Polymerization granulation system for bio-based material

By designing a prepolymerization reactor and mixing reactor system in bio-based material processing, controlling the polymerization reaction conditions, the problems of incomplete polymerization reaction and uneven mixing are solved, and the production of narrow high molecular weight distribution and high polymer quality is achieved. Meets the finished product quality requirements and reduces costs.

CN222131837UActive Publication Date: 2024-12-10QINGDAO PULI ELECTROMECHANICAL ENG CO LTD
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Patent Information

Application Number
CN202420246828.4
Authority / Receiving Office
CN · China
Patent Type
Utility models(China)
Current Assignee / Owner
Filing Date
2024-02-01
Publication Date
2024-12-10
Estimated Expiration
2034-02-01

AI Technical Summary

Technical Problem

In the existing bio-based material processing technology, the polymerization reaction is not thorough and the mixing is uneven, resulting in problems such as low molecular weight of the polymer, wide molecular weight distribution, product discoloration, and particle intercalation, which cannot meet the quality requirements of the finished product.

Method used

Design a polymerization granulation system including a prepolymerization reactor, a mixing reactor and a twin-screw extruder. By adding catalysts, initiators, terminators and antioxidants, the polymerization reaction conditions are controlled to achieve uniform mixing of materials and sufficient reaction. , transfer pumps and melt pumps are used to control material transmission to ensure narrow molecular weight distribution.

Benefits of technology

The production of high molecular weight polymers is achieved, with narrow molecular weight distribution, improving product yield and particle quality, simplifying system structure and operation and maintenance, and reducing construction costs.

✦ Generated by Eureka AI based on patent content.

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Abstract

The utility model discloses a polymerization granulation system for a bio-based material, and relates to the technical field of bio-based material production and processing. The device comprises a prepolymerization reaction kettle, the input end of the prepolymerization reaction kettle is connected with a material transfer pump I through a pipeline, the prepolymerization reaction kettle is provided with a catalyst adding port and an initiator adding port, the output end of the prepolymerization reaction kettle is connected with a material transfer pump II through a pipeline, the input end of the material transfer pump II is connected with a mixing reactor through a pipeline, and the mixing reactor is provided with a catalyst adding port and an initiator adding port. And the output end of the mixing reactor is in pipeline connection with a melt pump. The final product is a high polymer with the molecular weight of 12000-16000, the produced high polymer is narrow in molecular weight distribution and high in molecular weight, meanwhile, the system controls conveying of materials through the first material transfer pump, the second material transfer pump and the melt pump, the whole production system can be stably controlled, meanwhile, the number of devices needed in the system is small, and the production cost is low. The early-stage construction investment cost is reduced, and the operation and maintenance are relatively simple due to the simplified system.
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Description

Technical Field

[0001] The utility model belongs to the technical field of production and processing of bio-based materials, in particular to a polymerization granulation system for bio-based materials. Background Art

[0002] At present, under the background of global plastic restriction and low-carbon environmental protection, the processing and manufacturing of bio-based materials has received more and more attention, and the annual consumption is increasing. According to the statistics of the European Bioplastics Association, the production capacity of degradable materials is increasing at a rate of nearly 20% per year, while the demand is increasing at a rate of 30%. The products have been in short supply for a long time. The synthesis of most bio-based materials will eventually go through polymerization, extrusion granulation and other processes, but the current process is restricted by process conditions and equipment, the polymerization reaction is not thorough, the mixing is uneven, resulting in low polymer molecular weight, wide molecular weight distribution, product discoloration, and particle inclusions. The problems seriously affect the quality of the finished particles and cannot meet the requirements for the products during packaging, palletizing and warehousing. There is an urgent need for a process and system that can control the molecular weight and its distribution, the degree of polymerization, and improve the particle quality (purity and light transmittance) and yield, which will be of great significance to the production and sales of the above-mentioned bio-based materials. For this reason, we propose a polymerization granulation system for bio-based materials. Utility Model Content

[0003] The utility model aims to provide a bio-based material polymerization granulation system, which can make the materials mixed evenly and react fully through the prepolymerization reactor and the mixing reactor, so as to solve the problems that the current process is restricted by process conditions and equipment, the polymerization reaction is not thorough, the mixing is not uniform, and the polymerization results do not meet the granulation requirements, such as low polymer molecular weight, wide molecular weight distribution, product discoloration, and particles being half-cooked.

