Method for preparing (NH4)2MoS4

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

Inactive Publication Date: 2004-12-29
BC P INC CHINA NAT PETROLEUM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Documents have improved this method, mainly reducing the consumption of sodium sulfide and phosphoric acid by half, shortening the reaction time to 7 hours, and the productive rate of ammonium tetrathiom

Method used

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  • Method for preparing (NH4)2MoS4
  • Method for preparing (NH4)2MoS4
  • Method for preparing (NH4)2MoS4

Examples

Experimental program
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Embodiment 1

[0014] The 1000ml four-necked bottle that stirrer, reflux condenser and thermometer are equipped with is installed in water bath, takes by weighing 50g ammonium paramolybdate [(NH 4 ) 6 Mo 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, 450 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 cold distilled water 3 times (400ml each time), and finally wash the crystals 3 times with 600ml absolute ethanol (200ml each time), drain the solvent and place at room temperature After dryin...

Embodiment 2

[0019]Install a 1000ml four-necked bottle equipped with a stirrer, a reflux condenser and a thermometer in a water bath, weigh 30g of molybdenum 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, 360 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, 50.3 g of dark red needle crystals can b...

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Abstract

The present invention relates to improved preparation process of high purity chemical. High purity ammonium tetrathiomolybdate is prepared through the reaction between ammonium para-molybdate or molybdenum trioxide and ammonium sulfate solution. Preparing high purity ammonium tetrathiomolybdate 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 tetrathiomolybdate, which belongs to the improvement of the preparation method of high-purity chemicals. It is mainly through the use of ammonium paramolybdate [(NH 4 ) 6 Mo 7 o 24 4H 2 O] or molybdenum trioxide MoO 3 with ammonium sulfide [(NH 4 ) 2 S] solution reaction method to prepare high-purity ammonium tetrathiomolybdate [(NH 4 ) 2 MoS 4 ]. Background technique [0002] Ammonium tetrathiomolybdate [(NH 4 ) 2 MoS 4 ] (English name: ammonium tetrathiomolybdate, referred to as ATTM) is an intermediate for the preparation of high-efficiency solid lubricant molybdenum disulfide, and has been widely used in the synthesis of biological nitrogenase active center-molybdenum-iron-sulfur cluster compounds [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 molybdenum sulfide hydr...

Claims

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Application Information

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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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