Method for manufacturing molybdenum oxychloride and manufacturing equipment thereof

Abstract

Provided are a method for producing high-purity molybdenum oxychloride and an apparatus for producing the same. Specifically, provided are a method for producing molybdenum oxychloride and an apparatus for producing the same, the method comprising: a reaction process of adding molybdenum powder, chlorine gas, and oxygen to a reactor and heating to produce molybdenum oxychloride (MoO2Cl2); a solidification and coagulation process of transferring the reacted substance in the reactor from the reactor to a coagulation tank so as to solidify the reacted substance on the surface of the coagulation tank; a liquefaction process of heating the product cured in the curing coagulation process to convert the product into a liquid phase; and a purification process of filtering the product liquefied in the liquefaction process to increase purity.

Description

[0001] CROSS-REFERENCE TO RELATED APPLICATIONS

[0002] This application claims priority under 35 U.S.C. §119 to Korean Patent Application No. 10-2023-0156736 filed in the Korean Intellectual Property Office on November 13, 2023, the disclosure of which is incorporated herein by reference in its entirety. Technical Field

[0003] The following disclosure relates to a method for producing high purity molybdenum oxychloride and an apparatus for producing the same. Background Art

[0004] Tungsten hexafluoride (WF6) is a major precursor material for semiconductor wiring processes (i.e., 3D NAND flash memory) where copper plating processes are not applicable due to high aspect ratios. Since tungsten hexafluoride causes difficulties during the manufacturing process, such as increased resistance values ​​and / or etching caused by residual fluorine in the substrate, new material precursor development is needed to address these obstacles and difficulties.

[0005] In order to solve these difficulties and replace previous precursor materials, innovative technology development using molybdenum precursors in the form of molybdenum oxychloride has been completed for semiconductor wiring processes. In Korean Patent Publication No. 2022-0131312, a method for manufacturing molybdenum oxychloride by reacting MoO3 powder and chlorine has been disclosed. In addition, a solution using a glass reactor as an integrated reactor has been disclosed. However, glass reactors are difficult to operate due to their fragile characteristics and inefficient production efficiency. This is another obstacle to commercial large-scale production. The process of reacting MoO3 powder and chlorine requires a relatively high temperature of more than 800°C, because at lower temperatures, the reaction rate during the manufacturing process is delayed. Therefore, there is an urgent need to develop new technologies for the manufacturing method and equipment of molybdenum oxychloride, in which molybdenum metal and chlorine can react at lower temperatures, thereby supporting semi-continuous manufacturing processes including semi-batch, to achieve high productivity and efficiency as well as high purity.

[0006] [Related technical literature]

[0007] [Patent Document]

[0008] (Patent Document 1) (Related Document 1) Korean Patent Publication No. 2022-0131312 (September 27, 2022) Summary of the invention

[0009] One embodiment of the present invention is directed to providing a method for producing molybdenum oxychloride with significantly improved productivity.

[0010] Another embodiment of the present invention is directed to providing a molybdenum oxychloride manufacturing apparatus having significantly improved productivity.

[0011] Still another embodiment of the present invention is directed to providing a method for producing high-purity molybdenum oxychloride with improved productivity and an apparatus for producing the same.

[0012] The present inventors have studied to solve this problem, and as a result, can provide a new method and a production apparatus for producing high-purity molybdenum oxychloride. The production apparatus designs an apparatus using a reactor, a coagulation tank, and a purification system apparatus to produce high-purity molybdenum oxychloride.

[0013] By using this manufacturing equipment, the reactants (or reactants) can be continuously transferred to a manufacturing equipment including a reactor, a coagulation tank and a purification device and recovered and purified. Therefore, the manufacturing system can support a semi-continuous manufacturing method for semi-batch production. These manufacturing methods and equipment show a significantly improved productivity of high-purity platinum oxychloride as the final product.

