Method for preparing molybdenum pentachloride

A technology of molybdenum pentachloride and carbon tetrachloride, applied in the direction of molybdenum halide, etc., can solve the problems of high toxicity and strong corrosion of chlorine gas, difficulty in ensuring safety, high energy consumption in production, etc., and achieve single product phase structure and high production efficiency. The effect of low cost and high production efficiency

Inactive Publication Date: 2011-04-20
CENT IRON & STEEL RES INST +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Using metal molybdenum (powder or bar) as raw material has high cost; high-temperature reaction produces high energy consumption; at the same time, chlorine gas is highly toxic and corrosive, and it is difficult to guarantee the safety due to leakage during the production process, and will cause environmental pollution

Method used

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  • Method for preparing molybdenum pentachloride
  • Method for preparing molybdenum pentachloride

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] 10 g of molybdenum trioxide and 37.5 ml of dehydrated carbon tetrachloride (mass ratio 1:6) were put into a round-bottomed stainless steel reaction bottle for mixing, and the reaction bottle was degassed and then the valve was closed for sealing. Then submerge the entire reaction bottle in an oil bath and heat it to 150° C., keep it for 12 hours, and take it out after cooling. At this time, the reaction solution changed from colorless to brown-red, and black needle-like crystals were precipitated. Open reaction bottle valve and emit reaction gas, reaction solution is poured in evaporator, remove carbon tetrachloride by evaporation and promptly obtain black crystal, the phase structure analysis that carries out through X-ray diffraction confirms that this black crystal is molybdenum pentachloride (see attached figure 1 ). The product weighed 8.2 g, and the yield was 43%.

Embodiment 2

[0018] 10 g of molybdenum trioxide and 30 ml of dehydrated carbon tetrachloride (mass ratio 1:5) were put into a round-bottomed stainless steel reaction bottle for mixing, and the reaction bottle was degassed and then the valve was closed for sealing. Then all the reaction bottle was submerged in an oil bath and heated to 240° C., kept for 1 hour, and then taken out after cooling. At this time, the reaction solution changed from colorless to brown-red, and black needle-like crystals were precipitated. Open the valve of the reaction bottle to release the reaction gas, pour the reaction solution into the evaporator, remove carbon tetrachloride by evaporation to obtain 11.8 g of molybdenum pentachloride black crystals, and the product yield is 62%. Phase structure analysis result is the same as embodiment 1.

Embodiment 3

[0020] 10 g of molybdenum trioxide and 25 ml of dehydrated carbon tetrachloride (mass ratio 1:4) were put into a round-bottomed stainless steel reaction bottle for mixing, and the reaction bottle was degassed and then the valve was closed for sealing. Then put the whole reaction bottle into an oil bath and heat it to 180°C, keep it for 8 hours, take it out after cooling. At this time, the reaction solution changed from colorless to brown-red, and black needle-like crystals were precipitated. Open the valve of the reaction bottle to release the reaction gas, pour the reaction solution into the evaporator, and remove carbon tetrachloride by evaporation to obtain 14.8 g of molybdenum pentachloride black crystals, with a product yield of 78%. Phase structure analysis result is the same as embodiment 1.

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Abstract

The invention relates to a method for preparing molybdenum pentachloride, which belongs to the technical filed of inorganic chemistry. The method comprises the following steps of: firstly blending molybdenum trioxide and dehydrated carbon tetrachloride in mass ratio of 1:4-1:6 in a round-bottom stainless steel reaction bulb, and closing a valve for sealing after the reaction bulb is degassed; then completely immerging the reaction bulb into an oil bath pan and heating to 150 DEG-240 DEG, keeping the temperature for 1-12 hours, and taking out the reaction bulb after cooling; and at the moment, with the change of a reaction solution color from original colorlessness to brownish red and the precipitation of black acicular crystals, opening the valve of the reaction bulb to discharge reaction gas, pouring the reaction solution into an evaporator, and evaporating to remove the carbon tetrachloride to obtain black molybdenum pentachloride crystals. The method has the advantages of simple and easily-controlled technology, high production efficiency, lower raw material price, simple production condition, low production cost, single product phase structure and high purity, and because the reaction is carried out in a sealed system, less pollution is generated.

Description

technical field [0001] The invention belongs to the technical field of inorganic chemistry, in particular to a method for preparing molybdenum pentachloride. technical background [0002] Molybdenum pentachloride is an important catalyst in the field of organic chemical industry. For example, it is an effective catalyst for the chlorination of aromatic rings and the partial or complete chlorination of phthalic anhydride; it can be used to catalyze the synthesis of polypentene rubber. Great impact; it reacts with (benzene) phenol compounds to obtain (benzene) molybdenum phenate compounds, and it also reacts with Grignard reagents to generate biarsine and biarsine compounds. [0003] Molybdenum pentachloride is also used to achieve vapor deposition of molybdenum. The high-purity molybdenum obtained by the thermal decomposition of molybdenum pentachloride can be deposited on metal and non-metal surfaces to obtain a thin layer of uniformly adhered hard coating. The molybdenum ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G39/04
Inventor 李一袁凤艳李楠雷福伟柳学全唐思琪霍静孟庆伟石文郑难忘丁存光
Owner CENT IRON & STEEL RES INST
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