[0004] In order to solve the above technical problems, the utility model is realized by the following technical solutions:

[0005] The utility model discloses a polymerization granulation system for bio-based materials, comprising a prepolymerization reactor, wherein a pipeline at the input end of the prepolymerization reactor is connected with a material transfer pump 1, a catalyst adding port and an initiator adding port are provided on the prepolymerization reactor, a pipeline at the output end of the prepolymerization reactor is connected with a material transfer pump 2, a pipeline at the input end of the material transfer pump 2 is connected with a mixing reactor, a pipeline at the output end of the mixing reactor is connected with a melt pump, a pipeline at the output end of the melt pump is connected with a dynamic mixer, a terminator adding port and an antioxidant adding port are provided on the dynamic mixer, and a pipeline at the output end of the dynamic mixer is connected with a twin-screw extruder.

[0006] Furthermore, the catalyst added to the catalyst addition port is an acid composite compound, and the mass ratio of the catalyst to the bio-based material feed amount is 0.03% to 2%. The initiator added to the initiator addition port is dodecanol, and the mass ratio of the initiator to the bio-based material feed amount is 0.1% to 2%.

[0007] Furthermore, the terminator added to the terminator addition port is an AX-71 ester exchange inhibitor, and the mass ratio of the terminator to the bio-based material feed amount is 0.1% to 2%. The antioxidant added to the antioxidant addition port is an ANOX1315 type antioxidant, and the mass ratio of the antioxidant to the bio-based material feed amount is 0.1% to 2%.

[0008] Furthermore, the material temperature in the prepolymerization reactor is in the range of 110° C. to 150° C., and the residence time is in the range of 0.1 h to 0.5 h.

[0009] Furthermore, the mixing reactor is a uniaxial mixing reactor, the material temperature range in the mixing reactor is 150° C. to 200° C., and the residence time is 30 min to 90 min.

[0010] Furthermore, the material temperature range in the twin-screw extruder is 120°C to 200°C.

[0011] Furthermore, the material input into the first material transfer pump is a bio-based material with a purity of more than 99%.

[0012] The utility model has the following beneficial effects:

[0013] 1. The final product of the utility model is a polymer with a molecular weight of 12,000 to 16,000. The produced polymer has a narrow molecular weight distribution and a high molecular weight. At the same time, the system controls the transmission of materials through the transfer pump 1, the transfer pump 2 and the melt pump, so that the entire production system can be stably controlled. At the same time, less equipment is required in the system, which reduces the initial construction investment cost, and the streamlined system makes operation and maintenance relatively simple.

[0014] 2. When the utility model is in use, the materials are mixed evenly and reacted fully through the prepolymerization reactor and the mixing reactor, thereby avoiding the generation of dead zones in the material reaction and improving the product yield of the system.

[0015] 3. When the utility model is in use, the material inside the prepolymerization reactor can be heated and prepolymerized through the duct air heater and the heating tube. At the same time, when the stirring paddle is rotating, it can drive the arc scraper to rotate. When the arc scraper rotates, it can scrape off the material sticking to the inner wall of the shell to prevent the material sticking to the inner wall of the shell from being denatured due to long-term heating. BRIEF DESCRIPTION OF THE DRAWINGS

[0016] In order to more clearly illustrate the technical solutions of the embodiments of the present utility model, the drawings required for describing the embodiments are briefly introduced below.

