Method for manufacturing molybdenum oxychloride and manufacturing apparatus thereof

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 (WF 6 Tungsten hexafluoride is a major precursor material in semiconductor wiring processes in fields such as 3D NAND flash where copper plating is difficult to use due to the high aspect ratio. However, tungsten hexafluoride has problems in the manufacturing process, such as high resistance and etching caused by fluorine remaining in the molecule on the substrate, so it is necessary to develop a new precursor material to solve these problems.

[0003] To solve these problems, a technology has been developed to use 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 MoO 3 A method for producing molybdenum oxychloride by reacting powder with chlorine gas has been disclosed, and a solution using a glass reactor as an integrated reactor has also been disclosed, but the glass reactor is difficult to handle and is a batch reactor having an integrated structure, and the productivity is not sufficient, which is also an obstacle to commercial mass production.

[0004] The above MoO 3 The process of reacting molybdenum metal 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 device that can react molybdenum metal with chlorine gas and oxygen at low temperatures, enable semi-continuous manufacturing such as semi-batch, increase productivity, and efficiently manufacture a molybdenum oxychloride precursor with high purity. [Prior art documents]

Patent Document

[0005]

Patent Document 1

Summary of the Invention

Problems to be Solved by the Invention

[0006] One aspect of the present invention provides a method for manufacturing molybdenum oxychloride with significantly improved productivity.

[0007] Another aspect of the present invention provides an apparatus for manufacturing molybdenum oxychloride with significantly improved productivity.

[0008] Furthermore, another aspect of the present invention provides a manufacturing method and its manufacturing apparatus for increasing productivity and manufacturing high - purity molybdenum oxychloride.

Means for Solving the Problems

[0009] As a result of intensive research by the present inventors to solve the above problems, a new manufacturing method and manufacturing apparatus for synthesizing high - purity molybdenum oxychloride can be provided. This manufacturing apparatus is a manufacturing apparatus designed for manufacturing high - purity molybdenum oxychloride, in which a reactor, a condenser, and a purification device are connected in that order.

[0010] By using the above - mentioned manufacturing apparatus, reactants (or reacted substances) can be continuously transferred to a manufacturing apparatus including a reactor, a condenser, and a purification device for recovery and purification. Therefore, this manufacturing system supports a semi - continuous manufacturing method for semi - batch production. These manufacturing methods and manufacturing apparatuses show that they can significantly increase the productivity of high - purity molybdenum oxychloride as the final product.

[0011] In one embodiment of the present invention, molybdenum powder, chlorine gas, and oxygen are charged into a reactor and heated to produce molybdenum oxychloride (MoO 2 Cl 2 and a reaction step of producing 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 product solidified 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 the steps of:

[0012] In one embodiment, the reaction step may be carried out at 250-400°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 in the discharging step may be 0 to 100°C.

[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 still another embodiment, the solidification and condensation step may be a step of adjusting the temperature of the reactor to 120 to 400°C or, in the case of having a discharge step, transferring the vaporized product reheated at 120 to 400°C to a condenser at 0 to 100°C and solidifying it 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 can be performed at a temperature maintained at 180 to 250° C., preferably 180 to 220° C., and the molybdenum oxychloride can be present in a liquid phase.

[0022] In one embodiment, the purity of the molybdenum oxychloride produced by the above 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, comprising 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 that order.

[0024] In one embodiment, the apparatus for producing molybdenum oxychloride comprises: a reactor into which molybdenum powder, chlorine gas and oxygen are charged 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 section including a first filter section and a second filter section for removing solid impurities contained in the liquefied product introduced after liquefying the product solidified in the condensation tank, A storage tank for storing the product purified by the filter section May be arranged in that order.

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

[0026] In yet another embodiment, the condensation tank 20 may be provided with a discharge pipe 21 for discharging impurities by nitrogen purge introduced from the reactor and a liquid transfer pipe 22 for transferring the liquefied product of the condensation tank to the filter section.

