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A kind of ammonium carnallite dehydration material and the method for using it to prepare magnesium electrolyte melt

A technology of ammonium carnallite and electrolyte, which is applied in the preparation of chlorides, chemical instruments and methods, preparation/separation of ammonia, etc. It can solve the problems of single dehydration protection mechanism, low heat transfer efficiency, and hindrance to large-scale industrial production.

Active Publication Date: 2021-11-16
河北大有镁业有限责任公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] In summary, the above-mentioned methods for preparing high-purity electrolytic magnesium melts have the following common problems: (1) The dehydration protection mechanism is single, resulting in high content of hydrolyzed products
Due to the lack of research on the decomposition mechanism and kinetics of ammonium chloride, none of the current methods can solve this problem; (3) A heat transfer method with low heat transfer efficiency
The ammonium carnallite dehydrated material should not introduce a large amount of air during the high-temperature heating deammonization process. The above-mentioned method only relies on the heat conduction mode of the high-temperature chloride melt for heat transfer, and the heat transfer efficiency is low, which hinders the large-scale industrial production of the process.

Method used

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  • A kind of ammonium carnallite dehydration material and the method for using it to prepare magnesium electrolyte melt
  • A kind of ammonium carnallite dehydration material and the method for using it to prepare magnesium electrolyte melt
  • A kind of ammonium carnallite dehydration material and the method for using it to prepare magnesium electrolyte melt

Examples

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Effect test

Embodiment 1

[0062] 100g of potassium chloride was used as raw material to prepare potassium chloride melt at 800°C, and 30g of ammonium carnallite dehydrated material 1.2NH 4 Cl•MgCl 2 •0.5H 2 O (particle size distribution: >1.43mm material accounts for 20wt.%, 0.9-1.43mm material accounts for 20wt.%, 0.3-0.9mm material accounts for 50wt.%, 0.1-0.3mm material accounts for 10wt.%) spread on the above chlorinated above the potassium melt. Wherein, the ratio of the height of the ammonium carnallite dehydrated material column to its diameter is 0.5, and the ratio of the diameter of the ammonium carnallite dehydrated material column to the diameter of the chloride melt material is 0.5. The ammonium carnallite dehydrated material is first heated at 250°C for 0.5 hours, then heated at 400°C for 0.1 hour, then heated at 550°C for 0.5 hour, and finally heated at 700°C for 1.0 hour, and keep the ammonia and gas above the dehydrated material during the heating process. The sum of the partial pres...

Embodiment 2

[0066] Prepare sodium chloride melt with 100g sodium chloride at 800°C, and 35g ammonium carnallite dehydrated material 1.0NH 4 Cl•MgCl 2 •0.6H 2 O (particle size distribution: >1.43mm material accounts for 18wt.%, 0.9-1.43mm material accounts for 25wt.%, 0.3-0.9mm material accounts for 52wt.%, 0.1-0.3mm material accounts for 5wt.%) spread on the above chloride above the melt. Wherein, the ratio of the height of the ammonium carnallite dehydrated material column to its diameter is 1.0, and the ratio of the diameter of the ammonium carnallite dehydrated material column to the diameter of the chloride melt material is 0.3. The ammonium carnallite dehydrated material is first heated at 280°C for 1.5 hours, then heated at 370°C for 2.0 hours, then heated at 530°C for 1.0 hour, and finally heated at 650°C for 0.1 hour, and keep the ammonia and gas above the dehydrated material during the heating process. The sum of the partial pressures of hydrogen chloride is 30kpa, and a high-...

Embodiment 3

[0070] Prepare a chloride melt with 55g potassium chloride and 45g sodium chloride at 750°C, and 40g ammonium carnallite dehydrated material 1.4NH 4 Cl•MgCl 2 • 0H 2 O (particle size distribution: >1.43mm material accounts for 30wt.%, 0.9-1.43mm material accounts for 17wt.%, 0.3-0.9mm material accounts for 51wt.%, 0.1-0.3mm material accounts for 2wt.%) spread on the above chloride above the melt. Wherein, the ratio of the height of the ammonium carnallite dehydrated material column to its diameter is 10.0, and the ratio of the diameter of the ammonium carnallite dehydrated material column to the diameter of the chloride melt material is 0.7. The ammonium carnallite dehydrated material is first heated at 300°C for 0.1 hour, then heated at 350°C for 0.05 hour, then heated at 500°C for 0.2 hour, and finally heated at 720°C for 2.0 hours, and keep the ammonia and gas above the dehydrated material during the heating process. The sum of the partial pressures of hydrogen chloride ...

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Abstract

The invention discloses an ammonium carnallite dehydrated material n NH 4 Cl•MgCl 2 • m h 2 O and a method for preparing a magnesium electrolyte melt using the same, the preparation method comprising the following steps: (a) using alkali metal chloride as a raw material to prepare a chloride melt; (b) placing the ammonium carnallite dehydrated material in the chloride melt On the body, and form a solid material column; (c) heating the ammonium carnallite dehydrated material to form a magnesium electrolyte melt. The ammonium carnallite dehydrated material described in the present invention is easy to dehydrate during the heating process and can form a certain material structure at different temperatures. Combined with the preparation method of the magnesium electrolyte melt described in the present invention, the moisture in the dehydrated material can be dehydrated efficiently. It can remove and control the hydrolyzate, organic matter and other impurities in the material to an extremely low level, which can meet the electrolysis requirements of the most advanced multipolar electrolyzer.

Description

technical field [0001] The invention relates to the technical field of preparation of inorganic materials, in particular to an ammonium carnallite dehydrated material and a method for preparing a magnesium electrolyte melt based on the ammonium carnallite dehydrated material. Background technique [0002] my country is rich in liquid magnesium resources. For example, during the production of potassium fertilizer in Qinghai Salt Lake, magnesium chloride hexahydrate (MgCl) in waste brine discharged every year 2 ·6H 2 O) content reaches 24-36 million tons. A large number of magnesium chloride hexahydrate resources have nowhere to pile up and form a "magnesium hazard" in the local area. Its opening and utilization are very urgent, and it has become a hot spot that government departments and all walks of life pay attention to. Dehydration of magnesium chloride hexahydrate to prepare high-purity magnesium electrolyte melt (or anhydrous magnesium chloride), and then prepare metal...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C25C3/04C01C1/02C01B7/05
CPCC01B7/055C01C1/026C25C3/04
Inventor 卢旭晨张志敏闫岩王天华薛立强李金沙
Owner 河北大有镁业有限责任公司