CN103446997A - Method for adsorption treatment of uranium-containing wastewater through using magnesium modified attapulgite adsorbent - Google Patents
Method for adsorption treatment of uranium-containing wastewater through using magnesium modified attapulgite adsorbent Download PDFInfo
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- CN103446997A CN103446997A CN2012101794911A CN201210179491A CN103446997A CN 103446997 A CN103446997 A CN 103446997A CN 2012101794911 A CN2012101794911 A CN 2012101794911A CN 201210179491 A CN201210179491 A CN 201210179491A CN 103446997 A CN103446997 A CN 103446997A
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Abstract
The invention relates to a method for the adsorption treatment of uranium-containing wastewater through using a magnesium modified attapulgite adsorbent. The method is characterized in that the concentration of uranium in the wastewater is 5-150mg/L; the magnesium modified attapulgite adsorbent is added to the uranium-containing wastewater according to a mass ratio of uranium in the uranium-containing wastewater to the adsorbent of 1:(500-5000); and an adsorption process is carried out in a static and/or oscillation and stirring mode at 0-50DEG C. The magnesium modified attapulgite adsorbent comprises 7.74-58.7wt% of a magnesium element, and a magnesium modifier added in the magnesium modified attapulgite adsorbent is a magnesium compound easily soluble in water. The method has the advantages of high uranium adsorption efficiency, simple operation process, low adsorption condition requirement, low cost and high regeneration efficiency of the adsorption material, easy popularization, and good economic and environmentally-friendly benefits.
Description
Technical field
The present invention relates to the uranium-containing waste water process field, say further, relate to a kind of method of magnesium-modified attapulgite sorbent treatment uranium-containing waste water.
Background technology
Uranium is the 7th cycle MB family element in the periodic table of elements, and one of actinides, be important natural radioactive element.Uranium-containing waste water is the radioactive wastewater of class wide material sources, the waste water that the post processing of the waste water produced as the exploitation of uranium ore and hydrometallurgy, uranium refining and waste water that the nuclear fuel manufacture produces, waste water that reactor operation produces, reactor fuel produces, produces the waste water that radio isotope produces and uses radioisotopic factory and waste water that research department produces etc.Current, have in the world 22 countries and be engaged in the production of uranium ore industry, amount to more than 200 hundred million tons of uranium mine tailings.It is former thereby leak that a large amount of uranium mine tailings may break due to carrier pipe, heavy rain floods dam, mine tailing ore deposit etc., thereby make uranium enter earth's surface or body of groundwater, pollutes.Uranium and its compounds is one of important source material indispensable in nuclear industry, and the development of nuclear power is rapid especially in recent years.Expecting the nuclear power installed capacity of the year two thousand twenty China and will reach 4,000 ten thousand KW, be the twice of current nuclear power generated energy, and the light water reactor of every 1,000,000 KW standards will produce 550m
3put solid waste in/a low, these solid waste enter the ecosystem under nature aqueous vapor power or artificial action, and atmosphere pollution, soil, water body, by food chain effect and then harmful to human.
Uranium-containing waste water is very harmful to ecological environment and health.By approach such as drinking-water (account for total intake 64%) and food chains, a uranium part in water body finally can enter human body, research shows: the uranium entered after human body is mainly accumulated in liver, kidney and bone, with chemical toxicity and two kinds of forms of internal irradiation, human body is caused to damage, size according to dosage, can cause acute or slow poisoning, bring out various diseases.The uranium that enters into human body can discharge alpha ray, and human body is produced to the radioactivity internal irradiation.Low dose of chronic internal irradiation may cause the diseases such as alopecia, erythema, white blood cell minimizing, cataract; Heavy dose of acute internal irradiation meeting causes acute radiation sickness, and as large-area hemorrhage, bacterium infection, anaemia, endocrinopathy etc., anaphase effect may cause cancer, DNA variation etc., and extreme dosage causes death in a short period of time.
