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EP4321666A1 - Fibres extrudées en alcool polyvinylique et produits fibreux - Google Patents

Fibres extrudées en alcool polyvinylique et produits fibreux Download PDF

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Publication number
EP4321666A1
EP4321666A1 EP23191132.2A EP23191132A EP4321666A1 EP 4321666 A1 EP4321666 A1 EP 4321666A1 EP 23191132 A EP23191132 A EP 23191132A EP 4321666 A1 EP4321666 A1 EP 4321666A1
Authority
EP
European Patent Office
Prior art keywords
fibres
polyvinyl alcohol
molten
hydrolysis
butanediol
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
EP23191132.2A
Other languages
German (de)
English (en)
Inventor
John Williams
Sian Griffiths
Robert Ashworth
Jack EATON
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Aquapak IP Ltd
Original Assignee
Aquapak IP Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Aquapak IP Ltd filed Critical Aquapak IP Ltd
Publication of EP4321666A1 publication Critical patent/EP4321666A1/fr
Pending legal-status Critical Current

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    • D—TEXTILES; PAPER
    • D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
    • D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
    • D04H1/42—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties characterised by the use of certain kinds of fibres insofar as this use has no preponderant influence on the consolidation of the fleece
    • D04H1/4282—Addition polymers
    • D04H1/4309—Polyvinyl alcohol
    • A—HUMAN NECESSITIES
    • A47—FURNITURE; DOMESTIC ARTICLES OR APPLIANCES; COFFEE MILLS; SPICE MILLS; SUCTION CLEANERS IN GENERAL
    • A47K—SANITARY EQUIPMENT NOT OTHERWISE PROVIDED FOR; TOILET ACCESSORIES
    • A47K7/00—Body washing or cleaning implements
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00—Formation of filaments, threads, or the like
    • D01D5/08—Melt spinning methods
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00—Formation of filaments, threads, or the like
    • D01D5/08—Melt spinning methods
    • D01D5/098—Melt spinning methods with simultaneous stretching
    • D01D5/0985—Melt spinning methods with simultaneous stretching by means of a flowing gas (e.g. melt-blowing)
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00—Formation of filaments, threads, or the like
    • D01D5/12—Stretch-spinning methods
    • D01D5/16—Stretch-spinning methods using rollers, or like mechanical devices, e.g. snubbing pins
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F1/00—General methods for the manufacture of artificial filaments or the like
    • D01F1/02—Addition of substances to the spinning solution or to the melt
    • D01F1/10—Other agents for modifying properties
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/02—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D01F6/14—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolymers obtained by reactions only involving carbon-to-carbon unsaturated bonds from polymers of unsaturated alcohols, e.g. polyvinyl alcohol, or of their acetals or ketals
    • D—TEXTILES; PAPER
    • D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
    • D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
    • D04H1/42—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties characterised by the use of certain kinds of fibres insofar as this use has no preponderant influence on the consolidation of the fleece
    • D04H1/425—Cellulose series
    • D—TEXTILES; PAPER
    • D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
    • D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
    • D04H1/54—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties by welding together the fibres, e.g. by partially melting or dissolving
    • D04H1/56—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties by welding together the fibres, e.g. by partially melting or dissolving in association with fibre formation, e.g. immediately following extrusion of staple fibres
    • D—TEXTILES; PAPER
    • D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H3/00—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length
    • D04H3/005—Synthetic yarns or filaments
    • D04H3/007—Addition polymers
    • D—TEXTILES; PAPER
    • D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H3/00—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length
    • D04H3/02—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length characterised by the method of forming fleeces or layers, e.g. reorientation of yarns or filaments
    • D04H3/03—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length characterised by the method of forming fleeces or layers, e.g. reorientation of yarns or filaments at random
    • D04H3/033—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length characterised by the method of forming fleeces or layers, e.g. reorientation of yarns or filaments at random reorientation immediately after yarn or filament formation
    • D—TEXTILES; PAPER
    • D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H3/00—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length
    • D04H3/08—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length characterised by the method of strengthening or consolidating
    • D04H3/10—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length characterised by the method of strengthening or consolidating with bonds between yarns or filaments made mechanically
    • D04H3/105—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length characterised by the method of strengthening or consolidating with bonds between yarns or filaments made mechanically by needling
    • D—TEXTILES; PAPER
    • D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H3/00—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length
    • D04H3/08—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length characterised by the method of strengthening or consolidating
    • D04H3/10—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length characterised by the method of strengthening or consolidating with bonds between yarns or filaments made mechanically
    • D04H3/11—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length characterised by the method of strengthening or consolidating with bonds between yarns or filaments made mechanically by fluid jet
    • D—TEXTILES; PAPER
    • D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H3/00—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length
    • D04H3/08—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length characterised by the method of strengthening or consolidating
    • D04H3/12—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length characterised by the method of strengthening or consolidating with filaments or yarns secured together by chemical or thermo-activatable bonding agents, e.g. adhesives, applied or incorporated in liquid or solid form
    • D—TEXTILES; PAPER
    • D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H3/00—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length
    • D04H3/08—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length characterised by the method of strengthening or consolidating
    • D04H3/14—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length characterised by the method of strengthening or consolidating with bonds between thermoplastic yarns or filaments produced by welding
    • D—TEXTILES; PAPER
    • D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H3/00—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length
    • D04H3/08—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length characterised by the method of strengthening or consolidating
    • D04H3/16—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length characterised by the method of strengthening or consolidating with bonds between thermoplastic filaments produced in association with filament formation, e.g. immediately following extrusion
    • D—TEXTILES; PAPER
    • D10—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10B—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10B2201/00—Cellulose-based fibres, e.g. vegetable fibres
    • D10B2201/20—Cellulose-derived artificial fibres
    • D10B2201/22—Cellulose-derived artificial fibres made from cellulose solutions
    • D—TEXTILES; PAPER
    • D10—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10B—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10B2321/00—Fibres made from polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D10B2321/06—Fibres made from polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds polymers of unsaturated alcohols, e.g. polyvinyl alcohol, or of their acetals or ketals

