A hydrogen bromide acid concentration still

CN224656037UActive Publication Date: 2026-08-21NINGXIA HAITAI NEW MATERIAL CO LTD
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Patent Information

Application Number
CN202522094266.3
Authority / Receiving Office
CN · China
Patent Type
Utility models(China)
Current Assignee / Owner
Filing Date
2025-09-29
Publication Date
2026-08-21
Estimated Expiration
2035-09-29

AI Technical Summary

Technical Problem

[0002]氢溴酸(HBr)作为一种重要的化工原料,广泛应用于医药、染料及精细化学品合成中,在1,4-二溴丁烷等有机溴化物的制备过程中,常采用氢溴酸与醇类反应,反应后产生大量稀氢溴酸,为实现资源循环利用,需对稀氢溴酸进行浓缩回收,目前,工业上多采用浓缩釜对稀氢溴酸进行蒸发浓缩,但在实际运行过程中,由于氢溴酸具有强挥发性和腐蚀性,其浓缩过程易导致大量HBr气体逸出,不仅造成原料损失,还带来严重的环境污染和安全风险

Benefits of technology

1、本实用新型在顶盖内部设置螺旋冷凝管,并配合“Z”字形布置的导流板,构成高效的气相导流与冷凝回流系统,上升的HBr气体首先经过螺旋冷凝管冷却,部分蒸气被冷凝为液体并回流至釜内,有效减少挥发损失,导流板交替安装于釜体内壁两侧,引导气体沿曲折路径上升,延长其在气相空间的停留时间,增强冷凝效果,该多级冷凝结构布局合理,充分利用釜体上部空间,提升了氢溴酸的回收效率。

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Abstract

The utility model discloses a kind of hydrobromic acid concentration stills, it relates to the technical field of concentration still, the hydrobromic acid concentration still, including still body, top cover being set in the top of still body, feed pipe orifice and agitator being penetrated top cover, top cover still be equipped with spiral condenser, spiral condenser is fixed in the inside of top cover by mounting bracket, spiral condenser cooling medium inlet and outlet are penetrated the outer wall of still body and extend to outside, for inlet cooling water, and spiral condenser is located above the cavity of still body, for the preliminary condensation reflux of the mixture of ascending HBr gas and water vapor is carried out. The utility model is integrated spiral condenser, Z-shaped deflector and annular spray pipe linked with stirring system in top cover, constructs multistage gas phase processing system, realizes the step-by-step condensation reflux of HBr gas, prolongs residence time and dynamic spray absorption, improves hydrobromic acid recovery rate and tail gas purification efficiency, compact structure, stable operation, safety and environmental protection are considered simultaneously.
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Description

Technical Field

[0001] This utility model relates to the field of concentration kettle technology, and in particular to a hydrobromic acid concentration kettle. Background Technology

[0002] Hydrobromic acid (HBr) is an important chemical raw material widely used in the synthesis of pharmaceuticals, dyes, and fine chemicals. In the preparation of organic bromides such as 1,4-dibromobutane, hydrobromic acid is often reacted with alcohols, producing a large amount of dilute hydrobromic acid. To achieve resource recycling, the dilute hydrobromic acid needs to be concentrated and recovered. Currently, industrially, dilute hydrobromic acid is mostly concentrated by evaporation in a concentration vessel. However, in actual operation, due to the high volatility and corrosiveness of hydrobromic acid, the concentration process easily leads to the escape of a large amount of HBr gas, causing not only raw material loss but also serious environmental pollution and safety risks.

