Method and apparatus for producing molybdenum oxychloride

Abstract

To provide a method for manufacturing high-purity molybdenum oxychloride and a manufacturing apparatus thereof.SOLUTION: The present invention relates to a method for manufacturing molybdenum oxychloride including: a reaction step of adding molybdenum powder, chlorine gas, and oxygen to a reactor and heating them to prepare molybdenum oxychloride (MoO2Cl2); a solidification and condensation step of transferring a reacted material in the reactor from the reactor to a condensation tank to solidify the reacted material on a surface of the condensation tank; a liquefaction step of heating a product solidified in the solidification and condensation step to convert the product into a liquid phase; and a purification step of filtering the product liquefied in the liquefaction step to increase purity, and a manufacturing apparatus thereof.SELECTED DRAWING: Figure 1

Description

[Technical Field]

[0001] The present invention relates to a method and an apparatus for producing high-purity molybdenum oxychloride. [Background technology]

[0002] Tungsten hexafluoride (WF6) is a key precursor material for semiconductor wiring processes in fields such as 3D NAND flash, where copper plating is difficult to use due to the high aspect ratio. However, fluorine in the tungsten hexafluoride molecule remains on the substrate, causing problems during the manufacturing process such as increased resistance and etching by the fluorine. To solve these problems, the development of a new precursor material is necessary.

[0003] To solve these problems, a technology has been developed that uses molybdenum oxychloride as a molybdenum precursor for semiconductor wiring as an alternative to conventional precursor materials. For example, Korean Patent Publication No. 2022-0131312 discloses a method for producing molybdenum oxychloride by reacting MoO powder with chlorine gas. It also discloses a solution using a glass reactor that is manufactured as an integrated reactor. However, the glass reactor is difficult to handle and is a batch-type reactor with an integrated structure, resulting in insufficient productivity. This also poses an obstacle to commercial mass production.

[0004] The process of reacting MoO3 with chlorine gas requires a relatively high reaction temperature of about 800°C, and the reaction rate is slow at low temperatures. Therefore, there is a need to develop a manufacturing method and manufacturing apparatus that can react molybdenum metal with chlorine gas and oxygen at low temperatures, enable semi-continuous production such as semi-batch, increase productivity, and efficiently produce high-purity molybdenum oxychloride precursors. [Prior art documents] [Patent documents]

[0005] [Patent Document 1] Korean Patent Publication No. 2022-0131312 (September 27, 2022) Summary of the Invention [Problem to be solved by the invention]

[0006] One aspect of the present invention is to provide a method for producing molybdenum oxychloride with significantly improved productivity.

[0007] Another aspect of the present invention is to provide an apparatus for producing molybdenum oxychloride with significantly improved productivity.

[0008] Another aspect of the present invention is to provide a method and an apparatus for producing high-purity molybdenum oxychloride with increased productivity. [Means for solving the problem]

[0009] In order to solve the above problems, the present inventors have conducted extensive research and have been able to provide a new production method and production apparatus for synthesizing high-purity molybdenum oxychloride. This production apparatus is designed to produce high-purity molybdenum oxychloride, and comprises a reactor, a condensation tank, and a purification apparatus connected in that order.

[0010] By using the manufacturing equipment, reactants (or reacted materials) can be continuously transferred to a manufacturing equipment including a reactor, a condensation tank, and a purification equipment, and recovered and purified. Therefore, this manufacturing system supports a semi-continuous manufacturing method for semi-batch production. These manufacturing methods and manufacturing equipment have demonstrated a significant increase in productivity of high-purity molybdenum oxychloride as a final product.

[0011] One aspect of the present invention is a reaction step of charging molybdenum powder, chlorine gas, and oxygen into a reactor and heating to produce molybdenum oxychloride (MoO2Cl2); a solidification and condensation step of transferring the reactants from the reactor to a condensation tank and solidifying them on the surface of the condensation tank; a liquefaction step of heating the solidified product in the solidification and condensation step to convert it into a liquid phase; a purification step of filtering the liquefied product to increase its purity; The present invention provides a method for producing molybdenum oxychloride, comprising:

[0012] In one embodiment, the reaction step may be carried out at 250 to 400°C.

