CN109607849A - A kind of processing method of the low ammonia nitrogen uranium-containing waste water of nitrate anion system - Google Patents

A kind of processing method of the low ammonia nitrogen uranium-containing waste water of nitrate anion system Download PDF

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CN109607849A
CN109607849A CN201811425985.7A CN201811425985A CN109607849A CN 109607849 A CN109607849 A CN 109607849A CN 201811425985 A CN201811425985 A CN 201811425985A CN 109607849 A CN109607849 A CN 109607849A
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uranium
waste water
resin
ammonia nitrogen
concentration
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CN109607849B (en
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康绍辉
宋艳
樊兴
舒祖骏
赵凤岐
李大炳
陈树森
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Beijing Research Institute of Chemical Engineering and Metallurgy of CNNC
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Beijing Research Institute of Chemical Engineering and Metallurgy of CNNC
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    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F9/00—Multistage treatment of water, waste water or sewage
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/001—Processes for the treatment of water whereby the filtration technique is of importance
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/28—Treatment of water, waste water, or sewage by sorption
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/66—Treatment of water, waste water, or sewage by neutralisation; pH adjustment
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00—Nature of the contaminant
    • C02F2101/006—Radioactive compounds
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2303/00—Specific treatment goals
    • C02F2303/16—Regeneration of sorbents, filters

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  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Engineering & Computer Science (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Removal Of Specific Substances (AREA)
  • Treatment Of Water By Ion Exchange (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)
  • Water Treatment By Sorption (AREA)

Abstract

The present invention relates to a kind of processing methods of the low ammonia nitrogen uranium-containing waste water of nitrate anion system, comprising the following steps: (1) Wastewater Pretreatment；(2) it obtains resistance to nitrate anion chelating and inhales uranium resin, be packed into adsorption tower after sufficiently being soaked with water, resin bed height >=1m；(3) waste water retained in tower is ejected by load uranium saturated resin obtained by step (2) with the clear water of 1-3BV, then passes to prepared eluent, elutes time of contact >=10min, obtain leacheate；(4) resin after step (3) elution is washed, into wash water, lower than until 1.5g/L, the resin after washing again returns to carry out adsorption uranium for carbonate and bicarbonate total concentration.The present invention had not only realized effective recycling of trace uranium under nitrate anion system, but also realized effectively removing for waste water low-concentration ammonia-nitrogen, had been finally reached the purpose of discharged wastewater met the national standard.

