Synthesis and characterization of poly(copolyethers-block-polyamides) II. Characterization and properties of the multiblock copolymers

Boulares, Alya; Tessier, Martine; Maréchal, Ernest

doi:10.1016/s0032-3861(99)00526-1

Cited by 50 publications

(62 citation statements)

References 32 publications

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“…The multiple relaxations in PEBA copolymers have been studied by dynamic mechanical measurements, dielectric measurements, and thermally stimulated current methods [4][5][6][7]12,13]. These relaxation methods, in accordance with Figure 7.…”

Section: Microphase Separation Vs Hard and Soft Segment Block Lengthmentioning

confidence: 94%

“…Numerous techniques have been used to characterize the PEBA supermolecular structure including light microscopy, transmission electron microscopy (TEM), atomic force microscopy (AFM) [1][2][3][4], dynamical mechanical thermal analysis (DMTA) [4][5][6][7] solid-state nuclear magnetic resonance (solid-state NMR) [7], small-angle X-ray scattering (SAXS) [3,4], wide-angle X-ray scattering (WAXS) [4], small-angle light scattering (SALS) [4], and differential scanning calorimetry (DSC) [4,5,[8][9][10]. The latter is a common technique, often used to give practical information about the maximal service temperature of the materials, as well as additional information relative to the product composition.…”

Section: Thermal Transitionsmentioning

confidence: 99%

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Poly(Ether‐ b ‐Amide) Thermoplastic Elastomers: Structure, Properties, and Applications

Eustache

2005

Handbook of Condensation Thermoplastic Elastomers

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Structure and characterizationPoly(ether-b-amide) thermoplastic elastomers (PEBA) are segmented block copolymers where the hard blocks consist of polyamide segments, acting as physical crosslinks, and the soft blocks consist of flexible polyether segments having a glass transition temperature well below room temperature and acting as entropic springs.Consequently, the PEBA resins are first characterized by the chemical composition of the polyamide block (polyamide 6 (PA6), polyamide 66 (PA66), polyamide 11 (PA11), polyamide 12 (PA12), co-polyamide, etc.) and polyether block (poly(tetramethylene glycol) (PTMG), poly(ethylene glycol) (PEG), poly(propylene glycol) (PPG), etc.), which governs basic physico-chemical properties, such as melting range, density, or the hydrophilic/hydrophobic balance (see Chapter 9 for more information about the chemical composition and nomenclature of the polyamide and polyether structural units).The characterization based upon the mass ratio of the polyamide and the polyether structural units (PA/PE ratio) is useful because it concerns morphological aspects and the related mechanical behavior: (i) Products where the polyether matrix is the continuous phase (PA/PE < 1) show good elastic properties in a broad deformation range (100-300%) and a low modulus (10-30 MPa). These materials are often transparent. (ii) Products where the polyamide matrix is the continuous phase (PA/PE > 1) show a higher modulus

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Section: Microphase Separation Vs Hard and Soft Segment Block Lengthmentioning

confidence: 94%

Section: Thermal Transitionsmentioning

confidence: 99%

Poly(Ether‐ b ‐Amide) Thermoplastic Elastomers: Structure, Properties, and Applications

Eustache

2005

Handbook of Condensation Thermoplastic Elastomers

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“…열 가소성 탄성체는 올레핀계 TPE 및 올레핀계 TPV(thermoplastic vulcanizate), 스티렌계 TPE, 우레탄계 TPE(TPU), 불 소계 TPE, 폴리에스테르계 TPE, PVC계 TPE, polyamide계 TPE 등으로 다양하게 세분화되어 개발되었다. [1][2][3][4][5][6][7][8] 특히 polyamide(PA)계 TPE는 결정성의 PA가 hard segment 를 이루고 polyether polyol로 soft segment를 구성하는 블록 공중합체로 이 구성성분을 적당히 조절함으로써 다양한 특성 을 가지는 열가소성 탄성체를 제조할 수 있다. 특히 hard segment인 PA가 TPE의 열적, 기계적 성질에 중요한 영향을 준다.…”

Section: 서 론unclassified

Synthesis and Characterization of Thermoplastic Elastomer Poly(ether-b-amide) Containing Aromatic Moiety

