Wet spinning of Bombyx mori silk fibroin dissolved in N-methyl morpholine N-oxide and properties of regenerated fibres

Marsano, Enrico; Corsini, Paola; Arosio, C.; Boschi, Alessandra; Mormino, Michele; Freddi, Giuliano

doi:10.1016/j.ijbiomac.2005.10.005

Cited by 71 publications

(65 citation statements)

References 33 publications

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“…30,34 Silk fibroin concentration was fixed to 17% (w/w) with respect to the solution. Regenerated silkworm silk fibers were spun from the dopes with a dry-jet wet-spinning line composed of an extrusion unit, a coagulation bath, a take-up spool, an immersion postspinning drawing bath, that consists of a bath of water in which the spun fiber is subjected to postspinning drawing, and finally a collecting spool as shown in Figure l.…”

Section: Methodsmentioning

confidence: 99%

“…Thus, a number of dope compositions that yield spinnable solutions were reported, such as saturated ammonium sulfate solution, 19 concentrated orthophosphoric acid, 20 concentrated aqueous solution, 21,22 hexafluoro-2-propanol, 23 ' 24 hexafluoroacetone hydrate, 25 formic acid, 26,27 ionic liquids, 28,29 and N-methyl morpholine oxide. 30 However, the production of regenerated silkworm silk fibers has represented an extremely painstaking effort, as reflected by the poor tensile properties reported by most studies. 22,27,30,31 It was only after introducing subsequent changes in the basic wet-spinning process, especially related with the introduction of modified postspinning drawing processes, when the first reports of the production of high performance regenerated silkworm silk fibroin fibers with properties comparable with those of the natural material were found.…”

Section: Abstract: Biofibers; Biomimetic; Silkmentioning

confidence: 99%

“…30 However, the production of regenerated silkworm silk fibers has represented an extremely painstaking effort, as reflected by the poor tensile properties reported by most studies. 22,27,30,31 It was only after introducing subsequent changes in the basic wet-spinning process, especially related with the introduction of modified postspinning drawing processes, when the first reports of the production of high performance regenerated silkworm silk fibroin fibers with properties comparable with those of the natural material were found.…”

Section: Abstract: Biofibers; Biomimetic; Silkmentioning

confidence: 99%

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Correlation between processing conditions, microstructure and mechanical behavior in regenerated silkworm silk fibers

Plaza

Corsini

Marsano

et al. 2011

J Polym Sci B Polym Phys

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Regenerated silkworm fibers spun through a wetspinning process followed by an immersion postspinning drawing step show a work to fracture comparable with that of natural silkworm silk fibers in a wide range of spinning conditions. The mechanical behavior and microstructure of these high performance fibers have been characterized, and compared with those fibers produced through conventional spinning conditions. The comparison reveals that both sets of fibers share a common semicrystalline microstructure, but significant differen-

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Section: Methodsmentioning

confidence: 99%

Section: Abstract: Biofibers; Biomimetic; Silkmentioning

confidence: 99%

Section: Abstract: Biofibers; Biomimetic; Silkmentioning

confidence: 99%

See 1 more Smart Citation

Correlation between processing conditions, microstructure and mechanical behavior in regenerated silkworm silk fibers

Plaza

Corsini

Marsano

et al. 2011

J Polym Sci B Polym Phys

Self Cite

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“…The processes developed so far depend on extruding silk fibroin dissolved in formic acid, [5] N-methyl morpholine N-oxide (NMMO), [6] 1,1,1,3,3,3-hexafluoro-2-propanol (HFIP), [7] trifluoro-acetic acid (TFA), [5a] hexafluoroacetone (HFA) [8] or 1-ethyl-3-methylimidazolium chloride, [9] usually into a methanol bath. However, most of these silk solvents either severely degrade the silk fibroin or are too expensive or toxic for use in industrial processes.…”

mentioning

confidence: 99%

Silk Fibers Extruded Artificially from Aqueous Solutions of Regenerated Bombyx mori Silk Fibroin are Tougher than their Natural Counterparts

