Method for preparing molybdenum oxychloride and apparatus for preparing same

Abstract

The present invention relates to a method and an apparatus for preparing high-purity molybdenum oxychloride. Specifically, the present invention relates to a method for preparing molybdenum oxychloride and an apparatus for preparing same, the method comprising: a reaction step for adding molybdenum powder, chlorine gas, and oxygen to a reactor and heating the reactants to prepare molybdenum oxychloride (MoO2Cl2); a solidification and condensation step in which the reaction product in the reactor is transferred from the reactor to a condenser and solidified on the surface of the condenser; a liquefaction step for heating the product solidified in the solidification and condensation step and thereby converting the product into a liquid phase; and a purification step for filtering the product liquefied in the liquefaction step and thereby increasing the purity of the product.

Description

Method for producing molybdenum oxychloride and apparatus for producing the same

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

[0002] Tungsten hexafluoride (WF6) has been primarily used as a semiconductor wiring material in applications where copper plating is difficult due to its high aspect ratio, such as 3D NAND flash. However, WF6's use is limited by the presence of fluorine in its molecules, which remains on the substrate and acts as a foreign substance, increasing resistance and causing etching. Therefore, the development of a replacement material is necessary.

[0003] As an alternative material, a technology has been developed to use molybdenum oxychloride as a molybdenum precursor for semiconductor wiring. For example, Korean Patent Publication No. 2022-0131312 discloses a manufacturing method for producing molybdenum oxychloride by reacting MoO3 powder with chlorine gas. Furthermore, a glass reactor is known for manufacturing molybdenum oxychloride using an integrated glass reactor. However, this batch reactor, which has an integrated structure, is difficult to handle and has insufficient productivity, hindering commercialization.

[0004] The above process of reacting MoO3 with chlorine gas requires a relatively high reaction temperature of approximately 800°C, and has the problem of slow reaction rates at low temperatures. Therefore, there is a need for a manufacturing method and manufacturing apparatus that can react molybdenum metal with chlorine gas and oxygen at low temperatures and enable semi-continuous production, such as semi-batch, to increase productivity while producing a high-purity molybdenum oxychloride precursor.

[0005] (Patent Document 1) Korean Patent Publication No. 2022-0131312 (September 27, 2022)

[0006] The present disclosure provides a method for producing molybdenum oxychloride with significantly improved productivity.

[0007] The present disclosure provides a device for manufacturing molybdenum oxychloride with significantly improved productivity.

[0008] In addition, the present disclosure provides a manufacturing method and a manufacturing apparatus for manufacturing high-purity molybdenum oxychloride while simultaneously increasing productivity.

[0009] As a result of careful examination by the inventors of the present invention to solve the above problem, a new method and apparatus for producing molybdenum oxychloride were provided, in which a reactor, a condenser, and a purification device for synthesizing high-purity molybdenum oxychloride are sequentially connected.

[0010] By using the above manufacturing device, the reactants (or reacted materials) are continuously transferred to the reactor, condenser, and purification device for recovery and purification, thereby enabling semi-continuous manufacturing such as semi-batch production, thereby significantly increasing productivity and providing high-purity molybdenum oxychloride.

[0011] One aspect of the present disclosure comprises a reaction step of introducing molybdenum powder, chlorine gas, and oxygen into a reactor and heating the reactor to produce molybdenum oxychloride (MoO2Cl2).

[0012] A solidification and condensation step in which the reactants of the above reactor are transferred from the reactor to a condenser and solidified on the surface of the condenser.

[0013] A liquefaction step in which the solidified product in the above solidification and condensation step is heated to convert it into a liquid phase, and

[0014] A purification step in which the liquefied product is filtered in the above liquefaction step to increase its purity;

[0015] It provides a method for producing molybdenum oxychloride including .

[0016] In one embodiment, the reaction step may be performed at 250 to 400°C.

[0017] Another embodiment may further include a discharge step of cooling the reactor after the above reaction step to solidify the product inside the reactor and discharge unreacted oxygen and chlorine using nitrogen purge or vacuum means.