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

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

[0029] In one embodiment, the filter section and the storage tank may be a production apparatus for molybdenum oxychloride maintained at 180 to 220°C. Other features and aspects will also become apparent from the following detailed description, drawings, and claims.

Effect 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 the semi-batch method.

[0031] Furthermore, by performing the reaction step and the purification step separately, 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 reactants and transfer them to the purification step, and the molybdenum oxychloride solidified on the surface of the condensation tank is 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 filtering out impurities by sequentially connecting the first filter section and the second filter section. [Brief description of the drawings]

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

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

[0036] Further, 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 the present invention belongs. The terms used in the description of the present invention are merely for the purpose of effectively describing a particular embodiment 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 described as "comprising" a certain component, this means that it may further include other components, rather than excluding 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 two layers or two members.

[0040] Additionally, as used herein, the terms "about," "substantially," and the like are used in a numerical or approximate sense when the tolerances of manufacture and materials inherent in the recited meaning are given, and are used to prevent unscrupulous infringers from unfairly taking advantage of disclosures in which precise or absolute numerical values ​​are recited 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 the powder are not particularly limited, but include, for example, powders 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, the particle size is 0.05 to 0.5 mm.

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

[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 that order.

[0045] More specifically, the reactor 10 is a reactor into which molybdenum powder, chlorine gas, and oxygen are charged and heated to produce crude molybdenum oxychloride; a condensation tank 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 product solidified in the condensation tank and then removing solid impurities contained in the liquefied product to be introduced; A storage tank 40 for storing the product purified by the filter unit is provided. 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 above-mentioned manufacturing apparatus, the condensation tank 20 functions to condense the gaseous product in a solid phase on the surface of the condensation tank 20 through the transfer pipe 15 of the reactor 10 in a state where the temperature of the condensation tank 20 is cooled to 100°C or less, 80°C or less, 60°C or less, 40°C or less, for example, -10 to 100°C, 0 to 100°C, or a temperature between the above values, so that the crude molybdenum oxychloride synthesized in the reactor 10 can be condensed. After being collected, nitrogen is introduced from the reactor to purge and remove the chlorine gas and other by-products in the condensation tank 20. Furthermore, the condensation tank functions to liquefy the condensed product by heating it, and then to transfer the product in a liquid state to the filter unit 30, which is a purification unit, and also functions to act 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 liquefy the product by heating to 100 to 250°C. 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 equipped 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 product liquefied and 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 one filter unit having fine pores, but this may require frequent replacement due to the filtering load, which may cause a process burden and a decrease in productivity. Therefore, two or more filter units having different pores may be arranged in sequence for purification, and high-purity molybdenum oxychloride of 99.999 wt% or more can be provided through such a purification filter.

[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 the above 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 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 good 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 with respect to molybdenum oxychloride, and it is preferable to use a sintered filter, which is advantageous in terms of stability.

[0055] The product refined in the filter unit 30 may be stored in a storage tank 40 in a liquefied state, either at the same temperature as the filter unit or at a different temperature, and then bagged in the 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: Molybdenum powder, chlorine gas, and oxygen are charged into a reactor and heated to produce molybdenum oxychloride (MoO 2 Cl 2 and a reaction step of producing 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 product solidified 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; Molybdenum oxychloride (MoO 2 Cl 2 ) production method.

[0058] The molybdenum oxychloride (MoO 2 Cl 2 ) may be crude molybdenum oxychloride.

[0059] The reaction step may be carried out at any temperature, for example, 250 to 400° C., although there are no particular limitations as long as the reaction is possible.

[0060] In one embodiment, after the reaction step, the reactor is cooled to solidify the product, and the unreacted oxygen and chlorine are discharged using nitrogen purge or vacuum means. The cooling temperature is not particularly limited as long as the product is solidified inside the reactor, and may be, for example, 0 to 100°C.

