CN-122010179-A - Preparation method and device of molybdenum hexacarbonyl

Abstract

The application belongs to the technical field of metal organic compound preparation, and particularly relates to a preparation method and device of molybdenum hexacarbonyl. The preparation method comprises the steps of S1, introducing molybdenum powder and carbon monoxide into a reaction device, carrying out catalytic reaction under the action of a catalyst to generate crude molybdenum hexacarbonyl, S2, cooling the crude molybdenum hexacarbonyl to obtain liquid molybdenum hexacarbonyl, S3, carrying out reduced pressure distillation on the cooled liquid molybdenum hexacarbonyl, and S4, purifying the liquid molybdenum hexacarbonyl subjected to reduced pressure distillation to obtain a final product molybdenum hexacarbonyl. The preparation device comprises a storage tank, a purifier, a reaction kettle, a condenser, a reduced pressure distillation tower and a recrystallization device which are sequentially arranged along the material flow direction. The method prepares the high-purity molybdenum by utilizing the reduction reaction of the carbon monoxide and the molybdenum powder at high temperature, has the advantages of high raw material purity, accurate reaction temperature control, high reaction efficiency and the like, and is particularly suitable for high-quality production of the molybdenum.

Inventors

• BO LIN
• PEI JIAYING
• WANG YAFENG
• WANG KAI
• Lv tiefeng
• HE NING
• YANG YAOWU
• CHEN BAOJIAN

Assignees

• 中船(邯郸)派瑞特种气体股份有限公司

Dates

Publication Date

20260512

Application Date

20260228

Claims (10)

1. 1. The preparation method of the molybdenum hexacarbonyl is characterized by comprising the following steps: s1, introducing molybdenum powder and carbon monoxide into a reaction device, and carrying out catalytic reaction under the action of a catalyst to generate crude molybdenum hexacarbonyl; s2, cooling the crude molybdenum hexacarbonyl to obtain liquid molybdenum hexacarbonyl; s3, performing reduced pressure distillation on the liquid molybdenum hexacarbonyl obtained by cooling; and S4, purifying the liquid molybdenum hexacarbonyl after reduced pressure distillation to obtain a final product molybdenum hexacarbonyl.
2. 2. The method for preparing molybdenum hexacarbonyl according to claim 1, wherein the purity of the molybdenum powder in the step S1 is more than 99%, the granularity of the molybdenum powder is 1-100 μm, the purity of the carbon monoxide is more than or equal to 99.5%, the flow rate is 0.3-3L/min, and the molar ratio of the molybdenum powder to the carbon monoxide is 1:6-1:10.
3. 3. The method for preparing molybdenum hexacarbonyl according to claim 1, wherein the temperature of the catalytic reaction in the step S1 is 100-300 ℃, the pressure is 1-10 mpa, and the time of the catalytic reaction is 3-8 hours.
4. 4. The method for preparing molybdenum hexacarbonyl according to claim 1, wherein the catalyst in the step S1 is a metal halide, and the addition amount of the catalyst is 0.1% -5% of the mass of molybdenum powder.
5. 5. The method for producing molybdenum hexacarbonyl according to claim 4, wherein the metal halide is one or both of molybdenum chloride and molybdenum bromide.
6. 6. The method for preparing molybdenum hexacarbonyl according to claim 1, wherein the cooling temperature in the step S2 is-20 ℃.
7. 7. The method for preparing molybdenum hexacarbonyl according to claim 1, wherein the pressure of reduced pressure distillation in the step S3 is 0.01-0.1 mpa, and the temperature of reduced pressure distillation is 80-140 ℃.
8. 8. The method for preparing molybdenum hexacarbonyl according to claim 1, wherein the purification in the step S4 adopts a recrystallization mode, and specifically comprises the steps of dissolving liquid molybdenum hexacarbonyl distilled under reduced pressure in toluene or benzene, then cooling to-10 ℃ at a rate of 0.5-1 ℃ per minute, crystallizing and separating out the molybdenum hexacarbonyl, and filtering to obtain the final product molybdenum hexacarbonyl.
9. 9. A preparation device of molybdenum hexacarbonyl is used for the preparation method of molybdenum hexacarbonyl according to any of claims 1-8, and is characterized by comprising a storage tank (1) for storing carbon monoxide, a purifier (3) for purifying carbon monoxide, a reaction kettle (4) for catalytic reaction, a condenser (5) for condensing molybdenum hexacarbonyl, a reduced pressure distillation tower (6) for distilling liquid molybdenum hexacarbonyl and a recrystallization device (7) for purifying molybdenum hexacarbonyl, wherein valves are arranged on pipelines communicated with the storage tank (1), the purifier (3), the reaction kettle (4), the condenser (5), the reduced pressure distillation tower (6) and the recrystallization device (7), a flowmeter (2) is arranged on the pipeline communicated with the storage tank (1) and the purifier (3), and a pipeline communicated between the storage tank (1) and the purifier (3) is arranged above the reduced pressure distillation tower (6).
10. 10. The preparation device of the molybdenum hexacarbonyl is characterized in that the reaction kettle (4) is made of stainless steel, a magnetic stirring device and a jacket type heating and cooling device are arranged in the reaction kettle (4), the storage tank (1) is a high-pressure steel cylinder, one or two of active carbon and molecular sieve adsorbents are filled in the purifier (3), the condenser (5) is of a tubular condensation structure, a cooling medium is water or liquid nitrogen, the reduced pressure distillation tower (6) is of a packed tower structure, stainless steel wire nets or ceramic raschig rings are filled in the reaction kettle, and the recrystallization device (7) comprises a dissolution tank and a crystallizer.

