An electronic-grade halosilane distillation system

By setting up a heat-conducting tube bundle and a heat-conducting cavity in the distillation vessel, combined with a shell-and-tube condenser and a modular distillation column design, the problems of high energy consumption, low mass transfer efficiency and inaccurate quality monitoring in the electronic-grade halosilane distillation process are solved, and efficient and stable production of high-purity halosilanes is achieved.

CN224937671UActive Publication Date: 2026-11-06HEFEI ADCHEM SEMI-TECH CO LTD
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Patent Information

Application Number
CN202522677782.9
Authority / Receiving Office
CN · China
Patent Type
Utility models(China)
Current Assignee / Owner
Filing Date
2025-12-17
Publication Date
2026-11-06
Estimated Expiration
2035-12-17

AI Technical Summary

Technical Problem

Existing electronic-grade halosilane distillation processes suffer from high energy consumption, low mass transfer efficiency, insufficient separation purity, and inaccurate quality monitoring, making it difficult to meet the production demands for high-purity halosilanes.

Method used

The distillation vessel is equipped with a heat-conducting tube bundle and a heat-conducting cavity in the vessel body connected to a high-temperature heat transfer oil system. It also features a shell-and-tube condenser and a low-temperature heat transfer oil system. The reflux tank integrates reflux and extraction functions. The cooler uses a coaxial curved material pipeline. Combined with a modular distillation column design and a foam trap, it achieves efficient heating, condensation, and mass transfer.

Benefits of technology

It reduces energy consumption, improves mass transfer efficiency and separation purity, ensures product quality stability and accuracy in the collection stage, and is suitable for the production of high-purity electronic-grade halosilanes.

✦ Generated by Eureka AI based on patent content.

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Abstract

This utility model discloses an electronic-grade halosilane distillation system, relating to the field of distillation technology. The system includes a distillation vessel with an internal heat-conducting tube bundle and an external heat-conducting cavity. The heat-conducting tube bundle and the heat-conducting cavity are connected to a high-temperature heat transfer oil system. The condenser is a shell-and-tube structure with a low-temperature heat transfer oil inlet and outlet. The top of the reflux tank is connected to the condenser outlet, and the bottom reflux outlet is connected to the distillation column via a reflux pipeline. The outlet of the reflux tank is connected to the cooler inlet. The cooler includes a coaxially arranged curved material pipeline and a cooling medium cavity. The outlet of the curved material pipeline is connected to a receiving tank. This structure solves the problems of high energy consumption, uneven gas-liquid distribution, foam entrainment affecting separation efficiency, and inaccurate quality monitoring during the product collection stage in the electronic-grade halosilane distillation process.
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Description

Technical Field

[0001] This utility model relates to the field of distillation technology, and in particular to an electronic-grade halosilane distillation system. Background Technology

[0002] Electronic-grade halosilanes (purity ≥7N) are key basic materials in semiconductor manufacturing processes. Their purity directly affects the performance and reliability of semiconductor devices, playing an irreplaceable role in core areas such as chip manufacturing and integrated circuit packaging. For the purification of liquid halosilane materials, the industry widely adopts distillation technology as the core separation method. This technology, with its advantages of high separation efficiency and strong operational stability, has become the mainstream solution for achieving high-purity purification of the target product.

[0003] A typical process flow for conventional electronic-grade halosilane distillation is as follows: First, the distillation system is purged with nitrogen to remove impurities such as air, preventing them from reacting with the halosilane or affecting product purity. Then, the halosilane feedstock is poured into the reboiler and heated under a set negative pressure, causing the liquid to vaporize into steam. The steam rises into the distillation column, where it undergoes gas-liquid mass and heat transfer with the descending reflux liquid, achieving separation of different components. The steam rising to the top of the column further enters the condenser, where it is condensed into liquid and collected in the reflux tank. By adjusting the reflux ratio, some material is refluxed back to the distillation column, while some is collected as product, ultimately completing the separation and purification of the target product.

