WO1980000047A1 - Encapsulating wastes - Google Patents

Encapsulating wastes Download PDF

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Publication number
WO1980000047A1
WO1980000047A1 PCT/GB1979/000099 GB7900099W WO8000047A1 WO 1980000047 A1 WO1980000047 A1 WO 1980000047A1 GB 7900099 W GB7900099 W GB 7900099W WO 8000047 A1 WO8000047 A1 WO 8000047A1
Authority
WO
WIPO (PCT)
Prior art keywords
waste
process according
mixture
initiator
water
Prior art date
Application number
PCT/GB1979/000099
Other languages
English (en)
French (fr)
Inventor
P Williams
Original Assignee
Bp Chem Int Ltd
P Williams
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Bp Chem Int Ltd, P Williams filed Critical Bp Chem Int Ltd
Publication of WO1980000047A1 publication Critical patent/WO1980000047A1/en

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Classifications

    • 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
    • G21F9/162—Processing by fixation in stable solid media in an inorganic matrix, e.g. clays, zeolites
    • G21F9/165—Cement or cement-like matrix
    • 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
    • G21F9/167—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
    • G21F9/28—Treating solids
    • G21F9/30—Processing
    • G21F9/301—Processing by fixation in stable solid media
    • G21F9/302—Processing by fixation in stable solid media in an inorganic matrix
    • G21F9/304—Cement or cement-like matrix
    • 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

