EP0157683B1 - Procédé de bitumage de déchets radioactifs constitués par des résines échangeuses de cations et/ou par des résines échangeuses d'anions - Google Patents

Procédé de bitumage de déchets radioactifs constitués par des résines échangeuses de cations et/ou par des résines échangeuses d'anions Download PDF

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Publication number
EP0157683B1
EP0157683B1 EP85400496A EP85400496A EP0157683B1 EP 0157683 B1 EP0157683 B1 EP 0157683B1 EP 85400496 A EP85400496 A EP 85400496A EP 85400496 A EP85400496 A EP 85400496A EP 0157683 B1 EP0157683 B1 EP 0157683B1
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EP
European Patent Office
Prior art keywords
resins
exchange resins
pretreatment
water
ions
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Lifetime
Application number
EP85400496A
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German (de)
English (en)
French (fr)
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EP0157683A1 (fr
Inventor
Guy Lefillatre
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Commissariat a lEnergie Atomique et aux Energies Alternatives CEA
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Commissariat a lEnergie Atomique CEA
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    • G—PHYSICS
    • G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
    • G21F—PROTECTION AGAINST X-RADIATION, GAMMA RADIATION, CORPUSCULAR RADIATION OR PARTICLE BOMBARDMENT; TREATING RADIOACTIVELY CONTAMINATED MATERIAL; DECONTAMINATION ARRANGEMENTS THEREFOR
    • G21F9/00—Treating radioactively contaminated material; Decontamination arrangements therefor
    • G21F9/04—Treating liquids
    • G21F9/06—Processing
    • G21F9/12—Processing by absorption; by adsorption; by ion-exchange
    • G—PHYSICS
    • G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
    • G21F—PROTECTION AGAINST X-RADIATION, GAMMA RADIATION, CORPUSCULAR RADIATION OR PARTICLE BOMBARDMENT; TREATING RADIOACTIVELY CONTAMINATED MATERIAL; DECONTAMINATION ARRANGEMENTS THEREFOR
    • G21F9/00—Treating radioactively contaminated material; Decontamination arrangements therefor
    • G21F9/28—Treating solids
    • G21F9/30—Processing
    • G21F9/301—Processing by fixation in stable solid media
    • G21F9/307—Processing by fixation in stable solid media in polymeric matrix, e.g. resins, tars
    • G—PHYSICS
    • G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
    • G21F—PROTECTION AGAINST X-RADIATION, GAMMA RADIATION, CORPUSCULAR RADIATION OR PARTICLE BOMBARDMENT; TREATING RADIOACTIVELY CONTAMINATED MATERIAL; DECONTAMINATION ARRANGEMENTS THEREFOR
    • G21F9/00—Treating radioactively contaminated material; Decontamination arrangements therefor
    • G21F9/04—Treating liquids
    • G21F9/06—Processing
    • G21F9/16—Processing by fixation in stable solid media
    • G—PHYSICS
    • G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
    • G21F—PROTECTION AGAINST X-RADIATION, GAMMA RADIATION, CORPUSCULAR RADIATION OR PARTICLE BOMBARDMENT; TREATING RADIOACTIVELY CONTAMINATED MATERIAL; DECONTAMINATION ARRANGEMENTS THEREFOR
    • G21F9/00—Treating radioactively contaminated material; Decontamination arrangements therefor
    • G21F9/28—Treating solids
    • G21F9/30—Processing

