A continuous synthesis system and process for ethylene glycol antimony
By combining the sealed feeding device, explosion-proof valve assembly, and phase change insulation structure, the problems of discontinuous feeding and power failure blockage in the production of antimony glycol were solved, realizing continuous production of antimony glycol and improving production efficiency and product quality stability.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- YIYANG HUACHANG ANTIMONY IND CATALYST CO LTD
- Filing Date
- 2026-04-29
- Publication Date
- 2026-07-03
AI Technical Summary
In the existing antimony glycol production process, the unreasonable sealing structure of the feeding device leads to powder caking due to moisture, discontinuous feeding, and material cooling and solidification blocking the pipeline when power is cut off. Furthermore, there is a lack of effective power failure protection mechanisms, which affects production efficiency and safety.
It adopts a sealed feeding device, explosion-proof valve assembly and phase change insulation structure. A dynamic material sealing plug is formed by the conical drive shaft and the screw conveyor blade. The electromagnetic ring demagnetizes and quickly opens the valve seat to discharge residual material. The liquid phase change molten salt medium keeps the material warm and prevents it from cooling, ensuring the continuity of material conveying and the smooth flow of pipelines.
This enabled continuous production of antimony glycol, avoiding powder agglomeration and pipeline blockage, improving raw material utilization and production stability, and reducing the rate of defective products and equipment maintenance costs.
Smart Images

Figure CN122321760A_ABST
Abstract
Description
Technical Field
[0001] This invention belongs to the field of chemical production equipment technology, and relates to a continuous synthesis system and process for antimony glycol. Background Technology
[0002] Antimony glycolate, as an important polyester catalyst, is widely used in polyester synthesis, plastics processing and other industrial fields. Its purity, particle size and stability directly affect the quality of downstream products. Therefore, the synthesis process and production equipment of antimony glycolate have always been the focus of research in the industry. At present, the mainstream process for synthesizing antimony glycolate in industry is the esterification and dehydration reaction of antimony trioxide and ethylene glycol. This reaction needs to be carried out in a high temperature and closed environment, and has high requirements for reaction conditions, material transportation and process control.
[0003] The existing production methods for antimony glycol mainly suffer from the following technical problems, which severely restrict the efficiency, quality, and safety of industrial production, making it difficult to meet the demands of large-scale, high-quality production: Antimony trioxide is a solid powder. During the feeding process into the esterification reactor, the existing feeding device has an unreasonable sealing structure design. High-temperature steam in the esterification reactor is prone to backflow into the feeding channel, causing the antimony trioxide powder to become damp and clump together, blocking the feeding pipe. This not only affects the continuity of feeding but also causes raw material waste and may even lead to equipment failure and affect the production schedule.
[0004] Sudden power outages are unavoidable in industrial production. Existing synthesis systems lack effective power outage protection mechanisms. After a power outage, the high-temperature viscous material in the connecting conduit will rapidly cool and solidify due to the sudden drop in temperature, clogging the conduit. Furthermore, the residual material in the conduit cannot be recovered in time, resulting in material waste and requiring a significant amount of time to clean the conduit, making production recovery difficult and increasing economic losses.
[0005] Therefore, we propose a continuous synthesis system and process for antimony glycolate to solve the problems mentioned above. Summary of the Invention
[0006] In view of this, in order to solve the above problems, the present invention provides a continuous synthesis system and process for antimony glycolate.
[0007] To achieve the above objectives, the present invention provides the following technical solution: a continuous synthesis system for antimony glycolide, comprising: The esterification reactor, material transfer pump, precision filter, crystallization reactor, centrifuge, vacuum dryer and material collection tank are connected in sequence through connecting pipes; A sampling device is fixed to the outer wall of the esterification reactor. The sampling device includes a sealing sleeve and a sampling base slidably disposed therein. Both the top of the sealing sleeve and the sampling base are provided with a through hole I. When the sampling base is inserted into the esterification reactor, its outer end closes the through hole I on the sealing sleeve, and its own through hole I is exposed to form a storage cavity. When it is pulled out, the material in the storage cavity is taken out. An explosion-proof valve assembly is provided at the feed end of the precision filter. The explosion-proof valve assembly includes a valve body, a valve seat body, and an electromagnet ring provided at the bottom of the valve body. The bottom of the valve body is provided with a through hole II that is adapted to the valve seat body. In addition, a sealed feeding device is horizontally arranged at the top of the esterification reactor and connected to its feed pipe. The sealed feeding device includes a conveyor cylinder, a drive shaft rotatably arranged inside the conveyor cylinder, a spiral conveyor blade fixedly wound around the drive shaft, and a drive motor fixed to the outer end of the conveyor cylinder. The conveyor cylinder is connected to a first extension conduit for receiving ethylene glycol raw materials and a feed hopper for receiving antimony trioxide powder.
[0008] As a further improvement to the above technical solution: The connecting conduit includes an inner conduit and an outer conduit, with an interlayer formed between the inner and outer conduits. The interlayer contains a liquid phase change molten salt medium, which is configured to absorb heat from the material during normal production, solidify and release heat to replenish the material during power outages, and drive the inner conduit to deform during thermal expansion and contraction to clean residual material from its inner wall.
[0009] The outer wall of the esterification reactor body is fixedly fitted with a jacketed insulation layer, and a sandwich is formed between the jacketed insulation layer and the reactor body body. The outer wall of the jacketed insulation layer is fixedly fitted with a water inlet pipe, a water outlet pipe, and a plurality of resistance heaters extending into the sandwich. The bottom of the reactor body body is connected to a discharge pipe.
[0010] The outer end of the sealing sleeve is rotatably provided with a locking nut ring, and the locking nut ring is internally threaded with a transmission screw. One end of the transmission screw is fixedly connected to the sampling base. A manual rotating wheel is fixed to the outer wall of the locking nut ring. By rotating the manual rotating wheel, the sampling base can be driven to slide inside the sealing sleeve.
[0011] The conveyor cylinder is divided into a feeding zone, a liquid injection zone, and a heating zone in sequence. The heating zone is close to the feeding pipe of the esterification reactor, and the feeding zone is close to the drive motor. The drive shaft is tapered, with its large end close to the feed pipe of the esterification reactor; The groove depth of the spiral conveyor blades becomes shallower in the direction from the feed zone to the heating zone, so that the material is squeezed in the heating zone to form a dynamic material sealing plug for sealing the feed pipe.
[0012] The explosion-proof valve assembly also includes multiple guide columns and a valve base. The guide columns are threaded through the bottom end of the electromagnet ring. The valve base is slidably sleeved on the outer wall of the multiple guide columns. A gravity counterweight is fixedly provided on the top of the valve base. Multiple discharge through holes are opened on the top of the gravity counterweight. The valve seat body is fixed to the top of the gravity counterweight.
[0013] The top of the valve seat body is provided with an arc-shaped sealing surface that smoothly transitions with the inner wall of the valve body. The gravity counterweight, the electromagnet ring, the valve seat body, and the through hole II are all provided with sealing structures.
