GB1564878A - Method of improving the leaching resistance of solidified bitumen products containing radioactive substances - Google Patents
Method of improving the leaching resistance of solidified bitumen products containing radioactive substances Download PDFInfo
- Publication number
- GB1564878A GB1564878A GB2497877A GB2497877A GB1564878A GB 1564878 A GB1564878 A GB 1564878A GB 2497877 A GB2497877 A GB 2497877A GB 2497877 A GB2497877 A GB 2497877A GB 1564878 A GB1564878 A GB 1564878A
- Authority
- GB
- United Kingdom
- Prior art keywords
- bitumen
- sludges
- solidified
- solutions
- water
- 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
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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
- G21F9/28—Treating solids
- G21F9/34—Disposal of solid waste
- G21F9/36—Disposal of solid waste by packaging; by baling
-
- 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
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- Engineering & Computer Science (AREA)
- Physics & Mathematics (AREA)
- General Engineering & Computer Science (AREA)
- High Energy & Nuclear Physics (AREA)
- Environmental & Geological Engineering (AREA)
- Processing Of Solid Wastes (AREA)
Description
(54) A METHOD OF IMPROVING THE LEACHING
RESISTANCE OF SOLIDIFIED BITUMEN PRODUCTS
CONTAINING RADIOACTIVE SUBSTANCES
(71) We, KERNFORSCHUNGSZENTRUM KARLSRUHE GESELLSCHAFT MIT BESCHRAENKTER HAFTUNG, formerly Gesellschaft Fuer Kernforschung mbH., of 5 Weberstrasse, 75 Karlsruhe 1, Germany (Fed.
Rep.); a German body corporate, do hereby declare the invention, for which we pray that a patent may be granted to us, and the method by which it is to be performed, to be particularly described in and by the following statement:- The present invention relates to a method of improving the leaching resistance of solidified or compacted bitumen products wherein aqueous solutions and/or sludges of radioactive substances are charged into the liquid bitumen, and which solutions and/or sludges contain materials which cause an increase in the leaching rate of the solidified or compacted bitumen products.
The processing of radioactive liquids and/or sludges originating from reprocessing plants and nuclear research centres, and of the medium active to low active category (medium active: 10-to 103 C/m3, low active: maximum allowable concentration up to 10-' C/m3), with bitumen, or the solidifying or compacting of radioactive substances in a bitumen matrix has already been practised for years ["Bituminization of radioactive wastes" (Review of the present state of the development and industrial application).International Atomic Energy Agency
Vienna 1970; Technical Reports Series No. I 16i. Bitumen as a solidifying or compacting matrix, for example, for radioactive salts, especially from aqueous evaporator concentrates, is used with preference because, normally, the leaching rates of the solidification or compaction products deposited in distilled water, even over long periods for example, a year or longer, are relatively low, generally in the region of 10-4[g/cm2.day] to 10X5[g/cm2.day]; moreover, the volume reduction (volume of liquid or sludge reduced to the volume of the solidified block obtained therefrom) is relatively favourable.In the normal case, this meant that by far the greater proportion of the waste waters mixed with the liquid bitumen resulted in solidified products which had good leaching properties, i.e. low leaching rates.
It has now been found, however, that whilst the diffusion of waste water, the salt content of which comprises to a great proportion sodium carbonate or sodium sulphate, into bitumen may be carried out in a favourable manner i.e. the solidifying procedure posing no problems, the storage of such solidified products, for example in distilled water, shows abnormal leaching properties of such bitumen-salt products.
Waste water concentrates from water-cooled reactors contain sodium sulphate. Leaching investigations of solidified blocks of diverse bitumen-Na2SO4- mixtures having 50 percent by weight, 39 percent by weight and 30 percent by weight Na2SO4 in distilled water, have shown that, even at the beginning of the leaching period, a leaching behaviour of the products deviating from the normal behaviour is noticed. The results of the investigations showed that the leaching rates of bitumen-Na2SO4 blocks over a seven-day test period, were dependent upon the leaching time (t) as follows:
Product with 50 percent by weight Na2SO4: leaching approximately
proportional t' 5: Product with 39 percent by weight Na2SO4: leaching approximately
proportional t'-7:
Product with 30 percent by weight Na2SO4: leaching approximately
proportional t'-9.