For reducing the ecological risk of uranium in water environment, need to remove the uranium of sewage or surface water body middle and high concentration.Conventional method for treating water has the combination treatment method of physics, chemistry, bioanalysis and said method at present.With traditional complicated technology, compare, absorption method has the advantages such as technique is simple, treatment effect stable, price is relatively low.Patent publication No. is 200410020879 to have introduced a kind of method that the WK of utilization sorbing material is processed heavy metal and radioactive metal ion, patent publication No. is 200810000889 to have introduced a kind of method of utilizing oxidation type hydrophobic glucomannan adsorption material to process heavy metal and radionuclide, two kinds of methods all have higher clearance to heavy metal and radioactive metal ion, fully demonstrated the high absorption property of sorbing material, but both raw material types used are many, and preparation technology is numerous and diverse.And the WK sorbing material need to load in adsorption column and be adsorbed, higher to the conditional request of absorption, be difficult to promote the use of.Therefore, be badly in need of the removal of a kind of novel, economic sorbing material for water body uranium.Soil class sorbing material, because of cheap, of a great variety, becomes the focus of current research.The natural soil class sorbing material that the absorption research of relevant uranium adopts both at home and abroad, comprise illite clay, halloysite clay, diatomite etc., the modification of employing composite adsorbing material is also arranged as bentonite, zeolite etc., but natural soil class sorbing material exists adsorption capacity low, adsorption concentration is limited in scope, and is not suitable for removing the uranium of water body middle and high concentration.
Attapulgite is a kind of natural clay mineral, and due to bar-shaped, the fibrous crystal form with unique layer chain crystal structure and very tiny (approximately 0.01 μ m * 1 μ m) and larger specific area, (internal surface area can be up to 300-400m
2/ g, and external surface area depends on the size of attapulgite crystal grain, according to actual measurement, Soviet Union's Anhui attapulgite external surface area is about 23m
2/ g), determined that it has good absorption property.According to existing bibliographical information attapulgite, be heavy metal and organic strong sorbing material, and regenerative operation is simple, regeneration rate is high, belongs to the non-metal kind clay mineral of a kind of efficient, economy, environmental protection, has broad prospect of application.Current document has been reported the removal of attapulgite to waste water COD, and clearance can be up to more than 90%, and what have even reaches 100%, and regeneration rate is high, reusable, but the Adsorption that attapulgite is applied to uranium is not appeared in the newspapers.
Summary of the invention
For solving problems of the prior art, the invention provides a kind of method of magnesium-modified attapulgite sorbent treatment uranium-containing waste water.Adsorption efficiency to uranium is high, simple to operate, is easy to promote.
A kind of method that the purpose of this invention is to provide magnesium-modified attapulgite sorbent treatment uranium-containing waste water.
The concentration of described uranium in waste water is 5-150mg/L;
Add magnesium-modified attapulgite adsorbent at described uranium-containing waste water, the uranium in described uranium-containing waste water and the mass ratio of described adsorbent are 1: (500-5000), and preferably 1: 500;
Under the condition that described adsorption process is 0-50 ℃ in temperature, adopt static state and/or vibration, stirring action mode to carry out.
In concrete enforcement,
The pH value scope of described uranium-containing waste water is 7-13.
Described adsorption time is 1-12h.
The method of described magnesium-modified attapulgite sorbent treatment uranium-containing waste water also comprises the regeneration of adsorbent;
The regeneration of described adsorbent be by the saturated adsorbent of absorption with NaOH, mix, immersion, clear water wash and get final product, wherein
Described NaOH concentration can be 5%-15%,
Described soak time is 2-3h.
Magnesium-modified attapulgite adsorbent of the present invention is a kind of novel absorption material generated for the modification of attapulgite raw ore, and this material is higher to the adsorption efficiency of uranium, after regeneration, can reuse, and economy is strong, simple to operate.
In described magnesium-modified attapulgite adsorbent, magnesium element content is 7.74%-58.7% by weight percentage;
Magnesium-modified dose that in described magnesium-modified attapulgite adsorbent, adds is magnesium compound soluble in water.
Described magnesium compound soluble in water is preferably one or more that are selected from magnesium sulfate, magnesium nitrate, magnesium chloride, more preferably MgCl
26H
2o
The preparation process of described magnesium-modified attapulgite adsorbent is:
Attapulgite after purification is scattered in water and adds magnesium compound soluble in water, is hydrolyzed and regulates the pH value by magnesium salts and make described magnesium-modified attapulgite adsorbent.
