Vinylsilane gas production method and production device

Abstract

To provide a manufacturing method for vinylsilane gas which continuously refines vinylsilane gas, and inexpensively and safely fills high purity vinylsilane gas obtained by this result, and a manufacturing apparatus for the same.SOLUTION: A manufacturing method for vinylsilane gas includes a generation step of generating vinylsilane, a refining step of refining the generated vinylsilane, and a filling step of filling a filling container with the refined vinylsilane. The refining step includes a first refining step of separating a high boiling point substance from the vinylsilane generated in the generation step, and returning the separated high boiling point substance to the generation step, and a second refining step of further separating a high boiling point substance from the separated vinylsilane. The filling step cools the filling container to a temperature equal to or lower than a solidification point of the vinylsilane, fills the filling container with the vinylsilane, and removes a low boiling point substance from the solidified vinylsilane.SELECTED DRAWING: Figure 1

Description

[Technical Field]

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

[0002] Regarding methods for producing vinylsilanes, for example, Patent Document 1 (JP 2004-256494 A) discloses a method in which acetylene and a silane compound are reacted in the presence of a titanium compound to produce vinylsilane, and further, Patent Document 2 (International Publication WO2006 / 064628) discloses a method in which a vinylsilane is obtained by reacting a vinyl halide compound with a silicon halide compound in an aprotic solvent in the presence of aluminum.

[0003] However, vinylsilane gas, which has the CAS number 7291-09-0 and the structural formula CH2=CH-SiH3, is not currently produced industrially, and there is no integrated manufacturing process that combines the conventional methods of generation, purification, and filling. However, there are liquefied high-pressure gases with similar properties, such as carbon dioxide and organosilane gas, and there are several precedents for their purification, including reports of high-purity gases that use solidification with liquid nitrogen and vacuum evacuation.

[0004] For example, Patent Document 3 (JP 2012-240870 A) discloses an apparatus for purifying and supplying ultra-high purity liquefied carbon dioxide gas, which includes a liquefied carbon dioxide gas supply unit that supplies liquefied carbon dioxide gas recovered from a container filled with liquefied carbon dioxide gas or an apparatus using liquefied carbon dioxide gas, a vaporization unit that vaporizes the liquefied natural gas supplied from the liquefied carbon dioxide gas supply unit to leave high-boiling point liquid or solid impurities and discharge gaseous carbon dioxide gas from the gas phase, a liquefaction unit that liquefies the gaseous carbon dioxide gas, and a gas-liquid separator that separates the liquefied carbon dioxide gas from the liquefaction unit into gas and liquid and has a discharge pipe equipped with a discharge valve that discharges low-boiling point impurities outside the system, and a supply passage that supplies the high-purity liquefied carbon dioxide gas separated and purified by the gas-liquid separation unit to an apparatus using ultra-high purity liquefied carbon dioxide gas via a supply valve.

[0005] Furthermore, Patent Document 4 (JP 2001-48519 A) discloses a purification method in which partially substituted fluorosilane gas contained as an impurity of a low boiling point component is cooled in a container and evacuated in a solidified state, or in which the partially substituted fluorosilane gas is cooled in a container, evacuated in a solidified state, and then vaporized, cooled again, and evacuated in a solidified state. [Prior art documents] [Patent documents]

[0006] [Patent Document 1] Japanese Patent Application Laid-Open No. 2004-256494 [Patent Document 2] International Publication WO2006 / 064628 [Patent Document 3] Japanese Patent Application Laid-Open No. 2012-240870 [Patent Document 4] Japanese Patent Application Laid-Open No. 2001-48519 Summary of the Invention [Problem to be solved by the invention]

[0007] As described above, the methods disclosed in Patent Documents 3 and 4 increase the yield of carbon dioxide and organosilane gas recovery while removing only nitrogen and oxygen gases with lower boiling points than carbon dioxide and organosilane gases. However, with these methods, only the lower boiling point gas components, nitrogen and oxygen, are removed for purification, and high boiling point substances are not removed. Furthermore, for typical organosilane gases, a separation-type production method is used in which the gas is first liquefied and then transferred to a separate distillation apparatus, followed by distillation. After distillation, the gas is compressed to liquefaction pressure using a compression pump and filled. With vinylsilane gas, adiabatic compression using a compression pump can lead to rapid reactions, making it difficult to use a compression pump.

