Synthesis reaction device and synthesis method of sulfur-free odorizing agent

Abstract

This invention relates to the field of chemical synthesis equipment technology, and discloses a synthesis reaction apparatus and method for a sulfur-free odorant. The synthesis reaction apparatus for the sulfur-free odorant includes: a reaction vessel and multiple raw material storage tanks for storing different raw materials, each of which is connected to the reaction vessel via an independent feeding pipeline; at least one of the feeding pipelines is equipped with an automatic feeding mechanism, which includes: a metering pump located on the feeding pipeline and a pretreatment module located at the inlet of the metering pump. The pretreatment module includes: a pipe section, a viscosity sensing unit, a temperature control unit, a vibration generating unit, and a control unit, with the pipe section forming part of the feeding pipeline. This invention, by integrating a pretreatment module with real-time viscosity sensing, precise temperature control, and micro-pulse vibration, and combining it with an adaptive collaborative control algorithm based on multiple thresholds, achieves a transformation from passive static heat preservation to active dynamic regulation of the flow state of high-viscosity or easily crystallizing raw materials.

Description

Technical Field

[0001] This invention relates to the field of chemical synthesis equipment technology, and more specifically, to a synthesis reaction apparatus and synthesis method for a sulfur-free odorant-containing agent. Background Technology

[0002] Sulfur-free odorants are important additives for natural gas, coal gas, and other similar products. Their synthesis typically involves fine chemical processes such as esterification and distillation. The production of these products requires extremely high precision in raw material ratios and stability of reaction conditions, as even minor deviations can directly affect the odor characteristics and efficacy of the final product.

[0003] Currently, in the synthesis reaction of sulfur-free odorants, each raw material storage tank is generally fed into the reactor through independent pipelines and metering pumps. While this dedicated pipeline and automatic feeding method achieves basic automation to a certain extent, it still has limitations when handling raw materials with specific properties. For example, when the raw material is of the high viscosity or easily crystallizing type (such as certain acrylate monomers, long-chain alcohols, etc.), the raw material is prone to decreased fluidity due to changes in ambient temperature (such as low temperatures in winter), and may even experience localized crystallization or adhesion to the walls. This leads to unstable inlet conditions for the metering pump, resulting in flow fluctuations, cavitation, and in severe cases, blockage, directly affecting the feeding accuracy and initial reaction conditions.

[0004] To address the aforementioned issues, existing technologies typically employ fixed electric or steam heat tracing for static insulation of pipelines. However, this open-loop control method still has inherent drawbacks: its fixed temperature setpoints cannot respond to subtle differences in the physical properties (such as initial viscosity and distillation range) of different batches of raw materials. For example, the actual viscosity of the same raw material (such as allyl alcohol) from different suppliers may differ at the same temperature. A fixed heat tracing scheme cannot adaptively eliminate this difference, leading to inconsistent actual flowability of the material entering the metering pump, thus causing fluctuations in the feed flow rate. These fluctuations will propagate to subsequent reaction stages, affecting the instantaneous proportions of reactants and potentially impacting product yield and purity.

[0005] Therefore, there is an urgent need for a solution that can sense and actively regulate the flow of raw materials in real time to ensure accurate and stable feeding from beginning to end. Summary of the Invention

[0006] The purpose of this invention is to provide a synthesis apparatus and method for a sulfur-free odorant to solve the aforementioned technical problems.

[0007] The present invention solves the above-mentioned technical problems through the following technical solutions:

[0008] The present invention provides a synthesis reaction apparatus for a sulfur-free odorant, comprising: a reaction vessel and multiple raw material storage tanks for storing different raw materials, each of the raw material storage tanks being connected to the reaction vessel via an independent feeding pipeline;

[0009] At least one of the feeding pipelines is provided with an automatic feeding mechanism, which includes: a metering pump provided on the feeding pipeline and a pretreatment module provided at the inlet end of the metering pump;

[0010] The preprocessing module includes:

[0011] The pipe section forms part of the feeding pipeline;

