JP2006247485A - Method for treating/recovering strongly oxidizing metal ion in solid-coexistent aqueous solution by irradiating the aqueous solution with radial ray - Google Patents
Method for treating/recovering strongly oxidizing metal ion in solid-coexistent aqueous solution by irradiating the aqueous solution with radial ray Download PDFInfo
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- 239000007864 aqueous solution Substances 0.000 title claims abstract description 21
- 229910021645 metal ion Inorganic materials 0.000 title claims abstract description 15
- 230000001590 oxidative effect Effects 0.000 title claims abstract description 12
- 238000000034 method Methods 0.000 title claims description 15
- 230000001678 irradiating effect Effects 0.000 title abstract description 4
- JOPOVCBBYLSVDA-UHFFFAOYSA-N chromium(6+) Chemical compound [Cr+6] JOPOVCBBYLSVDA-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000007787 solid Substances 0.000 claims abstract description 26
- 238000006722 reduction reaction Methods 0.000 claims abstract description 18
- 239000000243 solution Substances 0.000 claims abstract description 14
- 230000005855 radiation Effects 0.000 claims abstract description 13
- 239000000463 material Substances 0.000 claims abstract description 6
- 229910052751 metal Inorganic materials 0.000 claims abstract description 3
- 239000002184 metal Substances 0.000 claims abstract description 3
- 238000006243 chemical reaction Methods 0.000 claims description 7
- 239000000843 powder Substances 0.000 claims description 6
- 238000011084 recovery Methods 0.000 claims description 5
- 239000000383 hazardous chemical Substances 0.000 claims description 4
- 150000002500 ions Chemical class 0.000 claims description 4
- 230000002285 radioactive effect Effects 0.000 claims description 4
- 230000003647 oxidation Effects 0.000 claims description 3
- 238000007254 oxidation reaction Methods 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 2
- 239000006104 solid solution Substances 0.000 claims description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims 1
- 238000010894 electron beam technology Methods 0.000 claims 1
- 239000000446 fuel Substances 0.000 claims 1
- 229910052739 hydrogen Inorganic materials 0.000 claims 1
- 239000001257 hydrogen Substances 0.000 claims 1
- 239000010808 liquid waste Substances 0.000 claims 1
- 230000033116 oxidation-reduction process Effects 0.000 claims 1
- 239000011651 chromium Substances 0.000 abstract description 19
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 abstract description 16
- 229910052804 chromium Inorganic materials 0.000 abstract description 16
- 239000000126 substance Substances 0.000 abstract description 7
- 230000001737 promoting effect Effects 0.000 abstract 1
- 231100000167 toxic agent Toxicity 0.000 abstract 1
- 239000003440 toxic substance Substances 0.000 abstract 1
- 230000009467 reduction Effects 0.000 description 8
- 238000001784 detoxification Methods 0.000 description 5
- 239000011343 solid material Substances 0.000 description 5
- 239000003054 catalyst Substances 0.000 description 4
- 238000007747 plating Methods 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 229910010413 TiO 2 Inorganic materials 0.000 description 2
- WGLPBDUCMAPZCE-UHFFFAOYSA-N Trioxochromium Chemical compound O=[Cr](=O)=O WGLPBDUCMAPZCE-UHFFFAOYSA-N 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 229910000423 chromium oxide Inorganic materials 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000002927 high level radioactive waste Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000012857 radioactive material Substances 0.000 description 2
- 239000002901 radioactive waste Substances 0.000 description 2
- 238000003608 radiolysis reaction Methods 0.000 description 2
- 238000012958 reprocessing Methods 0.000 description 2
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 description 2
- 239000002915 spent fuel radioactive waste Substances 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 description 1
- 206010007269 Carcinogenicity Diseases 0.000 description 1
- 229910052684 Cerium Inorganic materials 0.000 description 1