Definitions

  • the present invention relates to a process for encapsulating hazardous wastes. It is known to encapsulate various hazardous wastes by incorporating the waste into a fluid material which is then allowed to set to a solid so as to bind the waste. This enables the waste to be handled more easily and prevents hazardous components of the waste escaping to the environment. Thus it is known from British patent specification 1 116 319 to incorporate radio active wastes in bitumen, cement or a polymerisable resin. If bitumen is used the waste must be subjected to the elevated temperatures used to melt the bitumen. This is not always desirable and the requirement for a heating step leads to additional complications.
  • bitumen is not very suitable for wet wastes because the elevated temperature will lead to the evolution of steam which may carry with it hazardous components of the waste and because bitumen is hydrophobia.
  • cement as an encapsulating agent is not very satisfactory as the time required for the cement to set is usually undesirably long.
  • British patent specification 938 211 discloses a process for solidifying or encapsulating an aqueous radio active waste by mixing the waste with a finely divided hydraulically setting absorption material e.g. Portland Cement.
  • a self-hardening synthetic or casting resin e.g. "Palatal P6" sold by BASF.
  • Palatal P6 a self-hardening synthetic or casting resin
  • This is a mixture of unsaturated polyester and styrene and as is well known in the polyester art such resins are cured by the action of conventional organic peroxide curing agents.
  • the process is an impregnation process and is clearly only applicable to a block which has set and is free from water as otherwise the resin will not penetrate the block. Pressure is required for the impregnation process and it will be difficult to obtain satisfactory penetration of the resin into the core of the block.
  • the speed of the encapsulation process is dependent on the setting time of the hydraulic filler. The specification mentions setting times of 2 days. The process is thus not a very satisfactory method of encapsulating wastes.
  • British patent specification 1 353 121 discloses the encapsulation of a radio active waste in the form of a dry powder using a mixture of (1) an unsaturated polyester prepared from raaleic and phthalic anhydride reacted with propylene glycol and (2) a copolymerisable monomer e.g. styrene. Polymerisation is initiated by an initiator such as methyl ethyl ketone peroxide.
  • a WEP type polyester resin formulation which is suitable for use in small scale tests may be completely unsatisfactory when attempts are made to cast large blocks.
  • a formulation which is suitable for use with a waste with a given water content may be unsatisfactory when used with a waste with a different water content.
  • the process for encapsulating a hazardous waste by allowing to set an encapsulation mixture containing an unsaturated polyester an ethylenically unsaturated monomer copolymerisable with said polyester, and an initiator, which mixture incorporates the hazardous waste, is characterised in that the mixture contains a hydraulic filler, the initiator is an initiator which is activated by aqueous alkaline conditions and setting takes place under aqueous alkaline conditions.
  • the process of the present invention may be applied to a variety of wastes providing that they do not interfere with setting reaction to any substantial extent.
  • the process may be applied to wastes containing toxic heavy metals or mercury, or organochlorine compounds. It is particularly useful for the encapsulation of radioactive wastes
  • the wastes may be pieces of contaminated equipment or clothing, but the process is particularly suitable for the encapsulation of particulate wastes.
  • the wastes may be dry in which case water must be added to the mixture to cause it to set.
  • the process is particularly suitable for the treatment of wet particulate radio active wastes which are usually difficult to handle by alternative methods.
  • the quantity of water present in the waste may, for example, be in the range 20% to 60% by weight of waste, preferably below 50% by weight.
  • the process of the present invention is particularly suitable for the encapsulation of wet ion-exchange resins both anionic and cationic.
  • Other wet solid wastes to which the process of the invention may be applied are molecular sieves, graphite, sand and aluminosilicates, Magnox sludges (sludges containing magnesium hydroxide mixed with magnesium carbonate) filtration sludges.
  • the process of the present invention may also be used to encapsulate wastes in the form of aqueous solutions. It will be necessary to use sufficient hydraulic filler to bind all the water on setting.
  • Unsaturated polyesters and ethylenically unsaturated monomers copolymerisable with the polyesters are well known to those skilled in the art. A description of suitable polyesters is found in British patent 1 065053 (Cement Marketing Company), the disclosure of which is incorporated by reference.
  • a mixture which. gels in 30 to 90 minutes for example one which gels in less than1 hour
  • Mixtures gelling in therang to 30 minutes can be used however and a standard polyestermade from a mixture of an ether glycol and a non-ether glycol e.g. from diethylene glycol and ethylene glycol, may be used together with a metal accelerator e.g. copper naphthenate, a reducing agent e.g sodium metabisulphite and a soap emulsifier.
  • a metal accelerator e.g. copper naphthenate
  • a reducing agent e.g sodium metabisulphite
  • soap emulsifier e.g. an unsaturated polyester may be used which is inherently more reactive e.g. an unsaturated polyester produced from one or more glycols which are substantially all ether glycol in which case metal accelerators and reducing agents are not required.
  • the hydraulic filler may be any substance which on mixing with water at ambient temperature reacts to form a crystalline lattice structure exhibiting a degree of mechanical stability and/or physical strength.
  • Examples of hydraulic fillers are gypsum, calcium sulphate hemihydrate (plaster of Paris), and pulverised fuel ash.
  • the alkaline conditions required to activate the initiator may be provided by the addition of a substance which is not a hydraulic filler. However in a preferred embodiment of the invention, the substance which produces the alkaline conditions also acts as a hydraulic filler, and it is preferred to use an alkaline reacting hydraulic cement.
  • hydraulic cements are high alumina cements, blast furnace cements, lime-pozzolana cement. It is preferred however to use mixtures containing Portland cement.
  • the Portland cement may be substantially the only hydraulic filler present in the mixture. Alternatively it may be desirable to use mixtures of Portland cement with other fillers e.g. pulverised fuel ash.
  • the Portland cement content in such mixtures may be from 6 to 95% by. weight of total hydraulic filler, but is more preferably greater than 10% by weight, in particularly greater than 20% by weight.
  • the initiator used in the process of the present invention is one which is activated by aqueous alkaline conditions, which distinguishes it from the organic peroxides usually used in polyester moulding compositions. It is preferred to use a water soluble salt of a per acid, in particular salts of persulphuric acidi e.g. ammonium, sodium and potassium persulphate. It is particularly preferred to use ammonium persulphate.
