CN104907047A - Method used for treating highly concentrated ammonia-nitrogen in rare earth waste water - Google Patents
Method used for treating highly concentrated ammonia-nitrogen in rare earth waste water Download PDFInfo
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Abstract
The invention relates to a method used for treating highly concentrated ammonia-nitrogen in rare earth waste water, and belongs to the field of highly concentrated ammonia-nitrogen treatment. According to the method, a sticky solution is prepared from a prepared organic composite denitrfying agent modified magnesium aluminum iron hydrotalcite magnetic nano adsorption material and an adhesion agent at a mass ratio of 7:1; the surfaces of adsorption rods are coated with the sticky solution, and the adsorption rods are dried under ventilation states and are delivered into an adsorption tower; a rare earth waste water penetrating fluid is delivered through the adsorption tower so as to adsorb 8000 to 12000mg/L highly concentrated ammonia-nitrogen in the rare earth waste water, wherein aging of adsorption material surface layers can be realized via adsorption saturation; under action of applied magnetic field and current scour, layer-by-layer falling of the adsorption material surface layers is realized, and at last the ammonia-nitrogen content of the rare earth waste water is detected. The method is capable of realizing adsorption material renewal; regeneration is not needed; the ammonia-nitrogen concentration of discharged waste water is controlled to be lower than 0.7mg/L; ammonia-nitrogen removing rate is higher than 99.99%; and no secondary pollution is caused to the environment.
Description
Technical field
The present invention relates to a kind of process RE waste water middle and high concentration ammonia nitrogen method, belong to high ammonia-nitrogen wastewater process field.
Background technology
Rare-earth trade is an emerging industry, along with people's environmental consciousness strengthens, the pollution problem of rare-earth trade draws attention gradually, and ammonia nitrogen pollutant is one of three large waste water produced in rare-earth smelting, ammonia nitrogen has certain harm for human body and water body, in water quality index, ammonia nitrogen causes the important pollutant of the one of body eutrophication and environmental pollution, it can make water lose self-purification function, it enters human body and synthesizes nitroso compound, bring out canceration, the generation of gastrointestinal disorders and endemic illness when ammonia-nitrogen content is too high in drinking water, can be caused.
Discharge in Rare Earth Production process three kinds of waste water, the ammonium salt waste water that the acid waste water of mainly rare earth ore concentrate baking tail gases spray cleaning generation, carbonated rare earth production process produce and the ammonium salt waste water that Rare Earth Separation produces.For ammonia nitrogen, the wastewater flow rate that rare-earth trade produces every year reaches more than 1,500 ten thousand tons, wherein ammonia-nitrogen content 8000 ~ 12000mg/L, exceeds discharging standards tens doubly to hundreds of times.
Ammonia nitrogen waste water enters water body, particularly flow to lake more slowly, bay, easily cause algae and other microorganism amount reproduction in water, form eutrophication pollution, difficulty is run except water treatment plants can be made, cause outside the peculiar smell of drinking water, oxygen in water can be made time serious to decline, fish kill, lake even can be caused to be destroyed, ammonia nitrogen also makes to increase chlorine dosage in water disinfection and industrial circulating water sterilisation process, to some metal, particularly to copper, there is corrosivity, in order to reduce waste and the environmental pollution of water resource, improve Business Economic Benefit and society's effect, advanced treating carried out to ammonia nitrogen waste water imperative.
Modern technologies process RE waste water middle and high concentration ammonia nitrogen method mainly contains blow-off method and vaporizing extract process, ion-exchange.Blow-off method and vaporizing extract process refer to when in waste water, pH value is adjusted to alkalescence, ion state ammonium is converted into molecular state ammonia, again waste gas is contacted with gas, ammonia nitrogen is made to transfer to gas phase from liquid phase, the method is usually used in high-concentration ammonia nitrogenous wastewater process, but it is low to there is treatment effeciency when practical operation, occur incrustation scale impact operation, energy consumption and maintenance workload cause the phenomenons such as secondary pollution more greatly and easily; And be CN101372370 at publication number, by by 50% ~ 80% form organic denitrifier by lipid, 10% ~ 50% amine and 10% ~ 50% alkanes and add in high-concentration ammonia nitrogenous wastewater in a kind of method that name is called described in " organic denitrifier and denitrogenation method processing high-concentration ammonia nitrogenous wastewater ", to regulate after pH value of waste water aeration 2 hours, this invention effectively can improve ammonia nitrogen removal frank, but still cannot solve in stripping process due to secondary pollution problem that ammonia emission causes; The ion-exchange of next refers to select have the zeolite of very strong selectivity as exchanger resin to ion, thus reach the object removing ammonia nitrogen, to high-concentration ammonia nitrogenous wastewater, frequently operating difficulties can be caused because of resin regeneration, sub-exchange process clearance is lower, also can cause secondary pollution for environment.