- 229910017563 LaCrO Inorganic materials 0.000 description 1
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- -1 abrasive Substances 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 239000011449 brick Substances 0.000 description 1
- KOPBYBDAPCDYFK-UHFFFAOYSA-N caesium oxide Chemical compound [O-2].[Cs+].[Cs+] KOPBYBDAPCDYFK-UHFFFAOYSA-N 0.000 description 1
- 229910001942 caesium oxide Inorganic materials 0.000 description 1
- 230000007670 carcinogenicity Effects 0.000 description 1
- 231100000260 carcinogenicity Toxicity 0.000 description 1
- 238000010531 catalytic reduction reaction Methods 0.000 description 1
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 229940090961 chromium dioxide Drugs 0.000 description 1
- IAQWMWUKBQPOIY-UHFFFAOYSA-N chromium(4+);oxygen(2-) Chemical compound [O-2].[O-2].[Cr+4] IAQWMWUKBQPOIY-UHFFFAOYSA-N 0.000 description 1
- AYTAKQFHWFYBMA-UHFFFAOYSA-N chromium(IV) oxide Inorganic materials O=[Cr]=O AYTAKQFHWFYBMA-UHFFFAOYSA-N 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000007872 degassing Methods 0.000 description 1
- 229940077449 dichromate ion Drugs 0.000 description 1
- SOCTUWSJJQCPFX-UHFFFAOYSA-N dichromate(2-) Chemical compound [O-][Cr](=O)(=O)O[Cr]([O-])(=O)=O SOCTUWSJJQCPFX-UHFFFAOYSA-N 0.000 description 1
- 239000003302 ferromagnetic material Substances 0.000 description 1
- 230000005251 gamma ray Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 239000010842 industrial wastewater Substances 0.000 description 1
- 239000003456 ion exchange resin Substances 0.000 description 1
- 229920003303 ion-exchange polymer Polymers 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 239000011572 manganese Substances 0.000 description 1
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 238000011946 reduction process Methods 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000010802 sludge Substances 0.000 description 1
- 235000010265 sodium sulphite Nutrition 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 238000004017 vitrification Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 238000003911 water pollution Methods 0.000 description 1
- 229910001928 zirconium oxide Inorganic materials 0.000 description 1
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- Physical Water Treatments (AREA)
- Treatment Of Water By Oxidation Or Reduction (AREA)
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Abstract
Description
本発明は、固体材料を含む水溶液に放射線照射することにより誘起する還元反応を利用して、６価クロムなどの強酸化性金属イオンを処理あるいは回収する方法に関するものである。さらに詳しくは、この発明は、固体が放射線エネルギーを吸収して化学反応エネルギーに有効に変換する触媒（ここでは、放射線触媒と呼ぶ）としての機能することにより、環境有害物質の６価クロムなどを高効率で無害化し、より低い酸化状態の固体酸化物あるいはイオンの有用材料として回収する方法に関するものである。 The present invention relates to a method for treating or recovering a strong oxidizing metal ion such as hexavalent chromium using a reduction reaction induced by irradiating an aqueous solution containing a solid material with radiation. In more detail, the present invention functions as a catalyst (herein referred to as a radiation catalyst) in which a solid absorbs radiation energy and effectively converts it into chemical reaction energy, so that hexavalent chromium, which is an environmentally hazardous substance, can be used. The present invention relates to a method for recovering as a useful material of a solid oxide or ion having a lower oxidation state and a high efficiency and detoxification.
６価クロムを塗布した金属表面は耐食性・防食性に優れているため、現在多くの工業製品の表面処理に幅広く使用されているが、酸化力が強く発ガン性を有する有害物質であり、高濃度６価クロム廃液およびメッキ水洗液などの低濃度６価クロムの廃水の処理が不可欠である。６価クロムの無害化にはpH 2.5以下で添加した亜硫酸ソーダにより３価クロムへ還元するのが主流である。 Since the metal surface coated with hexavalent chromium is excellent in corrosion resistance and anticorrosion properties, it is currently widely used for surface treatment of many industrial products, but it is a hazardous substance with strong oxidizing power and carcinogenicity. Treatment of waste water of low concentration hexavalent chromium such as hexavalent chromium waste solution and plating water washing solution is indispensable. For detoxification of hexavalent chromium, the mainstream is to reduce it to trivalent chromium with sodium sulfite added at pH 2.5 or lower.
