Polymer based on cucurbituril structure and synthesis method thereof

By adopting strict purification treatment and controlling reaction conditions in polymer synthesis, the problems of impurities interference and irreconcilable structure during polymer synthesis in the prior art are solved, and high-quality and efficient polymer preparation is achieved, and the performance and structure of the polymer can be adjusted according to needs.

CN119798519APending Publication Date: 2025-04-11SUZHOU HENGRUN COMMODITY INSPECTION CO LTD
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Patent Information

Application Number
CN202411820304.2
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2024-12-11
Publication Date
2025-04-11

AI Technical Summary

Technical Problem

The existing polymers based on the cucurbit urea structure are difficult to reduce impurity interference during the synthesis process, resulting in the impact of the finished product accuracy and the structure is irreconcilable, so that polymers that meet the requirements cannot be prepared according to the requirements.

Method used

The polymer synthesis method including cucurbita, functional monomer, initiator, chain transfer agent, solvent, ether and precipitant is adopted. Through strict purification treatment and control of reaction conditions, the purity of the reaction raw materials is ensured and the structure of the polymer is adjusted.

Benefits of technology

It improves the selectivity of the polymerization reaction and the quality of the polymer, reduces the interference of impurities on the reaction, and can synthesize polymers with different properties and structures according to specific needs, meeting the requirements of different application scenarios.

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Abstract

The invention discloses a cucurbituril structure-based polymer and a synthesis method thereof, and relates to the field of cucurbituril structure-based polymers, and the cucurbituril structure-based polymer comprises cucurbituril, a functional monomer, an initiator, a chain transfer agent, a solvent, diethyl ether and a precipitator. According to the polymer based on the cucurbituril structure and the synthesis method of the polymer, the polymer based on the cucurbituril structure and having better structure and performance can be prepared through the detailed synthesis method and characterization analysis means, cucurbituril, monomers, an initiator and a chain transfer agent are strictly purified, and the preparation method is simple and easy to implement. The purity of reaction raw materials can be ensured, the reaction selectivity and the polymer quality can be improved, the interference of impurities on the polymerization reaction is reduced, and selection of various functional monomers, initiators and chain transfer agents is provided in the aspect of raw material selection; the cucurbituril structure-based polymers with different properties and structures can be synthesized according to specific requirements.
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Description

Technical Field

[0001] The invention relates to the field of polymers based on cucurbituril structures, and in particular to a polymer based on cucurbituril structures and a synthesis method thereof. Background Art

[0002] Cucurbituril-based polymers are a type of high-molecular compound constructed through various chemical reactions using cucurbituril as the basic structural unit. Cucurbituril is a barrel-shaped macrocyclic compound composed of glycoside urea units connected by methylene groups. It has a hydrophobic cavity and a hydrophilic carbonyl port. The size of the cavity varies with the number of glycoside urea units, and the structure has strong rigidity.

[0003] When synthesizing polymers based on cucurbituril structures, the interference of impurities on the polymerization reaction cannot be reduced, resulting in a certain impact on the accuracy of the finished product, and the structure is not adjustable, so that a polymer that meets the requirements cannot be prepared according to the use requirements. Summary of the invention

[0004] The main purpose of the present invention is to provide a polymer based on a cucurbituril structure and a synthesis method thereof, which can effectively solve the problems in the background technology.

[0005] To achieve the above object, the technical solution adopted by the present invention is:

[0006] A polymer based on cucurbituril structure comprises cucurbituril, functionalized monomer, initiator, chain transfer agent, solvent, ether and precipitant.

[0007] Preferably, the purity of the cucurbituril is greater than 95%; the functional monomers include but are not limited to acrylate monomers and acrylamide monomers, and the acrylate monomers and acrylamide monomers are both required to be purified by vacuum distillation to remove impurities, wherein the acrylate monomers include but are not limited to methyl methacrylate MMA and ethyl acrylate EA, and the acrylamide monomer is N,N-dimethylacrylamide DMAA; the initiator includes but is not limited to azobisisobutyronitrile, potassium persulfate, and a redox initiator system, and the initiator is recrystallized and purified before use; the chain transfer agent is dodecyl trithiocarbonate, and the purity is greater than 98%; the solvent is selected to have good solubility for the monomer, cucurbituril and initiator, including but not limited to N,N-dimethylformamide, dimethyl sulfoxide, and water, and the solvent is dried with anhydrous calcium chloride and then distilled for use; the precipitant is but not limited to methanol and n-hexane.