[0012] A viscosity sensing unit is used to detect the viscosity of the material flowing through the pipe section in real time;

[0013] The temperature control unit is used to regulate the temperature of the material inside the pipe section;

[0014] A vibration generating unit is attached to the outer wall of the pipe section and is used to apply mechanical vibration to the pipe section;

[0015] The control unit is connected to the viscosity sensing unit, temperature control unit, vibration generating unit, and metering pump signal, and is configured as follows:

[0016] Based on the viscosity data detected in real time by the viscosity sensing unit, a first control command is generated to coordinate the working state of the temperature control unit and the start / stop and working mode of the vibration generation unit.

[0017] Based on the pressure or viscosity data within the pipe section, a second control command is generated to dynamically adjust the operating parameters of the metering pump.

[0018] Preferably, the temperature control unit is a jacketed structure, which is wrapped around the outside of the pipe section; the jacket is filled with a heat exchange medium.

[0019] Preferably, the vibration generating unit is a piezoelectric ceramic vibrator, which is fixedly installed on the outer wall of the pipe section.

[0020] Preferably, the viscosity sensing unit is a viscosity sensor, which is disposed on the pipe section.

[0021] Preferably, the pretreatment module further includes a pressure sensor and a temperature sensor disposed on the pipe section, and the pressure sensor and temperature sensor are signal-connected to the control unit.

[0022] Preferably, the control unit is further configured to: before performing the feeding operation, activate the temperature control unit and the vibration generation unit to preheat and vibrate the material remaining in the pipe section until the detected viscosity value reaches the preset feeding start threshold.

[0023] Preferably, during steady-state feeding, the control unit is configured to control the vibration generating unit to operate in an intermittent pulse mode when the detected viscosity value is maintained within a preset optimal range.

[0024] Preferably, the control unit is further configured to: after a single feeding operation is completed, control the temperature control unit to stop heating and start cooling, and at the same time control the vibration generating unit to operate in cleaning mode to remove residual material from the inner wall of the pipe section.

[0025] A method for synthesizing a sulfur-free odorant includes the following steps:

[0026] S100, Raw Material Feeding: For at least one critical raw material with high viscosity or easy crystallization, the following feeding procedure shall be performed:

[0027] The pretreatment module corresponding to the key raw material is activated. Based on the viscosity data detected in real time by the viscosity sensor, the temperature control unit and the vibration generation unit are adjusted in coordination to ensure that the key raw material reaches and maintains a preset flow state before entering the metering pump.

[0028] Start the metering pump and dynamically adjust the pumping parameters according to the real-time data provided by the pretreatment module to deliver the key raw materials to the reactor in the set amount;

[0029] Other raw materials are transported to the reactor through their respective feed pipelines;

[0030] S200, Azeotropic Distillation Reaction: In a reaction vessel, a dehydrating agent is added, and an esterification reaction is carried out in the presence of a catalyst, while the water generated in the reaction is continuously removed through an azeotropic distillation device;

[0031] S300, Neutralization and Washing: After the reaction is completed, the materials in the reactor are neutralized, washed and the aqueous phase is removed;

[0032] S400, distillation: The obtained organic phase is subjected to vacuum distillation to collect the target fraction and obtain the sulfur-free odorant base monomer;

[0033] S500, compound: The basic monomer is mixed with other components according to the formula and stabilized to obtain the final sulfur-free odorant product.

[0034] In step S100, the intelligent delivery process for key raw materials specifically includes:

[0035] If the real-time viscosity is higher than the preset feeding threshold, the heating power of the temperature control unit is increased and the vibration generation unit is activated for enhanced processing.

[0036] If the real-time viscosity is within the preset optimal range, the current state of the temperature control unit is maintained and the vibration generation unit is controlled to work in intermittent pulse mode until delivery is completed.

