Micro-nano plastic integrated preparation device

Abstract

The application discloses a kind of micro-nano plastics integrated preparation device, including integrated rack, the integrated rack is equipped with sequentially connected feed pretreatment module, dispersion module, constant-temperature polymerization module, primary separation module, purification filtration module, vacuum drying module and sealed storage module.This device uses high-speed shearing and ultrasonic dislocation collaborative dispersion structure, cooperate with inclined no-residual tank, closed conveying pipeline and modular integrated layout, effectively solve the problem of traditional preparation equipment split layout, material transfer is easy to be contaminated, particle dispersion is not uniform, experimental repeatability is poor;The overall structure of the device is compact, integrated and good in airtightness, can stably prepare micro-nano plastic particles with uniform particle size and high purity, and can be widely applied to high-precision micro-nano plastic scientific experimental research of environmental water, soil and microbial toxicity, and has good practicability and popularization value.

Description

Technical Field

[0001] This invention relates to the field of experimental equipment for the preparation of micro- and nano-plastics, and in particular to a modular integrated micro- and nano-plastics preparation device, which is mainly applicable to experimental research scenarios of micro- and nano-plastics such as environmental ecology, water and soil pollution research, and microbial toxicology response. Background Technology

[0002] In existing environmental science experimental research, commercially available micro / nanoplastics generally suffer from high procurement costs, large batch-to-batch variations, and unstable particle performance, making them unsuitable for high-precision and highly repeatable experimental requirements. Meanwhile, the equipment currently used for laboratory-made micro / nanoplastics is mostly separate, independent instruments with low integration, and generally employs a single dispersion method, resulting in poor material dispersion uniformity and a high likelihood of particle agglomeration.

[0003] Existing preparation equipment has several substantial drawbacks: First, the single dispersion mode has limited dispersion effect, resulting in large differences in particle size and severe agglomeration of the prepared micro- and nano-plastic particles, leading to poor repeatability of experimental data; Second, the equipment is arranged in separate units, with each process—feeding, dispersion, polymerization, separation, purification, drying, and storage—being independent of each other. This requires frequent manual transfer of materials during the experiment, which can easily cause secondary contamination of particles and material loss; Third, conventional equipment has poor airtightness, making it impossible to achieve a closed-loop preparation process. External impurities can easily enter the system, seriously affecting the purity of the micro- and nano-plastic products and failing to meet the requirements of high-precision environmental experiments. Summary of the Invention

[0004] The purpose of this invention is to overcome the shortcomings of the prior art and provide an integrated micro-nano plastic preparation device. This device solves the technical problems of low integration, simple dispersion structure, easy contamination of materials, and poor uniformity of product particle size in existing preparation equipment. Through modular integration, synergistic dispersion, and fully enclosed sealed conveying structure design, a stable, high-purity, and highly repeatable integrated micro-nano plastic equipment is achieved, which is suitable for high-precision environmental experimental use.

[0005] The present invention is achieved through the following technical solution: an integrated micro-nano plastic preparation device, comprising an integrated frame, wherein the integrated frame is provided with a feeding pretreatment module, a dispersion module, a constant temperature polymerization module, a primary separation module, a purification and filtration module, a vacuum drying module and a sealed storage module;

[0006] The feed pretreatment module includes a monomer storage bottle, an initiator storage bottle and a deionized water storage bottle, and each storage bottle is connected in sequence to a filter assembly and a metering peristaltic pump.

[0007] The dispersion module includes a glass dispersion tank, a high-speed shear stirring assembly, and an ultrasonic dispersion assembly. The high-speed shear stirring assembly and the ultrasonic dispersion assembly are vertically staggered and inserted into the top of the glass dispersion tank. The top side wall of the glass dispersion tank is provided with a pH detection sealing interface for inserting a pH detection device. Each quantitative peristaltic pump is connected in parallel to a closed guide pipe with a control valve. The outlet of the closed guide pipe is connected to the inlet of the glass dispersion tank.

