CN105906099B - The immediate processing method of rare earth radioactive wastewater - Google Patents
The immediate processing method of rare earth radioactive wastewater Download PDFInfo
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- CN105906099B CN105906099B CN201610401828.7A CN201610401828A CN105906099B CN 105906099 B CN105906099 B CN 105906099B CN 201610401828 A CN201610401828 A CN 201610401828A CN 105906099 B CN105906099 B CN 105906099B
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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
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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
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
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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
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/66—Treatment of water, waste water, or sewage by neutralisation; pH adjustment
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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
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
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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
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
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- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Separation Of Suspended Particles By Flocculating Agents (AREA)
Abstract
The invention discloses a kind of methods that rare earth radioactive wastewater is quickly handled.Compound de- uranium agent and oxidant are added in the radioactive wastewater of pH3~7, pass through the synergistic effect of compound de- uranium agent and oxidant, efficient oxidation is carried out to organic extractant remaining in rare earth extraction waste water, destroy the complex state of extractant and uranium, uranium is set to generate stable compound in conjunction with compound de- uranium agent and realize removing, compound de- uranium agent can form loose suede grain in waste water, the suede grain has very strong adsorption capacity to other remaining radioactive element thoriums etc. in water, to the radioactive element and heavy metal ion in quickly cleaning water, realize the deep purifying of radioactive element, water outlet can stably reach radioactive element in " rare-earth industry pollutant emission standard " (GB26451-2011), the limit value of the discharge standards such as heavy metal, new approach is opened for the improvement of radioactive wastewater fast deep, tool There is good application prospect.
Description
Technical field:
The present invention relates to a kind of method that rare earth radioactive wastewater is quickly handled, especially a kind of pair of rare-earth trades to generate
The method of thoriated, uranium radioactive wastewater, belongs to technical field of radioactive wastewater treatment.
Background technique:
China's rare-earth industry is founded the factory from early 1960s, achieves significant achievements by development in more than 50 years,
As the world's largest Rare Earth Production state, rare-earth products country of consumption and exported country.With rare earth development and application study, tradition or
New and high technology rare-earth products are applied to the multiple fields of national economy, but " three wastes " and rare earth companion in rare-earth smelting production process
Raw radionuclide thorium, uranium are seriously polluted, if these radioactive liquid wastes timely and effective cannot be handled, are entered by environment compound
In vivo, a variety of pathogenic effects are generated, serious consequence finally is caused to ecology and human health.
Wherein uranium content is higher for the radioactive wastewater that contains generated in rare-earth industry production process at present, and about 5mg/L is high
In more than 1000 times of ordinary river, according to uranium geology radiological protection and environmental protection regulation, limitation of the uranium in open water
Concentration is 0.05mg/L, and thorium, total uranium amount 0.1mg/L are provided in " rare-earth industry pollutant emission standard " (GB26451-2011)
Emission limit, commonly pre-processing technique in rare-earth trade is neutralization of lime milk, main radioactive substance after processing
Emission request cannot be reached, it is necessary to just can outlet after advanced treating.
Uranium-bearing material is shut off as much as possible, Direct precipitation or is concentrated in by processing rare earth Spent Radioactive method for treating water at present
In water, to have the function that purifying water body.Traditional main concentration method of radioactive water processing method, including chemical precipitation, ion
The methods of exchange, evaporation and concentration, absorption.But due to evaporation concentration method higher cost, mud, which is concentrated, needs cured barrier to handle；Ion is handed over
It is high to change method removing coefficient, it is more demanding to raw water quality, be affected by competing ions, the regeneration of ion-exchanger and disposition compared with
The deficiencies of difficult and radiation resistance is poor.Absorption method has simple process, decontamination factor height, but higher cost；Chemical precipitation method etc.
