Pilot scale production device for reaction type nano pesticide

Abstract

The utility model discloses a reaction type nano pesticide pilot scale production device which comprises a digital temperature control reaction kettle and a nano pesticide preparation kettle, and a digital temperature control reaction kettle drainage device is connected with a liquid medicine conveying port of the nano pesticide preparation kettle through a corrosion-resistant pipeline; the digital temperature control reaction kettle is provided with a digital control screen A, a visual window, a feeding hole, a mechanical stirrer and an automatic water inlet cleaning device; the nano pesticide preparation kettle is provided with a digital control screen B, a nano carrier lead-in port, a liquid medicine conveying port and a discharge port; an ultrasonic dispersion device is also arranged in the nano pesticide preparation kettle, and a centrifugal device is arranged at the lower part of the kettle body. According to the device, laboratory production of the nano-pesticide is converted into Chinese production, the preparation efficiency of the nano-pesticide is improved, and a guarantee is provided for the field pesticide effect of the nano-pesticide.

Description

Technical Field

[0001] This utility model belongs to the field of pesticide processing, specifically relating to a pilot production device for reactive nano-pesticides. Background Technology

[0002] With the increasing demand for efficient and environmentally friendly pesticides in modern agriculture, nanopesticides have gradually become a research hotspot in the pesticide field due to their unique size effect, targeted slow release, and environmental compatibility. However, the large-scale production of nanopesticides still faces many technical bottlenecks. Traditional production methods (such as mechanical grinding and chemical precipitation) generally suffer from complex processes, high energy consumption, and poor product uniformity. Furthermore, the production process often relies on large amounts of organic solvents or surfactants, leading to increased costs and the risk of secondary pollution. In addition, existing laboratory preparation techniques are difficult to directly scale up to pilot or industrial scale. Equipment lacks precise control over the nucleation, growth, and surface modification processes of nanoparticles, resulting in unstable product performance and poor batch-to-batch consistency during scale-up, severely restricting the practical application of nanopesticides.

[0003] To address the aforementioned issues, existing pilot-scale equipment often employs a step-by-step process, such as first synthesizing the carrier and then loading the pesticide. Furthermore, the limitations of traditional equipment in terms of mixing efficiency, mass and heat transfer performance, and online monitoring capabilities further restrict the efficient and continuous production of nanopesticides. Utility Model Content

[0004] This invention addresses the aforementioned shortcomings by providing a pilot-scale production device for reactive nanopesticides. This invention solves the problems of low production efficiency, uneven dispersion, and high dependence on manual labor in existing technologies, enabling the transition from laboratory to pilot-scale production and improving the preparation efficiency and field efficacy stability of nanopesticides.

[0005] The present invention provides a pilot-scale production device for reactive nanopesticides, comprising a digitally controlled temperature reactor and a nanopesticide preparation vessel. The liquid discharge device of the digitally controlled temperature reactor is connected to the liquid delivery port of the nanopesticide preparation vessel via a corrosion-resistant pipe. The digitally controlled temperature reactor is equipped with a digital control screen A, a viewing window, a feed inlet, a mechanical stirrer, and an automatic water inlet cleaning device. The nanopesticide preparation vessel is equipped with a digital control screen B, a nanocarrier inlet, a liquid delivery port, and a discharge port. An ultrasonic dispersion device is also installed inside the nanopesticide preparation vessel to quickly and efficiently disperse the aggregated nanocarriers. A centrifuge device is also installed at the bottom of the nanopesticide preparation vessel to quickly precipitate the nanopesticides for convenient subsequent processing.

[0006] The feed inlet of the digitally temperature-controlled reactor is designed as an inverted funnel to prevent powdered drugs from clogging the inlet.

[0007] The mechanical stirrer inside the digital temperature-controlled reactor is a three-blade stirring device, which is divided into three groups in the longitudinal direction. It is suitable for operation of different reaction volumes. The gap between the blade and the bottom of the reactor is ≤5mm to ensure no dead corners in the mixing.

[0008] The nano-pesticide preparation vessel is equipped with a condensation device in the lower part of the vessel body, which uses circulating condensate water for condensation, thereby reducing the heat generated during the centrifugation process. The bottom of the ultrasonic dispersion device inside the vessel body is equipped with a titanium alloy amplitude transformer.

[0009] The digital temperature-controlled reactor has an embedded heating layer at the bottom, suitable for experiments requiring reaction temperatures, with an adjustable temperature range of 0-250℃; an automatic water inlet cleaning device is located at the top inside the reactor.

[0010] The feed inlet of the nano-pesticide preparation vessel is located at the bottom of the vessel, and the nano-carrier inlet is located at the top of the vessel.

[0011] The digital temperature-controlled reactor drainage device is located at the bottom of the reactor.

[0012] The beneficial effects of this invention are as follows: the device can realize the synchronous reaction and loading of pesticide active ingredients and nanocarriers, significantly shorten the production cycle, improve product stability, and reduce energy consumption and solvent dependence, thus providing technical support for the green and large-scale preparation of nano-pesticides.