Definitions

  • the present invention relates to a conditioning process by coating in bitumen radioactive waste consisting of ion exchange resins.
  • the coating of radioactive waste in bitumen is generally carried out by mixing an aqueous suspension of radioactive waste with bitumen in the fluidized state, then evaporating the water from the suspension and pouring the mixture thus obtained into a container to solidify it.
  • the treated waste is evaporation concentrates and / or precipitation sludges which contain salts such as sodium carbonates and sulphates.
  • the radioactive waste consists of organic ion exchange resins, in particular of the anionic type in OH- and / or CI- form
  • the implementation of these conditioning processes by coating in bitumen does not make it possible to obtain a capacity. sufficient treatment of the asphalt installation.
  • the bituminous mixes obtained have the major drawback of swelling when they are then immersed in water. In this case, the increase in volume of the coated materials can reach 20%, and exceed 100% in certain extreme cases, which leads to disaggregation of the coated waste.
  • thermosetting resins or in cement there are also known methods of conditioning ion exchange materials in thermosetting resins or in cement, as described in French patent FR-A 2361724 and in Japanese patent 48-28899. According to these methods, in order to obtain packaged products free of cracks, it is necessary to carry out a pretreatment of the ion exchange resins to replace the H + ions with other cations, in order to prevent the resins from being able to fix some of the reagents necessary to harden the thermosetting resin or set the cement.
  • German patent DE-A-3 102 473 also describes a process for pretreatment of a mixture of cation exchange resins and anion exchange resins which then makes it possible to condition the resins separately by incorporation in bitumen or cement.
  • the mixture of resins in order to separate the cation exchange resins from the anion exchange resins, the mixture of resins is brought into contact with an aqueous solution of a salt, such as a sulfate, a chloride, a nitrate or an acetate. of alkali metal, to replace the H + and / or Na + ions of cationic resins with sodium and the OH- ions of anionic resins with other anions.
  • the resins can then be separated by means of a liquid which has a density between that of the grains of one kind of resin and that of the grains of the other kind of resin.
  • the present invention relates specifically to a method of conditioning by bituminization of radioactive waste constituted either by cation exchange resins or by a mixture of cation exchange resins and anion exchange resins, which comprises a pretreatment step allowing solve the problems mentioned above.
  • the pretreatment is carried out by means of a salt such that the H + and / or Na + ions of the cation exchange resins are replaced by ions chosen from the group comprising Ca ++ , Sr ++ , and, Ba ++ and, the OH- and / or CI- ions of anion exchange resins by an anion chosen from the group comprising NO 3 - , HCO 2 - and CH 3 CO 2 - .
  • the pretreatment is carried out by bringing said resins into contact, preferably with stirring, with an aqueous solution of a calcium, strontium or barium salt, said salt being chosen from the group comprising: nitrates, acetates and formates.
  • This embodiment of the pretreatment is in particular suitable for the treatment of a mixture of cation exchange resins and anion exchange resins because it allows the replacement of OH- or CI- ions of anionic resins by anions simultaneously. nitrates, acetates or formates and also replace the H + ions of the cationic resins with calcium, strontium or barium.
  • the structure of the three-dimensional network of ion exchange resins is modified by introducing into the molecular chain ions such as Ba ++ and / or NO 3 - or CH a COO-, which occupy a place more important than the H + , OH- and CI- ions initially present.
  • This makes it possible to prevent the penetration of water into the denser macromolecular network of the pretreated resin and thus to decrease the degree of hydration of the resin.
  • the exchange, ion, anionic and cationic resins have the particularity of swelling in water in a significant manner.
  • Their increase in volume is generally of the order of 20% for anionic resins in OH- and / or CI- form and greater than 50% for cationic resins in Na + form.
  • This swelling is due to the penetration of water into the three-dimensional skeleton of the resins, which is particularly hydrophilic in the case of anionic resins which contain quaternary ammonium or amine groups and in the case of cationic resins which contain sodium sulfonate groups grafted to both types of resins on a polystyrene radical.
  • the processing capacity of bituminization plants is lower when dealing with resins of these types.
  • the bituminous mixes obtained after the bituminization treatment have the disadvantage of swelling in water.
  • the step of pretreatment of ion exchange resins with a salt such as barium nitrate does not have the same object as the step of pretreatment of prior processes (FR- A-2361724 and Japanese patent 48/28899), since it is not intended to prevent the ion-exchange resins from consuming some of the reagents necessary for the reaction to form the coating matrix.
  • the pretreatment step of the invention does not have the same object as the pretreatment step of French patent FR-A-2,356,246.
  • waste consists of concentrates of and / or radioactive material sludge such as chemical precipitation sludge containing salts, and the problem to be solved is to transform salts such as sulphate and sodium carbonate into salts having a less tendency to capture molecules of water.
  • the waste is ion exchange resins, which do not contain. salts, and the problem to be solved is to decrease the hydration capacity of the macromolecular network of ion exchange resins.