Description

A kind of processing method of the low ammonia nitrogen uranium-containing waste water of nitrate anion system
Technical field
The invention belongs to uranium resources to extract technical field of three-waste treatment, and in particular to a kind of low ammonia nitrogen uranium-bearing of nitrate anion system The processing method of waste water.
Background technique
In the production technology of natural uranium, produce core pure compound from ore, by the broken mill of ore, leach, extract and All multi-process such as purifying, during which can generate a large amount of radioactive wastewater.Due to being needed in the process using a certain amount of ammonium hydroxide and largely Nitric acid also contain a small amount of ammonium ion and a certain amount of nitric acid so in waste water outside deliming, magnesium and radioactive uranium element Radical ion, ammonium ion concentration is lower sometimes, is usually no more than 100mg/L, does not have recovery value, and nitrate ion is then reachable 1g/L or more can have an adverse effect to the Adsorption of uranium, and disposed of in its entirety difficulty is larger, thus such waste water never into Row processing.
Removal for Uranium in Waste Water has chemical precipitation method, zeroth order iron-deoxidize, membrane processing method, biological treatment at present Deng, uranium concentration could be down to outlet standard by generally requiring multistage using membrane separating, and application cost is higher, and gained separate Concentrated water afterwards also needs to be further processed；The main function of biomaterial is absorption, although can play a role, at present It is also only at the experimental study stage, is difficult to fairly large application in a short time；Zero-valent Iron is suitable for the removal of trace uranium, but to containing Uranium waste water quality is more demanding, and action time is relatively slow, and the excessive oxidation of iron is also noted that in use process.In addition, Beijing Inst. of Chemical Metallurgy, Ministry of Nuclear Industry has synthesized a kind of new resin, and (patent name: a kind of resistance to sulfuric acid chlorine-resistant root mentions uranium chelating Resin and its synthetic method, patent No. ZL201218001148.9), have to the absorption of higher concentration uranium under sulfuric acid and chlorine root system There are better effects, but is not directed to the processing of slightly enriched uranium in waste water.All in all, at present industrially using it is more be still that chemistry is heavy Shallow lake method, i.e., be added soluble ferric iron salt into waste water, adds milk of lime, adjusts the pH of waste water, and molysite is made to form flocculate, lime Newborn sediment and molysite flocculate adsorb the radioactive element uranium in carrier band waste water jointly, to reach removal effect, due to needing Using agitating device, stirs slurry and need long-time sedimentation separation, so required device is also more when wastewater treatment capacity is larger, It is added significantly to cost for wastewater treatment.
Processing for Low Concentration Ammonia Containing Wastewater, have at present material absorption method, chlorine oxidation process, the chemical agent precipitation method, Bioanalysis etc..The primary attachment material of material absorption method has ion exchange resin, zeolite, medical stone, vermiculite etc., these materials are past Toward for pure ammonium ion solution have certain adsorption effect, but for the ammonium ion solution containing calcium, magnesium, iron etc. by It is poor in selectivity, it produces little effect；And it loads leacheate caused by the adsorbent material of ammonium ion and still needs to handle, and restrict An important factor for this method uses.Chlorine oxidation process is passed through chlorine into waste water, chlorine, which is first reacted with ammonium ion, generates chlorine Amine, chloramines is being oxidized to nitrogen with chlorine reaction, so that ammonium ion be removed.Due to being related to gas liquid reaction, and by anti- Speed is answered to influence, required special equipment is often larger, and institute is used very few in this way.Chemical precipitation method is that magnesium is added into waste water Ion and phosphate anion react with ammonium ion under weak basic condition and generate magnesium ammonium phosphate sediment, thus by ammonium ion from It is removed in solution.Directly ammonium ion is handled using this method up to standard, generally requires magnesium ion and phosphate anion was kept Amount, and excessive phosphate anion will cause that Phosphorus From Wastewater is exceeded, therefore the presence of these problems is also applied to form Certain restriction.The cost of bioanalysis is generally lower, but it is more sensitive to temperature, and low-temperature treatment effect is often bad.
