Ammonium Trithiotungstate Preparing Method

Ammonium trithiothiotungstate [(NH₄)₂WOS₃] is an important thiometallic ammonium salt. After thermal decomposition, transition metal chalcogenide tungsten disulfide WS₂ can be obtained. At the activity center of biological nitrogenase, the synthesis of tungsten iron sulfur cluster compounds, semiconductors, superconductors, photochemical solar cells, storage batteries, lubricants and electrochemical reactions. Chemical sensors, nanomaterials, supercapacitors, new generation transistors, hydrogen storage materials and electrode materials have good applications.

Ammonium trithiotungstate reacts with ammonium sulfide solution by tungstate or tungsten trioxide. Ammonia gas produced in the reaction process is discharged from the reaction solution by vacuum pumping or by filling inert gas into the reaction solution, which promotes the reaction equilibrium to move towards the product ammonium trithiotungstate and adds appropriate amount to the reaction solution. Ammonium salt promotes the production of ammonium thiotungstate three and produces high purity three ammonium thiotungstate. The reaction is shown in the following figure:

4 451 kg ammonium sulfide solution with 8% sulphur content was added to the synthesis kettle with mechanical stirring, and then 1000 kg ammonium metatungstate was added to it. Nitrogen gas was bubbled in the reaction process, heated to 60 C by oil bath, stirred for 1 hour, then 572 kg ammonium acetate was added, crystallized for 2 hours, then drained and filtered. Cold distilled water (3 *10 000 mL) and ethanol (3 *10 000 mL) washed crystals three times, then dried at room temperature for 12 hours, 1220 kg yellow acicular crystals were obtained with a yield of 99% (calculated as ammonium metatungstate).

The reaction of tungstate or tungsten trioxide with ammonium sulfide solution was carried out. The ammonia produced during the reaction was discharged from the reaction solution by vacuum or by pumping nitrogen or inert gas into the reaction solution. The reaction equilibrium was promoted to move towards the product ammonium trithiotungstate, and the appropriate amount of ammonium salt was added to the reaction solution. To promote the production of ammonium thiotungstate three, high purity of three ammonium thiotungstate was prepared. This method can produce high purity ammonium trithiothiotungstate products from gram to ton with high efficiency. It is easy to realize large-scale industrial production and has a very high industrial application prospect.

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