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GB1600211A - Processes for the treatment of radioactive effluents - Google Patents

Processes for the treatment of radioactive effluents Download PDF

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Publication number
GB1600211A
GB1600211A GB1874878A GB1874878A GB1600211A GB 1600211 A GB1600211 A GB 1600211A GB 1874878 A GB1874878 A GB 1874878A GB 1874878 A GB1874878 A GB 1874878A GB 1600211 A GB1600211 A GB 1600211A
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GB
United Kingdom
Prior art keywords
boric acid
radio
distilled
residue
isotopes
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
Application number
GB1874878A
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
RWE AG
Original Assignee
Rheinisch Westfaelisches Elektrizitaetswerk AG
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 Rheinisch Westfaelisches Elektrizitaetswerk AG filed Critical Rheinisch Westfaelisches Elektrizitaetswerk AG
Publication of GB1600211A publication Critical patent/GB1600211A/en
Expired legal-status Critical Current

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Classifications

    • GPHYSICS
    • G21NUCLEAR PHYSICS; NUCLEAR ENGINEERING
    • G21FPROTECTION AGAINST X-RADIATION, GAMMA RADIATION, CORPUSCULAR RADIATION OR PARTICLE BOMBARDMENT; TREATING RADIOACTIVELY CONTAMINATED MATERIAL; DECONTAMINATION ARRANGEMENTS THEREFOR
    • G21F9/00Treating radioactively contaminated material; Decontamination arrangements therefor
    • G21F9/04Treating liquids
    • G21F9/06Processing

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  • Physics & Mathematics (AREA)
  • Engineering & Computer Science (AREA)
  • General Engineering & Computer Science (AREA)
  • High Energy & Nuclear Physics (AREA)
  • Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
  • Heat Treatment Of Water, Waste Water Or Sewage (AREA)
  • Removal Of Specific Substances (AREA)