[0003] Existing hydrobromic acid concentration equipment is generally equipped with only simple condensation and reflux devices, with limited condensation area and low capture efficiency of HBr vapor. Most of the uncondensed gas needs to be treated by an external absorption system, which has problems such as dispersed equipment, complex connections, and insufficient absorption. In addition, traditional equipment lacks an effective airflow guiding structure, resulting in short gas residence time in the vessel and low mass and heat transfer efficiency, leading to insufficient condensation. Utility Model Content

[0004] This utility model provides a hydrobromic acid concentration vessel, including a vessel body, a top cover disposed on the top of the vessel body, a feed inlet pipe penetrating the top cover, and a stirrer. The top cover is also provided with a spiral condenser tube, which is fixed inside the top cover by a mounting bracket. The cooling medium inlet and outlet of the spiral condenser tube extend to the outside through the outer wall of the vessel body for introducing cooling water. The spiral condenser tube is located above the inner cavity of the vessel body for preliminary condensation and reflux of the rising HBr gas and water vapor mixture.

[0005] Preferably, the inlet end of the spiral condenser is connected to the outlet end of the delivery pump via a pipe, and the inlet end of the delivery pump is connected to the outlet end of the storage cylinder via a pipe. Both the storage cylinder and the delivery pump are fixed to the outside of the vessel body.

[0006] Preferably, the rod at the upper end of the stirrer is fixedly connected to the lower end of the hollow tube, the upper end of the hollow tube passes through the top cover and is rotatably connected to the top cover, and an annular spray pipe is connected to the part of the hollow tube near the lower end, with multiple downwardly inclined atomizing nozzles evenly distributed on the annular spray pipe.

[0007] Preferably, the upper end of the hollow tube is rotatably connected to the delivery pipe, the delivery pipe is fixed by a support frame, the hollow tube is connected to an external dilute acid reflux pump, and the spray direction is towards the area below the spiral condenser tube, forming a spray absorption layer covering the entire gas phase space for capturing uncondensed HBr gas.

[0008] Preferably, the hollow tube is connected to a driven wheel at the part outside the top cover, and a driving wheel is rotatably mounted on the top cover. The driving wheel is driven by a motor and meshes with the driven wheel.

[0009] Preferably, multiple sets of guide plates are provided in the upper part of the inner cavity of the vessel and below the spiral condenser tube, with each guide plate alternately arranged on both sides of the inner wall of the vessel in a "Z" shape.

[0010] Preferably, the top of the top cover is provided with a closed vent, and the closed vent is connected to a Venturi absorber through a pipe. The Venturi absorber is integrated on the outside of the top cover and has an alkali nozzle at its throat.

[0011] Preferably, the outlet end of the Venturi absorber is connected to a tail gas emission pipe, and the alkali nozzle is connected to the alkali storage tank through a hose.

[0012] Preferably, the top cover is provided with a sensor interface, which is a threaded connection structure for installing an online pH probe, and a viewing window is provided on the outer wall of the vessel.

[0013] Preferably, the vessel body has a double-layer structure, and the interior of the vessel body is lined.

[0014] The hydrobromic acid concentration kettle provided in this embodiment of the invention has the following advantages compared to the prior art: 1. This utility model features a spiral condenser tube inside the top cover, along with Z-shaped guide plates, forming a highly efficient gas phase guiding and condensation reflux system. The rising HBr gas is first cooled by the spiral condenser tube, and some of the vapor is condensed into liquid and refluxed back into the reactor, effectively reducing volatilization loss. The guide plates are alternately installed on both sides of the inner wall of the reactor to guide the gas upward along a tortuous path, extending its residence time in the gas phase space and enhancing the condensation effect. This multi-stage condensation structure is rationally laid out, making full use of the upper space of the reactor and improving the recovery efficiency of hydrobromic acid.

[0015] 2. This utility model features an annular spray pipe located below the spiral condenser pipe, which can evenly spray the absorbent liquid into the gas phase region to dynamically capture uncondensed HBr gas, further improving the removal rate. The annular spray pipe is linked with the stirring system to expand the coverage area and ensure full gas-liquid contact. The overall structure is integrated inside the concentration vessel, with no movement interference from the stirrer, ensuring stable equipment operation. Through the synergistic effect of condensation, flow guidance, and spraying, efficient purification of exhaust gas is achieved, improving the safety and environmental performance of the concentration process. Attached Figure Description

[0016] To more clearly illustrate the technical solutions of the embodiments of this utility model, the drawings used in the embodiments will be briefly introduced below. It should be understood that the following drawings only show some embodiments of this utility model and should not be regarded as a limitation of the scope. For those skilled in the art, other related drawings can be obtained from these drawings without creative effort.

