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Synthesis method of molybdenum trichloride

A technology of molybdenum trichloride and synthesis method, applied in the directions of molybdenum halide, tin chloride, tin halide, etc., can solve the problem of unsatisfactory purity of molybdenum trichloride, affecting the purity of molybdenum trichloride, and low yield of molybdenum trichloride and other issues, to achieve the effect of being conducive to maximizing utilization, being environmentally friendly, and having high selectivity

Pending Publication Date: 2022-03-04
湖南省华京粉体材料有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, the synthesis method of molybdenum trichloride is mainly to prepare molybdenum trichloride by reducing molybdenum pentachloride with hydrogen. This method is easy to over-reduce or the reduction force is not enough to produce by-products such as molybdenum dichloride and molybdenum tetrachloride, which need to be added more In the separation step, because the boiling point of the by-product is relatively close to molybdenum trichloride, the yield of molybdenum trichloride is very low, and the purity is not more than 98%.
There are also attempts to reduce molybdenum pentachloride to prepare molybdenum trichloride by reducing agents such as aluminum and sodium, but there are also too many by-products due to the difficulty in controlling the reduction, the yield of molybdenum trichloride is low, and the obtained molybdenum trichloride is difficult to obtain. Separation from by-products affects the purity of molybdenum trichloride
The above-mentioned synthesis of molybdenum trichloride inevitably has the problem of unsatisfactory purity of molybdenum trichloride, so it is necessary to innovate the synthesis method of molybdenum trichloride

Method used

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  • Synthesis method of molybdenum trichloride

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] The molar ratio of molybdenum pentachloride to tin protochloride is 1.2:1, weigh 2.4 mol of molybdenum pentachloride and 2 mol of stannous chloride, mix them and put them into a replacement reactor, and after argon replacement, react after replacement The reactor was kept warm at 120°C, and the rear end of the reactor was cooled to collect tin tetrachloride liquid. After 4 hours of reaction, the molybdenum pentachloride cooling receiver was exhausted, and the temperature was raised to 250°C. After 4 hours of heat preservation, the reactor was cooled and collected, and three Molybdenum chloride 1.95 mol, purity 99.1%, molybdenum pentachloride 100g collected by cooling, tin tetrachloride liquid filtration obtains tin tetrachloride 1.98 mol, purity 99.4%, filter residue 1g, solid-liquid separation method is centrifugation or filtration, five Molybdenum chloride and filter residue can be reused as raw materials.

Embodiment 2

[0030] The molar ratio of molybdenum pentachloride and tin protochloride is 2:1, weigh 4 mol of molybdenum pentachloride and 2 mol of stannous chloride, mix and put into the replacement reactor, the volume ratio of argon and nitrogen is 1: 1. After the replacement, keep the reactor warm at 140°C, cool the rear end of the reactor to collect the tin tetrachloride liquid, react for 4 hours, exhaust from the molybdenum pentachloride cooling receiver, raise the temperature to 280°C, and keep it warm for 4 hours, The reactor was cooled to collect materials, and 1.98 mol of molybdenum trichloride was obtained with a purity of 99.3%, 540 g of molybdenum pentachloride collected by cooling, and 1.99 mol of tin tetrachloride was obtained by centrifugation of the tin tetrachloride liquid, with a purity of 99.6%, and 1.3 g of centrifuged residue. The solid-liquid separation method is a combination of decantation and gravity sedimentation, and molybdenum pentachloride and centrifugal slag ca...

Embodiment 3

[0032] The molar ratio of molybdenum pentachloride and tin protochloride is 3:1, weigh 6 mol of molybdenum pentachloride and 2 mol of stannous chloride, mix them and put them into a replacement reactor, after argon replacement, react after replacement The reactor was kept warm at 160°C, and the rear end of the reactor was cooled to collect the tin tetrachloride liquid. After 4 hours of reaction, the exhaust was exhausted from the molybdenum pentachloride cooling receiver, and the temperature was raised to 320°C. After 4 hours of heat preservation, the reactor was cooled and collected, and three Molybdenum chloride 1.96 mol, purity 99.5%, molybdenum pentachloride 1100g collected by cooling, tin tetrachloride liquid gravity settling after 1 day, extract supernatant, bottom suspension liquid filter, obtain tin tetrachloride 1.99 mol altogether, purity 99.5%, filter residue 3g, solid-liquid separation method is filtration, molybdenum pentachloride and filter residue can be reused a...

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Abstract

The invention discloses a process for preparing molybdenum trichloride, which comprises the following steps of: (1) mixing excessive molybdenum pentachloride and stannous chloride powder, and heating the mixed material in a reactor to carry out replacement reaction to generate molybdenum trichloride and stannic chloride; (2) gasifying the generated stannic chloride, leaving the reactor, entering a cooling system for receiving and cooling to obtain stannic chloride liquid; (3) after the reaction is completed, switching a cooling system into a molybdenum pentachloride receiver, heating the reactor to a certain temperature, and gasifying redundant molybdenum pentachloride into the molybdenum pentachloride receiver; and (4) cooling the reactor, and discharging to obtain a molybdenum trichloride product. And (5) hermetically filtering the tin tetrachloride liquid to obtain a tin tetrachloride product and molybdenum pentachloride filter residues, wherein the molybdenum pentachloride filter residues and cooled and collected molybdenum pentachloride can be recycled as reaction raw materials. According to the method, the yield of molybdenum trichloride is increased, meanwhile, the production cost is reduced, the purity of the by-product tin tetrachloride exceeds 99%, the waste gas amount in the production process is greatly reduced, and the method belongs to a green and environment-friendly process.

Description

technical field [0001] The invention relates to a method for synthesizing molybdenum trichloride, in particular to a method for simultaneously synthesizing molybdenum trichloride and tin tetrachloride at low cost, belonging to the field of synthesis of rare metal materials. Background technique [0002] Molybdenum trichloride, dark red monoclinic crystal, with a sublimation point lower than 400°C and higher than 375°C, is an important precursor of molybdenum-based catalysts used for nitrogen fixation in the current ammonia production process, because molybdenum-based catalysts can fix more Nitrogen is used to catalyze ammonia production from nitrogen, and ammonia is an important raw material for nitrogen fertilizer production, so molybdenum trichloride has a great application prospect. The boiling point of molybdenum pentachloride is 268°C, the melting point of tin tetrachloride is -33°C, the boiling point is 114.15°C, the melting point of tin protochloride is 247°C, and the...

Claims

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Application Information

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IPC IPC(8): C01G39/04C01G19/08
CPCC01G39/04C01G19/08
Inventor 李焌源王一舟黎静田吉英向小绢任改梅吴尔京
Owner 湖南省华京粉体材料有限公司
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