WO2014110014A1 - Strontium and cesium specific ion-exchange media - Google Patents
Strontium and cesium specific ion-exchange media Download PDFInfo
- Publication number
- WO2014110014A1 WO2014110014A1 PCT/US2014/010444 US2014010444W WO2014110014A1 WO 2014110014 A1 WO2014110014 A1 WO 2014110014A1 US 2014010444 W US2014010444 W US 2014010444W WO 2014110014 A1 WO2014110014 A1 WO 2014110014A1
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- WO
- WIPO (PCT)
- Prior art keywords
- water stream
- water
- group
- cations
- radionuclides
- Prior art date
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- 229910052712 strontium Inorganic materials 0.000 title claims abstract description 18
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 title claims abstract description 18
- 229910052792 caesium Inorganic materials 0.000 title claims abstract description 12
- TVFDJXOCXUVLDH-UHFFFAOYSA-N caesium atom Chemical compound [Cs] TVFDJXOCXUVLDH-UHFFFAOYSA-N 0.000 title claims abstract description 12
- 239000012500 ion exchange media Substances 0.000 title description 3
- 150000001768 cations Chemical class 0.000 claims abstract description 31
- 239000011575 calcium Substances 0.000 claims abstract description 14
- 239000013535 sea water Substances 0.000 claims abstract description 14
- 239000011777 magnesium Substances 0.000 claims abstract description 13
- 239000011734 sodium Substances 0.000 claims abstract description 13
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims abstract description 11
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims abstract description 11
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910052791 calcium Inorganic materials 0.000 claims abstract description 10
- 229910052749 magnesium Inorganic materials 0.000 claims abstract description 10
- 229910052708 sodium Inorganic materials 0.000 claims abstract description 10
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910052700 potassium Inorganic materials 0.000 claims abstract description 6
- 239000011591 potassium Substances 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 40
- 229910001868 water Inorganic materials 0.000 claims description 35
- 238000000034 method Methods 0.000 claims description 28
- 239000010936 titanium Substances 0.000 claims description 23
- 101100065719 Drosophila melanogaster Ets98B gene Proteins 0.000 claims description 7
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 claims description 7
- GNKTZDSRQHMHLZ-UHFFFAOYSA-N [Si].[Si].[Si].[Ti].[Ti].[Ti].[Ti].[Ti] Chemical compound [Si].[Si].[Si].[Ti].[Ti].[Ti].[Ti].[Ti] GNKTZDSRQHMHLZ-UHFFFAOYSA-N 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 6
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 5
- 239000003673 groundwater Substances 0.000 claims description 4
- 239000002352 surface water Substances 0.000 claims description 4
- 239000011230 binding agent Substances 0.000 claims description 3
- 239000008187 granular material Substances 0.000 claims description 3
- 235000012206 bottled water Nutrition 0.000 claims description 2
- 239000003651 drinking water Substances 0.000 claims description 2
- 230000005611 electricity Effects 0.000 claims description 2
- 238000005067 remediation Methods 0.000 claims description 2
- 239000003758 nuclear fuel Substances 0.000 claims 1
- 150000002500 ions Chemical class 0.000 abstract description 32
- 239000000463 material Substances 0.000 abstract description 15
- 239000000243 solution Substances 0.000 description 32
- 229910052719 titanium Inorganic materials 0.000 description 21
- -1 titanium silicates Chemical class 0.000 description 18
- 239000000499 gel Substances 0.000 description 16
- 239000010457 zeolite Substances 0.000 description 14
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 12
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 9
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 8
- 229910021536 Zeolite Inorganic materials 0.000 description 8
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 8
- 238000005342 ion exchange Methods 0.000 description 7
- 239000002808 molecular sieve Substances 0.000 description 7
- 239000011148 porous material Substances 0.000 description 7
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 7
- 229910001385 heavy metal Inorganic materials 0.000 description 6
- 230000002285 radioactive effect Effects 0.000 description 6
- 239000000377 silicon dioxide Substances 0.000 description 6
- 238000003756 stirring Methods 0.000 description 5
- 239000002699 waste material Substances 0.000 description 5
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 4
- JYIBXUUINYLWLR-UHFFFAOYSA-N aluminum;calcium;potassium;silicon;sodium;trihydrate Chemical compound O.O.O.[Na].[Al].[Si].[K].[Ca] JYIBXUUINYLWLR-UHFFFAOYSA-N 0.000 description 4
- 239000007864 aqueous solution Substances 0.000 description 4
- 230000008901 benefit Effects 0.000 description 4
- 229910001603 clinoptilolite Inorganic materials 0.000 description 4
- 229910052681 coesite Inorganic materials 0.000 description 4