[0014] It also includes a material recovery tank located below the explosion-proof valve assembly, the material recovery tank being used to collect residual material discharged from the through hole II when the power is cut off.
[0015] The melting point of the liquid phase change molten salt medium is set to be higher than the crystallization temperature of antimony glycolate to ensure that the heat released when it solidifies upon power failure is sufficient to maintain the temperature of the material inside the connecting conduit.
[0016] A continuous synthesis process for antimony glycolate, based on the aforementioned continuous synthesis system, includes the following steps: S1. Antimony trioxide powder and ethylene glycol raw material are received through the feed hopper and the first extension pipe of the sealed feeding device, respectively. In the conveyor cylinder, the material passes through the drying and mixing in the feeding zone, the micro-wetting in the liquid injection zone to form a paste, and the heating semi-melting and physical extrusion in the heating zone. After forming a dynamic material sealing plug, it is continuously and sealedly fed into the esterification reactor. S2. In the esterification reactor, antimony trioxide and ethylene glycol undergo an esterification and dehydration reaction to generate a slurry containing antimony glycol. During the reaction, the sampling device is used to take samples in real time for detection. S3. The slurry is transported to the precision filter by the material conveying pump to remove impurities. When the power is off, the electromagnet ring of the explosion-proof valve assembly loses its magnetism, and the valve seat body is disengaged from the through hole II under the action of gravity, and the residual material in the connecting conduit is discharged. S4. The filtered filtrate enters the crystallization reactor for cooling and crystallization to obtain a mixture of crystals and mother liquor; S5. The mixture is fed into the centrifugal separator, and the solid-liquid separation of the crystals and the mother liquor is achieved by centrifugal force; S6. The separated crystals are fed into the vacuum dryer for low-temperature vacuum drying to obtain antimony glycolate product; S7. Collect the dried finished product in the material collection tank.
[0017] The beneficial effects of this invention are as follows: 1. The continuous synthesis system for antimony glycol disclosed in this invention uses a sealed feeding device that, through the cooperation of a conical drive shaft and a variable-depth spiral conveyor blade, forms a highly dense dynamic material sealing plug during material conveying. This sealing plug can not only be propelled into the reactor synchronously with the material to participate in the reaction, but also fit tightly against the inner wall of the conveyor cylinder, effectively sealing the feed pipe of the reactor, completely preventing the backflow of high-temperature steam, avoiding the antimony trioxide powder from becoming damp and clumping, and ensuring smooth feeding. At the same time, through the segmented design of raw material pretreatment, it further prevents powder from flying and clumping, and improves the utilization rate of raw materials. 2. The continuous synthesis system for antimony glycol disclosed in this invention forms a dual power failure protection through the synergistic effect of the explosion-proof valve assembly and the phase change insulation structure: when the power is off, the electromagnet ring loses its magnetism, the gravity counterweight drives the valve seat body to open quickly, and the residual material is quickly discharged into the material recovery tank through the discharge hole. 3. The continuous synthesis system for antimony glycol disclosed in this invention uses the solidification and heat release of the liquid phase change molten salt medium in the jacket of the connecting pipe to keep the material inside the pipe warm and prevent the material from cooling and solidifying. In addition, the deformation caused by its thermal expansion and contraction can clean the residue on the inner wall of the pipe, further avoiding pipe blockage. 4. The continuous synthesis system for antimony glycol disclosed in this invention achieves leak-free sampling through the sliding fit between the sampling base and the sealing sleeve and the misaligned sealing of the through hole. The sampling is accurate and convenient, allowing operators to monitor the reaction status in real time, adjust the reaction parameters in a timely manner, effectively improve the purity and quality stability of the product, and reduce the yield of defective products.
[0018] Other advantages, objectives, and features of the invention will be set forth in part in the description which follows, and in part will be apparent to those skilled in the art from the following examination, or may be learned from practice of the invention. The objectives and other advantages of the invention can be realized and obtained through the following description. Attached Figure Description
[0019] To make the objectives, technical solutions, and advantages of the present invention clearer, the preferred embodiments of the present invention will be described in detail below with reference to the accompanying drawings, wherein: Figure 1 This is a schematic diagram of a continuous synthesis system for antimony glycol according to the present invention; Figure 2 This is a three-dimensional structural schematic diagram of the esterification reactor of a continuous synthesis system for antimony glycol according to the present invention. Figure 3 This is a partial cross-sectional view of the esterification reactor of a continuous synthesis system for antimony glycol according to the present invention. Figure 4 for Figure 3 Enlarged structural diagram of section A in the middle; Figure 5 This is a cross-sectional schematic diagram of the sealed feeding device of the continuous synthesis system of antimony glycol according to the present invention. Figure 6 This is a schematic cross-sectional view of the connecting conduit of a continuous synthesis system for antimony glycol according to the present invention. Figure 7 This is a cross-sectional schematic diagram of the explosion-proof valve assembly of a continuous synthesis system for antimony glycol according to the present invention.
[0020] Reference numerals: 1. Esterification reactor; 2. Material conveying pump; 3. Precision filter; 4. Crystallization reactor; 5. Centrifuge; 6. Vacuum dryer; 7. Material collection tank; 8. Antimony trioxide conveying pipeline; 9. Ethylene glycol raw material conveying pipeline; 11. Sampling device; 111. Sealing sleeve; 112. Sampling base; 113. Through hole I; 114. Locking nut ring; 115. Drive screw; 116. Manual rotary wheel; 12. Explosion-proof valve assembly; 121. Valve body; 122. Electromagnetic ring; 123. Valve base; 124. Guide column; 125. Gravity counterweight; 126. Discharge through hole; 27. Valve seat body; 128. Arc-shaped sealing surface; 129. Through hole II; 13. Material recovery tank; 14. Sealing feeding device; 141. Conveyor cylinder; 142. Drive shaft; 143. Drive motor; 144. Screw conveyor blade; 145. First extension conduit; 146. Feed hopper; 15. Connecting conduit; 151. Inner conduit; 152. Outer conduit; 153. Liquid phase change molten salt medium; 16. Flange connection plate; 101. Resistance heater; 102. Jacketed insulation layer; 103. Reactor body; 104. Water inlet conduit; 105. Drainage conduit; 106. Discharge conduit. Detailed Implementation
[0021] The following specific examples illustrate the implementation of the present invention. Those skilled in the art can easily understand other advantages and effects of the present invention from the content disclosed in this specification. The present invention can also be implemented or applied through other different specific embodiments, and various details in this specification can be modified or changed based on different viewpoints and applications without departing from the spirit of the present invention. It should be noted that the illustrations provided in the following embodiments are only schematic representations of the basic concept of the present invention. Unless otherwise specified, the following embodiments and features can be combined with each other.