  • the operation is carried out conventionally using for example the techniques described in French patents 1,315,162 and 2,052,903 or American patent 3,298,961.
  • the devices used are also of a conventional type and can be made up of thin-film evaporators, double or quadruple screw extruders, etc.
  • the method of the invention is particularly applicable to the treatment of cationic and optionally anionic resins with a polystyrene skeleton in beads and / or ground.
  • resins in the form of beads such as Iss resins sold under the brand Duolite by Diaprosim or resins sold under the brand Amberlite by Rohm and Haas.
  • ground resins mention may be made of the Microionex resins sold by Diaprosim.
  • anionic and cationic resins are treated as a mixture
  • any proportion of anionic resins in the range between 0 and 100% can be used.
  • the pretreatment step is preferably carried out by introducing into a tank a certain amount of an aqueous solution of a salt of Ba ++ , Ca ++ or Sr2 + containing N0 3 - , HCO 2 - or CH 3 CO 2 - ions.
  • the resins to be pretreated are suspended in the solution and the whole is stirred for a sufficient time which is chosen, depending on the salt concentration of the solution, so as to obtain the desired saturation rate of the exchange resins. ions.
  • the salt concentration and the treatment duration are chosen so as to obtain a saturation rate of anions: N0 3 -, HCO 2 - or CH 3 CO 2 - anion exchange resins close to 100%.
  • Figures 1 and 2 are diagrams representing the percentage increase in volume bituminous mixtures of cation exchange resins, obtained either by the process of the prior art, or by the process of the invention, depending on the time of immersion in water.
  • This example illustrates the treatment of cation exchange resins Amberlite IR 120 H.
  • the resins are transferred by means of a hydro-ejector using demineralized water, to a treatment tank provided with a mechanical agitator and with an ultrasonic detection device of the level of the solid-liquid interface.
  • a 0.37 mol.l -1 solution of barium nitrate is prepared and a volume V of this solution is introduced into the treatment tank, that is to say a volume identical to that occupied by decanted resins.
  • the whole is stirred for two hours. It is then left to settle for 1 h and the supernatant solution is removed by means of a pump or a steam ejector or by vacuum siphoning.
  • the volume of the solution removed corresponds to 1.22 V, which shows that not only was the pretreatment solution but also a certain amount of the water absorbed by the resins, this amount represents 14 % of the initial volume of decanted wet resins.
  • This operation is repeated three times to obtain a saturation rate in Ba "of the resins close to 100% due to the concentration of Ba (N0 3 ) 2 in the solution (0.37 mole.l -1 ) and the duration of contact.
  • the saturation pretreatment causes a release of 10 to 15% of the initial activity of the resins. Also, the supernatant radioactive solution is returned to the head of the liquid effluent treatment station, either upstream of an evaporator, or upstream of a chemical coprecipitation chain.
  • the pretreated resins are washed with demineralized water using a volume of washing water equal to 0.65 V, ie identical to that of the pretreated and decanted resins.
  • the pH of the suspension of resins is adjusted to 7.5 ⁇ 0.2 using a baryte milk at 300 gl - 'of Ba (OH) 3 .
  • This washing operation is repeated four times, controlling the concentration of N0 3 - of the washing water after each operation, until an N03 concentration of the washing water is obtained of less than 2 g -1 .
  • the transfer and washing waters are very weakly radioactive and they are sent to the effluent treatment station where their level of radioactivity is checked.
  • the pretreated and washed resins are then resuspended in demineralized water using 0.4 to 0.45 V of water for a proportion of 0.6 to 0.55 V of the resin mixture.
  • the suspension of pretreated organic resins is then sent to the asphalt plant, which is of the quadruple screw drying extruder type.
  • the properties of the asphalt leaving the asphalt plant are then checked.
  • the mixes are immersed in ordinary non-renewed water or non-renewed demineralized water, and the volume increase (in%) of the mixes is periodically measured as a function of the duration immersion (in days).
  • the volume ratio between the water and the mixes is 4.5 and the surface / volume ratio of the mixes is 10.5 cm -1.
  • the swelling of the coated materials after 365 days of immersion in ordinary water is 4.2% by volume, ie 4.45% by weight, and that it is 5, 0% by volume, or 5.1% by weight, after 365 days of immersion in demineralized water.
  • the volume of the solution eliminated corresponds to 1.35 V, which shows that not only the pretreatment solution, but also a certain amount of the water absorbed by the resins has been eliminated, this amount represents 21% of the volume of decanted wet resins.
  • the pretreated resins are washed with demineralized water using a volume of washing water equal to 0.83 V, ie identical to that of the pretreated and decanted resins.
  • the pH of the resin suspension is adjusted to 7.5 ⁇ 0.2 using a baryte milk containing 300 g of Ba (OH) 3 .
  • This washing operation is repeated three times, controlling the concentration of CH 3 CO 2 - of the washing water after each operation until a concentration of CH 3 C02 in the washing water of less than 2 g is obtained. .
  • the operation is continued as in Example 1 and the asphalting operation is carried out under the same conditions using blown bitumen MR 90/40.
  • the properties of the asphalt leaving the asphalt plant are then checked.
  • the swelling of the coated materials after 15 days of immersion in demineralized water or in ordinary water is very significant. Indeed, the swelling is 38.7% by volume, or 25.1% by weight, in the case of demineralized water, and 50.1% by volume, or 45.6% by weight, in the case of ordinary water.

