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Method for preparing anhydrous magnesium chloride for electrolyzing magnesium

A technology of anhydrous magnesium chloride and electrolytic magnesium, which is applied in the direction of magnesium chloride and magnesium halide, can solve the problems of industrialization difficulties and low ammonium utilization rate, and achieve the effects of cost reduction, low cost, and simple preparation and purification

Inactive Publication Date: 2011-08-10
INST OF PROCESS ENG CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But because the utilization rate of ammonium in this process is not high yet (70%), the material still contains MgO (1%) after deammonization, and the sublimation and decomposition of ammonium chloride in ammonium carnallite decomposition process can produce HCl and NH 3 and other corrosive gases, etc., which brings certain difficulties to the realization of industrialization
Therefore, this method has not yet been used in production

Method used

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  • Method for preparing anhydrous magnesium chloride for electrolyzing magnesium
  • Method for preparing anhydrous magnesium chloride for electrolyzing magnesium
  • Method for preparing anhydrous magnesium chloride for electrolyzing magnesium

Examples

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Embodiment 1

[0039] See figure 1 and figure 2 .

[0040] 1) Take 560 grams of triethanolamine and add it to the reaction crystallization kettle, control the temperature of the reaction kettle to 30°C, and slowly add 380.54 grams of industrial hydrochloric acid dropwise to the reaction crystallization kettle while stirring; the reaction time is 2 hours later , the crystal slurry is filtered, and the obtained solid is [HTEA]Cl ionic liquid crude product;

[0041] 2) Drying the crude [HTEA]Cl ionic liquid obtained in step 1) in a drying oven at 50°C for 8 hours to obtain the [HTEA]Cl ionic liquid;

[0042] 3) Add 203.3 grams of MgCl to the reaction crystallization kettle 2 ·6H 2 O, slowly heat up to 100°C, add 3.6 grams of water, stir to make it fully dissolved, then take 185.69 grams of [HTEA]Cl ionic liquid obtained in step 2) and add it to the reaction crystallization kettle, stir and dissolve to form a homogeneous phase, and then naturally cool to room temperature , the obtained cry...

Embodiment 2

[0046] See figure 1 and figure 2 .

[0047] 1) Take 560 grams of triethanolamine and add it to the reaction crystallization kettle, control the temperature of the reaction kettle to be 10°C, and slowly add 360.54 grams of hydrochloric acid dropwise to the reaction crystallization kettle while stirring; after the reaction time is 2 hours, The crystal slurry is filtered, and the obtained solid is [HTEA]Cl ionic liquid crude product;

[0048] 2) The crude [HTEA]Cl ionic liquid obtained in step 1) was washed twice with absolute ethanol, and then dried in a drying oven at 60°C for 5 hours to obtain [HTEA]Cl ionic liquid with a purity of 98.5%;

[0049] 3) Add 203.3 grams of MgCl to the reaction crystallization kettle 2 ·6H 2 O, slowly heat up to 100°C, add 3.6 grams of water, stir to make it fully dissolved, then take 185.69 grams of the [HTEA]Cl ionic liquid obtained in step 2) and add it to the reaction crystallization kettle, stir and dissolve to form a homogeneous phase, t...

Embodiment 3

[0053] See figure 1 and figure 2 .

[0054] 1) Add 82 grams of imidazole into the reaction crystallization kettle, control the temperature of the reaction kettle to 40°C, and slowly add 105.66 grams of hydrochloric acid dropwise into the reaction crystallization kettle while stirring; after the reaction time is 1 hour, the crystal slurry Filtration, the obtained solid is [HIM]Cl ionic liquid crude product;

[0055] 2) The crude [HIM]Cl ionic liquid obtained in step 1) was washed twice with absolute ethanol, and dried in a drying oven at 40°C for 10 hours to obtain [HIM]Cl ionic liquid with a purity of 99.0%;

[0056] 3) Add 203.3 grams of MgCl to the reaction crystallization kettle 2 ·6H 2 O, slowly warming up to 90°C, then adding 118.5 grams of [HIM]Cl ionic liquid obtained in step 2) into the reaction crystallization kettle, adding 1.8 grams of deionized water, stirring and dissolving into a homogeneous phase, and then naturally cooling to room temperature, the obtained...

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Abstract

The invention relates to a method for preparing anhydrous magnesium chloride for electrolyzing magnesium. The method comprises the following steps of: synthetizing ionic liquid with properties of ammonia and hydrogen chloride by using triethanolamine, imidazole or pyridine as raw materials, wherein the molar ratio of the synthetized ionic liquid to bischofite is 1:1 and the molar ratio of water to the ionic liquid is in the range of 0.1:1 to 0.2:1; heating a reaction kettle to the temperature of 90 to 100 DEG C with stirring until the ionic liquid is dissolved into a homogeneous phase; cooling the homogeneous phase into the room temperature to obtain crystals; drying the crystals for 6 to 12 hours at the temperature of 90 to 100 DEG C to obtain complex salt of magnesium triethanolamine chloride hydrate, complex salt of magnesium imidazole chloride hydrate or complex salt of magnesium pyridine chloride hydrate; and carrying out pyrolysis on the complex salt in a reactor heated by a solar heat storage medium to remove crystal water and the ionic liquid so as to obtain the anhydrous magnesium chloride. By the method, the energy consumption of preparing the anhydrous magnesium chloride is greatly reduced; no corrosive gas is generated; and the ionic liquid is recycled. The anhydrous magnesium chloride prepared by the method has the magnesium utilization rate of over 98.5 percent and the magnesium oxide content of less than 0.5 percent, so that the requirement for preparing magnesium by electrolysis is met.

Description

technical field [0001] The invention relates to a method for preparing anhydrous magnesium chloride, in particular to a method for preparing an ionic liquid by using triethanolamine, imidazole or pyridine and hydrochloric acid as raw materials, then forming a double salt with the ionic liquid and bischofite, and storing heat through solar energy A method for preparing anhydrous magnesium chloride for electrolytic magnesium by carrying out double salt dehydration and deionized liquid in a medium-heated reactor. Background technique [0002] Magnesium resources are abundant in salt lakes in my country, but due to the limitations of regional economy and technology, the comprehensive utilization of resources in salt lakes is still low, and it is still a single development. For example, the development of salt lake resources in Qinghai is mainly based on the production of potassium fertilizer, and 8 to 10 tons of magnesium chloride are produced by-product per 1 ton of potassium c...

Claims

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Application Information

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IPC IPC(8): C25C3/04C01F5/32
Inventor 李志宝王均凤
Owner INST OF PROCESS ENG CHINESE ACAD OF SCI
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