Acetylene chlorination column system and its production enhancement method
Patent Information
- Application Number
- CN202610882175.2
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2026-06-18
- Publication Date
- 2026-09-11
- Estimated Expiration
- 2046-06-18
AI Technical Summary
单孔孔径过大导致气体喷射动量不足,大量气体从喷头前段集中喷出,后端介质供给量锐减,塔内截面气相分布极不均匀
Smart Images

Figure CN122404095B_ABST
Abstract
Description
Technical Field
[0001] This application relates to the field of chlorination tower technology, and in particular to an acetylene chlorination tower system and a method for increasing its output. Background Technology
[0002] Acetylene chlorination is the core process for preparing organochlorine products such as tetrachloroethane. As the core equipment of this reaction, the uniformity of gas phase distribution, the stability of system vacuum, the efficiency of reaction heat removal, and the accuracy of liquid level monitoring directly determine the raw material conversion rate, product yield, and the safe operation level of the equipment.
[0003] In existing technologies, acetylene chlorination towers have the following systemic defects: (a) Severe imbalance in gas phase distribution The existing chlorine nozzles use a 7-row × 57-hole × 10mm orifice design, while the acetylene nozzles use a 7-row × 46-hole × 12mm orifice design. The excessively large orifice diameter results in insufficient gas injection momentum, causing a large amount of gas to be concentrated at the front of the nozzle, drastically reducing the media supply at the rear and leading to extremely uneven gas phase distribution within the tower cross-section. In some areas, chlorine and acetylene cannot fully react, resulting in a consistently low feed conversion rate (typically only 75%–80%) and an increase in by-products. More seriously, the uneven distribution causes the formation of explosive chlorine-acetylene mixtures in localized gas phase spaces, triggering detonations within the tower, occurring 3–5 times annually. This causes impact damage to the tower body and internal components, severely threatening production safety.
[0004] (ii) Conservative vacuum setting limits production capacity. The chlorination system operates under negative pressure. The original vacuum interlock value was set at -54 kPa, and the normal operating vacuum pressure is -55 kPa to -60 kPa. This makes it limited by uneven gas phase distribution and low heat exchange efficiency of the total condenser. Operators dare not increase the vacuum level, which leads to limited chlorine and acetylene feed rates. As a result, product output has been lower than the design value for a long time (usually only 80% to 85% of the design value), resulting in poor production efficiency.
[0005] (III) Decrease in heat exchange efficiency and corrosion of total condenser The existing total condenser is made of carbon steel, has no manholes, and uses an open cooling tower for circulating water cooling. The production area experiences frequent sandstorms, and the open cooling tower lacks effective filtration, resulting in a large amount of silt entering the circulating water and depositing and caking on the shell side of the total condenser. The carbon steel material, constantly exposed to corrosive circulating water, corrodes. The rust mixes with the silt, further exacerbating the blockage, reducing the circulating water flow area, significantly increasing heat exchange resistance, and drastically reducing condensation heat exchange efficiency. This leads to the inability to maintain system vacuum, shortened equipment lifespan, and forced maintenance cycles to be shortened to one month or even less.
[0006] (iv) Distorted liquid level monitoring increases safety hazards Current liquid level monitoring uses a capacitive level gauge directly inserted into a matching float, whose inner diameter is much larger than the gauge's outer diameter. Slight fluctuations in the liquid level within the tower are amplified and transmitted through the flow of the medium within the float, resulting in large, irregular fluctuations in the monitored values (with errors as high as ±15%), failing to accurately reflect the liquid level within the tower. When the liquid level is too low, acetylene and chlorine come into direct contact in the gas phase, easily leading to a violent explosion; when the liquid level is too high, the tower is flooded, the system becomes positively pressurized, the heat of reaction cannot dissipate in time, and flammable and explosive gases accumulate within the tower, similarly triggering detonations or explosions. Distorted liquid level monitoring is one of the core contributing factors to these serious accidents.
[0007] (v) Each system operates in isolation and lacks coordination. In existing technologies, nozzle modification, vacuum control, total condenser maintenance, and liquid level monitoring are all independent, and no coupling relationship has been established between the parameters.
[0008] Based on this, this application proposes an acetylene chlorination tower system and a method for increasing its output. Summary of the Invention
[0009] This application provides an acetylene chlorination tower system and a method for increasing its output, in order to solve the technical problems described in the background art above.
[0010] To solve the above-mentioned technical problems, this application adopts the following technical solution: In a first aspect, this application provides a method for increasing the output of an acetylene chlorination tower, the method comprising: S1. A first preset number of chlorine nozzles and a second preset number of acetylene nozzles are alternately arranged along the axial direction of the chlorination tower body. Each row of chlorine nozzles includes a first preset number of chlorine nozzles, and the orifice diameter of each chlorine nozzle is the first preset orifice diameter; each row of acetylene nozzles includes a second preset number of acetylene nozzles, and the orifice diameter of each acetylene nozzle is the second preset orifice diameter. S2. The vacuum level inside the chlorination tower body is set to a first preset threshold using a negative pressure device; S3. Handholes are provided on the shell side of the total condenser at a first preset height and a second preset height from the top, respectively. The shell side deposits of the total condenser are cleaned through the handholes by alternating high-pressure water jet and citric acid chemical cleaning, so that the condensation heat transfer coefficient of the total condenser is greater than or equal to the second preset threshold. S4. A sleeve is coaxially installed inside the float of the capacitive level meter inside the chlorination tower body, and the capacitive level meter is inserted into the sleeve. The upper section of the sleeve is provided with an exhaust hole, and the lower section is provided with a damping hole. S5. By real-time monitoring of the pressure drop and liquid level of the chlorine and acetylene nozzles inside the chlorination tower body, the vacuum degree of the negative pressure device, and the temperature difference of the total condenser, the normal operation of the reaction process inside the chlorination tower body is ensured.
[0011] Optionally, the first preset number of rows is 2-4 rows, the first preset number of items is 36-38, and the first preset aperture is 4mm-6mm; The second preset number of rows is 2-4 rows, the second preset number of items is 42-44 items, and the second preset aperture is 4mm-7mm.
[0012] Optionally, both the chlorine nozzle and the acetylene nozzle are inclined downwards, and the angle between their axes and the central axis of the chlorination tower body is 15° to 25°. The chlorine nozzles and acetylene nozzles are arranged alternately in every two adjacent rows.
[0013] Optionally, the first preset threshold is -72 kPa to -65 kPa.
[0014] Optionally, the total condenser is made of graphite. The second preset threshold is 38 W / (m·K)-42 W / (m·K).
[0015] Optionally, the inner diameter of the sleeve is 5mm-10mm larger than the outer diameter of the capacitive level gauge to form a narrow annular gap damping channel between them. The diameter of the exhaust port is 3mm-6mm; The diameter of the damping orifice is 2mm-3mm.
[0016] Optionally, the specific steps of S5 are as follows: S51, Level 1 Response: When the fluctuation of the liquid level in the chlorination tower body is greater than the third preset threshold or the temperature difference of the total condenser is greater than the fourth preset threshold, the Level 1 audible and visual warning module is triggered. S52, Secondary Response: When the fluctuation value of the liquid level in the chlorination tower body is greater than the fifth preset threshold or the vacuum degree deviates from the sixth preset threshold, reduce the amount of chlorine and acetylene fed into the chlorination tower body. S53, Level 3 Response: When the liquid level in the chlorination tower body is less than the lower limit or greater than the upper limit, or the vacuum degree in the chlorination tower body is greater than the seventh preset threshold, or the pressure drop of the chlorine nozzle and / or the acetylene nozzle is less than the eighth preset threshold, the feed of chlorine and acetylene is immediately cut off, and the nitrogen purging procedure is started.
[0017] Secondly, this application provides an acetylene chlorination tower system, applied to any of the above-described methods for increasing the output of a chlorination tower, comprising: The chlorination tower body is used to produce acetylene, and includes a first preset number of chlorine nozzles and a second preset number of acetylene nozzles. Wherein, each row of chlorine nozzles includes a first preset number of chlorine nozzles, and the orifice diameter of each chlorine nozzle is the first preset orifice diameter; Each row of acetylene nozzles includes a second preset number of acetylene nozzles, and the orifice diameter of each acetylene nozzle is the second preset orifice diameter; A negative pressure device is connected to the chlorination tower body via a negative pressure pipeline and is used to adjust the vacuum level inside the chlorination tower body. The total condenser is connected to the gas phase outlet of the chlorination tower body through a gas pipeline and is used to condense the gas phase coming out of the chlorination tower body to reduce the temperature inside the chlorination tower body and maintain a negative pressure state. A liquid level monitoring device, comprising a float, a sleeve coaxially disposed within the float, and a capacitive level gauge inserted within the sleeve; The DCS control unit is electrically connected to the negative pressure device, the total condenser, and the liquid level monitoring device, and is used to control the operation of the negative pressure device, the total condenser, and the liquid level monitoring device.
