Disilane upgrading device
By designing a silane purification device with internal temperature control components and purification equipment, the problems of complex structure and poor adaptability of existing equipment were solved, achieving efficient and safe silane purification, and reducing maintenance difficulty and production costs.
Patent Information
- Application Number
- CN202520278888.9
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- Filing Date
- 2025-02-21
- Publication Date
- 2025-12-05
- Estimated Expiration
- 2035-02-21
AI Technical Summary
In existing silane preparation processes, the upgrading equipment has a complex structure, is inconvenient to maintain, requires a lot of space, and has poor adaptability to different preparation processes, resulting in high production costs and significant safety risks.
A silane refining device was designed, comprising a cylinder, a temperature control component, a nozzle, a purification device, and a circulation pump. The temperature is regulated by the temperature control component, silane is dissolved by liquid ammonia, and impurities are adsorbed by the purification device, enabling both intermittent and continuous operation modes to adapt to different preparation processes.
The simplified device structure reduced maintenance difficulty, decreased space requirements, improved adaptability, reduced production costs and safety risks, and achieved efficient silane purification.
Smart Images
Figure CN223628374U_ABST
Abstract
Description
TECHNICAL FIELD
[0001] The utility model relates to the technical field of ethylsilane purification, in particular to an ethylsilane upgrading device. BACKGROUND
[0002] Ethylsilane is an inorganic compound, chemical formula is H6Si2, is colorless transparent gas at normal temperature and pressure, has irritating smell. In air, burns, concentration is above 0.2% when burning emits flame, concentration is below 0.2%, then, oxidation reaction generates white silica. Contact with sulfur hexafluoride then explodes. Ethylsilane can burn in air, ignition point is below room temperature, meets air and instantaneously burns, and decomposes into SiH4 and H2.
[0003] The existing ethylsilane preparation process often adopts: halogenated ethylsilane reduction method, silicon-magnesium alloy method and silane direct synthesis method, can produce silane, propylsilane and chlorosilane and other impurity gases, then the crude ethylsilane obtained by reaction is treated by rectification method, gasification method, adsorption method and other methods to obtain finished ethylsilane, however, the existing upgrading device structure is relatively complex, is not convenient for maintenance, and has higher space requirement. UTILITY MODEL CONTENT
[0004] The utility model aims at providing an ethylsilane upgrading device to solve the above-mentioned deficiencies in the prior art.
[0005] In order to realize the above-mentioned purpose, the utility model provides the following technical scheme:
[0006] An ethylsilane upgrading device, comprising a cylinder, a gas inlet is formed in the bottom of the cylinder, and a waste gas outlet and a connecting port are respectively formed in the top; a temperature control assembly is arranged outside the cylinder and is used for adjusting the temperature in the cylinder; a spray head is arranged inside the cylinder and is located below the waste gas outlet and is communicated with an external liquid ammonia source through a first pipeline; a purification device is connected with the connecting port through a second pipeline.
[0007] Further, the temperature control assembly comprises a refrigerant coil and a heat medium coil which are respectively spirally arranged on the outer surface of the cylinder.
[0008] Further, it further comprises a circulating pump, one end of the circulating pump is communicated with the bottom of the cylinder, and the other end is communicated with the first pipeline through a third pipeline.
[0009] Further, it further comprises a fourth pipeline communicated with the third pipeline and the purification device at two ends, and a heater is arranged on the fourth pipeline.
[0010] Further, the connecting port and the waste gas outlet are both provided with a mist removal filter screen.
[0011] Further, the cylinder is internally provided with a ring-shaped guide plate, the guide plate is arranged between the spray head and the air inlet, a middle part of the guide plate is provided with a filler, and an end of the guide plate towards the spray head is provided with an inclined surface from the inner wall of the cylinder to the filler.
[0012] In the above technical solution, the ethylsilane upgrading device provided by the utility model has the beneficial effects that:
[0013] The ethylsilane gas to be upgraded is introduced into the cylinder from the air inlet after the temperature control assembly reduces the temperature in the cylinder, and the ethylsilane is dissolved in the liquid ammonia, while other light component impurities continue to rise to the upper part of the cylinder and are discharged through the waste gas outlet (at this time, the connecting port is in a closed state); after the air inlet is completed, the waste gas outlet is closed after half an hour, the connecting port is opened, and then the temperature control assembly is controlled to heat the cylinder until the ammonia-ethylsilane mixed gas enters the purification device through the second pipeline, the purification device adsorbs the ammonia in the mixed gas, and finally the finished ethylsilane is obtained.
