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Dynamic covalent cross-linked material for enhancing polyethylene performance, its preparation method and application

A covalent cross-linking and dynamic cross-linking technology, applied in the field of polymer materials, can solve the problems of increasing the processing difficulty of cross-linked polyethylene materials, restricting the recycling and repeated processing and utilization of cross-linked polyethylene, and improving mechanical properties and synthesis. The effect of simple process and great application prospect

Active Publication Date: 2021-12-28
FUDAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The stable chemical structure significantly increases the processing difficulty of cross-linked polyethylene materials, and greatly limits the recycling and reprocessing of cross-linked polyethylene

Method used

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  • Dynamic covalent cross-linked material for enhancing polyethylene performance, its preparation method and application
  • Dynamic covalent cross-linked material for enhancing polyethylene performance, its preparation method and application
  • Dynamic covalent cross-linked material for enhancing polyethylene performance, its preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] The synthesis of embodiment 1 borate-containing polycyclooctene PCOE-B

[0039]

[0040] Take a 250 mL round bottom flask, add 4.40 g of cyclooctene, 1.66 g of cyclooctene borate monomer (compound 1), 100 mL of anhydrous dichloromethane, and stir at room temperature. 8.5 mg of Grubbs second-generation catalyst (Grubbs G2) was dissolved in 5 mL of dichloromethane and added to the monomer solution. After reacting at room temperature for 6 hours, 10 μL of vinyl n-butyl ether was added to terminate the reaction. The reaction liquid was dropped into anhydrous methanol to precipitate the polymer, and after vacuum drying at 40° C. for 12 hours, 5.56 g of the product was obtained, with a yield of 92%.

Embodiment 2

[0041] The synthesis of embodiment 2 borate-containing polyethylene PE-B

[0042]

[0043] Take a 150mL thick-walled explosion-proof pressure-resistant bottle, weigh cyclooctene copolymer PCOE-B (0.22g), and dissolve it with 10mL o-xylene. Add p-toluenesulfonyl hydrazide (1.86g, 10mmol), 2,6-di-tert-butyl-4-methylphenol (17.6mg, 0.08mmol), triethylamine (1.01g, 10mmol), tighten the bottle mouth to The bottle was sealed and heated to 120°C for 12 hours. After the reaction, the reaction solution was added dropwise into 100 mL of anhydrous methanol to precipitate a polymer, and vacuum-dried at 60° C. for 12 hours to obtain 0.22 g of the product, with a yield of 100%.

[0044] The second part of the synthesis of dynamically cross-linked polyethylene

Embodiment 3

[0045] The synthesis of embodiment 3 linking agent

[0046]

[0047] Synthesis of 1,6-hexanediboronic acid (2): Take a clean 250mL three-necked round-bottom flask, a spherical condenser, a 100mL constant pressure dropping funnel, apply vacuum silicone grease to the contact part of the grinding port, and inject nitrogen gas after the instrument is assembled. Reactants, solvents, etc. were all added under nitrogen atmosphere. 1,6-Dibromohexane (7.32g, 30.00mmol) was dissolved in 60mL of anhydrous tetrahydrofuran and transferred to a constant pressure dropping funnel, and 2.16g (90.00mmol) of magnesium powder was weighed and added to the flask. Open the constant pressure dropping funnel, drop about 10mL of 1,6-dibromohexane solution into the round bottom flask, heat rapidly to reflux the solvent. Add the remaining 1,6-dibromohexane solution dropwise. During the process, keep the solvent in a slightly boiling state. After the dropwise addition, continue to heat and reflux for ...

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Abstract

The invention belongs to the technical field of polymer materials, in particular to a dynamic covalent cross-linking material for enhancing the performance of polyethylene, a preparation method and application thereof. The dynamic covalent cross-linking material of the present invention is made of linear polyethylene with borate ester groups and boron obtained through dehydration condensation reaction of polyboric acid molecules and 1,2-diol molecules or 1,3-diol molecules The ester cross-linking agent is prepared by boron ester exchange reaction; the dynamic covalent cross-linked polyethylene material can realize the transformation and reorganization of the polymer network through the reversible exchange reaction between different borate ester groups. Add the dynamically covalently cross-linked polyethylene to commercial thermoplastic polyethylene to synthesize a polyethylene / dynamically cross-linked polyethylene composite polymer material; the mechanical properties of the composite polymer material (such as tensile strength, Young's modulus ), creep resistance, solvent resistance, heat resistance and other properties are significantly enhanced, and can be used for repeated processing, repeated shaping, and 3D printing.

Description

technical field [0001] The invention belongs to the technical field of polymer materials, and in particular relates to a dynamic covalent cross-linked polyethylene material and its preparation method and application. Background technique [0002] Polyethylene (PE) is one of the most widely produced and used general-purpose plastics in the world. As of 2019, the global annual output of polyethylene has exceeded 100 million tons, and it is widely used in film, packaging, pipe, insulation and other fields, and plays an extremely important role in human production and life. [0003] However, polyethylene products usually have poor heat resistance, and they are prone to creep in high temperature environments, resulting in irreversible deformation of the product. Therefore, polyethylene materials can only be used at lower temperatures (for example, below 80°C), which limits the use range of polyethylene materials (Chem.Rev.1957,57,665-742; J.Mater.Sci.1994 ,294-323; Patent No.: ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08J3/24C08L65/00C08K5/55C08G61/12C08L23/06
CPCC08J3/24C08G61/123C08J3/246C08G2261/12C08G2261/3322C08G2261/418C08G2261/3342C08G2261/724C08G2261/76C08J2365/00C08K5/55C08J2323/06C08J2465/00
Inventor 陈茂王宗涛
Owner FUDAN UNIV
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