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Preparation method of anhydrous magnesium chloride

A technology of anhydrous magnesium chloride and magnesium chloride, applied in the direction of magnesium chloride, chemical instruments and methods, magnesium halide, etc., can solve the problems that chlorine cannot be recycled, doubtful about safety, difficult to electrolyze raw materials, etc., and achieve low production cost, high quality, Product quality is stable and reliable

Pending Publication Date: 2022-02-08
SHENZHEN MAXCHEMTECH
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  • Claims
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AI Technical Summary

Problems solved by technology

However, these dehydration methods have their own shortcomings. For example, the gas-protected heating dehydration method requires a large amount of hydrogen chloride gas, which consumes a lot of energy and causes serious corrosion of equipment at high temperatures; organic solvent distillation and molecular sieve dehydration methods have organic reagents and magnesium chloride. Magnesium chloride products contain a large amount of carbon and magnesium oxide, which is difficult to be used as raw materials for electrolysis; magnesium chloride double salt and complex decomposition dehydration method mainly synthesizes magnesium chloride hexaammoniate, and then decomposes to prepare anhydrous magnesium chloride. Ammonia mixes with air at high temperature, there is a potential explosion hazard, and its safety is doubtful
In addition, if magnesium chloride hydrate is used as the starting material for the synthesis of magnesium chloride hexaammonia, the chlorine produced by electrolysis of magnesium cannot be recycled, and if the hydroxide or oxide of magnesium is used as the raw material, strong corrosion is required in the preparation process. Hydrochloric acid also uses ammonia, which increases the harm to the environment

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  • Preparation method of anhydrous magnesium chloride
  • Preparation method of anhydrous magnesium chloride
  • Preparation method of anhydrous magnesium chloride

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preparation example Construction

[0027] Most of the existing technological routes for preparing anhydrous magnesium chloride are researched around the problem of magnesium chloride dehydration itself, and in essence they all directly remove water molecules from magnesium chloride. Only the magnesium chloride double salt and complex decomposition dehydration method is to convert magnesium chloride into a coordination compound first, and then carry out high-temperature deamination. Inventor explores the preparation process of anhydrous magnesium chloride, finds that can react in anhydrous organic solvent by anhydrous magnesium formate or magnesium chloride hexaammoniate and hydrogen chloride gas, generates anhydrous magnesium chloride and formic acid, removes anhydrous organic solvent and Formic acid, or remove ammonium chloride, can obtain high-quality anhydrous magnesium chloride, and prepare anhydrous magnesium chloride compared with directly removing the crystal water in the magnesium chloride with crystal w...

Embodiment 1

[0048] Such as figure 1 and 2 Shown, with potassium carnallite (KCl MgCl 2 ·6H 2 O) be initial raw material, the preparation method of anhydrous magnesium chloride comprises the steps:

[0049] S0, potassium carnallite is ground into fine powder, after passing through a 100-mesh vibrating sieve, it is separated into potassium chloride (crystal precipitation) and magnesium chloride hexahydrate (dissolved in ethanol) in an ethanol-water solvent, and potassium chloride is removed by filtration , to obtain magnesium chloride hexahydrate; wherein, the removed potassium chloride has a purity>99%, step S4 can be carried out, and ammonium chloride and potassium sulfate can be reacted in step S4 to generate ammonium chloride and potassium sulfate, step S7 can also be carried out, and it can also be used as a product to the outside world Sold, and magnesium chloride hexahydrate carries out step S1;

[0050] S1, magnesium chloride hexahydrate is metathesis-reacted with ammonium forma...

Embodiment 2

[0064]The dried magnesium chloride hexaammoniate powder is put into 1L of anhydrous methanol, reacts with anhydrous hydrogen chloride in a closed container at 0-30°C and 0-3Mpa pressure to synthesize anhydrous magnesium chloride, and obtains by-product ammonium chloride (ammonium chloride micro Soluble in methanol, most of it precipitates out). After the ammonium chloride is removed by filtration, the solvent is distilled off under reduced pressure to obtain anhydrous magnesium chloride, further vacuum-dried under the protection of nitrogen, the solvent is fully removed, and then the temperature is raised to above 340°C to fully volatilize the residual ammonium chloride, namely About 95g of high-purity anhydrous magnesium chloride can be obtained, with a purity of >99.5%. Among them, after the filtered ammonium chloride is dried under negative pressure to remove the residual solvent, about 320 g is recovered in the form of by-products, which can be directly sold or recycled as...

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Abstract

The invention discloses a preparation method of anhydrous magnesium chloride, which comprises the following steps: reacting anhydrous magnesium formate powder with anhydrous hydrogen chloride gas in an anhydrous organic solvent to generate anhydrous magnesium chloride and formic acid, and removing the anhydrous organic solvent and formic acid to obtain anhydrous magnesium chloride, wherein the anhydrous magnesium formate powder is suspended in the anhydrous organic solvent, and the anhydrous hydrogen chloride gas is dissolved in the anhydrous organic solvent. The anhydrous magnesium chloride with extremely high quality can be obtained by the method disclosed by the invention.

Description

technical field [0001] The invention relates to the field of preparation of inorganic salts, in particular to a preparation method of anhydrous magnesium chloride. Background technique [0002] Anhydrous magnesium chloride is widely used, in addition to being used for pharmaceutical intermediates, catalyst carriers, desiccants, etc., it is mainly used as the basic raw material for electrolytic magnesium. In the prior art, the Pidgeon method is mainly used to prepare metallic magnesium. The main raw material of this method is high-grade dolomite, and there are disadvantages such as high energy consumption and environmental pollution in the process of preparing metallic magnesium. Compared with the Pidgeon method, the electrolysis method has the advantages of low energy consumption (the latter is about 2.86 times that of the former), continuous production, high degree of mechanization and automation, and high production indicators. [0003] One of the key problems in the prep...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01F5/32C01D5/12C01D5/00
CPCC01F5/32C01D5/12C01D5/00C01P2006/82
Inventor 谈宇清袁正明苏杭
Owner SHENZHEN MAXCHEMTECH
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