[0037] The beneficial effects of this invention are as follows:

[0038] This invention integrates a preprocessing module with real-time viscosity sensing, precise temperature control, and micro-pulse vibration, combined with a multi-threshold-based adaptive collaborative control algorithm, to achieve a shift from passive static heat preservation to active dynamic regulation of the flow pattern for high-viscosity or easily crystallizing raw materials. This invention can respond in real-time to differences in raw material properties and changes in ambient temperature, ensuring that the material is always in an optimal flow state before entering the metering pump, thus solving the problems of decreased feeding accuracy, unstable flow, and pipeline blockage caused by fluctuations in flowability. It not only ensures the accuracy and stability of the molar ratio of key reaction raw materials throughout the process but also improves the yield, purity, and batch consistency of sulfur-free odorant products. Attached Figure Description

[0039] Figure 1 This is a schematic diagram of the structure of a synthesis reaction device for a sulfur-free odorant according to the present invention;

[0040] Figure 2 This is a schematic diagram of the structure between the raw material storage tank and the automatic feeding mechanism in the synthesis reaction device of a sulfur-free odorant according to the present invention.

[0041] Figure 3 This is a schematic diagram of the automatic feeding mechanism in the synthesis reaction device of a sulfur-free odorant according to the present invention;

[0042] Figure 4 This is a structural block diagram of the pretreatment module in the synthesis reaction apparatus for a sulfur-free odorant according to the present invention;

[0043] Figure 5 This is a flowchart of the pretreatment module in the synthesis reaction apparatus for a sulfur-free odorant of the present invention;

[0044] Figure 6 This is a flowchart of a method for synthesizing a sulfur-free odorant according to the present invention.

[0045] In the diagram: 10, Reactor; 20, Raw material storage tank; 30, Feeding pipeline; 40, Automatic feeding mechanism; 401, Metering pump; 402, Pipe section; 403, Jacketed structure; 404, Piezoelectric ceramic vibrator; 405, Viscosity sensor; 406, Pressure sensor; 407, Temperature sensor. Detailed Implementation

[0046] The subject matter described herein will now be discussed with reference to exemplary embodiments. It should be understood that these embodiments are discussed only to enable those skilled in the art to better understand and implement the subject matter described herein, and changes may be made to the function and arrangement of the elements discussed without departing from the scope of this specification. Various processes or components may be omitted, substituted, or added as needed in the examples. Furthermore, features described in some examples may be combined in other examples.

[0047] Example 1:

[0048] Please refer to the following: Figures 1 to 5 A synthesis reaction apparatus for a sulfur-free odorant includes: a reaction vessel 10 and multiple raw material storage tanks 20 (for storing, for example, acrylic acid, allyl alcohol, toluene, etc.), each raw material storage tank 20 being connected to the reaction vessel 10 via an independent feed pipeline 30. The reaction vessel 10 is typically also equipped with auxiliary equipment such as an azeotropic distillation unit, a condenser, and a water separator (not fully shown in the figure).

[0049] For key raw materials such as acrylic acid, which have high viscosity or are prone to thickening at low temperatures, this invention provides an automatic feeding mechanism 40 on its feeding pipeline 30. This mechanism includes a metering pump 401 and a pretreatment module located at its inlet end. Specifically, the pretreatment module includes: a pipe section 402, a viscosity sensing unit, a temperature control unit, a vibration generating unit, a pressure sensor 406, a temperature sensor 407, and a control unit.

[0050] Pipe section 402 is part of the feed pipe 30, serving as a cavity through which materials flow and are processed. The viscosity sensing unit is preferably an insertion-type or pipe-wall-type online viscosity sensor 405, whose probe extends into pipe section 402 or is in direct contact with the flow channel, for continuously and in real time measuring the apparent viscosity value of the material and transmitting the signal to the control unit.

[0051] In this embodiment, the temperature control unit adopts a jacketed structure 403, which is tightly wrapped around the outside of the pipe section 402. A circulating heat exchange medium (such as hot water, heat transfer oil, or cooling water) can be introduced into the jacket. By adjusting the temperature and flow rate of the medium, the material in the pipe section 402 can be heated or cooled quickly and accurately.

