CN106834686A - In a kind of gallium production procedure except uranium technique - Google Patents
In a kind of gallium production procedure except uranium technique Download PDFInfo
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- 229910052733 gallium Inorganic materials 0.000 title claims abstract description 104
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 title claims abstract description 102
- 229910052770 Uranium Inorganic materials 0.000 title claims abstract description 48
- JFALSRSLKYAFGM-UHFFFAOYSA-N uranium(0) Chemical compound [U] JFALSRSLKYAFGM-UHFFFAOYSA-N 0.000 title claims abstract description 48
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 26
- 238000000034 method Methods 0.000 title claims abstract description 25
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 49
- 239000007787 solid Substances 0.000 claims abstract description 44
- 239000007788 liquid Substances 0.000 claims abstract description 35
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 26
- 238000003756 stirring Methods 0.000 claims abstract description 24
- 238000000926 separation method Methods 0.000 claims abstract description 19
- 238000005868 electrolysis reaction Methods 0.000 claims abstract description 9
- 238000001556 precipitation Methods 0.000 claims abstract description 9
- 229910052979 sodium sulfide Inorganic materials 0.000 claims abstract description 9
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical compound [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000003795 desorption Methods 0.000 claims abstract description 8
- 239000011790 ferrous sulphate Substances 0.000 claims abstract description 6
- 235000003891 ferrous sulphate Nutrition 0.000 claims abstract description 6
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims abstract description 6
- 229910000359 iron(II) sulfate Inorganic materials 0.000 claims abstract description 6
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000000843 powder Substances 0.000 claims abstract description 5
- 230000003068 static effect Effects 0.000 claims description 3
- 238000011084 recovery Methods 0.000 abstract description 13
- 230000002285 radioactive effect Effects 0.000 abstract description 3
- 238000004090 dissolution Methods 0.000 abstract description 2
- 239000010802 sludge Substances 0.000 abstract 3
- 239000000243 solution Substances 0.000 description 35
- 239000003792 electrolyte Substances 0.000 description 3
- -1 gallium ions Chemical class 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 229920005989 resin Polymers 0.000 description 3
- 239000011347 resin Substances 0.000 description 3
- 239000012670 alkaline solution Substances 0.000 description 2
- 150000001450 anions Chemical class 0.000 description 2
- 229920001429 chelating resin Polymers 0.000 description 2
- 239000008139 complexing agent Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- 238000004131 Bayer process Methods 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000010828 elution Methods 0.000 description 1
- IMBKASBLAKCLEM-UHFFFAOYSA-L ferrous ammonium sulfate (anhydrous) Chemical compound [NH4+].[NH4+].[Fe+2].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O IMBKASBLAKCLEM-UHFFFAOYSA-L 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 125000005289 uranyl group Chemical group 0.000 description 1
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Abstract
本发明属于放射性元素回收技术领域，具体涉及一种镓生产流程中的除铀工艺。本发明包括以下步骤：向镓的硫酸脱附液中加入硫酸亚铁盐或还原铁粉，搅拌溶解后用氢氧化钠调节溶液至碱性；加入硫化钠，搅拌溶解并静置沉淀；固液分离后回收液体部分，固体部分即为含铀尾渣；向回收的液体中加入浓硫酸调节溶液至酸性；固液分离后得到固体镓泥；向镓泥中加入氢氧化钠溶液得到镓泥溶解液；电解得到粗镓。本发明解决了现有镓生产流程中的除铀工艺镓回收率较低的技术问题，显著改善了镓产品的纯度及质量，镓的回收率得到有效提高。
The invention belongs to the technical field of recovery of radioactive elements, and in particular relates to a process for removing uranium in a gallium production process. The invention comprises the following steps: adding ferrous sulfate or reduced iron powder to the sulfuric acid desorption liquid of gallium, stirring and dissolving, and adjusting the solution to alkalinity with sodium hydroxide; adding sodium sulfide, stirring and dissolving and standing for precipitation; solid-liquid Recover the liquid part after separation, and the solid part is uranium-containing tailings; add concentrated sulfuric acid to the recovered liquid to adjust the solution to acidity; obtain solid gallium sludge after solid-liquid separation; add sodium hydroxide solution to the gallium sludge to obtain gallium sludge dissolution liquid; electrolysis to get crude gallium. The invention solves the technical problem of low gallium recovery rate in the uranium removal process in the existing gallium production process, significantly improves the purity and quality of gallium products, and effectively improves the gallium recovery rate.