[0004] However, existing conventional distillation processes have significant technical shortcomings in practical applications, making it difficult to fully meet the requirements for efficient and high-purity purification of electronic-grade halosilanes: First, halosilanes have high vapor pressures, requiring a large amount of heat energy to be supplied to the reboiler to maintain a stable discharge rate. However, conventional reboilers are limited by their structural design and have limited heat exchange area. To supply the heat required for material vaporization, high heating temperatures are often necessary, leading to high overall energy consumption and the potential for slight decomposition or deterioration of the material due to localized high temperatures, affecting product quality. Second, when the reflux liquid returns directly from the reflux tank to the distillation column, localized turbulence can easily form within the column, disrupting the stable contact between the gas and liquid phases, causing gas-liquid imbalance, reducing mass transfer efficiency, and affecting the stability of the separation effect. Finally, during the contact between halosilane vapor and the descending liquid in the distillation column, the intense disturbance between the gas and liquid phases easily generates a large amount of foam. These bubbles will enter the condensation unit with the rising steam, causing trace impurities to be carried in the condensed material. This not only weakens the effect of distillation and separation, but may also cause the final product purity to fail to meet the 7N electronic grade standard.

[0005] To address the problems existing in the above-mentioned technologies, there is an urgent need to develop an optimized electronic-grade halosilane distillation system. Through innovation and improvement in structural design, the system can solve the core pain points such as high energy consumption, low mass transfer efficiency, insufficient separation purity, and inaccurate quality monitoring, so as to meet the production needs of high-purity halosilanes in semiconductor manufacturing. Utility Model Content

[0006] This invention provides an electronic-grade halosilane distillation system that can solve the problems of high energy consumption, uneven gas-liquid distribution, foam entrainment affecting separation efficiency, and inaccurate quality monitoring during the product collection stage in the electronic-grade halosilane distillation process.

[0007] To address the aforementioned problems, this utility model provides an electronic-grade halosilane distillation system, comprising: a distillation kettle, a distillation column, a condenser, a reflux tank, a cooler, and a receiving tank; The distillation vessel is equipped with a heat-conducting tube bundle inside and a vessel body heat-conducting cavity outside. The heat-conducting tube bundle and the vessel body heat-conducting cavity are connected to a high-temperature heat-conducting oil system. The distillation column comprises, from bottom to top, a packing section, a recirculation section, and a trapping section. The recirculation section is equipped with a liquid distributor, and the trapping section is equipped with a foam trap. The condenser is a shell-and-tube structure, equipped with a low-temperature heat transfer oil inlet and a low-temperature heat transfer oil outlet; The top of the reflux tank is connected to the condenser outlet, and the bottom is provided with a reflux outlet and a collection outlet. The reflux outlet is connected to the distributor through a reflux pipeline, and the collection outlet is connected to the cooler inlet. The cooler includes a curved material pipeline and a cooling medium chamber arranged coaxially. The cooling medium chamber is provided with a low-temperature medium inlet and an outlet. The outlet of the curved material pipeline is connected to a receiving tank.

[0008] The electronic-grade halosilane distillation system provided by this utility model has, but is not limited to, the following beneficial effects compared with the prior art: This invention achieves efficient and uniform heating of the material inside the distillation vessel by incorporating a heat-conducting tube bundle inside and a heat-conducting cavity outside the vessel, both connected to a high-temperature heat transfer oil system. This effectively avoids localized overheating or uneven temperature gradients, thereby improving the vaporization efficiency and thermal stability of halosilanes and ensuring the acquisition of high-purity products. Simultaneously, the use of a coaxial condenser with independent low-temperature heat transfer oil inlets and outlets enables rapid and controllable condensation of the overhead vapor, improving condensation efficiency and reducing component loss. The reflux tank integrates reflux and collection functions, connecting the distillation column and cooler via reflux and collection outlets respectively, facilitating precise control of the reflux ratio and optimizing separation. The cooler employs a coaxial curved material pipeline and cooling medium cavity structure, increasing the heat exchange area and extending the residence time of the material during cooling, ensuring sufficient product cooling and preventing product decomposition or impurity generation due to excessive temperature. Finally, the fully cooled high-purity electronic-grade halosilane is transported to the receiving tank. The overall system has a compact structure, high heat and mass transfer efficiency, and stable operation. It is suitable for the distillation and purification of electronic-grade chemicals with extremely high purity and heat sensitivity requirements, significantly improving product quality and production safety.

