Facile synthesis of polyamide 6 (PA6)-based thermoplastic elastomers with a well-defined microphase separation structure by melt polymerization

Yuan, Ruchao; Fan, Shuo; Wu, Dequn; Wang, Xueli; Yu, Jianyong; Chen, Lijun; Li, Faxue

doi:10.1039/c8py00068a

Cited by 44 publications

(89 citation statements)

References 40 publications

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“…Figure 1c shows the 1 H-NMR spectrum of PEA-p-4k prepared by polycondensation of prePA6-p-4k with aromatic terephthalic acid as a blocking agent. The chemical shift at 8.2~8.6 ppm is the characteristic peak of the hydrogen atoms in the benzene ring [11]. Because of the high electron cloud density of benzene, the chemical environment of the hydrogen on the adjacent ε-aminocaproic acid is greatly influenced, leading to a high-field shift in this hydrogen.…”

Section: Resultsmentioning

confidence: 99%

“…Li-Kun Xiong et al [9] prepared cationic dyeable polyamide 6 fibre by using 5-sulfoisophthalic acid monosodium salt as a blocking agent and melt polymerization with polyethylene glycol. Juncheng Huang and Ruchao Yuan et al [10,11] prepared a polyamide 6 elastomer by using adipic acid and terephthalic acid as blocking agents and esterification of polytetrahydrofuran under melt conditions, respectively. However, in the process of caprolactam hydrolysis polymerization, approximately 8%–10% of oligomers are inevitably formed, also known as hot water extractables [12,13].…”

Section: Introductionmentioning

confidence: 99%

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A Novel Synthetic Strategy for Preparing Polyamide 6 (PA6)-Based Polymer with Transesterification

Zhang

Tang

et al. 2019

Polymers

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In the polymerization of caprolactam, the stoichiometry of carboxyl groups and amine groups in the process of melt polycondensation needs to be balanced, which greatly limits the copolymerization modification of polyamide 6. In this paper, by combining the characteristics of the polyester polymerization process, a simple and flexible synthetic route is proposed. A polyamide 6-based polymer can be prepared by combining caprolactam hydrolysis polymerization with transesterification. First, a carboxyl-terminated polyamide 6-based prepolymer is obtained by a caprolactam hydrolysis polymerization process using a dibasic acid as a blocking agent. Subsequently, ethylene glycol is added for esterification to form a glycol-terminated polyamide 6-based prepolymer. Finally, a transesterification reaction is carried out to prepare a polyamide 6-based polymer. In this paper, a series of polyamide 6-based polymers with different molecular weight blocks were prepared by adjusting the amount and type of dibasic acid added, and the effects of different control methods on the structural properties of the final product are analyzed. The results showed that compared with the traditional polymerization method of polyamide 6, the novel synthetic strategy developed in this paper can flexibly design prepolymers with different molecular weights and end groups to meet different application requirements. In addition, the polyamide 6-based polymer maintains excellent mechanical and hygroscopic properties. Furthermore, the molecular weight increase in the polyamide 6 polymer is no longer dependent on the metering balance of the end groups, providing a new synthetic route for the copolymerization of polyamide 6 copolymer.

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Section: Resultsmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

A Novel Synthetic Strategy for Preparing Polyamide 6 (PA6)-Based Polymer with Transesterification

Zhang

Tang

et al. 2019

Polymers

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“…1635 [24] Amide I, CO stretching 1170 [23] CH 2 twist/wag (amorphous phase) 1722 [1] CO attached to ester 1200 [23] CH 2 twist-wag (α-crystalline domains) 2866 [24] CH 2 symmetrical stretching 1213 [11] CH 2 twisting (Brill bands) 2931 [24] CH 2 asymmetrical stretching 1240 [23] Amide III and CH 2 wag 3060 [24] Fermi-resonance of NH stretching with the overtone of amide II 1265 [23] Amide III and CH 2 wag 3300 [24] Hydrogen-bonded NH stretching a) Parallel to the rolled plane; b) Perpendicular to the rolled plane.…”