The disadvantages of although cost is relatively low for technology, fluctuation of service, standard water discharge is difficult, it is difficult to promote.In recent years, people are constantly to biography
The shortcomings that technique of uniting, is improved, while continuously searching for new technology such as membrane technology and micro-compound technology.Membrane separation technique has
Many advantages, such as effluent quality is good, cycles of concentration is high, decontamination factor is big, stable and reliable operation.However, there is also easy to be raw for membrane technology
At dirt, service life is short, concentrated water need to be further processed etc., and significant drawbacks, micro- composite governance low-activity waste water are with micro- compound
Thallus adsorbs enriching and recovering and is present in the radionuclides such as the uranium in aqueous solution as composite treating agent, high-efficient, at low cost,
Energy consumption is few, and does not have secondary pollution, and the minimizing target of radioactive waste may be implemented, and can be the regeneration or geology of nucleic
Disposition creates favorable conditions.External Ghasemi etc. has studied the performance of U (VI) in capsule chain algae absorption waste water, and adsorption capacity can
Up to 318.15mg/g.For Silva etc. using the U (VI) in sargassum absorption waste water, removal rate can reach 64%.Domestic scholars
Have studied the research that domestic scholars have studied Biosorption of Uranium By Alginate Immobilized Saccharomyces Cerevisiae, the results showed that, through formaldehyde crosslinking,
After calcium alginate is fixed, brewer's yeast bacteria immobilized particle uranium absorption amount is obviously increased, up to 769.2mg/g.Foreign countries are existing to grind
Study carefully using it is single it is compound remove waterborne radioactivity element, process control is complicated, many places rarely have big in the experimental study stage at present
Technical scale application.
Summary of the invention:
The purpose of the invention is to overcome conventional physical chemical method at high cost, fluctuation of service, standard water discharge is difficult, newly
The technology UF membrane significant drawback short there are dirt easily generated, service life, and existing composite algorithm research is with single compound next
The radioactive element in waste water, and the defect that removal rate is not high are removed, rare earth can quickly be handled by proposing the compound de- uranium agent of one kind
The method of radioactive wastewater, activity concentration range 37~3.7 × 105Bq/L, contained major radiation element are
Other polluters such as uranium, thorium and heavy metal.Through the invention, work is cooperateed with using the compound de- more groups of uranium agent and oxidant
With thorium, uranium concentration in waste water being down to 0.005mg/L by 5mg/L content hereinafter, uranium, thorium total content are lower than in water outlet
0.01mg/L, and realize the deep purifying of heavy metal ions in wastewater, uranium, thorium concentration can stably reach " rare-earth industry pollution
Object discharge standard " emission limit of thorium, total uranium amount 0.1mg/L in (GB26451-2011).
The purpose of the present invention is what is be accomplished by the following way:
The method of rare earth radioactive wastewater quickly handled, comprising the following steps:
(1) rare earth radioactive wastewater is adjusted to acid or neutrality；
(2) compound de- uranium agent reaction is added in step (1) acquired solution；
The compound de- uranium agent is that bodied ferric sulfate, iron chloride, ferrous nitrate, ferrous sulfate heptahydrate, perchloric acid is sub-
Iron, potassium ferrate, polyaluminium sulfate, aluminum sulfate, the one or more and hydrogen peroxide of aluminium chloride and sulfuric acid reaction obtain molten
Liquid；
(3) oxidant is added according to the concentration of COD in waste water and carries out oxidation reaction；
(4) solution is then adjusted to acid or alkalinity, is stirred to react, is staticly settled separation.
The rare earth radioactive wastewater is the thoriated generated in rare-earth industry production process, the radioactive wastewater of uranium.
Using between the pH value of acid or alkali adjusting radioactive wastewater to 3~7 in step (1).
It is added under stirring according to the ratio that the mass ratio of compound de- uranium agent and uranium is 0.5~1.5:1 in step (2)
Compound de- uranium agent is reacted 5-15 minutes.
The specific preparation process of compound de- uranium agent described in step (2) is as follows:
A, by bodied ferric sulfate, iron chloride, ferrous nitrate, ferrous sulfate heptahydrate, ferrous perchlorate, potassium ferrate, polymerization
One or more dissolutions of aluminum sulfate, aluminum sulfate, aluminium chloride, mass fraction control control 20~40 DEG C of temperature 30~40%,
It is stirred to react at least 2 hours；
B, step a obtain in product be added mass percent 27% hydrogen peroxide and 50% strong sulfuric acid response 2~4 it is small
When, hydrogen peroxide mass concentration is 2~5% in reaction system after addition, concentrated sulfuric acid concentration 1~5% in reaction system after addition；On
Layer clear liquid is compound de- uranium agent.
