CN104876292A - Method for treating high-concentration ammonia nitrogen in urea - Google Patents
Method for treating high-concentration ammonia nitrogen in urea Download PDFInfo
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Abstract
The invention relates to a method for treating high-concentration ammonia nitrogen in urea and belongs to the field of wastewater treatment. The method comprises the following steps: preparing a viscous liquid by using a prepared organic compound denitrification agent modified magnesium-aluminum-iron hydrotalcite magnetic nano adsorption material and an adhesive in a mass ratio of 1:5, applying the viscous liquid to the surface of an adsorption rod, drying, putting the adsorption rod coated with the viscous liquid into an adsorption tower, enabling urea to flow through the adsorption tower until the organic compound denitrification agent modified magnesium-aluminum-iron hydrotalcite magnetic nano adsorption material on the surface of the adsorption rod adsorbs urea to be saturated, enabling aged surface layers of the organic compound denitrification agent modified magnesium-aluminum-iron hydrotalcite magnetic nano adsorption material one by one under the action of flashing of landfill leachate flow and an external magnetic field, and finally testing the content of ammonia nitrogen in wastewater. No ammonia gas can be generated to diffuse into the atmosphere, and no precipitate can be generated either, no secondary environment pollution can be caused, the adsorption material does not need to be regenerated, the ammonia nitrogen concentration is less than 1mg/L, and the removal rate is 99.99% or above.
Description
Technical field
The invention discloses a kind of method processing urine middle and high concentration ammonia nitrogen, belong to field of waste water treatment.
Background technology
Urine is slightly acidic, and pH value is about 6.5, and main component has urea, ammonia, phosphoric acid salt, organic substance, bacterium etc.And most of the nitrogen exists with the form of ammonia nitrogen in urine, the ammonia nitrogen in mankind's urine has accounted for 80% of influent ammonia nitrogen loading in wastewater treatment.A large amount of discharges of ammonia nitrogen, not only cause the phenomenons such as the pollution of water surrounding, body eutrophication and water body generation red tide, and in Industrial Wastewater Treatment and reuse project, cause the breeding of microorganism in watering equipment and form biofouling, blocking pipe and watering equipment, affect heat exchange.
At present, ammonia nitrogen in high density in process urine mainly contains By Bubble-floating Method, Shi Shuncun, ten thousand people such as august wisdom adopt the chemical by-product such as magnesia and phosphoric acid byproduct to carry out chemical floatation treatment process, ammonia nitrogen removal is effective, technical feasibility, environmental effect is obvious, but can only accomplish ammonia nitrogen in high density pretreating effect, high ammonia nitrogen in urine is removed not yet, easily produces environmental pollution.And in urine Separation Treatment Technology, first Urea Transformation is wherein ammonia nitrogen by urine hydrolytic bacteria, cause increasing sharply of pH in system.The aerial volatilization phenomenon of ammonia nitrogen can cause atmospheric pollution equally simultaneously.Also have by the method for sorbent material except ammonia nitrogen, 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, denitrfying agent solves the difficult problem that ammonia nitrogen in wastewater treatment industry is difficult to process and processing costs is high, is become by NH_3-N treating more convenient, economical and practical.Without the need to large equipment investment and transformation, dosage directly adds and can use, but the present invention combines with blow-off method, and ammonia can be caused to enter air and cause secondary pollution.
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.
In order to achieve the above object, the technical solution adopted in the present invention is:
(1) magnesium-aluminum-iron hydrotalcite preparation: take 3.8 ~ 6.0g magnesium nitrate, 4.2 ~ 9.7g aluminum nitrate respectively, 6.1 ~ 18.9g iron nitrate is dissolved in 300 ~ 500ml and contains in the ethanol solution of 4.3 ~ 7.6g urea, after stirred at ambient temperature 1h, pour in hydrothermal reaction kettle and be heated to 140 DEG C, reaction 13 ~ 14h; Be cooled to room temperature; With after ethanol and washed with de-ionized water two 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 the organic composite denitrfying agent of 10 ~ 50g, stirs 40 ~ 60min;
(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 9 ~ 00 DEG C, calcine 5 ~ 7h.