Can adopt following steps:
Attapulgite after purification is scattered in water, adds magnesium compound soluble in water;
It is neutral regulating the pH value;
Stir, centrifugal, make described magnesium-modified attapulgite adsorbent after drying, grinding.
(1) attapulgite is purified
Can adopt the method that in prior art, common attapulgite is purified, the purpose that reaches purification gets final product.In the present invention, can preferably purify according to the following steps:
A. former attapulgite pulverizing, grinding being obtained to particle diameter is 100 purpose powder;
B. add water in concave and convex rod stone powder, be made into the suspension that concentration is 5-10wt%, stir, concave and convex rod stone powder is uniformly dispersed;
C. add the calgon that mass ratio is 1-5% attapulgite quality in the suspension after dispersion treatment, stir 0.5h, ultrasonic 1h, standing 2h, dewater to the mud cake shape, 105 ℃ of dry 3h, the attapulgite after being purified;
(2) Concavo-convex and excellent after purifying stone modification
A. be added to the water stirring in the attapulgite after purifying, the concave and convex rod stone powder after making to purify is uniformly dispersed,
B. add magnesium compound soluble in water,
C. and by watery hydrochloric acid and dilute sodium hydroxide the pH value is adjusted to neutrality,
D. magnetic agitation 2-3h, centrifuge washing 2-3 time, dry 36-48h for 40 ℃, and grinding and obtaining particle diameter is the magnesium-modified attapulgite adsorbent of 100 purpose.
Described absorption is subject to the restriction of Competition and the chemical property of uranium own, and uranium ion is all easily reactions under acid, alkali condition, and known pH value has material impact to absorption, experimental results show that the preferred pH value of uranium solution scope is 7-13.It is little that absorption is affected by temperature, hunting speed, can be selected according to actual conditions, and adsorbing the preferred time is 1-12h, and adsorption effect increases along with the growth of time, after absorption 12h, reaches adsorption equilibrium fully, and after balance, eliminating rate of absorption reaches more than 99%.
Described magnesium-modified attapulgite regeneration, NaOH concentration is 5%-15%, and preferably NaOH concentration is 10%, soaks 2-3h, after the clear water washing, can continue on for the uranium in adsorbed water, and after regeneration, eliminating rate of absorption reaches 92.4%.
The present invention is directed to the waste water that polluted by uranium, by add magnesium-modified attapulgite adsorbent in waste water, carry out Adsorption, beneficial effect of the present invention:
1. high to the adsorption efficiency of uranium,
2. operating process is simple,
3. the adsorption conditions requirement is low,
4. sorbing material is with low cost, regeneration efficiency is high, be easy to popularization.
Therefore, the uranium that the present invention is applied to remove in water body has good economy and environmental benefit.
The accompanying drawing explanation
The impact of Fig. 1 time on eliminating rate of absorption
The impact of the initial concentration of Fig. 2 uranium on eliminating rate of absorption
The impact of Fig. 3 temperature on eliminating rate of absorption
The impact of Fig. 4 oscillation rate on eliminating rate of absorption
The impact of Fig. 5 pH on eliminating rate of absorption
The impact of the different magnesium amount of Fig. 6 modified attapulgite adsorbent on eliminating rate of absorption
The specific embodiment
Below in conjunction with embodiment, further illustrate the present invention.
Embodiment 1
The attapulgite taken after 5g purifies is placed in the 500mL beaker, adds 250mL distilled water, after magnetic agitation 0.5h, adds the MgCl of 1.269g
26H
2o (being equivalent to 0.15gMg), magnetic agitation 30min, guarantee MgCl
26H
2o dissolves fully, regulates pH value=7, continues stirring 1h, after centrifuge washing 3 times, in 40 ℃ of dry 48h, is ground to 100 orders and makes magnesium-modified attapulgite adsorbent.Magnesium element content in this adsorbent is 17.6% by weight percentage.