[0008] A method for synthesizing a polymer based on a cucurbituril structure comprises the following steps:

[0009] S1: Prepare materials, including cucurbituril, functional monomer, initiator, chain transfer agent, solvent, and precipitant;

[0010] S2: Prepare instruments, three-necked flask: equipped with thermometer, condenser and magnetic stirring device, used for setting up the reaction system and carrying out the reaction process; constant temperature water bath: used to accurately control the reaction temperature, the temperature control accuracy is within the range of ±1°C, used to provide a stable temperature environment for the polymerization reaction; magnetic stirrer; vacuum pump: used to decompress the reaction system; gel permeation chromatograph: used to determine the molecular weight and distribution of the polymer; nuclear magnetic resonance spectrometer: used to characterize the structure of the polymer; vacuum drying oven; thermogravimetric analyzer and differential scanning calorimeter;

[0011] S3: Preparation of cucurbituril functionalized monomers, dissolving cucurbituril in a dry solvent, stirring with a magnetic stirrer at room temperature until completely dissolved to form a cucurbituril solution, the concentration of which is controlled between 0.1-0.5 mol / L, slowly dropping the functionalized monomer into the cucurbituril solution, stirring under nitrogen protection, the molar ratio of the functionalized monomer to the cucurbituril being 1:1, after the addition is complete, heating the reaction system to 50-80°C, continuing to stir the reaction for 36 hours, after the reaction is completed, cooling the reaction solution to room temperature, and then precipitating in ether, collecting the precipitate and drying it in a vacuum drying oven to obtain the cucurbituril functionalized monomer, the yield being between 60% and 90%;

[0012] S4: Synthesis of polymer based on cucurbituril structure: in a dry three-necked flask, add purified cucurbituril functionalized monomer, functionalized monomer, chain transfer agent and initiator in sequence, the total monomer concentration is controlled at 2-5 mol / L, the molar ratio of cucurbituril functionalized monomer to ordinary monomer is 1:10, the molar ratio of chain transfer agent to initiator is 1:1, the amount of initiator is 2% of the total mass of monomer, fill the three-necked flask with nitrogen or argon to remove oxygen in the system, then seal it, place the three-necked flask in a constant temperature water bath, raise the temperature to 60-90°C, start the polymerization reaction, during the reaction , the reaction system is kept uniformly mixed by a magnetic stirrer, and the stirring speed is controlled at 300-800 rpm. After the reaction is carried out for 16 hours, the heating is stopped, the reaction system is cooled to room temperature, and the reaction solution is slowly added dropwise to a large amount of precipitant to precipitate the polymer, and then the polymer precipitate is collected by suction filtration using a Buchner funnel, and the polymer precipitate is washed 2-3 times with a small amount of precipitant to remove residual monomers and impurities, and finally the polymer is placed in a vacuum drying oven and dried at 40-60° C. to constant weight to obtain a polymer based on a cucurbituril structure with a yield of 70%-95%;

[0013] S5: Characterization and analysis of polymers, determination of molecular weight and molecular weight distribution: The molecular weight and molecular weight distribution of the synthesized polymers were determined using a gel permeation chromatograph, with a water-insoluble polymer as the mobile phase, the flow rate set at 1.0 mL / min, and the column temperature maintained at 30-40 °C. The number average molecular weight, weight average molecular weight and molecular weight distribution index of the polymers were calculated by comparison with standard polymers of known molecular weight;

[0014] Structural characterization: The structure of the polymer was characterized by using a nuclear magnetic resonance spectrometer. The polymer was dissolved in deuterated chloroform and deuterated water, and hydrogen and carbon spectra were tested. By analyzing the chemical shift, integrated area and splitting of each peak in the spectrum, the structural composition of the polymer was determined, and it was verified whether the cucurbituril structure was successfully introduced into the polymer, as well as the polymerization mode and ratio information of the monomers;