[0018] In one embodiment, the cooling temperature in the discharge step may be 0 to 100°C.

[0019] Another embodiment may be that the solidification step is performed under reduced pressure.

[0020] In one embodiment, after the solidification condensation step in the condenser, a purification step may be further included to additionally remove unreacted chlorine gas and by-products by purging with nitrogen or applying a vacuum.

[0021] As another embodiment, the solidification and condensation step may be a step of controlling the temperature of the reactor to 120 to 400°C or, if it has a discharge step, reheating the vaporized product to 120 to 400°C and transferring it to a condenser at 0 to 100°C to solidify it into crystals on the surface of the condenser.

[0022] In one embodiment, the liquefaction step of liquefying the product in a condenser after the solidification condensation step may be performed by raising the temperature of the condenser to 110 to 250°C.

[0023] As another embodiment, the purification step performed after the liquefaction step may be performed by filtering and purifying using a filter unit including two or more filter units having different pores.

[0024] In one embodiment, the purification step may be filtering using a first filter unit having pores of 5 to 50 μm and a second filter unit having pores of 1 to 30 μm.

[0025] As another embodiment, the purification step may be performed at a temperature of 180 to 250°C, preferably 180 to 220°C, such that the molybdenum oxychloride is present in a liquid phase.

[0026] In one embodiment, the purity of molybdenum oxychloride manufactured by the above manufacturing method may be 99.999 wt% or higher.

[0027] Another aspect of the present disclosure can provide a molybdenum oxychloride production device sequentially arranging a reactor (10), a condenser (20), a filter unit (30) including a first filter unit (31) and a second filter unit (32), and a storage tank (40).

[0028] In one embodiment, the molybdenum oxychloride manufacturing device comprises a reactor that inputs molybdenum powder, chlorine gas, and oxygen and heats the reactor to manufacture crude molybdenum oxychloride.

[0029] A condenser that condenses crude molybdenumoxychloride in a gaseous state transferred from the above reactor into a solid state on the surface;

[0030] A filter unit including a first filter unit and a second filter unit for removing solid impurities included in the liquefied product introduced after liquefying the solidified product in the above condenser, and

[0031] It may be possible to sequentially arrange storage tanks for storing the purified product in the above filter section.

[0032] In one embodiment, the reactor (10) may be a molybdenum oxychloride production device including a molybdenum powder injection tube (11), a chlorine gas injection tube (12), an oxygen injection tube (13), a vacuum purge and nitrogen introduction tube (14), and a transfer tube (15) for transferring the reactants of the reactor to a condenser (20).

[0033] As another embodiment, the condenser (20) may be provided with a discharge pipe (21) that can discharge impurities by nitrogen purge introduced from the reactor and a liquid transfer pipe (22) that transfers the liquefied product of the condenser to a filter unit.

[0034] In one embodiment, the filter unit (30) may be a molybdenum oxychloride manufacturing device that sequentially includes a first filter unit (31) having relatively large pores and a second filter unit (32) having relatively small pores.

[0035] As another embodiment, a molybdenum oxychloride manufacturing device may be provided in which the first filter unit (31) is a sintered filter having a pore size of 10 to 30 μm, and the second filter unit (32) is a sintered filter having a pore size of 5 to 10 μm.

[0036] In one embodiment, the filter unit and storage tank may be a molybdenum oxychloride manufacturing device maintained at 180 to 220°C.

[0037] According to the present disclosure, a method and apparatus for producing a molybdenum oxychloride precursor having the same effect as a semi-batch can be provided.

[0038] Additionally, by separating the reaction stage and the purification stage, new reactions can be performed even during the purification stage, thereby increasing production volume.

[0039] In addition, a separate condenser is provided to recover the reactants between the reaction stage and the purification stage and to transfer them to the purification stage, and the molybdenum oxychloride solidified on the surface of the condenser is purged with nitrogen once again to remove unreacted chlorine and other impurities, thereby further increasing the purity.

[0040] In addition, according to the present manufacturing method, the purity can be increased to 99.999% or more by sequentially connecting the first filter part and the second filter part to filter out impurities.