[0052] In this embodiment, the vibration generating unit employs a piezoelectric ceramic vibrator 404, which can be tightly attached and fixed to the outer wall of the pipe section 402 using a high-strength adhesive or clamps. During use, the piezoelectric ceramic vibrator 404 generates high-frequency (e.g., greater than 20kHz) low-amplitude micromechanical vibrations. These vibrations are transmitted through the pipe wall to the internal material, disrupting its internal structural forces, preventing it from adhering to the pipe wall or forming crystal nuclei, and reducing its viscosity without significantly increasing the temperature.

[0053] Pressure sensor 406 and temperature sensor 407 are also installed on pipe section 402. They are used to monitor the pressure and real-time temperature of the material, respectively, and send the monitored data to the control unit to provide auxiliary parameters for executing control commands.

[0054] The control unit can be a standalone PLC or integrated into a DCS. It is connected to the viscosity sensing unit, the regulating valve of the temperature control unit, the driver of the vibration generating unit, the frequency converter of the metering pump 401, and the pressure sensor 406 and temperature sensor 407.

[0055] The working process of the preprocessing module provided by this invention is as follows:

[0056] Pre-feeding pretreatment mode: After receiving the feeding command, the control unit first activates the temperature control unit and the vibration generating unit. The temperature control unit rapidly heats the material based on the difference between the current material temperature (from temperature sensor 407) and the target temperature. Simultaneously, the vibration generating unit operates at high intensity to shake off any condensed or adhering materials. The control unit continuously reads data from the viscosity sensing unit. When the viscosity value decreases and reaches the preset feeding start threshold V, the control unit will initiate the feeding process. start At this point, it is determined that the material is in the optimal conveying flow state, and then proceeds to the next step.

[0057] Steady-state collaborative feeding mode: Metering pump 401 is started. During the feeding process, the core task of the control unit is to maintain the detected viscosity value within a preset optimal range [V]. low V high If the viscosity value shows an upward trend but remains within the range, the control unit will generate a first control command to slightly increase the heating power of the temperature control unit and / or command the vibration generation unit to switch to intermittent pulse mode to maintain the flow state with minimal energy consumption; if the viscosity value increases significantly due to any reason (such as batch differences in raw materials) and exceeds the upper limit of the range, and is greater than or equal to the enhanced treatment threshold (V alert The control unit then instructs the temperature control unit and vibration generation unit to enter the enhanced processing mode, quickly intervene, and restore the flow state. At the same time, based on the stable reading of the pressure sensor 406 in the pipe section 402 (pressure stability is a prerequisite for flow stability) and viscosity data, the control unit generates a second control command to dynamically fine-tune the speed of the metering pump 401 to ensure a constant outlet flow.

[0058] Post-feeding cleaning mode: After a single feeding is completed, the control unit immediately instructs the temperature control unit to stop heating and switches to the cooling medium to cool the pipe section 402 quickly; at the same time, it instructs the vibration generation unit to work in a specific cleaning mode (such as sweep frequency vibration at a specific frequency) for a period of time, using thermal expansion and contraction and mechanical vibration to effectively remove trace residues on the inner wall of the pipe, preparing a clean flow channel for the next feeding.

[0059] As an example and not a limitation, the above-mentioned material feeding start threshold V start It can be set to 1.5 times the standard viscosity of the raw material at 25°C, while the optimal range [V] low V high The viscosity can be set to 0.8 to 1.2 times the standard viscosity; the strengthening treatment threshold V alert The viscosity can be set to 2.0 times the standard viscosity. The intermittent pulse mode can cycle for 2 seconds of operation and 8 seconds of rest. The sweep frequency range of the cleaning mode can be 18kHz to 25kHz, and the duration can be 30 seconds. Those skilled in the art can determine the optimal values ​​of the above parameters through limited experiments based on the rheological properties of the specific raw materials.

