Device and method for detecting concentration of volatile gas in water suspension granulation process
By designing an integrated device of drying module and gas concentration sensor in the water suspension granulation process, the problem of accuracy in detecting volatile gas concentration in high humidity environment is solved, enabling accurate judgment of granulation endpoint and safety warning, thereby improving the safety of production process and product quality.
Patent Information
- Application Number
- CN202511610131.6
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-11-05
- Publication Date
- 2026-02-13
AI Technical Summary
The existing water suspension granulation process lacks real-time and accurate monitoring of the concentration of volatile gases in the reactor, resulting in low detection accuracy and safety risks. In particular, the sensors are prone to failure in high humidity and high dust environments.
A detection device comprising a drying module, a pumping module, and a gas concentration sensor was designed. It is connected to the reaction vessel through a sealed pipeline to achieve active extraction and dehumidification of volatile gases. Combined with the integrated control of vacuum control and stirring parameters, a closed-loop system is formed.
It enables accurate detection of volatile gas concentrations in high humidity environments, provides objective judgment of granulation endpoints and safety warnings, and improves the safety of the production process and the consistency of product quality.
Smart Images
Figure CN121522089A_ABST
Abstract
Description
TECHNICAL FIELD
[0001] The application belongs to the field of energetic material safety and manufacturing technology, and particularly relates to a volatile gas concentration detection device and method in a water suspension granulation process. BACKGROUND
[0002] The water suspension granulation method is a commonly used method for preparing high polymer bonded explosive (PBX) molding powder. The basic principle is to suspend explosive crystals in water. Under the action of stirring, volatile organic solvents (such as ethyl acetate, acetone, petroleum ether, etc.) in which the binder (such as fluorine rubber, cis-butyl rubber, etc.) is dissolved are added dropwise, so that the binder is uniformly coated on the surface of the crystals. Subsequently, the solvent is removed by heating, vacuuming, etc., thereby forming spherical molding powder particles.
[0003] In the process, the concentration of volatile organic solvents in the reactor is a key parameter affecting the granulation effect and production safety. On the one hand, the solvent concentration directly affects the precipitation rate and coating effect of the binder, and is an important basis for determining the end point of granulation. On the other hand, when the solvent concentration accumulates to the lower explosive limit, there is a serious risk of ignition and even explosion when encountering an ignition source, which poses a great threat to safety production.
[0004] However, the current water suspension granulation process generally lacks real-time and effective monitoring of the concentration of volatile gases in the reactor. The existing technology relies on the experience of operators, and indirectly judges by observing the shape of the material or according to fixed process time. This method is highly subjective and has low accuracy, and cannot provide early warning for safety risks. Although there are gas concentration sensors on the market, the high humidity and high dust environment in the granulation reactor can seriously interfere with the detection accuracy of the sensor, and even cause the sensor to fail. In addition, the vacuum degree, temperature, and binder drop rate in the process are coupled with many parameters, which further increases the difficulty of real-time and accurate detection.
[0005] Therefore, there is an urgent need in the art for a special device and method that can resist high humidity interference and achieve online and accurate detection of volatile gas concentration in the water suspension granulation process, in order to improve product quality consistency and ensure the intrinsic safety of the production process. SUMMARY
[0006] Therefore, the application provides a volatile gas concentration detection device and method in a water suspension granulation process. The device and method can effectively overcome the interference of high humidity environment, realize accurate and online detection of volatile gas concentration in the granulation process, and thus provide technical support for accurate control of the granulation process and safety production.
[0007] To achieve the above purpose, the application adopts the following technical solutions:
[0008] The application discloses a volatile gas concentration detection device for a water suspension granulation process.
[0009] Further, the water suspension granulation reaction kettle is made of glass and comprises an upper cover and a kettle body which are connected through a sealing flange; the water suspension granulation reaction kettle is provided with an explosion-proof motor, a stirring paddle and a granulation temperature control unit, wherein the granulation temperature control unit comprises a water suspension granulation reaction kettle water bath jacket and a circulating water bath pot, and water suspension granulation under specific temperature and specific rotating speed conditions can be realized.