- 229910052906 cristobalite Inorganic materials 0.000 description 4
- 239000008367 deionised water Substances 0.000 description 4
- 229910021641 deionized water Inorganic materials 0.000 description 4
- 238000003795 desorption Methods 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 239000011541 reaction mixture Substances 0.000 description 4
- 229910052682 stishovite Inorganic materials 0.000 description 4
- 229910052905 tridymite Inorganic materials 0.000 description 4
- KEAYESYHFKHZAL-UHFFFAOYSA-N Sodium Chemical compound [Na] KEAYESYHFKHZAL-UHFFFAOYSA-N 0.000 description 3
- 239000004115 Sodium Silicate Substances 0.000 description 3
- 239000003513 alkali Substances 0.000 description 3
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 3
- 230000001186 cumulative effect Effects 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 238000000746 purification Methods 0.000 description 3
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 3
- 229910052911 sodium silicate Inorganic materials 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- CPELXLSAUQHCOX-UHFFFAOYSA-M Bromide Chemical compound [Br-] CPELXLSAUQHCOX-UHFFFAOYSA-M 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 229910052768 actinide Inorganic materials 0.000 description 2
- 150000001255 actinides Chemical class 0.000 description 2
- 229910052783 alkali metal Inorganic materials 0.000 description 2
- 150000008044 alkali metal hydroxides Chemical class 0.000 description 2
- 238000011109 contamination Methods 0.000 description 2
- RCJVRSBWZCNNQT-UHFFFAOYSA-N dichloridooxygen Chemical compound ClOCl RCJVRSBWZCNNQT-UHFFFAOYSA-N 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000002440 industrial waste Substances 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- NROKBHXJSPEDAR-UHFFFAOYSA-M potassium fluoride Chemical compound [F-].[K+] NROKBHXJSPEDAR-UHFFFAOYSA-M 0.000 description 2
- 238000000634 powder X-ray diffraction Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 239000011550 stock solution Substances 0.000 description 2
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 description 2
- 101100065718 Caenorhabditis elegans ets-4 gene Proteins 0.000 description 1
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- JLVVSXFLKOJNIY-UHFFFAOYSA-N Magnesium ion Chemical compound [Mg+2] JLVVSXFLKOJNIY-UHFFFAOYSA-N 0.000 description 1
- 239000004677 Nylon Substances 0.000 description 1
- 229910021626 Tin(II) chloride Inorganic materials 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 239000002250 absorbent Substances 0.000 description 1
- 230000002745 absorbent Effects 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 229910001515 alkali metal fluoride Inorganic materials 0.000 description 1
- 150000001342 alkaline earth metals Chemical group 0.000 description 1
- 238000011001 backwashing Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009933 burial Methods 0.000 description 1
- 229910052793 cadmium Inorganic materials 0.000 description 1
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 1
- 229910001424 calcium ion Inorganic materials 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000011651 chromium Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000011067 equilibration Methods 0.000 description 1
- 238000011010 flushing procedure Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000011491 glass wool Substances 0.000 description 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 1
- 230000002706 hydrostatic effect Effects 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 238000012994 industrial processing Methods 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000003456 ion exchange resin Substances 0.000 description 1
- 229920003303 ion-exchange polymer Polymers 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 229910001425 magnesium ion Inorganic materials 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 150000001455 metallic ions Chemical class 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 235000010755 mineral Nutrition 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000008239 natural water Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 229920001778 nylon Polymers 0.000 description 1
- 239000011698 potassium fluoride Substances 0.000 description 1
- 235000003270 potassium fluoride Nutrition 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 150000004760 silicates Chemical class 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 238000001694 spray drying Methods 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 230000035882 stress Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 150000003608 titanium Chemical class 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 229910009112 xH2O Inorganic materials 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28002—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their physical properties
- B01J20/28004—Sorbent size or size distribution, e.g. particle size
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