[0014] In one general aspect, a method for producing molybdenum oxychloride includes: adding molybdenum powder, chlorine gas, and oxygen into a reactor and heating to prepare a reaction process of molybdenum oxychloride (MoO2Cl2),

[0015] The solidification and coagulation process is to transfer the reacted material in the reactor from the reactor to the coagulation tank so that the reacted material is solidified on the surface of the coagulation tank,

[0016] A liquefaction process in which a product solidified in a solidification coagulation process is heated to convert the product into a liquid phase, and

[0017] A purification process in which the product liquefied during the liquefaction process is filtered to increase the purity.

[0018] In an exemplary embodiment, the reaction process may be performed at a temperature of 250°C to 400°C.

[0019] In another exemplary embodiment, after the reaction process, the reactor may be cooled to solidify the product inside the reactor and unreacted oxygen and chlorine may be exhausted by nitrogen purging and vacuum.

[0020] In an exemplary embodiment, the cooling temperature during the discharge process may be 0°C to 100°C.

[0021] In another exemplary embodiment, the solidification condensation process may be performed under reduced pressure.

[0022] In an exemplary embodiment, a purification process of applying nitrogen purge or vacuum to further remove unreacted chlorine and side reaction products may be further included after the solidification and condensation process in the condenser.

[0023] As another exemplary embodiment, when the reactor temperature is adjusted to 120°C to 400°C or includes a discharge process, the solidification condensation process can be a process in which the product vaporized due to reheating to 120°C to 400°C is transferred to a condenser at 0°C to 100°C so that the product is solidified into crystals on the surface of the condenser.

[0024] In an exemplary embodiment, after the solidification coagulation process, the liquefaction step of liquefying the product in the coagulator may be performed by increasing the temperature of the coagulator to 110°C to 250°C.

[0025] As another exemplary embodiment, the purification process performed after the liquefaction process may be purified by filtering using a filter member including two or more filter members having pores different from each other.

[0026] In an exemplary embodiment, the purification process may be filtered using a first filter component having pores of 5 μm to 50 μm and a second filter component having pores of 1 μm to 30 μm.

[0027] As another exemplary embodiment, the purification process may maintain a temperature of 180° C. to 250° C., preferably 180° C. to 220° C., such that molybdenum oxychloride exists as a liquid phase.

[0028] In an exemplary embodiment, the purity of molybdenum oxychloride manufactured by the manufacturing method may be 99.999 wt % or higher.

[0029] In another general aspect, a manufacturing apparatus for molybdenum oxychloride includes: a reactor 10 , a coagulation tank 20 , a filter member 30 including a first filter member 31 and a second filter member 32 , and a storage tank 40 , which are sequentially arranged.

[0030] In an exemplary embodiment, the manufacturing equipment of molybdenum oxychloride comprises the following in a sequential arrangement:

[0031] A reactor for preparing crude molybdenum oxychloride by adding molybdenum powder, chlorine and oxygen and heating,

[0032] A coagulation tank is used to coagulate the crude molybdenum oxychloride in a gaseous state transferred from the reactor into a solid phase on the surface of the coagulation tank.

[0033] a filter member including a first filter member and a second filter member for removing solid impurities contained in a liquefied product introduced after liquefying a product solidified in a coagulation tank, and

[0034] Storage tank for purified product in filter section.

[0035] In an exemplary embodiment, the reactor 10 may include: a molybdenum powder injection pipe 11; a chlorine gas injection pipe 12; an oxygen injection pipe 13; a vacuum purge, nitrogen introduction pipe 14; and a transfer pipe 15 for transferring the reacted substances in the reactor to the coagulation tank 20.

[0036] As another exemplary embodiment, the coagulation tank 20 may be provided with a discharge pipe 21 through which impurities may be discharged by purging with nitrogen introduced from the reactor, and a liquid transfer pipe 22 through which the liquefied product in the coagulation tank is transferred to a filter member.

[0037] In an exemplary embodiment, the filter member 30 may sequentially include a first filter member 31 having relatively large pores and a second filter member 32 having relatively small pores.