さらに、３価クロムはアルカリを使用して、pH 6.5-7.5程度で水酸化物Cr(OH)3沈殿として回収し、主に３価クロムスラッジとして埋め立て処分されている。メッキ廃水をイオン交換樹脂に通して直接６価クロムを回収する方法もある。いずれにしても、無害化や回収の工程では、複雑な化学処理が大量の化学薬品を使用して行われているのが現状である。 In addition, trivalent chromium is recovered as hydroxide Cr (OH) 3 precipitate at pH 6.5-7.5 using alkali and is mainly disposed of in landfill as trivalent chromium sludge. There is also a method of directly recovering hexavalent chromium by passing plating wastewater through an ion exchange resin. In any case, in the process of detoxification and recovery, the present situation is that complicated chemical treatment is performed using a large amount of chemicals.
６価クロムなどの無害化や回収の工程において、複雑な化学処理や大量の化学薬品を使用せずに、還元反応を促進し、低酸化状態のクロムを回収することが課題である。 In the process of detoxification and recovery of hexavalent chromium and the like, the problem is to promote the reduction reaction and recover low-oxidized chromium without using complicated chemical treatment and a large amount of chemicals.
本発明は、強酸化性金属イオンが溶存する水溶液に粉体ないしは塊状の固体を加えたものに、溶液を含む容器の外部からの放射線照射または放射線源を容器内に導入した内部からの放射線照射により、溶液中に誘起される還元反応を利用して、環境有害物質である強酸化性金属イオンを還元処理し有用材料として回収する方法である。 The present invention relates to an aqueous solution in which a strong oxidizing metal ion is dissolved and a powder or a massive solid added thereto, irradiation from the outside of the container containing the solution, or irradiation from the inside where a radiation source is introduced into the container. Thus, using a reduction reaction induced in the solution, a strong oxidizing metal ion which is an environmentally hazardous substance is reduced and recovered as a useful material.
上記粉体ないしは塊状の固体が酸化物である場合は、石英、アルミナ、酸化チタン、酸化ジルコニウム、酸化セシウム若しくは酸化クロム等、又はその混合物若しくは固溶体である。 When the powder or massive solid is an oxide, it is quartz, alumina, titanium oxide, zirconium oxide, cesium oxide or chromium oxide, or a mixture or solid solution thereof.
本発明による放射線触媒還元処理法の装置例を図１示す。６価クロムなどを含む水溶液中に少量の固体材料を添加し、キャプセル状の放射線源から放出されるガンマ線で外部照射、または溶液中に導入した放射性同位元素からのアルファ線、ベータ線で内部照射して、放射線触媒反応により６価クロムの還元反応を促進させて、３価ないしは４価クロムを固体またはイオンの状態で回収する。 FIG. 1 shows an example of an apparatus for a radiation catalytic reduction treatment method according to the present invention. Add a small amount of solid material in an aqueous solution containing hexavalent chromium, etc., and externally irradiate with gamma rays emitted from a capsule-like radiation source, or internally with alpha and beta rays from radioactive isotopes introduced into the solution Then, the reduction reaction of hexavalent chromium is promoted by a radiocatalytic reaction, and trivalent or tetravalent chromium is recovered in a solid or ionic state.