[0015] Thermal performance analysis: The thermal properties of polymers are studied using thermogravimetric analyzers and differential scanning calorimeters. In the TGA test, polymer samples are heated from room temperature to 800°C at a heating rate of 10-20°C / min in a nitrogen atmosphere, and the curve of the mass change with temperature is recorded to determine the thermal decomposition temperature and thermal stability of the polymer. In the DSC test, the test is also carried out in a nitrogen atmosphere at a heating rate of 5-10°C / min to observe the glass transition temperature and melting point of the polymer and understand the thermal performance characteristics of the polymer.

[0016] Compared with the prior art, the present invention has the following beneficial effects:

[0017] In the present invention, a cucurbituril structure-based polymer with better structure and performance can be prepared through a detailed synthesis method and characterization and analysis means. Cucurbituril, monomer, initiator and chain transfer agent are strictly purified to ensure the purity of the reaction raw materials, which is beneficial to improving the selectivity of the reaction and the quality of the polymer, and reducing the interference of impurities on the polymerization reaction. In terms of raw material selection, a variety of functionalized monomers and initiators and chain transfer agents are provided for selection, and cucurbituril structure-based polymers with different properties and structures can be synthesized according to specific needs. In the preparation process of cucurbituril functionalized monomers, the reaction solvent, temperature, time, and reactant ratio are specified in detail, and the degree of cucurbituril functionalization can be effectively adjusted, thereby accurately designing the structure of the polymer to meet the requirements of polymer performance in different application scenarios. DETAILED DESCRIPTION

[0018] The following will be combined with the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0019] A polymer based on cucurbituril structure comprises cucurbituril, functionalized monomer, initiator, chain transfer agent, solvent, ether and precipitant.

[0020] The purity of cucurbituril is greater than 95%; the functional monomers include but are not limited to acrylate monomers and acrylamide monomers, and both acrylate monomers and acrylamide monomers need to be purified by vacuum distillation to remove impurities, wherein acrylate monomers include but are not limited to methyl methacrylate MMA and ethyl acrylate EA, and acrylamide monomers are N,N-dimethylacrylamide DMAA; the initiator includes but is not limited to azobisisobutyronitrile, potassium persulfate, and redox initiator system, and the initiator is recrystallized and purified before use; the chain transfer agent is dodecyl trithiocarbonate, and the purity is greater than 98%; the solvent is selected to have good solubility for the monomer, cucurbituril and initiator, including but not limited to N,N-dimethylformamide, dimethyl sulfoxide, and water, and the solvent is dried with anhydrous calcium chloride and then distilled for use; the precipitant is but not limited to methanol and n-hexane.

[0021] A method for synthesizing a polymer based on a cucurbituril structure comprises the following steps:

[0022] S1: Prepare materials, including cucurbituril, functional monomer, initiator, chain transfer agent, solvent, and precipitant;

[0023] S2: Prepare instruments, three-necked flask: equipped with thermometer, condenser and magnetic stirring device, used for setting up the reaction system and carrying out the reaction process; constant temperature water bath: used to accurately control the reaction temperature, the temperature control accuracy is within the range of ±1°C, used to provide a stable temperature environment for the polymerization reaction; magnetic stirrer; vacuum pump: used to decompress the reaction system; gel permeation chromatograph: used to determine the molecular weight and distribution of the polymer; nuclear magnetic resonance spectrometer: used to characterize the structure of the polymer; vacuum drying oven; thermogravimetric analyzer and differential scanning calorimeter;

[0024] S3: Preparation of cucurbituril functionalized monomers, dissolving cucurbituril in a dry solvent, stirring with a magnetic stirrer at room temperature until completely dissolved to form a cucurbituril solution, the concentration of which is controlled between 0.1-0.5 mol / L, slowly dropping the functionalized monomer into the cucurbituril solution, stirring under nitrogen protection, the molar ratio of the functionalized monomer to the cucurbituril being 1:1, after the addition is complete, heating the reaction system to 50-80°C, continuing to stir the reaction for 36 hours, after the reaction is completed, cooling the reaction solution to room temperature, and then precipitating in ether, collecting the precipitate and drying it in a vacuum drying oven to obtain the cucurbituril functionalized monomer, the yield being between 60% and 90%;