  • the quantity of initiator used will depend on the speed of gelling required. Examples of suitable amounts are those in the range 1% to 5% by weight of the encapsulation mixture.
  • the quantity of waste incorporated in the encapsulation mixture may vary over a wide range. For economic reasons it is desirable to incorporate a large quantity of waste into the mixture.
  • the quantity of waste may be 30% to 60% of the total weight of encapsulation mixture and waste and is preferably more than 40% by weight of the total. It is preferred to use sufficient quantity of encapsulation mixture to prevent the appearance of excess water on the surface of the set product, when treating a wet waste.
  • the relative proportions of unsaturated polyester, ethylenically unsaturated monomer and hydraulic filler may vary over a wide range.
  • suitable compositions may contain 50 to 70 parts of polyester resin, 25 to 65 parts of unsaturated monomer and 80 to 150 parts of hydraulic filler and 3 to 5 parts of initiator.
  • the waste does not contain water it will be necessary to add it so as to cause the encapsulation mixture to set. Even if some water is present in the waste it may be desirable to add additional water.
  • the quantity of water initially present may for example be at least 50% by weight of the hydraulic filler.
  • the dry encapsulation mixture is prepared in advance of the encapsulation step it may be desirable to add fumaric acid to stabilise it. It may be desirable to add non-ionic surfactants.
  • the addition of fatty acids to control pot life i.e. the time for which the mixture remains fluid after water is added) and give ease of dispersion of the encapsulation mixture after prolonged storage may be useful.
  • the quantities of waste, hydraulic filler unsaturated polyester and copolymerisable monomer are preferably such as give a product which has a specific gravity of at least 1.2. This is important if the encapsulated material is to be disposed of by dumping in the ocean.
  • the encapsulation mixtures of the present invention may be prepared by simple low speed mixing apparatus without the necessity * (see GB 1098132, GB 1091325, GB 1092, 747). of using expensive high shear mixers such as are used in the production of WEPs (water extended polyesters). If the waste is particulate it may be introduced into the mixing apparatus with the other ingredients. The mixture is then discharged into a mould in which it is allowed to set. For non-particulate waste e.g. pieces of machinery, encapsulation mixture may be fed to the mould, the waste added and the mould may then be filled with additional encapsulation mixture.
  • the mixture may be removed from the mould.
  • the resulting moulded block may then be if required be inserted into a protective container and disposed of by dumping.
  • the mould in which the block is formed may act also as a container.
  • Polyester resin A 60 parts by weight was mixed at ambient temperature with a hydraulic cement (40 parts by weight) (sold under the name Hydracrete) ammonium persulphate (2 parts by weight), sodium metabisulphate (0.5 parts by weight), copper naphthenate (equivalent to 5 ppm copper) and liquid soap (1.0 parts by weight).
  • Ion exchange resin 50 parts by weight containing about 47% by weight of water was then mixed in and the mixture was allowed to set in a mould. The mixture gelled in 11 minutes and had set sufficiently to allow the block of encapsulated ion exchange resin to be removed from the mould in 2 to 3 hours.
  • Example 2 A composition was made by mixing together at ambient temperature polyester resin C, Portland cement and ammonium persulphate in the proportions shown in Table 1.
  • Waste in the form of wet ion exchange resin (75 grams) containing
  • Example 2 This was carried out in a similar way to Example 2 but using polyester resin B in place of polyester resin C.
  • the quantities used are shown in Table 2 and the same quantity (75 grams) of the wet ion exchange resin was added as in Example 2.
  • Example 5 This was carried out as in Example 4 but using potassium persulphate. The quantities used are given in Table 2.
  • the ingredients set out in Table 3 were mixed together at an ambient temperature of 20°C and allowed to set in a mould.
  • the pot life of the mixtures i.e. the time required for gelling to take place was measured and is given in Table 3. All the mixtures were readily demoulded in 1-2 hours and exhibited no separated water.
  • the white cement, high early strength cement, and oil well cement are all different types of cement well known to those skilled in the cement art.
  • Example 10 This was carried out as in Example 6 but using PFA (pulverised fuel ash). The mixture did not gel for 1-2 days and could only be demoulded after 3 days. Examples 10 to 17
  • compositions set out in Table 4 were prepared in the same way as in the previous examples at an ambient temperature of 20°C.
  • Example 22 The mixture of Example 20 was demoulded in 6-8 hours and showed a slight surface wetness.
  • Example 22
  • the mixed waste was a mixture of ion-exchange resins.
  • Lewatit Bead 5.5 parts by volume
  • Binder for encapsulation mixture as ' for Example 24 replacing the crushed Lewatit by 9 parts by weight of water.
  • Cast specimens were submitted to varying dosages of gamma radiation and tested before and after exposure. Table 9 shows the results.
  • Specimens were prepared using the formulation of Example 24 using radio active waste ion exchange resin contaminated with Caesium 137 isotope. These specimens were prepared and tested in accordance with "Leach Testing of I ⁇ imobilised Radio active Waste Solids", A Proposal for a Standard Method, E. D. Hespe Atomic Energy Review Vol. 9 page 195 (1971).
  • Peak exotherm measurements were made using thermocouples positioned at the centre points of the castings.
  • IRN-78 anionic polystyrene based ion exchange resin AW - 500 cationic modified alumino silicate zeolite molecular sieve.
  • Example 1 The mixed waste resin used in Examples 1 to 22 inclusive was that described in Example 6.
  • the water content in Examples 1 to 21 was 47% but in Example 22 was 42%.
  • Examples 27 to 31 and Comparative Test G are the mixed waste resin used in Examples 1 to 22 inclusive.
  • compositions were hand mixed and were readily pourable prior to gelation.
  • Compositions of Examples 27 to 30 could be demoulded between 1 and 4 hours after mixing showing no signs of separated water and on demoulding they were homogeneous and free from cracks and voids other than minor air inclusions.
  • the composition of Comparative Test G did not set within 24 hours.
  • the composition of Example 31 was demouldable within 24 hours. * Composition as given in Example 22.
  • compositions mixed by hand were readily pourable prior to gelation.
  • the compositions of Examples 32 to 34 were demouldable within 1 to 4 hours after mixing showing no signs of separated water, and on demoulding were homogeneous and free from cracks and voids other than minor air inclusions.
  • the composition of Comparative Test H did not set within 24 hours.
  • the mixtures according to the present invention were pourable and easily handled before setting and were prepared using low shear paddle mixers in contrast to the high shear mixers used to make water extended polyester mixtures. It should be noted that the water-in- polyester emulsions used in making water extended polyesters are often very thick and difficult to pour.
  • the mixtures of the present invention when set were uniform, free from major cracks and voids other than small air inclusions. They were mechanically strong and could be transported without crumbling or breaking. * Composition as given in Example 22.