Description

(54) IMPROVEMENTS IN OR RELATING TO PROCESSES FOR THE TREATMENT OF RADIO-ACTIVE EFFLUENTS (71) We, RHEINIsCH-WEsTFALIsCHES ELEKTRIZITATSWERK AKTIENGESELLSCHAFT, of Kruppstrasse 5, D-4300 Essen 1, Federal Republic of Germany, ajoint stock company organized under the laws of Germany, 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:- This invention relates to processes for the treatment of effluents containing boric acid, radio-antimony and other radio-isotopes, with particular reference, for example, to boiler concentrates from nuclear power plants.
Known effluents of this nature have hitherto been disposed of as a whole, i.e., without treatment. However, the disposal costs have substantially increased in recent years. Further substantial inflation is probable in the future. Moreover, concern for environmental conservation will probably give rise to greater opposition to the transporting of radio-active liquids in large quantities for disposal purposes.
Various means are known in the art for reducing the volume of radio-active material for disposal and thereby reducing the disposal costs, with reference to radio-active effluents in general; for example, radio-active effluents are already evaporated down, and again the radio-isotopes can be precipitated from the effluent (as described in German Patent Specification No. 1767999). However, the effluents originally referred to do not respond satifactorily to evaporation treatment, since all the other inactive salts in the effluents must still be disposed of along with the radio-isotopes.Attempts to isolate the radio-isotopes from such effluents by chemical precipitation have failed because the degree of decontamination remains too low, particularly with reference to the radioantimony present; the chemical precipitation of certain radio-isotopes is affected by interference from the salts and other radioisotopes also present.
It is also known (for example, see ABC Chemie, vol. 1, A-K, 2nd revised edition, Verlag Harri Deutsch, Frankfurt/Main and Zurich, 1975, page 198) that boric acid can be converted to its trimethyl ester by methanol in the presence of concentrated sulphuric acid, and that the trimethyl ester of boric acid can be converted back to boric acid and methanol by hydrolysis. This knowledge has not hitherto been applied to the problems of treating the effluents originally referred to.
The object of the invention is to provide an economical treatment process of the type originally referred to, whereby the radioisotopes are concentrated into a small volume of material, compared with the initial volume of effluent, and can therefore be disposed of at a reasonable cost.
According to the invention, this object is achieved by evaporating the effluent substantially to dryness, treating the residue with concentrated sulphuric acid and, after cooling, with methanol, distilling off the resulting trimethyl ester of boric acid, storing the residue until the antimony activity has been dissipated, precipitating the radio-isotopes chemically from the stored residue, and isolating the radio-active precipitate.
In other words, the first stage of the treatment process of the invention is the removal of boric acid from the effluent in the form of its trimethyl ester. The residue from the first stage, containing the radio-isotopes, is stored in the second stage until the antimony activity has been dissipated, since it is impossible in practice to precipitate the radio-antimony by chemical means along with the other radio-isotopes. Residue storage is no problem, since antimony (Sb'24) has a half-life of only 60.3 days and the antimony activity dies down to about 1.6 and 0.02% after 1 and 2 years respectively. The next, third, stage of the process is the chemical precipitation of the further radioisotopes.
This precipitation is surprisingly close to quantitative, since the radio-antimony concentration is more or less down to zero and the concentrations of other radio-isotopes are high. The isolated radio-active precipitate obtained by the process of the invention occupies at the most 1% of the original volume of effluent, and the disposal costs are no longer substantial.
The advantages accruing from the invention are to be seen substantially in the low cost of the treatment.
Various possibilities are open for further improvement within the scope of the invention. If the effluent contains large amounts of caustic soda as well as boric acid, which can be the case with boiler concentrates encountered in nuclear power plants, the boric acid will take the form of sodium dihydrogen borate; the residue from the first processing stage in this case will consist substantially of sulphuric acid, sodium sulphate, water and radio-isotopes. However, if the effluent is free from caustic soda, the process of the invention can be modified very advantageously. Water remaining after distilling off the trimethyl ester of boric acid is preferably itself distilled off, and before the residue is put into storage it is recycled at least once, as concentrated sulphuric acid for the treatment of further effluent, thereby additionally enriching it with radio-isotopes.In this case, the residue after distilling off the water of reaction from the boric acid/methanol reaction consists entirely of concentrated sulphuric acid and radio-isotopes. It is for practical purposes an impure concentrated sulphuric acid and it can be significantly enriched with radio-isotopes by recycling repeatedly, as convenient. These features of the invention not only reduce the sulphuric acid consumption in the first processing stage but also significantly reduce the volume of radioactive precipitate. A further preferred embodiment of the invention is that the distilled trimethyl ester of boric acid is decomposed with water and that the resulting methanol is distilled off and recycled to form the trimethyl ester of boric acid during the treatment of a further batch of effluent.
The methanol cycle can be made almost lossfree in this way, thereby still further and substantially reducing the reagent costs for the first processing stage. The decomposition of the distilled trimethyl ester of boric acid with water liberates crystalline boric acid, which can be recovered by centrifuging or pressing, for subsequent use; the precipitate is surprisingly of analytical purity. The radioactive precipitate for final disposal is preferably isolated from the stored residue by decantation, filtration or centrifuging.
The invention will now be described in more detail with reference to a typical embodiment thereof: Boiler concentrate (lton) from a nuclear power plant had a boric acid content of about 10% by weight and a specific gammaactivity of 0.26 Ci/ton, about 70% emanating from Sb'24 and the remainder substantially from radio-isotopes of caesium, cobalt and manganese. The boiler concentrate was evaporated down substantially to dryness and treated with 16 kg of concentrated sulphuric acid followed, after cooling, by 155 kg of methanol, thereby forming the trimethyl ester of boric acid and water of reaction.
The trimethyl ester of boric acid was distilled off at a temperature of 68.75 C, into a water condenser. The water was then distilled off also. The residue (16 kg) was used as concentrated sulphuric acid to treat a further batch of boiler concentrate in the same way, and was in fact recycled until the residue had been enriched with radio-isotopes to a specific gamma-activity of 100 Ci/ton. The enriched residue was bled from the sulphuric acid cycle, simultaneously replacing it with fresh concentrated sulphuric acid, and stored until its antimony activity had died down to 0.02% of its original level.
The radio-isotopes of caesium, cobalt and manganese were then precipitated chemically, the radio-active precipitate being isolated and eventually disposed of. The volume of precipitate was no more than 1% of the original volume treated. The trimethyl ester of boric acid, distilled into the water condenser, decomposed therein to methanol and boric acid. The methanol was distilled off and recycled for the boric acid/methanol reaction in a subsequent batch of boiler concentrate for treatment. The crystalline boric acid was recovered by centrifuging; it was 99.9% pure and could therefore be returned directly to a primary system of a nuclear power plant.
WHAT WE CLAIM IS: 1. A process for the treatment of effluents containing boric acid, radio-antimony and other radio-isotopes, the process comprising evaporating the effluent substantially to dryness, treatment the residue with concentrated sulphuric acid and, after cooling, with methanol, distilling off the resulting trimethyl ester of boric acid, storing the residue until the antimony activity has been dissipated, precipitating the radio-isotopes chemically from the stored residue, and isolating the radio-active precipitate.
2. A process as in Claim 1, wherein when the effluent contains no caustic soda water remaining after distilling off the trimethyl ester of boric acid is itself distilled off, and before the residue is put into storage it is recycled at least once, as concentrated sulphuric acid for the treatment of further
**WARNING** end of DESC field may overlap start of CLMS **.

