Method for preparing (NH4)2WS4

A technology of ammonium tetrathiotungstate and ammonium metatungstate, which is applied in the field of preparation of high-purity chemicals, and can solve the problems of large amount of sodium sulfide and phosphoric acid, failure to improve the treatment of hydrogen sulfide gas, etc.

Inactive Publication Date: 2004-12-29
BC P INC CHINA NAT PETROLEUM CORP +1
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Problems solved by technology

literature [3] This method has been improved, mainly reducing the consumption of sodium sulfide and phosphoric acid by half, shortening the reaction time to 11 hours, and increasing the yield of ammonium tetrathiotungstate (50-52%), but still not Can improve the treatment of highly toxic and foul-smelling hydrogen sulfide gas, the shortcomings of large amounts of sodium sulfide and phosphoric acid

Method used

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  • Method for preparing (NH4)2WS4
  • Method for preparing (NH4)2WS4
  • Method for preparing (NH4)2WS4

Examples

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Embodiment 1

[0014] A 1000ml four-necked bottle equipped with a stirrer, a reflux condenser and a thermometer was installed in a water bath, and 50g of ammonium metatungstate [(NH 4 ) 6 W 7 o 24 4H 2 O] Put the powder into a four-necked bottle, add 200ml of distilled water, and then add 60ml of concentrated ammonia water, stir and heat to 40-50°C to dissolve. Under stirring, 350 ml of ammonium sulfide solution with a sulfur content of 8% was added to the solution, the temperature was raised to 60-70° C., and the reaction was stirred for 1.0 hour to obtain a blood-red liquid. After the reaction, the reactant was cooled to room temperature and allowed to stand still for crystallization for 12 hours. Suction filter the liquid containing crystals with a Buchner funnel, wash with 1200ml of cold distilled water 3 times (400ml each time), and finally wash the crystals with 600ml of absolute ethanol 3 times (200ml each time), drain the solvent, and place at room temperature After drying for 2...

Embodiment 2

[0019]Install a 1000ml four-necked bottle equipped with a stirrer, reflux condenser and thermometer in a water bath, weigh 30g of tungsten trioxide powder into the four-necked bottle, add 200ml of distilled water, then add 60ml of concentrated ammonia water, stir and heat to 40 Dissolved at ~50°C. Under stirring, 230 ml of ammonium sulfide solution with a sulfur content of 8% was added to the solution, the temperature was raised to 60-70° C., and the reaction was stirred for 1.0 hour to obtain a blood-red liquid. After the reaction, the reactant was cooled to room temperature and allowed to stand still for crystallization for 10 hours. Suction filter the liquid containing crystals with a Buchner funnel, wash with 900ml of cold distilled water 3 times (300ml each time), and finally wash the crystals with 450ml of absolute ethanol 3 times (150ml each time), drain the solvent, and place at room temperature After drying for 24 hours, 27.3 g of dark red needle crystals can be obta...

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Abstract

The present invention relates to improved preparation process of high purity chemical. High purity ammonium tetrathiotungstate is prepared through the reaction between ammonium metatungstate or tungsten trioxide and ammonium sulfate solution. Preparing high purity ammonium tetrathiotungstate in the said process of the present invention has ammonium sulfate amount near the required stoichiometric amount, mild reaction condition, short reaction period, less waste exhaust, high product yield, high product purity, and no need of treating virulent and effluvial hydrogen sulfide gas.

Description

technical field [0001] The invention relates to a preparation method of ammonium tetrathiotungstate, which belongs to the improvement of the preparation method of high-purity chemicals. It is mainly through the use of ammonium metatungstate [(NH 4 ) 6 W 7 o 24 4H 2 O] or tungsten trioxide WO 3 with ammonium sulfide [(NH 4 ) 2 S] solution reaction method to prepare high-purity ammonium tetrathiotungstate [(NH 4 ) 2 WS 4 ]. Background technique [0002] Ammonium tetrathiotungstate [(NH 4 ) 2 WS 4 ] (English name: ammonium tetrathiotungstate, referred to as ATTT) has been widely used in the synthesis of tungsten, iron and sulfur atomic cluster compounds, the active center of biological nitrogenase [1] , is also the precursor of coal liquefaction and heavy oil hydrogenation catalysts, and can also be used as a raw material for the preparation of supported tungsten sulfide hydrogenation catalysts. The preparation method of tetrathioammonium tungstate reported in th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B17/98C01C1/00C01G41/00
Inventor 刘晨光柴永明赵会吉赵瑞玉殷长龙邢金仙方朝亮于建宁
Owner BC P INC CHINA NAT PETROLEUM CORP
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