[0022] The accompanying drawings are for illustrative purposes only and are schematic diagrams, not actual pictures. They should not be construed as limiting the invention. To better illustrate the embodiments of the invention, some parts in the drawings may be omitted, enlarged, or reduced, and do not represent the actual product dimensions. It is understandable to those skilled in the art that some well-known structures and their descriptions may be omitted in the drawings.
[0023] In the accompanying drawings of the embodiments of the present invention, the same or similar reference numerals correspond to the same or similar components. In the description of the present invention, it should be understood that if terms such as "upper," "lower," "left," "right," "front," and "rear" indicate the orientation or positional relationship based on the orientation or positional relationship shown in the drawings, they are only for the convenience of describing the present invention and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, or be constructed and operated in a specific orientation. Therefore, the terms used to describe positional relationships in the drawings are only for illustrative purposes and should not be construed as limiting the present invention. For those skilled in the art, the specific meaning of the above terms can be understood according to the specific circumstances.
[0024] Example 1 like Figures 1-7 As shown, a continuous synthesis system for antimony glycol is provided, which can realize the continuous synthesis of antimony glycol and solve problems such as material leakage, steam backflow, and residual material blockage during the synthesis process, ensuring the continuity and stability of production. It can be directly applied to large-scale industrial production.
[0025] The system includes an esterification reactor 1, a material conveying pump 2, a precision filter 3, a crystallization reactor 4, a centrifuge 5, a vacuum dryer 6, a material collection tank 7, an antimony trioxide conveying pipeline 8, an ethylene glycol raw material conveying pipeline 9, a sampling device 11, an explosion-proof valve assembly 12, a material recovery tank 13, a sealed feeding device 14, a connecting conduit 15, a flange connecting plate 16, a resistance heater 101, a jacketed insulation layer 102, a reactor body 103, a water inlet conduit 104, a drainage conduit 105, a discharge conduit 106, a sealing sleeve 111, a sampling base 112, a through hole I 113, a locking nut ring 114, and a transmission screw 1. 15. Manual rotary wheel 116, valve body 121, electromagnet ring 122, valve base 123, guide column 124, gravity counterweight 125, discharge through hole 126, valve seat body 127, arc-shaped sealing surface 128, through hole II 129, conveyor cylinder 141, transmission drive shaft 142, drive motor 143, screw conveyor blade 144, first extension guide tube 145, feed hopper 146, inner layer guide tube 151, outer layer guide tube 152, liquid phase change molten salt medium 153. All components cooperate and work together to form a complete continuous synthesis system, ensuring smooth connection of each process and realizing continuous production of antimony glycol.
[0026] The esterification reactor 1, material conveying pump 2, precision filter 3, crystallization reactor 4, centrifuge 5, vacuum dryer 6, and material collection tank 7 are arranged sequentially according to the production process, forming a complete continuous production line. Adjacent equipment is connected via connecting conduits 15, ensuring smooth material transfer from one process to the next without manual handling, thus improving production efficiency. Both ends of the connecting conduits 15 are fixedly connected to the interfaces of the corresponding equipment. Flange connecting plates 16 are installed at each connection point. The flange connecting plates 16 and the equipment interfaces, as well as the ends of the connecting conduits 15, are designed for close contact. Bolts on the flange connecting plates 16 firmly secure the connecting conduits 15 to the equipment. The bolts are evenly distributed along the edges of the flange connecting plates 16, ensuring uniform force distribution at the connection points, thereby guaranteeing a tight seal, preventing leakage of high-temperature viscous materials, avoiding material waste and environmental pollution. Furthermore, the detachable design of the flange connecting plates 16 facilitates disassembly, maintenance, and repair of the equipment, reducing maintenance costs. The flange connection plate 16 is made of stainless steel, which can adapt to the high temperature and corrosive environment in the synthesis process of antimony glycol. It is not easily corroded by materials and has a long service life. Its structural design can adapt to the pressure environment during normal production of the system, ensuring that there will be no deformation or leakage during the production process.
[0027] The sampling device 11 is fixed to the outer wall of the esterification reactor 1 and is used to sample and monitor the reaction of materials inside the reactor 1 in real time. This allows for timely monitoring of the reaction progress and material status, facilitating operators to adjust reaction parameters promptly, ensuring product quality, and preventing a decrease in product purity due to incomplete or excessive reaction. The sampling device 11 consists of a sealing sleeve 111 and a sampling base 112. The sealing sleeve 111 is made of seamless stainless steel tubing. The seamless structure prevents material leakage from pipe gaps. One end of the sleeve penetrates the outer wall of the jacketed insulation layer 102 and the reactor body 103, communicating with the interior of the esterification reactor 1 to ensure smooth sampling of materials inside the reactor. The other end extends to the outside of the esterification reactor 1 for easy sampling by operators. The penetration points of the sealing sleeve 111 with the jacketed insulation layer 102 and the reactor body 103 are sealed by welding. The weld is smooth and seamless, further preventing material leakage from gaps and preventing outside air from entering the esterification reactor 1 and affecting the reaction process. The sampling base 112 is slidably disposed inside the sealing sleeve 111. The outer wall of the sampling base 112 is tightly fitted with the inner wall of the sealing sleeve 111, which can achieve smooth sliding and ensure sealing during the sliding process. Both the top of the sampling base 112 and the sealing sleeve 111 are provided with through holes I113. The two through holes I113 are the same size and can be aligned or misaligned during the sliding of the sampling base 112. By aligning or misaligning the through holes I113, the switching between sampling and sealing can be realized, ensuring that the material does not leak in large quantities during the sampling process.
[0028] A locking nut ring 114 is rotatably mounted on the outer end of the sealing sleeve 111 via a bearing. The locking nut ring 114 has an internal thread, and the outer wall of the transmission screw 115 has an external thread that matches the internal thread. The transmission screw 115 is threaded into the locking nut ring 114, ensuring a tight fit and effective force transmission. One end of the transmission screw 115 is fixedly connected to the outer end of the sampling base 112 by welding to ensure a secure connection and prevent it from falling off during sliding. The other end extends to the outside of the locking nut ring 114. A manual rotating wheel 116 is fixedly mounted on the outer wall of the locking nut ring 114. The manual rotating wheel 116 and the locking nut ring 114 are integrally molded to ensure a secure connection. The surface of the manual rotating wheel 116 has anti-slip textures to increase friction when the operator grips it, facilitating easy rotation and preventing slippage during rotation. When the operator rotates the manual rotary wheel 116, it drives the locking nut ring 114 to rotate synchronously. Through the threaded engagement, the transmission screw 115 moves axially along the sealing sleeve 111, thereby causing the sampling base 112 to slide within the sealing sleeve 111, allowing the sampling base 112 to move in and out. When sampling is required, rotating the manual rotary wheel 116 pushes the sampling base 112 deeper into the esterification reactor 1. At this time, the outer end of the sampling base 112 seals the through hole I 113 on the sealing sleeve 111, preventing material and vapor in the esterification reactor 1 from leaking through the through hole I 113. Simultaneously, the through hole I 113 in the sampling base 112 is exposed, forming a storage cavity between it and the sealing sleeve 111. The material in the esterification reactor 1 enters the storage cavity under the reaction pressure, completing the sampling. After sampling, rotating the manual rotary wheel 116 in the opposite direction pulls the sampling base 112 out of the esterification reactor 1. The material in the storage chamber can be taken out for testing by pulling it out of the esterification reactor 1. The entire sampling process is convenient and will not cause a large amount of material leakage during sampling, ensuring the cleanliness and safety of the production environment. At the same time, the sampling is accurate and can truly reflect the reaction state of the material in the esterification reactor 1. In order to prevent the sampling base 112 from rotating circumferentially under the drive of the transmission screw 115, the inner wall of the sealing sleeve 111 is integrally formed with a guide protrusion along its axial direction, and the outer wall of the sampling base 112 is provided with a guide groove that slides in cooperation with the guide protrusion, thereby ensuring that the sampling base 112 can only slide linearly along the axial direction.