[0008] The present invention has been made in view of the above points, and provides a method and apparatus for producing vinylsilane that can remove high-boiling and low-boiling substances that are mixed in when vinylsilane is generated, and that can perform purification and filling safely and at low cost. [Means for solving the problem]

[0009] Therefore, the present invention provides a method for producing vinylsilane, which comprises at least a generation step of continuously generating vinylsilane, a purification step of purifying the generated vinylsilane, and a filling step of filling a filling container with the purified vinylsilane. The purification step comprises a first purification step of separating high-boiling substances from the vinylsilane generated in the generation step and returning the separated high-boiling substances to the generation step, and a second purification step of further separating high-boiling substances from the separated vinylsilane. In the filling step, the filling container is cooled to a temperature below the freezing point of vinylsilane, and vinylsilane is filled into the filling container, while low-boiling substances are removed from the filling container.

[0010] As a result, in the present invention, the majority of high-boiling substances other than vinylsilane generated in the generation stage, such as the raw materials vinyltrichlorosilane (melting point: -95°C, boiling point: 91.5°C), vinyldichlorosilane, and vinylchlorosilane, and the solvents tetrahydrofuran (melting point: -108.4°C, boiling point: 66°C) and dibutyl ether (melting point: -97.9°C, boiling point: 142°C), are removed in the purification stage and returned to the generation stage, and the vinylsilane further purified in the purification stage can be solidified and recovered in the charging stage, making it possible to remove low-boiling substances (such as oxygen, nitrogen, and argon gas) in the charging stage.

[0011] In addition, in the present invention, it is desirable that the generation stage be adjusted to a first temperature that is a predetermined value higher than the boiling point of the solvent used, and that the first purification stage be composed of an intermediate stage in which the temperature is adjusted to a second temperature that is a predetermined value lower than the first temperature, and a solvent recovery stage in which the temperature is adjusted to a third temperature in the range from the freezing point of the solvent used in the generation stage to the second temperature.

[0012] As a result, in the generation stage, the temperature is adjusted to a first temperature higher than the boiling point of the solvent, causing the vinylsilane and solvent to vaporize and reach the intermediate stage. In the intermediate stage, the temperature is adjusted to a second temperature that is a predetermined value lower than the first temperature, allowing the solvent to be sufficiently liquefied and returned to the generation stage. Furthermore, in the solvent recovery stage following the intermediate stage, the temperature is adjusted to a third temperature that is above the freezing point of the solvent and below the second temperature, causing most of the solvent to be liquefied. Here, the liquefied solvent is returned to the generation stage via the intermediate stage, thereby suppressing temperature drops in the generation stage and allowing vinylsilane gas to be continuously generated in the generation stage.

[0013] Furthermore, the second purification step is preferably adjusted to a fourth temperature that is higher than the liquefaction temperature of vinylsilane at atmospheric pressure and lower by a predetermined value than the boiling point of the high-boiling substance.

[0014] As a result, the vinylsilane passing through the second purification stage is in the gas phase and the high boiling point substances are in the liquid phase, and the high boiling point substances are dropped in the second purification stage, so that the vinylsilane and the high boiling point substances are separated.

[0015] Furthermore, during the filling step, the filling container is preferably adjusted to a fifth temperature that is a predetermined value lower than the freezing point of vinylsilane. In particular, the fifth temperature is preferably equal to or higher than the melting point of the low-boiling substance and equal to or lower than the freezing point of vinylsilane.

[0016] As a result, the vinylsilane gas that has reached the filling stage solidifies in the filling vessel as the vessel is adjusted to the fifth temperature during the filling stage, and accumulates as a solid phase within the filling vessel. At this time, since the low-boiling point substances remain in the gas or liquid phase, the low-boiling point substances (oxygen, nitrogen, argon gas, etc.) can be removed from the vinylsilane by suction.

