CN103274757B - Function ceramic material for efficiently filtering radioactive iodine and cesium, and preparation method thereof - Google Patents
Function ceramic material for efficiently filtering radioactive iodine and cesium, and preparation method thereof Download PDFInfo
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Abstract
The present invention discloses a function ceramic material for efficiently filtering radioactive iodine and cesium, and a preparation method thereof. The material is prepared through the following steps that: industrial sludge and clay are adopted as main materials, active carbon or wood chips, calcium hydroxide or calcium carbonate, iron powder or iron oxide powder, liquid paraffin and other auxiliary materials are matched, processes of mixing, stirring, granulation and the like are performed, and sintering in performed in an oxygen deficiency atmosphere or a reduction atmosphere to prepare the material. The function ceramic material has characteristics of porous property, rich pores, large specific surface area, strong absorption capacity, high water filtration flow, efficient removal and immobilization of radioactive iodine and cesium in nuclear wastewater, and easy shape and size adjustment, and can be used for purification treatments of nuclear wastewater and medical radioactive wastewater.
Description
Technical field
The present invention relates to a kind of ceramic material for Spent Radioactive purifying water process and preparation method thereof.
Background technology
According to the statistic data of 2005, countries in the world Nuclear power plants generated energy accounted for 16% of gross generation, and nuclear energy has become one of main energy in the world today.But the Nuclear power plants leakage accident occurring time and again makes the peaceful use of recognizing nuclear energy that people are deep not harmless.Except nuclear leakage, in Nuclear power plants normal operation situation, in the radioactive wastewater of a large amount of discharges, contain equally a large amount of radionuclides, if dealt with improperly, these radiocontamination will produce huge harm to environment, ecology and the mankind.Therefore, the safe handling of nuclear pollution has become a great problem of the world today, and in decades, various countries' scientists is all paid special attention to this, and hope can find a kind of effective means these radionuclides to be removed or fixed.
The radionuclide that in general, may exist in nuclear waste water mainly comprises
131i,
125i,
129i,
134cs,
137cs,
226ra,
228ra etc.The radionuclide discharging in nuclear leakage accident generally with
131i and
137cs is the most common.Compared to other radionuclide, these two kinds of nucleic human body ratios are easier to absorb, and its hazardness is very large.Therefore, in Spent Radioactive water treatment procedure, the removal of radioiodine and caesium and be fixedly crucial.Be inorganic ion exchange material processing radioactive wastewater area research and utilizing more in the world at present, what wherein radiocesium unit is have to a better removal effect has zeolite, ammonium phosphomolybdate and a yellow prussiate etc.
Zeolite can reach 2meq/g to the theoretical exchange capacity of caesium, and S. Bagosi etc. has studied cement-resin-clinoptilolite matrix material in radioactive wastewater
137the removal effect of Cs, found in 3 years
137the clearance of Cs can reach 70-75%[Cement and Concrete Research 1999,29: 479 – 485].Silicotitanate (CST) TAM5 of the use modifications such as C.V.Philip removes Cs[Separation Science and Technology 2003,38 (12-13): 009-3029. from overbasic radioactive wastewater].A. E. Osmanlioglu research remove from radioactive wastewater with using natural clinoptilolite several critical nuclides (
137cs,
60co,
90sr and
110mag) [Journal of Hazardous Materials B 2006,137:332 ~ 335].But zeolite is poor to the selectivity of caesium, be easily subject to the interference of other ions (as potassium ion), cause its actual loading capacity very low, be difficult to meet actual needs.Although ammonium phosphomolybdate has the selectivity of height to cesium ion, its crystal grain is too small, cannot carry out packed bed operation.Therefore, be difficult to carry out large-scale industrial application.