[0009] Preferably, the distillation vessel is provided with a heat-conducting pipe box head, and the inner cavity of the heat-conducting pipe box head is provided with a baffle, which divides the inner cavity into region one and region two. Region one is provided with a high-temperature heat-conducting oil inlet, and region two is provided with a high-temperature heat-conducting oil outlet.

[0010] Preferably, the heat-conducting tube bundle includes a plurality of U-shaped heat-conducting tubes, one axial side of the open end of the U-shaped heat-conducting tube is connected to region one of the heat-conducting tube box end cap, and the other axial side of the U-shaped heat-conducting tube is connected to region two of the heat-conducting tube box end cap.

[0011] Preferably, the distillation vessel is connected to the distillation column, and the distillation column comprises, from bottom to top, sequentially connected components: The packing section is filled with mass transfer packing material. A recirculation section is provided above the packing section, and a liquid distributor is provided in the recirculation section for receiving and distributing the recirculated liquid from the upper part. A collection section is located above the recirculation section, and a foam collector is installed in the collection section to collect and break up the foam entrained in the rising steam.

[0012] Preferably, the liquid distributor is a shower-type distributor, and the bottom of the shower-type distributor is provided with multiple evenly distributed spray holes.

[0013] Preferably, the distillation column has a gas phase outlet at the top, which is used to connect to a condenser; the recirculation section has a reflux liquid inlet, which is used to connect to an external reflux pipeline.

[0014] Preferably, the low-temperature medium inlet of the cooling medium chamber is connected to a second low-temperature heat transfer oil system, and the low-temperature heat transfer oil inlet of the condenser is connected to a first low-temperature heat transfer oil system. The oil supply temperature of the second low-temperature heat transfer oil system is lower than that of the first low-temperature heat transfer oil system.

[0015] Preferably, the cooler outlet is connected to the receiving tank via a diaphragm valve.

[0016] Preferably, ball valves are installed on both the material inlet pipe and the residue outlet pipe of the distillation vessel, and the ball valves are used to control the flow of material into the distillation vessel and the discharge of residue, respectively.

[0017] Preferably, a three-way valve is connected between the reflux tank, the distillation column, and the cooler. Attached Figure Description

[0018] To more clearly illustrate the technical solutions in the embodiments of this application, the accompanying drawings used in the description of the embodiments will be briefly introduced below. Obviously, the accompanying drawings described below are only some embodiments of this application. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.

[0019] Figure 1 This is a schematic diagram of the overall structure of an electronic-grade halosilane distillation system according to an embodiment of the present invention. Figure 2 This is a schematic diagram of the overall structure of the distillation vessel according to an embodiment of the present invention; Figure 3 This is a schematic diagram of the overall structure of the distillation column according to an embodiment of the present invention; Figure 4 This is a schematic diagram of the overall structure of the condenser and reflux tank according to an embodiment of the present invention; Figure 5 This is a schematic diagram of the overall structure of the cooler according to an embodiment of the present invention.