[0029] The explosion-proof valve assembly 12 is installed at the feed end of the precision filter 3 and is connected to the connecting conduit 15. Its core function is to quickly discharge residual material in the connecting conduit 15 in the event of a sudden power outage, preventing the residual material from cooling and solidifying due to a sudden drop in temperature, thus blocking the pipe and avoiding affecting the recovery of subsequent production, while also reducing material waste. The explosion-proof valve assembly 12 includes a valve body 121, a valve seat body 127, and an electromagnet ring 122. The valve body 121 serves as the main frame of the explosion-proof valve assembly 12, used to accommodate and install other components. It has a material channel inside, connected to the connecting conduit 15, to ensure that materials can pass through normally. The electromagnet ring 122 is fixedly installed at the bottom of the valve body 121 and is linked to the circuit of the production line, enabling synchronous response to power on and power off. In the energized state, the electromagnet ring 122 generates magnetic force, which can attract and fix the valve seat body 127. In the de-energized state, the electromagnet ring 122 loses magnetic force, releasing the attraction to the valve seat body 127, allowing the valve seat body 127 to move freely. A through hole II 129 is provided at the bottom of the valve body 121. The size of the through hole II 129 is adapted to the valve seat body 127. The valve seat body 127 can be embedded in the through hole II 129 to achieve a seal on the through hole II 129, thereby closing the explosion-proof valve assembly 12. Under normal conditions, the production line is powered normally. The electromagnet ring 122 is energized and generates magnetic force, which attracts and fixes the valve seat body 127 in the through hole II 129, ensuring that the explosion-proof valve assembly 12 is in the closed state and does not affect the normal material conveying. When a sudden power failure occurs, the production line circuit is interrupted, the electromagnet ring 122 instantly loses its magnetism, and the attraction force on the valve seat body 127 disappears. Under the action of its own weight and material pressure, the valve seat body 127 detaches from the through hole II 129, the through hole II 129 is opened, and the residual material in the connecting conduit 15 is discharged through the through hole II 129 under its own weight, preventing the residual material from cooling and solidifying and blocking the pipeline, thus providing a guarantee for subsequent production resumption.
[0030] Multiple guide posts 124 are threaded through the bottom end of the electromagnet ring 122. The multiple guide posts 124 are evenly distributed to ensure that the valve base 123 is subjected to uniform force when sliding. The valve base 123 is slidably sleeved on the outer wall of the guide posts 124. The valve base 123 can slide up and down along the axial direction of the guide posts 124. The guide posts 124 play a guiding and limiting role to prevent the valve base 123 from deviating or tilting when sliding, ensuring that the valve seat body 127 can be accurately inserted into or disengaged from the through hole II 129, ensuring the normal operation of the explosion-proof valve assembly 12. The valve base 123 is used in conjunction with the electromagnet ring 122. A gravity counterweight 125 is fixedly installed on the top of the valve base 123. The gravity counterweight 125 is made of high-density cast iron, and its weight can be adjusted according to the pressure and viscosity of the material in the connecting conduit 15 to ensure that sufficient gravity is generated when the power is off, so as to drive the valve seat body 127 to quickly disengage from the through hole II 129, avoiding the valve seat body 127 from failing to disengage in time due to insufficient gravity, which would cause residual material blockage. Multiple discharge through holes 126 are opened on the top of both the gravity counterweight 125 and the valve base 123. The discharge through holes 126 are evenly distributed on the gravity counterweight 125. When the valve seat body 127 disengages from the through hole II 129, the residual material in the connecting conduit 15 can be quickly discharged through the discharge through holes 126, increasing the discharge area, improving the residual material discharge efficiency, and reducing the retention of residual material in the explosion-proof valve assembly 12. The valve seat body 127 is fixedly installed on the top of the gravity counterweight 125. An arc-shaped sealing surface 128 is provided on the top of the valve seat body 127. The arc-shaped sealing surface 128 smoothly transitions with the inner wall of the valve body 121. When the valve seat body 127 is embedded in the through hole II 129, the arc-shaped sealing surface 128 can tightly fit against the inner wall of the valve body 121, increasing the sealing area and enhancing the sealing effect. This prevents material leakage from the through hole II 129 under normal conditions, ensuring normal material transport. Sealing structures are provided between the gravity counterweight 125 and the electromagnet ring 122, and between the valve seat body 127 and the through hole II 129. These sealing structures use fluororubber gaskets, which have excellent high-temperature resistance and corrosion resistance, making them suitable for the high-temperature and corrosive environment during the assembly process. This further enhances the sealing performance of the explosion-proof valve assembly 12 and prevents material leakage. The material recovery tank 13 is located below the explosion-proof valve assembly 12 and corresponds to the discharge end of the explosion-proof valve assembly 12. It is used to collect the residual material discharged when the power is off. The recovered residual material can be put back into production after simple processing, which improves the material utilization rate, reduces production costs, and avoids waste of residual material and environmental pollution. In order to further ensure that the valve seat body 127 can be reliably detached when the power is off, the guide column 124 is also fitted with a tension spring. One end of the tension spring is fixedly connected to the bottom of the valve base 123, and the other end is fixed to the bottom of the guide column 124.Under normal energized conditions, the magnetic force of the electromagnet ring 122 overcomes the tension of the spring and attracts and fixes the valve seat body 127. When the power is off, the magnetic force disappears, and the tension of the spring and the gravity of the counterweight 125 work together to drive the valve seat body 127 to quickly detach from the through hole II 129.