Description

Preparation method and device of molybdenum hexacarbonyl Technical Field The invention belongs to the technical field of metal organic compound preparation, and particularly relates to a preparation method and device of molybdenum hexacarbonyl. Background Molybdenum is an important industrial metal and is widely applied to the fields of nuclear reactor components, alloys, catalysts and the like. Traditional molybdenum preparation methods generally involve complex process flows and high energy consumption, and are difficult to meet the requirements of industrial production on high-purity molybdenum. In recent years, the reduction method for producing molybdenum has been attracting attention, because it can produce molybdenum by reducing molybdenum oxide (Mo 2O5) with carbon monoxide, and has high production efficiency and environmental protection. However, the existing reduction method has a certain technical bottleneck for preparing high-purity molybdenum, and is mainly characterized in the aspects of raw material purity, reaction temperature control, equipment efficiency and the like. Molybdenum hexacarbonyl is an important metal organic compound, and the unique chemical structure and the property of the molybdenum hexacarbonyl lead the molybdenum hexacarbonyl to have wide application prospect in a plurality of fields. The traditional molybdenum hexacarbonyl preparation method has some limitations, and limits the mass production and application of the molybdenum hexacarbonyl. Early molybdenum hexacarbonyl preparation methods are mainly based on high-pressure reaction conditions and need to be carried out at higher pressure and temperature, which has extremely high requirements on reaction equipment and increases production cost and safety risks. For example, chinese patent publication No. CN120311038A discloses a method for preparing molybdenum hexacarbonyl powder by high-pressure circulation, which adopts molybdenum raw material and carbon monoxide to make synthesis reaction in a synthesis kettle under the condition of 11.0-30.0MPa, so as to produce molybdenum hexacarbonyl and synthetic residue. For example, chinese patent publication No. CN105967242B discloses a preparation method of nano hexacarbonyl molybdenum powder, wherein a molybdenum raw material is placed into a high-pressure reaction kettle, CO gas is introduced into the high-pressure reaction kettle, and the reaction pressure is controlled to be 12-18 MPa. Still other processes require the reaction of molybdenum with carbon monoxide at pressures of several hundred atmospheres or even higher, and this high pressure environment not only requires extremely high pressure resistance of the reactor, but also presents a potential explosion hazard during operation. Along with the continuous development of technology, higher requirements are put on the quality and the yield of molybdenum hexacarbonyl, and the traditional method is not only harsh in reaction conditions, but also relatively low in reaction efficiency and long in reaction time, so that the production period is prolonged, and the production efficiency is difficult to meet the increasing market demands. Meanwhile, certain difficulties exist in the aspect of purity control of the product, and complicated separation and purification steps are often required to obtain a high-purity molybdenum hexacarbonyl product, which further increases the production cost and the process complexity. With the continuous development of technology, higher requirements are put on the quality and the yield of molybdenum hexacarbonyl. Therefore, there is a need to develop a preparation method and a device which are efficient, safe, low in cost and capable of producing high-purity molybdenum hexacarbonyl, so as to solve the problems existing in the prior art for producing high-purity molybdenum hexacarbonyl. Disclosure of Invention Aiming at the problems of low efficiency and high cost in the preparation of molybdenum hexacarbonyl in the prior art, the application provides a preparation method and a device of molybdenum hexacarbonyl. The scheme of the application is as follows: in one aspect, the application provides a method for preparing molybdenum hexacarbonyl, comprising the following steps: s1, introducing molybdenum powder and carbon monoxide into a reaction device, and carrying out catalytic reaction under the action of a catalyst to generate crude molybdenum hexacarbonyl; the reaction formula is Mo+6CO→Mo (CO) 6. S2, cooling the crude molybdenum hexacarbonyl to obtain liquid molybdenum hexacarbonyl; s3, performing reduced pressure distillation on the liquid molybdenum hexacarbonyl obtained by cooling; and S4, purifying the liquid molybdenum hexacarbonyl after reduced pressure distillation to obtain a final product molybdenum hexacarbonyl. Preferably, the purity of the molybdenum powder is more than 99%, the granularity of the molybdenum powder is 1-100 mu m, the purity of the carbon monoxide is more than or