DE1592254A1 - Process for the production of high purity molybdenum chloride, preferred molybdenum pentachloride - Google Patents

Description

Process for the production of high purity molybdenum chloride, preferably molybdenum pentachloride.

The invention relates to the production of high purity Molybdenum chloride, preferably molybdenum pentachloride, the is processed into high-purity molybdenum and / or high-purity molybdenum compounds.

There are procedures for purifying molybdenum compounds the plus sig liquid extraction, the sublimation of Molybdenum trioxide and the crystallization of molybdenum compounds known. These methods are used to manufacture high-purity connections very expensive, or do not lead to high-purity connections, in particular, the separation of tungsten is difficult.

Processes are purely for the purification of molybdenum halides known as distillation and sublimation. When distilling or subliming molybdenum chloride, mainly molybdenum pentachloride are elements such as iron, aluminum, but mainly Tungsten, due to the. The boiling or sublimation points of their chlorides are only slightly depleted.

The Irfindung is based on the task of molybdenum compounds of the highest purity by distillation or To produce sublimation of molybdenum chloride, in particular molybdenum pentachloride, such elements as for example, metal, aluminum, titanium, silicon, niobium, tantalum and mainly tungsten can be removed.

009849 / U80

According to the invention the object is achieved in that for the production of high purity molybdenum chloride by distillation or sublimation of molybdenum pentachloride this before and / or during the distillation or sublimation oxygen, water, oxygen- or water-containing Gases, oxygen-containing compounds that react easily with metal chlorides, their reaction products are volatile or easily separable, or no additional contamination of the Molybdenum compound mean, such as molybdenum oxides, molybdenum oxide chlorides, chlorine oxides, sulfur oxides, sulfur oxide chlorides, nitrogen oxides, carbon dioxide, phosgene and the like can be added.

This turns some metal chlorides into less volatile ones Oxides, others are converted into more volatile oxide chlorides and are light from molybdenum pentachloride to separate.

JU's cleaning agents are particularly oxygen, air, water, molybdenum oxides and oxide chlorides proven. The addition of oxygen must be at least as high be dimensioned so that the compounds to be removed are converted quantitatively into oxide or oxychloride can, an excess promoting the separation.

The oxygen-containing gases or compounds are before and / or during the distillation or sublimation, admixed with the molybdenum chloride or introduced into the evaporator part. From the molybdenum pentachloride prepared in this way the volatile oxide chlorides, in particular Tungsten oxychloride, distilled off or sublimed off and precipitated in a cooling chamber, the volatile oxides remain in the swamp back. In particular, the separation of the tungsten

009849 / U80

by heating the molybdenum chloride, preferably can be carried out in reflux, with or without carrier gas.

The advantage of this method over the previously known Process for producing high purity liolybdenum pentachloride is the convenient and fast technology, the variable throughput and the almost free use of material with very little loss of carcass of molybdenum pentachloride.

The invention is explained in more detail below using two exemplary embodiments.

1st embodiment '.

50-0 g of molybdenum pentachloride was added before the distillation a cm- * of water added by dropping, the Ghlorid distilled off at 280 ° 0, with the template was kept at 200 ° 0.

Trace elements

Fe

Al 'Si W

2, embodiment '

Through 500 g of molybdenum pentachloride was air passed in a moderate stream for 5 minutes and that Chloride distilled off after some time. Distillation at 300 ° C, receiver 250 ° C.

before later ppm ppm 60 6th 20th <0.3 50 <0.3 20th /1

009849 / U80

nte - 4 - 1592254 ■ learn before later ppm ppm Fe 20th 2 Al 13th <0.3 Si 90 <0.3 W. irersbeisOJ 100 <1 export Relate LeIe focus on a

multiple determination, the cleaning effects can through an Xblonnendistillation can be increased at will.

009849 / U80

Claims (2)

Claims 1 »Process for the production of high purity molybdenum chloride by distillation or sublimation of molybdenum pentachloride, characterized in that the molybdenum chloride before and / or during the Distillation or sublimation Oxygen, water, gases containing oxygen or water, oxygen-containing compounds that react easily with metal chlorides, dease. Reaction products volatile or are easily detachable, or no additional contamination of the MölybdSnverbinöung mean, such as molybdenum oxides, molybdenum oxide chlorides, chlorine oxides, sulfur oxides, sulfur oxide chlorides, Nitrogen oxides, carbon dioxide, phosgene and the like, or mixtures of these, are added 2. The method according to claim 1, characterized in that that the oxygen-containing agents entered, initiated and / or started in the molybdenum chloride be guided past the surface 3 · Process according to claims 1 and 2, characterized in that the tungsten in particular is made from molybdenum chloride as tungsten oxychloride. Heat is expelled with or without carrier gas. 009849/14 * 0