In general, the processing of the radioactive wastewater at present for not only uranium-bearing and nitrate anion, but also containing low-concentration ammonia-nitrogen lacks Actual case history, corresponding tests and comprehensive investigations are also carried out seldom, to constrain effective place up to standard of such waste water Reason adds somewhat to the environmental risk of uranium resource extraction, and there is an urgent need to the research and development of some new materials, new process, improves The treatment effeciency of such waste water, and then push the green production of China's natural uranium.
Summary of the invention
It is an object of the invention to: the problem of being directed to the low ammonia nitrogen concentration uranium-bearing in China, nitrate anion wastewater treatment, from The introducing of new material, novel agent is set about, and in conjunction with the research of new process, develops a kind of processing work of low-concentration ammonia-nitrogen uranium-containing waste water Skill realizes the recycling of exceeded component in waste water effectively removed with useful constituent, thus while guaranteeing discharged wastewater met the national standard, it is real The recycling of existing waste, provides a new way for the processing of the such radioactive wastewater in China, to promote China's green uranium mine Construction.
Technical scheme is as follows: a kind of processing method of the low ammonia nitrogen uranium-containing waste water of nitrate anion system, including following Step:
(1) Wastewater Pretreatment；
When the sum of carbonate, bicarbonate radical or both concentration is greater than 1g/L in waste water, addition sulphur acid for adjusting pH to 3-4, Then quickly stirring 20min or more, speed of agitator are greater than 200r/min, and stirring terminates, to resin adsorption；
When the sum of carbonate, bicarbonate radical or both concentration is less than or equal to 1g/L in waste water, and pH is greater than 8, sulphur is added Acid adjusts wastewater pH to after 8 or less, to resin adsorption；
When the sum of carbonate, bicarbonate radical or both concentration is less than or equal to 1g/L in waste water, and pH is between 2-8, directly Row resin adsorption is tapped into except uranium；
(2) it obtains resistance to nitrate anion chelating and inhales uranium resin, be packed into adsorption tower after sufficiently being soaked with water, resin bed height >= 1m；The waste water that step (1) pretreatment finishes is passed through adsorption tower, keeps absorption time of contact >=2min of waste water and resin, when When adsorption tail liquid uranium concentration reaches 0.05mg/L, tail washings, which accesses next adsorption tower, to be continued to adsorb, and so on；
When first tower adsorption tail liquid uranium concentration reaches stoste uranium concentration, that is, think the tower adsorption saturation, which stops absorption, from Second tower starts to squeeze into waste water；
(3) load uranium saturated resin obtained by step (2) is ejected the waste water retained in tower with the clear water of 1-3BV, then It is passed through prepared eluent, time of contact >=10min is eluted, obtains leacheate；
(4) resin after step (3) elution is washed, until carbonate and bicarbonate total concentration are lower than in wash water Until 1.5g/L, the resin after washing again returns to carry out adsorption uranium；
(5) ammonia is removed lower than ammonia nitrogen removal auxiliary agent is added in 0.05mg/L adsorption tail liquid to step (2) resulting uranium concentration Nitrogen ion obtains turbid after being stirred to react 10min under room temperature；
(6) step (5) resulting turbid is filtered, removes insoluble suspended matter, control suspension content in filtrate < 50mg/L, by the direct outlet of gained filtrate.
Preferably, in step (2), it is that " a kind of resistance to sulfuric acid chlorine-resistant root mentions patent that the described resistance to nitrate anion chelating, which inhales uranium resin, Mentioned resin in uranium chelating resin and its synthetic method (patent No. ZL201218001148.9) ".