The yellow prussiate of being fixed by transition metal is to radioactivity Cs
+there is good selection receptivity, at Na
+concentration is in the situation of 5mol/L, and such material is for Cs
+selectivity coefficient up to 1500000[Nucleat Science and Engineering 2001,137:206-214].Chinese invention patent 99805991.9 discloses a kind of sorbent material for Adsorption of Radioactive nucleic based on containing fine-fibered first gram material, and the units such as the caesium in the aqueous solution, uranium, plutonium, americium, curium are have to good adsorption effect.Chinese invention patent 200710064453.0 discloses a kind of preparation method of yellow prussiate/silicon dioxide hybrid materials of high capacity amount, has overcome yellow prussiate charge capacity low, granulation difficulty, the problem such as granule strength is not high.But the toxicity of yellow prussiate is one is all the time difficult to the problem of ignoring, and environment is had to larger harm.
All in all, over nearly 60 years, countries in the world scientist has obtained many important achievements in the research of Spent Radioactive water treatment field, and major part is also for practice.But these technology and associated materials more or less all exist some problems, crystal grain as low in the selectivity of zeolite filler, ammonium phosphomolybdate is too small, the toxicity of yellow prussiate etc.In addition, current Research Literature and disclosed patent mainly concentrate on the filtering of radiocesium, relate to less for filtering material and the technology of radioiodine.Be directed to this, the present invention has announced a kind of high-efficient filter and has removed ceramic material of radioiodine and caesium and preparation method thereof.
Summary of the invention
The object of the present invention is to provide a kind of high-efficient filter to remove ceramic material of radioiodine and caesium and preparation method thereof.
For achieving the above object, the technical solution used in the present invention is as follows:
High-efficient filter of the present invention, except the ceramic material of radioiodine and caesium, is to be fired and formed by following raw material, the consumption following (being weight part) of each composition:
Mud and clay 70-80 part, calcium carbonate or calcium hydroxide 11-14 part, wood chip or gac 5-8 part, whiteruss 1-5 part, iron powder or brown iron oxide 4-6 part.The above mud is the excess sludge of sewage work, and clay is kaolin, wilkinite or atlapulgite.
Clay in raw material is one or more in kaolin, wilkinite or atlapulgite.
In raw material, the weight part ratio of mud and clay is between 1:1-2:1.
High-efficient filter of the present invention, except the ceramic material preparation method of radioiodine and caesium, comprises the following steps:
(1) by above-mentioned formula, starting material are fully mixed, stirred, be modulated into mud, use tablets press mud to be made to the mud pellet of desired shape, dry into base;
(2) moulded pottery not yet put in a kiln to bake step (1) being made is placed in high temperature sintering furnace, under anoxic or reducing atmosphere, fire, temperature rise rate is no more than 100 DEG C per hour, in the time that furnace temperature reaches 550-600 DEG C, and insulation 1.5-2 hour, then continue to heat up with the temperature rise rate of 100 DEG C per hour, until 1050-1250 DEG C, insulation 2.5-4 hour, stops heating, furnace temperature is down to room temperature by speed with 150-200 per hour DEG C, obtains vesicular stupalith.
Ceramic material of the present invention can remove radioiodine and caesium by high-efficient filter, and technical characterstic is as follows:
(1) ceramic material of the present invention is a kind of porous material, in ceramic sintering process, due to organic decomposition, produces a large amount of micropores in granule interior and surface, and porosity can reach 80%, and specific surface area is large, has very strong physical adsorption crystallized ability.
(2) ceramic material of the present invention sintering under oxygen free condition, makes the organic carbon in mud.The porosity that has increased on the one hand material, makes material have the filtering function that is similar to gac on the other hand.
(3) in the batching of ceramic material of the present invention, contain ferro element, after high temperature sintering, the Si in mud and clay is combined, and forms complicated Si-Fe compound, makes material have stronger ion-exchange and crystallized ability.
(4) porosity of ceramic material of the present invention, pore size, physical dimension free adjustment as required, is applicable to various environment.