[0018] Optionally, the inner diameter of the sleeve is 5mm-10mm larger than the outer diameter of the capacitive level gauge to form a narrow annular gap damping channel between them. The upper section of the sleeve has an exhaust hole with a diameter of 3mm-6mm, and the lower section has a damping hole with a diameter of 2mm-3mm.
[0019] Optionally, the DCS control unit includes a primary audible and visual early warning module, a secondary automatic feeding adjustment module, and a tertiary emergency shut-off and nitrogen purging module; The first-level audible and visual early warning module is used to trigger the first-level audible and visual early warning module when the fluctuation of the liquid level in the chlorination tower body is greater than the third preset threshold or the temperature difference of the total condenser is greater than the fourth preset threshold. The secondary feed automatic adjustment module is used to reduce the amount of chlorine and acetylene fed into the chlorination tower when the fluctuation value of the liquid level in the chlorination tower body is greater than the fifth preset threshold or the vacuum degree deviates from the sixth preset threshold. The three-level emergency shut-off and nitrogen purging module is used to immediately shut off the feed of chlorine and acetylene and start the nitrogen purging program when the liquid level in the chlorination tower body is less than the lower limit or greater than the upper limit, or the vacuum degree in the chlorination tower body is greater than the seventh preset threshold, or the pressure drop of the chlorine nozzle and / or the acetylene nozzle is less than the eighth preset threshold.
[0020] 1) The method for increasing the output of the acetylene chlorination tower provided in this application firstly, by alternately setting chlorine and acetylene nozzles within the chlorination tower body, chlorine and acetylene can achieve more uniform and thorough contact and mixing in the radial and axial directions within the tower, effectively avoiding problems such as incomplete reaction and increased side reactions caused by excessively high or low local reactant concentrations. Simultaneously, by combining a negative pressure device to control the vacuum degree within the tower at a first preset threshold, the chlorination reaction can be promoted in the positive direction at lower temperatures, improving both the single-pass conversion rate and reaction selectivity of acetylene and significantly increasing the output of the chlorination tower per unit time. Secondly, manholes are respectively set at the first and second preset heights from the top of the shell side of the total condenser, which can accurately cover the main areas where deposits easily accumulate in the shell side, providing an effective operating channel for cleaning operations. The alternating use of high-pressure water jet and citric acid chemical cleaning can achieve a synergistic effect of physical scouring and chemical dissolution for deposits of different properties, efficiently removing shell side deposits and restoring and maintaining the condensation heat transfer coefficient of the total condenser above the second preset threshold. This effectively solves the bottleneck problem of reduced heat exchange efficiency and insufficient condensation capacity due to sediment, which limits production growth and extends the continuous operation cycle of the total condenser. Furthermore, by coaxially installing a sleeve inside the float of the capacitive level gauge, with vent holes in the upper section and damping holes in the lower section, interference from gas relative capacitance measurement can be effectively isolated. Simultaneously, the damping holes mitigate the impact of liquid level fluctuations on the medium inside the float, making the measurement signal of the capacitive level gauge more stable and accurate. This improves the monitoring accuracy and reliability of the liquid level in the chlorination tower, providing real data support for process control and avoiding feed or discharge imbalances caused by misjudgments of the liquid level, thereby ensuring the continuous and stable operation of the reaction process. Finally, by real-time monitoring of key process parameters such as pressure drop of chlorine and acetylene nozzles, liquid level in the tower, vacuum degree, and temperature difference in the total condenser, potential fault signs such as nozzle blockage, abnormal liquid level, vacuum leakage, or deterioration of heat exchange can be detected in a timely manner, facilitating rapid control decisions by operators. This not only significantly improves the safety and controllability of chlorination tower operation and reduces the operational risks in the flammable and explosive environment of acetylene, but also provides data support for process optimization and output improvement.
[0021] 2) The acetylene chlorination tower system provided in this application integrates alternating rows of chlorine and acetylene nozzles within the chlorination tower body, with each nozzle having a defined number of rows, number of nozzles per row, and orifice diameter. This allows for uniform and thorough contact and mixing of chlorine and acetylene within the tower, effectively preventing incomplete reactions or increased side reactions caused by uneven local concentrations. This structural layout provides optimized gas phase distribution conditions for the acetylene chlorination reaction, helping to improve the single-pass conversion rate and reaction selectivity of acetylene, thus laying a hardware foundation for increased production. The vacuum level within the tower is adjusted to a preset range via a connection between the negative pressure device and the chlorination tower body, reducing the operating temperature of the chlorination reaction and promoting forward reaction. Simultaneously, the total condenser is connected to the gas phase outlet of the chlorination tower body via a gas pipeline, not only condensing and recovering the gas phase products but also continuously removing gas phase heat during the condensation process, helping to maintain the stability of the negative pressure state within the tower. The negative pressure device and the total condenser work together to maintain a stable and controllable temperature and pressure environment within the chlorination tower, improving reaction efficiency and reducing the risk of acetylene decomposition and explosion under high temperature and pressure, significantly enhancing system safety. The level monitoring device employs a design with a coaxial sleeve inside the float and a capacitive level gauge inserted within the sleeve. Combined with the vent inlet in the upper section and the damping orifice in the lower section of the sleeve, it effectively isolates interference from gas-phase capacitance measurement and mitigates the impact of buffer level fluctuations on the measurement signal. This structure ensures high measurement accuracy and stability even under the complex operating conditions of the chlorination tower, providing reliable data for material balance control, preventing feed imbalances or reaction anomalies caused by level distortion, and guaranteeing long-term continuous and stable operation of the chlorination tower. Electrical connections between the DCS control unit and the negative pressure device, total condenser, and level monitoring device establish an automated control architecture with centralized monitoring and decentralized execution. The DCS control unit can collect and process operating parameters of each device in real time, enabling coordinated adjustment and precise control of key process indicators such as vacuum, condensation temperature, and level. Compared to traditional manual operation or single-point control modes, this integrated control method significantly improves the system's response speed and control accuracy, reduces human error, and ensures that all functional units are always in the best collaborative working state. Attached Figure Description
[0022] To more clearly illustrate the technical solutions in the embodiments of this application or the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are some embodiments of this application. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.
[0023] Figure 1 This is a schematic diagram of the structure of an acetylene chlorination tower system provided in an embodiment of this application; Figure 2 This is a schematic diagram of the structure within the chlorination tower body provided in an embodiment of this application; Figure 3 This is a schematic diagram of the structure of a liquid level monitoring device provided in one embodiment of this application; Figure 4 A schematic diagram of the electrical connections between the DCS control system and various structural components provided in an embodiment of this application; Figure 5 This is a schematic diagram of the modules included in a DCS control system provided in an embodiment of this application.
[0024] In the diagram: 100, Chlorination tower body; 101, Chlorine nozzle; 102, Acetylene nozzle; 200, Negative pressure device; 201, Negative pressure pipeline; 300, Total condenser; 301, Gas pipeline; 400, Liquid level monitoring device; 401, Float; 402, Sleeve; 4021, Exhaust port; 4022, Damping orifice; 403, Capacitive level gauge; 404, Narrow annular gap damping channel; 500, DCS control unit; 501, Primary audible and visual early warning module; 502, Secondary automatic feed adjustment module; 503, Tertiary emergency shut-off and nitrogen purging module. Detailed Implementation
[0025] To make the objectives, technical solutions, and advantages of the embodiments of this application clearer, the technical solutions in the embodiments of this application are described clearly and completely below. Obviously, the described embodiments are only some embodiments of this application, not all embodiments. Based on the embodiments in this application, all other embodiments obtained by those skilled in the art without creative effort are also within the scope of protection of this application.