[0020] Explanation of reference numerals in the attached figures: 100. Distillation vessel; 110. Heat-conducting tube bundle; 120. Heat-conducting cavity of the vessel body; 130. Heat-conducting tube box end cap; 131. Baffle; 132. Zone 1; 133. Zone 2; 134. High-temperature heat transfer oil inlet; 135. High-temperature heat transfer oil outlet; 200. Distillation column; 210. Packing section; 220. Recirculation section; 221. Liquid distributor; 222. Reflux inlet; 230. Collection section; 240. Gas Phase outlet; 300, condenser; 310, low-temperature heat transfer oil inlet; 320, low-temperature heat transfer oil outlet; 400, reflux tank; 410, reflux outlet; 420, production outlet; 500, cooler; 510, curved material pipeline; 520, cooling medium chamber; 530, low-temperature medium inlet; 540, low-temperature medium outlet; 600, receiving tank; 700, diaphragm valve; 800, ball valve; 900, three-way valve. Detailed Implementation

[0021] To make the objectives, technical solutions, and advantages of this application clearer, the technical solutions in the embodiments of this application will be clearly and completely described below with reference to the accompanying drawings showing multiple embodiments according to this application. It should be understood that the described embodiments are only a part of the embodiments of this application, and not all of the embodiments. All other embodiments obtained by those skilled in the art based on the embodiments described in this application without creative effort will fall within the scope of protection of this application.

[0022] Unless otherwise defined, all technical and scientific terms used in this application have the same meaning as commonly understood by one of ordinary skill in the art to which this application pertains; the terminology used in the description of this application is for the purpose of describing specific embodiments only and is not intended to limit this application; the terms "comprising," "including," "having," "containing," etc., in the description, claims, and accompanying drawings of this application are open-ended terms. Therefore, "comprising," "including," or "having" refers to, for example, a method or apparatus having one or more steps or elements, but is not limited to having only these one or more elements. The terms "first," "second," etc., in the description, claims, or accompanying drawings of this application are used to distinguish different objects, not to describe a specific order or hierarchy. Furthermore, the terms "first" and "second" are used for descriptive purposes only and should not be construed as indicating or implying relative importance or implicitly specifying the number of indicated technical features. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature. In the description of this application, unless otherwise stated, "a plurality of" means two or more.

[0023] In the description of this utility model, it should be understood that the terms "upper", "lower", "left", "right", "front", "rear", etc., indicate the orientation or positional relationship based on the orientation or positional relationship shown in the accompanying drawings. They are only for the convenience of describing this utility model and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, or be constructed and operated in a specific orientation. Therefore, they should not be construed as limitations on this utility model.

[0024] In the description of this application, it should be noted that, unless otherwise expressly specified and limited, the terms "installation," "connection," "linking," and "attachment" should be interpreted broadly. For example, they can refer to a fixed connection, a detachable connection, or an integral connection; they can refer to a direct connection or an indirect connection through an intermediate medium; and they can refer to the internal communication between two components. Those skilled in the art can understand the specific meaning of the above terms in this application according to the specific circumstances.

[0025] It should be emphasized that when the term "comprising / including" is used in this specification, it is used to explicitly indicate the presence of the stated feature, integer, step, or component, but does not exclude the presence or addition of one or more other features, integers, steps, parts, or groups of features, integers, steps, or parts.

[0026] like Figures 1 to 4 As shown in the figure, an electronic-grade halosilane distillation system provided by this utility model includes a distillation kettle 100, a distillation column 200, a condenser 300, a reflux tank 400, a cooler 500, and a receiving tank 600. The distillation vessel 100 is provided with a heat-conducting tube bundle 110 inside and a vessel body heat-conducting cavity 120 outside. The heat-conducting tube bundle 110 and the vessel body heat-conducting cavity 120 are connected to a high-temperature heat-conducting oil system. The distillation column 200 includes, from bottom to top, a packing section 210, a recirculation section 220, and a trapping section 230. The recirculation section 220 is equipped with a liquid distributor 221, and the trapping section 230 is equipped with a foam trap. The condenser 300 has a shell-and-tube structure and is equipped with a low-temperature heat transfer oil inlet 310 and a low-temperature heat transfer oil outlet 320. The top of the reflux tank 400 is connected to the outlet of the condenser 300, and the bottom is provided with a reflux outlet 410 and a collection outlet 420. The reflux outlet 410 is connected to the distributor through a reflux pipeline, and the collection outlet 420 is connected to the inlet of the cooler 500. The cooler 500 includes a curved material pipeline 510 and a cooling medium chamber 520 arranged coaxially. The cooling medium chamber 520 is provided with a low-temperature medium inlet 530 and an outlet. The outlet of the curved material pipeline 510 is connected to a receiving tank 600.