Ceramic material disclosed in this invention, the excess sludge and the clay that are employing sewage work are major ingredient, taking calcium source, charcoal source and ferrous source material etc. as auxiliary material, under anoxic or reducing atmosphere, fire a kind of porous ceramic film material forming, material has physical adsorption and chemisorption characteristic concurrently, can remove iodine and the cesium element in radioactive wastewater by high-efficient filter.
Ceramic material of the present invention is a kind of inorganic materials, and corrosion-resistant, high temperature resistant, radiation-resistant feature makes it have the wider scope of application than the organic resin ion-exchange of present extensive application and membrane separation technique.Ceramic material of the present invention is inorganic materials for radiocesium and iodine filtration than other, high to the selectivity of iodine and caesium, can make according to demand the particle of various size, be convenient to carry out packed bed operation, and nontoxic, environmentally friendly.Ceramic material of the present invention is a kind of composite functional material with physics and chemistry absorption feature, has better filtration result than the filtering technique of simple function.Ceramic material of the present invention is a large amount of use wastewater sludges in synthetic, are a kind of refuse reclamations, have realized the treatment of wastes with processes of wastes against one another, and the cost of another major ingredient clay in material and other auxiliary material is also extremely low simultaneously, is very suitable for large-scale application.
Brief description of the drawings
Fig. 1 is the outward appearance photo of the vesicular ceramic material that in step in embodiment 1 (2), gained diameter is 2mm.
Fig. 2 is the outward appearance photo of the vesicular ceramic material that in step in embodiment 2 (2), gained diameter is 5mm.
Fig. 3 is that diameter shown in Fig. 1 is vesicular ceramic material scanning electronic microscope (SEM) picture of 2mm.
Specific embodiments
Specific embodiments is preferred version of the present invention, and the present invention is not limited to this.
embodiment 1
Take according to the following ratio raw material,
Mud 40 Kg, clay (kaolin) 40 Kg, calcium carbonate 12 Kg, wood chip 8 Kg, whiteruss 5 Kg, brown iron oxide 6 Kg.
Preparation process is as follows:
(1) by above-mentioned formula, starting material are fully mixed, stirred, be modulated into mud, use tablets press that mud is made to diameter 4mm spheroidal particle, dry into base;
(2) moulded pottery not yet put in a kiln to bake step (1) being made is placed in high temperature sintering furnace, at H
2under atmosphere, fire, while being warmed up to 550 DEG C with 80 DEG C per hour, be incubated 2 hours, then continue to heat up with the temperature rise rate of 100 DEG C per hour, until 1050 DEG C, be incubated 4 hours, stop heating, with the speed of 150 DEG C per hour, furnace temperature is down to room temperature, obtaining diameter is the vesicular stupalith of 2mm.
embodiment 2
Take according to the following ratio raw material,
Mud 40 Kg, clay (wilkinite) 30 Kg, calcium carbonate 11 Kg, gac 5 Kg, whiteruss 3 Kg, brown iron oxide 6 Kg.
Preparation process is as follows:
(1) by above-mentioned formula, starting material are fully mixed, stirred, be modulated into mud, use tablets press that mud is made to diameter 4mm spheroidal particle, dry into base;
(2) moulded pottery not yet put in a kiln to bake step (1) being made is placed in high temperature sintering furnace, at H
2under atmosphere, fire, while being warmed up to 550 DEG C with 80 DEG C per hour, be incubated 2 hours, then continue to heat up with the temperature rise rate of 100 DEG C per hour, until 1100 DEG C, be incubated 3 hours, stop heating, with the speed of 150 DEG C per hour, furnace temperature is down to room temperature, obtaining diameter is the vesicular stupalith of 5mm.
embodiment 3
Take according to the following ratio raw material, the consumption of each composition is weight part:
Mud 40 Kg, clay (atlapulgite) 20 Kg, calcium carbonate 13 Kg, wood chip 7 Kg, whiteruss 2 Kg, iron powder 5 Kg.