[0010] Further, the volatile gas concentration detection unit comprises a drying module, a pump suction module and a gas concentration sensor; the drying module is used for dehumidifying the sampled gas to eliminate the interference of high humidity environment on the detection result; the pump suction module is used for actively and continuously extracting the gas in the reaction kettle to the detection unit; the gas concentration sensor can detect ethyl acetate, butyl acetate, acetone, petroleum ether and other commonly used solvents of PBX explosive water suspension granulation; and the volatile gas concentration detection unit is connected with the water suspension granulation reaction kettle through a sealing pipeline.
[0011] Further, the binder system dropping unit comprises a peristaltic pump and a binder system solution tank, and can realize dropping of the binder solution into the water suspension granulation reaction kettle at a certain rate; and the binder system dropping unit is connected with the water suspension granulation reaction kettle through a pipeline.
[0012] Further, the vacuum control unit comprises a vacuum controller and a vacuum circulating water pump, and can accurately control the vacuum degree in the water suspension granulation reaction kettle; and the vacuum control unit is connected with the water suspension granulation reaction kettle through a sealing pipeline.
[0013] Based on the same inventive concept, the application further provides a detection method using the above device; during detection, the granulation material is placed in the water suspension granulation reaction kettle, the explosion-proof motor, the stirring paddle and the circulating water bath pot are started, and the stirring speed and the water bath temperature are set.
[0014] Further, the vacuum control unit, the binder system dropping unit are adjusted or started in sequence, and the vacuum degree and the binder dropping rate are adjusted.
[0015] Further, the volatile gas concentration detection unit is started, the gas in the water suspension granulation reaction kettle is actively extracted, and the volatile gas concentration in the water suspension granulation reaction kettle is detected.
[0016] The application has the following beneficial effects:
[0017] 1. By arranging the special drying module, the sampled gas is pretreated, the interference of the high humidity environment in the water suspension granulation kettle on the gas concentration sensor is effectively eliminated, and the accuracy and reliability of the detection data are ensured.
[0018] 2. By combining the pump module and the gas concentration sensor, the concentration changes of volatile solvent gas in the reactor can be monitored in real time and continuously, providing an objective basis for accurately judging the granulation endpoint. At the same time, it can issue an alarm when the concentration approaches the dangerous threshold, greatly improving the inherent safety level of the production process.
[0019] 3. The gas concentration detection is integrated with the control of process parameters such as stirring, temperature, vacuum degree, and binder dripping, forming a complete closed-loop control system, which helps to optimize the granulation process and improve the consistency and stability of PBX molding powder product quality.
[0020] 4. The device can be adapted to detect a variety of commonly used organic solvents, and complex processes can be completed through controller settings. It is easy to operate, highly automated, and reduces human error. Attached Figure Description
[0021] Figure 1 This is a schematic diagram of the overall structure of the volatile gas concentration detection device in the water suspension granulation process of the present invention.
[0022] Figure reference numerals: 1. Water suspension granulation reactor; 2. Explosion-proof motor; 3. Stirring paddle; 4. Water bath jacket; 5. Peristaltic pump; 6. Binding system solution tank; 7. Vacuum controller; 8. Vacuum circulating water pump; 9. Drying module; 10. Pump suction module; 11. Gas concentration sensor. Detailed Implementation
[0023] To make the objectives, concepts, and beneficial effects of this invention more apparent and understandable, specific embodiments of the invention will be clearly and completely described in conjunction with the accompanying drawings. Obviously, the described embodiments are merely some, not all, of the embodiments of this invention. All other embodiments obtained by those skilled in the art based on the embodiments of this invention without inventive effort are within the scope of protection of this invention.
[0024] A device for detecting the concentration of volatile gases in an aqueous suspension granulation process, characterized in that:
[0025] The testing device includes
[0026] The water suspension granulation reactor 1 includes a top cover and a reactor body. The water suspension granulation reactor 1 is equipped with an explosion-proof motor 2, a stirring paddle 3 and a granulation temperature control unit. The granulation temperature control unit includes a water bath jacket 4 and a circulating water bath of the water suspension granulation reactor 1, which can realize water suspension granulation under specific temperature and speed conditions.
