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Preparation method of molybdenum hexafluoride

A technology of molybdenum hexafluoride and hydrogen fluoride gas, applied in the direction of molybdenum halide, etc., can solve the problems of difficult reaction conditions, complicated reaction process, complex reaction, etc., and achieve the effect of easy control of reaction conditions, simple reaction process and high purity of products

Active Publication Date: 2013-12-18
RES INST OF PHYSICAL & CHEM ENG OF NUCLEAR IND
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Problems solved by technology

[0009] In method (i), the raw material bromine trifluoride is a chemically active liquid, flammable, and the reaction conditions are not easy to control
In method (ii), molybdenum pentachloride is a volatile crystal with strong hygroscopicity, and the reaction is more complicated
[0010] In the preparation process of industrialized molybdenum hexafluoride, the reaction conditions are not easy to control, the reaction process is complex and a series of problems

Method used

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  • Preparation method of molybdenum hexafluoride

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preparation example Construction

[0033] Such as figure 1 Shown, a kind of preparation method of molybdenum hexafluoride comprises the following steps:

[0034] (i) Fluorine gas purification

[0035] The fluorine (F) in the fluorine buffer tank 1 2 ) into the cooling tower 2, cooled to -70~-90°C, first remove a large amount of hydrogen fluoride (HF) gas in the fluorine gas, and then pass the fluorine gas containing a small amount of hydrogen fluoride into the absorber equipped with sodium fluoride (NaF) In tower 3, a small amount of hydrogen fluoride remaining in the fluorine gas is removed at 100°C,

[0036] (ii) Synthesis reaction

[0037] Put the metal molybdenum in the reactor 4, preheat to 200°C, vacuumize the reactor 4 to -0.1~-0.09MPa, slowly introduce the purified fluorine gas, and the fluorine gas and the metal molybdenum contact in the reactor 4 Synthesis reaction occurs, the reaction temperature of reactor 4 is maintained at 200-350°C, the reaction time is 2-4 hours, the pressure is maintain...

Embodiment 1

[0045] 50g of metal molybdenum is placed in the reactor 4, and after the reactor is sealed and tested for leaks, it is preheated to 200°C, the heating is stopped, and the reactor 4 is evacuated to -0.1Mpa. The purified fluorine gas is slowly introduced into the reactor 4, and the metal molybdenum and the fluorine gas synthesize and react to generate molybdenum hexafluoride. The temperature of the reactor 4 is controlled at 200° C., and the pressure is maintained at -0.05 MPa. The reaction ends after 2 hours.

[0046] The crude molybdenum hexafluoride product from the reactor 4 enters the collector 5, and the temperature of the collector 5 is -50°C. The light component impurities such as oxygen and nitrogen in the molybdenum hexafluoride enter the tail gas treatment system, and the distillation of the collector 5 The temperature rises to 40°C, the temperature of the reflux column reaches 35°C, the temperature of the product steel cylinder 6 is maintained at 0°C, and the product ...

Embodiment 2

[0048] 100g of metal molybdenum is placed in the reactor 4, and after the reactor 4 is sealed and tested for leaks, it is preheated to 200°C, the heating is stopped, and the reactor 4 is evacuated to -0.05Mpa. The purified fluorine gas is slowly introduced into the reactor 4, and the metal molybdenum and the fluorine gas synthesize and react to form molybdenum hexafluoride. The temperature of the reactor 4 is controlled at 280° C., and the pressure is maintained at -0.08 MPa. After 3 hours, the reaction ends.

[0049] The crude molybdenum hexafluoride product from the reactor 4 enters the collector 5, and the temperature of the collector 5 is -25°C. The light component impurities such as oxygen and nitrogen in the molybdenum hexafluoride enter the tail gas treatment system, and the distillation of the collector 5 The temperature rises to 40°C, the temperature of the reflux column reaches 35°C, the temperature of the product steel cylinder 6 is maintained at -25°C, and the produ...

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Abstract

The invention discloses a process method for preparing molybdenum hexafluoride, which comprises the following steps: (i) fluorine purification: the hydrogen fluoride gas in the fluorine is removed; (ii) synthesis reaction: the fluorine contacts with metal molybdenum in a reactor to generate a synthesis reaction, wherein the reaction temperature is 200-350 DEG C, the reaction time is 2-4 hours, the pressure is (-0.05)-0MPa, and a crude product of molybdenum hexafluoride is generated by the reaction; (iii) removing light impurities in the crude product of molybdenum hexafluoride such as oxygen and nitrogen; and (iv) purifying the molybdenum hexafluoride to obtain a product with purity over 99%. The method disclosed by the invention has the advantages that the reaction process is simple, the reaction conditions are easy to control, and the product purity is high.

Description

technical field [0001] The invention belongs to a preparation method of fluoride, in particular to a preparation method of molybdenum hexafluoride. Background technique [0002] Molybdenum hexafluoride (MoF 6 ) is mainly used for isotope separation of molybdenum, and can be used as chemical vapor deposition of molybdenum silicide or molybdenum film in the microelectronics industry to make interconnect lines with low resistance and high melting point. At present, the preparation method of molybdenum hexafluoride has following two kinds: [0003] (i) Reaction of molybdenum and bromine trifluoride [0004] Molybdenum hexafluoride can be prepared by passing bromine trifluoride on molybdenum and heating it to 350°C. The reaction equation is as follows: [0005] Mo+2BrF 3 →MoF 6 +Br 2 [0006] (ii) In the presence of air, molybdenum pentachloride reacts with fluorine gas [0007] In the presence of air, to MoCl 5 Fluorine gas can also generate molybdenum hexafluoride, the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G39/04
Inventor 仝庆崔学文贺邓张淑娟
Owner RES INST OF PHYSICAL & CHEM ENG OF NUCLEAR IND
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