- B01J20/2803—Sorbents comprising a binder, e.g. for forming aggregated, agglomerated or granulated products
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
- B01J20/28047—Gels
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
- B01J20/28057—Surface area, e.g. B.E.T specific surface area
- B01J20/28061—Surface area, e.g. B.E.T specific surface area being in the range 100-500 m2/g
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
- B01J20/28069—Pore volume, e.g. total pore volume, mesopore volume, micropore volume
- B01J20/28071—Pore volume, e.g. total pore volume, mesopore volume, micropore volume being less than 0.5 ml/g
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J39/00—Cation exchange; Use of material as cation exchangers; Treatment of material for improving the cation exchange properties
- B01J39/08—Use of material as cation exchangers; Treatment of material for improving the cation exchange properties
- B01J39/14—Base exchange silicates, e.g. zeolites
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/42—Treatment of water, waste water, or sewage by ion-exchange
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/58—Treatment of water, waste water, or sewage by removing specified dissolved compounds
-
- 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
- G21F9/10—Processing by flocculation
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/006—Radioactive compounds
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/06—Contaminated groundwater or leachate
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/08—Seawater, e.g. for desalination
Definitions
- This invention relates to a novel ion exchange media capable of removing radionuclides from water, including seawater.
- ion exchangers both organic and inorganic, including crystalline molecular sieve zeolites
- ion exchangers both organic and inorganic, including crystalline molecular sieve zeolites
- a molecular sieve will function normally to the point at which the metal which is desirous of being removed effectively occupies some portion of the ionic sites in said zeolite.
- the zeolite must either be discarded or regenerated.
- U.S. 5,053,139 discloses that certain amorphous titanium and tin silicate gels demonstrate remarkable rates of uptake for heavy metal species such as lead, cadmium, zinc, chromium and mercury which are an order of magnitude greater than that of prior art absorbents or ion exchangers under the conditions tested which include the presence of competing ions such as calcium and magnesium.
- the combination of extraordinary lead selectivities, capacity and uptake rates allows such materials to strip lead from aqueous streams with minimal contact time allowing direct end use in filters for water purification, be it under-the-counter or under-the-faucet, or whole-house devices.
- This invention is directed to amorphous and crystalline titanosilicate materials that have an unexpected selectivity for cesium and strontium, especially in the presence of high levels of competing ions.
- the titanosilicates of this invention show very high, unexpected selectivity in the presence of such competing cations such as sodium, calcium, magnesium and potassium, such as present in seawater.
- the titanosilicates of this invention offer what is expected to be a more cost effective alternative at comparable performance to the specialized MST media noted above.
- the amorphous titanosilicates of this invention can be produced in agglomerated form without the need for a binder, thus providing a significant advantage over MST and CST materials that are produced in powder form and must be bound, for example according to the teachings of Hobbs, D. T. Journal of the South Carolina Academy of Science, [201 1 ], 9(1 ) "Properties and Uses of Sodium Titanates and Peroxotitanates".
- a further advantage of the proposed invention is that such inorganic materials can be vitrified making them suitable for long-term burial of radioactive nuclear waste. Organic ion exchange resins, for example, do not offer these benefits.
- the high titanium content of MST makes those materials more difficult to vitrify relative to the subject of this invention.
- amorphous and crystalline titanium silicates are admirably suited to remove radionuclides from water in the presence of competing ions normally found in seawater. More specifically, di- and tri-valent radionuclides are capable of being removed from contaminated aqueous streams, such as seawater, surface water and ground water which contain non- radio-active Groups I and II cations. Removal of cesium and strontium in the presence of competing ions by titanium silicates is readily achieved.
- silicate gels have long been known in the art to be useful for a wide variety of applications including ion exchangers, and recognition that certain silicate gels were so unusual that they could also effectively remove lead at an extremely high rate, as disclosed in U.S. 5,053,139, the use of titanium silicates for the removal of radionuclides such as cesium and strontium from seawater has not been recognized.