[0025] S4: Synthesis of polymer based on cucurbituril structure: in a dry three-necked flask, add purified cucurbituril functionalized monomer, functionalized monomer, chain transfer agent and initiator in sequence, the total monomer concentration is controlled at 2-5 mol / L, the molar ratio of cucurbituril functionalized monomer to ordinary monomer is 1:10, the molar ratio of chain transfer agent to initiator is 1:1, the amount of initiator is 2% of the total mass of monomer, fill the three-necked flask with nitrogen or argon to remove oxygen in the system, then seal it, place the three-necked flask in a constant temperature water bath, raise the temperature to 60-90°C, start the polymerization reaction, during the reaction , the reaction system is kept uniformly mixed by a magnetic stirrer, and the stirring speed is controlled at 300-800 rpm. After the reaction is carried out for 16 hours, the heating is stopped, the reaction system is cooled to room temperature, and the reaction solution is slowly added dropwise to a large amount of precipitant to precipitate the polymer, and then the polymer precipitate is collected by suction filtration using a Buchner funnel, and the polymer precipitate is washed 2-3 times with a small amount of precipitant to remove residual monomers and impurities, and finally the polymer is placed in a vacuum drying oven and dried at 40-60° C. to constant weight to obtain a polymer based on a cucurbituril structure with a yield of 70%-95%;

[0026] S5: Characterization and analysis of polymers, determination of molecular weight and molecular weight distribution: The molecular weight and molecular weight distribution of the synthesized polymers were determined using a gel permeation chromatograph, with a water-insoluble polymer as the mobile phase, the flow rate set at 1.0 mL / min, and the column temperature maintained at 30-40 °C. The number average molecular weight, weight average molecular weight and molecular weight distribution index of the polymers were calculated by comparison with standard polymers of known molecular weight;

[0027] Structural characterization: The structure of the polymer was characterized by using a nuclear magnetic resonance spectrometer. The polymer was dissolved in deuterated chloroform and deuterated water, and hydrogen and carbon spectra were tested. By analyzing the chemical shift, integrated area and splitting of each peak in the spectrum, the structural composition of the polymer was determined, and it was verified whether the cucurbituril structure was successfully introduced into the polymer, as well as the polymerization mode and ratio information of the monomers;

[0028] Thermal performance analysis: The thermal properties of polymers are studied using thermogravimetric analyzers and differential scanning calorimeters. In the TGA test, polymer samples are heated from room temperature to 800°C at a heating rate of 10-20°C / min in a nitrogen atmosphere, and the curve of the mass change with temperature is recorded to determine the thermal decomposition temperature and thermal stability of the polymer. In the DSC test, the test is also carried out in a nitrogen atmosphere at a heating rate of 5-10°C / min to observe the glass transition temperature and melting point of the polymer and understand the thermal performance characteristics of the polymer. Specific embodiment one:

[0030] A polymer based on cucurbituril structure comprises cucurbituril, functionalized monomer, initiator, chain transfer agent, solvent, ether and precipitant.

[0031] The purity of cucurbituril is greater than 95%; the functional monomer is an acrylate monomer, and the acrylamide monomer is purified by reduced pressure distillation to remove impurities, wherein the acrylate monomer is methyl methacrylate MMA; the initiator is azobisisobutyronitrile, and the initiator is recrystallized and purified before use; the chain transfer agent is dodecyl trithiocarbonate, and the purity is greater than 98%; the solvent is N,N-dimethylformamide, which is dried over anhydrous calcium chloride and then distilled for use; the precipitant is methanol.