Definitions

  • This invention relates to polyvinyl alcohol fibres, methods of making polyvinyl alcohol fibres and products manufactured from polyvinyl alcohol fibres.
  • the invention relates particularly but not exclusively to products comprising extruded polyvinyl alcohol fibres, methods of making extruded polyvinyl alcohol fibres and products incorporating such fibres.
  • Polyvinyl alcohol has many advantages in comparison to polymers which are traditionally used for manufacture of non-woven fibre products. Polyvinyl alcohol is soluble in water, particularly when heated, facilitating reclamation, recycling and environmental degradation.
  • Polyvinyl alcohol is manufactured by hydrolysis of homopolymer or co-polymers of polyvinyl acetate.
  • Polyvinyl alcohol manufactured by partial or complete hydrolysis of homopolymeric polyvinyl acetate is referred to as homopolymeric polyvinyl alcohol.
  • the degree of hydrolysis determines the properties of the resultant polymer.
  • Co-polymeric polyvinyl alcohols or homopolymeric polyvinyl alcohol with a low degree (LD) of hydrolysis are easy to process but have inferior mechanical and chemical properties.
  • Homopolymeric polyvinyl alcohol with a high degree (HD) of hydrolysis, for example 85% or greater, has superior properties but is not processable without degradation under conditions using apparatus employed for manufacture of polyolefin non-woven fibres.
  • Polyvinyl alcohol is soluble in water and fibres have traditionally been made by solution spinning methods using polyvinyl alcohol with a low degree (LD) of hydrolysis.
  • WO2017/046361 discloses a method for manufacture of processable polyvinyl alcohol having a degree of hydrolysis of 98% or greater.
  • WO2022/008521 discloses a method for manufacture of processable polyvinyl alcohol having a degree of hydrolysis in the range of 93% to 98% or more.
  • WO2022/008516 discloses a method for manufacture of plasticised polyvinyl alcohol having a degree of hydrolysis of 93 wt% to 98 wt% or more.
  • a method of manufacture of polyvinyl alcohol fibres comprises the steps of:
  • the degree of hydrolysis may be 95 wt% to 98 wt%, for example 93 wt% to 95 wt%.
  • the molecular weight of the homopolymeric polyvinyl alcohol may be in the range from 14,000 to 35,000.
  • Molecular weights in this specification are weight average molecular weights and are measured using conventional liquid chromatographic techniques.
  • the composition may be melted at a temperature from 220°C to 240°C, for example 220°C to 230°C.
  • the polyvinyl alcohol composition of this invention may have a melt flow index (MFI) of 30 to 80g/10min, for example 50 to 75g/10min, for example 70 to 75g/10min.
  • Melt flow indices referred to in this specification are determined at 230°C using a weight of 10kg by conventional techniques.
  • the polyvinyl alcohol composition of this invention is stable at the temperature at which it is melted and extruded.
  • Polyvinyl alcohol, not containing a plasticiser and stabiliser as disclosed herein, particularly the homopolymer having a high degree of hydrolysis, may be liable to decompose at the temperatures required for melting and extrusion processing.
  • Advantageous polyvinyl alcohol fibres of this invention are capable of being processed on a commercial scale, using conventional fibre processing apparatus.
  • Polyvinyl alcohol according to this invention can be processed into filaments or fibres. These may be converted by crimping and cutting into staple fibres suitable for carding, wet laying and air laying to form a range of non-woven products.
  • Advantageous polyvinyl alcohol fibres of this invention are capable of being processed on a commercial scale, for example using apparatus running at 4,500 m.min -1
  • the stabilised polyvinyl alcohol polymers used in this invention may be manufactured in accordance with WO2022/008516 and WO2022/008521 , the disclosures of which are incorporated into this specification by reference for all purposes.
  • the polyvinyl alcohol composition may be made by a method comprising the steps of:
  • a reactive mixing apparatus typically an extruder in accordance with this invention allows the processing aid and plasticiser to be reacted with the polyvinyl alcohol or blend thereof, without decomposition of the polymer followed by removal of all or most of the processing aid from the secondary outlet to give plasticised polyvinyl alcohol or a blend thereof.
  • a reactive stabiliser may result in an advantageous reduction in the extent of degradation during melt processing. This allows homopolymeric polyvinyl alcohol having a high degree of hydrolysis, for example 88 wt% or higher to be processed to form fibres or pellets from which fibres may be formed by extrusion.