Description
技术领域technical field
本发明属于放射性元素回收技术领域，具体涉及一种镓生产流程中的除铀工艺。The invention belongs to the technical field of recovery of radioactive elements, and in particular relates to a process for removing uranium in a gallium production process.
背景技术Background technique
目前，镓的生产主要是采用镓特效螯合树脂对拜耳法产铝的过程液进行选择性吸附，镓特效螯合树脂可有效回收碱性溶液中的镓离子。如图1所示，吸附饱和的树脂经硫酸洗脱、中和分离、沉淀溶解、除杂等系列工艺获得相应电解镓电解液，经电解后获得镓产品。At present, the production of gallium mainly uses gallium special-effect chelating resin to selectively adsorb the process liquid of aluminum produced by Bayer process. Gallium special-effect chelating resin can effectively recover gallium ions in alkaline solution. As shown in Figure 1, the saturated resin undergoes a series of processes such as sulfuric acid elution, neutralization and separation, precipitation and dissolution, and impurity removal to obtain the corresponding electrolytic gallium electrolyte, and the gallium product is obtained after electrolysis.
但是，上述工艺中镓特效树脂对放射性核素铀也具有一定的吸附作用。在强碱性溶液中铀酰离子可形成络阴离子，铀酰络阴离子与偏镓酸根离子部分性质相似，在镓的生产流程中铀的走向与镓的走向趋于一致，只有少部分铀在除杂工段得到分离，大部分铀同镓离子一同被镓特效树脂吸附。However, the gallium special-effect resin in the above process also has a certain adsorption effect on the radionuclide uranium. In strong alkaline solution, uranyl ions can form complex anions. The properties of uranyl complex anions and metagallate ions are partially similar. In the production process of gallium, the direction of uranium tends to be consistent with that of gallium, and only a small part of uranium is removed. The miscellaneous section is separated, and most of the uranium and gallium ions are adsorbed by the gallium special effect resin together.
存在于镓电解液中的杂质铀对镓的生产主要具有以下两方面的危害：一方面，铀的电解电势与镓接近，其存在严重影响镓的电解，使得镓产品中混杂铀杂质，影响镓产品的纯度及质量；另一方面，铀是一种放射性核素，若不经过有效去除，经电解后得到镓产品中铀的含量可达数个百分点的含量，影响从业人员的健康。同时，放射性核素铀也是一种宝贵的资源，当铀的含量超过一定值时有必要进行合理的回收利用，当铀的含量低于一定值时可忽略其回收意义。The impurity uranium in the gallium electrolyte mainly has the following two hazards to the production of gallium: on the one hand, the electrolytic potential of uranium is close to that of gallium, and its existence seriously affects the electrolysis of gallium, making the uranium impurity mixed in the gallium product, affecting the production of gallium. The purity and quality of the product; on the other hand, uranium is a radioactive nuclide. If it is not effectively removed, the content of uranium in the gallium product obtained after electrolysis can reach several percentage points, which will affect the health of employees. At the same time, radionuclide uranium is also a precious resource. When the content of uranium exceeds a certain value, it is necessary to carry out reasonable recycling. When the content of uranium is lower than a certain value, its recycling significance can be ignored.
现有技术中，镓生产流程中除铀工艺中采用的做法是在电解前加入络合剂将铀络合，但是该技术方案导致镓的回收率较低。因此，有必要对镓生产过程中的放射性核素铀进行分离，分离工艺的难点在于体系中铀的含量低、基体组分复杂；镓的生产工艺流程复杂，任何工段的变化均会影响整个流程。In the prior art, the method adopted in the uranium removal process in the gallium production process is to add a complexing agent to complex the uranium before electrolysis, but this technical solution leads to a low recovery rate of gallium. Therefore, it is necessary to separate the radionuclide uranium in the gallium production process. The difficulty of the separation process lies in the low content of uranium in the system and complex matrix components; the production process of gallium is complicated, and any change in the process section will affect the entire process .
发明内容Contents of the invention
本发明需要解决的技术问题为：现有镓生产流程中的除铀工艺采用电解前加入络合剂将铀络合的技术方案，导致镓回收率较低。The technical problem to be solved in the present invention is: the uranium removal process in the existing gallium production process adopts the technical scheme of adding a complexing agent to complex the uranium before electrolysis, resulting in a low recovery rate of gallium.
