Search

CN-121972090-A - Solid feeding device and method for probenecid intermediate synthesis

CN121972090ACN 121972090 ACN121972090 ACN 121972090ACN-121972090-A

Abstract

The invention relates to a solid charging system for synthesizing a probenecid intermediate, which is characterized in that a movable storage bin is integrally fixed on a stainless steel frame with movable wheels, a sealing open type charging port is arranged at the top of the storage bin, a pneumatic butterfly valve is assembled at a discharging port at the bottom of the storage bin, a discharging port of the pneumatic butterfly valve is in sealing butt joint with a feeding port of an automatic weighing and discharging system through a sealing short connector, the pneumatic butterfly valve of the movable storage bin, a shovel-shaped pneumatic regulating valve of the automatic weighing and discharging system and a pneumatic switch discharging valve are in one-to-one sealing connection through independent air source pipes, the safety risk of an oxidant caused by extrusion collision in the using process is avoided, and the intermediate with high purity and high yield can be continuously and stably prepared.

Inventors

  • LI BAORONG
  • REN CHAO
  • Hong Meixian
  • ZHU HOULIANG
  • WU XIAOHUI

Assignees

  • 安徽康正康元药业有限公司

Dates

Publication Date
20260505
Application Date
20260325

Claims (8)

  1. 1. A solid feeding device for synthesizing a probenecid intermediate comprises a movable storage bin, an automatic weighing and discharging system and an explosion-proof control system, wherein all components are in sealed fit to realize gravity-flow type accurate feeding of potassium permanganate; the automatic weighing and discharging device is characterized in that the movable storage bin is of a conical structure, is integrally fixed on a stainless steel frame with movable wheels, is provided with a sealing open type charging port at the top, is provided with a pneumatic butterfly valve at the bottom discharging port, and is in sealing butt joint with a feeding port of an automatic weighing and discharging system through a sealing short connector; The automatic weighing and discharging system is of a totally-enclosed welding structure, the upper part of the automatic weighing and discharging system is a square box, the lower part of the automatic weighing and discharging system is of a conical flow guiding structure, four side box walls of the square box are respectively provided with a detachable stainless steel buckle plate, the buckle plates are connected with the square box through sealing rubber strips and quick-mounting buckles, the inside of the square box is divided into independent sub-loading bins and weighing bins from top to bottom in sequence, the bottom discharge ends of the sub-loading bins are vertically aligned with the top feed inlet of the weighing bins, the bottom center position of the conical flow guiding structure is provided with a quick-mounting discharging port, the quick-mounting discharging port is in sealing butt joint with a feeding pipeline of a reaction kettle through a quick-mounting clamp, one side box wall of the square box is provided with a dust collecting port, the dust collecting port is in sealing connection with a tail gas recovery system through a flange, and the opening position of the dust collecting port corresponds to the material flowing areas of the sub-loading bins and the weighing bins; The explosion-proof control system is in one-to-one sealing connection with a pneumatic butterfly valve of the movable stock bin, a shovel-shaped pneumatic regulating valve of the automatic weighing and discharging system and a pneumatic switch discharging valve through independent air source pipes, electromagnetic valves electrically connected with the control system are arranged on each air source pipe, the control system realizes accurate regulation and control of the opening and the opening of each pneumatic element through independent control of the on-off of each electromagnetic valve, linkage control is completed, the control system is continuously connected with a central control room (SIS) system through a 24V signal wire and supplies power, the SIS system acquires temperature detection data of the reaction kettle in real time, when the temperature of the reaction kettle is detected to exceed a preset threshold value, the SIS system immediately cuts off a 24V power supply wire, the control system immediately controls the electromagnetic valves on all air source pipes to be powered off after receiving signals, so that each pneumatic element is reset and closed, the feeding system stops all feeding actions, and simultaneously the control system triggers an explosion-proof audible and visual alarm to perform audible and visual double alarm until the SIS system detects that the temperature of the reaction kettle is recovered to the preset threshold value and the 24V power supply wire is switched on again.