[0027] In this embodiment, the high-temperature heat transfer oil system includes components such as a high-temperature oil pump, an elevated oil tank, an expansion tank, and an oil heater. The high-temperature oil pump is responsible for delivering the heat transfer oil to the heat transfer tube bundle 110 and the heat transfer cavity 120 of the vessel body to ensure stable heat exchange; the elevated oil tank is used to store a certain amount of heat transfer oil to prevent the system from running out of oil; the expansion tank serves to balance the system pressure and accommodate the thermal expansion of the heat transfer oil; and the oil heater can heat the heat transfer oil to reach the required temperature.

[0028] Before the distillation process begins, heat transfer oil is drawn from the high-level oil tank by a high-temperature oil pump, heated to the set temperature by an oil heater, and then delivered to the heat transfer tube bundle 110 and the heat transfer chamber 120 of the distillation vessel 100. The design of several U-shaped heat transfer tubes in the heat transfer tube bundle 110 increases the heat exchange area, enabling more efficient heat transfer to the halosilane material in the distillation vessel 100, allowing it to vaporize at a lower heating temperature difference. This avoids material decomposition or deterioration caused by localized high temperatures and also reduces the overall process energy consumption.

[0029] In this embodiment of the application, a heat-conducting pipe box head 130 is provided inside the distillation kettle 100. A baffle 131 is provided in the inner cavity of the heat-conducting pipe box head 130. The baffle 131 divides the inner cavity into region one 132 and region two 133. A high-temperature heat-conducting oil inlet 134 is provided in region one 132, and a high-temperature heat-conducting oil outlet 135 is provided in region two 133.

[0030] In the above structure, during implementation, a heat-conducting pipe box head 130 is installed at one end of the distillation vessel 100. A baffle 131 is vertically welded into the internal cavity of this head, physically dividing the cavity into two independent, non-communicating chambers, defined as Region 1 132 and Region 2 133, respectively. An interface is opened on the outer wall of the head in Region 1 132 as a high-temperature heat transfer oil inlet 134, and an interface is opened on the outer wall of the head in Region 2 133 as a high-temperature heat transfer oil outlet 135.

[0031] Zone 132 receives high-temperature heat transfer oil pumped in from an external system and distributes the high-temperature heat transfer oil evenly to the inlet ends of all parallel U-shaped heat transfer pipes, so that the hot oil begins to flow into each heating pipe.

[0032] Zone 2, section 133 collects the heat transfer oil flowing out from the outlets of all U-shaped heat pipes, where a portion of the heat has been transferred to the material. This oil is then collected and discharged through the outlet, and returned to the external heating system for reheating.

[0033] By setting the heat-conducting tube box end cap 130 with baffle 131, a structural basis is created for the subsequent connection of the internal heat-conducting tube bundle 110. The formation of Region 132 and Region 2 133 ensures that the heat-conducting oil can flow through all heating pipes in an orderly and sufficient manner.

[0034] In this embodiment of the application, the heat-conducting tube bundle 110 includes a plurality of U-shaped heat-conducting tubes. One axial side of the open end of the U-shaped heat-conducting tube is connected to the region 132 of the heat-conducting tube box end cap 130, and the other axial side of the U-shaped heat-conducting tube is connected to the region 133 of the heat-conducting tube box end cap 130.