[0008] The constant temperature polymerization module includes a constant temperature water bath, a glass polymerization tank, a low-speed stirring component, and a temperature detection component; the glass polymerization tank is embedded in the constant temperature water bath, and the feed end of the glass polymerization tank is sealed to the bottom discharge end of the glass dispersion tank; the low-speed stirring component and the temperature detection component are installed on the top of the glass polymerization tank.

[0009] The primary separation module includes a vertical centrifuge tube mounted on a fixed support, the inlet of which is connected to the outlet of the glass polymerization tank.

[0010] The purification and filtration module includes a suspended funnel, a nanofiltration membrane assembly, and a collection beaker. The nanofiltration membrane assembly is detachably snapped onto the lower end of the suspended funnel, and the collection beaker is arranged directly below the suspended funnel.

[0011] The vertical centrifuge tube is connected to the suspended funnel via a sealed guide pipe with a control valve. The inlet of the sealed guide pipe extends into the vertical centrifuge tube, and its outlet extends into the suspended funnel. The purified suspension is transferred to the vacuum drying module via the collection beaker for drying. The dried micro-nano plastic powder is then transferred to the sealed storage module.

[0012] The stirring paddle of the high-speed shear stirring assembly and the probe of the ultrasonic dispersion assembly are vertically offset inside the glass dispersion tank, with a height difference of 3cm to 5cm between them.

[0013] Both the glass dispersion tank and the glass polymerization tank have a volume of 1L to 3L, and the inner wall of the tank is smooth and free of any residue.

[0014] The bottom of the vertical centrifuge tube is detachably equipped with a waste liquid receiving tank.

[0015] The bottom of the glass dispersion tank has a conical cross-section, and its sidewalls have an inclined surface structure.

[0016] The inclined surface structure forms a 15-degree angle with the central axis of the bottom discharge end of the glass dispersion tank.

[0017] The glass polymerization tank is equipped with a sealed sampling port on its side wall.

[0018] The vacuum drying module includes a vacuum drying chamber and a petri dish, with the petri dish placed inside the vacuum drying chamber; the purified suspension is transferred to the petri dish via the collection beaker.

[0019] The sealed storage module includes a sealed storage bottle and a sampling scraper, with the sampling scraper placed inside the sealed storage bottle; the sealed storage bottle includes a bottle body and a sealing cap placed at the bottle mouth, with a silicone sealing ring inside the sealing cap.

[0020] The pH detection sealing interface is a plug-in sealing structure. In the detection state, the pH detection sealing interface is sealed and fitted to the glass dispersion tank.

[0021] Compared with the prior art, the advantages of the present invention are as follows:

[0022] 1) This design features a vertically staggered high-speed shearing and ultrasonic synergistic dispersion structure, forming a three-dimensional physical dispersion area without dead angles. Compared with a single dispersion structure, it can significantly improve the material dispersion effect, effectively inhibit the agglomeration of micro and nano plastic particles, and greatly improve the uniformity of product particle size and the purity of finished product.

[0023] 2) This device adopts an integrated frame to integrate seven functional modules into one unit. It forms a fully closed-loop material conveying structure through a sealed guide pipe, replacing the traditional mode of separate placement of scattered equipment and manual material transfer. This effectively avoids secondary pollution and material loss of micro-nano plastic particles, and greatly improves product purity and experimental repeatability.

[0024] 3) This device is equipped with an inclined, residue-free dispersion tank, a sealed sampling structure, a gravity purification and filtration structure, and a low-temperature vacuum drying and sealed storage structure. The various structures work together to stably prepare micro-nano plastic particles with uniform particle sizes of 50nm to 300nm. The particles are non-agglomerated, highly pure, and have stable performance, making them suitable for various high-precision environmental experimental scenarios.