本发明的技术方案如下所述：Technical scheme of the present invention is as follows:
一种镓生产流程中的除铀工艺，包括以下步骤：A process for removing uranium in a gallium production process, comprising the following steps:
步骤一：向镓的硫酸脱附液中加入固体硫酸亚铁盐或还原铁粉，充分搅拌溶解后用固体氢氧化钠调节溶液至pH＝10～13，再加入硫化钠固体，充分搅拌溶解，静置沉淀；Step 1: adding solid ferrous sulfate or reduced iron powder to the sulfuric acid desorption solution of gallium, fully stirring and dissolving, adjusting the solution to pH=10-13 with solid sodium hydroxide, then adding solid sodium sulfide, fully stirring and dissolving, static precipitation;
步骤二：固液分离后回收液体部分，固体部分即为含铀尾渣；Step 2: After solid-liquid separation, the liquid part is recovered, and the solid part is uranium-containing tailings;
步骤三：向回收的液体中缓慢加入浓硫酸，调节溶液至pH＝5～9；Step 3: Slowly add concentrated sulfuric acid to the recovered liquid to adjust the solution to pH=5-9;
步骤四：固液分离后得到固体镓泥；Step 4: obtaining solid gallium mud after solid-liquid separation;
步骤五：向镓泥中加入饱和氢氧化钠溶液或氢氧化钠固体溶解镓泥，得到镓泥溶解液；Step 5: adding saturated sodium hydroxide solution or solid sodium hydroxide to the gallium mud to dissolve the gallium mud to obtain a gallium mud solution;
步骤六：电解，得到粗镓。Step 6: electrolysis to obtain crude gallium.
本发明的有益效果为：The beneficial effects of the present invention are:
(1)本发明的一种镓生产流程中的除铀工艺，经除铀分离后镓的生产得以顺利进行，显著改善了镓产品的纯度及质量；(1) The uranium removal process in a gallium production process of the present invention, the gallium production can be carried out smoothly after the uranium removal and separation, and the purity and quality of the gallium product are significantly improved;
(2)本发明的一种镓生产流程中的除铀工艺，镓的回收率得到有效提高；(2) In the uranium removal process in a gallium production process of the present invention, the recovery rate of gallium is effectively improved;
(3)本发明的一种镓生产流程中的除铀工艺，有效降低了现有镓生产流程电解液中存在的硫化钠消耗电能的缺点；(3) The uranium removal process in a gallium production process of the present invention effectively reduces the shortcoming of the sodium sulfide consumption of electric energy that exists in the electrolyte of the existing gallium production process;
(4)本发明的一种镓生产流程中的除铀工艺，避免了镓生产流程中放射性核素对从业人员的危害。(4) The uranium removal process in the gallium production process of the present invention avoids the harm of radionuclides to practitioners in the gallium production process.
附图说明Description of drawings
图1为现有技术中镓生产流程；Fig. 1 is the production process of gallium in the prior art;
图2为本发明的镓生产流程。Fig. 2 is the gallium production process of the present invention.
具体实施方式detailed description
下面结合附图和实施例对本发明的一种镓生产流程中的除铀工艺进行详细说明。The uranium removal process in a gallium production process of the present invention will be described in detail below with reference to the accompanying drawings and embodiments.
本发明的一种镓生产流程中的除铀工艺，包括以下步骤：A process for removing uranium in a gallium production flow process of the present invention comprises the following steps:
步骤一：向镓的硫酸脱附液中加入固体硫酸亚铁盐或还原铁粉，充分搅拌溶解后用固体氢氧化钠调节溶液至pH＝10～13，再加入适量硫化钠固体，充分搅拌溶解，静置沉淀；Step 1: Add solid ferrous sulfate or reduced iron powder to the sulfuric acid desorption solution of gallium, fully stir and dissolve, adjust the solution to pH=10-13 with solid sodium hydroxide, then add an appropriate amount of sodium sulfide solid, fully stir to dissolve , static precipitation;
步骤二：固液分离后回收液体部分，固体部分即为含铀尾渣；Step 2: After solid-liquid separation, the liquid part is recovered, and the solid part is uranium-containing tailings;
步骤三：向回收的液体中缓慢加入适量浓硫酸，调节溶液至pH＝5～9；Step 3: Slowly add an appropriate amount of concentrated sulfuric acid to the recovered liquid to adjust the solution to pH=5-9;
步骤四：固液分离后得到固体镓泥；Step 4: obtaining solid gallium mud after solid-liquid separation;
步骤五：向镓泥中加入饱和氢氧化钠溶液或氢氧化钠固体溶解镓泥，得到镓泥溶解液；Step 5: adding saturated sodium hydroxide solution or solid sodium hydroxide to the gallium mud to dissolve the gallium mud to obtain a gallium mud solution;
步骤六：电解，得到粗镓。Step 6: electrolysis to obtain crude gallium.