[0013] Yet another embodiment may further include a step of cooling the reactor after the reaction step to solidify the product inside the reactor, and discharging unreacted oxygen and chlorine using a nitrogen purge or vacuum means.

[0014] In one embodiment, the cooling temperature may be 0 to 100°C in the discharging step.

[0015] In yet another embodiment, the solidification and condensation step may be carried out under reduced pressure.

[0016] In one embodiment, after the solidification and condensation step in the condenser, a purification step of removing unreacted chlorine gas and by-products by purging with nitrogen or applying a vacuum may be further included.

[0017] In yet another embodiment, the solidification and condensation step may be a step of adjusting the temperature of the reactor to 120 to 400°C, or if a discharge step is included, reheating the reactor at 120 to 400°C to vaporize the product, transferring the vaporized product to a condenser at 0 to 100°C, and solidifying the product into crystals on the surface of the condenser.

[0018] In one embodiment, the liquefaction step of liquefying the product in a condenser after the solidification and condensation step may be performed by increasing the temperature of the condenser to 110 to 250°C.

[0019] In yet another embodiment, the purification step performed after the liquefaction step may be performed by filtering using a filter unit including two or more filter units having different pores.

[0020] In one embodiment, the purification step may involve filtering using a first filter section having pores of 5 to 50 μm and a second filter section having pores of 1 to 30 μm.

[0021] In yet another embodiment, the purification step may be carried out at a temperature maintained at 180 to 250°C, preferably 180 to 220°C, and the molybdenum oxychloride may be present in a liquid phase.

[0022] In one embodiment, the purity of the molybdenum oxychloride produced by the production method may be 99.999 wt % or more.

[0023] In yet another aspect of the present disclosure, there is provided an apparatus for producing molybdenum oxychloride, including a reactor 10, a condensation tank 20, a filter unit 30 including a first filter unit 31 and a second filter unit 32, and a storage tank 40 arranged in this order.

[0024] In one embodiment, the apparatus for producing molybdenum oxychloride comprises: a reactor into which molybdenum powder, chlorine gas, and oxygen are introduced and heated to produce crude molybdenum oxychloride; a condensation vessel for condensing the gaseous crude molybdenum oxychloride transferred from the reactor into a solid phase on its surface; a filter unit including a first filter unit and a second filter unit for liquefying the solidified product in the condensation tank and then removing solid impurities contained in the liquefied product; a storage tank for storing the product purified by the filter unit; They may be arranged in that order.

[0025] In one embodiment, the reactor 10 may be a molybdenum oxychloride production apparatus including a molybdenum powder injection tube 11, a chlorine gas injection tube 12, an oxygen injection tube 13, a vacuum purge and nitrogen inlet tube 14, and a transfer tube 15 for transferring the reactants of the reactor to a condensation tank 20.

[0026] In yet another embodiment, the condensation tank 20 may be provided with a discharge pipe 21 through which impurities can be discharged by nitrogen purging introduced from the reactor, and a liquid transfer pipe 22 through which the liquefied product in the condensation tank is transferred to a filter section.

[0027] In one embodiment, the filter unit 30 may be an apparatus for producing molybdenum oxychloride including a first filter unit 31 having relatively large pores and a second filter unit 32 having relatively small pores in that order.

[0028] In yet another embodiment, the apparatus for producing molybdenum oxychloride may be provided, in which the first filter section 31 is a sintered filter having a pore size of 10 to 30 μm, and the second filter section 32 is a sintered filter having a pore size of 5 to 10 μm.

[0029] In one embodiment, the filter unit and the storage tank may be an apparatus for producing molybdenum oxychloride, the apparatus being maintained at 180 to 220° C. Other features and aspects will become apparent from the following detailed description, drawings, and claims. [Effects of the Invention]

[0030] According to the present disclosure, it is possible to provide a method and an apparatus for producing a molybdenum oxychloride precursor that have the same effects as semi-batch production.

[0031] Furthermore, by separating the reaction step and the purification step, a new reaction can be carried out even during the purification step, thereby increasing the production amount.