Described organic composite denitrfying agent by ethyl lactate, ethylene-acetic acid ethyl ester, aminobutyric acid three kinds, by quality ratio, the ethyl lactate of 50% ~ 60%, the ethylene-acetic acid ethyl ester of 20% ~ 40%, 10% ~ 40% aminobutyric acid.
A kind of embody rule method of urine liquid middle and high concentration ammonia nitrogen is:
(1) by the organic composite denitrfying agent modification magnesium-aluminum-iron hydrotalcite magnetic nano adsorption material prepared and tackiness agent in mass ratio 6:1 be made into viscous fluid, by viscous fluid Tu in ceramic honey comb top layer, coat-thickness is 3 ~ 6 ㎝, by the ceramic honey comb of coated viscous fluid dry 10 ~ 20min under ventilation state, described tackiness agent counts 15 parts of polyimide N,N-DIMETHYLACETAMIDEs, 35 parts of dichloromethyl dimethylbenzene, 25 parts of vinylbenzene and 25 parts of diamyl ethene with parts by weight;
(2) ceramic honey comb of coated viscous fluid is placed in adsorption tower, every layer of ceramic honey comb mounting height is 10 ~ 50 ㎝, and space height is 50 ~ 100 ㎝, allow ammonia nitrogen concentration be the urine flow of 5000 ~ 10000mg/L through adsorption tower, flow rate control 5 ~ 15m
3/ h, absorption dwell time in the tower 40 ~ 60min, until the organic composite denitrfying agent modification magnesium-aluminum-iron hydrotalcite magnetic nano adsorption material ammonia nitrogen absorption on ceramic honey comb surface reaches capacity, organic composite denitrfying agent aging magnesium-aluminum-iron hydrotalcite magnetic Nano material top layer;
(3) wash away with under externally-applied magnetic field effect at urine current, aging sorbing material top layer comes off layer by layer;
(4) ammonia-nitrogen content in last wastewater measurement water outlet.
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 invention has the beneficial effects as follows:
(1) produce without ammonia, can not secondary environmental pollution be caused;
(2) organic composite denitrfying agent modification magnesium-aluminum-iron hydrotalcite nano magnetic adsorptive material is prepared, 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.
Embodiment
First 3.8 ~ 6.0g magnesium nitrate, 4.2 ~ 9.7g aluminum nitrate is taken respectively, 6.1 ~ 18.9g iron nitrate is dissolved in 300 ~ 500ml and contains in the ethanol solution of 4.3 ~ 7.6g urea, after stirred at ambient temperature 1h, pour in hydrothermal reaction kettle and be heated to 140 DEG C, reaction 13 ~ 14h; Be cooled to room temperature; With after ethanol and washed with de-ionized water two 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 ~ 50g organic composite denitrfying agent, wherein organic composite denitrfying agent comprises the ethyl lactate of 50% ~ 60%, the ethylene-acetic acid ethyl ester of 20% ~ 40%, 10% ~ 40% aminobutyric acid, then stir 40 ~ 60min; By modified nano magnalium molten iron talc materials washed with de-ionized water 3 times, dry under nitrogen protection condition; 5 ~ 7h is calcined at temperature is 800 DEG C ~ 900 DEG C.The organic composite denitrfying agent modification magnesium-aluminum-iron hydrotalcite magnetic nano adsorption material obtained and tackiness agent in mass ratio 6:1 are made into viscous fluid, by viscous fluid Tu in ceramic honey comb top layer, coat-thickness is 3 ~ 6 ㎝, by the ceramic honey comb of coated viscous fluid dry 10 ~ 20min under ventilation state; Again the ceramic honey comb of coated viscous fluid is placed in adsorption tower, every layer of mounting height is 10 ~ 50 ㎝, and space height is 50 ~ 100 ㎝, allow ammonia nitrogen concentration be the urine flow of 5000 ~ 10000mg/L through adsorption tower, flow rate control 5 ~ 15m
3/ h, absorption dwell time in the tower 40 ~ 60min, until the organic composite denitrfying agent modification magnesium-aluminum-iron hydrotalcite magnetic nano adsorption material ammonia nitrogen absorption on ceramic honey comb surface reaches capacity, organic composite denitrfying agent aging magnesium-aluminum-iron hydrotalcite magnetic Nano material top layer; Wash away with under externally-applied magnetic field effect at urine current, aging sorbing material top layer comes off layer by layer; Ammonia-nitrogen content in last wastewater measurement water outlet.