本発明は、放射線のエネルギーを固体材料が吸収し化学反応エネルギーに変換して、６価クロムなどの還元反応を促進する方法であり、後処理を要する還元剤や酸、アルカリを使用することなく、６価クロムの還元と３価ないしは４価クロムの回収を簡便かつ安価に実現することが可能となる。さらに、固体はそれ自体が壊れず、再利用可能であり、形状の自由度があり、かつ水溶液は脱気、pHなどの条件を選ばず、反応系が簡単である、などの利点がある。 The present invention is a method in which a solid material absorbs radiation energy and converts it into chemical reaction energy to promote a reduction reaction of hexavalent chromium, etc., without using a reducing agent, acid, or alkali that requires post-treatment. Further, reduction of hexavalent chromium and recovery of trivalent or tetravalent chromium can be realized easily and inexpensively. Further, the solid is not broken by itself, can be reused, has a degree of freedom in shape, and the aqueous solution has an advantage that the reaction system is simple regardless of conditions such as degassing and pH.
利用する放射線は、使用済み核燃料の再処理で取り出される放射性物質やその際に発生する高レベル廃液のガラス固化体からのガンマ線や、放射性同位元素からのアルファ線、ベータ線も対象としており、一般には利用されていない放射性廃棄物の資源化が可能となる。 The radiation used is also intended for gamma rays from radioactive materials extracted by reprocessing of spent nuclear fuel and vitrified solids of high-level waste, and alpha and beta rays from radioisotopes. Makes it possible to recycle unused radioactive waste.
本発明の処理対象である金属イオンは、４価セリウム、６価クロム、７価マンガン等があげられる。 Examples of the metal ion to be treated in the present invention include tetravalent cerium, hexavalent chromium, and heptavalent manganese.
（実施例１）
本発明の一具体例について説明する。重クロム酸イオンCr2O7 2-を含む希硫酸水溶液に、TiO2、γ-Al2O3、ZrO2などをそれぞれ単独に添加した。それらの溶液にガンマ線を照射して、６価クロムが還元される収量を測定した結果、単位エネルギーあたりの水の放射線分解による還元量と比較して、固体による還元量はそれぞれ100倍（TiO2）、280倍（γ-Al2O3）、70倍（ZrO2）程度の増大が見られた（図２）。これらの固体は還元反応では消費されず、いわゆる触媒として機能している。
（実施例２）
実施例１と同じ固体と６価クロムを含み、環境条件あるいは工業廃水の条件（pH 3-7）の水溶液にガンマ線照射して、照射後に溶液中の６価クロム濃度および全クロム量を分析し、固体表面のクロムの状態を分析した結果、水溶液のみの場合は６価クロムがほとんど還元しないのに対して、固体を添加することで６価クロムが顕著に還元する（図３）ことを明らかにするとともに、溶液中の６価クロムを環境への排出基準0.05 ppm（環境基本法）または0.5 ppm（水質汚濁防止法）以下まで減じ（表１）、４価あるいは３価クロムの酸化物に還元し、固化することがわかった。
Example 1
A specific example of the present invention will be described. TiO 2 , γ-Al 2 O 3 , ZrO 2 and the like were added individually to a dilute sulfuric acid aqueous solution containing the dichromate ion Cr 2 O 7 2- . As a result of measuring the yield of reduction of hexavalent chromium by irradiating these solutions with gamma rays, the amount of reduction by solids was 100 times that of reduction by radiolysis of water per unit energy (TiO 2 ), 280 times (γ-Al 2 O 3 ) and 70 times (ZrO 2 ) (Fig. 2). These solids are not consumed in the reduction reaction and function as so-called catalysts.
(Example 2)
Gamma rays were irradiated to an aqueous solution containing the same solid and hexavalent chromium as in Example 1 and environmental conditions or industrial wastewater conditions (pH 3-7), and the concentration of hexavalent chromium and the total chromium content in the solution were analyzed after irradiation. As a result of analyzing the state of chromium on the surface of the solid, it is clear that hexavalent chromium is remarkably reduced by adding solids, whereas hexavalent chromium is hardly reduced in the case of only an aqueous solution (FIG. 3). In addition, the hexavalent chromium in the solution is reduced to 0.05 ppm (Basic Environmental Law) or 0.5 ppm (Water Pollution Control Law) or below (Table 1) and reduced to tetravalent or trivalent chromium oxide. And found to solidify.