[0031] The sealed feeding device 14 is horizontally installed on top of the esterification reactor 1. Its discharge end is fixedly connected to the inlet pipe at the top of the esterification reactor 1. It is used to continuously and stably transport antimony trioxide powder and ethylene glycol raw materials into the esterification reactor 1, ensuring uninterrupted raw material supply. At the same time, it seals the inlet pipe of the esterification reactor 1 to prevent high-temperature steam in the reaction chamber from backflowing into the feeding device, avoids antimony trioxide powder from becoming damp and clumping, ensures smooth feeding, and ensures stable continuous production. The sealed feeding device 14 consists of a conveyor cylinder 141, a drive shaft 142, a drive motor 143, a screw conveyor blade 144, a first extension guide 145, and a feed hopper 146. The conveyor cylinder 141 is made of stainless steel, is horizontally set, and has a hollow internal structure to accommodate materials and provide a channel for material transportation. The stainless steel material can prevent material corrosion and extend the service life of the equipment. The drive motor 143, serving as the power source, is fixedly installed at the outer end of the conveyor cylinder 141. The output shaft of the drive motor 143 is fixedly connected to one end of the transmission drive shaft 142. The rotation of the drive motor 143 drives the transmission drive shaft 142 to rotate synchronously, thus providing power for material conveying. The transmission drive shaft 142 is conical and rotatably positioned inside the conveyor cylinder 141. Its large end is close to the feed pipe of the esterification reactor 1, and its small end is close to the drive motor 143. The conical structure, in conjunction with the spiral conveyor blades 144, enables the gradual compression of the material, providing conditions for the formation of a dynamic material sealing plug. The spiral conveyor blades 144 are fixedly wound around the transmission drive shaft 142 and rotate synchronously with it. The groove depth of the spiral conveyor blades 144 decreases sharply along the material's forward direction. From the feed zone to the heating zone, the groove depth of the spiral conveyor blades 144 gradually decreases, ensuring that the material is subjected to gradually increasing compressive force during conveying, thereby forming a dense dynamic material sealing plug.
[0032] The conveyor cylinder 141 is divided into a feeding zone, a liquid injection zone, and a heating zone, which are connected in sequence to ensure that the material can be successfully pretreated and the sealing plug formed. The heating zone is close to the feeding pipe of the esterification reactor 1, which facilitates the direct entry of the formed dynamic material sealing plug into the esterification reactor 1, and at the same time can quickly receive the heat in the reactor to assist in the semi-melting of the material. The feeding zone is close to the drive motor 143, which facilitates the rapid pushing of the raw material after it enters, reducing the retention of the raw material in the feeding zone. The liquid injection zone is located in the middle of the conveyor cylinder 141, between the feeding zone and the heating zone, which facilitates the micro-wetting of the dry material, preparing it for subsequent semi-melting and extrusion sealing. Both the first extension conduit 145 and the feed hopper 146 are connected to the feeding area of the conveyor cylinder 141, and are responsible for conveying ethylene glycol raw materials and antimony trioxide powder, respectively. The other end of the first extension conduit 145 is connected to the ethylene glycol raw material conveying pipeline 9 in the workshop, and is used to stably convey ethylene glycol raw materials into the conveyor cylinder 141 to ensure that the supply of ethylene glycol raw materials can match the production demand. The upper end of the feed hopper 146 has an open structure and is connected to the antimony trioxide conveying pipeline 8 in the workshop, and is used to convey antimony trioxide powder into the conveyor cylinder 141. The open design of the feed hopper 146 facilitates the replenishment of raw materials and at the same time prevents powder from flying and ensures a clean production environment.
[0033] During operation, the drive motor 143 starts, driving the transmission drive shaft 142 and the screw conveyor blade 144 to rotate. Antimony trioxide powder enters the feeding area of the conveyor cylinder 141 through the feed hopper 146, while ethylene glycol raw material enters the feeding area through the first extension conduit 145. The two are initially mixed in the feeding area by the rotation of the screw conveyor blade 144. At this time, the material remains dry, facilitating rapid feeding and preventing premature agglomeration of the powder. As the screw conveyor blade 144 continues to rotate, the material is slowly pushed to the liquid injection area. The liquid injection area can inject a small amount of ethylene glycol according to the dryness of the material, wetting the material into a paste. The paste material has a certain viscosity but is not too viscous, facilitating subsequent heating and extrusion, while also preventing powder from flying and reducing material loss. The material continues to be pushed into the heating zone, where it is heated by an external heating device until the paste reaches a semi-molten state. The semi-molten material has increased viscosity, facilitating the formation of a dense structure through extrusion. Simultaneously, due to the shallowing of the grooves in the screw conveyor blades 144, the material undergoes intense physical compression during transport, forming a highly dense dynamic material seal plug. This dynamic material seal plug can continue to advance with the rotation of the screw conveyor blades 144, entering the esterification reactor 1 to participate in the reaction and achieving continuous material transport. It also serves a sealing function, tightly adhering to the inner wall of the conveyor cylinder 141, preventing high-temperature steam from the esterification reactor 1 from flowing back into the conveyor cylinder 141, avoiding moisture absorption and clumping of the antimony trioxide powder, ensuring smooth feeding, and guaranteeing stable continuous production.
[0034] The esterification reactor 1, as the core equipment for the synthesis of antimony glycol, has a reactor body 103 made of stainless steel, which has excellent high-temperature resistance and corrosion resistance. It can withstand the high temperatures and material corrosion during the synthesis reaction, ensuring the stable progress of the reaction. A jacketed insulation layer 102 is fixedly fitted onto the outer wall of the reactor body 103. This jacketed insulation layer 102 is made of a material with excellent thermal insulation properties, serving to reduce heat loss within the reactor body 103, lower energy consumption, and prevent excessively high temperatures on the outer wall of the reactor body 103, thus ensuring the safety of the operators. A jacketed insulation layer 102 is formed between the vessel body 103 and the jacketed insulation layer 102. This jacket is used to contain cooling water to regulate the temperature of the vessel body 103. A water inlet pipe 104 and a water outlet pipe 105 are fixed through the outer wall of the jacketed insulation layer 102. The water inlet pipe 104 is used to introduce cooling water into the jacket, and the water outlet pipe 105 is used to discharge the cooling water from the jacket. Through the circulation of cooling water, excess heat of the vessel body 103 is carried away, thereby cooling the vessel body 103 and ensuring that the reaction temperature inside the vessel body 103 is stable within a suitable range, thus ensuring the smooth progress of the reaction. Multiple resistance heaters 101 are fixedly installed through the outer wall of the jacketed insulation layer 102. These heaters are evenly distributed on the jacketed insulation layer 102, with their heating ends extending into the jacket. The resistance heaters 101 convert electrical energy into heat energy to heat the reactor body 103 in the initial stage of the reaction, heating the material inside to the required reaction temperature. During production, the working state of the resistance heaters 101 can be adjusted in real time according to changes in material temperature to ensure stable reaction temperature and prevent temperature fluctuations from affecting reaction results and product quality. A discharge conduit 106 is connected to the bottom of the reactor body 103. The discharge conduit 106 is connected to the connecting conduit 15 and is used to transport the material after the esterification reaction to the material conveying pump 2 for subsequent refining, crystallization, and other processes. The structural design of the discharge conduit 106 ensures smooth material transport and prevents material stagnation and blockage.