[0035] In the above structure, specifically inside the distillation vessel 100, several U-shaped metal tubes are arranged parallel along the axial direction to form a U-shaped heat-conducting tube bundle 110. All the openings of these U-shaped tubes facing the end cap are connected to the heat-conducting tube box end cap 130 in a sealed connection area 132 by welding or flange; the openings at the other ends of all the U-shaped tubes are connected to the heat-conducting tube box end cap 130 in a sealed connection area 133.

[0036] High-temperature heat transfer oil enters from zone 132, flows through all the U-shaped tubes, and then flows out from zone 2133. This forms a long path and a large contact area, which is a highly efficient heating loop. This allows sufficient heat to be provided even at relatively low oil temperatures, thereby reducing the heating temperature difference and energy consumption, and reducing the risk of material deterioration due to local overheating. At the same time, the structural design of the U-shaped heat transfer tube bundle 110 greatly increases the heat exchange area inside the reactor.

[0037] In this embodiment, the U-shaped metal tube is a stainless steel tube.

[0038] In this embodiment, the distillation kettle 100 is connected to the distillation column 200. The distillation column 200 includes, from bottom to top, a packing section 210, a recirculation section 220, and a collection section 230 connected in sequence. The packing section 210 is filled with mass transfer packing. The recirculation section 220 is located above the packing section 210 and is equipped with a liquid distributor 221, which is used to receive and distribute the reflux liquid from the upper part. The collection section 230 is located above the recirculation section 220 and is equipped with a foam trap, which is used to capture and break up the foam entrained in the rising vapor.

[0039] In the above structure, the distillation column 200 is clearly divided into three functionally distinct sections: the packing section 210 provides the main mass transfer surface; the recirculation section 220 is dedicated to receiving and redistributing the reflux liquid, solving the local turbulence problem caused by direct reflux; and the trapping section 230 is dedicated to intercepting and breaking up foam entrained in the rising vapor, preventing foam from entering the condensation system and affecting purity. This modular design makes the function of the distillation column 200 more specialized and efficient, significantly improving the gas-liquid mass transfer efficiency and operational stability within the column.

[0040] In this embodiment of the application, the foam collector can be configured as a wire mesh demister.

[0041] In this embodiment of the application, the liquid distributor 221 is a shower-type distributor, and the bottom of the shower-type distributor is provided with a plurality of evenly distributed spray holes.

[0042] In the aforementioned structure, the shower-type distributor, through evenly distributed spray holes at the bottom, can spray the reflux liquid from the upper part into the packing section 210 below the recirculation section 220 in a relatively dispersed and uniform manner. This uniform liquid distribution effectively avoids the liquid flow deviation phenomenon that may occur with traditional distribution methods, allowing the liquid to come into more sufficient contact with the rising vapor, thereby greatly improving the gas-liquid mass transfer efficiency. Moreover, the uniform liquid distribution can also reduce local gas-liquid ratio imbalances, making the gas-liquid mass transfer process within the distillation column 200 more stable and efficient. At the same time, the shower-type distributor has a relatively simple structure, is easy to install and maintain, and reduces the operating cost and maintenance difficulty of the equipment while ensuring the distillation effect.

[0043] In this embodiment of the application, the distillation column 200 is provided with a gas phase outlet 240 at the top of the column, and the gas phase outlet 240 is used to connect to the condenser 300; the recirculation section 220 is provided with a reflux liquid inlet 222, and the reflux liquid inlet 222 is used to connect to an external reflux pipeline.

[0044] In the above structure, the vapor outlet 240 draws the rising vapor from the distillation column 200 to the condenser 300, where the vapor is cooled and liquefied. The reflux inlet 222 is a channel that returns a portion of the condensed liquid back into the distillation column 200. The vapor outlet 240 and reflux inlet 222 achieve the circulation and separation of vapor and liquid within the distillation column 200. When the vapor enters the condenser 300 from the vapor outlet 240, it is rapidly cooled into liquid by the low-temperature heat transfer oil. A portion of the liquid returns to the distillation column 200 through the reflux inlet 222, providing the necessary reflux liquid for the distillation process and ensuring vapor-liquid balance and mass transfer within the distillation column 200. The remaining liquid is discharged as product from the outlet 420 of the reflux tank 400. This design allows the distillation process to proceed continuously and stably, improving the separation efficiency and product quality of electronic-grade halosilanes.