Accurate weighing is through magnesium-modified attapulgite adsorbent 1.5000g (± 0.0005g), be placed in 250mL tool plug conical flask, add in the uranyl nitrate solution that 30mL concentration is 100mg/L, be placed in constant temperature oscillator, the rate oscillation of 150r/min at 25 ℃ of temperature, now the mass ratio of the uranium in uranium-containing waste water and adsorbent is 1: 500.At 0.5h, 1h, 3h, 6h, 6h, 24h, 48h, do not get supernatant, the concentration of with inductively coupled plasma emission spectrometer (ICP-AES), testing residual uranium.Three groups of each experiment settings are parallel, and result is with the arithmetic average value representation, and the calculating standard deviation, guarantees measuring accuracy.As calculated, the eliminating rate of absorption of uranium is respectively 99.3%, 99.4%, 99.6%, 99.6%, 99.7%, 99.7%, 99.7%.
Accompanying drawing 1 is the impact of time on eliminating rate of absorption.
Visible, be adsorbed on the 0.5h clearance and reach 99.3%, growth in time, clearance slightly increases, and after adsorption equilibrium, clearance reaches 99.7%.Adsorbing the preferred time is 1-12h.
Make magnesium-modified attapulgite adsorbent with embodiment 1.
Accurate weighing is through magnesium-modified attapulgite adsorbent 0.5000g (± 0.0005g), be placed in 250mL tool plug conical flask, add that 10mL concentration is respectively 10,20,50, in the uranyl nitrate solution of 100mg/L, be placed in constant temperature oscillator, at 25 ℃ of temperature, the rate oscillation 12h of 150r/min is to adsorption equilibrium, and now the mass ratio of the uranium in uranium-containing waste water and adsorbent is respectively 1: 5000,1: 2500,1: 1000,1: 500.Get the concentration that inductively coupled plasma emission spectrometer for supernatant (ICP-AES) is tested residual uranium, three groups of each experiment settings are parallel, and result is with the arithmetic average value representation, and the calculating standard deviation, guarantees measuring accuracy.As calculated, the eliminating rate of absorption of uranium is respectively 99.7%, 99.8%, 99.9%, 99.7%.Accompanying drawing 2 is the impact of uranyl nitrtate initial concentration on eliminating rate of absorption.
Visible, magnesium-modified attapulgite adsorbent has very high clearance to the uranium polluted-water of 5-150mg/L concentration.
Embodiment 3
Make magnesium-modified attapulgite adsorbent with embodiment 1.
Accurate weighing is through magnesium-modified attapulgite adsorbent 0.5000g (± 0.0005g), be placed in 250mL tool plug conical flask, add in the uranyl nitrate solution that 10mL concentration is 100mg/L, be placed in constant temperature oscillator, at 5,15,25,40 ℃ of temperature, the rate oscillation 12h of 150r/min is to adsorption equilibrium respectively, and now the mass ratio of the uranium in uranium-containing waste water and adsorbent is 1: 500.Get the concentration that inductively coupled plasma emission spectrometer for supernatant (ICP-AES) is tested residual uranium, three groups of each experiment settings are parallel, and result is with the arithmetic average value representation, and the calculating standard deviation, guarantees measuring accuracy.As calculated, the eliminating rate of absorption of uranium is respectively 99.5%, 99.4%, 99.7%, 99.5%.Accompanying drawing 3 is the impact of temperature on eliminating rate of absorption.
Visible, magnesium-modified attapulgite adsorbent adsorption uranium temperature influence is little, is applicable to the removal of uranium in the 0-50 ℃ of polluted-water under temperature conditions.
Make magnesium-modified attapulgite adsorbent with embodiment 1.
Accurate weighing is through magnesium-modified attapulgite adsorbent 0.5000g (± 0.0005g), be placed in 250mL tool plug conical flask, add in the uranyl nitrate solution that 10mL concentration is 100mg/L, be placed in constant temperature oscillator, at 25 ℃ of temperature, respectively with 0,100,150, the rate oscillation 12h of 250r/min is to adsorption equilibrium, now the mass ratio of the uranium in uranium-containing waste water and adsorbent is 1: 500.Get inductively coupled plasma emission spectrometer for supernatant (ICP-AES) and test residual uranium concentration, three groups of each experiment settings are parallel, and result is with the arithmetic average value representation, and the calculating standard deviation, guarantees measuring accuracy.As calculated, the uranium eliminating rate of absorption is respectively 99.5%, 99.7%, 99.7%, 99.7%.Accompanying drawing 4 is the impact of oscillation rate on eliminating rate of absorption.