[0026] In a first aspect, this application provides a method for increasing the output of an acetylene chlorination tower, the method comprising: S1. A first preset number of chlorine nozzles 101 and a second preset number of acetylene nozzles 102 are alternately arranged along their axial direction within the chlorination tower body 100. Each row of chlorine nozzles 101 includes a first preset number of chlorine nozzles 101, and the orifice diameter of each chlorine nozzle 101 is a first preset orifice diameter. Each row of acetylene nozzles 102 includes a second preset number of acetylene nozzles 102, and the orifice diameter of each acetylene nozzle 102 is a second preset orifice diameter. The second preset number is greater than the first preset number, and the second preset orifice diameter is greater than the first preset orifice diameter. Specifically, by alternately arranging chlorine nozzles 101 and acetylene nozzles 102 within the chlorination tower body 100, chlorine and acetylene can achieve more uniform and sufficient contact and mixing in the radial and axial directions within the chlorination tower body 100, effectively avoiding problems such as incomplete reaction and increased side reactions caused by excessively high or low local reactant concentrations.
[0027] S2. The vacuum degree inside the chlorination tower body 100 is set to a first preset threshold by the negative pressure device 200. By controlling the vacuum degree inside the tower to the first preset threshold by the negative pressure device 200, the chlorination reaction can be promoted in the positive direction at a lower temperature, which not only improves the single-pass conversion rate and reaction selectivity of acetylene, but also significantly increases the output of the chlorination tower per unit time.
[0028] S3. Handholes are installed on the shell side of the total condenser 300 at a first preset height (where the first preset height is 1 / 3 of the distance from the top of the shell side of the total condenser 300) and a second preset height (where the second preset height is 1 / 2 of the distance from the top of the shell side of the total condenser 300). High-pressure water jetting and citric acid chemical cleaning are alternately applied through these handholes to clean the shell side deposits of the total condenser 300, ensuring that the condensation heat transfer coefficient of the total condenser 300 is greater than or equal to a second preset threshold. The handholes at the first and second preset heights from the top of the shell side of the total condenser 300 precisely cover the main areas where deposits tend to accumulate within the shell side, providing an effective operating channel for the cleaning operation. The alternating high-pressure water jetting and citric acid chemical cleaning method achieves a synergistic effect of physical scouring and chemical dissolution for deposits of different properties, efficiently removing shell side deposits and restoring the condensation heat transfer coefficient of the total condenser 300 to above the second preset threshold. This effectively solves the bottleneck problem that reduces heat exchange efficiency and condensation capacity due to deposits, thus limiting production growth and extending the continuous operation cycle of the total condenser 300.
[0029] S4. A sleeve 402 is coaxially installed inside the float 401 of the capacitive level gauge 403 within the chlorination tower body 100, and the capacitive level gauge 403 is inserted into the sleeve 402. The upper section of the sleeve 402 has a vent hole 4021, and the lower section has a damping hole 4022. Specifically, the coaxial installation of the sleeve 402 inside the float 401 of the capacitive level gauge 403, with the vent hole 4021 in the upper section and the damping hole 4022 in the lower section, effectively isolates the interference of gas relative capacitance measurement. Simultaneously, the damping hole 4022 reduces the impact of liquid level fluctuations on the medium inside the float, making the measurement signal of the capacitive level gauge 403 more stable and accurate. This improves the monitoring accuracy and reliability of the liquid level within the chlorination tower body 100, providing real data support for process control, avoiding feed or discharge imbalances caused by misjudgments of the liquid level, and thus ensuring the continuous and stable operation of the reaction process.
[0030] S5. By real-time monitoring of the pressure drop and liquid level of chlorine nozzles 101 and acetylene nozzles 102 within the chlorination tower body 100, the vacuum level of the negative pressure device 200, and the temperature difference of the total condenser 300, the normal operation of the reaction process within the chlorination tower body 100 is ensured. Real-time monitoring of key process parameters such as the pressure drop of chlorine nozzles 101 and acetylene nozzles 102, the liquid level within the tower, the vacuum level, and the temperature difference of the total condenser 300 can promptly detect potential fault signs such as nozzle blockage, abnormal liquid levels, vacuum leaks, or deterioration of heat exchange, facilitating rapid control decisions by operators. This not only significantly improves the safety and controllability of the chlorination tower body 100 operation and reduces the operational risks in the flammable and explosive environment of acetylene, but also provides data support for process optimization and production improvement.
[0031] The method for increasing the output of the acetylene chlorination tower provided in this application improves the reaction rate and conversion rate by optimizing the nozzle arrangement and negative pressure operation; the efficient total condenser 300 cleaning method maintains the load capacity of the subsequent condensation and separation stages; and precise liquid level monitoring and multi-parameter monitoring ensure stable operation of the entire process. Furthermore, this method can effectively overcome the production bottleneck of the existing acetylene chlorination tower body 100 through synergistic optimization of the process and equipment without increasing the main equipment investment, achieving a significant increase in the output of the chlorination tower body 100, while reducing energy consumption and maintenance frequency, thus possessing good economic benefits and industrial application value.
[0032] In some embodiments, the first preset number of rows in this application is 2-4 rows, the first preset number of nozzles is 36-38, and the first preset orifice diameter is 4mm-6mm; wherein, chlorine nozzles 101 and acetylene nozzles 102 are respectively arranged in 2-4 alternating rows, with 36-38 chlorine nozzles 101 and 42-44 acetylene nozzles 102 per row. This configuration of the number of rows and nozzles allows the chlorination tower body 100 to form a multi-layered, dense, staggered spray grid in the axial and radial cross-sections, significantly increasing the contact area and turbulence of chlorine and acetylene. Simultaneously, the number of acetylene nozzles 102 is slightly greater than that of chlorine nozzles 101, which can create a more favorable local concentration field distribution within the chlorination tower body 100 for the reaction, effectively avoiding over-chlorination or side reactions caused by excessively high local chlorine concentrations, thereby improving the selectivity of the main reaction and the acetylene conversion rate.
[0033] The second preset number of rows is 2-4, the second preset number of orifices is 42-44, and the second preset orifice diameter is 4mm-7mm. Due to the differences in density, viscosity, and other physical properties between chlorine and acetylene, the aforementioned differentiated orifice diameter design allows for a more matched injection velocity and diffusion angle under similar or identical pressure drop conditions. Chlorine forms a more concentrated jet through the smaller orifice diameter (4-6mm), while acetylene forms a wider coverage area through the slightly larger orifice diameter (4-7mm). Both achieve momentum complementarity and efficient entrainment within the 100mm space of the chlorination tower body, further enhancing gas-phase mixing uniformity and providing ideal mass transfer conditions for the chlorination reaction.
[0034] Furthermore, in actual operation, specifically, the applicant sets the first preset row number and the second preset row number to 3, the first preset number of nozzles to 37, the first preset orifice diameter to 5mm, the second preset number of nozzles to 43, and the second preset orifice diameter to 6mm. In some embodiments, the chlorine nozzle 101 and the acetylene nozzle 102 in this application are both inclined downwards, and the angle between their axes and the central axis of the chlorination tower body 100 is 15°~25°. The downward inclination of the nozzles so that the nozzles face downwards can effectively prevent the accumulation and deposition of droplet backflow, condensate, or trace solid byproducts generated during the reaction process at the nozzles that may exist in the chlorination tower body 100. Compared to horizontally or upwardly positioned nozzles, this downwardly tilted structure fully utilizes gravity, allowing the falling liquid phase or particles to slide naturally, significantly reducing the risk of nozzle clogging. Furthermore, the tilted jet generates strong turbulence and entrainment effects within the chlorination tower body 100, significantly increasing the contact area and contact time between chlorine and acetylene, promoting momentum exchange and mass transfer between the gas phases. Additionally, when the angle is less than 15°, the radial dispersion of the jet is insufficient, making it difficult to achieve effective cross-mixing with adjacent nozzle jets in the central region of the chlorination tower body 100. When the angle is greater than 25°, the axial velocity component of the jet is too large, easily leading to a shortened residence time of the gas within the chlorination tower body 100 and potentially causing excessive impact on the lower liquid phase within the chlorination tower body 100. Angles within the range of 15° to 25° ensure sufficient radial mixing while maintaining a reasonable gas phase residence time and pressure drop distribution within the chlorination tower body 100, working synergistically with the negative pressure device 200 to provide a stable and efficient gas phase environment for the chlorination reaction.
[0035] In this design, the chlorine and acetylene nozzles 102 are staggered in every two adjacent rows, allowing the spray coverage areas of adjacent rows to compensate for each other across the tower's cross-section. This effectively eliminates radial dead zones and uneven concentration distribution that may exist between nozzles in the same layer or between layers. Chlorine and acetylene can achieve sufficient contact at different heights and radial positions within the chlorination tower body 100, avoiding problems such as over-chlorination, localized overheating, or aggravated side reactions caused by excessively high local reactant concentrations. This staggered arrangement significantly improves the utilization rate of the longitudinal section of the chlorination tower body 100, making the reaction conditions in all areas within the chlorination tower body 100 more consistent, which is beneficial for achieving a stable and controllable overall reaction process.