  2. 2. The solid feeding device for the probenecid intermediate synthesis is characterized in that a spade pneumatic adjusting valve is fixedly arranged at the bottom discharging end of a sub-charging bin, the spade pneumatic adjusting valve is a straight-travel pneumatic adjusting valve, the valve core opening of the spade pneumatic adjusting valve can be adjusted in a three-stage mode, the discharging end of the adjusting valve is in vertical and horizontal precise correspondence with the top feeding hole of a weighing bin, a control system controls the valve core opening of the spade pneumatic adjusting valve by adjusting the on-off time and the ventilation pressure of an electromagnetic valve on a corresponding air source pipe according to preset feeding time and feeding quantity, the valve core opening is synchronously increased when the valve core opening is gradually increased from slow to fast, the material conveying speed is accurately controlled by accurately adjusting the real-time opening of the valve core, the opening is 1, the flow speed is low, the adding quantity is 3kg/min, the opening is 2, the adding quantity is 4kg/min, the opening is 3, the flow speed is high, and the adding quantity is 5kg/min.
  3. 3. The solid feeding device for probenecid intermediate synthesis is characterized in that a weighing module with the precision of +/-0.1 KG is fixedly connected to the outer side of a weighing bin, a pneumatic switch discharging valve is arranged at the bottom of the weighing bin, a linkage control logic is formed by the weighing module and a time relay arranged in a control system, the linkage control logic is that the single feeding amount is preset to 3KG and the feeding time is 60 seconds, the weighing module collects weight in real time, the time relay counts down synchronously, when the weight reaches 3KG and the count down is full of 60 seconds, the pneumatic switch discharging valve is started to feed, and when the weight is not up but the count down is over, the system triggers an audible light alarm to prompt abnormal feeding.
  4. 4. The solid feeding device for probenecid intermediate synthesis according to claim 1, wherein the control system comprises a Kunlun on-state TPC7002Qi embedded integrated touch screen and an explosion-proof electric cabinet, a contactor, a relay and an electromagnetic valve are integrated in the electric cabinet, all electric control elements are integrated in the explosion-proof electric cabinet, compressed air is used as a pneumatic element driving power source by the system, and the explosion-proof grade BT6 is achieved.
  5. 5. The solid feeding device for the probenecid intermediate synthesis is characterized in that the movable storage bin has a volume of 180L, the bearing capacity of a stainless steel frame is more than or equal to 800KG, and a pneumatic butterfly valve, a shovel-shaped pneumatic regulating valve and a pneumatic switch discharging valve are all made of stainless steel, and the sealing grade is more than or equal to IP65.
  6. 6. The solid feeding device for the synthesis of the probenecid intermediate is characterized in that the weighing module is an explosion-proof pressure sensor, the measuring range is 0-50KG, and the timing precision of the time relay is +/-0.1 seconds.
  7. 7. The solid feeding device for synthesizing the probenecid intermediate according to claim 1, wherein the tail gas recovery system is a bag-type dust remover, and the dust recovery rate is more than or equal to 99.5%.
  8. 8. A solids charging device for the synthesis of probenecid intermediate according to claim 1, characterized in that the solids charging method comprises the steps of: (1) Filling potassium permanganate into a movable storage bin, sealing and shorting a pneumatic butterfly valve discharge port and a feed inlet of an automatic weighing and discharging system, and confirming that a control system is normally connected with a 24V power supply line of an SIS system; (2) Presetting single feeding amount 3KG and feeding time of 60 seconds by a control system, and starting a feeding program; (3) Opening a pneumatic butterfly valve and a shovel-shaped pneumatic regulating valve, enabling potassium permanganate to gravity flow to a weighing bin, and collecting weight by a weighing module in real time and feeding back to a control system; (4) When the weight reaches 3KG, the shovel-shaped pneumatic adjusting valve is closed, the pneumatic switch discharging valve is opened after the time relay is synchronized for 60 seconds and counting down is finished, and the discharging valve is closed after potassium permanganate automatically flows to the reaction kettle; (5) The method comprises the steps of automatically resetting a system, repeating continuous feeding in steps (3) - (4), continuously collecting dust by a tail gas recovery system in the whole feeding process, triggering an alarm by the system if the weight of a batch is less than 3KG and the countdown is finished, immediately cutting off power supply if an SIS system monitors that a reaction kettle is over-temperature, stopping the system and alarming, and recovering the power supply to restart after the abnormality is removed.