[0014] It should be understood that the foregoing general description and the following detailed description are merely exemplary and explanatory, and are not intended to limit the present disclosure.
[0015] This application file provides an overview of various implementations or examples of the technology described in this disclosure and is not intended to be a comprehensive or exhaustive disclosure of the technology disclosed. BRIEF DESCRIPTION OF DRAWINGS
[0016] In order to more clearly illustrate the technical solutions in the embodiments of the present application or the prior art, the drawings needed in the embodiments will be briefly introduced below. Obviously, the drawings in the following description are only some embodiments described in the present application, and other drawings can also be obtained by those skilled in the art based on these drawings.
[0017] Figure 1 The overall structure schematic diagram provided by the embodiments of the present application.
[0018] Explanation of reference signs:
[0019] 1, cylinder; 11, air inlet; 12, waste gas outlet; 13, connecting port; 21, cold medium coil; 22, hot medium coil; 3, spray head; 31, first pipeline; 4, purification device; 41, second pipeline; 5, circulating pump; 51, third pipeline; 52, fourth pipeline; 6, heater; 7, demisting filter screen; 8, guide plate; 9, filler. DETAILED DESCRIPTION
[0020] To make the purposes, technical solutions, and advantages of the embodiments of the present disclosure clearer, the technical solutions of the embodiments of the present disclosure will be described clearly and completely below with reference to the drawings of the embodiments of the present disclosure. Obviously, the described embodiments are some, but not all, of the embodiments of the present disclosure. Based on the described embodiments of the present disclosure, all other embodiments obtained by a person of ordinary skill in the art without creative effort belong to the scope of protection of the present disclosure.
[0021] Please refer to Figure 1 The device for upgrading ethylsilane comprises a cylinder 1, a gas inlet 11 is formed at the bottom of the cylinder 1, a waste gas outlet 12 and a connecting port 13 are respectively formed at the top of the cylinder 1; a temperature control assembly is arranged outside the cylinder 1 and used for adjusting the temperature in the cylinder 1; a spray head 3 is arranged inside the cylinder 1 and located at the lower side of the waste gas outlet 12, and the spray head 3 is communicated with an external liquid ammonia source through a first pipeline 31; a purification device 4 is connected with the connecting port 13 through a second pipeline 41. The purification device 4 is filled with 3A, 4A and 5A molecular sieves inside, which are used for adsorbing impurities such as ammonia in the mixed gas at the gas phase outlet of the upgrading device, so as to obtain finished ethylsilane.
[0022] A second electromagnetic valve and a waste gas electromagnetic valve are respectively arranged on the second pipeline 41 and the waste gas outlet 12, so as to respectively control the opening and closing states of the connecting port 13 and the waste gas outlet 12; the waste gas outlet 12 is connected with an external tail gas treatment device, so as to avoid pollution caused by direct discharge of waste gas, and the tail gas treatment device is a common technical means of a person skilled in the art, which will not be described in detail.
[0023] Further, the temperature control assembly comprises a refrigerant coil 21 and a heat medium coil 22 which are respectively spirally arranged on the outer surface of the cylinder 1. The refrigerant coil 21 and the heat medium coil 22 are both provided with heat preservation layers, and further heat insulation treatment can be performed between the refrigerant coil 21 and the heat medium coil 22, so as to avoid affecting the heating effect.
[0024] The low-temperature and low-pressure refrigerant gas enters the refrigerant coil 21, absorbs the heat in the cylinder 1 through the pipe wall, evaporates into high-temperature and low-pressure gas, is then sucked into and compressed into high-temperature and high-pressure gas by a compressor, enters a condenser to be cooled, becomes low-temperature and high-pressure liquid, and then enters the refrigerant coil 21 to circulate after being reduced in pressure by a throttling valve; the heat medium flows in the heat medium coil 22, and transfers heat to the cylinder 1 through the pipe wall, so that the temperature in the cylinder 1 is increased.