[0060] By utilizing the aforementioned pretreatment module, preliminary treatment of raw materials before feeding and subsequent processing after feeding are performed, solving the problem of unstable flow rate caused by decreased fluidity during the transportation of high-viscosity or easily crystallizing raw materials, thus ensuring the accuracy and continuity of feeding. Specifically, the pretreatment module intelligently adjusts the working status of the temperature control unit and vibration generation unit by monitoring the viscosity, pressure, and temperature of the material in real time, ensuring that the material reaches and maintains the optimal conveying flow state before entering the metering pump 401. During feeding, the control unit dynamically adjusts the speed of the metering pump 401 based on real-time monitoring data, further ensuring a constant outlet flow rate, thereby avoiding reaction instability and product quality problems caused by flow fluctuations. In addition, the post-feeding cleaning mode effectively prevents material residue on the inner wall of the pipe, reduces the risk of cross-contamination, and improves production efficiency and product purity.

[0061] Example 2:

[0062] Additionally, please refer to the following: Figure 6 The present invention also provides a method for synthesizing a sulfur-free odorant (e.g., an acrylate-based sulfur-free odorant) using the apparatus described in Example 1, specifically comprising the following steps:

[0063] S100, Intelligent Raw Material Feeding:

[0064] For key raw materials (such as acrylic acid), the aforementioned intelligent feeding process is implemented: the pretreatment module is started, and after reaching the optimal flow state through collaborative control, the metering pump 401 is started and dynamically adjusted to deliver acrylic acid of precise quality into the reactor 10; for other raw materials (such as allyl alcohol and toluene solvent), they can be sequentially fed into the reactor 10 through their conventional pipelines (with or without a pretreatment module).

[0065] S200, azeotropic distillation reaction:

[0066] Add an appropriate amount of water-removing agent (such as toluene) and catalyst (such as p-toluenesulfonic acid) to the reactor 10, start stirring and heating to carry out the esterification reaction. The water generated in the reaction forms an azeotrope with toluene and is distilled off. After condensation and water separation, the toluene is continuously returned to the reactor 10, and the water is removed from the system, pushing the reaction equilibrium to the right.

[0067] S300, neutralizing wash:

[0068] After the reaction is complete, the reaction mixture is cooled, an alkaline solution is added to neutralize the catalyst and residual acid, the mixture is allowed to stand and separate into layers, the lower aqueous phase is separated and discarded, and the organic phase is washed several times with deionized water until neutral.

[0069] S400, distillation:

[0070] The washed organic phase is transferred to a distillation unit and distilled under reduced pressure. Excess toluene and other low-boiling substances are first distilled off and recovered. Then, the target product fraction with a specific boiling range is collected to obtain a high-purity sulfur-free odorant base monomer.

[0071] S500, compound:

[0072] The obtained basic monomers and other functional components (such as other odor monomers, antioxidants, stabilizers, etc.) are precisely mixed and homogenized in a mixing tank according to a specific formula, and finally filtered to obtain the final sulfur-free odorant product.

[0073] In the entire method, step S100 is the most critical prerequisite for ensuring the consistency of all subsequent reactions and product quality. This invention achieves precise and controllable control of the entire process from raw materials to products by deeply integrating hardware (preprocessing module) and software (cooperative control logic) and embedding them into the complete synthesis process.

[0074] The embodiments of the present invention have been described above, but the present invention is not limited to the specific embodiments described above. The specific embodiments described above are merely illustrative and not restrictive. Those skilled in the art can make many other forms under the guidance of the present invention, all of which are within the protection scope of the present invention.