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 processing procedure for organic composite denitrifier, cause secondary environmental pollution problem, provide a kind of organic composite denitrifier 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 6.2 ~ 11.4g magnesium nitrate, 4.2 ~ 7.5g aluminum nitrate respectively, 5.3 ~ 11.4g ferric nitrate is dissolved in 430 ~ 550ml and contains in the ethanol solution of 5.8 ~ 8.6g urea; Stirred at ambient temperature 1h; Pour in hydrothermal reaction kettle and be heated to 130 DEG C, reaction 12 ~ 14h; The room temperature of cooling; With after ethanol and washed with de-ionized water two times at 100 DEG C dry 8h, obtain nano magnalium molten iron talcum;
(2) magnetize: be concentrated hydrochloric acid and the saturated potassium hydroxide solution immersion 6h of 36.5% successively by mass concentration by the nano magnalium molten iron talcum of above-mentioned preparation, be placed in Muffle furnace, dry at temperature is 110 DEG C, near magnetic field magnetisation;
(3) modification: the nano magnalium molten iron talc materials after pickling, alkali leaching and magnetization is immersed in 15 ~ 35g organic composite denitrifier, 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 ~ 900 DEG C, calcine 4 ~ 6h.
Described organic composite denitrifier is oxaloacetic acid, triethyl phosphate, prenol form, by quality ratio, and 10% ~ 45% oxaloacetic acid, 20% ~ 55% triethyl phosphate, 20% ~ 45% prenol.
Application process of the present invention is:
(1) by the organic composite denitrifier modification magnesium-aluminum-iron hydrotalcite magnetic nano adsorption material prepared and adhesive in mass ratio 7:1 be made into viscous fluid, by viscous fluid Tu in polytetrafluoroethylene (PTFE) tiny balloon top layer, coating layer thickness is 4 ~ 7cm, by the polytetrafluoroethylene (PTFE) tiny balloon of coated viscous fluid dry 15 ~ 25min under ventilation state, described adhesive with parts by weight count 30 parts of m-phenylene diamine (MPD)s, 15 parts of para aminoacet anilides, 15 part 3,3-MDA, 40 part 3,3,4,4-diphenyl ether dianhydride;
(2) the polytetrafluoroethylene (PTFE) tiny balloon of coated viscous fluid is placed in adsorption tower, every layer of setting height(from bottom) is 10 ~ 60cm, space height is 50 ~ 120cm, allow ammonia nitrogen concentration be the RE waste water permeate flow of 8000 ~ 12000mg/L through adsorption tower, flow control 5 ~ 20m
3/ h, absorption dwell time in the tower 45 ~ 60min, until the organic composite denitrifier modification magnesium-aluminum-iron hydrotalcite magnetic nano adsorption material ammonia nitrogen absorption on polytetrafluoroethylene (PTFE) tiny balloon surface reaches capacity, organic composite denitrifier aging magnesium-aluminum-iron hydrotalcite magnetic Nano material top layer;
(3) RE waste water penetrating fluid again current wash away with under externally-applied magnetic field effect, 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 area, belong to mesoporous material material, to ammonia nitrogen in waste water, there is absorption property through organic composite denitrifier is modified, the more important thing is, adding of organic composite denitrifier, 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 pernicious gas, can not secondary environmental pollution be caused;
(2) organic composite denitrifier 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;
(3) after coming off, residue is little without moisture, volume, separable under externally-applied magnetic field, and ammonia nitrogen removal frank is high, cost is low.
Detailed description of the invention
The preparation of organic composite denitrifier modification magnesium-aluminum-iron hydrotalcite magnetic nano adsorption material:
(1) magnesium-aluminum-iron hydrotalcite preparation: take 6.2 ~ 11.4g magnesium nitrate, 4.2 ~ 7.5g aluminum nitrate respectively, 5.3 ~ 11.4g ferric nitrate is dissolved in 430 ~ 550ml and contains in the ethanol solution of 5.8 ~ 8.6g urea; Stirred at ambient temperature 1h; Pour in hydrothermal reaction kettle and be heated to 130 DEG C, reaction 12 ~ 14h; The room temperature of cooling; With after ethanol and washed with de-ionized water two times at 100 DEG C dry 8h, obtain nano magnalium molten iron talcum;
(2) magnetize: be concentrated hydrochloric acid and the saturated potassium hydroxide solution immersion 6h of 36.5% successively by mass concentration by the nano magnalium molten iron talcum of above-mentioned preparation, be placed in Muffle furnace, dry at temperature is 110 DEG C, near magnetic field magnetisation;
(3) modification: the nano magnalium molten iron talc materials after pickling, alkali leaching and magnetization is immersed in 15 ~ 35g organic composite denitrifier, 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 ~ 900 DEG C, calcine 4 ~ 6h.