et al. 2009

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The dragline silk of certain spiders has excellent tensile properties [1] that are maintained over a remarkable temperature range.[2] Although the commercial Mulberry Silkworm (Bombyx mori) silk is considerably weaker and less tough than the best spider dragline silks, fibers with comprehensive mechanical properties approaching that of spiders can be obtained by force-reeling directly from silkworms.[3] Remarkably, both spider and silkworm silks are spun naturally from aqueous protein solutions at very low hydraulic pressures and at ambient temperature, not requiring a noxious coagulation bath.[4] These considerations have lead to the search for methods to extrude strong and tough fibers from regenerated silk protein solutions. The processes developed so far depend on extruding silk fibroin dissolved in formic acid, [5] N-methyl morpholine N-oxide (NMMO), [6] 1,1,1,3,3,3-hexafluoro-2-propanol (HFIP), [7] trifluoro-acetic acid (TFA), [5a] hexafluoroacetone (HFA) [8] or 1-ethyl-3-methylimidazolium chloride, [9] usually into a methanol bath. However, most of these silk solvents either severely degrade the silk fibroin or are too expensive or toxic for use in industrial processes. Moreover, in all cases described, fibers spun from silk fibroin generated fibers weaker than their natural counterparts, [10] with the exception of Ha et al.'s use of fibroin dissolved in TFA.[5a] However, the cold methanol coagulation bath used in these examples produced fibers that were much larger than the natural ones, lacked smooth surfaces, and were so stiff in their as-extruded form that their tensile properties could only be brought above those of natural fibers by manual neck drawing. This, and the cost of TFA, render Ha et al.'s process [5a] unsuitable for industrial scale up. In this report, we describe and evaluate a novel and environmentfriendly integral extrusion and drawing process that overcomes the limitations of earlier processes. This process produces stronger, tougher, and more extensible fibers, compared to natural undegummed B. mori silkworm cocoon silk (raw silk). The process is novel in two respects: first, it uses highly concentrated aqueous solutions of regenerated silk fibroin (RSF); and second, it employs a hot ammonium sulphate solution for the coagulation bath. The use of a high-concentration aqueous RSF solution as spinning dope is important to ensure the high packing fraction of the protein chains, required for good mechanical performance. For the coagulation bath, many other organic and inorganic compounds, including methanol, ethanol, isopropanol, n-butanol, glycol, glycerin, and various sodium, potassium, zinc, magnesium, and ammonium salts (chloride, sulphate, nitrate, phosphate and acetate), have been tried. We chose ammonium sulphate after careful consideration of the mechanism and rate of the conformation transition and solidification of silk fibroin during the extrusion and drawing process. The rate at which this occurs is crucial to the behavior of the silk during drawing, and consequently to the...

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“…Regenerated silkworm silk fibers are produced by dissolving natural silkworm silk, preparing a spinnable protein solution (dope) and synthesising the fibers through a wet spinning process [40]. Several processes were proposed following this basic scheme that differ in the use of different compositions for the dope [41][42][43]. However, the poor tensile properties reported for regenerated fibers did not allow inferring any reliable conclusion on the range of properties that could be reached through different processing paths from the same protein sequence.…”

Section: Recovery In the Context Of Biomimeticsmentioning

confidence: 99%

Polymeric fibers with tunable properties: Lessons from spider silk

Calafat

Guinea

Pérez‐Rigueiro

et al. 2011

Materials Science and Engineering: C

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Making artificial fibers inspired in spider silks is considered as one of the milestones in the field of biomimetics. The interest is usually justified by the outstanding tensile properties of natural fibers, but it is usually overlooked that spider silk is endowed with a number of related properties -supercontraction, recovery and the existence of a ground state -that impart the material with additional desirable features, such as the possibility of tuning its mechanical behaviour. In this work we present a review on the experimental Kevwordsanalysis and significance of these properties, stressing the contributions of our research group to the field. It is Spider silk a ' s0 demonstrated how the knowledge gained in the basic study of the natural material has been essential for Supercontraction the improvement of the properties exhibited by artificially processed bio-inspired silk fibers. Regenerated silk

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Wet spinning of Bombyx mori silk fibroin dissolved in N-methyl morpholine N-oxide and properties of regenerated fibres

Cited by 71 publications

References 33 publications

Correlation between processing conditions, microstructure and mechanical behavior in regenerated silkworm silk fibers

Correlation between processing conditions, microstructure and mechanical behavior in regenerated silkworm silk fibers

Silk Fibers Extruded Artificially from Aqueous Solutions of Regenerated Bombyx mori Silk Fibroin are Tougher than their Natural Counterparts

Polymeric fibers with tunable properties: Lessons from spider silk

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