[0017] Figure 1 This is a schematic diagram of the overall structure of an embodiment of the present utility model; Figure 2 This is a side view of the overall structure of an embodiment of the present utility model; Figure 3 This is a second side view of the body structure of an embodiment of the present utility model; Figure 4 The following is an embodiment of this utility model Figure 3 Schematic diagram excluding section AA; Figure 5 This is a schematic diagram of the structure of the spiral condenser tube and other components according to an embodiment of the present utility model; Figure 6 This is a schematic diagram of the structure of the Venturi absorber and other components according to an embodiment of the present invention; Figure 7 This is a schematic diagram of the structure of the annular spray pipe and other components according to an embodiment of the present utility model; Figure 8 This is a structural breakdown diagram of the hollow tube, stirrer, etc., according to an embodiment of this utility model.

[0018] Figure label: 1. Reactor body; 2. Viewing window; 3. Sensor interface; 4. Liner; 5. Sealed exhaust port; 6. Venturi absorber; 7. Tail gas discharge pipe; 8. Alkali nozzle; 9. Baffle plate; 10. Spiral condenser tube; 11. Mounting bracket; 12. Storage cylinder; 13. Transfer pump; 14. Hollow tube; 15. Transfer pipe; 16. Stirrer; 17. Annular spray pipe; 18. Driven wheel; 19. Driving wheel; 20. Support frame. Detailed Implementation

[0019] The following detailed description, in conjunction with the accompanying drawings, outlines some embodiments of the present invention. Unless otherwise specified, the following embodiments and features can be combined with each other.

[0020] Please refer to Figures 1-8 This utility model provides a hydrobromic acid concentration kettle, including a kettle body 1, a top cover disposed on the top of the kettle body 1, a feed inlet through the top cover, and a stirrer 16.

[0021] The vessel body 1 is a vertical cylindrical structure with a double-layer design. The outer layer is a carbon steel shell, and the inner layer is equipped with an inner liner 4. The inner liner 4 is made of polytetrafluoroethylene (PTFE) or perfluoroalkoxy resin (PFA) material with a thickness of 2-5 mm. It is tightly bonded to the inner wall of the vessel body 1 through molding or thermal spraying processes, and has excellent resistance to hydrobromic acid corrosion.

[0022] The top cover is a detachable flange cover with a central mounting hole. The agitator 16 penetrates the top cover and extends into the interior of the vessel body 1 through a mechanical seal structure to promote uniform heating of the liquid inside the vessel and prevent local overheating or scaling.

[0023] like Figure 5 As shown, a spiral condenser tube 10 is provided inside the top cover. The spiral condenser tube 10 is horizontally coiled and fixed on the mounting bracket 11 on the inner wall of the top cover. The mounting bracket 11 is a stainless steel bracket and is fixed to the top cover by bolts. The cooling medium inlet and outlet of the spiral condenser tube 10 pass through the outer wall of the vessel body 1 and extend to the outside, connecting to the cooling water circulation system. Cooling water enters from one end inlet and flows out from the other end outlet to achieve countercurrent heat exchange.

[0024] When dilute hydrobromic acid is heated in the reactor, the mixed vapor formed by the azeotropic evaporation of HBr and water rises to the upper part of the reactor body 1. It first comes into contact with the low-temperature spiral condenser 10, and part of the vapor condenses into liquid and flows back into the reactor, achieving preliminary reflux and reducing the loss of HBr volatilization.

[0025] The cooling medium inlet of the spiral condenser 10 is connected to the outlet of the transfer pump 13 through a pipe. The inlet of the transfer pump 13 is connected to the outlet of the storage tank 12 through a pipe. The storage tank 12 and the transfer pump 13 are both fixed on the external support of the vessel body 1, forming an independent cooling liquid circulation system, which is convenient for maintenance and repair.

