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Method for preparing anhydrous manganese chloride under anhydrous reaction conditions

An anhydrous manganese chloride, anhydrous technology, applied in manganese halide and other directions, can solve the problems of high energy consumption, difficult to achieve special chemical products and pharmaceutical production, etc., to achieve good safety, high product yield, simple operation Effect

Active Publication Date: 2015-01-28
JIANGXI SILINCO
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Using the traditional drying process, the drying process consumes a lot of energy, and there are side reactions such as oxidation and hydrolysis, resulting in impurities such as basic manganese chloride and manganese dioxide in the anhydrous manganese chloride product, and it is difficult for the anhydrous manganese chloride product to reach Some special chemical products and pharmaceutical production requirements

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0012] The reaction was carried out in an enamel reactor. The reactor is equipped with a temperature control and temperature measuring device with heating and cooling functions, a stirring device, a solid feeding device, a liquid feeding device, a gas exhaust valve, and a special mass flow meter for hydrogen chloride. Under the protection of nitrogen, 276g of absolute ethanol (6mol) solvent and 55g (1.0mol) of metal manganese powder with an average particle diameter of about 5 microns are put into the reactor, and the gas feed pipe of the reactor is below the liquid level of the solvent. The gaseous hydrogen chloride accurately measured by the mass flow meter is added to the solvent through the feeding pipe. The total amount of hydrogen chloride added is 109.5g (3mol). After reaching room temperature, filter to obtain anhydrous manganese chloride ethanol solution. Stir and distill the anhydrous manganese chloride ethanol solution in the hydrogen chloride stream to recover the...

Embodiment 2

[0014] Under the protection of helium, put 128g of anhydrous methanol solvent (4 mol) and 55g (1.0mol) of metal manganese powder with an average particle size of about 15 microns into the reactor, and the gas feeding pipe of the reactor is below the liquid level of the solvent The gaseous hydrogen chloride accurately measured by the mass flow meter is added to the solvent through the feeding pipe. The total amount of hydrogen chloride added is 146g (4mol). After reaching room temperature, filter to obtain anhydrous manganese chloride methanol solution. Stir and distill the anhydrous manganese chloride methanol solution in the hydrogen chloride stream to recover the solvent, and obtain the manganese chloride crystalline methanol complex, then put the manganese chloride crystalline methanol complex into a closed desiccator, and heat it to 120°C under agitation , decompressed to 1000Pa, dried for 2 hours to remove methanol to obtain anhydrous manganese chloride with a content of ...

Embodiment 3

[0016] Under the protection of carbon dioxide gas, put 240g of anhydrous propanol (4mol), 240g of anhydrous isopropanol (4mol), and 55g (1.0mol) of metal manganese powder with an average particle size of about 10 microns into the reactor. The gas feeding pipe is below the liquid level of the solvent. The gaseous hydrogen chloride accurately measured by the mass flow meter is added to the solvent through the feeding pipe. The total amount of hydrogen chloride added is 73g (2mol). Gaseous hydrogen chloride until the metal manganese powder is completely dissolved, and after reaching room temperature, filter to obtain anhydrous manganese chloride alcohol solution. Stir and distill the anhydrous manganese chloride alcohol solution in the hydrogen chloride stream to reclaim propanol and isopropanol solvent, and obtain the manganese chloride crystalline propanol complex and the manganese chloride crystalline isopropanol complex, and then the manganese chloride crystalline propanol Pu...

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Abstract

The invention discloses a method for preparing anhydrous manganese chloride under anhydrous reaction conditions, which comprises the following steps: (1) mixing metal manganese powder and solvent alcohol, introducing gas hydrogen chloride into the solvent alcohol in a metering mode to react with the metal manganese powder until the manganese powder is completely dissolved, and filtering to obtain an anhydrous manganese chloride alcohol solution; (2) stirring and distilling under normal pressure in a hydrogen chloride atmosphere to recover the solvent and obtain a manganese chloride crystal alcohol complex; and putting the manganese chloride crystal alcohol complex into a closed dryer, heating in a stirring state, and dealcoholizing under reduced pressure to obtain the anhydrous manganese chloride. The method has the characteristics of simple technique, simple after-treatment, high safety and high product yield, and does not have the basic manganese chloride and manganese peroxide impurities in the conventional preparation method. The anhydrous manganese chloride is obtained under anhydrous conditions, so the method has the advantages of high product yield, high safety and the like, and is simple to operate and suitable for industrial production.

Description

technical field [0001] The invention belongs to the technical field of preparation methods of anhydrous metal chlorides, and in particular relates to a method for preparing anhydrous manganese chloride by reacting metal manganese powder and hydrogen chloride in an alcohol solvent system under anhydrous conditions. Background technique [0002] Anhydrous manganese chloride is widely used in medicine, organic chlorination catalyst, paint drier, analytical reagent, magnesium-manganese alloy, aluminum-manganese alloy, high-purity metal manganese powder, dye and pigment manufacturing, brown-black brick production and dry battery manufacturing etc. It is also the key raw material for the production of gasoline antiknock agent methenyl manganese compounds. In recent years, with the rapid development of the market for high-efficiency gasoline antiknock agent cyanocene-manganese compounds—methylcyclopentadiene manganese tricarbonyl, the market demand for anhydrous manganese chloride ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G45/06
CPCC01G45/06
Inventor 廖维林许招会廖婧熊斌林春花
Owner JIANGXI SILINCO
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