- the amorphous titanium silicates useful in the novel process of this invention are titanium silicates, which preferably contain a silicon-to-titanium ratio of from 2:1 to 0.5:1 , with silicon-to-titanium ratios of 1 .5:1 to 1 .2:1 being most preferred.
- the titanium silicates useful in the novel process of this invention are prepared by merely contacting a solution of a soluble titanium salt, such as the chloride, the bromide, the oxychloride, etc. with a sodium silicate solution and sufficient alkali with vigorous stirring.
- a soluble titanium salt such as the chloride, the bromide, the oxychloride, etc.
- the pH of the solution should fall between 4 and 9, and preferably between 7 and 8, and if this is not the case, the pH is adjusted with dilute HCI or any other acid or dilute sodium hydroxide.
- the sample is then washed free of salts and dried. It is usually dried at about 70° C for 24 to 48 hours, although the drying temperature and time are not critical.
- the amorphous titanium silicates are formed as a precipitated gel.
- the gel can be used as made, which is usually in its sodium form, or in other alkali or alkaline earth metal forms, as well as in its hydrogen form.
- the gel is washed and then dried, the dried gel being stable in water. If the gel is dried by spray drying, then the material forms a powder. If the gel is tray dried, the material forms a rock-like state, which resembles dried mud with shrinkage cracks. The rock-like material is ground to make granules or stress fractured via hydrostatic pressure.
- the amorphous nature of these titanium silicates can be evidenced by a powder X-ray diffraction pattern with no crystalline character.
- the present invention also includes stable crystalline titanium silicate molecular sieve zeolites which have a pore size of approximately 3-4 Angstrom units and a titania/silica mole ratio in the range of from 1 .0 to 10. These materials are known as ETS-4 and are described in U.S. 4,938,939.
- the ETS-4 titanium silicates have a definite X-ray diffraction pattern unlike other molecular sieve zeolites and can be identified in terms of mole ratios of oxides as follows:
- M is at least one cation having a valence of n
- y is from 1 .0 to 10.0
- z is from 0 to 100.
- M is a mixture of alkali metal cations, particularly sodium and potassium
- y is at least 2.5 and ranges up to about 5.
- ETS molecular sieve zeolites have an ordered crystalline structure and an X-ray powder diffraction pattern having the following significant lines:
- ETS-4 molecular sieve zeolites can be prepared from a reaction mixture containing a titanium source such as titanium tetrachloride, a source of silica, a source of alkalinity such as an alkali metal hydroxide, water and, optionally, an alkali metal fluoride having a composition in terms of mole ratios falling within the following ranges.
- a titanium source such as titanium tetrachloride
- silica a source of silica
- alkalinity such as an alkali metal hydroxide
- water optionally, an alkali metal fluoride having a composition in terms of mole ratios falling within the following ranges.
- M indicates the cations of valence n derived from the alkali metal hydroxide and potassium fluoride and/or alkali metal salts used for preparing the titanium silicate according to the invention.
- the reaction mixture is heated to a temperature of from about 100°C to 300°C for a period of time ranging from about 8 hours to 40 days, or more.
- the hydrothermal reaction is carried out until crystals are formed and the resulting crystalline product is thereafter separated from the reaction mixture, cooled to room temperature, filtered and water washed.
- the reaction mixture can be stirred although it is not necessary. It has been found that when using gels, stirring is unnecessary but can be employed.
- the preferred temperature range is 100°C. to 175°C for a period of time ranging from 12 hours to 15 days. Crystallization is performed in a continuous or batchwise manner under autogeneous pressure in an autoclave or static bomb reactor. Following the water washing step, the crystalline ETS- 4 is dried at temperatures of 100 to 400°F for periods ranging up to 30 hours.
- the ETS-4 material is synthesized as a powder, typically, as a slurry of distinct particles in the micron size range. To utilize this material in a packed bed requires agglomeration of the ETS-4 with a binder, as, for example, disclosed in U.S. 4,938,939.
- a binder as, for example, disclosed in U.S. 4,938,939.
- ion exchangers having extraordinary selectivity, capacity and rate of exchange can be prepared by precipitating hydrous metal oxides wherein the mole ratio of silicon to titanium is in the range from 1 :4 to 1 .9:1 . Preferred mole ratios have been set forth above.