[0032] Furthermore, a separate condensation tank is provided between the reaction step and the purification step to recover the reactant and transfer it to the purification step. Molybdenum oxychloride solidified on the surface of the condensation tank can be purged again with nitrogen to remove unreacted chlorine and other impurities, thereby further increasing the purity.

[0033] Furthermore, according to this manufacturing method, the purity can be increased to 99.999% or more by sequentially connecting the first filter section and the second filter section to filter out impurities. [Brief explanation of the drawings]

[0034] [Figure 1] FIG. 1 is a schematic diagram of an apparatus for synthesizing molybdenum oxychloride. DETAILED DESCRIPTION OF THE INVENTION

[0035] The present invention will be described in more detail below. However, the following specific examples or examples are merely references for explaining the present invention in detail, and the present invention is not limited thereto and may be realized in various forms.

[0036] Furthermore, unless otherwise defined, all technical and scientific terms have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terms used to describe the present invention are merely for the purpose of effectively describing particular embodiments and are not intended to limit the present invention.

[0037] Furthermore, as used in the specification and the appended claims, the singular forms "a," "an," and "the" can be intended to include the plural forms as well, unless the context clearly indicates otherwise.

[0038] Furthermore, when a part is said to "comprise" a certain component, this does not mean that it may exclude other components, but may further include other components, unless specifically stated to the contrary.

[0039] Furthermore, unless otherwise specified in the present invention, when a layer or member is said to be "on" another layer or member, this includes not only the case where a layer or member is in contact with the other layer or member, but also the case where another layer or member exists between the two layers or two members.

[0040] Furthermore, the terms "about," "substantially," and the like, as used herein, are used to mean a numerical value or a approximation thereof when tolerances for manufacturing and materials inherent in the stated meaning are given, and are used to prevent unscrupulous infringers from unfairly exploiting disclosures in which precise or absolute numerical values ​​are stated to aid in the understanding of the present invention.

[0041] In one aspect of the present invention, a method for producing molybdenum oxychloride by reacting molybdenum metal, chlorine gas, and oxygen is described in detail below.

[0042] First, molybdenum metal is used in the form of powder to increase the contact area between chlorine and oxygen in the gas phase. Examples of powders are not particularly limited, but include those having an average particle size (D 50 ) of about 0.01 mm to 2 mm may be used, and the smaller the average particle size, the higher the reaction rate, which is preferable. Preferably, particles of 0.05 to 0.5 mm may be used.

[0043] The production method and the apparatus will be described below with reference to the molybdenum oxychloride precursor production apparatus shown in Fig. 1. Fig. 1 illustrates one embodiment of the present invention, and the production apparatus of the present invention is not limited to this.

[0044] The manufacturing apparatus 100 of the present disclosure includes a reactor 10, a condensation tank 20, a filter unit 30 including a first filter unit 31 and a second filter unit 32, and a storage tank 40, arranged in this order.

[0045] More specifically, the reactor 10 is configured to charge molybdenum powder, chlorine gas, and oxygen, and heat the charged mixture to produce crude molybdenum oxychloride; a condensation vessel 20 for condensing the gaseous crude molybdenum oxychloride transferred from the reactor into a solid phase on its surface; a filter unit 30 including a first filter unit 31 and a second filter unit 32 for liquefying the solidified product in the condensation tank and then removing solid impurities contained in the liquefied product; A storage tank 40 for storing the product purified by the filter unit They are arranged in that order.

[0046] First, the reactor will be described as follows.

[0047] The reactor 10 includes a molybdenum powder injection tube 11, a chlorine gas injection tube 12, an oxygen injection tube 13, a vacuum purge, a nitrogen inlet tube 14, and a transfer tube 15 for transferring the reactants in the reactor to a condensation tank, and the reactor may be equipped with temperature and pressure control devices.

[0048] The reaction temperature of the reactor may be 250 to 400° C., but is not particularly limited thereto.