[0038] As another exemplary embodiment, the first filter member 31 is a sintered filter having a pore size of 10 μm to 30 μm, and the second filter member 32 is a sintered filter having a pore size of 5 μm to 10 μm.

[0039] In an exemplary embodiment, the filter component and the storage tank temperature may be controlled at 180°C to 220°C.

[0040] Other features and aspects will become apparent from the following detailed description, drawings, and claims. BRIEF DESCRIPTION OF THE DRAWINGS

[0041] Figure 1 Schematic diagram of the apparatus used to synthesize molybdenum oxychloride.

[0042] [Explanation of Reference Numerals]

[0043] 100: Manufacturing equipment

[0044] 10: Reactor

[0045] 11: Molybdenum powder injection tube

[0046] 12: Chlorine injection pipe

[0047] 13: Oxygen injection tube

[0048] 14: Vacuum purge and nitrogen introduction tube

[0049] 15: Transfer tube

[0050] 20: Coagulation tank

[0051] 21: Discharge pipe

[0052] 22: Liquid transfer tube

[0053] 30: Filter components

[0054] 31: First filter component

[0055] 32: Second filter component

[0056] 40: Storage tank DETAILED DESCRIPTION

[0057] Hereinafter, the present invention will be described in more detail. However, the following specific examples or exemplary embodiments are only references for describing the present invention in detail, and the present invention is not limited thereto and may be implemented in various forms.

[0058] In addition, unless otherwise defined, all technical terms and scientific terms have the same meanings as those commonly understood by those skilled in the art to which the present disclosure belongs. The terms used herein are only used to effectively describe a specific example and do not limit the present disclosure.

[0059] Furthermore, unless the context indicates otherwise, the singular forms used in this specification and the appended claims are intended to include the plural forms.

[0060] In addition, unless specifically described to the contrary, “comprising” any elements should be understood to imply the inclusion of other elements rather than the exclusion of any other elements.

[0061] In addition, unless particularly limited, when one layer or a member is disposed on another layer or a member, not only is the layer or the member in contact with the other layer or the member, but also another layer or the member exists between the two layers or the two members.

[0062] In addition, the terms "about", "substantially" and the like used in this specification are used in the meaning of a numerical value or in the meaning close to a numerical value when the mentioned meaning implies allowable errors of unique manufacturing and materials, and are used to prevent the present disclosure, which mentions correct or absolute numerical values ​​for a better understanding of the present invention, from being unfairly used by unreasonable infringers.

[0063] Hereinafter, a method for producing molybdenum oxychloride by reacting molybdenum metal, chlorine gas, and oxygen in an exemplary embodiment of the present invention will be described in detail.

[0064] First, molybdenum metal in powder form is used to increase the contact area between gaseous chlorine and oxygen. Examples of the powder are not particularly limited, but for example, may have an average particle size (D 50 ), and a smaller average particle size may be preferred because the reaction rate will increase. Preferably, a powder of 0.05 mm to 0.5 mm may be used.

[0065] In the following, please refer to Figure 1The present invention relates to a molybdenum oxychloride precursor manufacturing device to describe a manufacturing method and a device thereof. Figure 1 One embodiment of the present invention is shown, however the manufacturing apparatus of the present invention is not limited thereto.

[0066] The manufacturing apparatus 100 of the present disclosure includes a reactor 10 , a coalescer 20 , a filter member 30 including a first filter member 31 and a second filter member 32 , and a storage tank 40 , which are sequentially arranged.

[0067] More specifically, a reactor 10 is arranged in sequence to prepare crude molybdenum oxychloride by adding molybdenum powder, chlorine gas and oxygen and heating,

[0068] The coagulation tank 20 is used to coagulate the crude molybdenum oxychloride in gaseous state transferred from the reactor into a solid phase on the surface.