[0032] A method for synthesizing a polymer based on a cucurbituril structure comprises the following steps:

[0033] S1: Prepare materials, including cucurbituril, functional monomer, initiator, chain transfer agent, solvent, and precipitant;

[0034] S2: Prepare instruments, three-necked flask: equipped with thermometer, condenser and magnetic stirring device, used for setting up the reaction system and carrying out the reaction process; constant temperature water bath: used to accurately control the reaction temperature, the temperature control accuracy is within the range of ±1°C, used to provide a stable temperature environment for the polymerization reaction; magnetic stirrer; vacuum pump: used to decompress the reaction system; gel permeation chromatograph: used to determine the molecular weight and distribution of the polymer; nuclear magnetic resonance spectrometer: used to characterize the structure of the polymer; vacuum drying oven; thermogravimetric analyzer and differential scanning calorimeter;

[0035] S3: Preparation of cucurbituril functionalized monomers, dissolving cucurbituril in a dry solvent, stirring with a magnetic stirrer at room temperature until completely dissolved to form a cucurbituril solution, the concentration of which is controlled between 0.1-0.5 mol / L, slowly dropping the functionalized monomer into the cucurbituril solution, stirring under nitrogen protection, the molar ratio of the functionalized monomer to the cucurbituril being 1:1, after the addition is complete, heating the reaction system to 50-80°C, continuing to stir the reaction for 36 hours, after the reaction is completed, cooling the reaction solution to room temperature, and then precipitating in ether, collecting the precipitate and drying it in a vacuum drying oven to obtain the cucurbituril functionalized monomer, the yield being between 60% and 90%;

[0036] S4: Synthesis of polymer based on cucurbituril structure: in a dry three-necked flask, add purified cucurbituril functionalized monomer, functionalized monomer, chain transfer agent and initiator in sequence, the total monomer concentration is controlled at 2-5 mol / L, the molar ratio of cucurbituril functionalized monomer to ordinary monomer is 1:10, the molar ratio of chain transfer agent to initiator is 1:1, the amount of initiator is 2% of the total mass of monomer, fill the three-necked flask with nitrogen or argon to remove oxygen in the system, then seal it, place the three-necked flask in a constant temperature water bath, raise the temperature to 60-90°C, start the polymerization reaction, during the reaction , the reaction system is kept uniformly mixed by a magnetic stirrer, and the stirring speed is controlled at 300-800 rpm. After the reaction is carried out for 16 hours, the heating is stopped, the reaction system is cooled to room temperature, and the reaction solution is slowly added dropwise to a large amount of precipitant to precipitate the polymer, and then the polymer precipitate is collected by suction filtration using a Buchner funnel, and the polymer precipitate is washed 2-3 times with a small amount of precipitant to remove residual monomers and impurities, and finally the polymer is placed in a vacuum drying oven and dried at 40-60° C. to constant weight to obtain a polymer based on a cucurbituril structure with a yield of 70%-95%;

[0037] S5: Characterization and analysis of polymers, determination of molecular weight and molecular weight distribution: The molecular weight and molecular weight distribution of the synthesized polymers were determined using a gel permeation chromatograph, with a water-insoluble polymer as the mobile phase, the flow rate set at 1.0 mL / min, and the column temperature maintained at 30-40 °C. The number average molecular weight, weight average molecular weight and molecular weight distribution index of the polymers were calculated by comparison with standard polymers of known molecular weight;

[0038] Structural characterization: The structure of the polymer was characterized by using a nuclear magnetic resonance spectrometer. The polymer was dissolved in deuterated chloroform and deuterated water, and hydrogen and carbon spectra were tested. By analyzing the chemical shift, integrated area and splitting of each peak in the spectrum, the structural composition of the polymer was determined, and it was verified whether the cucurbituril structure was successfully introduced into the polymer, as well as the polymerization mode and ratio information of the monomers;

[0039] Thermal performance analysis: The thermal properties of polymers are studied using thermogravimetric analyzers and differential scanning calorimeters. In the TGA test, polymer samples are heated from room temperature to 800°C at a heating rate of 10-20°C / min in a nitrogen atmosphere, and the curve of the mass change with temperature is recorded to determine the thermal decomposition temperature and thermal stability of the polymer. In the DSC test, the test is also carried out in a nitrogen atmosphere at a heating rate of 5-10°C / min to observe the glass transition temperature and melting point of the polymer and understand the thermal performance characteristics of the polymer. Specific embodiment 2:

[0041] A polymer based on cucurbituril structure comprises cucurbituril, functionalized monomer, initiator, chain transfer agent, solvent, ether and precipitant.

