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Preparation method of low-valence halide of variable-valence metal

A technology of variable valence metals and halides, applied in the field of material science, can solve the problems of low concentration and large dosage, and achieve the effects of simple operation, low equipment requirements and strong practicability

Inactive Publication Date: 2020-04-21
INST OF HIGH ENERGY PHYSICS CHINESE ACADEMY OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] However, the traditional preparation of SmI 2 The biggest shortcoming of the method existence is: what obtain is the organic solution of samarium iodide, concentration is low (the THF solution that is generally 0.1mol / mL), but, for most reactions, SmI 2 The dosage is larger

Method used

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  • Preparation method of low-valence halide of variable-valence metal
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  • Preparation method of low-valence halide of variable-valence metal

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preparation example Construction

[0048] The preparation process of the electrolyte is as follows: First, the raw material reagents are transferred to a glove box with water and oxygen content less than 10ppm for storage; high-purity anhydrous AlI is prepared according to the molar ratio of 1:1 3 -KI (purity greater than 99%), after mixing evenly, put it in a corundum crucible, heat up to 300 ° C; then use a two-electrode system for electrolysis, the anode and the anode are both made of aluminum rods, and after constant current electrolysis for 10 hours, use 200 mesh molybdenum Net filter to remove suspended impurities, that is.

[0049] The preparation method of other molten salt electrolytes is the same as above.

Embodiment 1

[0051] 50g AlI 3 -KI molten salt (AlI3 and KI molar ratio is 1:1) is placed in the alumina crucible, and the temperature control is 280 ℃; figure 1 It is a schematic diagram of electrolysis, using high-purity metal samarium (purity not less than 99%) as the anode, aluminum wire as the cathode (purity not less than 99.999%); the control cell voltage is 2.0V, electrolysis for 2 hours, and the electrolysis current is maintained at about 60mA About; After the electrolysis, filter with a 200-mesh metal molybdenum filter to obtain a blue precipitate; vacuum distill the blue precipitate at 500°C for 1 hour to obtain 0.766g such as figure 2 The black-green samarium dichloride solid is shown.

[0052] Such as image 3 Shown is a photo of the prepared samarium dichloride dissolved in tetrahydrofuran, which is dark blue.

[0053] Simultaneously, adopt weighing method, compare the weight loss of anode and the quality that obtains product, record the recovery rate of samarium diiodide ...

Embodiment 2

[0055] This embodiment provides a kind of method for preparing samarium diiodide, and the difference with embodiment 1 is only, change high-purity metal samarium into samarium aluminum alloy, electrolytic current has increased 3 times, and this method prepares samarium diiodide The recovery rate was 89%.

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Abstract

The invention provides a preparation method of a low-valence halide of a variable-valence metal. The preparation method comprises the steps that a high-purity simple substance of variable-valence metal or an aluminum alloy of the variable-valence metal serves as an anode, AlX3-MX is used as a molten salt electrolyte, the molten salt electrolyte is heated and molten, then constant-temperature electrolysis is conducted so as to obtain the low-valence halide of the variable-valence metal, wherein X is one of I<->, Br<-> and Cl<->, and M is one of K<+>, Na<+> and Li<+>. A preparation method provided by the invention has universality and can be used for preparing the low-valence halide of most transition metal elements in the periodic table of elements; the problems of complex preparation and high cost of the low-valence halide in the prior art are solved, and the preparation rate of the low-valence halide can be increased by controlling reaction conditions; the low-valence halide of metalor alloy can be directly prepared through anodic oxidation, only the electrolytic voltage needs to be controlled in the anodic dissolution process, and the purity can be improved through reduced pressure distillation. The method has advantages of simple operation, mild reaction condition, low equipment requirement, good economy and high practicability.

Description

technical field [0001] The invention belongs to the technical field of material science and relates to the preparation technology of catalytic materials, in particular to a preparation method of low-valent halides of variable-valence metals. Background technique [0002] The subvalent halides of variable valence metals have a wide range of applications in the field of catalysis (general organic chemistry, sequential reactions, organic phase change chemistry, catalytic chemistry). [0003] Samarium diiodide (SmI), a low-valent halide of rare earth metals 2 ) as an example, SmI 2 As a Kagan reagent, it is a very important one-electron reducing agent. It has many applications in organic synthesis, especially in reductive coupling reactions involving free radical processes. It has mild reaction conditions and many excellent selectivities. Features. [0004] However, the traditional preparation of SmI 2 The biggest shortcoming of the method existence is: what obtain is the or...

Claims

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Application Information

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IPC IPC(8): C25B1/24B01J27/08B01J27/10
CPCB01J27/08B01J27/10C25B1/24
Inventor 石伟群钟宇科刘雅兰
Owner INST OF HIGH ENERGY PHYSICS CHINESE ACADEMY OF SCI
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