Preparation process is as follows:
(1) by above-mentioned formula, starting material are fully mixed, stirred, be modulated into mud, use tablets press that mud is made to diameter 4mm spheroidal particle, dry into base;
(2) moulded pottery not yet put in a kiln to bake step (1) being made is placed in high temperature sintering furnace, at N
2under atmosphere, fire, while being warmed up to 600 DEG C with 80 DEG C per hour, be incubated 2 hours, then continue to heat up with the temperature rise rate of 100 DEG C per hour, until 1050 DEG C, be incubated 4 hours, stop heating, with the speed of 200 DEG C per hour, furnace temperature is down to room temperature, obtain vesicular stupalith.
embodiment 4
Take according to the following ratio raw material,
Mud 50 Kg, clay (kaolin) 30Kg, calcium hydroxide 14 Kg, gac 6 Kg, whiteruss 1 Kg, iron powder 4 Kg.
Preparation process is as follows:
(1) by above-mentioned formula, starting material are fully mixed, stirred, be modulated into mud, use tablets press that mud is made to diameter 6mm spheroidal particle, dry into base;
(2) moulded pottery not yet put in a kiln to bake step (1) being made is placed in high temperature sintering furnace, under Ar atmosphere, fire, while being warmed up to 550 DEG C with 80 DEG C per hour, be incubated 2 hours, then continue to heat up with the temperature rise rate of 100 DEG C per hour, until 1250 DEG C, be incubated 2.5 hours, stop heating, with the speed of 150 DEG C per hour, furnace temperature is down to room temperature, obtain vesicular stupalith.
embodiment 5
The adsorptive power test experiments situation of the ceramic material of preparing with embodiment 1 to radioactivity iodine-125.
Equipment and sample: 2L chromatography column, 10 milligrams of potassiumiodides, iodine-125 mark liquid, ceramic material described in 300g embodiment 1, high purity germanium detector
Experimentation: after 10 milligrams of potassiumiodides are dissolved in 250 ml distilled waters, this liquor kalii iodide of getting 12.5 milliliters is diluted to 1 liter.Add after 100 microlitre iodine-125 mark liquid, for water inlet solution, get the measurement of two 100 microlitre samples for feed liquor sample radioactive intensity simultaneously.Described in 300 grams of embodiment 1, after ceramic material dress post, adding distil water soaked after 15 minutes, discharged.
Pour 1 liter of water inlet solution into chromatography column, start to filter.60 milliliters of initial fluids, have a small amount of naked eyes visible, as waste liquid.Solution after all the other filtrations is concentrated and is placed in 1.25 liters of containers.After all collecting, in collection container, get the measurement of three 100 microlitre samples for fluid radioactive intensity.After 3 days, getting three 100 microlitre samples measures again.
Sample is placed in to GWL HpGe (HPGe) trap type detector (EG & G ORTEC, USA), Measuring Time 1200-12000 s.
Experimental result: sample introduction solution specific radioactivity is 1.85 × 10
3bq/ml.Relatively sample introduction solution and go out the specific activity of liquor, calculating ceramic material prepared by embodiment 1 is 92.1 ± 0.5% to iodine-125 clearance.(this result is provided by core analytical technology key lab of Institute of High Energy Physcis, Academia Sinica).
embodiment 6
The adsorptive power test experiments situation of the ceramic material of preparing with embodiment 2 to on-radiation cesium ion.
Equipment and sample: 2L chromatography column, 0.1 milliliter of caesium reference liquid (1000mg/L), ceramic material described in 500g embodiment 2, icp ms (ICP-MS)
Experimentation: 0.1 milliliter of caesium reference liquid is diluted to 5L, makes caesium stoste.
Described in 500g embodiment 2, after ceramic material dress post, add pure water and soak after half hour, be released into liquid level and reach filter material surface.