[0042] The purity of cucurbituril is greater than 95%; the functional monomer is acrylamide monomer, which is purified by vacuum distillation to remove impurities, wherein N,N-dimethylacrylamide DMAA is selected as the acrylamide monomer; the initiator is a redox initiator system, which is recrystallized and purified before use; the chain transfer agent is dodecyl trithiocarbonate, and the purity is greater than 98%; the solvent is dimethyl sulfoxide, which is dried with anhydrous calcium chloride and then distilled for standby use; the precipitant is n-hexane.

[0043] A method for synthesizing a polymer based on a cucurbituril structure comprises the following steps:

[0044] S1: Prepare materials, including cucurbituril, functional monomer, initiator, chain transfer agent, solvent, and precipitant;

[0045] S2: Prepare instruments, three-necked flask: equipped with thermometer, condenser and magnetic stirring device, used for setting up the reaction system and carrying out the reaction process; constant temperature water bath: used to accurately control the reaction temperature, the temperature control accuracy is within the range of ±1°C, used to provide a stable temperature environment for the polymerization reaction; magnetic stirrer; vacuum pump: used to decompress the reaction system; gel permeation chromatograph: used to determine the molecular weight and distribution of the polymer; nuclear magnetic resonance spectrometer: used to characterize the structure of the polymer; vacuum drying oven; thermogravimetric analyzer and differential scanning calorimeter;

[0046] S3: Preparation of cucurbituril functionalized monomers, dissolving cucurbituril in a dry solvent, stirring with a magnetic stirrer at room temperature until completely dissolved to form a cucurbituril solution, the concentration of which is controlled between 0.1-0.5 mol / L, slowly dropping the functionalized monomer into the cucurbituril solution, stirring under nitrogen protection, the molar ratio of the functionalized monomer to the cucurbituril being 1:1, after the addition is complete, heating the reaction system to 50-80°C, continuing to stir the reaction for 36 hours, after the reaction is completed, cooling the reaction solution to room temperature, and then precipitating in ether, collecting the precipitate and drying it in a vacuum drying oven to obtain the cucurbituril functionalized monomer, the yield being between 60% and 90%;

[0047] S4: Synthesis of polymer based on cucurbituril structure: in a dry three-necked flask, add purified cucurbituril functionalized monomer, functionalized monomer, chain transfer agent and initiator in sequence, the total monomer concentration is controlled at 2-5 mol / L, the molar ratio of cucurbituril functionalized monomer to ordinary monomer is 1:10, the molar ratio of chain transfer agent to initiator is 1:1, the amount of initiator is 2% of the total mass of monomer, fill the three-necked flask with nitrogen or argon to remove oxygen in the system, then seal it, place the three-necked flask in a constant temperature water bath, raise the temperature to 60-90°C, start the polymerization reaction, during the reaction , the reaction system is kept uniformly mixed by a magnetic stirrer, and the stirring speed is controlled at 300-800 rpm. After the reaction is carried out for 16 hours, the heating is stopped, the reaction system is cooled to room temperature, and the reaction solution is slowly added dropwise to a large amount of precipitant to precipitate the polymer, and then the polymer precipitate is collected by suction filtration using a Buchner funnel, and the polymer precipitate is washed 2-3 times with a small amount of precipitant to remove residual monomers and impurities, and finally the polymer is placed in a vacuum drying oven and dried at 40-60° C. to constant weight to obtain a polymer based on a cucurbituril structure with a yield of 70%-95%;