Lee¹,

Kim²

2014

Polymer Korea

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초록: 방향족 구조를 포함하고 분자량이 조절된 polyamide(PA) 올리고머를 4-aminobenzoic acid와 12-aminododecanoic acid의 축합반응으로 합성하였다. 이 올리고머를 여러 분자량의 polytetramethylene glycol(PTMG)과 축합하여 PA를 hard segment로 하고 PTMG를 soft segment로 하는 열가소성 탄성체로서 poly(ether-b-amide)(PEBA)를 제조하였다. 합성된 PEBA의 구조는 FTIR과 1 H NMR로 확인하였으며 DSC와 UTM을 사용하여 hard segment의 구조변화에 따 른 열적특성과 기계적 성질의 변화를 비교해 본 결과 방향족 구조를 3 0%까지 포함할 때 결정성의 변화 없이 PEBA들의 용융온도는 높아졌고 초기 modulus와 strength는 더 크게 나타났다.Abstract: Polyamide (PA) oligomers, which are the hard segment of poly(ether-block-amide) (PEBA), presenting thermoplastic and high performance elastomeric properties were prepared by polycondensation between 4-aminobenzoic acid and 12-aminododecanoic acid. Subsequently PEBAs were obtained by addition polymerization of the PA oligomers and various molecular weights of poly(tetramethylene glycol) (PTMG). The structure of the final PEBA was identified by using FTIR and 1 H NMR and the thermal properties depending on changes in the structure of hard segment were collected by using DSC and UTM analysis. As the results, the melt temperature (T m ), the initial modulus, and the maximum strength of PEBAs increased with an increase in aromatic moiety up to 30% without reducing crystallinity.Keywords: oligomer, polyamide 12, ω-amino carboxylic acid, poly (ether-b-amide) (C-H aromatic bending)가 방향족 단량체 비율이 커질수록 흡 수가 증가되는 것으로 확인되었다. 그리고 Figure 5는 oPA30 (N-H stretching), 2258 cm -1 (N=C=O stretching), 1719 cm -1 (C=O ester bending) 피크 가 존재하는 것으로 확인됨에 따라 합성이 성공적으로 이루 어졌다고 판단하였다.PEBA의 구조 확인. Figure 7은 PEBA의 FTIR spectrum 이다. Hard segment인 PA의 특성 피크인 3307 cm -1 (N-H stretching), 1645 cm -1 (C=O ester bending)가 나타나며 soft segment인 polyether의 특성 피크인 1119 cm -1 (C-O ether bending)가 존재하는 것으로 확인됨에 따라 합성이 성공적으 로 이루어졌다고 여겨진다.oPA의 평균분자량 확인. Figure 8은 방향족 구조인 4-aminobenzoic acid 함량변화에 따른 PA12 올리고머의 DSC thermogram이 다. Table 3을 보면 PA에 방향족 구조를 주는 단량체를 30% 정도까지 도입한 경우 분자사슬이 더욱 단단해진 탓에 T m 과 ∆H가 약간 증가하였다. 하지만, 50 mol% 이상 함유되었을 경 우 오히려 T m 과 ∆H이 떨어졌다. 그 이유는 많은 양이 방향 족 구조가 도입됨으로써 오히려 아미드기에 의한 수소결합을 방해하여 결정성을 떨어뜨린 결과라고 생각된다. 한편, Figure 9는 방향족 구조인 4-aminobenzoic acid의 함량을 변화시켜 Figure 5.

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“…The solvent was removed under reduced pressure, and the residue was dissolved in 100 mL of cold water, then the solution was decanted and 5 mL of concentrated HCl was added. A white precipitate was formed, filtered off, and dried to give compounds N,N¢-(bicyclo [2,2,2]oct-7-enetetracarboxylic)-bis-L-amino acids 3a-f. Bis(3-amino phenyl) phenyl phosphine oxide 4 This compound was prepared according to our previous methods.…”

Section: Experimental Materialsmentioning

confidence: 99%

“…1 The processing of these thermoplastic polymers has been greatly hindered because they lack softening or melting behavior at usual processing temperatures, and they tend to degrade before or at the softening temperature. 2 Various attempts have been made to bring down the T g or melting temperature of aromatic polyamides to make them processable by introducing linked and flexible bridging units [3][4][5] into the polymer chains. Unfortunately, the loss of thermal stability and significant decrease in mechanical properties on heating are usually a consequence of the reduced chain stiffness.…”

Section: Introductionmentioning

confidence: 99%

Novel Flame‐Retardant and Thermally Stable Poly(Amide‐imide)s Based on Bicyclo[2,2,2]oct‐7‐Ene‐2,3,5,6‐Tetracarboxylic Diimide and Phosphine Oxide in the Main Chain: Synthesis and Characterization

Faghihi

Hajibeygi

Shabanian

2009

J Chinese Chemical Soc

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Six novel poly(amide-imide)s PAIs 5a-f were synthesized through the direct polycondensation reaction of six chiral N, N¢-(bicyclo[2,2,2]oct-7-ene-tetracarboxylic)-bis-L-amino acids 3a-f with bis(3-amino phenyl) phenyl phosphine oxide 4 in a medium consisting of N-methyl-2-pyrrolidone (NMP), triphenyl phosphite (TPP), calcium chloride (CaCl 2 ) and pyridine. The polymerization reaction produced a series of flame-retardant and thermally stable poly(amide-imide)s 5a-f with high yield and good inherent viscosity of 0.39-0.83 dLg -1 . The resultant polymers were fully characterized by means of FTIR, 1 H NMR spectroscopy, elemental analyses, inherent viscosity, specific rotation and solubility tests. Thermal properties and flame retardant behavior of the PAIs 5a-f were investigated using thermal gravimetric analysis (TGA and DTG) and limited oxygen index (LOI). Data obtained by thermal analysis (TGA and DTG) revealed that these polymers show good thermal stability. Furthermore, high char yields in TGA and good LOI values indicated that resultant polymers exhibited good flame retardant properties. N, N¢-(bicyclo[2,2,2]oct-7-ene-tetracarboxylic)-bis-L-amino acids 3a-f were prepared in quantitative yields by the condensation reaction of bicyclo[2,2,2]oct-7-ene-2,3,5,6-tetracarboxylic dianhydride 1 with L-alanine 2a, L-valine 2b, L-leucine 2c, L-isoleucine 2d, L-phenyl alanine 2e and L-2-aminobutyric acid 2f in acetic acid solution. These polymers can be potentially utilized in flame retardant thermoplastic materials.

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Synthesis and characterization of poly(copolyethers-block-polyamides) II. Characterization and properties of the multiblock copolymers

Cited by 50 publications

References 32 publications

Poly(Ether‐ b ‐Amide) Thermoplastic Elastomers: Structure, Properties, and Applications

Poly(Ether‐ b ‐Amide) Thermoplastic Elastomers: Structure, Properties, and Applications

Synthesis and Characterization of Thermoplastic Elastomer Poly(ether-b-amide) Containing Aromatic Moiety

Novel Flame‐Retardant and Thermally Stable Poly(Amide‐imide)s Based on Bicyclo[2,2,2]oct‐7‐Ene‐2,3,5,6‐Tetracarboxylic Diimide and Phosphine Oxide in the Main Chain: Synthesis and Characterization

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