[0025] 4) The overall equipment has a compact structure, is modular and detachable, is easy to disassemble and clean, has low manufacturing cost, operates in a completely closed and pollution-free manner, has strong practicality and wide adaptability, and has good promotion and application value. Attached Figure Description

[0026] Figure 1 This is a schematic diagram of the structure of an embodiment of the present invention.

[0027] The following are the meanings of the labels in the diagram: 1. Integrated frame; 2. Feed pretreatment module; 21. Monomer storage bottle; 22. Initiator storage bottle; 23. Deionized water storage bottle; 24. Filter assembly; 25. Metering peristaltic pump; 3. Dispersion module; 31. Glass dispersion tank; 32. High-speed shear stirring assembly; 33. Ultrasonic dispersion assembly; 34. pH detection sealed interface; 4. Constant temperature polymerization module; 41. Constant temperature water bath; 42. Glass polymerization tank; 43. Low-speed stirring group. Components; 44. Temperature detection component; 45. Sealed sampling interface; 5. Primary separation module; 51. Fixing bracket; 52. Vertical centrifuge tube; 53. Waste liquid receiving tank; 6. Purification and filtration module; 61. Suspended funnel; 62. Nanofiltration membrane component; 63. Collection beaker; 7. Vacuum drying module; 71. Vacuum drying chamber; 72. Petri dish; 8. Sealed storage module; 81. Sealed storage bottle; 82. Sampling scraper; 9. Sealed flow guide pipeline; 10. Control valve. Detailed Implementation

[0028] The present invention will now be described in further detail with reference to the accompanying drawings and specific embodiments.

[0029] Example

[0030] See Figure 1 The device is an integrated micro-nano plastic preparation device, including an integrated frame 1. The integrated frame 1 is equipped with a feeding pretreatment module 2, a dispersion module 3, a constant temperature polymerization module 4, a primary separation module 5, a purification and filtration module 6, a vacuum drying module 7, and a sealed storage module 8.

[0031] The feed pretreatment module 2 includes a monomer storage bottle 21 for storing polymerization monomers, an initiator storage bottle 22 for storing initiators, and a deionized water storage bottle 23 for storing reaction solvents. Each storage bottle is connected in sequence to a filter assembly 24 and a metering peristaltic pump 25. The bottom of each storage bottle is equipped with a filter assembly 24, which can perform pre-treatment of the raw materials to remove impurities. The filtered material is independently, quantitatively, and uniformly conveyed through the metering peristaltic pump 25 at the bottom. The material is then conveyed to the glass dispersion tank 31 through a closed guide pipe 9, realizing the standardization of raw materials and the pretreatment operation without impurities.

[0032] The dispersion module 3 includes a glass dispersion tank 31, a high-speed shear stirring assembly 32, and an ultrasonic dispersion assembly 33. The high-speed shear stirring assembly 32 and the ultrasonic dispersion assembly 33 are vertically staggered and inserted into the top of the glass dispersion tank 31. The top side wall of the glass dispersion tank 31 is provided with a pH detection sealing interface 34 for inserting a pH detection device. Each quantitative peristaltic pump 25 is connected in parallel to a closed flow guide pipe 9 with a control valve 10. The outlet of the closed flow guide pipe 9 is connected to the inlet of the glass dispersion tank 31.

[0033] The constant-temperature polymerization module 4 includes a constant-temperature water bath 41, a glass polymerization tank 42, a low-speed stirring component 43, and a temperature detection component 44. The glass polymerization tank 42 is embedded in the constant-temperature water bath 41. The feed end of the glass polymerization tank 42 is sealed to the bottom discharge end of the glass dispersion tank 31 through a closed guide pipe 9 with a control valve 10, which can ensure that the material is conveyed in a closed manner without exposure. The low-speed stirring component 43 and the temperature detection component 44 are installed on the top of the glass polymerization tank 42. The low-speed stirring component 43 can stir the material at a low speed to avoid the agglomeration of micro and nano particles. The temperature detection component 44 can monitor the reaction temperature inside the tank in real time to ensure that the polymerization reaction proceeds at a constant temperature and is stable.