Example 1
First 6.0g magnesium nitrate is taken respectively, 4.8g aluminum nitrate, 15.6g iron nitrate is dissolved in 350ml and contains in the ethanol solution of 7.0g urea, at room temperature stir 1h to fall back in thermal response still and be heated to 140 DEG C, reaction 12h, be cooled to room temperature, with after ethanol and washed with de-ionized water two 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% more 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, then will through pickling, alkali leaching and the nano magnalium molten iron talc materials after magnetizing are immersed in the organic composite denitrfying agent of 10g, wherein it comprises 5.0g ethyl lactate, 2.0g ethylene-acetic acid ethyl ester, 3.0g aminobutyric acid, stir 40min again, again 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 800 DEG C, organic composite denitrfying agent modification magnesium-aluminum-iron hydrotalcite magnetic nano adsorption material can be obtained, by itself and tackiness agent in mass ratio 6:1 be made into viscous fluid, by viscous fluid Tu in ceramic honey comb top layer, coat-thickness is 6 ㎝, by the ceramic honey comb of coated viscous fluid dry 15min under ventilation state, the ceramic honey comb of coated viscous fluid is placed in adsorption tower, and every layer of ceramic honey comb mounting height is 45 ㎝, and space height is 50 ㎝, allow ammonia nitrogen concentration be the urine flow of 5200mg/L through adsorption tower, flow rate control 10m
3/ h, absorption dwell time in the tower 60min, until the organic composite denitrfying agent modification magnesium-aluminum-iron hydrotalcite magnetic nano adsorption material ammonia nitrogen absorption on ceramic honey comb surface reaches capacity, organic composite denitrfying agent aging magnesium-aluminum-iron hydrotalcite magnetic Nano material top layer, wash away with under externally-applied magnetic field effect at urine current, aging sorbing material top layer comes off layer by layer, in last wastewater measurement water outlet, ammonia-nitrogen content is below 0.5mg/L, and clearance reaches more than 99.99%.
Example 2
First 5.0g magnesium nitrate is taken respectively, 5.2g aluminum nitrate, 13.6g iron nitrate is dissolved in 400ml and contains in the ethanol solution of 6.4g urea, at room temperature stir 1h to fall back in thermal response still and be heated to 140 DEG C, reaction 12h, be cooled to room temperature, with after ethanol and washed with de-ionized water two 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% more 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, then will through pickling, alkali leaching and the nano magnalium molten iron talc materials after magnetizing are immersed in the organic composite denitrfying agent of 20g, wherein it comprises 10g ethyl lactate, 4g ethylene-acetic acid ethyl ester, 6g aminobutyric acid, stir 40min, again 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 800 DEG C, organic composite denitrfying agent modification magnesium-aluminum-iron hydrotalcite magnetic nano adsorption material can be obtained, by itself and tackiness agent in mass ratio 5:1 be made into viscous fluid, by viscous fluid Tu in ceramic honey comb top layer, coat-thickness is 6 ㎝, by the ceramic honey comb of coated viscous fluid dry 15min under ventilation state, the ceramic honey comb of coated viscous fluid is placed in adsorption tower, and every layer of mounting height is 45 ㎝, and space height is 50 ㎝, allow ammonia nitrogen concentration be the urine flow of 6000mg/L through adsorption tower, flow rate control 10m
3/ h, absorption dwell time in the tower 60min, until the organic composite denitrfying agent modification magnesium-aluminum-iron hydrotalcite magnetic nano adsorption material ammonia nitrogen absorption on ceramic honey comb surface reaches capacity, organic composite denitrfying agent aging magnesium-aluminum-iron hydrotalcite magnetic Nano material top layer, wash away with under externally-applied magnetic field effect at urine current, aging sorbing material top layer comes off layer by layer, in last wastewater measurement water outlet, ammonia-nitrogen content is below 0.6mg/L, and clearance reaches more than 99.99%.