[0048] S5: Characterization and analysis of polymers, determination of molecular weight and molecular weight distribution: The molecular weight and molecular weight distribution of the synthesized polymers were determined using a gel permeation chromatograph, with a water-insoluble polymer as the mobile phase, the flow rate set at 1.0 mL / min, and the column temperature maintained at 30-40 °C. The number average molecular weight, weight average molecular weight and molecular weight distribution index of the polymers were calculated by comparison with standard polymers of known molecular weight;

[0049] Structural characterization: The structure of the polymer was characterized by using a nuclear magnetic resonance spectrometer. The polymer was dissolved in deuterated chloroform and deuterated water, and hydrogen and carbon spectra were tested. By analyzing the chemical shift, integrated area and splitting of each peak in the spectrum, the structural composition of the polymer was determined, and it was verified whether the cucurbituril structure was successfully introduced into the polymer, as well as the polymerization mode and ratio information of the monomers;

[0050] Thermal performance analysis: The thermal properties of polymers are studied using thermogravimetric analyzers and differential scanning calorimeters. In the TGA test, polymer samples are heated from room temperature to 800°C at a heating rate of 10-20°C / min in a nitrogen atmosphere, and the curve of the mass change with temperature is recorded to determine the thermal decomposition temperature and thermal stability of the polymer. In the DSC test, the test is also carried out in a nitrogen atmosphere at a heating rate of 5-10°C / min to observe the glass transition temperature and melting point of the polymer and understand the thermal performance characteristics of the polymer.

[0051] The performance of the polymer prepared by the present invention and the polymer prepared by the prior art are compared, wherein the present invention is recorded as Examples 1-2, and the prior art is recorded as Comparative Example 1. The following is a comparison table:

[0052]

[0053]

[0054] This shows that the polymer prepared by the present invention has excellent performance.

[0055] In the present invention, a cucurbituril structure-based polymer with better structure and performance can be prepared through a detailed synthesis method and characterization and analysis means. Cucurbituril, monomer, initiator and chain transfer agent are strictly purified to ensure the purity of the reaction raw materials, which is beneficial to improving the selectivity of the reaction and the quality of the polymer, and reducing the interference of impurities on the polymerization reaction. In terms of raw material selection, a variety of functionalized monomers and initiators and chain transfer agents are provided for selection, and cucurbituril structure-based polymers with different properties and structures can be synthesized according to specific needs. In the preparation process of cucurbituril functionalized monomers, the reaction solvent, temperature, time, and reactant ratio are specified in detail, and the degree of cucurbituril functionalization can be effectively adjusted, thereby accurately designing the structure of the polymer to meet the requirements of polymer performance in different application scenarios.

[0056] Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions and variations may be made to the embodiments without departing from the principles and spirit of the present invention, and that the scope of the present invention is defined by the appended claims and their equivalents.

Claims

1. A polymer based on a cucurbituril structure, characterized in that: The invention comprises cucurbituril, functionalized monomer, initiator, chain transfer agent, solvent, ether and precipitant.

2. A cucurbituril structure-based polymer according to claim 1, characterized in that: The purity of the cucurbituril is greater than 95%; the functional monomers include but are not limited to acrylate monomers and acrylamide monomers, and the acrylate monomers and acrylamide monomers are both required to be purified by reduced pressure distillation to remove impurities, wherein the acrylate monomers include but are not limited to methyl methacrylate MMA and ethyl acrylate EA, and the acrylamide monomer is N,N-dimethylacrylamide DMAA; the initiator includes but is not limited to azobisisobutyronitrile, potassium persulfate, and a redox initiator system, and the initiator is recrystallized and purified before use; the chain transfer agent is dodecyl trithiocarbonate, and the purity is greater than 98%; the solvent is selected to have good solubility for the monomer, cucurbituril and initiator, including but not limited to N,N-dimethylformamide, dimethyl sulfoxide, and water, and the solvent is dried with anhydrous calcium chloride and then distilled for use; the precipitant is but not limited to methanol and n-hexane.