[0034] The primary separation module 5 includes a vertical centrifuge tube 52 mounted on a fixed support 51. The inlet of the vertical centrifuge tube 52 is connected to the outlet of the glass polymerization tank 42 through a closed guide pipe 9 with a control valve 10.

[0035] The purification and filtration module 6 includes a suspended funnel 61, a nanofiltration membrane assembly 62, and a collection beaker 63. The nanofiltration membrane assembly 62 is detachably snapped onto the lower end of the suspended funnel 61, and the collection beaker 63 is arranged directly below the suspended funnel 61.

[0036] The vertical centrifuge tube 52 is connected to the suspended funnel 61 through a closed guide pipe 9 with a control valve 10. The inlet of the closed guide pipe 9 extends into the vertical centrifuge tube 52, and its outlet extends into the suspended funnel 61. The purified suspension is transferred to the vacuum drying module 7 through the collection beaker 63 for drying. The dried micro-nano plastic powder is transferred to the sealed storage module 8.

[0037] The stirring paddle of the high-speed shear stirring component 32 and the probe of the ultrasonic dispersion component 33 are vertically staggered inside the glass dispersion tank 31, with a height difference of 3cm to 5cm between them. This forms a three-dimensional collaborative dispersion area inside the tank. Through the dual physical effects of high-speed shear stirring and ultrasonic cavitation, the material is efficiently and uniformly dispersed. The material in the glass dispersion tank 31 can be physically dispersed in all directions without dead angles, effectively improving the uniformity of material dispersion.

[0038] Both the glass dispersion tank 31 and the glass polymerization tank 42 have a volume of 1L to 3L, and the inner wall of the tank is smooth and has no wall-hanging structure.

[0039] The bottom of the vertical centrifuge tube 52 is detachably equipped with a waste liquid receiving tank 53.

[0040] The bottom of the glass dispersion tank 31 has a conical cross-section, and its sidewalls have an inclined surface structure.

[0041] The inclined surface structure forms a 15-degree angle with the central axis of the bottom discharge end of the glass dispersion tank 31, which can avoid material residue on the wall and ensure complete discharge of material.

[0042] The glass polymerization tank 42 has a sealed sampling interface 45 on its side wall, which can complete sampling and testing without compromising the airtightness of the system and avoid contamination by external impurities.

[0043] The vacuum drying module 7 includes a vacuum drying chamber 71 and a petri dish 72, with the petri dish 72 placed inside the vacuum drying chamber 71; the purified suspension is transferred to the petri dish 72 via a collection beaker 63.

[0044] The sealed storage module 8 includes a sealed storage bottle 81 and a sampling scraper 82, with the sampling scraper 82 placed inside the sealed storage bottle 81. The sealed storage bottle 81 includes a bottle body and a sealing cap placed at the bottle mouth. The sealing cap is equipped with a silicone sealing ring, which can seal and prevent contamination during storage.

[0045] The pH detection sealing interface 34 is a plug-in sealing structure. In the detection state, the pH detection sealing interface 34 is sealed and fitted with the glass dispersion tank 31, which can prevent external impurities from entering the reaction system. The pH detection and adjustment of the system can be completed under closed conditions, effectively maintaining the stability of the dispersion system and preventing external impurities from entering.

[0046] In this embodiment, the pore size of the nanofiltration membrane module 62 is 20nm to 50nm, which is suitable for the sieving and purification of micro-nano plastic particles with a particle size of 50nm to 300nm. The inner diameter of the closed flow guide pipe 9 is 0.8cm to 1cm, the inner wall of the pipe is smooth, and each section of the pipe is independently equipped with a control valve 10, which can independently control the flow and conveying rate of materials at each stage.