[0026] To further improve the capture efficiency of HBr in the gas phase, this invention provides multiple sets of guide plates 9 in the upper part of the inner cavity of the vessel body 1 and below the spiral condenser tube 10. Each guide plate 9 is a rectangular corrosion-resistant metal plate, which is alternately welded to the left and right sides of the inner wall of the vessel body 1. Each guide plate 9 extends from the inner wall to the opposite side, but does not contact the opposite wall surface, forming an interlaced "Z"-shaped channel. The free end of the guide plate 9 is inclined downward to guide the rising gas to flow along a tortuous path, prolong its residence time in the gas phase space, and enhance the contact efficiency with the condensation surface and the spray liquid.

[0027] The upper end of the stirrer 16 is fixedly connected to the lower end of a vertically arranged hollow tube 14. The upper end of the hollow tube 14 passes through the top cover and is rotatably connected to the top cover through a rotary sealing structure. A ring spray pipe 17 is connected to the lower end of the hollow tube 14. The ring spray pipe 17 is a ring pipe fixed around the hollow tube 14. Multiple downward-sloping atomizing nozzles are evenly distributed on it. Since the hollow tube 14 and the stirrer 16 rotate synchronously, the ring spray pipe 17 rotates accordingly, realizing the circumferential dynamic spraying of the spray liquid, covering the entire cross-section of the gas phase space, and forming a uniform spray absorption layer.

[0028] The upper end of the hollow tube 14 is rotatably connected to the conveying pipe 15 via a rotary joint. The conveying pipe 15 is fixed to the outside of the top cover via a support frame 20. The hollow tube 14 is connected to an external dilute acid reflux pump via the conveying pipe 15. The pumped spray liquid can be part of the condensate or alkaline absorbent, which is sprayed out in the area below the spiral condenser tube 10 to chemically absorb the uncondensed HBr gas and further reduce the emission concentration.

[0029] like Figure 7 As shown, the hollow tube 14 is connected to a driven wheel 18 at the part outside the top cover. A driving wheel 19 is also rotatably mounted on the top cover. The driving wheel 19 is driven by an independent motor and meshes with the driven wheel 18 to drive the hollow tube 14 and the annular spray pipe 17 to rotate synchronously.

[0030] like Figure 6 As shown, a closed exhaust port 5 is provided on the top of the cover. The closed exhaust port 5 is connected to a Venturi absorber 6 through a pipe. The Venturi absorber 6 is integrated on the outside of the cover. Its structure includes a constriction section, a throat, and a diffuser section. An alkaline nozzle 8 is provided in the throat. The alkaline nozzle 8 is connected to an alkaline storage tank through a hose. The spray direction is towards the central axis of the Venturi absorber 6, spraying sodium hydroxide solution inward. When the exhaust gas passes through the throat at high speed, a negative pressure is formed, which drives the alkaline solution to atomize and react with the residual HBr gas. The purified gas is discharged through the exhaust pipe 7 to ensure that the emission meets the standards.

[0031] To facilitate operation monitoring, a sensor interface 3 is provided at the top of the top cover. It is a standard threaded interface that can be used to install an online pH probe to monitor the acidity and alkalinity of the spray liquid in real time. A viewing window 2 is provided on the outer wall of the vessel body 1. It is made of corrosion-resistant transparent material (such as polytetrafluoroethylene sight glass) to facilitate observation of the internal spray status, liquid level and scaling.

[0032] In summary, dilute hydrobromic acid is added to the reactor 1 through the feed port. The stirrer 16 stirs and heats to concentrate the HBr and water vapor. The HBr rises and is initially condensed and refluxed through the spiral condenser 10. The uncondensed gas flows in a "Z" shape between the guide plates 9 to prolong the residence time. The annular spray pipe 17 sprays the absorbent liquid along with the hollow tube 14 to capture the residual HBr. The tail gas enters the Venturi absorber 6 through the closed exhaust port 5. The alkaline nozzle 8 sprays NaOH solution into the absorber to neutralize the HBr. After purification, the gas is discharged through the tail gas discharge pipe 7.