Described organic composite denitrifier is oxaloacetic acid, triethyl phosphate, prenol form, by quality ratio, and 10% ~ 45% oxaloacetic acid, 20% ~ 55% triethyl phosphate, 20% ~ 45% prenol.
Nano adsorption material removes the embody rule of high-concentration ammonia nitrogenous wastewater:
(1) by the organic composite denitrifier modification magnesium-aluminum-iron hydrotalcite magnetic nano adsorption material prepared and adhesive in mass ratio 7:1 be made into viscous fluid, by viscous fluid Tu in polytetrafluoroethylene (PTFE) tiny balloon top layer, coating layer thickness is 4 ~ 7cm, by the polytetrafluoroethylene (PTFE) tiny balloon of coated viscous fluid dry 15 ~ 25min under ventilation state, described adhesive with parts by weight count 30 parts of m-phenylene diamine (MPD)s, 15 parts of para aminoacet anilides, 15 part 3,3-MDA, 40 part 3,3,4,4-diphenyl ether dianhydride;
(2) the polytetrafluoroethylene (PTFE) tiny balloon of coated viscous fluid is placed in adsorption tower, every layer of setting height(from bottom) is 10 ~ 60cm, space height is 50 ~ 120cm, allow ammonia nitrogen concentration be the RE waste water permeate flow of 8000 ~ 12000mg/L through adsorption tower, flow control 5 ~ 20m
3/ h, absorption dwell time in the tower 45 ~ 60min, until the organic composite denitrifier modification magnesium-aluminum-iron hydrotalcite magnetic nano adsorption material ammonia nitrogen absorption on polytetrafluoroethylene (PTFE) tiny balloon surface reaches capacity, organic composite denitrifier aging magnesium-aluminum-iron hydrotalcite magnetic Nano material top layer;
(3) RE waste water penetrating fluid again current wash away with under externally-applied magnetic field effect, aging sorbing material top layer comes off layer by layer;
(4) ammonia-nitrogen content in last wastewater measurement water outlet.
Example 1
First take respectively 6.2g magnesium nitrate, 4.2g aluminum nitrate, 5.3g ferric nitrate be dissolved in 430ml and contain in the ethanol solution of 5.8g urea; Stirred at ambient temperature 1h; Pour in hydrothermal reaction kettle and be heated to 130 DEG C, reaction 12h, the room temperature of cooling; With after ethanol and washed with de-ionized water two times at 100 DEG C dry 8h, obtain nano magnalium molten iron talcum; Be concentrated hydrochloric acid and the saturated potassium hydroxide solution immersion 6h of 36.5% more successively by mass concentration by the nano magnalium molten iron talcum of above-mentioned preparation, be placed in Muffle furnace, dry at temperature is 110 DEG C, near magnetic field magnetisation; Then the nano magnalium molten iron talc materials after pickling, alkali leaching and magnetization is immersed in 15g organic composite denitrifier, wherein comprise 6.5g oxaloacetic acid, 4.5g triethyl phosphate, 4g prenol, stir 40min; 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, organic composite denitrifier modification magnesium-aluminum-iron hydrotalcite magnetic nano adsorption material can be obtained, by the organic composite denitrifier modification magnesium-aluminum-iron hydrotalcite magnetic nano adsorption material prepared and adhesive in mass ratio 7:1 be made into viscous fluid, by viscous fluid Tu in polytetrafluoroethylene (PTFE) tiny balloon top layer, coating layer thickness is 4cm, by the polytetrafluoroethylene (PTFE) tiny balloon of coated viscous fluid dry 15min under ventilation state; The polytetrafluoroethylene (PTFE) tiny balloon of coated viscous fluid is placed in adsorption tower, and every layer of setting height(from bottom) is 10cm, and space height is 50cm, allow ammonia nitrogen concentration be the RE waste water permeate flow of 8000mg/L through adsorption tower, flow control 5m
3/ h, absorption dwell time in the tower 45min, until the organic composite denitrifier modification magnesium-aluminum-iron hydrotalcite magnetic nano adsorption material ammonia nitrogen absorption on polytetrafluoroethylene (PTFE) tiny balloon surface reaches capacity, organic composite denitrifier aging magnesium-aluminum-iron hydrotalcite magnetic Nano material top layer; RE waste water penetrating fluid again current wash away with under externally-applied magnetic field effect, aging sorbing material top layer comes off layer by layer, and in last wastewater measurement water outlet, ammonia-nitrogen content is 0.6mg/L, and ammonia nitrogen removal frank is more than 99.99%.