The average leaching rates for the products were, with
50 percent by weight Na2SO4=8.2x l0-2lg. cm 2 d-'i 39 percent by weight Na2SO4=3.0x 21g . cm-2 .d-'l 30 percent by weight Na2SO4=3. lx 10-31g. cm -2 d-11 Optically, it was noted that in these products the surfaces thereof, smooth from the water storage of the blocks, swelled and, at the end of the leaching period, even had coniform protuberances or raised portions thereon. A similar behaviour was ascertained in solidified blocks of bitumen-Na2CO3 mixture (e.g. having 38.5 percent by weight Na2CO3).
It is an object of the present invention to provide a method which ensures that during the solidification of radioactive liquids and/or sludges with such Na2CO3 and/or Na2SO4 contents, which cause an increase in the leaching rate of the solidified products, products of high leach-resistance are produced, and that without great technical expenditure and with a minimum of radiation problems, such methods can be safely carried out at lowest possible costs.
According to the present invention there is provided a method of improving the leach-resistance of solidified bitumen products wherein aqueous solutions and/or sludges of radioactive substances are charged into liquid bitumen, which solutions and/or sludges contain materials which cause an increase in the leaching rate of the solidified products, in which
a) prior to charging the solutions and/or sludges into the liquid bitumen, such solutions and/or sludges are treated with substances which are able to convert salts contained in the solutions and/or sludges having a considerable tendency to absorb water of crystallisation molecules into their crystal lattice during storage in water of the solidified end products, at least partly into salts having a less or reduced tendency to absorb water of crystallisation molecules into their crystal lattice;;
b) mixing the pre-treated solutions and/or sludges with the liquid bitumen with evaporation of water in a known manner, whereby the water content of the bitumen and solids mixture produced is brought to 110/, by weight; and
c) allowing the bitumen and solids mixture to flow into water-impermeable corrosion-resistant, resilient, bitumenophilic linings for the casks or containers to be used for the end storage of radioactive wastes.
Preferably alkaline earth compounds are used as substances for the pretreatment of the solutions and/or sludges, which bring the pH of the solutions and/or sludges to a value of from 7 to 11.
A further development of the method in accordance with the invention is characterised by the feature that the substances utilised to treat the solutions and/or sludges are used in such an amount that only from 50, " to 95 ,, of the salts with considerable tendency to absorb water of crystallisation are converted into salts having a lesser or reduced tendency to absorb water of crystallisation.
The alkaline earth compounds which may be used to treat the aqueous solutions and/or sludges are not limited to such which possess no or only a little tendency to absorb water of crystallisation. They have to be used only to bring the pH of the solutions and/or sludges to a value of from 7 to 11, especially from 8 to 10.
An excess of alkaline earth compounds is to be avoided, because, on the one hand, the production of compounds having a considerable tendency towards rendering possible the absorption of water of crystallisation in the solidified block would result, whilst on the other hand combining therewith an unnecessary increase of the inactive salt load in the solidified block. Also the volume reduction factor would then be reduced.
Experiments have shown that it suffices for more than half the salts with considerable tendency to absorb water of crystallisation to be converted into salts with a lesser or reduced tendency with the aid of alkaline earth compounds, e.g.
calcium chloride, to obtain solidified products, the leaching property of which are to be considered good or substantially good.
Particularly suitable alkaline earth compounds are salts of barium, strontium, and calcium.
The solutions and/or sludges which contain carbonates, sulphates and phosphates of alkali metals are the most radioactive. They are most favourably converted with CaC12 or BaCl2 into their corresponding Ca or Ba salts. In contrast to untreated evaporation concentrates containing, for example, Na2SO4, which to avoid crystallisation have to be stored and dosed at increased temperatures (e.g.
400C), the pre-treated evaporation concentrates which contain only finely dispersed precipitates, may be dosed at room temperature. Bv using the method in accordance with the invention, particularlv for untreated evaporation concentrates which contain the said substances, additional heating devices for containers and pipe lines are superfluous. Blockages in pipe lines, difficult to remove, caused bv the crystallization of large crystals when such heating fails, need no longer be feared.
A favourable further development of the invention is characterised by the feature that as water-impermeable, corrosion-resistant, resilient bitumenophilic lining, a carrier material is used which is steeped or coated with the same bitumen or a bitumen similar to the kind of bitumen used for the bitumen-solids mixture.
The steeped or coated carrier material maybe made of glass fibres, asbestos fibres.
paper or cardboard. The steeped or coated paper or the suitably treated cardboard
may be reinforced with glass fibres or asbestos fibres. Furthermore, for a safe storage, it is advantageous if the bitumen paper or bitumen cardboard used as lining is treated with an anti-inflammatory agent. Bitumenophilic means that after solidification of the bitumen-solids mixture the latter is in intimate contact with the
lining i.e. has entered an adhesive physical bond which neither due to mechanical
action or to alternating temperature influences, will split open on storage in water
or salt solutions or become so loose that water can enter between the lining and the
solidified waste.