[0049] In the production apparatus, the condensation tank 20 condenses the crude molybdenum oxychloride synthesized in the reactor 10. The condensation tank 20 is cooled to a temperature of 100°C or less, 80°C or less, 60°C or less, or 40°C or less, e.g., -10 to 100°C, 0 to 100°C, or a temperature between these values, and the gaseous product is collected by condensing it as a solid on the surface of the condensation tank 20 through the transfer pipe 15 of the reactor 10. After collection, nitrogen is introduced from the reactor to purge and remove chlorine gas and other by-products from the condensation tank 20. The condensation tank further heats the condensed product to liquefy it, and then transfers the liquid product to the filter unit 30, which serves as a purification unit. It also functions as a buffer between the reactor 10 and the filter unit 30. That is, the reactants of each batch in the reactor are continuously stored in the condensation tank so that they can be continuously reacted in the reactor. In order to liquefy the product condensed in the condensation tank 20, it is necessary to raise the temperature to 100 to 250°C for liquefaction. The liquefaction temperature is not particularly limited as long as it is within the above range, but it is preferable to liquefy the product by heating to 110 to 250°C, 120 to 220°C, or 120 to 180°C.

[0050] The condensation tank 20 may be provided with a discharge pipe 21 capable of discharging impurities by nitrogen purging introduced from the reactor, and a liquid transfer pipe 22 for transferring the liquefied product of the condensation tank to a filter section.

[0051] The filter unit 30 removes additional solid impurities contained in the liquefied product introduced from the condensation tank 20. The filter unit 30 may have a first filter unit 31 having relatively large pores and a second filter unit 32 having relatively small pores. The filter unit may have a single filter unit having fine pores, but this may require frequent replacement due to the filtering load, which may result in process burden and reduced productivity. Therefore, two or more filter units having different pores may be arranged in sequence for purification. Through such a purification filter, high-purity molybdenum oxychloride of 99.999 wt% or higher can be obtained.

[0052] The pore size of the first filter section 31 may be 5 to 50 μm, and the pore size of the second filter section 32 may be 1 to 30 μm, preferably 1 to 20 μm, more preferably 5 to 10 μm, or may be a size between these numerical values. That is, the pore size of the first filter section 31 may be larger than the pore size of the second filter section 32.

[0053] The temperature of the filter section is not particularly limited as long as the molybdenum oxychloride is safely present in a liquid phase, and it is preferable to maintain the temperature at, for example, 150 to 250°C, preferably 180 to 220°C, and more preferably 200°C, in order to achieve a satisfactory filtering effect.

[0054] The material of the filter of the filter portion is not particularly limited as long as it is a material that is stable against molybdenum oxychloride, and it is preferable to use a sintered filter, which is advantageous in terms of stability.

[0055] The product purified in the filter unit 30 may be stored in a storage tank 40 in a liquefied state, maintained at the same temperature as the filter unit or at a different temperature, and then bagged in a liquid state. After being packaged, the product may be solidified in the packaged state at room temperature and sold.

[0056] The manufacturing method will be described below.

[0057] The manufacturing method of the present disclosure includes: a reaction step of charging molybdenum powder, chlorine gas, and oxygen into a reactor and heating to produce molybdenum oxychloride (MoO2Cl2); a solidification and condensation step of transferring the reactants from the reactor to a condensation tank and solidifying them on the surface of the condensation tank; a liquefaction step of heating the solidified product in the solidification and condensation step to convert it into a liquid phase; a purification step of filtering the liquefied product to increase its purity; The present invention provides a method for producing molybdenum oxychloride (MoO2Cl2), comprising:

[0058] The molybdenum oxychloride (MoO2Cl2) produced in the reaction step may be crude molybdenum oxychloride.

[0059] The reaction step is not particularly limited as long as the temperature is such that the reaction can be carried out, but the reaction may be carried out at 250 to 400°C, for example.

[0060] In one embodiment, the method may further include a step of cooling the reactor after the reaction step to solidify the product, and discharging unreacted oxygen and chlorine using nitrogen purging or vacuum means. The cooling temperature is not particularly limited as long as it is a temperature at which the product solidifies inside the reactor, and may be, for example, 0 to 100°C.

[0061] In yet another embodiment, the solidification and condensation step can be performed under reduced pressure. In this case, the product can be easily transferred from the reactor to the condensation tank and solidified on the surface of the condensation tank, which is more preferable.

[0062] The condenser on which the molybdenum oxychloride has solidified on its surface can be purged with nitrogen or evacuated at the solidification temperature to further remove unreacted chlorine gas and by-products, for example, metal chlorides such as tungsten chloride that have reacted with tungsten contained in molybdenum metal and various impurity metals.