[0036] In some embodiments, the first preset threshold in this application is -72 kPa to -65 kPa.
[0037] In the above embodiments, the vacuum level within the chlorination tower body 100 is controlled within the range of -72 kPa to -65 kPa, enabling acetylene chlorination reaction to proceed at an operating pressure significantly lower than atmospheric pressure. According to the principle of chemical equilibrium, reducing system pressure promotes the chlorination reaction towards product formation, while simultaneously achieving an ideal reaction rate at a lower temperature. This negative pressure range effectively avoids the thermal decomposition and polymerization of acetylene under high-temperature conditions, significantly reducing carbon buildup, blockage, and safety risks caused by acetylene decomposition, and improving reaction selectivity and the yield of the target product. In some embodiments, the total condenser 300 in this application is made of graphite. Because the acetylene chlorination reaction system contains highly corrosive media such as chlorine and hydrogen chloride, conventional metal total condensers are prone to corrosion and perforation, leading to leakage. Using graphite to manufacture the total condenser fully utilizes graphite's excellent corrosion resistance, effectively resisting chemical erosion from chlorine-containing media, significantly reducing corrosion thinning and leakage risks in the shell and tube sides, greatly extending the service life of the total condenser 300, reducing equipment replacement frequency and maintenance costs, and ensuring long-term continuous operation of the acetylene chlorination tower system.
[0038] The second preset threshold is 38 W / (m·K)-42 W / (m·K). This heat transfer coefficient threshold ensures that the gaseous material exiting the chlorination tower body 100 can be fully condensed, removing residual heat from the reaction system in a timely manner, thereby helping to maintain the negative pressure state inside the tower. If the heat transfer coefficient is too low, the condensation capacity is insufficient, and the gaseous phase accumulates inside the chlorination tower body 100, leading to increased pressure, disrupting the negative pressure environment, and thus reducing the reaction rate and acetylene conversion rate. The setting of this threshold range effectively overcomes the bottleneck that limits production increase due to deteriorated condensation effect.
[0039] In some embodiments, the inner diameter of the sleeve 402 in this application is 5mm-10mm larger than the outer diameter of the capacitive level gauge 403 to form a narrow annular gap damping channel 404 between them; wherein, the narrow annular gap damping channel 404 has significant flow resistance characteristics. When the liquid level in the chlorination tower body 100 fluctuates violently due to feed fluctuations, reaction disturbances, or gas-liquid impacts, the narrow annular gap can significantly slow down the rate at which the liquid phase enters and flows out of the sleeve, playing a mechanical damping role on the liquid level fluctuation, making the liquid level change in the sleeve 402 tend to be stable, and avoiding a drastic deviation between the liquid level in the float 401 and the actual liquid level in the chlorination tower body 100.
[0040] The vent hole 4021 has a diameter of 3mm-6mm. This 3mm-6mm diameter vent hole 4021 allows the gaseous phase entering the sleeve 402 to be promptly discharged to the upper space of the sleeve 4021 and returned to the gaseous phase zone within the chlorination tower body 100. Under the negative pressure operating environment of the acetylene chlorination tower, if the gaseous medium accumulates in the upper part of the sleeve 402, it will interfere with the electric field distribution of the capacitive level gauge 403, leading to distorted liquid level measurement. This aperture range ensures smooth gas discharge without weakening the damping effect due to excessively large apertures, ensuring that the capacitive level gauge 403 only responds to a stable liquid level within the sleeve 402, significantly improving the accuracy of liquid level measurement. The damping orifice 4022 has a diameter of 2mm-3mm. The damping orifice 4022 serves as the main channel for liquid phase entry into the sleeve 402. Its small orifice diameter creates local resistance to liquid flow, effectively filtering high-frequency liquid level fluctuations within the chlorination tower body 100 caused by rising bubbles, flooding, or pulsed feeding. This orifice diameter range has been optimized: if the orifice diameter is too large (greater than 3 mm), the damping effect is insufficient, and the liquid level within the sleeve 402 fluctuates drastically with the fluctuations within the chlorination tower body 100; if the orifice diameter is too small (less than 2 mm), the liquid phase entry and exit are too slow, resulting in a severe lag in the liquid level response within the sleeve 402, failing to reflect the true liquid level in a timely manner. The 2 mm-3 mm damping orifice 4022 achieves a good balance between response speed and fluctuation suppression.
[0041] In some embodiments, the specific steps of S5 in this application are as follows: S51, Level 1 Response: When the liquid level fluctuation within the chlorination tower body 100 exceeds the third preset threshold (where the third preset threshold is, for example, ±5%) or the temperature difference in the total condenser 300 exceeds the fourth preset threshold (where the fourth preset threshold is 6℃), the Level 1 audible and visual warning module 501 is triggered. Setting the trigger condition for Level 1 response to a liquid level fluctuation greater than ±5% or a total condenser temperature difference greater than 6℃ constitutes an early and sensitive identification of process anomalies. The ±5% liquid level fluctuation threshold can promptly detect feed imbalances, poor discharge, or gas-liquid balance disruptions in the initial stage of the reaction; the 6℃ temperature difference threshold can quickly reflect a decrease in the heat exchange efficiency of the total condenser 300 or abnormal gas phase load. At this time, only the audible and visual warning is triggered to remind operators to pay attention and make preventive adjustments, avoiding the continued deterioration of the anomaly in a concealed state, reserving sufficient response window for subsequent process adjustments, and effectively preventing small problems from evolving into major failures.
[0042] S52. Secondary Response: When the fluctuation value of the liquid level in the chlorination tower body 100 is greater than the fifth preset threshold (where the second preset threshold is greater than the fourth preset threshold, and the fifth preset threshold is, for example, ±8%) or the vacuum degree deviates from the sixth preset threshold (where the sixth preset threshold is 3 kPa), the feed amount of chlorine and acetylene added to the chlorination tower body 100 is reduced (wherein, the feed amount at this time is 10%~15% of the feed amount under normal conditions); when the liquid level fluctuation reaches ±8% or the vacuum degree deviates from the sixth preset threshold (3 kPa), the system automatically executes the secondary response, reducing the feed amount of chlorine and acetylene to 10%~15% of the normal amount. The technical advantages of this design are as follows: On the one hand, by significantly reducing the feed rate of reactants, the rate of heat generation and the amount of gas generated within the chlorination tower body 100 are rapidly reduced, thereby suppressing drastic fluctuations in liquid level or continuous deterioration of vacuum from the source; on the other hand, maintaining a low-load operation of 10%~15% instead of direct shutdown allows the chlorination tower body 100 to maintain basic material circulation and temperature field stability under abnormal operating conditions, facilitating rapid troubleshooting and restoration of full-load production after the fault is eliminated, significantly shortening the abnormal recovery time and reducing material loss and capacity loss during start-up and shutdown.
[0043] S53. Level 3 Response: When the liquid level inside the chlorination tower body 100 is below the lower limit or above the upper limit, or the vacuum level inside the chlorination tower body 100 is greater than the seventh preset threshold (wherein, the seventh preset threshold is less than the sixth preset threshold, and the seventh preset threshold is, for example, -58 kPa), or the pressure drop of the chlorine nozzle 101 and / or the acetylene nozzle 102 is less than the eighth preset threshold (wherein, the eighth preset threshold is 0.05 MPa), the feed of chlorine and acetylene is immediately cut off, and the nitrogen purging procedure is initiated. Specifically, the triggering conditions for Level 3 response are set as follows: liquid level exceeding the upper or lower limit, vacuum level greater than -58 kPa (i.e., severe loss of vacuum, system tending towards atmospheric pressure), or nozzle pressure drop less than 0.05 MPa. These thresholds correspond to the inherent safety red lines of the acetylene chlorination process: 1) Exceeding the liquid level limit may cause gas to enter the liquid phase pipeline or liquid to backflow into the gas phase system, leading to flooding or pressure shock; 2) A vacuum level deteriorating to -58 kPa (compared to the normal operating range of -72 kPa to -65 kPa, the absolute pressure is significantly higher), indicating system seal failure or abnormal gas intake, resulting in increased acetylene partial pressure and a sharp rise in the risk of decomposition and explosion; 3) A nozzle pressure drop of less than 0.05 MPa indicates that the nozzle is severely blocked or the gas supply is interrupted, which may lead to an imbalance in reactant ratios, local overheating, or uncontrolled reaction. Immediately cutting off the chlorine and acetylene feed and initiating nitrogen purging can terminate the reaction and replace flammable and explosive gases within 100°C of the chlorination tower body in the shortest possible time, fundamentally preventing serious safety accidents such as acetylene decomposition, chloroacetylene generation, or mixed gas explosion. In the above embodiments, a three-tiered response mechanism—primary audible and visual warning 501, secondary automatic feed reduction, and tertiary emergency shut-off and nitrogen purging—achieves graded control of the operational risks of the chlorination tower 100. Compared to the traditional "single threshold shutdown" mode, this graded strategy can provide early warnings and allow operator intervention when process parameters deviate slightly; automatically reduce load to prevent escalation when parameters are moderately abnormal; and only execute emergency shutdown when severe abnormalities occur. This progressive response significantly reduces the frequency of unplanned shutdowns caused by minor fluctuations or brief disturbances, and significantly increases the annual cumulative operating time of the chlorination tower 100 while ensuring inherent safety, providing process continuity assurance for increased production.