Though diverse proposals have become known in the literature in which the
bitumen lining was placed around the solidified radioactive waste, e.g. by steeping the solidified block in liquid bitumen, these proposals all have disadvantages which
are described hereinafter.
To solidify radioactive wastes originating from nuclear fuels irradiated in
reprocessing plants, some average active wastes and highly active wastes such as
e.g. water soluble fluorides, water soluble sulphates or mixtures of these
substances, U.S. Patent Specification No. 3557013 proposes stirring sufficient lime
into the said substances so that the free sulphuric acid is neutralised and the free
fluorides are precipitated, the water being evaporated until a settable paste is
obtained which solidifies when cooling, and finally the solid composition so formed
being either surrounded with a thin layer of insoluble material such as bitumen or
charged into a container of metal or concrete lined with bitumen and the open
space filled with molten bitumen, or if the radiation-resistance of the coating
material is insufficient for the level of radiation emitted from the solid composition,
being charged into a sealed container formed of anti-corrosion alloy. This coating
or this container serves as barrier against leaching of radioactive components of the
solid composition. The quantity of lime which is used must at least be equal to the
quantity which is required to neutralise the H2SO4 and/or to precipitate the
fluoride.
Steel casks, even if they were varnished, have not proved with years of storage
resistant enough against external and/or internal corrosion, especially when the
dry, solidified composition contained from 10 to 20 percent by weight water.
Absolutely corrosion-resistant containers would considerably increase the costs of
waste disposal and the method of operation of pouring liquid bitumen into the
space between the solid waste composition and container is cumbersome, space
and time consuming and moreover, increases the radiation hazard to the operators.
The disadvantages of the last-mentioned method of operation also apply undiminished even when solidified products of mixtures of bitumen and salt having a high salt content ( > 40 percent by weight salts) are enclosed with a layer of 5 mm thickness of pure bitumen [W. Baehr, W. Hild. W. Kluger: Berichte der Gesellschaft fuer Kernforschung m.b.H. Karlsruhe, No. KFK-2l 19 (October, 1974) page 121.
In contrast to the method of coating solidified products with bitumen or the like before being charged into a transport container, the method in accordance with the invention is at least just as safe for the operators, even with respect to radiation hazards, as the charging of "normal" mixtures of waste solutions or sludges and liquid bitumen into conventional casks or containers, because the prefabricated linings, before allowing the mixture of bitumen and solids to flow into the casks or containers, may be located therein. The linings prevent the leaching of radioactive components from the solidified products even after a long period of storage, even if the cask or container is destroyed from the outside by corrosion.
Internal corrosion can no longer occur. The danger of a solidified block of bitumen burning during an accidental fire is considerably reduced.
The following experiments are given to illustrate leaching values.
Experiment I
Comparison of solidification of a sodium sulphate solution after pretreatment.
as provided by the method in accordance with the invention (a) and solidification of a sodium sulphate solution without pretreatment (b).
a) A 20 percent by weight Na2SO4 solution was brought with solid Ca(OH)2 to pH 10 and mixed with a quantity of solid CaC12 (sicc.), which corresponds to 50 " of the stoichiometrically required quantity for converting the existing Na2SO4 into CaSO4. The solution pre-treated in this manner was stirred. under conventional working temperatures (up to 1800C), in a laboratory extruder into bitumen of the commercial kind 'Ebano 15'. The solidified product has the composition
52 percent by weight Ebano 15
17.3 percent by weight Na2SO4
16.6 percent by weight CaSO4 14.1 percent by weight NaCI and after 7 days storage in distilled water had an appearance as shown in Figure 1.
After 66 days of storage in distilled water, an average leaching rate of RL=l .7X l0-4t(cm2/g)-1xd-1] was measured (SOg-ions as indicator).
b) In comparison, a 20 percent by weight Na2SO4 solution without pretreatment was stirred under the same conditions in the laboratory extruder into the same type of bitumen, so that the end composition of the solidified product contained more bitumen; viz:
61 percent by weight Ebano 15
39 percent by weight Na2SO4
After 7 days storage in distilled water the sample had the appearance as shown in figure 2. After this time period, short for water storage, an average leaching rate of R,-3 .Ox 10-2[(cm2/g)-l xd-1] was measured.
leached fraction (e.g. SO4") (RL= surface of the sample/weight of samplexleaching period
This solidified sample after 7 days water storage was swelled, had conical protuberances, and also was porous.