[0063] In one embodiment, the solidification and condensation step can be performed at the temperature of the reactor, or if a discharge step is included, the vaporized product can be reheated to 120 to 400°C and transferred to a condenser at 0 to 100°C, where it can be solidified into crystals on the surface of the condenser.

[0064] After the product is solidified in the condenser or solidified and purified, a liquefaction step is carried out in which the solidified product in the condenser is heated to liquefy. The temperature range during the liquefaction step can be 110 to 250°C, and is not particularly limited as long as the temperature is within the above temperature range, but preferably, the product may be heated to 110 to 220°C, or 120 to 180°C.

[0065] The liquefied product is transferred to a filter unit and filtered to perform a purification step, which is accomplished by filtering through two or more filter units having different pores.

[0066] In the purification step, the filter unit is a first filter unit having pores of 5 to 50 μm and a second filter unit having pores of 1 to 30 μm, thereby providing a method for producing molybdenum oxychloride (MoO2Cl2) with a purity of 99.9999% or more. The first filter unit may have a larger pore size than the second filter unit.

[0067] In yet another embodiment, the method may further include bagging the molybdenum oxychloride (MoO2Cl2) after the filtering step.

[0068] One embodiment may be a method for producing MoO2Cl2, in which the temperature is maintained at 180 to 220°C from the filtering step to the bagging step, and MoO2Cl2 is maintained in a liquid phase.

[0069] In still another embodiment, the production method may be such that when unreacted oxygen and chlorine are discharged in the discharge step, they are discharged after purging with nitrogen.

[0070] In yet another aspect of the present disclosure, in the production method, the purity of the molybdenum oxychloride may be 99.999% by weight or more.

[0071] In the present disclosure, after the product is transferred from the reactor to the condensation tank, the inside of the reactor is purged and cleaned, and then molybdenum powder, chlorine gas, and oxygen are again introduced to react. The solidified product in the condensation tank is then liquefied and purified, allowing for continuous post-processing and shipping, which significantly increases productivity and enables the production of products with excellent purity.

[0072] The present disclosure will be specifically described below using the following examples. However, the following examples are provided to explain one embodiment for understanding the technical content of the present invention, and the present disclosure is not limited to the following examples.

[0073] The average particle size is D 50 means D 50 The average particle size is calculated from the particle size distribution of particles collected according to ISO 13320-1 and analyzed using a Microtrac S3500.

[0074] Purity was analyzed using ICP_MS (Agilent, ICP-MS 7900s).

[0075] In an acrylic glove box with the air replaced with dedicated N2 gas, approximately 0.1 g of sample was collected using a spatula and placed in a 100 ml HDPE bottle. The weight of the collected sample was precisely measured using a scale capable of measuring to four decimal places.

[0076] After preparing a mixed acid with a concentration of 2% HNO3 and 1% HF, 50 g of the prepared mixed acid was added to the sampled HDPE bottle. After adding the mixed acid, the weight was measured again using a balance capable of measuring to four decimal places and recorded.

[0077] The sample to which the mixed acid had been added was subjected to ultrasonic treatment for 10 minutes using an ultrasonic cleaner.

[0078] The analysis was performed using an ICP-MS 7900s. To do this, a standard solution was prepared for the analytical instrument, and a calibration curve was established before quantitative analysis of the samples. 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.

[0079] Example 1 Average particle size (D 50 Molybdenum metal powder with a particle size of 0.1 mm was filled into a reactor at 1 / 5 volume and heated to 350°C. Chlorine gas and oxygen were then introduced through a gas supply pipe to synthesize MoO2Cl2. The vaporized MoO2Cl2 was transferred to a condensation tank maintained at 60°C, and the product was thoroughly solidified on the surface of the condensation tank. A vacuum (30 torr) was then applied to the reactor to remove unreacted chlorine gas and impurities. A purge was then introduced from the reactor, and nitrogen was purged up to the condensation tank and then discharged from the condensation tank to remove further unreacted materials and impurities. The purity of the molybdenum oxychloride was 99.99 wt% as determined by ICP-MS analysis.