Preferably, in step (3), resulting leacheate is divided into three parts: first part, starts for elution to leacheate uranium Concentration is 500mg/L；Second part is down to the leacheate of 500mg/L for uranium concentration, as qualification again after 500mg/L rising Liquid；Part III is that uranium concentration declines from 500mg/L up to the part of elution end；
Preferably, the qualifying liquid is used to prepare uranium product, first part, second part is successively returned to leaching next time It washes, insufficient section supplements new eluent.
Preferably, in step (3), the eluent group become soluble carbonate salt and bicarbonate, bicarbonate and Carbonate molar concentration rate 1-9, total molar concentration are greater than 0.2mol/L.
Preferably, the soluble carbonate salt is sodium carbonate, potassium carbonate.
Preferably, the soluble bicarbonate is sodium bicarbonate, saleratus.
Preferably, in step (5), the ingredient of the ammonia nitrogen removal auxiliary agent are as follows: hypochlorite+quick lime or hydroxide Calcium, using the slurry that liquid-solid ratio 1:1-10:1 is preceding made, hypochlorite and quick lime or calcium hydroxide rub ammonia nitrogen removal auxiliary agent You are than being 3:1-1:1；The pH6-8 of reaction is controlled, the additional amount of ammonia nitrogen removal auxiliary agent is 1-1.5 times of its theoretical amount.
Remarkable result of the invention is: being adsorbed containing the low ammonia nitrogen uranium-containing waste water of nitrate anion using the chelating resin of resistance to nitrate anion Uranium --- tail washings ammonia nitrogen auxiliary agent removes the technique of ammonia nitrogen, and one circular treatment wastewater flow rate of resin is up to 5000BV, processed waste water uranium Concentration is down to 0.05mg/L or less；After ammonia nitrogen auxiliary agent is added, ammonia nitrogen concentration is down to 10mg/L or less in waste water.In terms of result, both Effective recycling of trace uranium under nitrate anion system is realized, and realizes effectively removing for waste water low-concentration ammonia-nitrogen, is finally reached The purpose of discharged wastewater met the national standard.
Detailed description of the invention
Fig. 1 is a kind of flow diagram of the processing method of the low ammonia nitrogen uranium-containing waste water of nitrate anion system of the present invention.
Specific embodiment
With reference to the accompanying drawing and specific embodiment is to a kind of low ammonia nitrogen uranium-containing waste water of nitrate anion system of the present invention Processing method is described in further detail.
In the targeted waste water of the present invention in addition to radioactive uranium element, also contain a small amount of ammonium ion and a certain amount of nitre Acid ion, wherein ammonium ion concentration is typically not greater than 100mg/L, does not have recovery value, nitrate ion is then up to 1g/ L or more can have an adverse effect to the removal of uranium.Based on the above situation, the present invention resin of resistance to nitrate anion preferably suitable first, Utilize the UO in cationic form in the chelation group and solution of resin2 2+Deng generation chelation, to realize radioactivity member The efficient removal of plain uranium, it is suitable for that eluent elutes uranium that the saturated resin for loading uranium, which recycles, realizes recycling and the tree of uranium Rouge recycles.Except containing the waste water of low-concentration ammonia-nitrogen, being added after uranium and remove ammonia nitrogen auxiliary agent, using the hypochlorite in auxiliary agent first with Ammonium ion reaction generates amino (NH2), amino, which is further reacted with hypochlorite, is oxidized to nitrogen, to complete low The innoxious removal of concentration ammonia nitrogen, while using except the basic component in ammonia nitrogen auxiliary agent, the spent acid generated in ammonium oxidation is neutralized, Keep the suitable PH of handled waste water, the final qualified discharge for realizing waste water.
As shown in Figure 1, a kind of processing method of the low ammonia nitrogen uranium-containing waste water of nitrate anion system, comprising the following steps:
(1) Wastewater Pretreatment；