[0041] Figure 1 is a schematic diagram of an apparatus for synthesizing molybdenum oxychloride.

[0042] 100: Manufacturing equipment

[0043] 10: Reactor

[0044] 11: Molybdenum powder injection tube, 12: Chlorine gas injection tube, 13: Oxygen injection tube

[0045] 14: Vacuum purge and nitrogen introduction pipe, 15: Transfer pipe

[0046] 20: Condenser 21: Discharge pipe 22: Liquid transfer pipe

[0047] 30: Filter section 31: First filter section 32: Second filter section

[0048] 40: Storage tank

[0049] 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 implemented in various forms.

[0050] Additionally, unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention pertains. The terminology used herein is for the purpose of describing specific embodiments only and is not intended to be limiting.

[0051] Additionally, the singular forms used in the specification and the appended claims are intended to include the plural forms as well, unless the context clearly dictates otherwise.

[0052] Additionally, when a part is said to "include" a component, this does not mean that it excludes other components, but rather that it may include other components, unless otherwise specifically stated.

[0053] Additionally, unless otherwise specifically defined in the present invention, when a layer or member is said to be located “on” another layer or member, this includes not only cases where a layer or member is in contact with another layer or member, but also cases where another layer or member exists between the two layers or two members.

[0054] In addition, the terms "about", "substantially", etc. used in this specification are used in a meaning close to or at the numerical value when manufacturing and material tolerances inherent to the meanings mentioned are presented, and are used to prevent unscrupulous infringers from unfairly using the disclosure contents in which exact or absolute values ​​are mentioned to aid understanding of the present invention.

[0055] 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.

[0056] First, molybdenum metal is used in powder form to increase the contact area with gaseous chlorine and oxygen. Examples of powders are not particularly limited, but include average particle diameter (D 50 ) can be used with an average particle size of 0.01 mm to 2 mm, and a smaller average particle size is preferred because the reaction speed increases. Preferably, a particle size of 0.05 to 0.5 mm can be used.

[0057] Hereinafter, the manufacturing method and the device thereof will be described with reference to the molybdenum oxychloride precursor manufacturing device of Fig. 1. Fig. 1 illustrates one embodiment of the present invention, and the manufacturing device of the present invention is not limited thereto.

[0058] The manufacturing device (100) of the present disclosure is provided with a reactor (10), a condenser (20), a filter unit (30) including a first filter unit (31) and a second filter unit (32), and a storage tank (40) arranged sequentially.

[0059] More specifically, a reactor (10) for producing crude molybdenum oxychloride by introducing molybdenum powder, chlorine gas, and oxygen and heating the same.

[0060] A condenser (20) that condenses crude molybdenumoxychloride in a gaseous state transferred from the above reactor into a solid state on the surface;

[0061] After liquefying the solidified product in the above condenser, a filter unit (30) including a first filter unit (31) and a second filter unit (32) for removing solid impurities included in the liquefied product introduced, and

[0062] Storage tanks (40) for storing the purified product in the above filter section are arranged sequentially.

[0063] First, let me explain the reactor as follows.

[0064] The above reactor (10) includes a molybdenum powder injection tube (11), a chlorine gas injection tube (12), an oxygen injection tube (13), a vacuum purge and nitrogen introduction tube (14), and a transfer tube (15) for transferring the reactants of the reactor to a condenser, and the reactor may be equipped with a temperature and pressure control device.

[0065] The reaction temperature of the above reactor may be 250 to 400°C, but is not particularly limited thereto.