[0013] 1. Increased production capacity: Single batch output reaches 50-200L, which is 10-20 times that of laboratory scale, meeting the needs of pilot production and shortening the production cycle by 40%;

[0014] 2. Dispersion uniformity: The dual dispersion of ultrasound and mechanical dispersion results in an average particle size of ≤100nm for the nanocarrier and a particle size distribution CV value of <5%.

[0015] 3. Automation level: Temperature control, cleaning, and centrifugation are all automated, reducing manual intervention by 90%;

[0016] 4. Safety: The sealed design combined with automatic cleaning reduces the risk of solvent exposure by 80%;

[0017] 5. Guaranteed efficacy in the field: Nanopesticides have a suspension rate of >98%, a photolysis rate reduced by 50%, and a residual effect extended by 30%. Attached image description:

[0018] Figure 1 The diagram shown is a schematic representation of the basic structure of this utility model.

[0019] In the diagram, 1. Digital temperature-controlled reactor, 2. Nanopesticide preparation vessel, 3. Digital control screen A, 4. Viewing window, 5. Feed inlet, 6. Mechanical stirrer, 7. Heating layer, 8. Automatic water inlet cleaning device, 9. Drainage device, 10. Digital control screen B, 11. Nanocarrier inlet, 12. Pesticide delivery inlet, 13. Ultrasonic dispersion device, 14. Condensation device, 15. Centrifuge device, 16. Discharge port. Detailed implementation method:

[0020] To better understand this utility model, specific examples are used below to illustrate the technical solution of this utility model in detail, but this utility model is not limited thereto.

[0021] This invention consists of a digitally temperature-controlled reactor 1 (for carrier synthesis and pesticide loading) and a nano-pesticide preparation reactor 2 (for dispersion, volume adjustment, and purification) connected by corrosion-resistant pipelines. The specific structure is as follows:

[0022] 1. Digital temperature-controlled reactor

[0023] Cauldron structure:

[0024] Material: 316L stainless steel inner liner, with an outer layer of polytetrafluoroethylene for corrosion protection;

[0025] Capacity: 50-200L, length-to-diameter ratio 2:1, bottom is tapered (60° angle) for easy drainage.

[0026] Functional components:

[0027] Digital control panel A3: Embedded PLC controller, preset temperature, stirring rate, and reaction time parameters, supports data recording and export;

[0028] Viewing window 4: Double-layer tempered glass (10mm thick), with a hydrophobic coating on the inside to prevent fog from interfering with observation;

[0029] Mechanical mixer 6: Three-bladed propeller + anchor paddle combination, speed stepless adjustment from 0-1000r / min, gap between paddle and bottom of the vessel ≤5mm, ensuring no dead corners in mixing;

[0030] Heating layer 7: Silicone electric heating film (power 5kW), with PID temperature control algorithm, temperature control range 25-150℃, accuracy ±1℃;

[0031] Automatic water inlet cleaning device 8: Top annular spray pipe (orifice diameter 0.5mm, spray pressure 0.3-0.5MPa), connected to the pure water system and the drain solenoid valve to achieve one-button cleaning;

[0032] Drainage device 9: A pneumatic ball valve (DN50) is installed at the bottom and connected to the liquid delivery port 12 of the nano-pesticide preparation vessel 2 via a polyurethane hose.

[0033] 2. Nanopesticide Preparation Reactor 2

[0034] Cauldron structure:

[0035] Material: 304 stainless steel, inner wall polished to Ra≤0.4μm to reduce material adhesion;

[0036] Capacity: Matches temperature-controlled reactor 1, with a volume error of ≤5%.

[0037] Functional components:

[0038] Digital control panel B10: Embedded PLC controller, preset temperature and response time parameters, supports data recording and export;

[0039] Ultrasonic dispersion device 13: A titanium alloy amplitude transformer (50mm diameter) is mounted at the bottom; frequency adjustable from 20-40kHz; power 0-2000W; sound intensity density ≥0.5W / cm². 3 ;

[0040] Condensing unit 14: serpentine coil (Hastelloy alloy material), externally connected to circulating cooling water (temperature 4-10℃), condensing area ≥1.5m² 2 ;

[0041] Centrifuge device 15: Built-in tubular centrifuge (speed 0-10000r / min, centrifugal force ≥12000×g), separation chamber capacity 20L, impurity removal rate >99%;

[0042] Viewing window: Same specifications as the temperature-controlled reactor, located on the side of the reactor body, used to observe the dispersion and centrifugation status;

[0043] Discharge port 16: A pneumatic butterfly valve (DN80) is installed at the bottom, which can be switched to the circulation pipeline (connected to the top of the preparation vessel) or the finished product collection tank.

[0044] 3. Collaborative work

[0045] 1. Vector synthesis stage:

[0046] The raw materials are added to the digitally temperature-controlled reactor 1 through the feed inlet, and the temperature (e.g., 60℃) and stirring rate (e.g., 500r / min) are set, and the reaction is carried out for 2-4 hours.