[0069] a filter member 30 including a first filter member 31 and a second filter member 32 for removing solid impurities contained in a liquefied product introduced after liquefying a product solidified in a coagulation tank, and

[0070] A storage tank 40 stores the purified product from the filter element.

[0071] First, the reactor will be described as follows.

[0072] The reactor 10 includes: a molybdenum powder injection pipe 11; a chlorine injection pipe 12; an oxygen injection pipe 13; a vacuum purge, nitrogen introduction pipe 14; and a transfer pipe 15 for transferring the reacted substances in the reactor to the condensation tank, and the reactor may include temperature and pressure regulating devices.

[0073] The reaction temperature of the reactor may be 250° C. to 400° C., but is not particularly limited.

[0074] In the manufacturing apparatus, the coagulation tank 20 is used to condense the gaseous product passing through the transfer pipe 15 of the reactor 10 into a solid state on the surface of the coagulation tank 20 and recover the product, wherein the temperature of the coagulation tank 20 is cooled to 100° C. or less, 80° C. or less, 60° C. or less, 40° C. or less, such as -10° C. to 100° C., 0° C. to 100° C., or a temperature between the values, so that the crude molybdenum oxychloride synthesized from the reactor 10 is condensed. After the product is recovered, nitrogen is introduced from the reactor to purge and remove chlorine and other side reaction substances in the coagulation tank. In addition, the coagulation tank is used to heat the coagulated product and liquefy it, and then transfer the liquid product to the filter part 30 which is a purification part, and also has a role as a buffer for the reactor 10 and the filter part 30. That is, it continuously stores each batch of reaction substances of the reactor in the coagulation tank and allows continuous reaction in the reactor. In order to liquefy the product condensed in the coagulation tank 20, it is necessary to liquefy it by heating to 100°C to 250°C, and the liquefaction temperature is not particularly limited as long as it is within the temperature range, but can be 110°C to 250°C, 120°C to 220°C, or 120°C to 180°C.

[0075] The coagulation tank 20 may be provided with a discharge pipe 21 through which impurities may be discharged by purging with nitrogen introduced from a reactor, and a liquid transfer pipe 22 through which the liquefied product in the coagulation tank is transferred to a filter member.

[0076] The filter member 30 removes additional solid impurities contained in the product that is liquefied and introduced from the coagulation tank 20. The filter member 30 may include a first filter member 31 having relatively large pores and a second filter member 32 having relatively small pores. The filter member may have a filter member having fine pores, but should be frequently replaced with the applied filtering load, which may cause a burden on the process and a decrease in productivity, and therefore, purification may be performed by sequentially arranging two or more filter members having pores different from each other, and high-purity molybdenum oxychloride having a purity of 99.999 wt % or more may be provided by the purification filter.

[0077] The first filter component 31 may be a filter having a pore size of 5 μm to 50 μm, and the pore size of the second filter component 32 may be 1 μm to 30 μm, preferably 1 μm to 20 μm, and more preferably 5 μm to 10 μm or a size between the values. That is, the pore size of the first filter component 31 may be larger than the pore size of the second filter component 32.

[0078] The temperature of the filter member is not specified as long as molybdenum oxychloride safely exists as a liquid phase, but is preferably maintained at, for example, 150° C. to 250° C., preferably 180° C. to 220° C., and more preferably 200° C. for filtering effect.

[0079] The material of the filter of the filter member is not particularly limited and is not restricted as long as it is a material stable to molybdenum oxychloride, and preferably, a sintered filter is preferably used in terms of stability.

[0080] The product purified in the filter part 30 is stored in a liquefied state in the storage tank even if the temperature of the filter part in the storage tank 40 is maintained the same as or different from that in the storage tank, and can then be bagged in liquid form, and after bagging, solidified at room temperature and sold in a bagged state.

[0081] Hereinafter, a manufacturing method will be described.