[0066] In the above manufacturing device, the condenser (20) serves to condense the crude molybdenumoxychloride synthesized from the reactor (10), by cooling the temperature of the condenser (20) to 100°C or lower, 80°C or lower, 60°C or lower, 40°C or lower, for example, -10 to 100°C, 0 to 100°C, and a temperature between the above values, and to condense the gaseous product into a solid state on the surface of the condenser (20) through the transfer pipe (15) of the reactor (10) and recovering the product. After recovery, nitrogen is introduced from the reactor to purge and remove chlorine gas or other by-products in the condenser. In addition, the condensed product is heated to liquefy it, and then transferred to the filter unit (30), which is a purification unit, in a liquid state, and also serves 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 condenser so that they can be continuously reacted in the reactor. In order to liquefy the product condensed in the condenser (20), it is necessary to liquefy it by raising the temperature to 100 to 250°C, and the liquefaction temperature is not particularly limited as long as it is within the above range, but preferably, it may be liquefied by heating to 110 to 250°C, 120 to 220°C, or 120 to 180°C.

[0067] The above condenser (20) may be equipped with a discharge pipe (21) that can discharge impurities by nitrogen purge introduced from the reactor and a liquid transfer pipe (22) that transfers the liquefied product of the condenser to the filter unit.

[0068] The above filter unit (30) removes additional solid impurities included in the product introduced as a liquefaction from the condenser (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. Although the filter unit may have one filter unit having micropores, it may have a filtering load and need to be replaced frequently, which may cause a burden on the process and a decrease in productivity. Therefore, at least two or more filter units having different pores may be sequentially arranged to perform purification, and high-purity molybdenum oxychloride of 99.999 wt% or more may be provided through such a purification filter.

[0069] The pore size of the first filter unit (31) may be a filter of 5 to 50 μm, and the pore size of the second filter unit (32) may be 1 to 30 μm, preferably 1 to 20 μm, and even more preferably 5 to 10 μm, and may have a size between the above values. That is, the pore size of the first filter unit (31) may be larger than the pore size of the second filter unit (32).

[0070] The above filter section does not specify the temperature as long as the molybdenum oxychloride is safely present in a liquid state, and for example, it is preferred to maintain it at 150 to 250°C, preferably 180 to 220°C, and even more preferably 200°C for the filtering effect.

[0071] The filters of the above filter section are not particularly limited in terms of material, and are not limited to materials that are stable to molybdenum oxychloride. It is preferable to use a sintered filter as it is advantageous in terms of stability.

[0072] The product purified in the filter unit (30) is stored in the storage tank (40) in a liquefied state at a temperature that is the same as or different from that of the filter unit, and then packaged in a liquid state (bagging), and after packaging, solidified in the packaged state at room temperature and sold.

[0073] The manufacturing method is described below.

[0074] The manufacturing method of the present disclosure comprises a reaction step of introducing molybdenum powder, chlorine gas, and oxygen into a reactor and heating to manufacture molybdenum oxychloride (MoO2Cl2);

[0075] A solidification and condensation step in which the reactants of the above reactor are transferred from the reactor to a condenser and solidified on the surface of the condenser.

[0076] A liquefaction step in which the solidified product in the above solidification and condensation step is heated to convert it into a liquid phase, and

[0077] A purification step in which the liquefied product is filtered in the above liquefaction step to increase its purity;

[0078] A method for producing molybdenum oxychloride (MoO2Cl2) including the above can be provided.

[0079] The molybdenum oxychloride (MoO2Cl2) produced in the above reaction step may be crude molybdeniumoxychloride.

[0080] The above reaction step is not particularly limited as long as the reaction temperature is possible, but for example, the reaction may be performed at 250 to 400°C.

[0081] In one embodiment, after the reaction step, the reactor may be cooled to solidify the product and an additional exhaust step may be provided to exhaust unreacted oxygen and chlorine using nitrogen purge or vacuum means. The cooling temperature is not particularly limited as long as it is the temperature at which the product solidifies within the reactor, but may be, for example, 0 to 100°C.

[0082] Another embodiment may be a manufacturing method in which the solidification and condensation step is performed under reduced pressure. This is preferred because it allows the product from the reactor to be easily transferred to the condenser and solidified on the surface of the condenser.

[0083] The condenser on which the above molybdenum oxychloride is solidified on the surface can be purged with nitrogen or vacuumed at the solidification temperature to additionally remove unreacted chlorine gas and by-products, such as metal chlorides such as tungsten chloride that have reacted with various impurity metals, such as tungsten contained in molybdenum metal.