[0044] The present invention will be further described in detail below with reference to embodiments. However, it should be understood that the embodiments are for illustrative purposes only and are not intended to limit the scope of the present invention.
[0045] Example 1
[0046] The method for increasing the output of the acetylene chlorination tower in this embodiment includes the following steps: S1. Three rows of chlorine gas nozzles 101 and three rows of acetylene gas nozzles 102 are alternately arranged along their own axial direction inside the chlorination tower body 100. Each row of chlorine nozzles 101 comprises 37 chlorine nozzles 101, each with an orifice diameter of 5 mm; each row of acetylene nozzles 102 comprises 43 acetylene nozzles 102, each with an orifice diameter of 6 mm. Furthermore, the chlorine nozzles are inclined downwards with their axes forming an angle of 15° with the central axis of the chlorination tower body, and the acetylene nozzles are inclined downwards with their axes forming an angle of 25° with the central axis of the chlorination tower body.
[0047] S2. The vacuum pressure inside the chlorination tower body 100 is set to -65 kPa by the negative pressure device 200; S3. Handholes are installed on the shell side of the total condenser 300 at 1 / 3 and 1 / 2 of the distance from the top. The shell side deposits of the total condenser 300 are cleaned through the handholes by alternating high-pressure water jet and citric acid chemical cleaning, so that the condensation heat transfer coefficient of the total condenser 300 is greater than or equal to 38 W / (m·K). S4. A sleeve 402 is coaxially installed inside the float 401 of the capacitive level meter 403 inside the chlorination tower body 100, and the capacitive level meter 403 is inserted into the sleeve 402; wherein, the upper section of the sleeve 402 is provided with an exhaust hole 4021, and the lower section is provided with a damping hole 4022. S5. By real-time monitoring of the pressure drop and liquid level of chlorine nozzles 101 and acetylene nozzles 102 in the chlorination tower body 100, the vacuum degree of the negative pressure device 200, and the temperature difference of the total condenser 300, the normal operation of the reaction process in the chlorination tower body 100 is ensured. The specific steps of S5 above are as follows: S51, Level 1 Response: When the fluctuation of the liquid level in the chlorination tower body 100 is greater than the third preset threshold (wherein, the third preset threshold is, for example, ±5%) or the temperature difference in the total condenser 300 is greater than the fourth preset threshold (wherein, the fourth preset threshold is 6℃), the Level 1 audible and visual warning module is triggered. S52. Secondary Response: When the fluctuation value of the liquid level in the chlorination tower body 100 is greater than the fifth preset threshold (wherein, the second preset threshold is greater than the fourth preset threshold, and the fifth preset threshold is, for example, ±8%) or the vacuum degree deviates from the sixth preset threshold (wherein, the sixth preset threshold is 3kPa), reduce the amount of chlorine and acetylene fed into the chlorination tower body 100 (wherein, the amount fed at this time is 10% of the amount fed under normal conditions). S53, Level 3 Response: When the liquid level inside the chlorination tower body 100 is less than the lower limit or greater than the upper limit, or the vacuum degree inside the chlorination tower body 100 is greater than the seventh preset threshold (wherein, the seventh preset threshold is less than the sixth preset threshold, and the seventh preset threshold is, for example, -58kPa), or the pressure drop of the chlorine nozzle 101 and / or the acetylene nozzle 102 is less than the eighth preset threshold (wherein, the eighth preset threshold is 0.05MPa), immediately cut off the feed of chlorine and acetylene, and start the nitrogen purging procedure.
[0048] Example 2
[0049] The method for increasing the output of the acetylene chlorination tower in this embodiment includes the following steps: S1. Four rows of chlorine gas nozzles 101 and four rows of acetylene nozzles 102 are alternately arranged along their own axial direction inside the chlorination tower body 100. Each row of chlorine nozzles 101 comprises 38 chlorine nozzles 101, each with an orifice diameter of 4 mm; each row of acetylene nozzles 102 comprises 44 acetylene nozzles 102, each with an orifice diameter of 4 mm. Furthermore, the chlorine nozzles are inclined downwards with their axes forming a 25° angle with the central axis of the chlorination tower body, while the acetylene nozzles are inclined downwards with their axes forming a 15° angle with the central axis of the chlorination tower body.
[0050] S2. The vacuum pressure inside the chlorination tower body 100 is set to -72kPa by the negative pressure device 200; S3. Handholes are installed on the shell side of the total condenser 300 at 1 / 3 and 1 / 2 of the distance from the top. The shell side deposits of the total condenser 300 are cleaned through the handholes by alternating high-pressure water jet and citric acid chemical cleaning, so that the condensation heat transfer coefficient of the total condenser 300 is greater than or equal to 38 W / (m·K). S4. A sleeve 402 is coaxially installed inside the float 401 of the capacitive level meter 403 inside the chlorination tower body 100, and the capacitive level meter 403 is inserted into the sleeve 402; wherein, the upper section of the sleeve 402 is provided with an exhaust hole 4021, and the lower section is provided with a damping hole 4022. S5. By real-time monitoring of the pressure drop and liquid level of chlorine nozzles 101 and acetylene nozzles 102 in the chlorination tower body 100, the vacuum degree of the negative pressure device 200, and the temperature difference of the total condenser 300, the normal operation of the reaction process in the chlorination tower body 100 is ensured. The specific steps of S5 above are as follows: S51, Level 1 Response: When the fluctuation of the liquid level in the chlorination tower body 100 is greater than the third preset threshold (wherein, the third preset threshold is, for example, ±5%) or the temperature difference in the total condenser 300 is greater than the fourth preset threshold (wherein, the fourth preset threshold is 6℃), the Level 1 audible and visual warning module is triggered. S52. Secondary Response: When the fluctuation value of the liquid level in the chlorination tower body 100 is greater than the fifth preset threshold (wherein, the second preset threshold is greater than the fourth preset threshold, and the fifth preset threshold is, for example, ±8%) or the vacuum degree deviates from the sixth preset threshold (wherein, the sixth preset threshold is 3kPa), reduce the amount of chlorine and acetylene fed into the chlorination tower body 100 (wherein, the amount fed at this time is 15% of the amount fed under normal conditions). S53, Level 3 Response: When the liquid level inside the chlorination tower body 100 is less than the lower limit or greater than the upper limit, or the vacuum degree inside the chlorination tower body 100 is greater than the seventh preset threshold (wherein, the seventh preset threshold is less than the sixth preset threshold, and the seventh preset threshold is, for example, -58kPa), or the pressure drop of the chlorine nozzle 101 and / or the acetylene nozzle 102 is less than the eighth preset threshold (wherein, the eighth preset threshold is 0.05MPa), immediately cut off the feed of chlorine and acetylene, and start the nitrogen purging procedure.
[0051] Example 3
[0052] The method for increasing the output of the acetylene chlorination tower in this embodiment includes the following steps: S1. Two rows of chlorine gas nozzles 101 and two rows of acetylene nozzles 102 are alternately arranged along their own axial direction inside the chlorination tower body 100. Each row of chlorine nozzles 101 comprises 36 chlorine nozzles 101, each with an orifice diameter of 6 mm; each row of acetylene nozzles 102 comprises 42 acetylene nozzles 102, each with an orifice diameter of 7 mm. Furthermore, the chlorine nozzles are inclined downwards with their axes forming an angle of 25° with the central axis of the chlorination tower body, and the acetylene nozzles are inclined downwards with their axes forming an angle of 15° with the central axis of the chlorination tower body.