When the sum of carbonate, bicarbonate radical or both concentration is greater than 1g/L in waste water, addition sulphur acid for adjusting pH to 3-4, Then quickly stirring 20min or more, speed of agitator are greater than 200r/min, and stirring terminates, to resin adsorption；
When the sum of carbonate, bicarbonate radical or both concentration is less than or equal to 1g/L in waste water, and pH is greater than 8, sulphur is added Acid adjusts wastewater pH to after 8 or less, to resin adsorption；
When the sum of carbonate, bicarbonate radical or both concentration is less than or equal to 1g/L in waste water, and pH is between 2-8, directly Row resin adsorption is tapped into except uranium；
(2) it obtains resistance to nitrate anion chelating and inhales uranium resin, be packed into adsorption tower after sufficiently being soaked with water, resin bed height >= 1m；The waste water that step (1) pretreatment finishes is passed through adsorption tower, keeps absorption time of contact >=2min of waste water and resin, when When adsorption tail liquid uranium concentration reaches 0.05mg/L, tail washings, which accesses next adsorption tower, to be continued to adsorb, and so on；
When first tower adsorption tail liquid uranium concentration reaches stoste uranium concentration, that is, think the tower adsorption saturation, which stops absorption, from Second tower starts to squeeze into waste water；
(3) load uranium saturated resin obtained by step (2) is ejected the waste water retained in tower with the clear water of 1-3BV, then It is passed through prepared eluent, time of contact >=10min is eluted, obtains leacheate；
(4) resin after step (3) elution is washed, until carbonate and bicarbonate total concentration are lower than in wash water Until 1.5g/L, the resin after washing again returns to carry out adsorption uranium；
(5) ammonia is removed lower than ammonia nitrogen removal auxiliary agent is added in 0.05mg/L adsorption tail liquid to step (2) resulting uranium concentration Nitrogen ion obtains turbid after being stirred to react 10min under room temperature；
(6) step (5) resulting turbid is filtered, removes insoluble suspended matter, control suspension content in filtrate < 50mg/L, by the direct outlet of gained filtrate.
Preferably, in step (2), it is that " a kind of resistance to sulfuric acid chlorine-resistant root mentions patent that the described resistance to nitrate anion chelating, which inhales uranium resin, Mentioned resin in uranium chelating resin and its synthetic method (patent No. ZL201218001148.9) ".
Preferably, in step (3), resulting leacheate is divided into three parts: first part, starts for elution to leacheate uranium Concentration is 500mg/L；Second part is down to the leacheate of 500mg/L for uranium concentration, as qualification again after 500mg/L rising Liquid；Part III is that uranium concentration declines from 500mg/L up to the part of elution end；
Preferably, the qualifying liquid is used to prepare uranium product, first part, second part is successively returned to leaching next time It washes, insufficient section supplements new eluent.
Preferably, in step (3), the eluent group become soluble carbonate salt and bicarbonate, bicarbonate and Carbonate molar concentration rate 1-9, total molar concentration are greater than 0.2mol/L.
Preferably, the soluble carbonate salt is sodium carbonate, potassium carbonate.
Preferably, the soluble bicarbonate is sodium bicarbonate, saleratus.
Preferably, in step (5), the ingredient of the ammonia nitrogen removal auxiliary agent are as follows: hypochlorite+quick lime or hydroxide Calcium, using the slurry that liquid-solid ratio 1:1-10:1 is preceding made, hypochlorite and quick lime or calcium hydroxide rub ammonia nitrogen removal auxiliary agent You are than being 3:1-1:1；The pH6-8 of reaction is controlled, the additional amount of ammonia nitrogen removal auxiliary agent is 1-1.5 times of its theoretical amount.
1. embodiment
The concrete composition of waste water is shown in Table 1, process conditions and the results are shown in Table 2.
1 waste water main component of table
The low ammonia nitrogen uranium-containing waste water of table 2 handles experimental condition and result
Above-described embodiment is only of the invention more excellent as a result, still the present invention is not limited to above-described embodiments, in this field Those of ordinary skill within the scope of knowledge, can also make corresponding combination without departing from the purpose of the present invention Variation.