[0045] In this embodiment, the low-temperature medium inlet 530 of the cooling medium cavity 520 is connected to a second low-temperature heat transfer oil system, and the low-temperature heat transfer oil inlet 310 of the condenser 300 is connected to a first low-temperature heat transfer oil system. The oil supply temperature of the second low-temperature heat transfer oil system is lower than that of the first low-temperature heat transfer oil system.

[0046] In the above structure, the system is equipped with two independent low-temperature heat transfer oil circulation systems. The outlet of the first low-temperature heat transfer oil system (higher temperature, for example, 0℃ to -10℃) is connected to the low-temperature heat transfer oil inlet 310 of the condenser 300. The outlet of the second low-temperature heat transfer oil system (lower temperature, for example, -20℃ to -40℃) is connected to the low-temperature medium inlet 530 of the cooling medium chamber 520 of the cooler 500, and then discharged through the low-temperature medium outlet 540.

[0047] Employing a gradient cooling strategy, condenser 300 uses a high-temperature cold source, sufficient to condense the vast majority of vapor, thus saving cryogenic energy consumption. Cooler 500 uses an even lower-temperature cold source to deeply cool the liquefied product, ensuring that the material's temperature is well below its boiling point before entering receiving tank 600, completely eliminating the possibility of vaporization due to heat absorption in receiving tank 600. This solves the core problem of inaccurate weighing and quality monitoring caused by material vaporization, guaranteeing the accuracy and stability of product measurement.

[0048] In this embodiment of the application, the outlet of the cooler 500 is connected to the receiving tank 600 through a diaphragm valve 700.

[0049] In the above structure, a diaphragm valve 700 is installed on the connecting pipe between the outlet of the curved material pipeline 510 of the cooler 500 and the inlet of the receiving tank 600. The diaphragm valve 700 can be used to precisely control the flow rate of the product to the receiving tank 600, or to completely shut off the pipeline when the receiving tank 600 is replaced or the system is maintained.

[0050] In this embodiment of the application, ball valves 800 are provided on both the material inlet pipe and the residue outlet pipe of the distillation kettle 100. The ball valves 800 are used to control the flow of material into the distillation kettle 100 and the discharge of residue, respectively.

[0051] In the above structure, the material inlet ball valve 800 is used to control the input of raw materials during the feeding stage; the residue outlet ball valve 800 is used to control the discharge of residue from the bottom of the vessel after distillation.

[0052] In this embodiment of the application, a three-way valve 900 is connected between the reflux tank 400, the distillation column 200, and the cooler 500.

[0053] The three-way valve 900 allows for flexible control of the reflux liquid flow direction, enabling different operating modes. When it is necessary to increase the reflux ratio within the distillation column 200 to improve the distillation effect, the three-way valve 900 can guide more reflux liquid to the re-reflux section 220 of the distillation column 200, providing more sufficient liquid-phase reflux for the distillation process, enhancing gas-liquid mass transfer, and thus improving product purity and separation efficiency.

[0054] The above-disclosed embodiments are only a few specific examples of the present utility model. However, the embodiments of the present utility model are not limited thereto. Any changes that can be conceived by those skilled in the art should fall within the protection scope of the present utility model.