[0033] The above are merely preferred embodiments of this utility model and are not intended to limit the scope of this utility model. Various modifications and variations can be made to this utility model by those skilled in the art. Any modifications, equivalent substitutions, or improvements made within the spirit and principles of this utility model should be included within the protection scope of this utility model.

Claims

1. A hydrobromic acid concentration vessel, comprising a vessel body (1), a top cover disposed on the top of the vessel body (1), a feed inlet penetrating the top cover, and a stirrer (16), characterized in that: The top cover is also provided with a spiral condenser tube (10). The spiral condenser tube (10) is fixed inside the top cover by a mounting bracket (11). The cooling medium inlet and outlet of the spiral condenser tube (10) extend through the outer wall of the vessel body (1) to the outside for introducing cooling water. The spiral condenser tube (10) is located above the inner cavity of the vessel body (1) for preliminary condensation and reflux of the rising HBr gas and water vapor mixture.

2. The hydrobromic acid concentration kettle according to claim 1, characterized in that: The inlet end of the spiral condenser (10) is connected to the outlet end of the delivery pump (13) through a pipe. The inlet end of the delivery pump (13) is connected to the outlet end of the storage cylinder (12) through a pipe. Both the storage cylinder (12) and the delivery pump (13) are fixed outside the vessel body (1).

3. The hydrobromic acid concentration kettle according to claim 2, characterized in that: The upper end of the stirrer (16) is fixedly connected to the lower end of the hollow tube (14). The upper end of the hollow tube (14) passes through the top cover and is rotatably connected to the top cover. The part of the hollow tube (14) near the lower end is connected to an annular spray pipe (17). Multiple downward-sloping atomizing nozzles are evenly distributed on the annular spray pipe (17).

4. The hydrobromic acid concentration kettle according to claim 3, characterized in that: The upper end of the hollow tube (14) is rotatably connected to the conveying pipe (15), the conveying pipe (15) is fixed by the support frame (20), the hollow tube (14) is connected to the external dilute acid reflux pump, and the spray direction is towards the area below the spiral condenser (10) to form a spray absorption layer covering the entire gas phase space, which is used to capture uncondensed HBr gas.

5. The hydrobromic acid concentration kettle according to claim 4, characterized in that: The hollow tube (14) is connected to a driven wheel (18) at the part outside the top cover, and a driving wheel (19) is rotatably provided on the top cover. The driving wheel (19) is driven by a motor to mesh with the driven wheel (18).

6. The hydrobromic acid concentration kettle according to claim 5, characterized in that: Multiple sets of guide plates (9) are provided in the upper part of the inner cavity of the vessel body (1) and below the spiral condenser tube (10). Each guide plate (9) is alternately arranged on both sides of the inner wall of the vessel body (1) in a "Z" shape.

7. The hydrobromic acid concentration kettle according to claim 1, characterized in that: The top of the cover is provided with a closed exhaust port (5), and the closed exhaust port (5) is connected to a Venturi absorber (6) through a pipe. The Venturi absorber (6) is integrated on the outside of the cover and has an alkaline nozzle (8) at its throat.

8. The hydrobromic acid concentration kettle according to claim 7, characterized in that: The outlet end of the Venturi absorber (6) is connected to the exhaust pipe (7), and the alkali nozzle (8) is connected to the alkali storage tank through a hose.

9. The hydrobromic acid concentration kettle according to claim 8, characterized in that: The top cover is provided with a sensor interface (3), which is a threaded connection structure for installing an online pH probe. The outer wall of the vessel body (1) is provided with a viewing window (2).

10. The hydrobromic acid concentration kettle according to claim 1, characterized in that: The vessel body (1) has a double-layer structure, and the vessel body (1) is provided with an inner lining (4).