[0053] S2. The vacuum pressure inside the chlorination tower body 100 is set to -68kPa by the negative pressure device 200; S3. Handholes are installed on the shell side of the total condenser 300 at 1 / 3 and 1 / 2 of the distance from the top. The shell side deposits of the total condenser 300 are cleaned through the handholes by alternating high-pressure water jet and citric acid chemical cleaning, so that the condensation heat transfer coefficient of the total condenser 300 is greater than or equal to 38 W / (m·K). S4. A sleeve 402 is coaxially installed inside the float 401 of the capacitive level meter 403 inside the chlorination tower body 100, and the capacitive level meter 403 is inserted into the sleeve 402; wherein, the upper section of the sleeve 402 is provided with an exhaust hole 4021, and the lower section is provided with a damping hole 4022. S5. By real-time monitoring of the pressure drop and liquid level of chlorine nozzles 101 and acetylene nozzles 102 in the chlorination tower body 100, the vacuum degree of the negative pressure device 200, and the temperature difference of the total condenser 300, the normal operation of the reaction process in the chlorination tower body 100 is ensured. The specific steps of S5 above are as follows: S51, Level 1 Response: When the fluctuation of the liquid level in the chlorination tower body 100 is greater than the third preset threshold (wherein, the third preset threshold is, for example, ±5%) or the temperature difference in the total condenser 300 is greater than the fourth preset threshold (wherein, the fourth preset threshold is 6℃), the Level 1 audible and visual warning module is triggered. S52. Secondary Response: When the fluctuation value of the liquid level in the chlorination tower body 100 is greater than the fifth preset threshold (wherein, the second preset threshold is greater than the fourth preset threshold, and the fifth preset threshold is, for example, ±8%) or the vacuum degree deviates from the sixth preset threshold (wherein, the sixth preset threshold is 3kPa), reduce the amount of chlorine and acetylene fed into the chlorination tower body 100 (wherein, the amount fed at this time is 10% of the amount fed under normal conditions). S53, Level 3 Response: When the liquid level inside the chlorination tower body 100 is less than the lower limit or greater than the upper limit, or the vacuum degree inside the chlorination tower body 100 is greater than the seventh preset threshold (wherein, the seventh preset threshold is less than the sixth preset threshold, and the seventh preset threshold is, for example, -58kPa), or the pressure drop of the chlorine nozzle 101 and / or the acetylene nozzle 102 is less than the eighth preset threshold (wherein, the eighth preset threshold is 0.05MPa), immediately cut off the feed of chlorine and acetylene, and start the nitrogen purging procedure.
[0054] Comparative Example 1 In S1, the chlorine nozzle 101101 adopts a 7-row × 57-hole × 10mm orifice design, and the acetylene nozzle 102102 adopts a 7-row × 46-hole × 12mm orifice design. The remaining steps in S1, as well as S2, S3, S4 and S5, are the same as in Example 1.
[0055] Comparative Example 2 The vacuum pressure of the chlorination tower body 100 in S2 is -58 kPa, and the remaining steps are the same as in Example 1.
[0056] Comparative Example 3 The S3 condenser 300 has no handhole and uses an open cooling tower circulating water cooling system. The total condenser 300 is made of carbon steel.
[0057] The remaining steps are the same as in Example 1.
[0058] Comparative Example 4 In S4, the float 401 of the capacitive level meter 403 is not fitted with a sleeve 402, and the capacitive level meter 403 is directly inserted into the float 401. The inner diameter of the float 401 is much larger than the outer diameter of the capacitive level meter 403. The remaining steps are the same as in Example 1.
[0059] The parameters of acetylene single-pass conversion rate (in %), tetrachloroethane daily production (in t / d), condensation heat transfer coefficient (in W / (m·K)), liquid level monitoring error (in %), and explosion / abnormal events (in times / year) in Examples 1, 2, and 3, and Comparative Examples 1, 2, 3, and 4 were calculated. The calculation period for the above parameters was 12 months. The calculation of acetylene single-pass conversion rate and tetrachloroethane daily production was based on SH / T 1141-2015 "Gas Chromatography for Determination of Hydrocarbon Composition of Cracked C4 for Industrial Use" or GB / T The determination of hydrocarbon impurities in industrial ethylene was performed using gas chromatography (GC) according to GB / T 27698.1-2011 "Test Methods for Performance of Heat Exchangers and Heat Transfer Elements". The calculation of the condensation heat transfer coefficient was performed according to JJG 971-2002 "Verification Procedure for Level Gauges". The calculation of the liquid level monitoring error was performed according to JJG 971-2002 "Verification Procedure for Level Gauges". The calculation of the number of explosions / abnormal events was performed according to GB 50160-2008 "Fire Protection Design Standards for Petrochemical Enterprises" and AQ 3013-2008 "General Specifications for Safety Standardization of Hazardous Chemical Enterprises". The specific calculation results are shown in Table 1. Table 1
[0060] By comparing Comparative Examples 1, 2, 3, and 4 with Example 1, it can be seen that, compared with the existing chlorine nozzle 101 and acetylene nozzle 102, this application reduces the nozzle orifice diameter (4-6 mm), reduces the number of rows (2-4 rows), staggers the arrangement, and tilts downwards (15°-25°), enabling uniform and sufficient contact and mixing of chlorine and acetylene in the radial and axial directions within the chlorination tower body 100. This significantly increases the gas phase contact area and turbulence, thereby stably increasing the single-pass conversion rate to over 91%. However, comparing Comparative Examples 2 and 3 with Example 1, it can be seen that although the total condenser 300 in Comparative Example 2 is made of graphite (the same as in Example 1), the vacuum degree is only -58 kPa (the absolute pressure is about 7 kPa higher than -65 kPa), causing the gas phase temperature at the top of the chlorination tower body 100 to rise, increasing the partial pressure of non-condensable gases. Consequently, the actual operating heat transfer coefficient drops to 33 due to the deteriorating operating conditions. W / (m·K) indicates that the optimization of vacuum pressure and the performance of the total condenser 300 are mutually dependent, and improving one alone cannot achieve maximum efficiency. The liquid level error of Comparative Example 4 is as high as ±15% (about 6 times that of Example 1), while the errors of Examples 1 to 3 are only ±2.5% to ±2.6%. ±15% is about 6 times that of the Examples, which means that the design of the sleeve 402 structure (the inner diameter is 5 to 10 mm larger than the outer diameter of the capacitive level gauge 403 to form a narrow annular gap damping channel 404, with a 3 to 6 mm vent hole 4021 in the upper section and a 2 to 3 mm damping hole 4022 in the lower section) greatly improves the accuracy of liquid level monitoring. Although the liquid level errors of Comparative Examples 1 to 3 are lower than those of Comparative Example 4, they are still higher than those of Example 1. This means that process fluctuations (uneven nozzles, low vacuum, material of condenser 300, manhole settings, etc.) are transmitted to the measurement stage through liquid phase dynamics, thus affecting the accuracy of the measurement results. This further illustrates the importance of "multi-parameter synergistic optimization" in this application.
[0061] Furthermore, by comparing Examples 2 and 3 with Example 1, it can be seen that after simultaneously improving multiple factors such as the chlorine nozzle 101, acetylene nozzle 102, vacuum pressure, total condenser 300, and liquid level monitoring in this application, even though there are slight differences between the parameters in Examples 1 to 3, the final calculation results in Table 1 are not significantly different, and the calculation results of each parameter in Examples 1 to 3 are better than those in Comparative Example 1. In other words, this application, through multi-parameter synergistic optimization, not only solves the systemic defects of the acetylene chlorination tower such as "low output, high energy consumption, and high risk," but also ensures that the chlorination tower body 100 can operate safely, stably, and efficiently.
[0062] Secondly, refer to Figures 1 to 5 This application provides an acetylene chlorination tower system, applied to any of the above-described methods for increasing the output of an acetylene chlorination tower, comprising: The chlorination tower body 100 is used to produce acetylene and includes a first preset number of chlorine nozzles 101 and a second preset number of acetylene nozzles 102. Each row of chlorine nozzles 101 includes a first preset number of chlorine nozzles 102, and the orifice diameter of each chlorine nozzle 101 is a first preset orifice diameter. Each row of acetylene nozzles 102 includes a second preset number of acetylene nozzles 102, and the orifice diameter of each acetylene nozzle 102 is a second preset orifice diameter. Specifically, by integrating the first preset number of chlorine nozzles 101 and the second preset number of acetylene nozzles 102 alternately arranged within the chlorination tower body 100, and by defining the number of rows, the number of nozzles per row, and the orifice diameter of each nozzle, the system can achieve uniform and sufficient contact and mixing of chlorine and acetylene within the tower, effectively avoiding incomplete reactions or increased side reactions caused by uneven local concentrations. This structural layout provides optimized gas-phase distribution conditions for the acetylene chlorination reaction, which helps to improve the single-pass conversion rate and reaction selectivity of acetylene, thus laying a hardware foundation for increased yield.