实施例1Example 1
步骤一：向铀含量约为12μg/mL的100m3镓的硫酸脱附液中加入固体硫酸亚铁15.0kg，充分搅拌溶解后用固体氢氧化钠调节至pH＝10.0，再加入3.0kg硫化钠固体，充分搅拌溶解，静置沉淀；Step 1: Add 15.0kg of solid ferrous sulfate to the 100m gallium sulfuric acid desorption solution with a uranium content of about 12μg/mL, stir and dissolve it, adjust the pH to 10.0 with solid sodium hydroxide, and then add 3.0kg of sodium sulfide Solid, stir well to dissolve, let stand to settle;
步骤二：固液分离后收集液体部分，固体部分即为含铀尾渣，溶液中镓的回收率>94％，铀的去除率＞95％；Step 2: Collect the liquid part after solid-liquid separation, the solid part is uranium-containing tailings, the recovery rate of gallium in the solution is >94%, and the removal rate of uranium is >95%;
步骤三：向收集的液体中边搅拌边缓慢加入适量浓硫酸，调节溶液至pH＝9.0，静置得到白色固体沉淀，镓的回收率＞95％；Step 3: Slowly add an appropriate amount of concentrated sulfuric acid to the collected liquid while stirring, adjust the solution to pH = 9.0, and leave to stand to obtain white solid precipitation, and the recovery rate of gallium is > 95%;
步骤四：固液分离后得到固体镓泥；Step 4: obtaining solid gallium mud after solid-liquid separation;
步骤五：向镓泥中加入饱和氢氧化钠溶液充分搅拌，直至镓泥溶解，得到镓泥溶解液；Step 5: Add saturated sodium hydroxide solution to the gallium mud and stir well until the gallium mud dissolves to obtain a gallium mud solution;
步骤六：电解镓泥溶解液，得粗镓。Step 6: Electrolyzing gallium mud solution to obtain crude gallium.
实施实例2Implementation Example 2
步骤一：向铀含量约为18μg/mL的100m3镓的硫酸脱附液中加入固体硫酸亚铁10.0kg，充分搅拌溶解后用固体氢氧化钠调节至pH＝11.0，再加入6.0kg硫化钠固体，充分搅拌溶解，静置沉淀；Step 1: Add 10.0kg of solid ferrous sulfate to the 100m gallium sulfuric acid desorption solution with a uranium content of about 18μg/mL, stir and dissolve it, adjust the pH to 11.0 with solid sodium hydroxide, and then add 6.0kg of sodium sulfide Solid, stir well to dissolve, let stand to settle;
步骤二：固液分离后收集液体部分，固体部分即为含铀尾渣，溶液中镓的回收率>96％，铀的去除率＞99％；Step 2: Collect the liquid part after solid-liquid separation, the solid part is uranium-containing tailings, the recovery rate of gallium in the solution is >96%, and the removal rate of uranium is >99%;
步骤三：向收集的液体中边搅拌边缓慢加入适量浓硫酸，调节溶液至pH＝8.0，静置得到白色固体沉淀，镓的回收率＞99％；Step 3: Slowly add an appropriate amount of concentrated sulfuric acid to the collected liquid while stirring, adjust the solution to pH = 8.0, and let it stand to obtain white solid precipitation, and the recovery rate of gallium is >99%;
步骤四：固液分离后得到固体镓泥；Step 4: obtaining solid gallium mud after solid-liquid separation;
步骤五：向镓泥中加入饱和氢氧化钠溶液充分搅拌，直至镓泥溶解，得到镓泥溶解液；Step 5: Add saturated sodium hydroxide solution to the gallium mud and stir well until the gallium mud dissolves to obtain a gallium mud solution;
步骤六：电解镓泥溶解液，得粗镓。Step 6: Electrolyzing gallium mud solution to obtain crude gallium.