Claims

1. An electronic-grade halosilane distillation system, characterized in that, It includes a distillation kettle (100), a distillation column (200), a condenser (300), a reflux tank (400), a cooler (500), and a receiving tank (600); The distillation vessel (100) is provided with a heat-conducting tube bundle (110) inside and a vessel body heat-conducting cavity (120) outside. The heat-conducting tube bundle (110) and the vessel body heat-conducting cavity (120) are connected to a high-temperature heat-conducting oil system. The condenser (300) is a sleeve structure and is provided with a low-temperature heat transfer oil inlet (310) and a low-temperature heat transfer oil outlet (320). The top of the reflux tank (400) is connected to the outlet of the condenser (300), and the bottom is provided with a reflux outlet (410) and a collection outlet (420). The reflux outlet (410) is connected to the distillation column (200) through a reflux pipeline, and the collection outlet (420) is connected to the inlet of the cooler (500). The cooler (500) includes a curved material pipeline (510) and a cooling medium chamber (520) arranged coaxially. The cooling medium chamber (520) is provided with a low-temperature medium inlet (530) and an outlet. The outlet of the curved material pipeline (510) is connected to a receiving tank (600).

2. The electronic-grade halosilane distillation system according to claim 1, characterized in that, The distillation vessel (100) is provided with a heat-conducting tube box head (130). The inner cavity of the heat-conducting tube box head (130) is provided with a baffle (131). The baffle (131) divides the inner cavity into region one (132) and region two (133). Region one (132) is provided with a high-temperature heat transfer oil inlet (134), and region two (133) is provided with a high-temperature heat transfer oil outlet (135).

3. The electronic-grade halosilane distillation system according to claim 2, characterized in that, The heat-conducting tube bundle (110) includes a plurality of U-shaped heat-conducting tubes. One axial side of the open end of the U-shaped heat-conducting tube is connected to the first region (132) of the heat-conducting tube box head (130), and the other axial side of the U-shaped heat-conducting tube is connected to the second region (133) of the heat-conducting tube box head (130).

4. The electronic-grade halosilane distillation system according to claim 1, characterized in that, The distillation vessel (100) is connected to the distillation column (200), and the distillation column (200) includes, from bottom to top, the following sequentially connected components: The packing section (210) is filled with mass transfer packing. A recirculation section (220) is disposed above the packing section (210), and a liquid distributor (221) is disposed in the recirculation section (220) for receiving and distributing the recirculated liquid from the upper part; The capture section (230) is located above the recirculation section (220), and a foam trap is provided in the capture section (230) for capturing and breaking up foam entrained in the rising steam.

5. The electronic-grade halosilane distillation system according to claim 4, characterized in that, The liquid distributor (221) is a shower-type distributor, and the bottom of the shower-type distributor is provided with multiple evenly distributed spray holes.

6. The electronic-grade halosilane distillation system according to claim 4, characterized in that, The distillation column (200) is provided with a gas phase outlet (240) at the top of the column, which is used to connect the condenser (300); the recirculation section (220) is provided with a reflux liquid inlet (222), which is used to connect the external reflux pipeline.

7. The electronic-grade halosilane distillation system according to claim 1, characterized in that, The low-temperature medium inlet (530) of the cooling medium chamber (520) is connected to the second low-temperature heat transfer oil system, and the low-temperature heat transfer oil inlet (310) of the condenser (300) is connected to the first low-temperature heat transfer oil system. The oil supply temperature of the second low-temperature heat transfer oil system is lower than that of the first low-temperature heat transfer oil system.

8. The electronic-grade halosilane distillation system according to claim 7, characterized in that, The outlet of the cooler (500) is connected to the receiving tank (600) via a diaphragm valve (700).

9. The electronic-grade halosilane distillation system according to claim 1, characterized in that, Ball valves (800) are installed on the material inlet pipe and the residue outlet pipe of the distillation kettle (100). The ball valves (800) are used to control the flow of material into the distillation kettle (100) and the discharge of residue.

10. The electronic-grade halosilane distillation system according to claim 1, characterized in that, A three-way valve (900) is connected between the reflux tank (400), the distillation column (200), and the cooler (500).