[0017] It is also desirable that the filled container be cooled gradually from the bottom to the top.

[0018] This ensures that vinylsilane is accumulated in the filling container from the bottom of the container.

[0019] Furthermore, the generating step, the purifying step, and the filling step are carried out at a concentration of 1×10 -2 It is desirable to have a sealed structure that can block the penetration of low-boiling-point substances at pressures of Torr or less (hereinafter referred to as high vacuum).

[0020] This prevents low boiling point substances, particularly oxygen, from entering the path along which the flammable vinylsilane travels, ensuring safety.

[0021] Furthermore, it is desirable to completely prevent the intrusion of impurity gases such as oxygen, nitrogen, and moisture by using a highly airtight structure so as to ensure a high degree of vacuum, and in particular to prevent decomposition and polymerization of vinylsilane due to the intrusion of moisture.

[0022] Preferably, the filling step is performed by alternately and intermittently filling with vinylsilane gas and evacuating to a vacuum.

[0023] The present invention provides a vinylsilane production system comprising at least a generator that continuously generates vinylsilane, a purification device that purifies the generated vinylsilane, a filling device that fills a filling container with the purified vinylsilane, and a suction device that transfers vinylsilane from the generator to the purification device and the filling device.The purification device comprises a first purification device that separates high-boiling-point substances from the vinylsilane generated in the generator and returns the separated high-boiling-point substances to the generator, and a second purification device that further separates high-boiling-point substances from the separated vinylsilane.The filling device comprises a cooling device that cools the filling container to a temperature below the freezing point of vinylsilane, and a suction device that suctions low-boiling-point substances from the filling container.

[0024] As a result, in the present invention, the vinylsilane generated in the generator and the high-boiling substances contained therein, such as the raw materials vinyltrichlorosilane (melting point: -95°C, boiling point: 91.5°C), vinyldichlorosilane, and vinylchlorosilane, and the solvents tetrahydrofuran (melting point: -108.4°C, boiling point: 66°C) and dibutyl ether (melting point: -97.9°C, boiling point: 142°C), are largely removed in the purification device and returned to the generator, and the vinylsilane further purified in the purification device can be solidified and recovered in the charging device, making it possible to remove low-boiling substances such as oxygen, nitrogen, and argon gas in the charging device.

[0025] It is also desirable that the generator be adjusted to a first temperature that is a predetermined value higher than the boiling point of the solvent, and that the first purification device be composed of an intermediate container adjusted to a second temperature that is a predetermined value lower than the first temperature, and a solvent recovery container adjusted to a third temperature in the range from the freezing point of the solvent used in the generator to the second temperature.

[0026] Furthermore, it is preferable that the first purification device is disposed vertically relative to the generator, so that the gas generated in the generator rises to the first purification device, while the high-boiling-point substance liquefied in the first purification device can freely fall.

[0027] Furthermore, it is desirable that the temperature of the second purification device be adjusted to a predetermined value higher than the liquefaction temperature of vinylsilane at atmospheric pressure. Furthermore, the second purification device may be configured as an upright column of a predetermined height to ensure a reaction distance, or the reaction distance may be ensured by connecting multiple separation vessels in series. The high-boiling-point substances separated in the second purification device may be accumulated in a predetermined location or may be circulated to the generator.

[0028] The filling device preferably includes a cooling device that adjusts the temperature of the filling container to a predetermined value lower than the freezing point of vinylsilane, and a suction device that moves vinylsilane from the generator through the purification device to the upstream side of the filling container. The cooling device preferably cools the filling container with liquid nitrogen.

[0029] As a result, the vinylsilane sucked up to the upstream side of the filling container by the suction device is sucked into the filling container and solidified as the filling container cools. This allows the vinylsilane to be accumulated. Furthermore, by providing multiple filling containers in parallel, it becomes possible to fill them sequentially.