Experiment 2
Solidification of a sodium sulphate solution after pre-treatment. A 20 percent by weight Na2SO4 solution was brought with solid Ca(OH)2 to a pH 10 and mixed with a quantity of solid CaCl2 (sicc.) which corresponds to 90% of the stoichiometric quantity required for converting the existing Na2SO4 into CaSO4.
The pre-treated solution, as described in Experiment 1, was charged into bitumen and the solidified sample created thereby stored for 10 days in distilled water.
Then, as shown in Figure 3, the sample had a completely unchanged appearance.
Experiment 3
Pouring of the mixture of liquid bitumen and solids into a lining of bituminised cardboard.
A liquid bitumen-Na2SO4 mixture (40qd by weight Na2SO4), arriving from the laboratory extruder was poured into a cylindrical lining made of a cardboard of approximately 0.6 mm thickness steeped in bitumen B 15 and provided with a cover of the same cardboard and steeped in the same bitumen. This lining with the solidified product was then stored for 18 days in distilled water. Within this period no components were leached out.
Claims (9)
1. A method of improving the leach-resistance of solidified bitumen products wherein aqueous solutions and/or sludges of radioactive substances are charged into liquid bitumen, which solutions and/or sludges contain materials which cause an increase in the leaching rate of the solidified products. in which
a) prior to charging solution and/or sludges into the liquid bitumen. such solutions and/or sludges are treated with substances which are able to convert halts contained in the solutions and/or sludges having a considerable tendency t( absorb water of crystallisation molecules into their crystal lattice during storage in water of the solidified end products, at least partly into salts having a less or reduced tendency to absorb water of crystallisation molecules into their crvstal lattice::
b) mixing the pre-treated solutions and/or sludges with the liquid bitumen with evaporation of water in a known manner, whereby the water content of the bitumen and solids mixture produced is brought to s1 " by weight; and
c) allowing the bitumen and solids mixture to flow into water-impermeable corrosion-resistant, resilient, bitumenophilic linings for the casks or containers to be used for the end storage of radioactive wastes.
2. A method as claimed in claim 1, in which substances of step a) are alkaline earth compounds which bring the pH of the solutions and/or sludges to a value of from 7 to 11.
3. A method as claimed in claim 1 or 2 in which the substances utilised for the treatment of solutions and/or sludges are used in such an amount that only from 50",, to 950,, of the salts with considerable tendency to absorb water of crystallisation are converted into salts having a lesser or reduced tendency to absorb water of crystallisation.
4. A method as claimed in any preceding claim, in which, as water impermeable, corrosion-resistant, resilient, bitumenophilic lining, a carrier material is used steeped or coated with a bitumen of the same or similar properties to those of the bitumen used for the bitumen-solids mixture.
5. A method as claimed in claim 4, in which the steeped or coated carrier material is made of glass fibres, asbestos fibres, paper or cardboard.
6. A method as claimed in claim 5, in which the steeped or coated paper or the similarly treated cardboard is reinforced with glass fibres or asbestos fibres.
7. A method as claimed in claim 4 or 5, in which the bitumen paper used as lining or the bitumen cardboard used as lining is treated with a flame-resistant agent.
8. A method of improving the leach resistance of solidified bitumen products, as claimed in any preceding claim, substantially as hereinbefore described.