[0082] The manufacturing method of the present disclosure may provide a method for manufacturing molybdenum oxychloride (MoO2Cl2), which includes: adding molybdenum powder, chlorine gas, and oxygen into a reactor and heating to prepare a reaction process of molybdenum oxychloride (MoO2Cl2),

[0083] The solidification and coagulation process is to transfer the reacted material in the reactor from the reactor to the coagulation tank so that the reacted material is solidified on the surface of the coagulation tank,

[0084] A liquefaction process in which a product solidified in a solidification coagulation process is heated to convert the product into a liquid phase, and

[0085] A purification process in which the product liquefied during the liquefaction process is filtered to increase the purity.

[0086] The molybdenum oxychloride (MoO2Cl2) prepared during the reaction may be crude molybdenum oxychloride.

[0087] The temperature of the reaction process is not particularly limited as long as the reaction is possible at the temperature, but may be, for example, 250°C to 400°C.

[0088] In an exemplary embodiment, after the reaction process, the reactor may be cooled to solidify the product and the unreacted oxygen and chlorine may be discharged by nitrogen purge and vacuum. The cooling temperature is not particularly limited as long as the product is solidified inside the reactor at this temperature, but for example, it may be 0° C. to 100° C.

[0089] In the manufacturing method of another exemplary embodiment, the solidification coagulation process may be performed under reduced pressure, which is more preferred because the product is easily transferred from the reactor to the coagulation tank under reduced pressure and the product is allowed to solidify on the surface of the coagulation tank.

[0090] The agglomerator having molybdenum oxychloride solidified on its surface may be further freed of unreacted chlorine and side reaction products, such as metal chlorides such as tungsten chloride from the reaction of molybdenum metal and tungsten contained in various impurity metals, by applying a nitrogen purge or vacuum at the solidification temperature.

[0091] As an exemplary embodiment, the solidification condensation process can transfer the product vaporized at the temperature of the reactor, or when a discharge process is included, the product vaporized due to reheating to 120°C to 400°C to a condenser at 0°C to 100°C and solidify the product into crystals on the surface of the condenser.

[0092] After the product is solidified in a solidification coagulator or both solidified and purified, a liquefaction process of heating the solidified product of the coagulator and liquefying it is performed. The temperature during heating in the liquefaction process may range from 110° C. to 250° C., and the liquefaction temperature is not particularly limited as long as it is within the temperature range, but liquefaction may be performed by heating to preferably 110° C. to 220° C. or 120° C. to 180° C.

[0093] The liquefied product is transferred to a filter member and filtered to undergo a purification process. The purification process is performed by filtering in two or more filter members having pores different from each other, thereby completing the purification process.

[0094] In the purification process, purification is performed in a filter member including a first filter member having pores of 5 μm to 50 μm and a second filter member having pores of 1 μm to 30 μm to provide molybdenum oxychloride (MoO2Cl2) having a purity of 99.9999% or more. The first filter member may have a larger pore size than the second filter member.

[0095] Another exemplary embodiment further includes bagging the molybdenum chloride (MoO2Cl2) after the filtration process.

[0096] One exemplary embodiment may be a method for manufacturing MoO2Cl2, wherein the temperature from the filtering process to the bagging process is maintained at 180°C to 220°C so that MoO2Cl2 is maintained in a liquid phase.

[0097] Another exemplary embodiment may be a manufacturing method, wherein when unreacted oxygen and chlorine are exhausted in the exhaust process, they are exhausted by nitrogen purge.

[0098] In another embodiment of the present disclosure, the purity of molybdenum oxychloride may be 99.999 wt % or higher through the manufacturing method.

[0099] In the present disclosure, after the product is transferred from the reactor to the coagulation tank, the interior of the reactor is cleaned by purging, molybdenum powder, chlorine gas and oxygen are added again and reacted, and at the same time, the solidified product in the coagulation tank is continuously subjected to subsequent steps of the liquefaction process and the purification process and is available for transportation, thereby significantly improving productivity and producing products with excellent purity.