Oxidant and the mass ratio of COD are 2.0~5.0:1 in step (3), oxidation time 15~30 minutes.It is described
Oxidant be the hydrogen peroxide of acidification, potassium permanganate, hypochlorite, chlorate or perchlorate aqueous solution.
Step (4) is added alkali and adjusts pH value to 7~9, is stirred to react 10-15 minutes, staticly settles separation.
The alkali being added in step (4) include alkali metal hydroxide and oxide, alkaline-earth metal metal hydroxides,
Liquid alkali or carbide slurry.
When step (4) staticly settles while flocculant can also be added.
The present invention passes through compound de- uranium using the uranium in compound de- uranium agent technique fast deep removing rare earth radioactive wastewater
The synergistic effect of agent and oxidant generates hydroxyl radical free radical and high price iron al-based compound, has to remaining in rare earth extraction waste water
Machine medicament carries out efficient oxidation destruction, and the complex state substance for forming the uranium in waste water and extraction medicament loses stabilization, compound de-
The flocculant compounded in uranium agent can form loose suede grain in waste water, and the suede grain is to other remaining radioactive elements in water
Thorium etc. has very strong adsorption capacity, so that radioactive element, heavy metal ion in quickly cleaning water, realize radioactive element
Deep purifying, water outlet can stably reach radioactive element in " rare-earth industry pollutant emission standard " (GB26451~2011),
The limit value of heavy metal ion discharge standard opens new approach for radioactive wastewater deep treatment, before having application well
Scape.
Method for treating water containing Spent Radioactive of the present invention has following significant technical effect:
1, in the water according to specified in " rare-earth industry pollutant emission standard " (GB26451~2011) trace uranium analysis
With the analysis method measurement of thorium in water, influent density is thorium, uranium concentration total amount is 5mg/L, is discharged thorium after processing, total uranium amount is lower than
0.1mg/L can stably reach " rare-earth industry pollutant emission standard " (GB26451~2011) limit value；
2, due to using compound de- uranium agent method, the present invention is stablizing the radioactive element thorium in removing RE waste water, uranium
While can remove the heavy metals such as lead, cadmium, nickel, arsenic, chromium in waste water, realize radioactive element and an a variety of huge sum of moneys in waste water
The deep purifying of category, process flow quickly, simply, have a good application prospect.
Detailed description of the invention
Fig. 1 present invention process flow diagram.
Specific embodiment
It is intended to further illustrate the present invention with reference to embodiments, is not intended to limit the present invention.
Embodiment 1
The preparation of compound de- uranium agent:
A, by bodied ferric sulfate (Fe2(OH)n(SO4)3~n/2)m, iron chloride (FeCl3·6H2O), ferrous nitrate (Fe
(NO3)2·6H2O), ferrous sulfate heptahydrate (FeSO4·7H2O), ferrous perchlorate (Fe (ClO4)2), potassium ferrate (K2FeO4)、
Polyaluminium sulfate [Al2(OH)m(SO4)3-]n, aluminum sulfate (Al2(SO4)3), aluminium chloride (AlCl3) one or more dissolutions, matter
Fractional domination is measured 30~40%, 20~40 DEG C of temperature is controlled, is stirred to react 2 hours；
B, by step a obtain product and be added mass percent be 2~5% hydrogen peroxide (mass fraction 27%) and 1~
5% concentrated sulfuric acid (mass fraction 50%) reacts 2~4 hours.Supernatant liquor is compound de- uranium agent.