Claims (8)

1. a kind of processing method of the low ammonia nitrogen uranium-containing waste water of nitrate anion system, which comprises the following steps:
(1) Wastewater Pretreatment；
When the sum of carbonate, bicarbonate radical or both concentration is greater than 1g/L in waste water, addition sulphur acid for adjusting pH to 3-4, then Quickly stirring 20min or more, speed of agitator are greater than 200r/min, and stirring terminates, to resin adsorption；
When the sum of carbonate, bicarbonate radical or both concentration is less than or equal to 1g/L in waste water, and pH is greater than 8, sulfuric acid tune is added Wastewater pH is saved to after 8 or less, to resin adsorption；
When the sum of carbonate, bicarbonate radical or both concentration is less than or equal to 1g/L in waste water, and when pH is between 2-8, directly into Row resin adsorption removes uranium；
(2) it obtains resistance to nitrate anion chelating and inhales uranium resin, be packed into adsorption tower after sufficiently being soaked with water, resin bed height >=1m； The waste water that step (1) pretreatment finishes is passed through adsorption tower, absorption time of contact >=2min of waste water and resin is kept, works as absorption When tail washings uranium concentration reaches 0.05mg/L, tail washings, which accesses next adsorption tower, to be continued to adsorb, and so on；
When first tower adsorption tail liquid uranium concentration reaches stoste uranium concentration, that is, think the tower adsorption saturation, which stops absorption, from second Root tower starts to squeeze into waste water；
(3) waste water retained in tower is ejected by load uranium saturated resin obtained by step (2) with the clear water of 1-3BV, is then passed to Prepared eluent elutes time of contact >=10min, obtains leacheate；
(4) resin after step (3) elution is washed, until carbonate and bicarbonate total concentration are lower than 1.5g/L in wash water Until, the resin after washing again returns to carry out adsorption uranium；
(5) to step (2) resulting uranium concentration lower than being added ammonia nitrogen removal auxiliary agent in 0.05mg/L adsorption tail liquid, removal ammonia nitrogen from Son obtains turbid after being stirred to react 10min under room temperature；
(6) step (5) resulting turbid is filtered, removes insoluble suspended matter, control suspension content in filtrate < 50mg/L, by the direct outlet of gained filtrate.
2. the processing method of the low ammonia nitrogen uranium-containing waste water of a kind of nitrate anion system as described in claim 1, it is characterised in that: step (2) in, it is that " a kind of resistance to sulfuric acid chlorine-resistant root mentions uranium chelating resin and its synthesis side to patent that the described resistance to nitrate anion chelating, which inhales uranium resin, Mentioned resin in method (patent No. ZL201218001148.9) ".
3. the processing method of the low ammonia nitrogen uranium-containing waste water of a kind of nitrate anion system as described in claim 1, it is characterised in that: step (3) in, resulting leacheate is divided into three parts: first part, starts to leacheate uranium concentration to be 500mg/L for elution；Second Part is down to the leacheate of 500mg/L for uranium concentration, as qualifying liquid again after 500mg/L rising；Part III is that uranium is dense It spends from the part that 500mg/L decline terminates up to elution.
4. the processing method of the low ammonia nitrogen uranium-containing waste water of a kind of nitrate anion system as claimed in claim 3, it is characterised in that: by institute The qualifying liquid stated is used to prepare uranium product, and first part, second part are successively returned to elution next time, the new leaching of insufficient section supplement Lotion.
5. the processing method of the low ammonia nitrogen uranium-containing waste water of a kind of nitrate anion system as described in claim 1, it is characterised in that: step (3) in, the eluent group becomes soluble carbonate salt and bicarbonate, bicarbonate and carbonate molar concentration rate 1-9, Total molar concentration is greater than 0.2mol/L.
6. the processing method of the low ammonia nitrogen uranium-containing waste water of a kind of nitrate anion system as claimed in claim 5, it is characterised in that: described Soluble carbonate salt be sodium carbonate, potassium carbonate.
7. the processing method of the low ammonia nitrogen uranium-containing waste water of a kind of nitrate anion system as claimed in claim 5, it is characterised in that: described Soluble bicarbonate be sodium bicarbonate, saleratus.
8. the processing method of the low ammonia nitrogen uranium-containing waste water of a kind of nitrate anion system as described in claim 1, it is characterised in that: step (5) in, the ingredient of the ammonia nitrogen removal auxiliary agent are as follows: hypochlorite+quick lime or calcium hydroxide, before ammonia nitrogen removal auxiliary agent use The molar ratio that the slurry of liquid-solid ratio 1:1-10:1, hypochlorite and quick lime or calcium hydroxide is made is 3:1-1:1；Control reaction PH6-8, the additional amount of ammonia nitrogen removal auxiliary agent is 1-1.5 times of its theoretical amount.
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CN111170474A (en) * 2020-01-21 2020-05-19 西南科技大学 Method for removing uranium in ryegrass-enriched degradation residual liquid by microorganisms under aerobic condition

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Publication number Priority date Publication date Assignee Title
CN111039446A (en) * 2019-12-06 2020-04-21 核工业北京化工冶金研究院 Method for removing uranium, manganese and thallium from seepage water of tailing pond
CN111170474A (en) * 2020-01-21 2020-05-19 西南科技大学 Method for removing uranium in ryegrass-enriched degradation residual liquid by microorganisms under aerobic condition

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