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  • Physics & Mathematics (AREA)
  • Engineering & Computer Science (AREA)
  • General Engineering & Computer Science (AREA)
  • High Energy & Nuclear Physics (AREA)
  • Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Processing Of Solid Wastes (AREA)
  • Manufacturing Of Micro-Capsules (AREA)
  • Manufacture Of Porous Articles, And Recovery And Treatment Of Waste Products (AREA)
PCT/GB1979/000099 1978-06-08 1979-06-07 Encapsulating wastes WO1980000047A1 (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
GB7826549 1978-06-08
GB7826549 1978-06-08

Publications (1)

Publication Number Publication Date
WO1980000047A1 true WO1980000047A1 (en) 1980-01-10

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Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/GB1979/000099 WO1980000047A1 (en) 1978-06-08 1979-06-07 Encapsulating wastes

Country Status (4)

Country Link
EP (1) EP0006329A1 (enrdf_load_stackoverflow)
JP (1) JPS55500406A (enrdf_load_stackoverflow)
ES (1) ES481367A1 (enrdf_load_stackoverflow)
WO (1) WO1980000047A1 (enrdf_load_stackoverflow)

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2545258A1 (fr) * 1983-04-29 1984-11-02 Barrow Investments Enrobage de dechets radioactifs
FR2550969A1 (fr) * 1983-08-23 1985-03-01 Barrow Investments Procede pour le transport et/ou le stockage de dechets
US4828761A (en) * 1988-05-04 1989-05-09 The United States Of America As Represented By The United States Department Of Energy Process for impregnating a concrete or cement body with a polymeric material
US4943394A (en) * 1988-01-30 1990-07-24 Kernforschungsanlage Julich Gesellschaft Mit Beschrankter Haftung Method of storing radioactive waste without risk of hydrogen escape
US5481064A (en) * 1992-05-08 1996-01-02 Sanko Motor Chemical Co., Ltd. Waste fluid treatment process

Families Citing this family (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
FR2607957A1 (fr) * 1986-12-05 1988-06-10 Commissariat Energie Atomique Bloc contenant des dechets en vue de leur stockage et procede de realisation d'un tel bloc
US5900258A (en) * 1996-02-01 1999-05-04 Zeolitics Inc. Anti-bacterial compositions
FR2773504B1 (fr) * 1998-01-12 2000-03-31 Bouygues Sa Procede pour conditionner des particules de resines echangeuses d'ions et application au traitement d'une eau radioactive
GB0130593D0 (en) 2001-12-21 2002-02-06 British Nuclear Fuels Plc Treatment of waste products