Description

Solid feeding device and method for probenecid intermediate synthesis Technical Field The invention relates to the technical field of raw material medicine synthesis, in particular to a solid feeding system for probenecid intermediate synthesis. Background Probenecid is white crystalline powder, is an auxiliary drug for anti-gout drugs and antibiotic treatment, and sodium salt (probenecid sodium) is white crystalline powder, has no odor and slightly bitter taste, and is extremely easy to dissolve in water. The probenecid (sodium) can obviously optimize the pharmacokinetics characteristics of various beta-lactam antibiotics, and has clinical application with compound preparations consisting of antibiotics such as ampicillin, and the like, and the combined use of the probenecid (sodium) and the antibiotics can greatly reduce the dosage of the antibiotics, reduce the incidence of adverse reactions, promote the treatment compliance and reduce the selection of drug-resistant bacteria, thereby having important clinical value and positive social significance. In the synthesis process of probenecid sodium, potassium permanganate is used as an oxidant to prepare an intermediate p-carboxybenzenesulfonamide, (potassium permanganate, chemical formula KMnO 4 is a purple black crystal, has strong oxidizing property, is used for preventing extrusion and collision, and has the characteristics of extremely high feeding parameters (feeding quantity, feeding rate and feeding temperature) critical to the conversion rate, selectivity and safety of oxidation reaction, namely, too high feeding speed or too high feeding speed can lead to severe reaction, increased byproducts, reduced product purity, even peroxide generation, easy initiation of overtemperature runaway and material flushing risk, and too low feeding speed can lead to incomplete reaction, reduced yield and prolonged reaction period. Meanwhile, when potassium permanganate is mixed with organic matters and inflammables, severe oxidation-reduction reaction can occur under slight friction, impact or heating, a large amount of heat is instantaneously released to cause combustion or explosion, and strict requirements are set for the safety of charging equipment. The solid charging equipment in the existing raw material medicine synthesis field has the defects that firstly, a screw feeder, a star valve feeder, a belt transmission and other transmission structures are adopted, friction heating is easy, potassium permanganate combustion explosion is easy to cause, the charging structure is easy to block, secondly, the charging quantity and the charging rate cannot be accurately controlled, the technological requirements of probenecid sodium synthesis are difficult to meet, thirdly, the sealing performance is poor, potassium permanganate dust leakage is easy to cause, the environment is polluted, the health of operators is threatened, fourthly, the manual operation dependency is high, the efficiency is low, personal errors are easy to occur, and fifthly, special design is not performed aiming at the explosion-proof requirements of class A workshops, and the safety redundancy is insufficient. Therefore, the development of a solid feeding system which has the functions of automatic quantitative and timing continuous feeding and the explosion-proof performance of a class A workshop and can adapt to the feeding characteristics of potassium permanganate becomes a key for solving the pain point of the prior art. Disclosure of Invention The invention aims to provide a solid feeding system for synthesizing a probenecid intermediate, which can realize automatic, quantitative and timed continuous feeding of an oxidant solid raw material so as to meet the special technological requirements of oxidation reaction, avoid side reaction, ensure the reaction conversion rate, simultaneously avoid the safety risk of the oxidant caused by extrusion collision in the use process, and continuously and stably prepare the intermediate with high purity and high yield. The solid feeding system for synthesizing the probenecid intermediate comprises a movable storage bin, an automatic weighing and discharging system and an explosion-proof control system, wherein the components are matched in a sealing manner to realize gravity-flow type accurate feeding of potassium permanganate; the automatic weighing and discharging device is characterized in that the movable storage bin is of a conical structure, is integrally fixed on a stainless steel frame with movable wheels, is provided with a sealing open type charging port at the top, is provided with a pneumatic butterfly valve at the bottom discharging port, and is in sealing butt joint with a charging port of an automatic weighing and discharging system through a sealing short connector; The automatic weighing and discharging system is of a totally-enclosed welding structure, the upper part of the automatic weighing and discharging system is a square box, the