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Method for preparing dithio-metal acid ammonium

A disulfide metal, metal technology, applied in non-metallic elements, chemical instruments and methods, sulfur compounds, etc., can solve the problems of complex preparation process, low product yield, long reaction time, etc., to achieve simple operation and reduce harm. , the effect of avoiding the influence of product purity and reaction yield

Active Publication Date: 2010-01-13
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage of this method is that the preparation process is relatively complicated, the reaction time is long, and the product yield is low.

Method used

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  • Method for preparing dithio-metal acid ammonium
  • Method for preparing dithio-metal acid ammonium
  • Method for preparing dithio-metal acid ammonium

Examples

Experimental program
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Embodiment 1

[0020] Pour 5g of industrial grade ammonium metatungstate (containing 83% tungsten trioxide) crystals into a conical beaker, then slowly add 35ml of 8wt% ammonium sulfide solution, at this time the color of the reaction solution will gradually change from blue to light yellow , pour all the ammonium sulfide solution into the beaker, stir at room temperature for 30 minutes, and finally let the reaction solution stand for 12 hours to obtain yellow crystals, filter and wash with deionized water and absolute ethanol three times respectively, vacuum at room temperature After drying, the final ammonium dithiotungstate crystal is obtained, and the yield is about 93% (calculated according to the tungsten content).

[0021] The XRD spectrogram of the product obtained in this embodiment is shown in figure 1 , XRF elemental analysis results are shown in Table 1.

[0022] From figure 1 It can be seen that the XRD spectrum of the product is completely consistent with the standard spectru...

Embodiment 2

[0026] Pour 8.3g of tungsten trioxide crystals into a conical beaker, and then slowly add 56ml of 10wt% ammonium sulfide solution. At this time, put the reaction solution in a water bath and heat up to 60°C. At this time, the color of the reaction solution will gradually change from blue to blue. After stirring for 10 minutes, the reaction solution was left to stand for 12 hours to obtain yellow crystals, which were filtered and washed three times with deionized water and absolute ethanol respectively, and vacuum-dried at room temperature to obtain the final thiooxytungstic acid Ammonium crystals, the yield is about 93% (calculated based on tungsten content).

Embodiment 3

[0028] Pour 12.36g of industrial-grade ammonium molybdate crystals into a conical beaker, and then slowly add 60ml of 8wt% ammonium sulfide solution. At this time, the color of the reaction solution will gradually change from blue to dark red. Pour all the ammonium sulfide solution into After being placed in the beaker, stir at room temperature for 30 minutes, and finally let the reaction solution stand for 12 hours to obtain blood-red crystals. After filtering, wash with deionized water and absolute ethanol three times respectively, and vacuum-dry at room temperature to obtain the final thioxo Ammonium molybdate crystals, the yield is about 93% (calculated based on molybdenum content).

[0029] The XRD spectrogram of the product obtained in this embodiment is shown in figure 2 , XRF elemental analysis results are shown in Table 2.

[0030] figure 2 It can be seen that the XRD spectrum of the product is completely consistent with the standard spectrum, and each peak type i...

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Abstract

The invention discloses a method for preparing dithio-metal acid ammonium, which comprises the following steps: adding ammonium sulfide water solution into metal acid ammonium and / or metal oxide, reacting the mixture, standing the mixture and filtering, washing and drying the mixture to obtain a product, wherein the metal is selected from one or more metals from group VIB, and the molar ratio of the sulfur to the metal is 2-2.1. The provided method has the characteristics of simple operation, high product yield and purity, little harm to environments and operators, and the like.

Description

technical field [0001] The invention relates to a preparation method of ammonium dithiometalate, in particular to a method for preparing high-purity ammonium dithiometalate through liquid-solid reaction. Background technique [0002] Transition metal sulfides have become a research hotspot in chemistry, solid state physics, and materials chemistry due to their special structural chemistry, electrical properties, and rich intercalation chemistry. Among them, thiometallates are widely used in the biological field, the preparation of enzymes and non-supported catalyst precursors. Among them, ammonium thiotungstate or ammonium thiomolybdate is an important class of thiometallates, after thermal decomposition, tungsten oxide or molybdenum oxide sulfide intermediates can be obtained. The phase transition of the process is of great significance, and it is also an important precursor for the preparation of highly active hydrogenation catalysts. [0003] U.S. Patent No. 4,604,278 d...

Claims

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Application Information

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IPC IPC(8): C01G1/00C01B17/98C01C1/00C01G41/00C01G39/00
Inventor 毕云飞曾双亲聂红李大东杨清河李洪宝
Owner CHINA PETROLEUM & CHEM CORP
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