[発明の効果]
本発明は以下の特徴から、有利な効果を有する。
１）６価クロムの還元収量が非常に大きく、かつガンマ線は水溶液に対して高い透過能力を有しているため、高濃度６価クロム廃液をはじめとして、着色した固体あるいは溶液や、濁った溶液にも十分に適用可能である。
[The invention's effect]
The present invention has advantageous effects from the following features.
1) Since the reduction yield of hexavalent chromium is very large and gamma rays have a high permeability to aqueous solutions, colored solids or solutions such as high-concentration hexavalent chromium waste liquid, and turbid solutions It is also fully applicable to.
２）還元に必要な固体材料は触媒であり、固体はそれ自体が壊れず、回収可能であり半永久的に使用可能であり、経済性に優れている。
３）６価クロム処理に化学薬品を使用しないため、３価ないしは４価クロムの回収に後処理を必要とせず、高純度の３価ないしは４価クロムの回収が容易である。３価クロムはイオンとして３価クロムメッキに使用可能であり、固体としてはその形状の違いにより耐火レンガ、研磨剤、顔料（Cr2O3）、抵抗発熱体、高温用電極（LaCrO3）などの用途が考えられる。また、４価クロムは二酸化クロムCrO2として回収可能であり、強磁性材料として非常に優れた特徴を有する。さらに、３価ないしは４価クロムの固体は放射線触媒反応の固体材料としても利用できる。このように、有害な６価クロムの無害化と有用材料への転換が同時に実現可能となる。
2) The solid material necessary for the reduction is a catalyst, and the solid itself is not broken, can be recovered, can be used semipermanently, and is excellent in economic efficiency.
3) Since no chemicals are used for the hexavalent chromium treatment, no post-treatment is required for the recovery of trivalent or tetravalent chromium, and high purity trivalent or tetravalent chromium can be easily recovered. Trivalent chromium can be used as ions for trivalent chromium plating. As solid, refractory brick, abrasive, pigment (Cr 2 O 3 ), resistance heating element, high temperature electrode (LaCrO 3 ), etc. Can be used. Tetravalent chromium can be recovered as chromium dioxide CrO 2 and has very excellent characteristics as a ferromagnetic material. Further, a trivalent or tetravalent chromium solid can be used as a solid material for the radiocatalytic reaction. Thus, detoxification of harmful hexavalent chromium and conversion to useful materials can be realized at the same time.
４）利用する放射線は、使用済み核燃料の再処理で取り出される放射性物質やその際に発生する高レベル廃液のガラス固化体からのガンマ線や、放射性同位元素からのアルファ線、ベータ線も対象にしており、一般には利用されていない放射性廃棄物の資源化が可能となる。 4) The radiation to be used also covers gamma rays from radioactive materials extracted by reprocessing of spent nuclear fuel and high-level waste liquid vitrification, alpha rays and beta rays from radioactive isotopes. Therefore, it is possible to recycle radioactive waste that is not generally used.
Claims (6)
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| JP2010065261A (en) * | 2008-09-09 | 2010-03-25 | Japan Atomic Energy Agency | Method for recovering noble metal, method for producing functional material and method for treating strongly oxidizing metal ion-containing aqueous solution using this functional material |
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|---|---|---|---|---|
| JPS496765A (en) * | 1972-05-08 | 1974-01-21 |
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| JPS496765A (en) * | 1972-05-08 | 1974-01-21 |
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| JP2010065261A (en) * | 2008-09-09 | 2010-03-25 | Japan Atomic Energy Agency | Method for recovering noble metal, method for producing functional material and method for treating strongly oxidizing metal ion-containing aqueous solution using this functional material |
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