[0063] The negative pressure device 200 is connected to the chlorination tower body 100 through the negative pressure pipe 201 and is used to adjust the vacuum degree inside the chlorination tower body 100. By adjusting the vacuum degree inside the chlorination tower body 100 to a preset range through the connection structure between the negative pressure device 200 and the chlorination tower body 100, the operating temperature of the chlorination reaction can be reduced and the forward reaction can be promoted.
[0064] The total condenser 300 is connected to the gas phase outlet of the chlorination tower body 100 via a gas pipeline 301. It is used to condense the gaseous products exiting the chlorination tower body 100 to lower the temperature and maintain a negative pressure state within the chlorination tower body 100. The total condenser 300, connected to the gas phase outlet of the chlorination tower body 100 via gas pipeline 301, not only condenses and recovers the gaseous products but also continuously removes heat from the gas phase during the condensation process, helping to maintain the stability of the negative pressure state within the chlorination tower body 100. The negative pressure device 200 and the total condenser 300 form a synergistic working mechanism, ensuring that the temperature and pressure environment within the chlorination tower body 100 remains stable and controllable over a long period. This improves reaction efficiency and reduces the risk of decomposition and explosion of acetylene under high temperature and pressure, significantly enhancing the safety of system operation.
[0065] The liquid level monitoring device 400 includes a float 401, a sleeve 402 coaxially disposed within the float 401, and a capacitive level gauge 403 inserted within the sleeve 402. The liquid level monitoring device 400 employs a structural design where the sleeve 402 is coaxially disposed within the float 401, and the capacitive level gauge 403 is inserted within the sleeve 402. Combined with the vent 4021 in the upper section and the damping orifice 4022 in the lower section of the sleeve 402, it effectively isolates interference from gas phase capacitance measurement and mitigates the influence of buffer level fluctuations on the measurement signal. This structure enables the liquid level monitoring device 400 to maintain high measurement accuracy and stability even under the complex operating conditions of the chlorination tower 100, providing reliable data for material balance control, avoiding feed imbalance or reaction abnormalities caused by liquid level distortion, and ensuring the long-term continuous and stable operation of the chlorination tower 100.
[0066] The DCS control unit 500 is electrically connected to the negative pressure device 200, the total condenser 300, and the liquid level monitoring device 400, and is used to control the operation of these devices. Through the electrical connection between the DCS control unit 500 and these devices, an automated control architecture of centralized monitoring and decentralized execution is established. The DCS control unit 500 can collect and process the operating parameters of each device in real time, achieving coordinated adjustment and precise control of key process indicators such as vacuum degree, condensing temperature, and liquid level. Compared with traditional manual operation or single-point control modes, this integrated control method significantly improves the system's response speed and control accuracy, reduces human error, and ensures that all functional units are always in optimal collaborative working condition.
[0067] In some embodiments, reference Figure 3In this application, the inner diameter of the sleeve 402 is 5mm-10mm larger than the outer diameter of the capacitive level gauge 403 to form a narrow annular gap damping channel 404 between them. The 3mm-6mm vent hole 4021 allows the gas phase entering the sleeve 402 to be promptly discharged to the upper space of the sleeve 402 and returned to the gas phase zone within the chlorination tower body 100. Under the negative pressure operating environment of the acetylene chlorination tower, if the gaseous medium accumulates in the upper part of the sleeve 402, it will interfere with the electric field distribution of the capacitive level gauge 403, leading to distorted liquid level measurement. This orifice diameter range ensures smooth gas discharge without weakening the damping effect due to excessively large orifices, ensuring that the capacitive level gauge 403 only responds to the stable liquid level within the sleeve 402, significantly improving the accuracy of liquid level measurement. The upper section of the sleeve 402 has a 3mm-6mm vent hole 4021, and the lower section has a 2mm-3mm damping hole 4022. The damping orifice 4022 serves as the main channel for liquid phase entry into the sleeve 402. Its small aperture creates local resistance to liquid flow, effectively filtering high-frequency liquid level fluctuations within the chlorination tower body 100 caused by rising bubbles, flooding, or pulsed feeding. This aperture range has been optimized: if the aperture is too large (greater than 3 mm), the damping effect is insufficient, and the liquid level within the sleeve 402 fluctuates drastically with changes within the tower; if the aperture is too small (less than 2 mm), the liquid phase inflow and outflow are too slow, resulting in a severe lag in the liquid level response within the sleeve 402, failing to reflect the true liquid level in a timely manner. The 2-3 mm damping orifice 4022 achieves a good balance between response speed and fluctuation suppression.
[0068] In some embodiments, reference Figure 5 The DCS control unit 500 in this application includes a primary audible and visual warning module 501, a secondary automatic feeding adjustment module 502, and a tertiary emergency shut-off and nitrogen purging module 503. Specifically, the DCS control unit 500 is divided into a primary audible and visual warning module 501, a secondary automatic feeding adjustment module 502, and a tertiary emergency shut-off and nitrogen purging module 503, thereby realizing the hierarchical decoupling of control functions.
[0069] The primary audible and visual early warning module 501 is triggered when the liquid level fluctuation within the chlorination tower body 100 exceeds a third preset threshold (where the third preset threshold is ±5%) or the temperature difference in the total condenser exceeds a fourth preset threshold (where the fourth preset threshold is 6℃). Specifically, the primary audible and visual early warning module 501 provides timely alerts to operators through a dual audible and visual warning system for initial abnormal operating conditions, such as liquid level fluctuations exceeding ±5% or temperature differences in the total condenser 300 exceeding 6℃. The technical advantage of this module is that it can issue a clear alarm in the early stages when process parameters deviate from the normal range but have not yet caused substantial damage to the system. This provides operators with ample time for judgment and intervention, allowing them to eliminate the root cause of the abnormality through preventative operations such as manually fine-tuning the feed, checking the condensation system, or cleaning the filter. This effectively prevents minor disturbances from escalating into serious malfunctions, thereby significantly reducing the frequency of unplanned shutdowns and ensuring the continuous and stable operation of the chlorination tower.
[0070] The secondary feed automatic adjustment module 502 is used to reduce the amount of chlorine and acetylene fed into the chlorination tower body 100 when the fluctuation value of the liquid level in the chlorination tower body 100 is greater than the fifth preset threshold (wherein the fifth preset threshold is ±8%) or the vacuum degree deviates from the sixth preset threshold (wherein the sixth preset threshold is 3kPa). The feed amount at this time is 10%~15% of the feed amount under normal conditions. When the liquid level fluctuation reaches ±8% or the vacuum degree deviates from 3 kPa, the secondary feed automatic adjustment module automatically reduces the amount of chlorine and acetylene fed to 10%~15% of the normal amount. The technical benefits of this module are twofold: First, by rapidly reducing the reactant supply, it lowers the rate of heat generation and gas production within the chlorination tower body 100 at the source, effectively curbing the trend of drastic liquid level fluctuations or continuous deterioration of vacuum. Second, by maintaining a low-load operation of 10%–15% instead of directly cutting off the feed and shutting down, it ensures that the chlorination tower body 100 maintains basic material circulation, temperature field distribution, and negative pressure environment stability, avoiding sudden cooling, heating, or pressure shocks caused by emergency shutdowns. This not only provides relatively stable operating conditions for troubleshooting and root cause analysis but also enables a rapid return to full-load production after anomalies are eliminated, significantly shortening recovery time and material losses during start-up and shutdown, indirectly increasing the unit's average annual effective capacity.