Example 2
First take respectively 8.3g magnesium nitrate, 5.9g aluminum nitrate, 7.6g ferric nitrate be dissolved in 500ml and contain in the ethanol solution of 7.1g urea; Stirred at ambient temperature 1h; Pour in hydrothermal reaction kettle and be heated to 130 DEG C, reaction 13h, the room temperature of cooling; With after ethanol and washed with de-ionized water two times at 100 DEG C dry 8h, obtain nano magnalium molten iron talcum; Be concentrated hydrochloric acid and the saturated potassium hydroxide solution immersion 6h of 36.5% more successively by mass concentration by the nano magnalium molten iron talcum of above-mentioned preparation, be placed in Muffle furnace, dry at temperature is 110 DEG C, near magnetic field magnetisation; Then the nano magnalium molten iron talc materials after pickling, alkali leaching and magnetization is immersed in 20g organic composite denitrifier, wherein comprise 7g oxaloacetic acid, 8g triethyl phosphate, 5g prenol, stir 55min; 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, organic composite denitrifier modification magnesium-aluminum-iron hydrotalcite magnetic nano adsorption material can be obtained, by the organic composite denitrifier modification magnesium-aluminum-iron hydrotalcite magnetic nano adsorption material prepared and adhesive in mass ratio 7:1 be made into viscous fluid, by viscous fluid Tu in polytetrafluoroethylene (PTFE) tiny balloon top layer, coating layer thickness is 6cm, by the polytetrafluoroethylene (PTFE) tiny balloon of coated viscous fluid dry 20min under ventilation state; The polytetrafluoroethylene (PTFE) tiny balloon of coated viscous fluid is placed in adsorption tower, and every layer of setting height(from bottom) is 20cm, and space height is 70cm, allow ammonia nitrogen concentration be the RE waste water permeate flow of 10000mg/L through adsorption tower, flow control 15m
3/ h, absorption dwell time in the tower 55min, until the organic composite denitrifier modification magnesium-aluminum-iron hydrotalcite magnetic nano adsorption material ammonia nitrogen absorption on polytetrafluoroethylene (PTFE) tiny balloon surface reaches capacity, organic composite denitrifier aging magnesium-aluminum-iron hydrotalcite magnetic Nano material top layer; RE waste water penetrating fluid again current wash away with under externally-applied magnetic field effect, aging sorbing material top layer comes off layer by layer, and in last wastewater measurement water outlet, ammonia-nitrogen content is 0.4mg/L, and ammonia nitrogen removal frank is more than 99.99%.
Example 3
First take respectively 11.4g magnesium nitrate, 7.5g aluminum nitrate, 11.4g ferric nitrate be dissolved in 550ml and contain in the ethanol solution of 8.6g urea; Stirred at ambient temperature 1h; Pour in hydrothermal reaction kettle and be heated to 130 DEG C, reaction 14h, the room temperature of cooling; With after ethanol and washed with de-ionized water two times at 100 DEG C dry 8h, obtain nano magnalium molten iron talcum; Be concentrated hydrochloric acid and the saturated potassium hydroxide solution immersion 6h of 36.5% more successively by mass concentration by the nano magnalium molten iron talcum of above-mentioned preparation, be placed in Muffle furnace, dry at temperature is 110 DEG C, near magnetic field magnetisation; Then the nano magnalium molten iron talc materials after pickling, alkali leaching and magnetization is immersed in 35g organic composite denitrifier, wherein comprise 8g oxaloacetic acid, 14g triethyl phosphate, 13g prenol, stir 60min; 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, organic composite denitrifier modification magnesium-aluminum-iron hydrotalcite magnetic nano adsorption material can be obtained, by the organic composite denitrifier modification magnesium-aluminum-iron hydrotalcite magnetic nano adsorption material prepared and adhesive in mass ratio 7:1 be made into viscous fluid, by viscous fluid Tu in polytetrafluoroethylene (PTFE) tiny balloon top layer, coating layer thickness is 7cm, by the polytetrafluoroethylene (PTFE) tiny balloon of coated viscous fluid dry 25min under ventilation state; The polytetrafluoroethylene (PTFE) tiny balloon of coated viscous fluid is placed in adsorption tower, and every layer of setting height(from bottom) is 20cm, and space height is 120cm, allow ammonia nitrogen concentration be the RE waste water permeate flow of 12000mg/L through adsorption tower, flow control 20m
3/ h, absorption dwell time in the tower 60min, until the organic composite denitrifier modification magnesium-aluminum-iron hydrotalcite magnetic nano adsorption material ammonia nitrogen absorption on polytetrafluoroethylene (PTFE) tiny balloon surface reaches capacity, organic composite denitrifier aging magnesium-aluminum-iron hydrotalcite magnetic Nano material top layer; RE waste water penetrating fluid again current wash away with under externally-applied magnetic field effect, aging sorbing material top layer comes off layer by layer, and in last wastewater measurement water outlet, ammonia nitrogen is content 0.3mg/L, and ammonia nitrogen removal frank is more than 99.99%.