[0030] Furthermore, it is desirable that the cooling device gradually cools the filled container from the bottom toward the top, thereby solidifying the vinylsilane in order from the bottom of the container, thereby efficiently accumulating the vinylsilane in the filled container.

[0031] Furthermore, the generating device, the purifying device, and the filling device are configured to perform the 1×10 -2It is desirable to have a sealed structure that can block the penetration of low-boiling-point substances at pressures below Torr (high vacuum).

[0032] This makes it possible to prevent oxygen in the air from being mixed into the flammable vinylsilane passing through the device.

[0033] It is also desirable that the suction device alternately and intermittently fill and exhaust the vinylsilane, thereby enabling exhaust from the filled container and releasing the low-boiling-point substance in the filled container into the atmosphere. [Effects of the Invention]

[0034] As described above, the present invention enables the generation, purification, and filling of highly reactive vinylsilane gas in a short time, efficiently, and safely. Unlike typical reactive gas purification methods such as adsorption and liquefaction distillation, this method offers the advantage of being continuous and does not require large-scale equipment, unlike liquefaction followed by purification. Furthermore, in the case of flammable and highly reactive vinylsilane, this method offers the advantage of eliminating the possibility of ignition due to adiabatic compression in the compression pump used for liquefaction, thereby enabling efficient purification. [Brief explanation of the drawings]

[0035] [Figure 1] FIG. 1 is a schematic diagram illustrating the outline of the device according to the present invention. DETAILED DESCRIPTION OF THE INVENTION

[0036] The method for producing vinylsilane according to the present invention comprises at least a generation step of continuously generating vinylsilane, a purification step of purifying the generated vinylsilane, and a filling step of filling a filling container with the purified vinylsilane.

[0037] In the generation step, vinylsilane gas is generated from a required amount of raw material, such as vinyltrichlorosilane (melting point: -95°C, boiling point: 91.5°C), supplied from a raw material supply device, and a solvent, such as tetrahydrofuran (melting point: -108.4°C, boiling point: 66°C) or dibutyl ether (melting point: -97.9°C, boiling point: 142°C). However, the vinylsilane gas generated in the generation step contains high-boiling-point substances such as the solvent. The generation step is also adjusted to a first temperature that is higher by a predetermined value than the boiling point of the solvent used.

[0038] The purification step comprises a first purification step in which high-boiling substances are separated from the vinylsilane generated in the generation step and the separated high-boiling substances are returned to the generation step, and a second purification step in which further high-boiling substances are separated from the separated vinylsilane.

[0039] The first purification step comprises an intermediate step in which the temperature is adjusted to a second temperature that is a predetermined temperature lower than the first temperature, and a separation step in which the temperature is adjusted to a third temperature in the range from the freezing point of the solvent used in the generation step to the second temperature, and the second purification step is adjusted to a fourth temperature that is higher than the liquefaction temperature of vinylsilane at atmospheric pressure and lower than the boiling point of the high-boiling substance.

[0040] In the first purification stage, the high-boiling substances are liquefied in an intermediate stage adjusted to a second temperature that is a predetermined temperature lower than the first temperature, and most of the high-boiling substances are liquefied in a separation stage adjusted to a third temperature, and the resulting mixture is returned to the generation stage via the intermediate stage. By providing the intermediate stage, the temperature drop in the generation stage can be suppressed, thereby maintaining continuous generation of vinylsilane gas in the generation stage.

[0041] In the filling step, the container is cooled to a temperature below the freezing point of vinylsilane to fill the container with vinylsilane and remove low-boiling-point substances from the solidified vinylsilane. To this end, the container is adjusted to a temperature lower than the freezing point of vinylsilane by a predetermined value, and the container is gradually cooled from the bottom to the top. Furthermore, in the filling step, the filling of vinylsilane gas and the evacuation are alternately and intermittently performed.

[0042] This allows the vinylsilane to be efficiently accumulated in the filling vessel, and also allows low boiling point substances such as oxygen to be efficiently removed.