[0035] Material conveying pump 2 is installed between esterification reactor 1 and precision filter 3, connected to connecting conduit 15. It serves as the power unit for material conveying, pressurizing and conveying the slurry from the esterification reactor 1 to the precision filter 3, ensuring the material can smoothly enter the subsequent refining process. Precision filter 3 filters and removes unreacted solid impurities and small amounts of impurity particles from the slurry after the esterification reaction, ensuring the smooth progress of the subsequent crystallization process and improving product purity. The filtration structure of precision filter 3 enables continuous filtration, adapting to the continuous production of the entire system. Filtered impurities can be cleaned periodically without affecting the continuity of production. Crystallization reactor 4 is connected to precision filter 3 via connecting conduit 15, receiving the filtrate from precision filter 3. The filtrate is slowly cooled within crystallization reactor 4, causing antimony glycolate crystals to precipitate from the filtrate. The structural design of crystallization reactor 4 ensures uniform cooling, preventing localized low temperatures that could lead to crystal agglomeration. It also enables continuous feeding and discharging, ensuring the continuous operation of the crystallization process.
[0036] Centrifuge 5 is connected to crystallization reactor 4 via connecting conduit 15. It receives the mixture of crystals and mother liquor from crystallization reactor 4. Through centrifugal force, solid-liquid separation is achieved between the crystals and mother liquor. The separated crystals enter the subsequent drying process, while the separated mother liquor can be recycled, reducing production costs. Centrifuge 5 enables continuous feeding and discharging, adapting to the continuous production requirements of the system. It has high separation efficiency and can effectively separate the mother liquor from the crystals, improving crystal purity. Vacuum dryer 6 is connected to centrifuge 5 via connecting conduit 15. It is used to dry the crystals separated by centrifuge 5, removing moisture from the crystals and ensuring product quality. Vacuum dryer 6 lowers the air pressure of the drying environment by drawing a vacuum, thereby lowering the boiling point of water in the crystals, achieving low-temperature drying, and preventing crystal decomposition due to high temperatures. It also has high drying efficiency and can achieve continuous drying, adapting to the continuous production of the system. The material collection tank 7 is connected to the vacuum dryer 6 via a connecting conduit 15. It is used to collect the antimony glycol product dried by the vacuum dryer 6. The material collection tank 7 adopts a sealed structure to prevent the product from getting damp and contaminated, ensuring the quality of the product, and facilitating the storage and transportation of the product.
[0037] Antimony trioxide conveying pipe 8 and ethylene glycol raw material conveying pipe 9 serve as channels for conveying raw materials. They are used to convey antimony trioxide powder and ethylene glycol raw materials to the feed hopper 146 and the first extension conduit 145 of the sealed feeding device 14, respectively, to ensure uninterrupted supply of raw materials. The pipes are made of stainless steel to prevent corrosion and leakage of raw materials. At the same time, the structural design of the pipes can ensure smooth conveying of raw materials and avoid blockage.
[0038] The system also includes a controller (not shown in the figure), which is electrically connected to the drive motor 143, the electromagnet ring 122, and the resistance heater 101. The controller controls the speed and start / stop of the drive motor 143 to regulate the feeding speed; it also supplies power to the electromagnet ring 122 during normal production to maintain its magnetic attraction and demagnetizes the electromagnet ring 122 when a mains power failure is detected. Furthermore, the controller controls the heating power of the resistance heater 101 based on feedback from a temperature sensor inside the esterification reactor 1.
[0039] Example 2 Reference Figures 1-7A continuous synthesis system for antimony glycolate is disclosed, with connecting conduit 15 serving as the core channel for material transport. It consists of an inner conduit 151 and an outer conduit 152, both made of stainless steel. Stainless steel possesses excellent high-temperature resistance, corrosion resistance, and high strength, making it suitable for transporting high-temperature, viscous, and corrosive materials during the synthesis process and extending the service life of the connecting conduit 15. The inner and outer conduits 151 and 152 are coaxially arranged, forming a sandwich between the outer wall of the inner conduit 151 and the inner wall of the outer conduit 152. This sandwich is a closed structure filled with a liquid phase change molten salt medium 153. The liquid phase change molten salt medium 153 has excellent heat storage and release properties, enabling it to play different roles during normal production and sudden power outages, ensuring smooth material transport. The melting point of the liquid phase change molten salt medium 153 is set above the crystallization temperature of antimony glycol, which ensures that in the event of a sudden power outage, the heat released by the liquid phase change molten salt medium 153 is sufficient to maintain the material temperature and prevent the material from cooling and solidifying. The liquid phase change molten salt medium 153 is a mixed molten salt of potassium nitrate and sodium nitrite (mass ratio 55:45), with a melting point set at 142℃-148℃, which is higher than the crystallization temperature of antimony glycol (120℃-130℃). Under normal conditions, the liquid phase change molten salt medium 153 absorbs heat from the material in the inner conduit 151. When power is cut off, it solidifies and releases heat to keep the material warm, maintaining the material temperature above the crystallization temperature. The volume change caused by thermal expansion and contraction drives the inner conduit 151 to deform slightly, cleaning the residual material on the inner wall. During normal production, the material in the inner conduit 151 is in a high-temperature state. The liquid phase change molten salt medium 153 can absorb the heat from the material in the inner conduit 151, playing a cooling role, preventing the material from decomposing due to excessive temperature, ensuring the quality of the material, and at the same time storing heat to prepare for heat preservation in the event of a sudden power outage. In the event of a sudden power outage, the external heating device stops working, and the temperature of the material inside the inner conduit 151 drops rapidly. At this time, the liquid phase change molten salt medium 153 begins to solidify, releasing a large amount of latent heat of phase change during the solidification process. This heat insulates the material inside the inner conduit 151, ensuring that the material does not cool and solidify during the venting process and preventing pipe blockage. Simultaneously, the liquid phase change molten salt medium 153 undergoes a certain volume change during thermal expansion and contraction. The force generated by this volume change drives a slight deformation of the inner conduit 151. During this deformation, the inner wall of the inner conduit 151 generates minute vibrations, which can clean residual material from the inner wall of the inner conduit 151, reducing material buildup and further preventing pipe blockage, thus ensuring the smooth resumption of production. The outer ends of the inner conduit 151 and the outer conduit 152 are fixedly installed with the same flange connecting plate 16. The flange connecting plate 16 enables connection with other equipment, ensuring the sealing of the connection part and preventing material leakage and heat loss. The flange connecting plate 16 has an inner ring welding surface and an outer ring welding surface. The end of the inner conduit 151 is welded to the inner ring welding surface, and the end of the outer conduit 152 is welded to the outer ring welding surface.The flange connecting plate 16 is provided with an annular sealing groove on the side facing the equipment. A fluororubber sealing ring is installed in the annular sealing groove to ensure that the material will not leak into the interlayer when the flange connecting plate 16 is pressed with the equipment interface flange, and at the same time, the liquid phase change molten salt medium 153 in the interlayer will not leak out.