[0017] Figure 1 This is a process flow chart of the utility model;

[0018] Figure 2 This is a schematic diagram of the structure of the prepolymerization reactor of the utility model;

[0019] Figure 3 This is a schematic diagram of the rear structure of the prepolymerization reactor of the utility model;

[0020] Figure 4 It is a cross-sectional view of the prepolymerization reactor of the utility model;

[0021] Figure 5 It is a structural schematic diagram of the stirring rod and the arc-shaped scraper of the utility model.

[0022] In the accompanying drawings, the components represented by the reference numerals are listed as follows:

[0023] 1. Transfer pump 1; 2. Prepolymerization reactor; 3. Mixing reactor; 4. Dynamic mixer; 5. Twin-screw extruder; 6. Melt pump; 7. Catalyst addition port; 8. Initiator addition port; 9. Terminator addition port; 10. Antioxidant addition port; 11. Transfer pump 2; 100. Connecting bottom plate; 110. Support column 1; 200. Shell; 210. Heating tube; 300. Feed tube; 310. Connection port; 320. Adding tube; 400. Stirring paddle; 410. Stirring rod; 420. Connecting block; 430. Arc scraper; 500. Motor frame; 510. Drive motor; 600. Support column 2; 610. Pipeline air heater; 620. Connecting pipe 1; 630. Connecting pipe 2; 700. Discharge pipe; 710. Valve. DETAILED DESCRIPTION

[0024] The technical solutions in the embodiments of the present invention will be described clearly and completely below in conjunction with the accompanying drawings in the embodiments of the present invention.

[0025] See also Figure 1As shown, the utility model is a bio-based material polymerization granulation system, comprising a prepolymerization reactor 2, the prepolymerization reactor 2 input end pipeline is connected to a transfer pump 1, the prepolymerization reactor 2 is provided with a catalyst addition port 7 and an initiator addition port 8, the prepolymerization reactor 2 output end pipeline is connected to a transfer pump 11, the transfer pump 11 input end pipeline is connected to a mixing reactor 3, the mixing reactor 3 output end pipeline is connected to a melt pump 6, the melt pump 6 output end pipeline is connected to a dynamic mixer 4, the dynamic mixer 4 is provided with a terminator addition port 9 and an antioxidant addition port 10, the dynamic mixer 4 output end pipeline is connected to a twin-screw extruder 5, the material input into the transfer pump 1 is a bio-based material with a purity of more than 99%, the bio-based material with a purity of more than 99% is pumped into the production system through the transfer pump 1, the catalyst added in the catalyst addition port 7 is an acid compound, and the mass ratio of the catalyst to the bio-based material feed is 0. 03% to 2%, the initiator added in the initiator addition port 8 is dodecanol, and the mass ratio of the initiator to the bio-based material feed amount is 0.1% to 2%, the material temperature range in the prepolymerization reactor 2 is 110°C to 150°C, and the residence time is 0.1h to 0.5h. The bio-based material entering the prepolymerization reactor 2 undergoes a prepolymerization reaction under the action of the acid compound and dodecanol to obtain a prepolymer with a molecular weight of 3000 to 6000, and then the prepolymer with a molecular weight of 3000 to 6000 is mixed and finalized in the mixing reactor 3 to finally obtain a polymer with a molecular weight of 12000 to 16000. The terminator added in the terminator addition port 9 is AX-71 ester exchange inhibitor, and the mass ratio of the terminator to the bio-based material feed amount is 0.1% to 2%, and the antioxidant added in the antioxidant addition port 10 is ANOX 1315 antioxidant, the mass ratio of antioxidant to bio-based material feed is 0.1% to 2%, the material temperature range in the mixing reactor 3 is 150°C to 200°C, the residence time is 30min to 90min, the polymer with a molecular weight of 12000 to 16000 in the dynamic mixer 4 is fully and uniformly mixed with the AX-71 ester exchange inhibitor and the ANOX 1315 antioxidant, and the mixed material is pushed into the feed port of the twin-screw extruder 5.