[0043] Furthermore, the generating step, the purifying step, and the filling step are carried out at a concentration of 1×10 -2 It has a sealed structure that can block the intrusion of low-boiling-point substances at pressures below Torr (high vacuum), which prevents the intrusion of oxygen from the outside and ensures the reliable absorption of vinylsilane from the generation stage to the filling stage. [Example]

[0044] As shown in FIG. 1, the vinylsilane production apparatus 1 according to the present invention comprises at least a generator D equipped with a generator vessel D1 for continuously generating vinylsilane, a purifier B for purifying the generated vinylsilane, and a filling apparatus C for filling the purified vinylsilane into filling vessels C1 and C2.

[0045] The generator D generates vinylsilane gas using a required amount of raw material, such as vinyltrichlorosilane (melting point: -95°C, boiling point: 91.5°C), and a solvent, such as tetrahydrofuran (melting point: -108.4°C, boiling point: 66°C) or dibutyl ether (melting point: -97.9°C, boiling point: 142°C), supplied from the raw material supply device A (raw material container A1 and solvent container A2). However, the vinylsilane gas generated in the generator D contains high-boiling-point substances such as the solvent. The generator D is also adjusted to a first temperature T1, which is higher by a predetermined value than the boiling point of the solvent used.

[0046] The purification unit B comprises a first purification unit BA which separates high boiling substances from the vinylsilane generated in the generation unit D and returns the separated high boiling substances to the generation unit D, and a second purification unit BB which further separates high boiling substances from the separated vinylsilane.

[0047] Here, the first purification device BA is composed of an intermediate vessel B1 adjusted to a second temperature T2 that is a predetermined temperature lower than the first temperature T1, and a separation vessel B2 adjusted to a third temperature T3 in the range from the freezing point of the solvent used in the generator D to the second temperature T2. Furthermore, the second purification vessel BB is adjusted to a fourth temperature T4 that is higher than the liquefaction temperature of vinylsilane at atmospheric pressure and lower than the boiling point of the high-boiling substance.

[0048] In the first purification apparatus BA, high boiling point substances are liquefied in intermediate vessel B1, which is adjusted to a second temperature T2 that is a predetermined temperature lower than the first temperature T1, and most of the high boiling point substances are liquefied in separation vessel B2, which is adjusted to a third temperature T3, and the liquefied liquor is returned to generator D via intermediate vessel B1. By providing intermediate vessel B1, a decrease in the temperature of generator D can be suppressed, thereby maintaining continuous generation of vinylsilane gas in generator D.

[0049] Furthermore, the first purifier BA is disposed vertically relative to the generator D. This allows the gas generated in the generator D to rise to the first purifier BA, while the high-boiling-point substances liquefied in the first purifier BA can freely fall and return to the generator D via the intermediate vessel B1.

[0050] Furthermore, the second purification apparatus BB is adjusted to a third temperature T3, which is a predetermined value higher than the liquefaction temperature of vinylsilane at atmospheric pressure. The second purification apparatus BB may be configured as an upright tower of a predetermined height to ensure a reaction distance, or a plurality of separation vessels B3, B4, B5, and B6 may be connected in series to ensure the reaction distance. The high-boiling-point substances separated in the second purification apparatus BB may be accumulated in a predetermined location or may be circulated to the generator D. The high-boiling-point substances separated in the first purification apparatus BB are recovered in a recovery vessel E, but may also be returned to the generator D.

[0051] Furthermore, in the filling device C, the filling containers C1 and C2 are cooled to a temperature below the freezing point of vinylsilane to fill the filling containers C1 and C2 with vinylsilane, and low-boiling-point substances are removed from the solidified vinylsilane. To this end, the filling device C adjusts the filling containers C1 and C2 to a temperature (fifth temperature T5) that is a predetermined value lower than the freezing point of vinylsilane, and the filling containers C1 and C2 are gradually cooled from the bottom to the top. Furthermore, in the filling device C, the filling and exhaust of vinylsilane gas are alternately and intermittently performed.