Claims (7)

**WARNING** start of CLMS field may overlap end of DESC **. third, stage of the process is the chemical precipitation of the further radioisotopes. This precipitation is surprisingly close to quantitative, since the radio-antimony concentration is more or less down to zero and the concentrations of other radio-isotopes are high. The isolated radio-active precipitate obtained by the process of the invention occupies at the most 1% of the original volume of effluent, and the disposal costs are no longer substantial. The advantages accruing from the invention are to be seen substantially in the low cost of the treatment. Various possibilities are open for further improvement within the scope of the invention. If the effluent contains large amounts of caustic soda as well as boric acid, which can be the case with boiler concentrates encountered in nuclear power plants, the boric acid will take the form of sodium dihydrogen borate; the residue from the first processing stage in this case will consist substantially of sulphuric acid, sodium sulphate, water and radio-isotopes. However, if the effluent is free from caustic soda, the process of the invention can be modified very advantageously. Water remaining after distilling off the trimethyl ester of boric acid is preferably itself distilled off, and before the residue is put into storage it is recycled at least once, as concentrated sulphuric acid for the treatment of further effluent, thereby additionally enriching it with radio-isotopes.In this case, the residue after distilling off the water of reaction from the boric acid/methanol reaction consists entirely of concentrated sulphuric acid and radio-isotopes. It is for practical purposes an impure concentrated sulphuric acid and it can be significantly enriched with radio-isotopes by recycling repeatedly, as convenient. These features of the invention not only reduce the sulphuric acid consumption in the first processing stage but also significantly reduce the volume of radioactive precipitate. A further preferred embodiment of the invention is that the distilled trimethyl ester of boric acid is decomposed with water and that the resulting methanol is distilled off and recycled to form the trimethyl ester of boric acid during the treatment of a further batch of effluent. The methanol cycle can be made almost lossfree in this way, thereby still further and substantially reducing the reagent costs for the first processing stage. The decomposition of the distilled trimethyl ester of boric acid with water liberates crystalline boric acid, which can be recovered by centrifuging or pressing, for subsequent use; the precipitate is surprisingly of analytical purity. The radioactive precipitate for final disposal is preferably isolated from the stored residue by decantation, filtration or centrifuging. The invention will now be described in more detail with reference to a typical embodiment thereof: Boiler concentrate (lton) from a nuclear power plant had a boric acid content of about 10% by weight and a specific gammaactivity of 0.26 Ci/ton, about 70% emanating from Sb'24 and the remainder substantially from radio-isotopes of caesium, cobalt and manganese. The boiler concentrate was evaporated down substantially to dryness and treated with 16 kg of concentrated sulphuric acid followed, after cooling, by 155 kg of methanol, thereby forming the trimethyl ester of boric acid and water of reaction. The trimethyl ester of boric acid was distilled off at a temperature of 68.75 C, into a water condenser. The water was then distilled off also. The residue (16 kg) was used as concentrated sulphuric acid to treat a further batch of boiler concentrate in the same way, and was in fact recycled until the residue had been enriched with radio-isotopes to a specific gamma-activity of 100 Ci/ton. The enriched residue was bled from the sulphuric acid cycle, simultaneously replacing it with fresh concentrated sulphuric acid, and stored until its antimony activity had died down to 0.02% of its original level. The radio-isotopes of caesium, cobalt and manganese were then precipitated chemically, the radio-active precipitate being isolated and eventually disposed of. The volume of precipitate was no more than 1% of the original volume treated. The trimethyl ester of boric acid, distilled into the water condenser, decomposed therein to methanol and boric acid. The methanol was distilled off and recycled for the boric acid/methanol reaction in a subsequent batch of boiler concentrate for treatment. The crystalline boric acid was recovered by centrifuging; it was 99.9% pure and could therefore be returned directly to a primary system of a nuclear power plant. WHAT WE CLAIM IS:
1. A process for the treatment of effluents containing boric acid, radio-antimony and other radio-isotopes, the process comprising evaporating the effluent substantially to dryness, treatment the residue with concentrated sulphuric acid and, after cooling, with methanol, distilling off the resulting trimethyl ester of boric acid, storing the residue until the antimony activity has been dissipated, precipitating the radio-isotopes chemically from the stored residue, and isolating the radio-active precipitate.
2. A process as in Claim 1, wherein when the effluent contains no caustic soda water remaining after distilling off the trimethyl ester of boric acid is itself distilled off, and before the residue is put into storage it is recycled at least once, as concentrated sulphuric acid for the treatment of further
effluent, thereby enriching it with radioisotopes.
3. A process as in Claim 1 or Claim 2, wherein the distilled trimethyl ester of boric acid is decomposed with water, and the resulting methanol is distilled off and recycled to form the trimethyl ester of boric acid during the treatment of a further batch of effluent.
4. A process as in Claim 3, wherein the crystalline boric acid formed during the decomposition with water of the distilled trimethyl ester of boric acid is recovered and if necessary dried.
5. A process as in Claim 4, wherein the crystalline boric acid is isolated by centrifuging or pressing.
6. A process as in any one of Claims 1 to 5, wherein the radio-active precipitate is isolated by decantation, filtation or centrifuging.
7. A process for the treatment of boiler concentrate from a nuclear power plant substantially as hereinbefore described.
GB1874878A 1977-05-21 1978-05-10 Processes for the treatment of radioactive effluents Expired GB1600211A (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
DE19772723025 DE2723025C3 (en) 1977-05-21 1977-05-21 Process for treating wastewater containing boric acid, radioactive antimony and other radioactive nuclides