9. Solidified bitumen products whenever prepared by a method as claimed in any preceding claim.
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE19762628286 DE2628286C2 (en) | 1976-06-24 | 1976-06-24 | Process to improve the leaching resistance of bitumen solidification products from radioactive substances |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| GB1564878A true GB1564878A (en) | 1980-04-16 |
Family
ID=5981304
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| GB2497877A Expired GB1564878A (en) | 1976-06-24 | 1977-06-15 | Method of improving the leaching resistance of solidified bitumen products containing radioactive substances |
Country Status (3)
| Country | Link |
|---|---|
| DE (1) | DE2628286C2 (en) |
| FR (1) | FR2356246A1 (en) |
| GB (1) | GB1564878A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4834915A (en) * | 1987-12-16 | 1989-05-30 | Societe Anonyme: Societe Generale Pour Les Techniques Nouvelles - Sgn | Process for the immobilization of ion exchange resins originating from the secondary circuits of pressurized water nuclear reactors and gas-cooled graphite-moderated reactors |
Families Citing this family (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE2748098A1 (en) * | 1977-10-27 | 1979-05-10 | Kernforschungsz Karlsruhe | PROCESS FOR IMPROVING THE LEAKAGE RESISTANCE OF BITUMEN FASTENING PRODUCTS |
| DE2910677C2 (en) * | 1979-03-19 | 1983-12-22 | Kraftwerk Union AG, 4330 Mülheim | Process for the treatment of radioactive concentrates containing boron from wastewater from pressurized water reactors |
| JPS574599A (en) * | 1980-04-09 | 1982-01-11 | Belgonucleaire Sa | Method and device for solidifying radioactive waste liquid |
| JPS58109895A (en) * | 1981-12-23 | 1983-06-30 | 株式会社日立製作所 | Solidified material of radioactive waste |
| FR2544909B1 (en) * | 1983-04-21 | 1985-06-21 | Commissariat Energie Atomique | PROCESS FOR THE PACKAGING OF CONTAMINATED WASTE IN AN ACIDIC MEDIUM, IN PARTICULAR OF CATION EXCHANGE MATERIALS |
| SE8304278L (en) * | 1983-08-04 | 1985-02-05 | Studsvik Energiteknik Ab | PROCEDURE FOR TREATMENT OF USE, RADIOACTIVE, ORGANIC ION EXCHANGE MASS |
| JPH0677071B2 (en) * | 1984-02-09 | 1994-09-28 | 株式会社日立製作所 | Method and apparatus for solidifying radioactive waste liquid |
| FR2561812B1 (en) * | 1984-03-21 | 1989-02-17 | Commissariat Energie Atomique | PROCESS FOR BITUMENING RADIOACTIVE WASTE CONSTITUTED BY CATION EXCHANGE RESINS AND / OR ANION EXCHANGE RESINS |
| CH664843A5 (en) * | 1984-11-12 | 1988-03-31 | Industrieorientierte Forsch | METHOD FOR IMPROVING THE STABILITY PROPERTIES OF STRENGTHENED RADIOACTIVE ION EXCHANGE RESIN PARTICLES. |
| JPH0631850B2 (en) * | 1985-02-08 | 1994-04-27 | 株式会社日立製作所 | How to dispose of radioactive liquid waste |
| JPH0646236B2 (en) * | 1985-04-17 | 1994-06-15 | 株式会社日立製作所 | How to dispose of radioactive waste |
| FR2957710B1 (en) | 2010-03-19 | 2012-05-11 | Onectra | METHOD FOR CONDITIONING RADIOACTIVE WASTE, IN PARTICULAR ION EXCHANGE RESINS |
Family Cites Families (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| BE679231A (en) * | 1966-04-07 | 1966-10-07 | ||
| BE788911A (en) * | 1971-09-15 | 1973-01-02 | Magyar Asvanyolaj Es Foeldgaz | METHOD AND DEVICE FOR THE INCORPORATION IN BITUMEN OF BIOLOGICALLY HARMFUL WASTE |
| JPS5118941A (en) * | 1974-08-08 | 1976-02-14 | Denki Kagaku Kogyo Kk | KINZOKUJOHATSUYOYOKI |
| US4058479A (en) * | 1975-05-12 | 1977-11-15 | Aerojet-General Corporation | Filter-lined container for hazardous solids |
| DE2553569C2 (en) * | 1975-11-28 | 1985-09-12 | Kernforschungszentrum Karlsruhe Gmbh, 7500 Karlsruhe | Process for the solidification of radioactive aqueous waste materials by spray calcination and subsequent embedding in a matrix made of glass or glass ceramic |
-
1976
- 1976-06-24 DE DE19762628286 patent/DE2628286C2/en not_active Expired
-
1977
- 1977-05-06 FR FR7713929A patent/FR2356246A1/en active Granted
- 1977-06-15 GB GB2497877A patent/GB1564878A/en not_active Expired
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4834915A (en) * | 1987-12-16 | 1989-05-30 | Societe Anonyme: Societe Generale Pour Les Techniques Nouvelles - Sgn | Process for the immobilization of ion exchange resins originating from the secondary circuits of pressurized water nuclear reactors and gas-cooled graphite-moderated reactors |
Also Published As
| Publication number | Publication date |
|---|---|
| FR2356246A1 (en) | 1978-01-20 |
| FR2356246B1 (en) | 1982-06-18 |
| DE2628286C2 (en) | 1986-04-10 |
| DE2628286A1 (en) | 1977-12-29 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PS | Patent sealed | ||
| PCNP | Patent ceased through non-payment of renewal fee |