Embodiment 2
Radioactive wastewater 3.24mg/L containing uranium concentration, the COD 445mg/L of certain rare earth processing enterprise discharge, pH value are
10.4, dilute sulfuric acid is added in waste water and is pre-processed, pH to 3.0 or so is adjusted, according to 1.2kg/m3Compound de- uranium agent is added in amount,
It is stirred to react 10min, according to 1.0kg/m3Oxidant is added, oxidation reaction 20min adds sodium hydroxide solution and is adjusted to pH
=9.0 or so, reaction time 15min stand 10 minutes, and supernatant is taken to carry out to uranium analysis detection, and uranium is dense in test water outlet
Degree is < 0.087mg/L, lower than thorium, total uranium amount 0.1mg/L in " rare-earth industry pollutant emission standard " (GB26451~2011)
Emission limit.
Embodiment 3
Radioactive wastewater 10L is taken, thoriated concentration 0.8mg/L, 2.1mg/L containing uranium concentration, pH 7.3, COD in waste water
322.4mg/L adds compound de- uranium agent 1.0L in waste water and carries out reaction 10min, be then added 10mL oxidant aoxidize it is anti-
20min is answered, Ca (OH) is added2Solution is adjusted to pH=9.0 or so, reaction time 10min, adds 2mL flocculant PAM
(mass fraction 0.1%) stands after stirring 1min, is separated by solid-liquid separation.Supernatant is taken to carry out the analysis detection of thorium, uranium.Through dividing
The concentration of thorium is 0.01mg/L in analysis test water outlet, and the concentration of uranium is 0.005mg/L, and thorium, total uranium amount 0.015mg/L are lower than
The emission limit of thorium, total uranium amount 0.1mg/L in " rare-earth industry pollutant emission standard " (GB26451~2011).
Embodiment 4
Certain Rare Earth Enterprises radioactive wastewater 10L is taken, heavy metal element wherein included and content are shown in Table 1, using sulfuric acid tune
Wastewater pH is saved to 5.0 or so.It adds compound de- uranium agent 10mL and carries out reaction 15min, oxidant 0.8mL is added and carries out catalysis oxidation
20min is reacted, Ca (OH) is added2Solution is adjusted to pH=9.0 or so, reaction time 10min, adds 2mL flocculant PAM
(mass fraction 0.1%) stands after stirring 1min, is separated by solid-liquid separation.Taking supernatant analysis, the results are shown in Table 1.In waste water
Concentration of heavy metal ion and radioactive element be below row in " rare-earth industry pollutant emission standard " (GB26451~2011)
Put limit value.
The compound de- uranium agent of 1 radioactive wastewater of table heavy metal residual concentration (unit: except mg/L, pH) before and after the processing
Claims (9)
1. the method for rare earth radioactive wastewater quickly handled, which comprises the following steps:
(1) rare earth radioactive wastewater is adjusted to acid or neutrality；
(2) compound de- uranium agent reaction is added in step (1) acquired solution；
The compound de- uranium agent is by bodied ferric sulfate, iron chloride, ferrous nitrate, ferrous sulfate heptahydrate, ferrous perchlorate, height
The solution that potassium ferrite, polyaluminium sulfate, aluminum sulfate, the one or more and hydrogen peroxide of aluminium chloride and sulfuric acid reaction obtain；
(3) oxidant is added according to the concentration of COD in waste water and carries out oxidation reaction；
(4) solution is then adjusted to acid or alkalinity, is stirred to react, is staticly settled separation.
2. the method for rare earth radioactive wastewater according to claim 1 quickly handled, which is characterized in that the rare earth
Radioactive wastewater is the thoriated generated in rare-earth industry production process, the radioactive wastewater of uranium.
3. the method for rare earth radioactive wastewater according to claim 1 or 2 quickly handled, which is characterized in that step (1)
It is middle to adjust the pH value of radioactive wastewater between 3 ~ 7 using acid or alkali.
4. the method for rare earth radioactive wastewater according to claim 1 quickly handled, which is characterized in that in step (2)
Compound de- uranium agent is added according to the ratio that the mass ratio of compound de- uranium agent and uranium is 0.5 ~ 1.5:1 under stirring, reacts 5-
15 minutes.