[0027] Volatile gas concentration detection unit; the volatile gas concentration detection unit includes a drying module 9, a pump module 10, and a gas concentration sensor 11, which can actively draw in gas while resisting interference from high humidity environments; the volatile gas concentration detection unit is connected to the top cover of the water suspension granulation reactor 1 through a sealed pipeline;
[0028] The adhesive system dripping unit includes a peristaltic pump 5 and an adhesive system solution tank 6, which can drip adhesive solution into the water suspension granulation reactor 1 at a certain rate; the adhesive system dripping unit is connected to the water suspension granulation reactor 1 through a pipeline.
[0029] Vacuum control unit; the vacuum control unit includes a vacuum controller 7 and a vacuum circulating water pump 8, used to control the vacuum level inside the water suspension granulation reactor 1; the vacuum control unit is connected to the water suspension granulation reactor 1 through a sealed pipeline.
[0030] The present invention provides a specific embodiment in which the water suspension granulation reactor 1 is made of glass, and the top cover is connected to the reactor body through a sealing flange.
[0031] This invention provides a specific embodiment in which the gas concentration sensor 11 can detect ethyl acetate, butyl acetate, acetone, and petroleum ether, commonly used solvents in the water suspension granulation of PBX explosives.
[0032] This invention provides a specific implementation method in which the gas inside the water suspension granulation reactor 1 enters the vacuum circulating water pump 8 via the vacuum controller 7.
[0033] This invention provides a method for detecting the concentration of volatile gases in a water suspension granulation process. During detection, the granulation material is placed in a water suspension granulation reactor 1, and the explosion-proof motor 2, the stirring paddle 3, and the circulating water bath are started. The stirring rate and the water bath temperature are set.
[0034] The present invention provides a specific implementation method in which the vacuum control unit and the adhesive system dripping unit are adjusted or activated in sequence, the vacuum degree is adjusted and the adhesive dripping acceleration rate is set.
[0035] The present invention provides a specific implementation method in which a volatile gas concentration detection unit is activated to detect the volatile gas concentration in the water suspension granulation reactor 1 by actively absorbing the gas in the water suspension granulation reactor 1.
[0036] Example 1: Detection of volatile gas concentration during the granulation process of a cis-butadiene rubber / petroleum ether system.
[0037] 1. Preparation: Add HMX explosive crystals and water to the water suspension granulation reactor 1 to form a suspension. Dissolve cis-butadiene rubber in petroleum ether and place it in the binder system solution tank 6. Open the water bath jacket 4 and control the temperature inside the reactor at 50℃.
[0038] 2. Parameter Settings: Start the explosion-proof motor 2 and set the stirring paddle 3 speed to 300 rpm. Adjust and stabilize the vacuum level inside the reactor at -0.05 MPa using the vacuum controller 7 and vacuum circulating water pump 8. Set the drip rate of the peristaltic pump 5 to 2 mL / min.
[0039] 3. Detection and Process Control: The volatile gas concentration detection unit is activated, and the pump module 10 begins operation, continuously extracting gas from the reactor. After dehumidification by the drying module 9, the gas is sent to the gas concentration sensor 11 for detection. The gas concentration sensor 11 is calibrated for measuring petroleum ether gas. The binder solution is then added dropwise, and gas concentration data is recorded in real time.
[0040] 4. Endpoint Determination and Post-processing: As the solvent evaporates and is removed, when the monitored concentration of petroleum ether gas continuously decreases and stabilizes at a preset low concentration plateau value, the granulation endpoint is determined to have been reached. Stop adding the binder, and subsequent processes such as heating and high-vacuum solvent removal can then be performed.
[0041] Example 2: Detection of volatile gas concentration during the granulation process of a fluororubber / ethyl acetate system.
[0042] 1. Preparation: Add CL-20 explosive crystals and water to the water suspension granulation reactor 1 to form a suspension. Dissolve fluororubber in ethyl acetate and place it in the binder system solution tank 6. Turn on the water bath jacket 4 and control the temperature inside the reactor at 70℃.