[0025] Further, a circulating pump 5 is further included, one end of the circulating pump 5 is communicated with the bottom of the cylinder 1, and the other end of the circulating pump 5 is communicated with the first pipeline 31 through a third pipeline 51. The circulating pump 5 can realize the cyclic utilization of liquid ammonia, so as to reduce the use amount of liquid ammonia.
[0026] Further, a fourth pipeline 52 is also included, which is in communication with the third pipeline 51 and the purification device 4 respectively, and a heater 6 is arranged on the fourth pipeline 52. The heater 6 is used to heat the liquid ammonia and the ethylsilane mixed liquid in the liquid phase to the gas phase; and the third pipeline 51 and the fourth pipeline 52 are respectively provided with third and fourth electromagnetic valves for controlling the opening and closing.
[0027] The conventional upgrading device also has the problem of poor adaptability. Different upgrading devices are needed for upgrading ethylsilane gas prepared by different ethylsilane preparation processes, which causes high energy consumption, safety risks and large investment. However, the device can realize two working modes of intermittent upgrading and continuous upgrading, so that different working modes can be selected according to the impurity content and type of different processes, thereby effectively improving the adaptability of the device and reducing the total investment and production risk of the enterprise. See the working principle below.
[0028] Further, a mist removal filter screen 7 is arranged in the connecting port 13 and the exhaust port 12. The mist removal filter screen 7 can filter the liquid phase to reduce the loss of liquid ammonia.
[0029] Further, a ring-shaped flow guide plate 8 is arranged in the cylinder body 1, the flow guide plate 8 is arranged between the spray head 3 and the gas inlet port 11, the middle part of the flow guide plate 8 is provided with a filler 9, and the end of the flow guide plate 8 facing the spray head 3 is provided with an inclined surface from the inner wall of the cylinder body 1 to the filler 9.
[0030] After the sprayed liquid ammonia falls on the flow guide plate 8, the flow guide plate 8 moves into the filler 9 and fully contacts with the gas to be upgraded, so that the ethylsilane is fully dissolved in the liquid ammonia.
[0031] Working principle:
[0032] I. Intermittent upgrading (for halogenated ethylsilane synthesis route and silicon-magnesium method for preparing ethylsilane):
[0033] The temperature inside the cylinder body 1 is controlled at -35 to -40℃ by passing the refrigerant through the refrigerant disc port, and the ethylsilane gas to be upgraded is introduced into the cylinder body 1 through the feed port (the connecting port 13, the second pipeline 41 and the fourth pipeline 52 are closed, and the third pipeline 51 and the exhaust port 12 are opened). The ethylsilane is fully contacted with the liquid ammonia sprayed by the spray head 3 at the filler 9, so that the ethylsilane is dissolved in the liquid ammonia. Other light component impurities continue to rise to the upper part of the cylinder body 1, and are treated by the mist removal filter screen 7 of the exhaust port 12 before being discharged to the existing tail gas treatment system.
[0034] After the end of the gas to be upgraded gas inlet, the cylinder 1 is continuously circulated under the action of circulating pump 5 for half an hour, and after half an hour, the exhaust port 12 is closed, the connecting port 13 is opened, the heat medium is introduced into the heat medium disc port to heat the cylinder 1, the temperature in the cylinder 1 is controlled to be not more than-10℃, the ammonia gas-ethylsilane mixed gas rises and moves to the purification device 4 through the second pipeline 41, the purification device 4 adsorbs the ammonia gas in the mixed gas, and finally the finished ethylsilane is obtained.
[0035] The liquid ammonia is directly transported by the first pipeline 31 in the early stage, and after the liquid ammonia in the cylinder 1 reaches a certain height, the circulating pump 5 is started, and the circulating spray is controlled, and the ratio of gas treatment amount to liquid ammonia is 1:5-7.