Visible, magnesium-modified attapulgite adsorbent can directly be added in uranium-containing waste water, without vibration, easy to use.
Embodiment 5
Make magnesium-modified attapulgite adsorbent with embodiment 1.
Accurate weighing is through magnesium-modified attapulgite adsorbent 0.5000g (± 0.0005g), be placed in 250mL tool plug conical flask, add in the uranyl nitrate solution that 10mL concentration is 100mg/L, regulator solution pH value is respectively 1,3,5,7,9,11,13 and is placed in constant temperature oscillator, at 25 ℃ of temperature, the rate oscillation 12h of 150r/min is to adsorption equilibrium, and now the mass ratio of the uranium in uranium-containing waste water and adsorbent is 1: 500.Get the concentration that inductively coupled plasma emission spectrometer for supernatant (ICP-AES) is tested residual uranium, three groups of each experiment settings are parallel, and result is with the arithmetic average value representation, and the calculating standard deviation, guarantees measuring accuracy.As calculated, the uranium eliminating rate of absorption is respectively 27.5%, 61.5%, 74.7%, 99.7%, 99.1%, 98.3%, 85.5%.Accompanying drawing 5 is the impact of pH on eliminating rate of absorption.
Visible, pH is larger to Adsorption Effect, and preferred solution pH value scope is 7-13.
The attapulgite taken after 5g purifies is placed in the 500mL beaker, adds 250mL distilled water, after magnetic agitation 0.5h, adds respectively the MgCl of 0.423g, 1.269g, 2.115g, 4.229g, 6.344g
26H
2o (being equivalent to respectively 0.05g, 0.15g, 0.25g, 0.50g, 0.75g Mg), magnetic agitation 30min, guarantee MgCl
26H
2o dissolves fully, regulates pH value=7, continues stirring 1h, in 40 ℃ of dry 48h, is ground to the magnesium-modified attapulgite adsorbent that 100 orders make different magnesium amounts after centrifugal 3 times.In adsorbent, magnesium element content is designated as respectively 7.74%, 17.6%, 25.3%, 48.5%, 58.7% by weight percentage.
Accurate weighing is through magnesium-modified attapulgite adsorbent 0.5000g (± 0.0005g) respectively, be placed in 250mL tool plug conical flask, add in the uranyl nitrate solution that 10mL concentration is 100mg/L, be placed in constant temperature oscillator, at 25 ℃ of temperature, with the rate oscillation 12h of 150r/min, to adsorption equilibrium, now the mass ratio of the uranium in uranium-containing waste water and adsorbent is 1: 500.Get the concentration that inductively coupled plasma emission spectrometer for supernatant (ICP-AES) is tested residual uranium, three groups of each experiment settings are parallel, and result is with the arithmetic average value representation, and the calculating standard deviation, guarantees measuring accuracy.As calculated, the uranium eliminating rate of absorption is respectively 99.6%, 99.7%, 99.8%, 100%, 99.9%.Accompanying drawing 6 is the impacts of different magnesium amount modified attapulgite adsorbents on eliminating rate of absorption.
Embodiment 7
Take the 0.5000g absorption magnesium-modified Concave-convex clay rod (uranyl nitrtate of absorption 100mg/L) after saturated in centrifuge tube, add the NaOH solution that 10mL concentration is 10% to soak 3 hours, with distilled water washing 3 times, centrifugal by Separation of Solid and Liquid, solid absorbent takes out and is placed in tool plug conical flask, add the uranyl nitrate solution that 10mL concentration is 100mg/L, adsorb saturated after, get the concentration that inductively coupled plasma emission spectrometer for supernatant (ICP-AES) is tested residual uranium, three groups of each experiment settings are parallel, result is with the arithmetic average value representation, and calculating standard deviation, guarantee measuring accuracy.So, repeated regeneration three times, as calculated, after each regeneration is used, the clearance of uranium is respectively 99.7%, 97.7%, 92.5%.