Example 3
First 7.1g magnesium nitrate is taken respectively, 4.8g aluminum nitrate, 15.6g iron nitrate is dissolved in 350ml and contains in the ethanol solution of 6.4g urea, at room temperature stir 1h to fall back in thermal response still and be heated to 140 DEG C, reaction 12h, be cooled to room temperature, with after ethanol and washed with de-ionized water two 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% more 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, then will through pickling, alkali leaching and the nano magnalium molten iron talc materials after magnetizing are immersed in the organic composite denitrfying agent of 30g, wherein it comprises 15g ethyl lactate, 6g ethylene-acetic acid ethyl ester, 9g aminobutyric acid, stir 40min, again 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 800 DEG C, organic composite denitrfying agent modification magnesium-aluminum-iron hydrotalcite magnetic nano adsorption material can be obtained, by itself and tackiness agent in mass ratio 6:1 be made into viscous fluid, by viscous fluid Tu in adsorbing bar top layer, coat-thickness is 6 ㎝, by the ceramic honey comb of coated viscous fluid dry 15min under ventilation state, the ceramic honey comb of coated viscous fluid is placed in adsorption tower, and every layer of adsorbing bar mounting height is 45 ㎝, and space height is 50 ㎝, allow ammonia nitrogen concentration be the urine flow of 7500mg/L through adsorption tower, flow rate control 10m
3/ h, absorption dwell time in the tower 60min, until the organic composite denitrfying agent modification magnesium-aluminum-iron hydrotalcite magnetic nano adsorption material ammonia nitrogen absorption on ceramic honey comb surface reaches capacity, organic composite denitrfying agent aging magnesium-aluminum-iron hydrotalcite magnetic Nano material top layer, wash away with under externally-applied magnetic field effect at urine current, aging sorbing material top layer comes off layer by layer, in last wastewater measurement water outlet, ammonia-nitrogen content is below 0.5mg/L, and clearance reaches more than 99.9%.
Claims (3)
1. process a method for urine 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 3.8 ~ 6.0g magnesium nitrate, 4.2 ~ 9.7g aluminum nitrate respectively, 6.1 ~ 18.9g iron nitrate is dissolved in 300 ~ 500ml and contains in the ethanol solution of 4.3 ~ 7.6g urea, after stirred at ambient temperature 1h, pour in hydrothermal reaction kettle and be heated to 140 DEG C, reaction 13 ~ 14h; Be cooled to room temperature; With after ethanol and washed with de-ionized water two 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 ~ 50g organic composite denitrfying agent, stirs 40 ~ 60min;
(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 9 ~ 00 DEG C, calcine 5 ~ 7h.
2. a kind of method processing urine middle and high concentration ammonia nitrogen according to claim 1, it is characterized in that: described organic composite denitrfying agent is by ethyl lactate, ethylene-acetic acid ethyl ester, aminobutyric acid three kinds, by quality ratio, the ethyl lactate of 50% ~ 60%, the ethylene-acetic acid ethyl ester of 20% ~ 40%, 10% ~ 40% aminobutyric acid.
3. process a method for urine 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 6:1 be made into viscous fluid, by viscous fluid Tu in ceramic honey comb top layer, coat-thickness is 3 ~ 6 ㎝, by the ceramic honey comb of coated viscous fluid dry 10 ~ 20min under ventilation state, described tackiness agent counts 15 parts of polyimide N,N-DIMETHYLACETAMIDEs, 35 parts of dichloromethyl dimethylbenzene, 25 parts of vinylbenzene and 25 parts of diamyl ethene with parts by weight;
(2) ceramic honey comb of coated viscous fluid is placed in adsorption tower, every layer of ceramic honey comb mounting height is 10 ~ 50 ㎝, and space height is 50 ~ 100 ㎝, allow ammonia nitrogen concentration be the urine flow of 5000 ~ 10000mg/L through adsorption tower, flow rate control 5 ~ 15m
3/ h, absorption dwell time in the tower 40 ~ 60min, until the organic composite denitrfying agent modification magnesium-aluminum-iron hydrotalcite magnetic nano adsorption material ammonia nitrogen absorption on ceramic honey comb surface reaches capacity, organic composite denitrfying agent aging magnesium-aluminum-iron hydrotalcite magnetic Nano material top layer;
(3) wash away with under externally-applied magnetic field effect at urine current, aging sorbing material top layer comes off layer by layer;
(4) ammonia-nitrogen content in last wastewater measurement water outlet.
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Application publication date: 20150902 |