[0061] In yet another embodiment, the solidification and condensation step can be carried out under reduced pressure. In the case of the reduced pressure, the product can be easily transferred from the reactor to the condensation tank and can be 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 the molybdenum metal and various impurity metals.

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

[0064] After the product is solidified in the condenser and solidified or purified, a liquefaction step is performed in which the product solidified in the condenser is heated to liquefy. The temperature range during the liquefaction step may be 110 to 250°C, and is not particularly limited as long as the temperature is within the above temperature range, but may be preferably 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 the liquefied product 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, and the purity of the molybdenum oxychloride (MoO 2 Cl 2 The first filter portion may have a larger pore size than the second filter portion.

[0067] In yet another embodiment, after the filtering step, molybdenum oxychloride (MoO 2 Cl 2 The method may further include the step of bagging the container.

[0068] In one embodiment, the temperature is maintained at 180 to 220°C from the filtering step to the bagging step, and MoO 2 Cl 2 MoO maintains a liquid phase 2 Cl 2 The manufacturing method may be as follows:

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

[0070] In still 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, and the solidified product in the condensation tank is liquefied and purified, so that the subsequent steps can be continuously carried out and the product can be shipped, which can significantly increase productivity and produce products with excellent purity.

[0072] The present disclosure will be specifically described below using the following examples. However, the following examples are merely for explaining 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 by taking a sample of the particles to be measured according to the ISO 13320-1 standard and analyzing it with a Microtrac S3500.

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

[0075] Acrylic glove box with dedicated N 2 After replacing the gas, a spatula was used to collect approximately 0.1 g of sample into 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] 2% HNO 3 After preparing a mixed acid with a concentration of 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 scale 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 instrument. To this end, a standard solution was prepared for the analytical instrument, and a calibration curve was obtained, after which the 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.

[0079] Example 1 Average particle size (D 50 Molybdenum metal powder with a diameter of 0.1 mm was filled into the reaction vessel at 1 / 5 of its volume, heated at 350°C, and then chlorine gas and oxygen were introduced from the gas supply pipe to form MoO 2 Cl 2 The vaporized MoO 2 Cl 2 The product was transferred to a condensation tank maintained at 60°C, and the product was thoroughly solidified on the surface of the condensation tank. Next, a vacuum (30 torr) was applied from the reactor to discharge unreacted chlorine gas and impurities. A purge was also introduced from the reactor, and nitrogen was purged up to the condensation tank and discharged from the condensation tank to remove further unreacted materials and impurities. Here, the purity of the molybdenum oxychloride was 99.99 wt% as a result of analysis using ICP_MS.

[0080] Next, the reactor and the condensation tank were isolated, and molybdenum metal powder was again added to the reactor, and oxygen and chlorine gas were added to perform a batch reaction. At the same time, the reactants in the condensation tank, which liquefies the reactants, were isolated from the outside of the condensation tank and liquefied by raising the temperature to 200°C. Then, the mixture was filtered through a first filter, which was a sintered filter with 10 μm pores, and a second sintered filter with 5 μm pores in succession. As a result, the purity of the obtained molybdenum oxychloride was 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 are charged into a reactor and heated to produce molybdenum oxychloride (MoO ２ C ２ and a reaction step of producing 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 product solidified 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 steps 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. 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 a reactor to 120 to 400° C. or, in the case of having a discharge step, transferring a product vaporized by reheating at 120 to 400° C. to a condenser at 0 to 100° C. and solidifying it as crystals on a 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 180-250° C. and the molybdenum oxychloride is 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 charged 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 product solidified in the condensation tank; A storage tank for storing the product refined 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 includes a molybdenum powder injection tube, a chlorine gas injection tube, an oxygen injection tube, a vacuum purge and nitrogen introduction 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 section.

16. 14. The apparatus for producing molybdenum oxychloride according to claim 13, wherein the filter section includes a first filter section having relatively large pores and a second filter section 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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