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  • Physics & Mathematics (AREA)
  • Engineering & Computer Science (AREA)
  • General Engineering & Computer Science (AREA)
  • High Energy & Nuclear Physics (AREA)
  • Treatment Of Water By Ion Exchange (AREA)
  • Working-Up Tar And Pitch (AREA)
  • Processing Of Solid Wastes (AREA)
EP85400496A 1984-03-21 1985-03-14 Procédé de bitumage de déchets radioactifs constitués par des résines échangeuses de cations et/ou par des résines échangeuses d'anions Expired - Lifetime EP0157683B1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FR8404390 1984-03-21
FR8404390A FR2561812B1 (fr) 1984-03-21 1984-03-21 Procede de bitumage de dechets radioactifs constitues par des resines echangeuses de cations et/ou par des resines echangeuses d'anions

Publications (2)

Publication Number Publication Date
EP0157683A1 EP0157683A1 (fr) 1985-10-09
EP0157683B1 true EP0157683B1 (fr) 1990-06-20

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EP85400496A Expired - Lifetime EP0157683B1 (fr) 1984-03-21 1985-03-14 Procédé de bitumage de déchets radioactifs constitués par des résines échangeuses de cations et/ou par des résines échangeuses d'anions

Country Status (8)

Country Link
US (1) US4663086A (https=)
EP (1) EP0157683B1 (https=)
JP (1) JPS60213895A (https=)
KR (1) KR940000023B1 (https=)
CA (1) CA1266768A (https=)
DE (1) DE3578358D1 (https=)
FR (1) FR2561812B1 (https=)
ZA (1) ZA851746B (https=)