[0052] This allows vinylsilane to be efficiently accumulated in the filling vessels C1 and C2, and also allows low boiling point substances such as oxygen to be efficiently removed.

[0053] Furthermore, the generator D, the purifier B and the filling device C are suctioned by a vacuum pump P to achieve a 1×10 -2It has a sealed structure that can block the intrusion of low-boiling-point substances at pressures below Torr (high vacuum). This prevents oxygen from entering from the outside, and ensures that vinylsilane can be sucked in reliably from the generator D to the filling device C.

[0054] To implement the above control, the present invention provides on-off valves V1 to V9. In the vinylsilane production apparatus 1 configured as described above, the raw material (vinyltrichlorofuran) and the solvent (tetrahydrosilane) serving as a high-boiling substance supplied from the material supply device A are heated and stirred in the generation vessel D1 of the generator D to a first temperature T1 (approximately 80°C), which is a predetermined value higher than the boiling point temperature of the solvent (e.g., 66°C). The vaporized vinylsilane and solvent are then elevated through the intermediate vessel B1, which is adjusted to a second temperature (e.g., 5 to 10°C), to the separation vessel B2, which is adjusted to a third temperature (e.g., −40°C). In the intermediate vessel B1 and the separation vessel B2, the vinylsilane remains in a gaseous state, while the solvent (high-boiling substance) is liquefied and returned to the generation vessel D1. When it is confirmed that a sufficient amount of vinylsilane gas has been generated in the separation vessel B2, the on-off valves V1, V2, and V5 are opened, and the vacuum pump P is driven to introduce the gas in the separation vessel B2 into the second purification device BB.

[0055] In the second purification unit BB, multiple separation vessels B3, B4, B5, and B6 are installed side by side, and the separation vessels B3, B4, B5, and B6 are connected in series. The high-boiling-point substances separated in the separation vessels B3, B4, B5, and B6 are collected in a collection vessel E.

[0056] In addition, when filling the filling container B1 with vinylsilane from the second purification device BB, for example, to reduce the pressure in the filling container C1, the on-off valve V3 is closed and the on-off valves V4 and V7 are opened simultaneously. This allows the filling container C1 to be evacuated by the vacuum pump P, while the filling container C1 is cooled by the cooling device F. The on-off valves V5, V6, and V7 are closed simultaneously with the on-off valves V2, V3, and V4 being opened. The vinylsilane gas that has passed through the second purification device BB is drawn into the filling container C1, where it cools, solidifies, and fills the filling container C1. After this, the on-off valve V3 is closed, the on-off valves V4 and V7 are opened, and the vacuum pump P is used to evacuate the filling container C1, releasing low-boiling substances (e.g., oxygen, nitrogen, argon gas, etc.) present in the gas phase within the filling container C1 to the outside air. By intermittently alternately performing this filling operation and the vacuuming of the low-boiling substances, the vinylsilane can be efficiently filled and the low-boiling substances can be removed.

[0057] Furthermore, when the filling container C1 becomes full, by operating the on-off valves V6, V8, and V9 in the same manner instead of the on-off valves V3, V4, and V7, it is possible to similarly fill the filling container C2 with vinylsilane and remove low-boiling substances. [Explanation of symbols]

[0058] 1 Manufacturing equipment A Material supply device B Purification equipment BA No. 1 Refining Unit BB Second refinery C Filling device D generator E. Collection container F Cooling device P Vacuum pump V1~V9 on-off valves