[0040] The continuous synthesis process of antimony glycolate is described in detail below. This process is based on the aforementioned continuous synthesis system, and the specific steps are as follows: The first step is raw material pretreatment and conveying: Antimony trioxide powder is conveyed to the feed hopper 146 of the sealed feeding device 14 through the antimony trioxide conveying pipe 8, and ethylene glycol raw material is conveyed to the first extension conduit 145 of the sealed feeding device 14 through the ethylene glycol raw material conveying pipe 9. Both enter the feeding area of the conveyor cylinder 141 respectively, and are initially mixed under the rotation of the screw conveyor blades 144, maintaining a dry state. Subsequently, the material is pushed to the liquid injection area, where a small amount of ethylene glycol is injected to wet the material into a paste, avoiding powder residue. The material is pushed into the heating zone and heated to a semi-molten state by an external heating device. At this point, the material becomes more viscous. Under the extrusion action caused by the shrinking groove of the screw conveyor blade 144, a highly dense dynamic material sealing plug is formed. The dynamic material sealing plug rotates with the screw conveyor blade 144 and continues to enter the esterification reactor 1. At the same time, it seals the feed pipe of the esterification reactor 1, preventing the backflow of high-temperature steam in the reaction chamber and ensuring continuous and stable raw material delivery.
[0041] The second step is the esterification reaction: after antimony trioxide and ethylene glycol raw materials enter the esterification reactor 1, an esterification and dehydration reaction occurs in the reactor body 103 to produce antimony glycolate and water. This reaction needs to be carried out in a certain high-temperature environment. The reactor body 103 is heated by the resistance heater 101 on the outer wall of the jacketed insulation layer 102 to maintain the temperature inside the reactor within a suitable range. At the same time, cooling water is introduced into the jacket between the jacketed insulation layer 102 and the reactor body 103 through the water inlet pipe 104. The excess heat is removed by the cooling water circulation to ensure a stable reaction temperature and avoid temperature fluctuations affecting the reaction effect. During the reaction, sampling is performed in real time using sampling device 11. The operator rotates manual rotary wheel 116 to push sampling base 112 into esterification reactor 1. The through hole I 113 in sampling base 112 is connected to the inside of the reactor, and the material enters the storage chamber. After sampling base 112 is pulled out, the material is tested. The reaction parameters are adjusted according to the test results to ensure that the reaction proceeds fully and to generate qualified antimony glycol slurry. The water generated during the reaction is discharged through the exhaust structure of esterification reactor 1 to avoid water accumulation affecting the reaction balance.
[0042] The third step is filtration and impurity removal: After the esterification reaction is completed, the generated antimony glycol slurry enters the connecting pipe 15 through the discharge pipe 106. Under the pressure of the material conveying pump 2, it is transported to the precision filter 3. Through the filtration structure of the precision filter 3, unreacted antimony trioxide solid impurities and a small amount of impurity particles in the slurry are removed to ensure the purity of the slurry. The impurities after filtration are cleaned regularly to avoid affecting the continuity of the filtration process. The filtered antimony glycol filtrate enters the subsequent crystallization process through the connecting pipe 15. When a sudden power failure occurs, the electromagnet ring 122 loses its magnetism, and the gravity counterweight 125 drives the valve seat body 127 to detach under its own gravity. The residual material in the connecting conduit 15 is discharged through the discharge hole 126 after passing through the through hole II 129 and enters the material recovery tank 13. At the same time, the liquid phase change molten salt medium 153 in the jacket of the connecting conduit 15 begins to solidify and release heat, which keeps the material in the inner conduit 151 warm, ensuring that the residual material will not cool and solidify during the discharge process. The thermal expansion and contraction of the liquid phase change molten salt medium 153 drives the inner conduit 151 to deform, cleaning the residual material on the inner wall. After the power supply is restored, the electromagnet ring 122 is energized and adsorbs the valve seat body 127, closing the through hole II 129. The residual material in the material recovery tank 13 is then processed and put back into production, thus restoring the normal operation of the system.
[0043] Step 4, crystallization: The filtered antimony glycolate filtrate enters the crystallization reactor 4 and is slowly cooled inside the reactor. As the temperature gradually decreases, the solubility of antimony glycolate decreases, and crystals precipitate from the filtrate. During the crystallization process, uniform cooling is maintained to avoid localized low temperatures that could cause crystal agglomeration, ensuring uniform crystal morphology. The resulting mixture is a mixture of antimony glycolate crystals and mother liquor, which is continuously transported to the centrifugal separation process through connecting conduit 15.
[0044] Step 5, centrifugal separation: The mixture of crystals and mother liquor enters centrifugal separator 5. After centrifugal separator 5 is started, centrifugal force is generated. Under the action of centrifugal force, the denser antimony glycolate crystals are thrown to the inner wall of centrifugal separator 5 to form a solid layer, while the less dense mother liquor remains in the middle and is discharged through the discharge structure of centrifugal separator 5, realizing solid-liquid separation of crystals and mother liquor. The separated mother liquor is recycled to the raw material storage device, and after processing, it is put back into the esterification reaction to improve material utilization and reduce production costs. The separated antimony glycolate crystals are discharged through the discharge structure of centrifugal separator 5 and enter the subsequent drying process.
[0045] Step 6, Vacuum Drying: The centrifugally separated antimony glycolate crystals enter the vacuum dryer 6. The vacuum dryer 6 performs vacuum treatment inside to reduce the air pressure of the drying environment, thereby lowering the boiling point of the water in the crystals and achieving low-temperature drying. This avoids the crystals from decomposing due to high temperatures and ensures the quality of the finished product. During the drying process, the water in the crystals is evaporated and discharged. After drying, the finished antimony glycolate product is obtained. The finished product is transported to the material collection tank 7 through the connecting conduit 15.
[0046] Step 7, Finished Product Storage and Residual Material Recycling: After the antimony glycol finished product enters the material collection tank 7, it is sealed and stored to prevent the finished product from getting damp or contaminated, ensuring the quality of the finished product. The stored finished product can be transferred and packaged according to production needs. If a power outage occurs during production, the residual material in the connecting conduit 15 is discharged through the explosion-proof valve assembly 12 and enters the material recycling tank 13. After simple treatment, the residual material is put back into the esterification reactor 1 to participate in the reaction, further improving the material utilization rate and reducing waste.
[0047] However, as is well known to those skilled in the art, the working principles and wiring methods of the esterification reactor 1, material conveying pump 2, precision filter 3, crystallization reactor 4, centrifuge 5, vacuum dryer 6, electromagnet ring 122 and drive motor 143 are all conventional means or common knowledge, and will not be described in detail here. Those skilled in the art can make any selections according to their needs or convenience.
[0048] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention and are not intended to limit it. Although the present invention has been described in detail with reference to preferred embodiments, those skilled in the art should understand that modifications or equivalent substitutions can be made to the technical solutions of the present invention without departing from the spirit and scope of the present invention, and all such modifications or substitutions should be covered within the scope of the claims of the present invention.