[0071] The three-level emergency shut-off and nitrogen purging module 503 is used to immediately shut off the feed of chlorine and acetylene and initiate a nitrogen purging procedure when the liquid level in the chlorination tower body 100 is below the lower limit or above the upper limit, or the vacuum degree in the chlorination tower body 100 is greater than the seventh preset threshold (wherein the seventh preset threshold is -58 kPa), or the pressure drop of the chlorine nozzle 101 and / or the acetylene nozzle 102 is less than the eighth preset threshold (wherein the eighth preset threshold is 0.05 MPa). Specifically, the three-level emergency shut-off and nitrogen purging module 503 performs the interlocking action of immediately shutting off the feed and initiating nitrogen purging in response to serious anomalies that trigger intrinsic safety limits, such as excessive liquid level, vacuum deterioration to -58 kPa, or nozzle pressure drop below 0.05 MPa. The technical advantages of this module are as follows: Through millisecond-level automatic interlocking response, it terminates the chlorination reaction and cuts off the source of flammable and explosive materials in the shortest possible time. Simultaneously, the nitrogen purging process rapidly replaces residual acetylene, chlorine, and reaction products within the tower, quickly reducing the concentration of flammable gases below the explosion limit. This fundamentally prevents serious safety accidents such as high-temperature decomposition of acetylene, accumulation of chloroacetylene, or explosion of the mixed gas. As the system's final safety barrier, this module's independent operating logic is unaffected by the states of the preceding two modules, ensuring reliable triggering under any extreme conditions and significantly improving the intrinsic safety level of the acetylene chlorination tower system.
[0072] In the above embodiments, by setting the response modules at each level in the DCS control unit 500, the judgment bias and lag caused by differences in operator experience, fatigue, or information transmission delays in the traditional manual operation mode are eliminated. Regardless of the shift or operating condition in which the anomaly occurs, the system performs consistent automated handling according to preset thresholds and response logic, reducing the anomaly response time from minutes in the traditional manual mode to seconds, significantly improving the reliability, safety, and standardization of process control in the acetylene chlorination tower operation.
[0073] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of this application, and are not intended to limit them. Although this application has been described in detail with reference to the foregoing embodiments, those skilled in the art should understand that modifications can still be made to the technical solutions described in the foregoing embodiments, or equivalent substitutions can be made to some or all of the technical features therein. Such modifications or substitutions do not cause the essence of the corresponding technical solutions to deviate from the scope of the technical solutions of the embodiments of this application.
Claims
1. A method for increasing the production of an acetylene chlorination column, characterized in that, The method includes: S1. A first preset number of chlorine nozzles and a second preset number of acetylene nozzles are alternately arranged along the axial direction of the chlorination tower body. Each row of chlorine nozzles includes a first preset number of chlorine nozzles, and the orifice diameter of each chlorine nozzle is the first preset orifice diameter; each row of acetylene nozzles includes a second preset number of acetylene nozzles, and the orifice diameter of each acetylene nozzle is the second preset orifice diameter. The first preset number of rows is 2-4 rows, the first preset number of items is 36-38, and the first preset aperture is 4mm-6mm; The second preset number of rows is 2-4 rows, the second preset number of items is 42-44 items, and the second preset aperture is 4mm-7mm; S2. The vacuum pressure inside the chlorination tower body is set to a first preset threshold using a negative pressure device; The first preset threshold is -72 kPa to -65 kPa; S3. Handholes are provided on the shell side of the total condenser at a first preset height and a second preset height from the top, respectively. The shell side deposits of the total condenser are cleaned through the handholes by alternating high-pressure water jet and citric acid chemical cleaning, so that the condensation heat transfer coefficient of the total condenser is greater than or equal to the second preset threshold. The total condenser is made of graphite. The second preset threshold is 38 W / (m·K) - 42 W / (m·K); S4. A sleeve is coaxially installed inside the float of the capacitive level meter inside the chlorination tower body, and the capacitive level meter is inserted into the sleeve. The upper section of the sleeve is provided with an exhaust hole, and the lower section is provided with a damping hole. The inner diameter of the sleeve is 5mm-10mm larger than the outer diameter of the capacitive level gauge so that a narrow annular gap damping channel is formed between the two. The diameter of the exhaust port is 3mm-6mm; The diameter of the damping orifice is 2mm-3mm; S5. By real-time monitoring of the pressure drop and liquid level of the chlorine and acetylene nozzles inside the chlorination tower body, the vacuum degree of the negative pressure device, and the temperature difference of the total condenser, the normal operation of the reaction process inside the chlorination tower body is ensured.
2. The acetylene chlorination column production enhancement method of claim 1, wherein, Both the chlorine nozzle and the acetylene nozzle are inclined downwards, and the angle between their axes and the central axis of the chlorination tower body is 15° to 25°. The chlorine nozzles and acetylene nozzles are arranged alternately in every two adjacent rows.
3. The acetylene chlorination column production enhancement method of claim 1, wherein, The specific steps of S5 are as follows: S51, Level 1 Response: When the fluctuation of the liquid level in the chlorination tower body is greater than the third preset threshold or the temperature difference of the total condenser is greater than the fourth preset threshold, the Level 1 audible and visual warning module is triggered. S52, Secondary Response: When the fluctuation value of the liquid level in the chlorination tower body is greater than the fifth preset threshold or the vacuum degree deviates from the sixth preset threshold, reduce the amount of chlorine and acetylene fed into the chlorination tower body. S53, Level 3 Response: When the liquid level in the chlorination tower body is less than the lower limit or greater than the upper limit, or the vacuum degree in the chlorination tower body is greater than the seventh preset threshold, or the pressure drop of the chlorine nozzle and / or the acetylene nozzle is less than the eighth preset threshold, the feed of chlorine and acetylene is immediately cut off, and the nitrogen purging procedure is started.
4. An acetylene chlorination column system characterized by, The method for increasing the output of an acetylene chlorination tower according to any one of claims 1 to 3 includes: The chlorination tower body is used to produce acetylene, and includes a first preset number of chlorine nozzles and a second preset number of acetylene nozzles. Wherein, each row of chlorine nozzles includes a first preset number of chlorine nozzles, and the orifice diameter of each chlorine nozzle is the first preset orifice diameter; Each row of acetylene nozzles includes a second preset number of acetylene nozzles, and the orifice diameter of each acetylene nozzle is the second preset orifice diameter; The first preset number of rows is 2-4 rows, the first preset number of items is 36-38, and the first preset aperture is 4mm-6mm; The second preset number of rows is 2-4 rows, the second preset number of items is 42-44 items, and the second preset aperture is 4mm-7mm; A negative pressure device is connected to the chlorination tower body via a negative pressure pipeline and is used to adjust the vacuum level inside the chlorination tower body. The total condenser is connected to the gas phase outlet of the chlorination tower body through a gas pipeline and is used to condense the gas phase coming out of the chlorination tower body to reduce the temperature inside the chlorination tower body and maintain a negative pressure state. A liquid level monitoring device, comprising a float, a sleeve coaxially disposed within the float, and a capacitive level gauge inserted within the sleeve; The inner diameter of the sleeve is 5mm-10mm larger than the outer diameter of the capacitive level gauge so that a narrow annular gap damping channel is formed between the two. The upper section of the sleeve is provided with an exhaust hole with a diameter of 3mm-6mm, and the lower section is provided with a damping hole with a diameter of 2mm-3mm. The DCS control unit is electrically connected to the negative pressure device, the total condenser, and the liquid level monitoring device, and is used to control the operation of the negative pressure device, the total condenser, and the liquid level monitoring device.
5. The acetylene chlorination column system of claim 4, wherein, The DCS control unit includes a primary sound and light warning module, a secondary automatic feeding adjustment module, and a tertiary emergency cut-off and nitrogen purging module. The first-level audible and visual early warning module is used to trigger the first-level audible and visual early warning module when the fluctuation of the liquid level in the chlorination tower body is greater than the third preset threshold or the temperature difference of the total condenser is greater than the fourth preset threshold. The secondary feed automatic adjustment module is used to reduce the amount of chlorine and acetylene fed into the chlorination tower when the fluctuation value of the liquid level in the chlorination tower body is greater than the fifth preset threshold or the vacuum degree deviates from the sixth preset threshold. The three-level emergency shut-off and nitrogen purging module is used to immediately shut off the feed of chlorine and acetylene and start the nitrogen purging program when the liquid level in the chlorination tower body is less than the lower limit or greater than the upper limit, or the vacuum degree in the chlorination tower body is greater than the seventh preset threshold, or the pressure drop of the chlorine nozzle and / or the acetylene nozzle is less than the eighth preset threshold.
Citation Information
Patent Citations
Tetrachloroethane production device and method
CN110479124A
Impinging stream reactor for preparing dichlorobutene by gas phase chlorination of butadiene
CN114505022A
Condenser with labyrinth settlement structure
CN219890209U