Claims

1. A method for producing vinylsilane represented by the structural formula CH2=CH-SiH3, comprising at least a generating step of continuously generating vinylsilane, a purifying step of purifying the vinylsilane by removing high-boiling substances from the generated vinylsilane, and a filling step of filling a filling vessel with the purified vinylsilane and removing low-boiling substances from the filling vessel, the generating step is adjusted to a first temperature higher than the boiling point of a high-boiling substance contained in the vinylsilane to be generated; the purification step comprises a first purification step in which high boiling point substances are separated from the vinylsilane generated in the generation step and the separated high boiling point substances are returned to the generation step, and a second purification step in which the high boiling point substances are further separated from the separated vinylsilane; the first purification stage is composed of an intermediate stage adjusted to a second temperature lower than the first temperature, and a solvent recovery stage adjusted to a third temperature higher than the freezing point of the high-boiling substance used in the generation stage and lower than the second temperature; the second purification step is adjusted to a fourth temperature higher than the liquefaction temperature of the vinylsilane at atmospheric pressure and lower than the boiling point of the high-boiling substance; in the filling step, the filling vessel is cooled to a fifth temperature lower than the freezing point of vinylsilane to fill the filling vessel with vinylsilane, and low-boiling-point substances contained in the vinylsilane are removed from the filling vessel by evacuation; The high-boiling substance is one or more substances selected from vinyltrichlorosilane, vinyldichlorosilane, vinylchlorosilane, tetrahydrofuran, and dibutyl ether; and The method for producing vinylsilane, wherein the low-boiling substance is one or more substances selected from the group consisting of oxygen, nitrogen, and argon.

2. 2. The method for producing vinylsilane according to claim 1, wherein the filled container is cooled gradually from the bottom to the top.

3. The generating step, the purifying step, and the filling step are carried out at 1×10 －２ 3. The method for producing vinylsilane according to claim 1, wherein the reactor has a sealed structure capable of blocking the intrusion of low-boiling substances at a pressure of Torr or less.

4. In the filling step, filling of the vinylsilane gas and removal of the low boiling point substance by evacuation are alternately and intermittently carried out, and the removal by evacuation is carried out at a rate of 1×10 －２ 4. The method for producing vinylsilane according to claim 1, wherein the method is carried out at a pressure of Torr or less.

5. An apparatus for producing vinylsilane represented by the structural formula CH2=CH-SiH3, comprising at least a generator for continuously generating vinylsilane, a purifier for purifying the generated vinylsilane by removing high-boiling substances from the vinylsilane, a filling device for filling a filling container with the purified vinylsilane and removing low-boiling substances from the filling container, and a suction device for transferring vinylsilane from the generator to the purifier and the filling device, the generator is adjusted to a first temperature higher than the boiling point of a high-boiling substance contained in the vinylsilane to be generated; the purification device comprises a first purification device that separates high boiling point substances from the vinylsilane generated in the generation device and returns the separated high boiling point substances to the generation device, and a second purification device that further separates high boiling point substances from the separated vinylsilane; the first purification device is composed of an intermediate vessel adjusted to a second temperature lower than the first temperature, and a solvent recovery device adjusted to a third temperature higher than the freezing point of the high-boiling-point substance used in the generation device and lower than the second temperature; the second purification device is adjusted to a fourth temperature that is higher than the liquefaction temperature of the vinylsilane at atmospheric pressure and lower than the boiling point of the high-boiling substance; and the filling device cools the filling container to a fifth temperature that is lower than the freezing point of vinylsilane, filling the filling container with vinylsilane, and removing low-boiling-point substances contained in the vinylsilane from the filling container by evacuation; The high-boiling substance is one or more substances selected from vinyltrichlorosilane, vinyldichlorosilane, vinylchlorosilane, tetrahydrofuran, and dibutyl ether; and 1. The vinylsilane production apparatus, wherein the low-boiling substance is one or more substances selected from the group consisting of oxygen, nitrogen, and argon.

6. 6. The vinylsilane production apparatus according to claim 5, wherein the first purification device is disposed vertically relative to the generator.

7. The generator, the purifier, and the filling device are suctioned at 1×10 －２ 7. The vinylsilane production apparatus according to claim 5, further comprising a sealed structure capable of blocking the intrusion of low-boiling-point substances at a pressure of Torr or less.

8. The suction device alternately and intermittently fills with vinylsilane gas and removes low-boiling-point substances by evacuation, and the removal by evacuation is 1×10 －２ 8. The vinylsilane production apparatus according to claim 5, wherein the reaction is carried out at a pressure of Torr or less.

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