[0047] After pre-purification by the filter assembly 24, the materials in each storage bottle are conveyed at a constant speed by the quantitative peristaltic pump 25 and then transported to the glass dispersion tank 31 through the sealed guide pipe 9, where they are dispersed at high speed and uniformly. The materials then enter the glass polymerization tank 42 from the glass dispersion tank 31 for polymerization. After polymerization, the materials enter the primary separation module 5, where the vertically fixed centrifuge tube 52 accurately receives the polymerization products. Centrifugation is used to achieve preliminary separation of the micro-nano plastic solid particles from the supernatant waste liquid. The separated waste liquid falls into the waste liquid receiving tank 53 at the bottom for unified collection and treatment, completing the preliminary solid-liquid separation operation.

[0048] The coarse suspension of micro-nano plastics after initial separation is transported to the suspended funnel 61 of the purification and filtration module 6. The material naturally permeates under gravity and passes through the nano-filter membrane assembly 62 at the bottom of the funnel to complete particle size sieving and purification. The 20nm to 50nm filter membrane can effectively intercept micro-nano plastic particles, while water and trace soluble impurities pass through. The purified suspension drips into the collection cup below, completing pollution-free fine purification.

[0049] The purified suspension is transferred to a petri dish 72 within the vacuum drying module 7. The suspension is evenly spread on the surface of the petri dish 72, and moisture is removed through low-temperature vacuum drying to obtain dried micro-nano plastic powder. Finally, the dried micro-nano plastic powder is collected into a sealed storage bottle 81 in the sealed storage module 8, and completely sealed using a silicone sealing ring on the sealing cap. Sampling is then performed using a dedicated sampling spatula 82.

[0050] This device effectively overcomes the shortcomings of traditional micro-nano plastic preparation equipment, such as poor dispersion, fragmented equipment, easy introduction of contamination, and uneven product particle size, through a reasonable modular integrated layout and synergistic dispersion structure. The entire device has a simple and compact structure, is easy to disassemble and clean, and operates stably. It can continuously, in a closed loop, and without pollution, complete the preparation of micro-nano plastics. The prepared particles have high purity, uniform particle size, and good repeatability, which can fully meet the needs of various high-precision environmental science experiments.

[0051] In this embodiment, the device also includes a processor, which is a mature, existing device. It can be a Central Processing Unit (CPU), or other general-purpose processors, Digital Signal Processors (DSPs), Application Specific Integrated Circuits (ASICs), Field-Programmable Gate Arrays (FPGAs), or other programmable logic devices, discrete gate or transistor logic devices, discrete hardware components, etc. The general-purpose processor can be a microprocessor or any conventional processor. The processor is the control center of the device, connecting various parts through various interfaces and lines. In this embodiment, the quantitative peristaltic pump 25, high-speed shear stirring assembly 32, ultrasonic dispersion assembly 33, low-speed stirring assembly 43, temperature detection assembly 44, control valve 10, and vacuum drying chamber 71 are all connected to and controlled by the processor. The quantitative peristaltic pump 25, high-speed shear stirring assembly 32, ultrasonic dispersion assembly 33, low-speed stirring assembly 43, temperature detection assembly 44, control valve 10, and vacuum drying chamber 71 are all mature commercially available products, requiring detailed structural analysis. The control valve 10 is a key device in industrial automation systems used to regulate parameters such as fluid flow, pressure, and temperature. It typically consists of two parts: a valve body and an actuator. It achieves precise control by automatically changing the valve opening by receiving control signals from the processor.

[0052] The above detailed description is a specific description of feasible embodiments of the present invention. These embodiments are not intended to limit the patent scope of the present invention. All equivalent implementations or modifications that do not depart from the present invention should be included in the patent scope of this case.