[0084] As an example, the solidification condensation step may be performed by reheating the vaporized product to 120 to 400°C at the temperature of the reactor or, if it has a discharge step, transferring the vaporized product to a condenser at 0 to 100°C to solidify it into crystals on the surface of the condenser.

[0085] After the above product is solidified or solidified and purified in a solidified condenser, a liquefaction step is performed to liquefy the solidified product in the condenser by heating it. The temperature range during the temperature increase in the liquefaction step needs to be raised to 110 to 250°C to liquefy it, and there are no particular limitations on the temperature so long as it is within the above temperature range, but preferably, it can be liquefied by heating it to 110 to 220°C, 120 to 180°C.

[0086] The above liquefied product is transferred to a filter section and undergoes a purification step by being filtered. The purification step is completed by filtering in two or more filter sections having different pores.

[0087] In the above purification step, the filter unit may be 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) having a purity of 99.9999% or higher. The first filter unit may have pores larger in size than the second filter unit.

[0088] Another embodiment may further include a step of bagging molybdenum oxychloride (MoO2Cl2) after the filtering step.

[0089] 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 so that MoO2Cl2 remains in a liquid phase.

[0090] Another embodiment may be a manufacturing method in which nitrogen is purged and discharged when emitting unreacted oxygen and chlorine in the discharge step.

[0091] Another aspect of the present disclosure may be that the purity of molybdenum oxychloride may be 99.999 wt% or more by the above manufacturing method.

[0092] In the present disclosure, after transferring the product from the reactor to the condenser, the inside of the reactor is purged and cleaned, and then molybdenum powder, chlorine gas, and oxygen are re-introduced to cause a reaction, and at the same time, the solidified product in the condenser is continuously processed through liquefaction and purification steps to be shipped to the next step, so that productivity can be significantly increased and a product with excellent purity can be manufactured.

[0093] Hereinafter, the present disclosure will be specifically described using the following examples. However, the following examples are intended to illustrate specific examples for understanding the technical contents of the present disclosure, and the present disclosure is not limited to the following examples.

[0094] The average particle size is referred to as D50, which is the particle size of particles that constitute 50% of the total volume. The average particle size can be derived from the particle size distribution results analyzed using MICROTRAC's S3500 after collecting samples according to the ISO 13320-1 standard for the particles being measured.

[0095] Purity was analyzed using ICP_MS (Agilent, ICP-MS 7900s).

[0096] In an acrylic glove box, with dedicated N₂ gas replaced, a spatula was used to collect approximately 0.1 g of a 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.

[0097] 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.

[0098] For the sample with mixed acid added, ultrasonic treatment was performed for 10 minutes using an ultrasonic cleaner.

[0099] Analysis was conducted using an ICP-MS 7900s instrument. To this end, standard solutions for the analytical instrument were prepared, a calibration curve was established, 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.

[0100]

[0101] (Example 1)

[0102] Molybdenum metal powder with an average particle size (D50) of 0.1 mm was charged to 1 / 5 of the volume of a reaction vessel, heated at 350°C, and then chlorine gas and oxygen were introduced from a gas supply pipe to synthesize MoO2Cl2. The vaporized MoO2Cl2 was transferred to a condenser maintained at 60°C, and the product was sufficiently solidified on the surface of the condenser. Subsequently, a vacuum (30 torr) was applied from the reactor to discharge unreacted chlorine gas and impurities. Again, a purge was introduced from the reactor, and nitrogen was purged to the condenser and discharged from the condenser to remove additional unreacted products and impurities. At this time, the purity of the molybdenum oxychloride was 99.99 wt% as analyzed using ICP-MS.

[0103] Next, the reactor and the condenser were shut off, and molybdenum metal powder was again introduced into the reactor, followed by oxygen and chlorine gas to perform an additional batch reaction. At the same time, the reactant in the condenser, which liquefies the reactant, was shut off from the outside of the condenser, and the temperature was raised to 200°C to liquefy it. Thereafter, the reactant was filtered by passing it continuously through the first filter, which was a sintered filter with pores of 10 μm, and the second sintered filter with pores of 5 μm. The purity of the molybdenum oxychloride obtained as a result was 99.9998 wt%.