[0100] Hereinafter, the present disclosure will be described in detail using the following examples. However, the following examples show specific examples for understanding the technical contents of the present invention, and the present disclosure is not limited to the following examples.

[0101] The average particle size is D 50 , and D 50 It refers to the particle size corresponding to 50% of the particles according to the volume-based integrated fraction. The average particle size can be derived from the particle size distribution results obtained by collecting a sample of particles to be measured according to the standard of ISO 13320-1 and analyzing it using S3500 available from MICROTRAC.

[0102] The purity was analyzed using ICP_MS (Agilent, ICP-MS 7900s).

[0103] 0.1 g of sample was collected into a 100 ml HDPE bottle using a spatula, where the dedicated N2 gas was replaced with an acrylic glove box. The weight of the collected sample was accurately measured with a scale capable of measuring four decimal places.

[0104] A mixed acid of 2% HNO3 and 1% HF was prepared and 50 g of the mixed acid was added to the sampling HDPE bottle. After adding the mixed acid, the weight was measured again using a scale capable of measuring to four decimal places and recorded.

[0105] The sample to which the mixed acid was added was sonicated using an ultrasonic cleaner for 10 minutes.

[0106] The analysis was performed using an ICP-MS 7900s device. For this purpose, standard solutions for the analytical instrument were prepared, calibration curves were ensured, and quantitative analysis of the samples was performed. The metals measured in this analysis included Ag, Al, As, Au, Ba, Ca, Co, Cr, Cu, Fe, K, Li, Mg, Mn, Na, Ni, Pb, Sn, V, W, and Zn.

[0107] (Example 1)

[0108] The average particle size (D 50) is 0.1mm, is filled into the reaction vessel to 1 / 5 of the volume and is heated at 350 ℃, and then chlorine and oxygen are added from the gas supply pipe to synthesize MoO2Cl2. The vaporized MoO2Cl2 is transferred to a coagulation tank controlled at 60 ℃ so that the product is fully solidified on the surface of the coagulation tank. Subsequently, a vacuum (30 Torr) is applied from the reactor to discharge unreacted chlorine and impurities. Purge is introduced again from the reactor to purge nitrogen into the coagulation tank and discharge nitrogen from the coagulation tank, thereby removing residual unreacted substances and impurities. At this time, as a result of analyzing the purity of molybdenum oxychloride using ICP_MS, the purity is 99.99 weight %.

[0109] Subsequently, the reactor and the coagulation tank were closed, and another batch reaction was performed in the reactor by adding molybdenum metal powder again and adding oxygen and chlorine gas, and at the same time, the reacted material in the coagulation tank (which liquefied the reaction material) was closed from the outside of the coagulation tank and heated to a temperature of 200° C. for liquefaction. Thereafter, filtration was performed by continuously passing through a first filter which was a sintered filter having pores of 10 μm and a second sintered filter having pores of 5 μm. The purity of the obtained molybdenum oxychloride was 99.9998% by weight.

[0110] According to the present disclosure, a method and a manufacturing apparatus for manufacturing a molybdenum oxychloride precursor having the same effect as semi-batch can be provided.

[0111] Furthermore, since the reaction process and the purification process are operated separately, new reactions can be performed even during the purification process to increase the yield.

[0112] In addition, in order to recover the reacted substances between the reaction process and the purification process and transfer the reacted substances to the purification process, a standby coagulation tank is separately set up so that the molybdenum oxychloride solidified on the surface of the coagulation tank is purged again with nitrogen to remove unreacted chlorine and other impurities, thereby further improving the purity.

[0113] Furthermore, according to the present manufacturing method, the first filter member and the second filter member are sequentially connected to filter impurities, thereby improving the purity to 99.999% or more.