- the titanium silicates which are operable in the novel process of this invention have cumulative desorption pore volumes in cubic centimeters per gram ranging from about 0.03 to about 0.25. Cumulative desorption pore volume is determined by the method as described in U.S. 5,053,139.
- tin silicates would also be useful in removing radionuclides from aqueous streams containing competing ions.
- the tin silicate gels can be prepared as mentioned above by contacting a solution of a soluble tin salt, such as the chloride, bromide, oxychloride, etc. with a sodium silicate solution and sufficient alkali, and vigorous stirring.
- the titanium silicates and tin silicates of this invention are capable of removing radionuclide cations from aqueous streams containing substantial amounts of competing cations.
- the invention is applicable for removing such cations from natural surface and ground water, such as for purification of potable water, as well as for remediation of natural water sources, which have become contaminated.
- the invention is capable of removing the radionuclide cation contamination from natural aqueous sources, which have become contaminated due to industrial waste runoff, or accidental leakage of such materials from industrial processing.
- a particularly contemporary use would be the removal of such radionuclide cations from industrial process streams, such as, for example, from fuel pool water of a nuclear reactor used to produce electricity, as well as from nuclear electrical generating plants which have been overrun by seawater, such as in the recent tsunami which afflicted Japan several years ago, or from other industrial process streams.
- the silicates of the present invention are capable of removing radionuclide cations including, but not limited to, cesium and strontium from aqueous systems, which contain at least 10 times the amount of cations other than the radionuclide cations on an equivalent basis.
- radionuclide cations including, but not limited to, cesium and strontium from aqueous systems, which contain at least 10 times the amount of cations other than the radionuclide cations on an equivalent basis.
- Such other cations would include Group I and Group II metal cations such as sodium, potassium, calcium and magnesium.
- the invention is also useful in removing the radionuclide cations from aqueous systems, in which the aqueous stream contains at least 100 times the amount of the light Group I and Group II metal cations and, even, when such aqueous streams contain at least 1 ,000 times and more of the competing Group I and Group II cations relative to the radionuclide cations on an equivalent basis.
- solution A Two liters of a 1 .5M titanium chloride solution (solution A) are made by adding 569.1 1 g TiCI 4 to enough deionized water to make 2 liters.
- solution B Two liters of 1 .5M sodium silicate solution (solution B) are made by dissolving 638.2 g of Na 2 S1O3.5H 2 O in enough 3M NaOH to make 2 liters.
- Solution B is added to solution A at a rate of 16 cc/minute with extremely vigorous stirring. After addition is complete, the mixture is allowed to continue mixing for an additional 15 minutes.
- the pH of the solution should fall between 7.5 and 7.9; if this is not the case, the pH is adjusted with dilute HCI or dilute NaOH. The sample is then allowed to age one hour.
- any water on top of the gel is decanted off.
- the sample is then filtered, washed with 1 liter deionized water per liter of gel, reslurried in 4-6 liters of deionized water, filtered, and finally rewashed with 2 liters of water per liter of gel.
- the sample is then dried at 100°C for 24-48 hours.
- the gel produced from this method has a silicon-to-titanium ratio of approximately 1 :1 and a surface area of approximately 295 m 2 /g.
- the large gel particulates are crushed into small particulates predominantly in the range of 20-60 mesh.
- the particles are then subjected to ion exchange testing.
- the pore size distribution as measured by nitrogen desorption is found to have an average pore radius of 15 angstroms.
- the cumulative desorption pore volume of this sample is found to be 0.148 cc/g.
- a solution using reagent grade chemicals in deionized distilled water was prepared as shown in Table 3, which provides a summary of a composition for a simulated high-level nuclear waste solution used to evaluate the titanium silicate of this invention.
- a targeted amount of 5.2 ppm of non-radioactive Sr was added to the solution shown in Table 3.
- 2.5 mg of titanosilicate formed in Example 1 was added to 25 ml of the simulated solution and allowed to equilibrate with agitation for 40 hours at ambient room temperature. After equilibration, the solution was filtered through a 0.45 micron pore size nylon membrane filter to remove any residual solids.
- Strontium levels were effectively reduced to the following concentrations in a series of six separate experiments as described in this example: 1 .7 ppm, 1 .5 ppm, 1 .5 ppm, 1 .4 ppm, 1 .4 ppm, and 1 .5 ppm.
