Method for directly synthesizing metal (tungsten or molybdenum) carbonyl complex from tungsten oxide or molybdenum oxide

A metal carbonyl and oxide technology, applied in the field of powder metallurgy, can solve problems such as harsh reaction conditions, low synthesis efficiency, and complicated process, and achieve the effects of mild synthesis conditions, easy operation, and high synthesis efficiency

Inactive Publication Date: 2012-11-14
BEIJING CISRI GAONA TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Generally speaking, the existing methods have harsh reaction conditions, complicated process, low synthesis efficiency and high cost

Method used

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  • Method for directly synthesizing metal (tungsten or molybdenum) carbonyl complex from tungsten oxide or molybdenum oxide
  • Method for directly synthesizing metal (tungsten or molybdenum) carbonyl complex from tungsten oxide or molybdenum oxide
  • Method for directly synthesizing metal (tungsten or molybdenum) carbonyl complex from tungsten oxide or molybdenum oxide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] First add 60g of tungsten trioxide, 100ml of carbon tetrachloride, 2030ml of anhydrous acetone, 180g of independently packaged iron powder (60g) and a reducing agent mixed with iron pentacarbonyl (120g) in a mass ratio of 1:2 (mass The percentages are 3%, 8%, 80%, 9% successively); 2MPa carbon monoxide is charged and discharged 3 times in the reactor to replace the air in the reaction system and removed, then the reactor is heated to 200°C and kept for 4 hours; the reaction system After cooling down to 30°C, feed carbon monoxide to 8MPa and maintain the pressure, then turn on the stirring device of the reactor, break the packaged reducing agent container, the stirrer rotates at 100 rpm, and continue the reaction for 1 hour; after the reaction is completed, the solution is cooled to room temperature Finally, the reaction solution was taken out, and 10.9 g of colorless crystals of tungsten hexacarbonyl were obtained by distillation and heating sublimation, and the product ...

Embodiment 2

[0023] First add 60g of tungsten trioxide, 85ml of carbon tetrachloride, 1580ml of anhydrous ether, 180g of independently packaged zinc powder (60g) and nickel tetracarbonyl (120g) in a 1:2 mass ratio mixed reducing agent (mass The percentages are 4%, 9%, 75%, 12% successively); 2MPa carbon monoxide is charged and discharged 3 times in the reactor to replace the air in the reaction system and removed, then the reactor is heated to 220°C and kept for 6 hours; the reaction system After cooling down to 40°C, feed carbon monoxide to 10MPa and keep the pressure, then turn on the stirring device of the reactor, break the packaged reducing agent container, the stirrer rotates at 150 rpm, and continue the reaction for 6 hours; after the reaction is completed, the solution is cooled to room temperature Finally, the reaction solution was taken out, and 24.6 g of colorless crystals of tungsten hexacarbonyl were obtained by distillation and heating sublimation, and the product yield was ab...

Embodiment 3

[0025] First add 80g of tungsten trioxide, 100ml of carbon tetrachloride, 1570ml of anhydrous ether, 240g of independently packaged aluminum powder (80g) and a reducing agent mixed with iron pentacarbonyl (160g) in a mass ratio of 1:2 (mass The percentages are 5%, 10%, 70%, 15% successively); 2MPa carbon monoxide is charged and discharged 3 times in the reactor to replace the air in the reaction system and removed, then the reactor is heated to 250°C and kept for 8 hours; the reaction system After cooling down to 50°C, feed carbon monoxide to 20MPa and keep the pressure, then turn on the stirring device of the reactor, break the packaged reducing agent container, the stirrer speed is 200 rpm, and continue the reaction for 12 hours; after the reaction is completed, the solution is cooled to room temperature Finally, the reaction solution was taken out, and 55.8 g of colorless crystals of tungsten hexacarbonyl were obtained by distillation and heating sublimation, and the product...

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Abstract

The invention relates to a method for directly synthesizing a metal (tungsten or molybdenum) carbonyl complex from tungsten oxide or molybdenum oxide, belonging to the technical field of powder metallurgy. The method comprises the following steps: putting tungsten or molybdenum oxide, carbon tetrachloride, a nonpolar organic solvent and an independently packaged reducer into a sealed reaction kettle provided with a stirrer; replacing air in the reaction system by repeatedly charging carbon monoxide into the reaction kettle and discharging the carbon monoxide from the reaction kettle, heating the reaction kettle to 200-250 DEG C, and keeping the temperature for 4-8 hours; after the reaction system is cooled to 30-50 DEG C, introducing carbon monoxide to 5-20 MPa, keeping the pressure, starting the stirrer of the reaction kettle, breaking the container packaging the reducer, wherein the stirring is carried out at the rotation speed of 100-200 rpm for 1-12 hours; and after the reaction finishes and the solution is cooled to room temperature, taking out the reaction solution, distilling and heating for sublimation to obtain the clear crystal of tungsten hexacarbonyl or molybdenum hexacarbonyl. The invention has the advantages of simple technique, high safety in production, low cost and high synthesis efficiency, and has wide application prospects in the market.

Description

technical field [0001] The invention belongs to the field of powder metallurgy, in particular to a method for directly synthesizing tungsten or molybdenum carbonyl metal complexes from tungsten oxide or molybdenum. Background technique [0002] Both tungsten and molybdenum are rare metals, which are widely used in the national economy and military industry, and have become an indispensable strategic resource. In addition to being used in the field of iron and steel metallurgy, tungsten and molybdenum are also widely used in many fields such as electric light source, machinery, and chemical industry. For example, adding tungsten or molybdenum to steel can reduce its decomposition temperature and expand the temperature range and depth of heat treatment; the high melting point of tungsten and molybdenum, high strength and excellent electrical conductivity at high temperatures make it widely used in the electric light source industry ; In the machinery industry, tungsten disulf...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G1/04C01G39/00C01G41/00
Inventor 李一李楠霍静柳学全石文丁存光李红印姜丽娟任勃
Owner BEIJING CISRI GAONA TECH
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