Publications (1)

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GB1600211A true GB1600211A (en) 1981-10-14

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FR (1) FR2391533A1 (en)
GB (1) GB1600211A (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4540512A (en) * 1983-04-06 1985-09-10 Westinghouse Electric Corp. Recovery of boric acid from nuclear waste

Families Citing this family (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2459536A1 (en) * 1979-06-14 1981-01-09 Commissariat Energie Atomique PROCESS FOR TREATING DECONTAMINATION EFFLUENTS, IN PARTICULAR NUCLEAR REACTOR COMPONENTS AND DEVICE FOR IMPLEMENTING SAID METHOD
DE2950601A1 (en) * 1979-12-15 1981-06-19 Rainer Dr. 6843 Biblis Ambros METHOD FOR THE RECOVERY OF BORSAEUR FROM A WASTE WATER CONCENTRATE OF A NUCLEAR POWER PLANT
HU195967B (en) * 1985-05-13 1988-08-29 Tatabanyai Szenbanyak Process for recovering boric acid solution, reusable in atomic power station, from radioactive solutions of atomic power station
DE3638053A1 (en) * 1985-05-25 1988-05-19 Licentia Gmbh Electrophotographic recording material
DE3600358A1 (en) * 1986-01-09 1987-07-16 Mtt Metalltrenntechnik Fuer Nu Method and device for cleaning water-containing machinery oil from nuclear energy installations
DD293219A5 (en) * 1988-12-14 1991-08-22 ������@������������k�� PROCESS FOR PREPARING BORONIC COMPOUNDS AND RADIONUCLIDE-CONTAINING WASTE WATER

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
BE838533A (en) * 1976-02-13 1976-05-28 PROCESS FOR DRYING SOLUTIONS CONTAINING BORIC ACID

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4540512A (en) * 1983-04-06 1985-09-10 Westinghouse Electric Corp. Recovery of boric acid from nuclear waste

Also Published As

Publication number Publication date
DE2723025C3 (en) 1980-03-13
FR2391533A1 (en) 1978-12-15
FR2391533B1 (en) 1980-06-20
DE2723025A1 (en) 1978-11-23
DE2723025B2 (en) 1979-07-05

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