[0026] Among them Figure 2-5As shown, the prepolymerization reactor 2 includes a shell 200, a heating tube 210 for heating the inside of the shell 200 is fixedly installed around the outer wall of the shell 200, a feed pipe 300 is fixedly installed on the rear side of the upper end of the side wall of the shell 200, a connection port 310 is fixedly installed on the upper end of the outer wall of the feed pipe 300, an addition pipe 320 is fixedly installed symmetrically on the upper end of the side wall of the shell 200, a catalyst addition port 7 is fixedly installed on the upper end of the outer wall of the right addition pipe 320, and an initiator addition port 8 is fixedly installed on the upper end of the outer wall of the left addition pipe 320, a stirring paddle 400 is rotatably connected to the upper end of the inner wall of the shell 200, a stirring rod 410 is fixedly installed on the side wall of the stirring paddle 400, a connection block 420 is fixedly installed above and below the side wall of the stirring paddle 400, and the upper and lower connection blocks 420 are fixedly installed. 0, a discharge pipe 700 is fixedly installed at the lower end of the outer wall of the prepolymerization reactor 2, a valve 710 is fixedly installed on the discharge pipe 700, and the connection port 310 is connected to the pipeline at the output end of the transfer pump 1, and the material can enter the shell 200 from the feed pipe 300. The rotation of the stirring paddle 400 drives the arc scraper 430 to rotate, thereby driving the stirring rod 410 to rotate, and the material, catalyst and initiator inside the shell 200 are stirred by the rotation of the stirring rod 410. At the same time, under the action of the heating tube 210, the material inside the shell 200 can be heated, so that the material inside the shell 200 undergoes a prepolymerization reaction, and when the stirring paddle 400 is rotating, it can drive the arc scraper 430 to rotate. 0 rotates, and the arc scraper 430 can scrape off the materials sticking to the inner wall of the shell 200 when rotating, so as to prevent the materials sticking to the inner wall of the shell 200 from being denatured due to long-term heating. The lower end of the outer wall of the prepolymerization reactor 2 is fixedly installed with a support column 110, and the lower end of the outer wall of the support column 110 is fixedly installed with a connecting bottom plate 100, and the upper end of the outer wall of the connecting bottom plate 100 is fixedly installed with a support column 2 600, and the upper end of the outer wall of the support column 2 600 is fixedly installed with a duct air heater 610, and the output end of the duct air heater 610 is fixedly installed with a connecting pipe 1 620, and the upper end of the outer wall of the connecting pipe 1 620 is fixedly connected to the lower end of the outer wall of the heating pipe 210, and the input end of the duct air heater 610 is fixedly installed with a connecting pipe 2 630, and the connecting pipe 2 630 is fixedly installed with the connecting pipe 2 630. 0 The upper end of the outer wall is fixedly connected to the upper end of the outer wall of the heating tube 210. The duct air heater 610 adopts the XTGD-800 duct air heater. The duct air heater 610 can circulate and heat the air in the heating tube 210. The motor frame 500 is fixedly installed on the upper end of the outer wall of the prepolymerization reactor 2. The drive motor 510 is fixedly installed on the motor frame 500. The output end of the drive motor 510 passes through the upper end of the inner wall of the prepolymerization reactor 2 and is fixedly connected to the stirring paddle 400. The stirring paddle 400 is rotated by starting the drive motor 510, and the material can enter the shell 200 from the feed pipe 300. The stirring paddle 400 is rotated by starting the drive motor 510. The arc scraper 430 is driven to rotate by the rotation of the rod stirring paddle 400.Thus, the stirring rod 410 is driven to rotate, and the materials, catalysts and initiators inside the shell 200 are stirred by the rotation of the stirring rod 410. At the same time, the air in the heating tube 210 can be circulated and heated by the duct air heater 610. Under the action of the heating tube 210, the materials inside the shell 200 can be heated, so that the materials inside the shell 200 undergo a prepolymerization reaction. When the stirring paddle 400 rotates, the arc scraper 430 can be driven to rotate, and the arc scraper 430 can scrape the materials sticking to the inner wall of the shell 200 when rotating.