3. The method for synthesizing a cucurbituril-based polymer according to claim 1, characterized in that: The steps include: S1: Prepare materials, including cucurbituril, functional monomer, initiator, chain transfer agent, solvent, and precipitant; S2: Prepare instruments, three-necked flask: equipped with thermometer, condenser and magnetic stirring device, used for setting up the reaction system and carrying out the reaction process; constant temperature water bath: used to accurately control the reaction temperature, the temperature control accuracy is within the range of ±1°C, used to provide a stable temperature environment for the polymerization reaction; magnetic stirrer; vacuum pump: used to decompress the reaction system; gel permeation chromatograph: used to determine the molecular weight and distribution of the polymer; nuclear magnetic resonance spectrometer: used to characterize the structure of the polymer; vacuum drying oven; thermogravimetric analyzer and differential scanning calorimeter; S3: Preparation of cucurbituril functionalized monomers, dissolving cucurbituril in a dry solvent, stirring with a magnetic stirrer at room temperature until completely dissolved to form a cucurbituril solution, the concentration of which is controlled between 0.1-0.5 mol / L, slowly dropping the functionalized monomer into the cucurbituril solution, stirring under nitrogen protection, the molar ratio of the functionalized monomer to the cucurbituril being 1:1, after the addition is complete, heating the reaction system to 50-80°C, continuing to stir the reaction for 36 hours, after the reaction is completed, cooling the reaction solution to room temperature, and then precipitating in ether, collecting the precipitate and drying it in a vacuum drying oven to obtain the cucurbituril functionalized monomer, the yield being between 60% and 90%; S4: Synthesis of polymer based on cucurbituril structure: in a dry three-necked flask, add purified cucurbituril functionalized monomer, functionalized monomer, chain transfer agent and initiator in sequence, the total monomer concentration is controlled at 2-5 mol / L, the molar ratio of cucurbituril functionalized monomer to ordinary monomer is 1:10, the molar ratio of chain transfer agent to initiator is 1:1, the amount of initiator is 2% of the total mass of monomer, fill the three-necked flask with nitrogen or argon to remove oxygen in the system, then seal it, place the three-necked flask in a constant temperature water bath, raise the temperature to 60-90°C, start the polymerization reaction, during the reaction , the reaction system is kept uniformly mixed by a magnetic stirrer, and the stirring speed is controlled at 300-800 rpm. After the reaction is carried out for 16 hours, the heating is stopped, the reaction system is cooled to room temperature, and the reaction solution is slowly added dropwise to a large amount of precipitant to precipitate the polymer, and then the polymer precipitate is collected by suction filtration using a Buchner funnel, and the polymer precipitate is washed 2-3 times with a small amount of precipitant to remove residual monomers and impurities, and finally the polymer is placed in a vacuum drying oven and dried at 40-60° C. to constant weight to obtain a polymer based on a cucurbituril structure with a yield of 70%-95%; S5: Characterization and analysis of polymers, determination of molecular weight and molecular weight distribution: The molecular weight and molecular weight distribution of the synthesized polymers were determined using a gel permeation chromatograph, with a water-insoluble polymer as the mobile phase, the flow rate set at 1.0 mL / min, and the column temperature maintained at 30-40 °C. The number average molecular weight, weight average molecular weight and molecular weight distribution index of the polymers were calculated by comparison with standard polymers of known molecular weight; Structural characterization: The structure of the polymer was characterized by using a nuclear magnetic resonance spectrometer. The polymer was dissolved in deuterated chloroform and deuterated water, and hydrogen and carbon spectra were tested. By analyzing the chemical shift, integrated area and splitting of each peak in the spectrum, the structural composition of the polymer was determined, and it was verified whether the cucurbituril structure was successfully introduced into the polymer, as well as the polymerization mode and ratio information of the monomers; Thermal performance analysis: The thermal properties of polymers are studied using thermogravimetric analyzers and differential scanning calorimeters. In the TGA test, polymer samples are heated from room temperature to 800°C at a heating rate of 10-20°C / min in a nitrogen atmosphere, and the curve of the mass change with temperature is recorded to determine the thermal decomposition temperature and thermal stability of the polymer. In the DSC test, the test is also carried out in a nitrogen atmosphere at a heating rate of 5-10°C / min to observe the glass transition temperature and melting point of the polymer and understand the thermal performance characteristics of the polymer.