Claims (3)
1. process a RE waste water middle and high concentration ammonia nitrogen method, it is characterized in that organic composite denitrifier modification magnesium-aluminum-iron hydrotalcite magnetic nano adsorption material preparation process is:
(1) magnesium-aluminum-iron hydrotalcite preparation: take 6.2 ~ 11.4g magnesium nitrate, 4.2 ~ 7.5g aluminum nitrate respectively, 5.3 ~ 11.4g ferric nitrate is dissolved in 430 ~ 550ml and contains in the ethanol solution of 5.8 ~ 8.6g urea; Stirred at ambient temperature 1h; Pour in hydrothermal reaction kettle and be heated to 130 DEG C, reaction 12 ~ 14h; The room temperature of cooling; With after ethanol and washed with de-ionized water two times at 100 DEG C dry 8h, obtain nano magnalium molten iron talcum;
(2) magnetize: be concentrated hydrochloric acid and the saturated potassium hydroxide solution immersion 6h of 36.5% successively by mass concentration by the nano magnalium molten iron talcum of above-mentioned preparation, be placed in Muffle furnace, dry at temperature is 110 DEG C, near magnetic field magnetisation;
(3) modification: the nano magnalium molten iron talc materials after pickling, alkali leaching and magnetization is immersed in 15 ~ 35g organic composite denitrifier, 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 ~ 900 DEG C, calcine 4 ~ 6h.
2. one processes RE waste water middle and high concentration ammonia nitrogen method according to claim 1, it is characterized in that described organic composite denitrifier is oxaloacetic acid, triethyl phosphate, prenol form, by quality ratio, 10% ~ 45% oxaloacetic acid, 20% ~ 55% triethyl phosphate, 20% ~ 45% prenol.
3. process a RE waste water middle and high concentration ammonia nitrogen method, it is characterized in that embody rule method is:
(1) by the organic composite denitrifier modification magnesium-aluminum-iron hydrotalcite magnetic nano adsorption material prepared and adhesive in mass ratio 7:1 be made into viscous fluid, by viscous fluid Tu in polytetrafluoroethylene (PTFE) tiny balloon top layer, coating layer thickness is 4 ~ 7cm, by the polytetrafluoroethylene (PTFE) tiny balloon of coated viscous fluid dry 15 ~ 25min under ventilation state, described adhesive with parts by weight count 30 parts of m-phenylene diamine (MPD)s, 15 parts of para aminoacet anilides, 15 part 3,3-MDA, 40 part 3,3,4,4-diphenyl ether dianhydride;
(2) the polytetrafluoroethylene (PTFE) tiny balloon of coated viscous fluid is placed in adsorption tower, every layer of setting height(from bottom) is 10 ~ 60cm, space height is 50 ~ 120cm, allow ammonia nitrogen concentration be the RE waste water permeate flow of 8000 ~ 12000mg/L through adsorption tower, flow control 5 ~ 20m
3/ h, absorption dwell time in the tower 45 ~ 60min, until the organic composite denitrifier modification magnesium-aluminum-iron hydrotalcite magnetic nano adsorption material ammonia nitrogen absorption on polytetrafluoroethylene (PTFE) tiny balloon surface reaches capacity, organic composite denitrifier aging magnesium-aluminum-iron hydrotalcite magnetic Nano material top layer;
(3) RE waste water penetrating fluid again current wash away with under externally-applied magnetic field effect, 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: 20150916 |