[0080] Next, the reactor and condensation tank were isolated, and molybdenum metal powder was again added to the reactor, followed by oxygen and chlorine gas for further batch reaction. At the same time, the reactants in the condensation tank were isolated from the outside and heated to 200°C for liquefaction. The mixture was then filtered successively through a first sintered filter with 10 μm pores and a second sintered filter with 5 μm pores. The resulting molybdenum oxychloride had a purity of 99.9998 wt%. [Explanation of symbols]

[0081] 100 Manufacturing equipment 10. Reactor 11 Molybdenum powder injection tube 12 Chlorine gas injection pipe 13 Oxygen injection tube 14 Vacuum purge and nitrogen inlet tube 15 Transfer pipe 20 Condensation tank 21 Discharge pipe 22 Liquid transfer tube 30 Filter section 31 First filter section 32 Second filter section 40 Storage Tank

Claims

1. Molybdenum powder, chlorine gas, and oxygen were charged into a reactor and heated to produce molybdenum oxychloride (MoO ２ Cl ２ a reaction step to produce a solidification and condensation step of transferring the reactants from the reactor to a condensation tank and solidifying them on the surface of the condensation tank; a liquefaction step of heating the solidified product in the solidification and condensation step to convert it into a liquid phase; a purification step of filtering the liquefied product to increase its purity; A method for producing molybdenum oxychloride, comprising:

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

3. 2. The method of claim 1, further comprising the step of cooling the reactor after the reacting step to solidify the product and venting unreacted oxygen and chlorine using a nitrogen purge or vacuum means.

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

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

6. 2. The method for producing molybdenum oxychloride according to claim 1, further comprising a purification step of purging with nitrogen or applying a vacuum after the solidification and condensation step to further remove unreacted chlorine gas and by-products.

7. 2. The method for producing molybdenum oxychloride according to claim 1, wherein the solidification and condensation step is a step of adjusting the temperature of the reactor to 120 to 400°C or, in the case of a discharge step, transferring the vaporized product by reheating at 120 to 400°C to a condenser at 0 to 100°C and solidifying it as crystals on the surface of the condenser.

8. 2. The method for producing molybdenum oxychloride according to claim 1, wherein the liquefaction is carried out by raising the temperature of a condenser in the liquefaction step to 110 to 250°C.

9. 2. The method for producing molybdenum oxychloride according to claim 1, wherein the purification step comprises filtering using two or more filters having different pores.

10. 10. The method for producing molybdenum oxychloride according to claim 9, wherein the purification step comprises filtering using a first filter section having pores of 5 to 50 μm and a second filter section having pores of 1 to 30 μm.

11. 2. The method for producing molybdenum oxychloride according to claim 1, wherein the purification step is maintained at 180 to 250° C., and the molybdenum oxychloride exists in a liquid phase.

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

13. a reactor into which molybdenum powder, chlorine gas, and oxygen are introduced and heated to produce crude molybdenum oxychloride; a condensation vessel for condensing the gaseous crude molybdenum oxychloride transferred from the reactor into a solid phase on its surface; a filter unit including a first filter unit and a second filter unit for removing solid impurities contained in the liquefied product introduced after liquefying the solidified product in the condensation tank; a storage tank for storing the product purified by the filter unit; The molybdenum oxychloride manufacturing equipment is arranged in that order.

14. 14. The apparatus for producing molybdenum oxychloride according to claim 13, wherein the reactor comprises a molybdenum powder injection tube, a chlorine gas injection tube, an oxygen injection tube, a vacuum purge and nitrogen inlet tube, and a transfer tube for transferring the reactants in the reactor to a condensation tank.

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

16. 14. The apparatus for producing molybdenum oxychloride according to claim 13, wherein the filter unit comprises a first filter unit having relatively large pores and a second filter unit having relatively small pores, in that order.

17. 17. The apparatus for producing molybdenum oxychloride according to claim 16, wherein the first filter unit is a sintered filter having a pore size of 10 to 30 μm, and the second filter unit is a sintered filter having a pore size of 5 to 10 μm.

18. 14. The apparatus for producing molybdenum oxychloride according to claim 13, wherein the filter unit and the storage tank are maintained at 180 to 220°C.

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