Families Citing this family (15)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
SE449183B (sv) * 1985-08-30 1987-04-13 Hoglund Lars Olov Sett att framstella ett alster av fast bitumen med inbeddad eller inkapslad korn- och/eller pulverformig jonbytarmassa och anvendning av settet for langtidslagring av radioaktivt avfall
JPS63145997A (ja) * 1986-07-04 1988-06-18 株式会社荏原製作所 放射性廃棄物の固化方法
FR2615315B1 (fr) * 1987-05-15 1989-08-25 Sgn Soc Gen Tech Nouvelle Procede d'immobilisation de resines echangeuses d'ions radioactives, par un liant hydraulique
US5143653A (en) * 1987-05-15 1992-09-01 Societe Anonyme: Societe Generale Pour Les Techniques Nouvelles-Sgn Process for immobilizing radioactive ion exchange resins by a hydraulic binder
NO172967C (no) * 1987-11-06 1993-10-06 Rohm & Haas Fremgangsmaate til innkapsling eller til aa bringe i fast tilstand et produkt som omfatter en stort sett kontinuerligvandig fase og loeste eller suspenderte stoffer
FR2624769B1 (fr) * 1987-12-16 1991-04-19 Sgn Soc Gen Tech Nouvelle Procede d'immobilisation de resines echangeuses d'ions provenant des circuits secondaires des reacteurs nucleaires a eau pressurisee et des reacteurs graphite-gaz
FR2624768B1 (fr) * 1987-12-16 1992-03-13 Sgn Soc Gen Tech Nouvelle Procede d'immobilisation de resines echangeuses d'ions provenant des centres de retraitement des produits radioactifs
IT1264267B1 (it) * 1993-11-12 1996-09-23 Alessio Bianchi Metodo ed impianto per rendere inerti i rifiuti solidi e per il loro successivo stoccaggio definitivo.
US20060037913A1 (en) * 2004-08-20 2006-02-23 Resintech Incorporated Modified anion exchange materials with metal inside the materials, method of making same and method of removing and recovering metals from solutions
DE102009006518A1 (de) * 2009-01-28 2010-09-16 Areva Np Gmbh Verfahren und Vorrichtung zur Behandlung eines Ionenaustauscherharzes
US20100247415A1 (en) * 2009-03-26 2010-09-30 Michael C Gottlieb Method of Removing and Recovering Silica Using Modified Ion Exchange Materials
JP2011069753A (ja) * 2009-09-28 2011-04-07 Hitachi-Ge Nuclear Energy Ltd 使用済樹脂の固型化処理システム及び固型化処理方法
FR2957710B1 (fr) 2010-03-19 2012-05-11 Onectra Procede de conditionnement de dechets radioactifs, notamment de resines echangeuses d'ions
ES2602481T3 (es) 2010-07-01 2017-02-21 Janssen Pharmaceutica, N.V. Combinaciones antimicrobianas de compuestos de piriona con polietileniminas
EP2819125B1 (en) * 2013-06-21 2018-08-08 Hitachi-GE Nuclear Energy, Ltd. Radioactive organic waste treatment method and system

Family Cites Families (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB1188396A (en) * 1967-12-11 1970-04-15 Belge Pour L Ind Nucleaire S A Treatment of Radioactive Liquids
US4204974A (en) * 1975-07-15 1980-05-27 Kraftwerk Union Aktiengesellschaft Method for removing radioactive plastic wastes and apparatus therefor
DE2628286C2 (de) * 1976-06-24 1986-04-10 Kernforschungszentrum Karlsruhe Gmbh, 7500 Karlsruhe Verfahren zur Verbesserung der Auslaugbeständigkeit von Bitumenverfestigungsprodukten radioaktiver Stoffe
FR2361724A1 (fr) * 1976-08-12 1978-03-10 Commissariat Energie Atomique Procede de stockage de resines echangeuses d'ions contaminees
JPS5614195A (en) * 1979-07-17 1981-02-10 Japan Gasoline Method of improving waterrresistance of radioactive waste asphalttsolidified body
SE420249B (sv) * 1980-01-31 1981-09-21 Asea Atom Ab Sett for behandling av en i en reningskrets i en kernreaktoranleggning anvend organisk jonbytarmassa
IT1195040B (it) * 1981-05-11 1988-09-28 Snial Resine Poliestere Spa Ca Composizioni di materia contenenti materiale radioattivo a base di resine scambiatrici di ioni
US4530723A (en) * 1983-03-07 1985-07-23 Westinghouse Electric Corp. Encapsulation of ion exchange resins
SE8304278L (sv) * 1983-08-04 1985-02-05 Studsvik Energiteknik Ab Forfarande for behandling av anvend, radioaktiv, organisk jonbytarmassa

Also Published As

Publication number Publication date
CA1266768A (en) 1990-03-20
KR850006886A (ko) 1985-10-21
FR2561812B1 (fr) 1989-02-17
FR2561812A1 (fr) 1985-09-27
EP0157683A1 (fr) 1985-10-09
ZA851746B (en) 1985-11-27
US4663086A (en) 1987-05-05
JPS60213895A (ja) 1985-10-26
JPH0360399B2 (https=) 1991-09-13
KR940000023B1 (ko) 1994-01-05
DE3578358D1 (de) 1990-07-26

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