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR1246848A (fr) * 1959-10-13 1960-11-25 Commissariat Energie Atomique Procédé d'élimination de déchets radioactifs et produits obtenus suivant ce procédé
DE2356253A1 (de) * 1973-11-10 1975-05-22 Kernforschung Gmbh Ges Fuer Verfahren zum vorbereiten von organischen, radioaktive stoffe enthaltenden abfallfluessigkeiten zur umweltfreundlichen und sicheren handhabung, transportierung und endlagerung
FR2273350A2 (en) * 1974-05-27 1975-12-26 Commissariat Energie Atomique Radioactive waste storage using ion exchange resin - or filtration or flocculation adjuvants
DE2549195A1 (de) * 1974-11-05 1976-05-06 Asea Atom Ab Verfahren, um verbrauchte, kornfoermige, organische ionenaustauschmasse in zement einzubetten
US4077901A (en) * 1975-10-03 1978-03-07 Arnold John L Encapsulation of nuclear wastes
FR2361724A1 (fr) * 1976-08-12 1978-03-10 Commissariat Energie Atomique Procede de stockage de resines echangeuses d'ions contaminees
FR2366234A1 (fr) * 1976-04-27 1978-04-28 Crouzet Pierre Procede de fabrication d'un produit a base d'une emulsion et d'un agent de prise, et produit obtenu par application de ce procede

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR1246848A (fr) * 1959-10-13 1960-11-25 Commissariat Energie Atomique Procédé d'élimination de déchets radioactifs et produits obtenus suivant ce procédé
DE2356253A1 (de) * 1973-11-10 1975-05-22 Kernforschung Gmbh Ges Fuer Verfahren zum vorbereiten von organischen, radioaktive stoffe enthaltenden abfallfluessigkeiten zur umweltfreundlichen und sicheren handhabung, transportierung und endlagerung
FR2273350A2 (en) * 1974-05-27 1975-12-26 Commissariat Energie Atomique Radioactive waste storage using ion exchange resin - or filtration or flocculation adjuvants
DE2549195A1 (de) * 1974-11-05 1976-05-06 Asea Atom Ab Verfahren, um verbrauchte, kornfoermige, organische ionenaustauschmasse in zement einzubetten
US4077901A (en) * 1975-10-03 1978-03-07 Arnold John L Encapsulation of nuclear wastes
FR2366234A1 (fr) * 1976-04-27 1978-04-28 Crouzet Pierre Procede de fabrication d'un produit a base d'une emulsion et d'un agent de prise, et produit obtenu par application de ce procede
FR2361724A1 (fr) * 1976-08-12 1978-03-10 Commissariat Energie Atomique Procede de stockage de resines echangeuses d'ions contaminees

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2545258A1 (fr) * 1983-04-29 1984-11-02 Barrow Investments Enrobage de dechets radioactifs
GB2140194A (en) * 1983-04-29 1984-11-21 Barrow Investments A method of packaging radioactive waste
EP0124825A3 (fr) * 1983-04-29 1986-03-26 W.R. Grace & Co. Enrobage de déchets radioactifs
FR2550969A1 (fr) * 1983-08-23 1985-03-01 Barrow Investments Procede pour le transport et/ou le stockage de dechets
EP0136496A3 (fr) * 1983-08-23 1986-03-19 W.R. Grace & Co. Procédé pour le tranport et/ou le stockage de déchets
US4943394A (en) * 1988-01-30 1990-07-24 Kernforschungsanlage Julich Gesellschaft Mit Beschrankter Haftung Method of storing radioactive waste without risk of hydrogen escape
US4828761A (en) * 1988-05-04 1989-05-09 The United States Of America As Represented By The United States Department Of Energy Process for impregnating a concrete or cement body with a polymeric material
US5481064A (en) * 1992-05-08 1996-01-02 Sanko Motor Chemical Co., Ltd. Waste fluid treatment process

Also Published As

Publication number Publication date
ES481367A1 (es) 1980-02-01
JPS55500406A (enrdf_load_stackoverflow) 1980-07-10
EP0006329A1 (en) 1980-01-09

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