[0027] A specific application of this embodiment is as follows: when in use, first, a bio-based material with a purity of more than 99% is pumped into the production system through a transfer pump 1, and the bio-based material is pumped into a prepolymerization reactor 2 through a transfer pump 1, and the bio-based material entering the prepolymerization reactor 2 undergoes a prepolymerization reaction under the action of the acid compound and dodecanol to obtain a prepolymer with a molecular weight of 3000 to 6000, and then the prepolymer with a molecular weight of 3000 to 6000 is mixed and subjected to a final polymerization reaction in a mixing reactor 3 to finally obtain a high polymer with a molecular weight of 12000 to 16000, and the high polymer with a molecular weight of 12000 to 16000 is transported to a dynamic mixer 4 through a melt pump 6, and the high polymer with a molecular weight of 12000 to 16000 in the dynamic mixer 4 is mixed with the AX-71 ester exchange inhibitor and the ANOX The 1315 type antioxidant is fully and evenly mixed, and the mixed material is pushed into the feed port of the twin-screw extruder 5. The material temperature range in the twin-screw extruder 5 is 120°C to 200°C. The high molecular polymer entering therein is extruded, devolatilized, and granulated by the twin-screw extruder 5.

[0028] Attached Figure 2 and attached Figure 3 The heating method of the duct air heater 610 is one of many heating methods. Other heating methods, such as using a mold temperature controller, a gas furnace, or electric heating, are also suitable for the heating method of this system. Figure 3 and attached Figure 4 The heating pipe 210 can be in the form of a heating jacket or an inner / outer coil, and heat transfer oil or steam is passed through the interior to heat the material. Figure 4 and attached Figure 5 The stirring rod 410, the connecting block 420, and the arc-shaped scraper 430 are only for illustration in this example and do not represent their specific structures. In practical applications, stirring rods, connecting blocks, or scrapers of other shapes with different forms and functions can be designed according to the specific characteristics of different materials and the requirements of the process system to meet the mixing and reaction requirements of different process systems.

[0029] In addition, it is not excluded to add other types of catalysts, initiators, terminators and antioxidants to the system. The above reagents described in the utility model are only preferred recommendations for the bio-based materials. Other reagents that are more suitable for the bio-based materials may appear in the future, which is not limited here. Other better reagents obtained in subsequent experiments, as long as their functions are similar, also fall within the protection scope of the utility model.

[0030] The above are only preferred embodiments of the present invention and do not limit the present invention. Any modification to the technical solutions recorded in the aforementioned embodiments and any equivalent replacement of some of the technical features therein, any modification, equivalent replacement, and improvement made are all within the protection scope of the present invention.

Claims

1. A bio-based material polymerization granulation system, comprising a prepolymerization reactor (2), characterized in that: The input end pipeline of the prepolymerization reactor (2) is connected to a transfer pump (1), the prepolymerization reactor (2) is provided with a catalyst addition port (7) and an initiator addition port (8), the output end pipeline of the prepolymerization reactor (2) is connected to a transfer pump (11), the input end pipeline of the transfer pump (11) is connected to a mixing reactor (3), the output end pipeline of the mixing reactor (3) is connected to a melt pump (6), the output end pipeline of the melt pump (6) is connected to a dynamic mixer (4), the dynamic mixer (4) is provided with a terminator addition port (9) and an antioxidant addition port (10), and the output end pipeline of the dynamic mixer (4) is connected to a twin-screw extruder (5).

2. The bio-based material polymerization granulation system according to claim 1, characterized in that: The catalyst added to the catalyst addition port (7) is an acid compound, and the mass ratio of the catalyst to the bio-based material feed is 0.03% to 2%. The initiator added to the initiator addition port (8) is dodecanol, and the mass ratio of the initiator to the bio-based material feed is 0.1% to 2%.