Claims

1. A method for producing molybdenum oxychloride, the method comprising: The reaction process of adding molybdenum powder, chlorine and oxygen into a reactor and heating to prepare molybdenum oxychloride (MoO2Cl2) a solidification and coagulation process of transferring the reacted material in the reactor from the reactor to a coagulation tank so that the reacted material is solidified on the surface of the coagulation tank, a liquefaction process in which the solidified product in the solidification coagulation process is heated to convert the product into a liquid phase, and A purification process in which the product liquefied in the liquefaction process is filtered to increase the purity.

2. The method for producing molybdenum oxychloride according to claim 1, wherein the reaction process is carried out at 250°C to 400°C.

3. The method for producing molybdenum oxychloride according to claim 1, further comprising: After the reaction process, the reactor is cooled to solidify the product and the unreacted oxygen and chlorine are purged using nitrogen purge or vacuum.

4. The method for producing molybdenum oxychloride according to claim 3, wherein the cooling temperature is 0°C to 100°C.

5. The method for producing molybdenum oxychloride according to claim 1, wherein the solidification condensation process is carried out under reduced pressure.

6. The method for producing molybdenum oxychloride according to claim 1, further comprising: After the solidification coagulation process, a nitrogen purge or vacuum is applied to further remove the unreacted chlorine and side reaction products during the purification process.

7. The method for producing molybdenum oxychloride according to claim 1, wherein in the case where the reactor temperature is adjusted to 120°C to 400°C or the discharge process is included, the solidification condensation process is to transfer the product vaporized by reheating to 120°C to 400°C to the condenser at 0°C to 100°C so that the product is solidified as crystals on the surface of the condenser.

8. The method for producing molybdenum oxychloride according to claim 1, wherein the liquefaction is performed by increasing the agglomerator temperature to 110°C to 250°C during the liquefaction.

9. The method for producing molybdenum oxychloride according to claim 1, wherein the purification process is filtered using two or more filters having pores different from each other.

10. The method for producing molybdenum oxychloride according to claim 9, wherein the purification process performs filtration using a first filter member having pores of 5 μm to 50 μm and a second filter member having pores of 1 μm to 30 μm.

11. The method for producing molybdenum oxychloride according to claim 1, wherein the purification process is maintained at 180°C to 250°C so that the molybdenum oxychloride exists as a liquid phase.

12. The method for producing molybdenum oxychloride according to claim 1, wherein the purity of molybdenum oxychloride produced by the method is 99.999 wt% or more.

13. A manufacturing device for molybdenum oxychloride, comprising: Sequentially arranged A reactor for preparing crude molybdenum oxychloride by adding molybdenum powder, chlorine and oxygen and heating, a coagulation tank, wherein the crude molybdenum oxychloride in a gaseous state transferred from the reactor is coagulated into a solid phase on the surface of the coagulation tank, a filter member including a first filter member and a second filter member for removing solid impurities contained in a liquefied product introduced after liquefying the solidified product in the coagulation tank, and A storage tank stores the product purified in the filter unit.

14. The manufacturing apparatus for molybdenum oxychloride according to claim 13, wherein the reactor comprises: Molybdenum powder injection tube; chlorine injection tube; oxygen injection tube; vacuum purge and nitrogen introduction tube; and a transfer pipe for transferring the reacted substances in the reactor to the coagulation tank.

15. The manufacturing equipment of molybdenum oxychloride according to claim 13, wherein the coagulation tank is provided with a discharge pipe capable of discharging impurities by purging with nitrogen introduced from the reactor and a liquid transfer pipe for transferring the liquefied product in the coagulation tank to the filter member.

16. The manufacturing apparatus of molybdenum oxychloride according to claim 13, wherein the filter member sequentially comprises a first filter member having relatively large pores and a second filter member having relatively small pores. 17 . The manufacturing apparatus of molybdenum oxychloride according to claim 16 , wherein the first filter member is a sintered filter having a pore size of 10 μm to 30 μm, and the second filter member is a sintered filter having a pore size of 5 μm to 10 μm.

18. The manufacturing apparatus of molybdenum oxychloride according to claim 13, wherein the filter member and the storage tank are maintained at 180°C to 220°C.

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