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Method for preparing tungsten pentachloride

A technology of tungsten pentachloride and tungsten hexachloride, applied in tungsten halide and other directions, can solve the problems of easy reduction, instability, easy hydrolysis, etc., and achieve the effect of facilitating subsequent purification, reducing excessive reduction and improving conversion rate

Active Publication Date: 2018-07-20
绿菱电子材料(天津)有限公司
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Problems solved by technology

[0013] To sum up, tungsten pentachloride is a short-lived special metal halide that is extremely unstable, easy to oxidize, easy to reduce, easy to hydrolyze, and easy to interact with the environment. There is also no reference for its preparation, separation and purification technology. to report

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  • Method for preparing tungsten pentachloride

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Embodiment 1

[0047] A preparation method of tungsten pentachloride, combining figure 1 , including the following steps:

[0048] (1) The reactor and its accessory collectors, raw material sampling equipment, analytical balance, connecting pipelines, glass containers and other equipment were dried overnight, and purged with high-purity nitrogen for 2 hours, and the tail gas was detected by chromatography to ensure that there was no moisture and air;

[0049] (2) Grind the raw material tungsten hexachloride to a particle size of 40 μm in a glove box under a nitrogen atmosphere, weigh 1 kg of the raw material tungsten hexachloride with a balance, transfer it to the reactor, and continuously feed nitrogen protection;

[0050] (3) The temperature of the reactor is raised to 280°C, the heating rate is 5-20°C / min, and when the temperature is raised to 100°C, the temperature is kept for 2 hours;

[0051] (4) Feed high-purity hydrogen, the flow rate of high-purity hydrogen is 100mL / min, the inter...

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Abstract

The invention discloses a method for preparing tungsten pentachloride. The method includes the steps of grinding and transferring raw material tungsten hexachloride into a reactor, introducing high-purity hydrogen to perform reduction reaction on tungsten pentachloride, wherein the reaction temperature is 280-400 DEG C, the reaction pressure is 0.01-0.5 MPa and the reaction duration is 2-5 s, andobtaining crude tungsten pentachloride with a concentration of 95% or above, wherein the conversion rate of tungsten pentachloride is larger than 80%; by sublimation and deposition, purifying the crude tungsten pentachloride, wherein the sublimation temperature is in a range of 200-250 DEG C, the deposition temperature is in a range of 100-150 DEG C, and the purity of the collected high-purity tungsten pentachloride can reach 99.99% or above. According to the method, the reduction reaction process is precisely regulated, the stability and purification rate of the product tungsten pentachlorideare improved, the method is simple, convenient, practical, high in controllability and low in cost, and large-scale industrial production is easy.

Description

technical field [0001] The invention relates to the synthesis and purification of a metal halide, in particular to a preparation method of tungsten pentachloride. Background technique [0002] Tungsten pentachloride (CAS: 13470-14-9), monoclinic crystal system, needle-shaped dark green crystal, as a rare compound with a tungsten-to-chlorine ratio of 1:5, has a unique tungsten valence change and chlorine atom decomposition Characteristics, its price change law and the release of chlorine free radicals have the advantages of strong controllability in timing and positioning, and are regarded as potential substances in high-tech fields such as semiconductors, solar energy, catalysis, and military and national defense in the future. [0003] Tungsten pentachloride was first recorded in the manuscripts (Acta.Cryst.1978.B34, 2833-2834) in the 1960s. It was scientists who were studying the synthesis of other valence tungsten chlorides (such as tungsten hexachloride, tetrachloride B...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G41/04
CPCC01G41/04C01P2006/80
Inventor 马建修靖宇王新鹏张学刚王维佳
Owner 绿菱电子材料(天津)有限公司
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