[0047] The mechanical agitator features a dual-blade design: a bottom anchor blade to prevent sedimentation, and an upper propeller to enhance convection.

[0048] 2. Drug transfer stage:

[0049] After the reaction is complete, the draining device delivers the liquid to the nanocarrier inlet 11 of the nanopesticide preparation vessel 2, with a delivery time of ≤10 minutes (the flow rate is controlled by the valve opening).

[0050] 3. Dispersion and purification stage:

[0051] Start the ultrasonic dispersion device 13 (e.g., 30kHz, 1200W) for 30 minutes, while the condensation device 14 maintains a constant liquid level.

[0052] Centrifuge device 15 is run at 8000 r / min for 10 minutes to separate unloaded free pesticides or aggregated particles.

[0053] 4. Cleaning stage:

[0054] After production, the automatic water inlet cleaning device 8 sprays pure water, and the mechanical agitator 6 rotates at low speed (200 r / min). The cleaning solution is discharged through the draining device, and the cycle repeats 3 times.

[0055] Example 1

[0056] Taking the preparation of imidacloprid-silica nanocapsules as an example

[0057] 1. Feeding: Add 50L of ethyl silicate ethanol solution (20% concentration) and imidacloprid technical (10% concentration) into the digital temperature-controlled reactor 1 through feed inlet 5;

[0058] 2. Reaction: Set the temperature to 60℃ and the stirring speed to 600 r / min, and react for 3 hours;

[0059] 3. Transfer: Open the pneumatic ball valve, and the liquid pesticide is transported through the pipeline to nano-pesticide preparation vessel 2 (flow rate controlled at 8L / min);

[0060] 4. Dispersion: Start the ultrasonic dispersion device 13 for treatment (frequency 28kHz, power 1500W) for 40 minutes, while the condensation device 14 maintains the temperature at 25℃.

[0061] 5. Centrifugation: Centrifuge at 8500 r / min for 15 minutes using centrifuge device 15, and collect the lower layer of nanocapsule suspension;

[0062] 6. Discharge: The finished product is discharged into a sterile storage tank through the discharge port, and the remaining liquid is recycled to the nano-pesticide preparation reactor 2 for secondary treatment;

[0063] 7. Cleaning: The automatic water inlet cleaning device 8 rinses both kettles with pure water, taking 20 minutes.

[0064] Effect verification:

[0065] The average particle size of the nanocapsules is 85 nm, and the PDI (polydispersity index) is 0.12.

[0066] Imidacloprid has an encapsulation rate of 92% and its field residual effect is extended to 21 days (compared to 14 days for traditional formulations).

Claims

1. A pilot-scale production device for reactive nanopesticides, characterized in that, It includes a digitally controlled temperature reactor and a nano-pesticide preparation vessel. The liquid discharge device of the digitally controlled temperature reactor is connected to the liquid delivery port of the nano-pesticide preparation vessel through a corrosion-resistant pipe. The digitally controlled temperature reactor is equipped with a digital control screen A, a viewing window, a feed inlet, a mechanical stirrer, and an automatic water inlet cleaning device. The nano-pesticide preparation vessel is equipped with a digital control screen B, a nano-carrier inlet, a liquid delivery port, and a discharge port. The nano-pesticide preparation vessel is also equipped with an ultrasonic dispersion device inside, and a centrifuge device is installed at the bottom of the vessel.

2. The pilot-scale production device for reactive nanopesticides according to claim 1, characterized in that, The feed inlet of the digitally temperature-controlled reactor is designed as an inverted funnel.

3. The pilot-scale production device for reactive nanopesticides according to claim 1, characterized in that, The mechanical stirrer inside the digital temperature-controlled reactor is a three-blade stirring device, which is divided into three groups longitudinally, with a gap of ≤5mm between the blades and the bottom of the reactor.

4. The pilot-scale production device for reactive nanopesticides according to claim 1, characterized in that, The lower part of the nano-pesticide preparation vessel is equipped with a condensation device, and a titanium alloy amplitude transformer is installed at the bottom of the ultrasonic dispersion device inside the vessel.

5. The pilot-scale production device for reactive nanopesticides according to claim 1, characterized in that, The digital temperature-controlled reactor has an embedded heating layer at the bottom, and an automatic water inlet cleaning device is located at the top inside the reactor.

6. The pilot-scale production device for reactive nanopesticides according to claim 1, characterized in that, The feed inlet of the nano-pesticide preparation vessel is located at the bottom of the vessel, and the nano-carrier inlet is located at the top of the vessel.

7. The pilot-scale production device for reactive nanopesticides according to claim 1, characterized in that, The digital temperature-controlled reactor drainage device is located at the bottom of the reactor.

8. The pilot-scale production device for reactive nanopesticides according to claim 1, characterized in that, The digital temperature-controlled reactor has a capacity of 50-200L, a length-to-diameter ratio of 2:1, and a conical bottom with a 60° inclination angle; the nano-pesticide preparation vessel has a capacity of 50-200L, a length-to-diameter ratio of 2:1, and a conical bottom.

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