实施实例3Implementation Example 3
步骤一：向1铀含量约为6μg/mL的00m3镓的硫酸脱附液中加入固体硫酸亚铁铵3.0kg，充分搅拌溶解后用固体氢氧化钠调节至pH＝12.0，再加入5.0kg硫化钠固体，充分搅拌溶解，静置沉淀；Step 1: Add 3.0 kg of solid ferrous ammonium sulfate to the sulfuric acid desorption solution of 100 m3 gallium with a uranium content of about 6 μg/mL, stir and dissolve it, adjust the pH to 12.0 with solid sodium hydroxide, and then add 5.0 kg Sodium sulfide solid, stir well to dissolve, let stand to settle;
步骤二：固液分离后收集液体部分，固体部分即为含铀尾渣，溶液中镓的回收率>99％，铀的去除率＞96％；Step 2: Collect the liquid part after solid-liquid separation, the solid part is uranium-containing tailings, the recovery rate of gallium in the solution is >99%, and the removal rate of uranium is >96%;
步骤三：向收集的液体中边搅拌边缓慢加入适量浓硫酸，调节溶液至pH＝6.5，静置得到白色固体沉淀；Step 3: Slowly add an appropriate amount of concentrated sulfuric acid to the collected liquid while stirring, adjust the solution to pH=6.5, and let stand to obtain a white solid precipitation;
步骤四：固液分离后得到固体镓泥；Step 4: obtaining solid gallium mud after solid-liquid separation;
步骤五：向镓泥中加入饱和氢氧化钠溶液充分搅拌，直至镓泥溶解，得到镓泥溶解液；Step 5: Add saturated sodium hydroxide solution to the gallium mud and stir well until the gallium mud dissolves to obtain a gallium mud solution;
步骤六：电解镓泥溶解液，得粗镓。Step 6: Electrolyzing gallium mud solution to obtain crude gallium.
实施实例4Implementation Example 4
步骤一：向铀含量约为26μg/mL的100m3镓的硫酸脱附液中加入固体还原铁粉3.0kg，充分搅拌溶解后用固体氢氧化钠调节至pH＝13.0，再加入7.0kg硫化钠固体，充分搅拌溶解，静置沉淀；Step 1: Add 3.0kg of solid reduced iron powder to the 100m gallium sulfuric acid desorption solution with a uranium content of about 26μg/mL, stir and dissolve it, adjust the pH to 13.0 with solid sodium hydroxide, and then add 7.0kg of sodium sulfide Solid, stir well to dissolve, let stand to settle;
步骤二：固液分离后收集液体部分，固体部分即为含铀尾渣，溶液中镓的回收率>99％，铀的去除率＞95％；Step 2: Collect the liquid part after solid-liquid separation, the solid part is uranium-containing tailings, the recovery rate of gallium in the solution is >99%, and the removal rate of uranium is >95%;
步骤三：向收集的液体中边搅拌边缓慢加入适量浓硫酸，调节溶液至pH＝5.0，静置得到白色固体沉淀；Step 3: Slowly add an appropriate amount of concentrated sulfuric acid to the collected liquid while stirring, adjust the solution to pH=5.0, and let stand to obtain white solid precipitation;
步骤四：固液分离后得到固体镓泥；Step 4: obtaining solid gallium mud after solid-liquid separation;
步骤五：向镓泥中加入饱和氢氧化钠溶液充分搅拌，直至镓泥溶解，得到镓泥溶解液；Step 5: Add saturated sodium hydroxide solution to the gallium mud and stir well until the gallium mud dissolves to obtain a gallium mud solution;
步骤六：电解镓泥溶解液，得粗镓。Step 6: Electrolyzing gallium mud solution to obtain crude gallium.
Claims (2)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201510885233.9A CN106834686B (en) | 2015-12-04 | 2015-12-04 | Uranium technique is removed in a kind of gallium production procedure |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2780519A (en) * | 1950-12-21 | 1957-02-05 | Kaufman David | Recovery of uranium from ores |
| JPS5817130B2 (en) * | 1980-04-02 | 1983-04-05 | 理化学研究所 | Manufacturing method of ultra-high purity alumina |
| CN102527493A (en) * | 2010-12-15 | 2012-07-04 | 核工业北京地质研究院 | Uranium and beryllium separating technology for ore containing uranium and beryllium |
| CN102741433A (en) * | 2010-02-02 | 2012-10-17 | 奥图泰有限公司 | Extraction process |
| CN102747225A (en) * | 2012-07-10 | 2012-10-24 | 中南大学 | Method for comprehensively recycling copper, selenium and uranium from stone coal extraction vanadic acid immersion liquid |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2780519A (en) * | 1950-12-21 | 1957-02-05 | Kaufman David | Recovery of uranium from ores |
| JPS5817130B2 (en) * | 1980-04-02 | 1983-04-05 | 理化学研究所 | Manufacturing method of ultra-high purity alumina |
| CN102741433A (en) * | 2010-02-02 | 2012-10-17 | 奥图泰有限公司 | Extraction process |
| CN102527493A (en) * | 2010-12-15 | 2012-07-04 | 核工业北京地质研究院 | Uranium and beryllium separating technology for ore containing uranium and beryllium |
| CN102747225A (en) * | 2012-07-10 | 2012-10-24 | 中南大学 | Method for comprehensively recycling copper, selenium and uranium from stone coal extraction vanadic acid immersion liquid |
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