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Method for preparing anhydrous manganese chloride

An anhydrous manganese chloride, manganese powder technology, applied in manganese halide and other directions, can solve the problems of difficult to achieve, large energy consumption, etc., and achieve the effects of good safety, simple process, ideal product yield and purity

Active Publication Date: 2015-01-21
JIANGXI SILINCO
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the traditional drying process consumes a lot of energy during the drying process, and there are side reactions such as oxidation and hydrolysis, resulting in anhydrous manganese chloride products containing a large amount of impurities such as basic manganese chloride and manganese dioxide, and anhydrous chlorine It is difficult for manganese products to meet the requirements of some special chemical products and pharmaceutical production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] The reaction is carried out in an enamel reaction kettle, which is equipped with a temperature control and temperature measurement device with heating and cooling functions, a stirring device, a solid feeding device, a liquid feeding device, a liquid feeding metering tank and a gas exhaust valve. Under the protection of nitrogen, 276g of absolute ethanol (6mol) and 55g (1.0mol) of metal manganese powder with an average particle diameter of 5 microns are put into the reactor, and then 141.5ml (2.0mol) of acetyl chloride is added dropwise to the reactor. The reaction temperature was maintained at 30° C. until the metal manganese powder was completely dissolved, and the mixed solution was filtered with neutral filter paper to obtain an anhydrous manganese chloride ethanol solution. Under the state of stirring, distill the anhydrous manganese chloride ethanol solution under normal pressure to reclaim ethanol and ethyl acetate solvent to obtain the anhydrous manganese chlorid...

Embodiment 2

[0015] Under the protection of helium, put 128g of methanol (4mol) and 55g (1.0mol) of metal manganese powder with an average particle size of 15 microns into the reactor, and then add 277.5g (3.0mol) of propionyl chloride dropwise to the reactor, The reaction temperature was maintained at 10°C until the metal manganese powder was completely dissolved, and the mixed solution was filtered to obtain anhydrous manganese chloride methanol solution. Distill the anhydrous manganese chloride methanol solution under the stirring state to reclaim methanol and methyl propionate solvent to obtain the anhydrous manganese chloride methanol crystal complex, then put the anhydrous manganese chloride crystal methanol complex into a closed desiccator, Heating to 150°C under stirring, depressurizing to 1000Pa, drying for 6 hours to remove methanol to obtain anhydrous manganese chloride with a content of 99.2%, and the yield of anhydrous manganese chloride based on metal manganese powder is 99%. ...

Embodiment 3

[0017] Under the protection of carbon dioxide gas, put 360g of propanol (6mol), 360g of isopropanol (6mol), and 55g (1.0mol) of metal manganese powder with an average particle size of 10 microns into the reactor, and then dropwise add 106 g (1.0 mol) of isobutyryl chloride, the reaction temperature was maintained at 60°C until the metal manganese powder was completely dissolved, and the mixed solution was filtered to obtain anhydrous manganese chloride alcohol solution. Atmospheric pressure distillation anhydrous manganese chloride alcohol solution reclaims propanol, isopropanol, isopropyl isobutyrate, isopropyl isobutyrate solvent to obtain anhydrous manganese chloride propanol crystal complex, and then anhydrous Put the manganese chloride crystalline propanol complex in a closed desiccator, heat it to 180°C under agitation, reduce the pressure to 100Pa, and dry it for 4 hours to remove the propanol to obtain anhydrous manganese chloride with a content of 99.1%. The anhydrous...

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Abstract

The invention discloses a method for preparing anhydrous manganese chloride. The method comprises the following steps: (1) mixing metal manganese powder and solvent alcohol, dropwise adding fatty acyl chloride to react with the metal manganese powder, thereby obtaining an anhydrous manganese chloride alcohol liquid; and (2) stirring and distilling to recover the solvent at normal pressure, obtaining an anhydrous manganese chloride crystallization alcohol complex, adding the complex into a closed dryer, dealcoholizing under reduced pressure, thereby preparing the anhydrous manganese chloride. The method disclosed by the invention is simple and convenient in process, simple in after-treatment, high in safety and high in product yield, and alkali type manganese chloride and manganese dioxide impurities in the conventional preparation method are avoided. The prepared anhydrous manganese chloride has the advantages of ideal product yield and purity, simplicity in operation and safety, and the product meets the requirements of special chemical products and medical production and is suitable for industrial production.

Description

technical field [0001] The invention belongs to the technical field of anhydrous metal chloride preparation, and in particular relates to a method for preparing anhydrous manganese chloride by reacting metal manganese powder and fatty acid chloride in an alcohol solvent system under anhydrous conditions. Background technique [0002] Anhydrous manganese chloride is a basic chemical raw material with a wide range of uses. It is mainly used as an organic chlorination catalyst, a paint drier, and an industrial raw material in the fields of non-ferrous metal welding and ceramics. It is also the key raw material of methanocene manganese gasoline antiknock agent. With the further increase of the localization scale of gasoline antiknock agents in my country. At present, the domestic demand for high-purity anhydrous manganese chloride continues to rise, resulting in a shortage of high-purity anhydrous manganese chloride. [0003] At present, there are three main methods for produc...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G45/06
CPCC01G45/06
Inventor 廖维林许招会廖婧涂媛鸿夏剑辉
Owner JIANGXI SILINCO
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