Section: Mixing Of Pa6 Amorphous Domains With Soft Domains (>60 °C)mentioning

confidence: 99%

“…Polyamide-based thermoplastic elastomers (TPAEs), typical block copolymers composed of polyamide (PA, hard segments) and polyether segments (soft segments), are one of the most attractive polymers owing to their extraordinary combination of excellent physical and mechanical properties of vulcanized rubbers and the abilities to be recycled. [1][2][3][4] So far TPAEs have been widely employed in various fields, e.g., automobile, spinning tires, and textiles. [2,5,6] In situ IR spectroscopy was often employed to study the morphological transitions of TPAEs at elevated temperatures, but weak intensity variation of several important bands cannot be distinguished directly.…”

Section: Introductionmentioning

confidence: 99%

Phase Evolution of Polyamide 6 (PA6)‐Based Thermoplastic Elastomers during Heating and Cooling Investigated by Moving‐Window 2D Correlation Infrared Spectroscopy

Yuan

Wang

et al. 2020

Macro Materials & Eng

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To illustrate the complex phase evolution of polyamide 6 (PA6)‐based thermoplastic elastomer (TPAE‐50) with a three‐phase system (a pure PA6 crystalline phase, a phase‐separated mesophase, and a mixed phase) during cooling and heating, the in situ IR spectroscopy combined with moving‐window 2D correlation analysis is employed. The mixing of PA6 amorphous domains with soft domains and the melting of imperfect PA6 crystalline domains of TPAE‐50 occur from 60 °C with the increasing temperature. Brill transition happens to the elastomer during heating and cooling at 140–160 and 170–135 °C, respectively. Microphase separation of TPAE‐50 during cooling is formed and can be composed of three processes: the first process (200–180 °C) is motivated by the crystallization of the elastomer; the second process (170–140 °C) results from the transition of homo‐mixed domains in the mixed phase to PA6 amorphous and soft domains; the third process (125–60 °C) leads to the formation of imperfect PA6 crystalline domains in phase‐separated mesophase.

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“…Most of them are block copolymers consisting of soft segments and hard segments synthesized by solution or anionic polymerization such as poly(styrene‐ b ‐butadiene‐ b ‐styrene) (SBS), poly(diol citrate) and poly(glycerol sebacate) (PGS) . Unlike these polymerization strategies, however, melt polymerization offers the following benefits: good quality, high efficiency, little pollution and low cost, and is a better route for the industrial fabrication of TPEs …”

Section: Introductionmentioning

confidence: 99%

Enhanced Mechanical Properties of PET‐Based Thermoplastic Elastomers: Brittle–Ductile Transition via Micro Cross‐linking Technology

Yuan

Fan

Sun

et al. 2019

Macro Chemistry & Physics

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A novel micro cross‐linking technology is proposed to enhance the mechanical properties of poly(ethylene terephthalate) (PET)‐based thermoplasctic elastomers (TPEEs) whose molecular weights are difficultly increased via traditional synthetic technologies. It is found that the brittle fractures of TPEEs, usually observed in polymers with low molecular weights, can be converted into ductile form with the introduction of a certain fraction of 1,2,3,4‐butane tetracarboxylic acid as a cross‐linking agent. Unlike the traditional cross‐linking technologies, which usually cause the elastomers to suffer the deficiencies of extremely high stiffness, inherent weakness, and the inability to be efficiently reused, TPEEs still maintain their elastomeric characteristics well with the incorporation of micro cross‐linking structure and are endowed with a well‐defined microphase‐separated structure, excellent tensile properties, and the abilities to be melt‐processed and reused. This work offers a new guideline to improve the mechanical properties for polymers with relatively low molecular weights.

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Facile synthesis of polyamide 6 (PA6)-based thermoplastic elastomers with a well-defined microphase separation structure by melt polymerization

Abstract: A facile melt polymerization method for polyamide-6 based thermoplastic elastomers with a well-defined microphase separation structure is proposed.

Cited by 44 publications

References 40 publications

A Novel Synthetic Strategy for Preparing Polyamide 6 (PA6)-Based Polymer with Transesterification

A Novel Synthetic Strategy for Preparing Polyamide 6 (PA6)-Based Polymer with Transesterification

Phase Evolution of Polyamide 6 (PA6)‐Based Thermoplastic Elastomers during Heating and Cooling Investigated by Moving‐Window 2D Correlation Infrared Spectroscopy

Enhanced Mechanical Properties of PET‐Based Thermoplastic Elastomers: Brittle–Ductile Transition via Micro Cross‐linking Technology

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