- Clinoptilolite and zeolite 4A are common zeolites with known selectivity for heavy cations and were thus compared to the titanosilicate of Example 1 .
- Titanosilicate 1 10 4910 128 2 5 0.012
- Titanosilicate 1 100 3530 342 44 52 0.335
- Titanosilicate 1 1000 3260 377 99 1 12 3
- Clinoptilolite 1 1000 3200 364 107 120 5
- Example 7 To further show the advantages of the present invention relative to current technology, the experiment of Example 4 was repeated using a standard granular zeolite type 4A supplied by BASF under the designation 4A BF. The results of the dynamic breakthrough test are shown in Table 7. The emergence of strontium in the effluent (also referred to as breakthrough) is nearly immediate and much sooner than in Example 4 despite this zeolite having more than twice the ion exchange capacity than the titanosilicate. Table 7
Abstract
Description
Claims
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CN201480004252.XA CN104903253A (en) | 2013-01-09 | 2014-01-07 | Strontium and cesium specific ion-exchange media |
RU2015133020A RU2664939C2 (en) | 2013-01-09 | 2014-01-07 | Ion-exchange materials selective to strontium and cesium |
JP2015552727A JP6618803B2 (en) | 2013-01-09 | 2014-01-07 | A method for selective removal of strontium radionuclides from water streams. |
CA2896971A CA2896971A1 (en) | 2013-01-09 | 2014-01-07 | Strontium and cesium specific ion-exchange media |
KR1020157021083A KR20150105392A (en) | 2013-01-09 | 2014-01-07 | Strontium and cesium specific ion-exchange media |
BR112015016324A BR112015016324A2 (en) | 2013-01-09 | 2014-01-07 | method of removing divalent and / or trivalent radionuclides from a water stream |
SG11201504720QA SG11201504720QA (en) | 2013-01-09 | 2014-01-07 | Strontium and cesium specific ion-exchange media |
EP14738180.0A EP2943441A4 (en) | 2013-01-09 | 2014-01-07 | Strontium and cesium specific ion-exchange media |
MX2015008682A MX2015008682A (en) | 2013-01-09 | 2014-01-07 | Strontium and cesium specific ion-exchange media. |
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CA (1) | CA2896971A1 (en) |
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WO2017015318A1 (en) * | 2015-07-20 | 2017-01-26 | Basf Corporation | Mesoporous titanosilicates and uses thereof |
KR20170022522A (en) | 2015-08-21 | 2017-03-02 | 안동대학교 산학협력단 | Method for preparing titanosilicate using dropwise method and titanosilicate absorbent for removing radioactive nuclides prepared thereby |
KR20180032337A (en) * | 2016-09-22 | 2018-03-30 | 안동대학교 산학협력단 | Titanosilicates absorbants substituted tetravalance cation |
US20200131052A1 (en) * | 2017-06-29 | 2020-04-30 | Solenis Technologies Cayman, L.P. | Water stable granules and tablets |
KR102035801B1 (en) * | 2017-10-19 | 2019-10-24 | 한국과학기술원 | Titanosilicate Adsorbent Having Sodium and Potassium for Simultaneously Removing Cesium and Strontium and Method of Preparing the Same |
JP2020018971A (en) * | 2018-07-31 | 2020-02-06 | Dic株式会社 | Adsorbent granulated body, manufacturing method of adsorbent granulated body, and purification method of solution containing radioactive strontium |
CN110293001A (en) * | 2019-07-01 | 2019-10-01 | 中国科学院青海盐湖研究所 | Rubidium, the precipitate flotation separation system of caesium and its application in a kind of aqueous solution |
US11577014B2 (en) | 2019-07-09 | 2023-02-14 | Uop Llc | Process for removing strontium ions from bodily fluids using metallate ion exchange compositions |
US20220370979A1 (en) * | 2019-11-04 | 2022-11-24 | Basf Corporation | Porous aluminosilicate compositions for contaminant metal removal in water treatment |
WO2023215755A2 (en) * | 2022-05-03 | 2023-11-09 | Graver Technologies Llc | Sorbent for removal of ions from liquid streams and method of making the same |
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