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A Synthetic Method for Reproducible Thermoset Polymers

A technology of repeated processing and synthesis method, which is applied in the synthesis field of thermosetting polymers, can solve the problems of poor tolerance to organic solvents, pollution, organic solvent corrosion, etc., and achieve the effect of improving mechanical properties, simple synthesis process, and good operability

Active Publication Date: 2022-03-18
FUDAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Thermoplastic polymers have excellent processability and solubility. When the heating temperature reaches the melting temperature, they have good fluidity and ductility, but they have poor tolerance to organic solvents and are easily corroded by organic solvents; while traditional Thermosetting polymers, although having high stability, mechanical strength, creep resistance and chemical stability, play an important role in aerospace, automotive, construction, electronics and other fields
However, compared with thermoplastic polymers, traditional thermosetting materials have an obvious disadvantage—molecules are cross-linked with each other through irreversible covalent bonds, resulting in insolubility and non-melting, which cannot meet the purpose of repeated processing and recycling (Chem .Sci.2016,7,30-38), so it will inevitably cause waste and pollution during production and use (Science 2011,334,965–968)

Method used

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  • A Synthetic Method for Reproducible Thermoset Polymers
  • A Synthetic Method for Reproducible Thermoset Polymers
  • A Synthetic Method for Reproducible Thermoset Polymers

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Example 1 Synthesis of repeatable crosslinked styrene (a method of synthesizing a thermosetting polymer thereof) of styrene and its derivative monomer.

[0038] Styrene 100 mmol, monomer A (glycidyl methacrylate), 0.1 mmol, and azo diisobutyronitrile 0.02 mmol. 10 ml of dimethyl sulfoxide was added, and then the reaction bottle was stirred in an oil bath at 110 ° C for 24 hours, then the reaction was cooled to room temperature, and the reaction liquid was poured into methanol precipitation, vacuum dried to constant weight. To obtain a polymer 1. Its synthetic route is:

[0039]

[0040] Styrene 10 mmol is added to the Schlenk reaction flask, monomer B (vinylbenzyl bio), RAFT initiator 0.01 mmol, azo diisobutyronitrile 0.002 mmol. 2 mL of dimethyl sulfoxide was added, then the reaction bottle was stirred in an oil bath at 110 ° C for 24 hours, then the reaction was cooled to room temperature, and the reaction liquid was poured into methanol precipitation, vacuum drying to ...

Embodiment 2

[0045] Example 2, Synthesis of Methyl Crosslinked Polymethyl methacrylate (a method of synthesizing thermosetting polymers representing a methacrylate monomer).

[0046] Methyl methacrylate 100 mmol, monomer A (glycidyl methacrylate), 0.1 mmol, and azo diisobutyronitrile 0.02 mmol. 10 ml of dimethyl sulfoxide was added, and then the reaction bottle was stirred in an oil bath at 65 ° C for 16 hours, then the reaction was cooled to room temperature, and the reaction liquid was poured into methanol precipitation, vacuum dried to constant weight. To obtain a polymer 4. Its synthetic route is:

[0047]

[0048] Methyl methacrylate 10 mmol, monomer B (vinyl bio), 0.002 mmol of Azobimobutyronitrile 0.002 mmol. 2 ml of dimethyl sulfoxide was added, and then the reaction bottle was stirred in an oil bath at 65 ° C for 16 hours, then the reaction was cooled to room temperature, and the reaction liquid was poured into methanol precipitation, vacuum dried to constant weight. To obtain a pol...

Embodiment 3

[0053] Example 3, synthesis of a repeatable crosslinked acrylate niutate (a method of synthesizing a thermosetting polymer representing an acrylate monomer).

[0054] A n-butyl acrylate 100 mmol, monomer A (glycidyl methacrylate), 0.1 mmol, azo diisobutyronitrile 0.02 mmol. 10 ml of dimethyl sulfoxide as a solvent was added, and then the reaction bottle was stirred in an oil bath at 65 ° C for 8 hours, then the reaction was cooled to room temperature and 10 ml of tetrahydrofuran was added, and the mixture was mixed into petroleum ether and precipitated. The vacuum is dried to constant weight to give the polymer 7. Its synthetic route is:

[0055]

[0056] N-acrylate 10 mmol, monomer B (vinyl bio), Raft initiator 0.01 mmol, 0.002 mmol of Azobiobutyrignonium. 2 ml of dimethyl sulfoxide was added, and then the reaction bottle was stirred in an oil bath at 65 ° C for 8 hours, and then the reaction was cooled to room temperature and 10 ml of tetrahydrofuran was added, and the mixed u...

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Abstract

The invention belongs to the technical field of polymer synthesis, in particular to a method for synthesizing a repeatable thermosetting polymer. The present invention uses a macromolecular cross-linking agent to utilize the reversible cross-linking effect between polymer chains and polymer chains to synthesize cross-linked polymers that can be processed repeatedly; specifically, it includes two parts: the synthesis of functionalized copolymers and the cross-linking and curing of copolymers. ; The copolymer is mainly composed of vinyl monomers such as (meth)acrylic acid (ester), acrylamide, styrene and its derivatives, and vinyl monomers with crosslinkable functional groups as secondary components; crosslinking and curing through The dynamic chemical bond formed between functional groups is realized. Compared with thermoplastic materials with similar chemical composition, the material synthesized by the invention has better mechanical strength, solvent resistance, creep resistance, aging resistance and the like.

Description

Technical field [0001] The present invention belongs to the field of polymer synthesis, and more particularly to a synthesis method of repeatable thermosetting polymers. Background technique [0002] Typically, polymer materials can be divided into two types, thermoplastic polymers and thermosetting polymers. The thermoplastic polymer has excellent processability and solubility. When the heat-resistant temperature reaches the melting temperature, it has good fluidity and ductility, but the tolerance of the organic solvent is relatively poor, it is easy to corrode it by organic solvent; The thermoset polymer, although high stability, mechanical strength, antigenicity and chemical stability, play an important role in aerospace, automotive, construction, and electronics. However, compared to thermoplastic polymers, conventional thermoset materials have a significant disadvantage - the molecular inter-apex is crosslinked by irreversible covalent bonds, resulting in non-dissolving, no...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G81/02C08F212/08C08F230/06C08F220/14C08F220/18C08F220/54C08L87/00
CPCC08G81/021C08F212/08C08F220/14C08F220/18C08F220/54C08L87/005C08F230/06
Inventor 陈茂王宗涛
Owner FUDAN UNIV
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