5. the method for rare earth radioactive wastewater according to claim 1 or 4 quickly handled, which is characterized in that step (2)
Described in compound de- uranium agent specific preparation process it is as follows:
A, by bodied ferric sulfate, iron chloride, ferrous nitrate, ferrous sulfate heptahydrate, ferrous perchlorate, potassium ferrate, polyaluminum sulfate
One or more dissolutions of aluminium, aluminum sulfate, aluminium chloride, mass fraction control control 20 ~ 40 DEG C of temperature, stirring is anti-30 ~ 40%
It should be at least 2 hours；
B, step a obtains the hydrogen peroxide that mass percent 27% is added in product and strong sulfuric acid response 2 ~ 4 hours of 50%, after addition
Hydrogen peroxide mass concentration is 2 ~ 5% in reaction system, concentrated sulfuric acid concentration 1 ~ 5% in reaction system after addition；Supernatant liquor is multiple
Close de- uranium agent.
6. the method for rare earth radioactive wastewater according to claim 1 quickly handled, which is characterized in that the oxidation
Agent is the aqueous solution of the hydrogen peroxide being acidified, potassium permanganate, hypochlorite, chlorate or perchlorate.
7. the method for rare earth radioactive wastewater according to claim 1 quickly handled, which is characterized in that step (4) adds
Enter alkali and adjust pH value to 7 ~ 9, is stirred to react 10-15 minutes, staticly settles separation.
8. the method for rare earth radioactive wastewater according to claim 1 or claim 7 quickly handled, which is characterized in that step (4)
The alkali of middle addition includes the hydroxide or the oxide of alkali metal, the metal hydroxides of alkaline-earth metal, liquid alkali of alkali metal
Or carbide slurry.
9. the method for rare earth radioactive wastewater according to claim 1 or claim 7 quickly handled, which is characterized in that step (4)
When staticly settling while flocculant is added.
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| CN108117187A (en) * | 2017-11-29 | 2018-06-05 | 中铝广西国盛稀土开发有限公司 | The process of heavy metal in a kind of intermittent processing RE waste water |
| CN109014175B (en) * | 2018-08-03 | 2021-06-29 | 南华大学 | Uranium-removing aluminum powder and uranium-removing method based on aluminum pop can as raw material |
| CN109626631A (en) * | 2018-12-18 | 2019-04-16 | 中国科学院广州地球化学研究所 | Low content radioactive pollutant treatment process in a kind of rare earth metallurgy |
| CN111018184A (en) * | 2019-12-21 | 2020-04-17 | 钢研集团稀土科技有限公司 | Process method for treating rare earth wastewater |
| CN111018223A (en) * | 2019-12-26 | 2020-04-17 | 湖南中核金原新材料有限责任公司 | Method for realizing zero discharge of wastewater in process of producing rare earth chloride from monazite |
| 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 |
| CN114249451B (en) * | 2020-09-22 | 2024-03-12 | 西南科技大学 | Novel method for treating high-temperature gas cooled reactor element core preparation process wastewater |
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| CN103224256B (en) * | 2013-04-09 | 2015-01-28 | 华南理工大学 | Polymerization ferric sulfate water treatment agent and preparation method thereof |
| CN103693819B (en) * | 2014-01-02 | 2015-03-04 | 中南大学 | Thallium-containing heavy metal wastewater advanced treatment method |
| US8802041B1 (en) * | 2014-01-24 | 2014-08-12 | Toxco, Inc. | Decontamination of radioactive metals |
| CN105118540B (en) * | 2015-08-20 | 2018-01-12 | 中电投远达环保工程有限公司 | Radioactive myocardial damage handling process |
| CN105621809B (en) * | 2016-02-19 | 2018-09-14 | 博天环境集团股份有限公司 | A kind of processing method of shale gas fracturing outlet liquid |
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Inventor after: Zhang Liping Inventor after: Chen Runhua Inventor after: Tan Qin Inventor after: Zhao Shuhong Inventor after: Gao Weirong Inventor after: Fu Yunli Inventor after: Yan Guomeng Inventor before: Zhang Liping Inventor before: Chen Runhua Inventor before: Tan Qin Inventor before: Zhao Shuhong Inventor before: Gao Weirong Inventor before: Fu Yunli Inventor before: Yan Guomeng |