[0043] 2. Parameter Settings: Start the explosion-proof motor 2 and set the stirring paddle 3 speed to 400 rpm. Adjust and stabilize the vacuum level inside the reactor at -0.085 MPa using the vacuum controller 7 and vacuum circulating water pump 8. Set the drip rate of the peristaltic pump 5 to 5 mL / min.
[0044] 3. Detection and Process Control: The volatile gas concentration detection unit is activated, and the pump module 10 and drying module 9 operate continuously. The gas concentration sensor 11 monitors the gas concentration inside the reactor in real time. The gas concentration sensor 11 is calibrated for the petroleum ether gas being measured. The safe upper limit for concentration is set to 25% of the lower explosive limit (LEL) of ethyl acetate.
[0045] 4. Process Control: Closely monitor gas concentration changes throughout the dropping and granulation process. If the concentration approaches the safety limit, the system can issue an audible and visual alarm and can also link with the vacuum control unit to increase the vacuum level to accelerate solvent removal, ensuring that the production process is always within a safe range.
[0046] The above description is merely a preferred embodiment of the present invention, but the scope of protection of the present invention is not limited thereto. Any equivalent substitutions or modifications made by those skilled in the art within the scope of the technology disclosed in the present invention, based on the technical solution and inventive concept of the present invention, should be covered within the scope of protection of the present invention.
Claims
1. A device for detecting the concentration of volatile gases in an aqueous suspension granulation process, characterized in that: The testing device includes A water suspension granulation reactor; comprising a top cover and a reactor body, the water suspension granulation reactor is equipped with an explosion-proof motor, a stirring paddle and a granulation temperature control unit, wherein the granulation temperature control unit includes a water bath jacket and a circulating water bath of the water suspension granulation reactor, which can realize water suspension granulation under specific temperature and speed conditions; A volatile gas concentration detection unit; the volatile gas concentration detection unit includes a drying module, a pump module, and a gas concentration sensor, and is capable of actively aspirating gas while resisting interference from high humidity environments; the volatile gas concentration detection unit is connected to the top cover of the water suspension granulation reactor through a sealed pipeline; A binder system dripping unit; the binder system dripping unit includes a peristaltic pump and a binder system solution tank, which can drip binder solution into the water suspension granulation reactor at a certain rate; the binder system dripping unit is connected to the water suspension granulation reactor through a pipeline; Vacuum control unit; the vacuum control unit includes a vacuum controller and a vacuum circulating water pump, used to control the vacuum level inside the water suspension granulation reactor; the vacuum control unit is connected to the water suspension granulation reactor through a sealed pipeline.
2. The volatile gas concentration detection device for the water suspension granulation process according to claim 1, characterized in that: The water suspension granulation reactor is made of glass, and the top cover is connected to the reactor body via a sealing flange.
3. The volatile gas concentration detection device for the water suspension granulation process according to claim 1, characterized in that: The gas concentration sensor can detect ethyl acetate, butyl acetate, acetone, and petroleum ether, which are commonly used solvents in the water suspension granulation of PBX explosives.
4. The volatile gas concentration detection device for the water suspension granulation process according to claim 1, characterized in that: The gas inside the water suspension granulation reactor is fed into the vacuum circulating water pump via a vacuum controller.
5. The method for detecting volatile gas concentration in the water suspension granulation process of the apparatus according to any one of claims 1-4, characterized in that, During testing, the granulated material is placed in a water suspension granulation reactor, and the explosion-proof motor, stirring paddle, and circulating water bath are started. The stirring rate and water bath temperature are set.
6. The method according to claim 5, characterized in that, Adjust or start the vacuum control unit and the adhesive system dripping unit in sequence, adjust the vacuum level and set the adhesive dripping acceleration rate.
7. The method according to claim 5, characterized in that, The volatile gas concentration detection unit is activated to detect the concentration of volatile gases inside the water suspension granulation reactor by actively absorbing the gas.