Claims (10)
1. the method for a magnesium-modified attapulgite sorbent treatment uranium-containing waste water is characterized in that:
The concentration of described uranium in waste water is 5-150mg/L;
Add magnesium-modified attapulgite adsorbent in described uranium-containing waste water, the uranium in described uranium-containing waste water and the mass ratio of described adsorbent are 1: (500-5000);
Under the condition that described adsorption process is 0-50 ℃ in temperature, adopt static state and/or vibration, agitating mode to carry out;
In described magnesium-modified attapulgite adsorbent, magnesium element content is 7.74%-58.7% by weight percentage;
Magnesium-modified dose that in described magnesium-modified attapulgite adsorbent, adds is magnesium compound soluble in water.
2. the method for magnesium-modified attapulgite sorbent treatment uranium-containing waste water as claimed in claim 1 is characterized in that:
Uranium in described uranium-containing waste water and the mass ratio of described adsorbent are 1: 500.
3. the method for magnesium-modified attapulgite sorbent treatment uranium-containing waste water as claimed in claim 2 is characterized in that:
The pH value scope of described uranium-containing waste water is 7-13.
4. the method for magnesium-modified attapulgite sorbent treatment uranium-containing waste water as claimed in claim 3 is characterized in that:
Described adsorption time is 1-12h.
5. the method for magnesium-modified attapulgite sorbent treatment soil uranium-containing waste water as claimed in claim 1 is characterized in that:
The method of described magnesium-modified attapulgite sorbent treatment uranium-containing waste water also comprises the regeneration of adsorbent;
The regeneration of described adsorbent be by the saturated adsorbent of absorption with NaOH, mix, immersion, clear water wash and get final product, wherein
Described NaOH concentration is 5%-15%; Described soak time is 2-3h.
6. as the method for the magnesium-modified attapulgite sorbent treatment uranium-containing waste water of one of claim 1～5, it is characterized in that:
Described magnesium compound soluble in water is selected from one or more in magnesium sulfate, magnesium nitrate, magnesium chloride.
7. the method for magnesium-modified attapulgite sorbent treatment uranium-containing waste water as claimed in claim 6 is characterized in that:
Described magnesium compound soluble in water is MgCl
26H
2o.
8. the method for magnesium-modified attapulgite sorbent treatment uranium-containing waste water as claimed in claim 6, it is characterized in that: the preparation process of described magnesium-modified attapulgite adsorbent is:
Attapulgite after purification is scattered in water and adds magnesium compound soluble in water, is hydrolyzed and regulates the pH value by magnesium salts and make described magnesium-modified attapulgite adsorbent.
9. the method for magnesium-modified attapulgite sorbent treatment uranium-containing waste water as claimed in claim 8, it is characterized in that: the preparation process of described magnesium-modified attapulgite adsorbent is:
Attapulgite after purification is scattered in water, adds magnesium compound soluble in water;
It is neutral regulating the pH value;
Stir, centrifugal, make described magnesium-modified attapulgite adsorbent after drying, grinding.
10. the method for magnesium-modified attapulgite sorbent treatment uranium-containing waste water as claimed in claim 9 is characterized in that:
Regulate the pH value with watery hydrochloric acid and dilute sodium hydroxide.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111234827A (en) * | 2020-01-17 | 2020-06-05 | 湖南大学 | Heavy metal contaminated soil remediation agent and preparation method and application thereof |
| CN113083221A (en) * | 2021-03-12 | 2021-07-09 | 华南理工大学 | Si/Mg modified halloysite material and preparation method and application thereof |
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| US5098612A (en) * | 1988-12-10 | 1992-03-24 | Rowsell Farrell D | Method of preparing solidified and stabilized hazardous or radioactive liquids |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111234827A (en) * | 2020-01-17 | 2020-06-05 | 湖南大学 | Heavy metal contaminated soil remediation agent and preparation method and application thereof |
| CN111234827B (en) * | 2020-01-17 | 2021-12-10 | 湖南大学 | Heavy metal contaminated soil remediation agent and preparation method and application thereof |
| CN113083221A (en) * | 2021-03-12 | 2021-07-09 | 华南理工大学 | Si/Mg modified halloysite material and preparation method and application thereof |
| CN113083221B (en) * | 2021-03-12 | 2022-06-14 | 华南理工大学 | Si/Mg modified halloysite material and preparation method and application thereof |
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| C06 | Publication | ||
| PB01 | Publication | ||
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| DD01 | Delivery of document by public notice |
Addressee: Sun Danni Document name: the First Notification of an Office Action |
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| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20131218 |