Degussa Aktiengesellschaft

Erich Splett

Ludwig Lange

Walter Hinrichs

Friedrich Bittner

Lutz Hippe

Herbert Hovestadt

Kurt A Ruppert

Herbert Hovestadt, Deceased

Methods for the preparation of lower sodium polysulfides such as sodium disulfide from higher sodium polysulfides and sodium. To this end, either molten sodium polysulfide placed in a receiver is reacted with sodium in a stoichiometric ratio corresponding to the desired product under vigorous agitation and under protective gas or the higher polysulfide and the sodium are dosed into a polysulfide melt in a receiver under the same conditions either alternatively or simultaneously. In all instances, the dosing of the sodium is set so that the reaction mixture remains capable of being agitated and the agitation is continued until the desired product composition has been achieved.

Method of preparing lower sodium polysulfides from higher sodium

A method of preparing sodium monosulfide by means of reacting a sodium polysulfide with sodium under protective gas, the sodium polysulfide is placed in a first stage in a finely distributed, solid state in a receiver, preheated to temperatures of 100.degree.-150.degree. C., liquid sodium is gradually added in the required amount to the material in the receiver under intensive mixing, whereby the temperature of the reaction mixture is maintained at 120.degree.-250.degree. C. and in a second stage the formed initial product is allowed to continue to react, or postreact under continuation of the mixing at 250.degree.-480.degree. C., until a Na.sub.2 S content of at least 95% by weight has been attained.

Method of preparing Na.sub.2 S (II)

In a method of preparing sodium monosulfide by means of reacting sodium and sulfur under protective gas, the entire sodium determined for reaction is placed in a receiver in a first stage, preheated to temperatures of 100.degree.-150.degree. C., sulfur is gradually added in the required amount of the material in the receiver under intensive mixing, whereby the temperature of the reaction mixture is maintained at 120.degree.-250.degree. C., and in a second stage the formed initial product is allowed to react under continuation of the mixing at 250.degree.-480.degree. C., until a Na.sub.2 S content of at least 95% by weight has been attained.

Method of preparing NA2S (I)

A method of preparing sodium monosulfide by means of reacting sodium and sulfur under protective gas, wherein sodium monosulfide is placed in a first stage in a receiver in a finely distributed, solid state, the initial material is preheated to 120.degree.-150.degree. C. and sulfur and sodium are alternately added in the required amount ratio under intensive mixing, whereby the temperature of the reation mixture is maintained at 120.degree.-250.degree. C., and in a second stage the formed initial product is allowed to continue to react or postreact under continuation of the mixing at 250.degree.-480.degree. C., until a Na.sub.2 S content of at least 95% by weight has been attained.

Method of preparing Na.sub.2 S (III)

A process for converting the filtration residue of crude sodium produced by fusion electrolysis into a sodium alcoholate with a low NaOH content. The residue first is intensively and continuously mixed for 2-5 hours at 300.degree.-600.degree. C. and then is added with stirring to the particular alcohol, possibly with heat added. The alcoholate solution so formed is filtered and the alcoholate may be obtained from the filtrate by distilling off the solvent.

Process for working up the filtration residue of crude sodium prepared

A process is described for creating the flow properties to filtration residues from sodium production. These viscous-to-hard filter residues can be changed into a thin-fluid consistency by intensively agitating them under an inert gas for 2-6 hours at temperatures between 300.degree. and 600.degree. C.

Process for creating the flow properties to sodium-production filter

There is described a process for the production of pure sodium polysulfides directly from the elements sodium and sulfur. For this purpose, the sodium and the sulfur under a protective gas and in a stoichiometrical ratio corresponding to the desired polysulfide are alternatingly dosed into a previously present melt of a polysulfide with vigorous stirring, the dosing being in portions such that upon introduction of the sodium the reaction mixture remains in the condition of a stirrable suspension and upon introduction of the sulfur this is completely reacted to a polysulfide of the desired or higher sulfur content.

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Huerth-Berrenrath, Germany

Erich Splett