[0036] II. Continuous upgrading (for the process route of direct synthesis of silane):
[0037] The temperature in the cylinder 1 is controlled to be-35--40℃ by introducing the refrigerant through the refrigerant disc port, and the ethylsilane gas to be upgraded is introduced into the cylinder 1 through the feed port, (the second pipeline 41 and the third pipeline 51 are closed, and the exhaust port 12 and the fourth pipeline 52 are opened) is fully contacted with the liquid ammonia sprayed by the spray head 3 at the packing 9, so that the ethylsilane is dissolved in the liquid ammonia. And other light component impurities continue to rise to the upper part of the cylinder 1, and after being treated by the demisting filter screen 7 of the exhaust port 12, they are discharged to the existing tail gas treatment system.
[0038] After a certain liquid level is established in the cylinder 1, the circulating pump 5 is started to circulate and spray, and one fifth of the liquid ammonia circulation amount is taken out, and then a corresponding amount of liquid ammonia is supplemented through the first pipeline 31 to maintain the liquid level in the cylinder 1. Then, the heater 6 is heated, the ammonia gas and ethylsilane in the fourth pipeline 52 are gasified and introduced into the purification device 4, the ammonia gas is removed by adsorption, and finally the finished gas phase ethylsilane is obtained.
[0039] The ratio of gas treatment amount to liquid ammonia is controlled to be 1:5-7.
[0040] The above only describes some exemplary embodiments of the present application in a descriptive manner, without doubt, for ordinary skilled in the art, without departing from the spirit and scope of the present application, the described embodiments can be modified in various ways. Therefore, the above figures and description are illustrative in nature and should not be understood as limiting the scope of protection of the claims of the present application.
Claims
1. A di-silane upgrading apparatus characterized by: The application relates to a liquid ammonia purification device, which comprises a cylinder (1), an air inlet (11) is arranged at the bottom of the cylinder (1), a waste gas outlet (12) and a connecting port (13) are arranged at the top of the cylinder (1) respectively; The application relates to a liquid ammonia purification device, which comprises a cylinder (1), an air inlet (11) is arranged at the bottom of the cylinder (1), a waste gas outlet (12) and a connecting port (13) are arranged at the top of the cylinder (1) respectively; The application relates to a liquid ammonia purification device, which comprises a cylinder (1), an air inlet (11) is arranged at the bottom of the cylinder (1), a waste gas outlet (12) and a connecting port (13) are arranged at the top of the cylinder (1) respectively; The application relates to a liquid ammonia purification device, which comprises a cylinder (1), an air inlet (11) is arranged at the bottom of the cylinder (1), a waste gas outlet (12) and a connecting port (13) are arranged at the top of the cylinder (1) respectively; 2. A di-silane upgrading apparatus as claimed in claim 1, wherein, The application relates to a liquid ammonia purification device, which comprises a cylinder (1), an air inlet (11) is arranged at the bottom of the cylinder (1), a waste gas outlet (12) and a connecting port (13) are arranged at the top of the cylinder (1) respectively; 3. The ethylsilane upgrading apparatus of claim 1, wherein The application relates to a liquid ammonia purification device, which comprises a cylinder (1), an air inlet (11) is arranged at the bottom of the cylinder (1), a waste gas outlet (12) and a connecting port (13) are arranged at the top of the cylinder (1) respectively; 4. A di-silane upgrading apparatus as claimed in claim 3, wherein, The application relates to a liquid ammonia purification device, which comprises a cylinder (1), an air inlet (11) is arranged at the bottom of the cylinder (1), a waste gas outlet (12) and a connecting port (13) are arranged at the top of the cylinder (1) respectively; 5. The ethylsilane upgrading apparatus of claim 1, wherein The application relates to a liquid ammonia purification device, which comprises a cylinder (1), an air inlet (11) is arranged at the bottom of the cylinder (1), a waste gas outlet (12) and a connecting port (13) are arranged at the top of the cylinder (1) respectively; 6. The ethylsilane upgrading apparatus of claim 1, wherein, The application relates to a liquid ammonia purification device, which comprises a cylinder (1), an air inlet (11) is arranged at the bottom of the cylinder (1), a waste gas outlet (12) and a connecting port (13) are arranged at the top of the cylinder (1) respectively; The application relates to a liquid ammonia purification device, which comprises a cylinder (1), an air inlet (11) is arranged at the bottom of the cylinder (1), a waste gas outlet (12) and a connecting port (13) are arranged at the top of the cylinder (1) respectively;