Connect after 5L sample introduction solution tank, start to collect the rear solution of filtration.Within every 10 minutes, collect first-time filtrate, 5L sample introduction liquid has filtered after 160 minutes.
Use ICP-MS to analyze cesium ion concentration in caesium stoste and filtrate.
Experimental result: the water inlet solution that caesium original liquid concentration is 11.56ppb, after ceramic material described in embodiment 2 filters, goes out aqueous solution cesium ion undetected, is less than the resolving power of detector.Described in embodiment 2, ceramic material reached 100% to the adsorption rate of cesium ion at 10 minutes, and afterwards to 160 minute keeps adsorption rate stable.Experimental result is in table one (this result is provided by core analytical technology key lab of Institute of High Energy Physcis, Academia Sinica).
In table 1 table, cesium ion concentration one hurdle shows that negative value is because its concentration is less than due to detector sensing range
| Time | No. | Cesium ion concentration (ppb) | Adsorption rate |
| 0min | 17 | 11.56 | 0% |
| 10min | 16 | -0.003 | 100% |
| 20min | 15 | -0.002 | 100% |
| 30min | 14 | -0.002 | 100% |
| 40min | 13 | -0.002 | 100% |
| 50min | 12 | -0.002 | 100% |
| 60min | 11 | -0.003 | 100% |
| 70min | 10 | -0.002 | 100% |
| 80min | 9 | -0.003 | 100% |
| 90min | 8 | -0.003 | 100% |
| 100min | 7 | -0.003 | 100% |
| 110min | 6 | -0.003 | 100% |
| 120min | 5 | -0.003 | 100% |
| 130min | 4 | -0.003 | 100% |
| 140min | 3 | -0.003 | 100% |
| 150min | 2 | -0.003 | 100% |
| 160min | 1 | -0.002 | 100% |
Claims (4)
1. high-efficient filter, except a ceramic material for radioiodine and caesium, is characterized in that being fired and being formed by following raw material, and the consumption of each composition is weight part:
Mud and clay 70-80 part, calcium carbonate or calcium hydroxide 11-14 part, wood chip or gac 5-8 part, whiteruss 1-5 part, iron powder or brown iron oxide 4-6 part;
Its preparation method comprises the steps:
(1) by above-mentioned formula, starting material are fully mixed, stirred, be modulated into mud, use tablets press mud to be made to the mud pellet of desired shape, dry into base;
(2) moulded pottery not yet put in a kiln to bake step (1) being made is placed in high temperature sintering furnace, under anoxic or reducing atmosphere, fire, temperature rise rate is no more than 100 DEG C per hour, in the time that furnace temperature reaches 550-600 DEG C, and insulation 1.5-2 hour, then continue to heat up with the temperature rise rate of 100 DEG C per hour, until 1050-1250 DEG C, insulation 2.5-4 hour, stops heating, furnace temperature is down to room temperature by speed with 150-200 per hour DEG C, obtains vesicular stupalith.
2. high-efficient filter, except the ceramic material of radioiodine and caesium, is characterized in that: the clay in raw material is one or more in kaolin, wilkinite or atlapulgite as claimed in claim 1.
3. the high-efficient filter as described in claims 1 or 2, except the ceramic material of radioiodine and caesium, is characterized in that: in raw material, the weight part ratio of mud and clay is between 1:1-2:1.
4. high-efficient filter, except the ceramic material of radioiodine and caesium, is characterized in that: described in step (2), anoxic or reducing atmosphere can be any one in vacuum, nitrogen atmosphere, argon atmospher or nitrogen atmosphere as claimed in claim 1.
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| WO2015180772A1 (en) * | 2014-05-28 | 2015-12-03 | Itn Nanovation Ag | Method and system for removing radioactive nuclides from water |
| CN105645924B (en) * | 2015-12-30 | 2018-09-18 | 深圳市新陶环保特种材料科技有限公司 | A kind of functional ceramic material, preparation method and application |
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