Claims

1. A synthesis reaction apparatus for sulfur-free odorant, characterized in that, include: The reactor and multiple raw material storage tanks for storing different raw materials, each of which is connected to the reactor via an independent feeding pipeline; At least one of the feeding pipelines is provided with an automatic feeding mechanism, which includes: a metering pump provided on the feeding pipeline and a pretreatment module provided at the inlet end of the metering pump; The preprocessing module includes: The pipe section forms part of the feeding pipeline; A viscosity sensing unit is used to detect the viscosity of the material flowing through the pipe section in real time; The temperature control unit is used to regulate the temperature of the material inside the pipe section; A vibration generating unit is attached to the outer wall of the pipe section and is used to apply mechanical vibration to the pipe section; The control unit is connected to the viscosity sensing unit, temperature control unit, vibration generating unit, and metering pump signal, and is configured as follows: Based on the viscosity data detected in real time by the viscosity sensing unit, a first control command is generated to coordinate the working state of the temperature control unit and the start / stop and working mode of the vibration generation unit. Based on the pressure or viscosity data within the pipe section, a second control command is generated to dynamically adjust the operating parameters of the metering pump. The control unit is further configured to: before performing the feeding operation, activate the temperature control unit and the vibration generation unit to preheat and vibrate the material remaining in the pipe section until the detected viscosity value reaches the preset feeding start threshold. During steady-state feeding, the control unit is configured to control the vibration generating unit to operate in intermittent pulse mode when the detected viscosity value is maintained within a preset optimal range. The control unit is further configured to: after a single feeding operation is completed, control the temperature control unit to stop heating and start cooling, and at the same time control the vibration generating unit to work in cleaning mode to remove residual material from the inner wall of the pipe section.

2. The synthesis reaction apparatus for a sulfur-free odorant according to claim 1, characterized in that, The temperature control unit has a jacketed structure, which is wrapped around the outside of the pipe section; the jacket is filled with heat exchange medium.

3. The synthesis reaction apparatus for a sulfur-free odorant according to claim 1, characterized in that, The vibration generating unit is a piezoelectric ceramic vibrator, which is fixedly installed on the outer wall of the pipe section.

4. The synthesis reaction apparatus for a sulfur-free odorant according to claim 1, characterized in that, The viscosity sensing unit is a viscosity sensor, which is installed on the pipe section.

5. The synthesis reaction apparatus for a sulfur-free odorant according to claim 1, characterized in that, The pretreatment module also includes a pressure sensor and a temperature sensor installed on the pipe section, and the pressure sensor and temperature sensor are connected to the control unit via signal connection.

6. A method for synthesizing a sulfur-free odorant, using a reaction apparatus for synthesizing a sulfur-free odorant as described in any one of claims 1-5, characterized in that, The following steps are included: S100, Raw Material Feeding: For at least one critical raw material with high viscosity or easy crystallization, the following feeding procedure shall be performed: The pretreatment module corresponding to the key raw material is activated. Based on the viscosity data detected in real time by the viscosity sensor, the temperature control unit and the vibration generation unit are adjusted in coordination to ensure that the key raw material reaches and maintains a preset flow state before entering the metering pump. Start the metering pump and dynamically adjust the pumping parameters according to the real-time data provided by the pretreatment module to deliver the key raw materials to the reactor in the set amount; Other raw materials are transported to the reactor through their respective feed pipelines; S200, Azeotropic Distillation Reaction: In a reaction vessel, a dehydrating agent is added, and an esterification reaction is carried out in the presence of a catalyst, while the water generated in the reaction is continuously removed through an azeotropic distillation device; S300, Neutralization and Washing: After the reaction is completed, the materials in the reactor are neutralized, washed, and the aqueous phase is removed. S400, distillation: The obtained organic phase is subjected to vacuum distillation to collect the target fraction and obtain the sulfur-free odorant base monomer; S500, compound: The basic monomer is mixed with other components according to the formula and stabilized to obtain the final sulfur-free odorant product.

7. The method for synthesizing a sulfur-free odorant according to claim 6, characterized in that, In step S100, the intelligent delivery process for key raw materials specifically includes: If the real-time viscosity is higher than the preset feeding threshold, the heating power of the temperature control unit is increased and the vibration generation unit is activated for enhanced processing. If the real-time viscosity is within the preset optimal range, the current state of the temperature control unit is maintained and the vibration generation unit is controlled to work in intermittent pulse mode until delivery is completed.

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