Claims

1. An integrated micro / nano plastic fabrication device, characterized in that: It includes an integrated frame, which is equipped with a feeding pretreatment module, a dispersion module, a constant temperature polymerization module, a primary separation module, a purification and filtration module, a vacuum drying module, and a sealed storage module; The feed pretreatment module includes a monomer storage bottle, an initiator storage bottle and a deionized water storage bottle, and each storage bottle is connected in sequence to a filter assembly and a metering peristaltic pump. The dispersion module includes a glass dispersion tank, a high-speed shear stirring assembly, and an ultrasonic dispersion assembly. The high-speed shear stirring assembly and the ultrasonic dispersion assembly are vertically staggered and inserted into the top of the glass dispersion tank. The top side wall of the glass dispersion tank is provided with a pH detection sealing interface for inserting a pH detection device. Each quantitative peristaltic pump is connected in parallel to a closed guide pipe with a control valve. The outlet of the closed guide pipe is connected to the inlet of the glass dispersion tank. The constant temperature polymerization module includes a constant temperature water bath, a glass polymerization tank, a low-speed stirring component, and a temperature detection component; the glass polymerization tank is embedded in the constant temperature water bath, and the feed end of the glass polymerization tank is sealed to the bottom discharge end of the glass dispersion tank; the low-speed stirring component and the temperature detection component are installed on the top of the glass polymerization tank. The primary separation module includes a vertical centrifuge tube mounted on a fixed support, the inlet of which is connected to the outlet of the glass polymerization tank. The purification and filtration module includes a suspended funnel, a nanofiltration membrane assembly, and a collection beaker. The nanofiltration membrane assembly is detachably snapped onto the lower end of the suspended funnel, and the collection beaker is arranged directly below the suspended funnel. The vertical centrifuge tube is connected to the suspended funnel via a sealed guide pipe with a control valve. The inlet of the sealed guide pipe extends into the vertical centrifuge tube, and its outlet extends into the suspended funnel. The purified suspension is transferred to the vacuum drying module via the collection beaker for drying. The dried micro-nano plastic powder is then transferred to the sealed storage module.

2. The integrated micro / nano plastics fabrication device according to claim 1, characterized in that: The stirring paddle of the high-speed shear stirring assembly and the probe of the ultrasonic dispersion assembly are vertically offset inside the glass dispersion tank, with a height difference of 3cm to 5cm between them.

3. The integrated micro / nano plastic fabrication device according to claim 1, characterized in that: Both the glass dispersion tank and the glass polymerization tank have a volume of 1L to 3L, and the inner wall of the tank is smooth and free of any residue.

4. The integrated micro / nano plastics fabrication device according to claim 1, characterized in that: The bottom of the vertical centrifuge tube is detachably equipped with a waste liquid receiving tank.

5. The integrated micro / nano plastic fabrication device according to claim 1, characterized in that: The bottom of the glass dispersion tank has a conical cross-section, and its sidewalls have an inclined surface structure.

6. The integrated micro / nano plastic fabrication apparatus according to claim 5, characterized in that: The inclined surface structure forms a 15-degree angle with the central axis of the bottom discharge end of the glass dispersion tank.

7. The integrated micro / nano plastics fabrication apparatus according to claim 1, characterized in that: The glass polymerization tank is equipped with a sealed sampling port on its side wall.

8. The integrated micro / nano plastics fabrication apparatus according to claim 1, characterized in that: The vacuum drying module includes a vacuum drying chamber and a petri dish, with the petri dish placed inside the vacuum drying chamber; the purified suspension is transferred to the petri dish via the collection beaker.

9. The integrated micro / nano plastics fabrication device according to claim 1, characterized in that: The sealed storage module includes a sealed storage bottle and a sampling scraper, with the sampling scraper placed inside the sealed storage bottle; the sealed storage bottle includes a bottle body and a sealing cap placed at the bottle mouth, with a silicone sealing ring inside the sealing cap.

10. The integrated micro / nano plastic fabrication apparatus according to claim 1, characterized in that: The pH detection sealing interface is a plug-in sealing structure. In the detection state, the pH detection sealing interface is sealed and fitted to the glass dispersion tank.

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