process is:
(1) magnesium-aluminum-iron hydrotalcite preparation: take 4.8 ~ 10.3g magnesium nitrate, 4.2 ~ 7.5g aluminum nitrate respectively, 5.5 ~ 13.9g iron nitrate is dissolved in 220 ~ 380ml and contains in the ethanol solution of 3.6 ~ 7.2g urea, stirred at ambient temperature 1h, pour in hydrothermal reaction kettle and be heated to 140 DEG C, reaction 13 ~ 15h, be cooled to room temperature, with after ethanol and washed with de-ionized water three times at 60 DEG C dry 6h, obtain nano magnalium molten iron talcum;
(2) magnetize: be concentrated hydrochloric acid and the saturated potassium hydroxide solution immersion 8h of 36.5% successively by mass concentration by the nano magnalium molten iron talcum of above-mentioned preparation, be placed in retort furnace, dry at temperature is 105 DEG C, near magnetic field magnetisation;
(3) modification: the nano magnalium molten iron talc materials after pickling, alkali leaching and magnetization is immersed in 10 ~ 40g organic composite denitrfying agent, stirs 25 ~ 65min;
(4) dry: by modified nano magnalium molten iron talc materials washed with de-ionized water 3 times, dry under nitrogen protection condition;
(5) activate: at temperature is 800 DEG C ~ 900 DEG C, calcine 4 ~ 6h.
2. a kind of method processing Metallurgical Waste Water middle and high concentration ammonia nitrogen according to claim 1, it is characterized in that: described organic composite denitrfying agent is: oxaloacetic acid, potassium oxalate, octadecyl acrylate three kinds, by quality ratio: 10% ~ 30% oxaloacetic acid, 20% ~ 45% potassium oxalate, 15% ~ 70% octadecyl acrylate.
3. process a method for Metallurgical Waste Water middle and high concentration ammonia nitrogen, it is characterized in that embody rule method is:
(1) by the organic composite denitrfying agent modification magnesium-aluminum-iron hydrotalcite magnetic nano adsorption material prepared and tackiness agent in mass ratio 5:1 be made into viscous fluid, by even for viscous fluid Tu in plastic hollow microballoon top layer, coat-thickness is 4 ~ 7cm;
(2) by the plastic hollow microballoon of coated viscous fluid under ventilation state after dry 9 ~ 17min, be placed in adsorption tower, every layer of mounting height is 15 ~ 60cm, space height is 40 ~ 85cm, ammonia nitrogen concentration is allowed to be that the Metallurgical Waste Water of 2000 ~ 6000mg/L flows through in adsorption tower, flow rate control 7 ~ 18m
3/ h, stops 25 ~ 60min in adsorption tower, and the absorption of organic composite denitrfying agent is constantly tending towards saturated, and magnesium-aluminum-iron hydrotalcite magnetic nano adsorption material top layer is constantly aging;
(3) under the effect of washing away with externally-applied magnetic field of Metallurgical Waste Water current, aging sorbing material top layer comes off layer by layer;
(4) finally ammonia-nitrogen content in water outlet waste water is measured.
4. a kind of method processing Metallurgical Waste Water middle and high concentration ammonia nitrogen according to claim 3, is characterized in that: described tackiness agent by weight proportioning is: 35 parts of glycerol, 15 parts of polyoxyethylene glycol, 30 parts of citric acids and 20 parts of boric acid.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2006075815A (en) * | 2004-09-13 | 2006-03-23 | Shimane Univ | Molding for denitrifying/dephosphorizing and method for denitrifying/dephosphorizing sewage or waste water |
| CN102060399A (en) * | 2010-11-30 | 2011-05-18 | 常州大学 | Ammonia nitrogen removing device assisting organic compound denitrifier in treating high concentration ammonia nitrogen wastewater |
| CN104261547A (en) * | 2014-10-10 | 2015-01-07 | 武汉工程大学 | Hydrotalcite magnetite composite water treatment material |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2006075815A (en) * | 2004-09-13 | 2006-03-23 | Shimane Univ | Molding for denitrifying/dephosphorizing and method for denitrifying/dephosphorizing sewage or waste water |
| CN102060399A (en) * | 2010-11-30 | 2011-05-18 | 常州大学 | Ammonia nitrogen removing device assisting organic compound denitrifier in treating high concentration ammonia nitrogen wastewater |
| CN104261547A (en) * | 2014-10-10 | 2015-01-07 | 武汉工程大学 | Hydrotalcite magnetite composite water treatment material |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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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