Claims
1. A continuous synthesis system for antimony glycol, characterized in that, include: The esterification reactor (1), material transfer pump (2), precision filter (3), crystallization reactor (4), centrifuge (5), vacuum dryer (6) and material collection tank (7) are connected in sequence through connecting conduit (15). The sampling device (11) is fixed to the outer wall of the esterification reactor (1). The sampling device (11) includes a sealing sleeve (111) and a sampling base (112) slidably disposed therein. The top of the sealing sleeve (111) and the sampling base (112) are both provided with a through hole I (113). When the sampling base (112) is inserted into the esterification reactor (1), its outer end closes the through hole I (113) on the sealing sleeve (111), and its own through hole I (113) is exposed to form a storage cavity. When it is pulled out, the material in the storage cavity is taken out. An explosion-proof valve assembly (12) is provided at the feed end of the precision filter (3). The explosion-proof valve assembly (12) includes a valve body (121), a valve seat body (127), and an electromagnet ring (122) provided at the bottom of the valve body (121). The bottom of the valve body (121) is provided with a through hole II (129) that is compatible with the valve seat body (127). In addition, a sealed feeding device (14) is horizontally arranged on the top of the esterification reactor (1) and connected to its feed pipe. The sealed feeding device (14) includes a conveyor cylinder (141), a transmission drive shaft (142) rotatably arranged in the conveyor cylinder (141), a spiral conveyor blade (144) fixedly wound around the transmission drive shaft (142), and a drive motor (143) fixed to the outer end of the conveyor cylinder (141). The conveyor cylinder (141) is connected to a first extension conduit (145) for receiving ethylene glycol raw materials and a feed hopper (146) for receiving antimony trioxide powder.
2. The continuous synthesis system for antimony glycol according to claim 1, characterized in that, The connecting conduit (15) includes an inner conduit (151) and an outer conduit (152), with an interlayer formed between the inner conduit (151) and the outer conduit (152). A liquid phase change molten salt medium (153) is provided in the interlayer. The liquid phase change molten salt medium (153) is configured to absorb heat from the material during normal production, solidify and release heat to replenish the material during power failure, and drive the inner conduit (151) to deform during thermal expansion and contraction to clean the residual material on its inner wall.
3. The continuous synthesis system for antimony glycol according to claim 1, characterized in that, The outer wall of the esterification reactor (1) body (103) is fixedly fitted with a jacketed insulation layer (102). The jacketed insulation layer (102) and the reactor body (103) form a sandwich. The outer wall of the jacketed insulation layer (102) is fixedly fitted with a water inlet pipe (104), a drain pipe (105) and a plurality of resistance heaters (101) extending into the sandwich. The bottom of the reactor body (103) is connected to a discharge pipe (106).
4. The continuous synthesis system for antimony glycol according to claim 1, characterized in that, The outer end of the sealing sleeve (111) is rotatably provided with a locking nut ring (114), and the locking nut ring (114) is internally threaded with a transmission screw (115). One end of the transmission screw (115) is fixedly connected to the sampling base (112). The outer wall of the locking nut ring (114) is fixed with a manual rotating wheel (116). By rotating the manual rotating wheel (116), the sampling base (112) can be driven to slide inside the sealing sleeve (111).
5. The continuous synthesis system for antimony glycol according to claim 1, characterized in that, The conveyor cylinder (141) is divided into a feeding zone, a liquid injection zone and a heating zone in sequence. The heating zone is close to the feeding pipe of the esterification reactor (1) and the feeding zone is close to the drive motor (143). The drive shaft (142) is tapered, with its large end close to the feed pipe of the esterification reactor (1); The groove depth of the spiral conveyor blade (144) becomes shallower in the direction from the feed zone to the heating zone, so that the material is squeezed in the heating zone to form a dynamic material sealing plug for sealing the feed pipe.
6. The continuous synthesis system for antimony glycol according to claim 1, characterized in that, The explosion-proof valve assembly (12) also includes multiple guide columns (124) and a valve base (123). The guide columns (124) are threaded through and disposed at the bottom end of the electromagnet ring (122). The valve base (123) is slidably sleeved on the outer wall of the multiple guide columns (124). A gravity counterweight (125) is fixedly provided on the top of the valve base (123). Multiple discharge through holes (126) are opened on the top of the gravity counterweight (125). The valve seat body (127) is fixed on the top of the gravity counterweight (125).
7. The continuous synthesis system for antimony glycol according to claim 6, characterized in that, The top of the valve seat body (127) is provided with an arc-shaped sealing surface (128) that smoothly transitions with the inner wall of the valve body (121). The gravity counterweight (125) and the electromagnet ring (122), as well as the valve seat body (127) and the through hole II (129), are all provided with sealing structures.
8. The continuous synthesis system for antimony glycol according to claim 1, characterized in that, It also includes a material recovery tank (13) located below the explosion-proof valve assembly (12), the material recovery tank (13) being used to collect residual material discharged from the through hole II (129) when the power is cut off.
9. The continuous synthesis system for antimony glycol according to claim 2, characterized in that, The melting point of the liquid phase change molten salt medium (153) is set to be higher than the crystallization temperature of antimony glycol to ensure that the heat released when it solidifies upon power failure is sufficient to maintain the temperature of the material inside the connecting conduit (15).
10. A continuous synthesis process for antimony glycol, characterized in that, The continuous synthesis system according to any one of claims 1-9 is implemented by the following steps: S1. Antimony trioxide powder and ethylene glycol raw material are received through the feed hopper (146) and the first extension conduit (145) of the sealed feeding device (14). In the conveyor cylinder (141), the material passes through the drying and mixing in the feeding zone, the micro-wetting in the liquid injection zone to form a paste, and the heating semi-melting and physical extrusion in the heating zone. After forming a dynamic material sealing plug, it is continuously and sealedly fed into the esterification reactor (1). S2. In the esterification reactor (1), antimony trioxide and ethylene glycol undergo an esterification and dehydration reaction to generate a slurry containing antimony glycol. During the reaction, the slurry is sampled and detected in real time by the sampling device (11). S3. The slurry is transported to the precision filter (3) by the material conveying pump (2) for filtration to remove impurities. When the power is off, the electromagnet ring (122) of the explosion-proof valve assembly (12) loses its magnetism, and the valve seat body (127) is separated from the through hole II (129) under the action of gravity, and the residual material in the connecting conduit (15) is discharged. S4. The filtered filtrate enters the crystallization reactor (4) for cooling and crystallization to obtain a mixture of crystals and mother liquor; S5. The mixture is fed into the centrifuge (5) to achieve solid-liquid separation of crystals and mother liquor by centrifugal force; S6. The separated crystals are put into the vacuum dryer (6) for low-temperature vacuum drying to obtain antimony glycol product; S7. Collect the dried finished product in the material collection tank (7).