3. The bio-based material polymerization granulation system according to claim 1, characterized in that: The terminator added to the terminator addition port (9) is an AX-71 transesterification inhibitor, and the mass ratio of the terminator to the bio-based material feed amount is 0.1% to 2%. The antioxidant added to the antioxidant addition port (10) is an ANOX 1315 type antioxidant, and the mass ratio of the antioxidant to the bio-based material feed amount is 0.1% to 2%.

4. The bio-based material polymerization granulation system according to claim 1, characterized in that: The material temperature in the prepolymerization reactor (2) is in the range of 110° C. to 150° C., and the residence time is in the range of 0.1 h to 0.5 h.

5. The bio-based material polymerization granulation system according to claim 1, characterized in that: The mixing reactor (3) is a single-shaft mixing reactor. The temperature range of the materials in the mixing reactor (3) is 150° C. to 200° C., and the residence time is 30 min to 90 min.

6. The bio-based material polymerization granulation system according to claim 1, characterized in that: The temperature range of the material in the twin-screw extruder (5) is 120°C to 200°C.

7. The bio-based material polymerization granulation system according to claim 1, characterized in that: The prepolymerization reactor (2) comprises a shell (200), a heating pipe (210) for heating the interior of the shell (200) is fixedly installed around the outer wall of the shell (200), a feed pipe (300) is fixedly installed on the rear side of the upper end of the side wall of the shell (200), a connection port (310) is fixedly installed on the upper end of the outer wall of the feed pipe (300), and an addition pipe (320) is fixedly installed on the upper end of the side wall of the shell (200) in a left-right symmetrical manner, the catalyst addition port (7) is fixedly installed on the upper end of the outer wall of the addition pipe (320) on the right side, and the catalyst addition port (7) is fixedly installed on the upper end of the outer wall of the addition pipe (320) on the left side. The initiator addition port (8) is fixedly installed on the upper end of the outer wall of the shell (200), a stirring paddle (400) is rotatably connected to the upper end of the inner wall of the shell (200), a stirring rod (410) is fixedly installed on the side wall of the stirring paddle (400), a connecting block (420) is fixedly installed above and below the side wall of the stirring paddle (400), an arc-shaped scraper (430) is fixedly installed between the upper and lower connecting blocks (420), a discharge pipe (700) is fixedly installed on the lower end of the outer wall of the prepolymerization reactor (2), and a valve (710) is fixedly installed on the discharge pipe (700).

8. The bio-based material polymerization granulation system according to claim 7, characterized in that: The lower end of the outer wall of the prepolymerization reactor (2) is fixedly mounted with a support column 1 (110), the lower end of the outer wall of the support column 1 (110) is fixedly mounted with a connecting base plate (100), the upper end of the outer wall of the connecting base plate (100) is fixedly mounted with a support column 2 (600), the upper end of the outer wall of the support column 2 (600) is fixedly mounted with a duct air heater (610), the output end of the duct air heater (610) is fixedly mounted with a connecting pipe 1 (620), the upper end of the outer wall of the connecting pipe 1 (620) is fixedly connected to the lower end of the outer wall of the heating pipe (210), the input end of the duct air heater (610) is fixedly mounted with a connecting pipe 2 (630), the upper end of the outer wall of the connecting pipe 2 (630) is fixedly connected to the upper end of the outer wall of the heating pipe (210).

9. The bio-based material polymerization granulation system according to claim 7, characterized in that: A motor frame (500) is fixedly mounted on the upper end of the outer wall of the prepolymerization reactor (2), a driving motor (510) is fixedly mounted on the motor frame (500), and an output end of the driving motor (510) passes through the upper end of the inner wall of the prepolymerization reactor (2) and is fixedly connected to the stirring paddle (400).

Citation Information

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