Claims

1. Molybdenum powder, chlorine gas, and oxygen are added to the reactor and heated to produce molybdenum oxychloride (MoO 2 Cl 2 ) reaction step for manufacturing, A solidification and condensation step in which the reactants of the above reactor are transferred from the reactor to a condenser and solidified on the surface of the condenser. A liquefaction step in which the solidified product in the above solidification and condensation step is heated to convert it into a liquid phase, and A purification step for increasing purity by filtering the liquefied product in the above liquefaction step; A method for producing molybdenum oxychloride comprising:

2. In paragraph 1, A method for producing molybdenum oxychloride, wherein the above reaction step is performed at 250 to 400°C.

3. In paragraph 1, A method for producing molybdenum oxychloride, further comprising a discharge step of cooling the reactor after the above reaction step to solidify the product and discharging unreacted oxygen and chlorine using a nitrogen purge or vacuum means.

4. In paragraph 3, A method for producing molybdenum oxychloride, wherein the cooling temperature is 0 to 100°C.

5. In paragraph 1, A method for producing molybdenum oxychloride, wherein the above solidification and condensation step is performed under reduced pressure.

6. In paragraph 1, A method for producing molybdenum oxychloride, comprising, after the above solidification and condensation step, further comprising a purification step of additionally removing unreacted chlorine gas and by-products by purging with nitrogen or applying a vacuum.

7. In paragraph 1, A method for producing molybdenum oxychloride, wherein the above-mentioned solidification and condensation step is a step of controlling the temperature of the reactor to 120 to 400°C or, if it has a discharge step, reheating the vaporized product to 120 to 400°C and transferring it to a condenser at 0 to 100°C to solidify it into crystals on the surface of the condenser.

8. In paragraph 1, A method for producing molybdenum oxychloride, wherein the temperature of the condenser in the above liquefaction step is increased to 110 to 250°C to liquefy.

9. In paragraph 1, A method for producing molybdenum oxychloride, wherein the above purification step is performed by filtering using two or more filters having different pores.

10. In paragraph 9, A method for producing molybdenum oxychloride, wherein the above purification step is performed by 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. In paragraph 1, A method for producing molybdenum oxychloride, wherein the above purification step is maintained at 180 to 250°C so that molybdenum oxychloride exists in a liquid phase.

12. In paragraph 1, A method for producing molybdenum oxychloride, wherein the purity of molybdenum oxychloride produced by the above method is 99.999 wt% or higher.

13. A reactor for producing crude molybdenum oxychloride by adding molybdenum powder, chlorine gas, and oxygen and heating it. A condenser for condensing crude molybdenumoxychloride in a gaseous state transferred from the above reactor into a solid state on the surface; A filter unit including a first filter unit and a second filter unit for removing solid impurities included in the liquefied product introduced after liquefying the solidified product in the above condenser, and A molybdenum oxychlorite manufacturing device having storage tanks sequentially arranged to store the purified product in the above filter section.

14. In paragraph 13, A molybdenum oxychloride manufacturing device, wherein the reactor comprises 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 of the reactor to a condenser.

15. In paragraph 13, A molybdenum oxychloride manufacturing device, wherein the condenser is equipped with a discharge pipe capable of discharging impurities by nitrogen purge introduced from a reactor and a liquid transfer pipe for transferring the liquefied product of the condenser to a filter unit.

16. In paragraph 13, A molybdenum oxychloride manufacturing device, wherein the filter section sequentially includes a first filter section having relatively large pores and a second filter section having relatively small pores.

17. In paragraph 16, A molybdenum oxychloride manufacturing device, wherein the first filter part is a sintered filter having a pore size of 10 to 30 μm, and the second filter part is a sintered filter having a pore size of 5 to 10 μm.

18. In Article 13 A molybdenum oxychloride manufacturing device wherein the filter unit and storage tank are maintained at 180 to 220°C.

Images