  • the reactive stabiliser may be used in an amount of about 0.1 wt% to about 5 wt%, for example about 0.1 wt% to about 3 wt%, for example 0.1 wt% to about 1.5 wt%, for example from about 0.2 wt% to about 0.5 wt%, for example about 0.25 wt%.
  • the reactive stabilisers of this invention may decrease the extent of degradation of the polymer during processing.
  • Homopolymeric polyvinyl alcohol has been difficult to process due to degradation at the high temperatures required.
  • the liability of degradation has led to use of polyvinyl alcohol co-polymers with a consequent loss of engineering properties. This can be seen by UV spectral analysis of the amount of conjugation present in the polymer. Sodium benzoate has been found to be particularly effective.
  • Homopolymeric polyvinyl alcohol is manufactured by hydrolysis of homopolymeric polyvinyl acetate, the degree of hydrolysis being 93wt% or more in embodiments of this invention.
  • Polyvinyl alcohol co-polymers made by hydrolysis of polyvinyl acetate copolymers have inferior properties compared to homopolymeric polyvinyl alcohol.
  • Homopolymeric polyvinyl alcohol may exhibit advantageous properties.
  • Polyvinyl alcohol polymers of this invention may have high tensile strength and flexibility.
  • the polyvinyl alcohol may be manufactured by hydrolysis of homopolymeric polyvinyl acetate, wherein the extent of hydrolysis is in the range from 88 wt% up to 98 wt%, for example 93 wt% to less than 98 wt%, for example 93 wt% to 97 wt%, for example 93 wt% to 95 wt%.
  • a blend of two or more polyvinyl alcohol polymers may be employed, for example a blend of two polyvinyl alcohol polymers with a relatively high molecular weight and a relatively low molecular weight respectively.
  • a blend of polyvinyl alcohols with the same molecular weight and different degrees of hydrolysis can be combined. Blending different polyvinyl alcohol grades together enables the properties of the resultant polymer to be enhanced, for example melt strength.
  • a blend of two polyvinyl alcohol polymers with a molecular weight in the range 22,000 to 38,000 a first polymer having a low degree of hydrolysis and a second polymer having a high degree of hydrolysis may be blended in a ratio of 40:60 to 60:40, for example about 50:50 by weight.
  • the blends of different molecular weight polymers employed are selected in accordance with the physical properties required in the finished product. This may require different molecular weight materials being used. Use of more than two different molecular weight polymers may be advantageous. The use of a single molecular weight polymer is not precluded.
  • a blend may allow control of the viscosity of the polymer. Selection of a stabiliser in accordance with the present invention allows use of blends of a desired viscosity without a loss of other properties. Alternatively, use of a blend may permit use of polyvinyl alcohol with one or more stabilisers while maintaining viscosity or other properties to permit manufacture of pellets or films.
  • the processing aid is preferably water.
  • the processing aid may comprise a mixture of water and one or more hydroxyl compounds with a boiling point less than the boiling point or melting point of the plasticiser. Use of water is preferred for cost and environmental reasons.
  • Two or more plasticisers may be employed.
  • a binary mixture may be preferred.
  • the plasticiser may be selected from the group consisting of: diglycerol, triglycerol, xylose, D-mannitol, triacetin, dipentaerythritol, 1,4-butanediol, 3,3-dimethyl-1,2-butanediol, and caprolactam.
  • the total amount of plasticiser in the formulation may be from about 15 wt% to about 30 wt%.
  • Polymer compositions and fibres of the present invention may not include any or any substantial amount of a water soluble salt, oil, wax or ethylene homopolymer or copolymer.
  • the method of this invention provides many advantages.
  • the method allows formation of thermally processable polyvinyl alcohol which can be used to create economical fibres that are highly functional while eliminating plastic pollution.
  • Polyvinyl alcohol is water-soluble, non-toxic to the environment and inherently biodegradable.
  • Hydrophilic polymers for example, polyvinyl alcohol degrade environmentally faster than hydrophobic polymers and do not show bioaccumulation.
  • Thermoplastic polyvinyl alcohol can be mechanically recycled into pellets for repeated use.
  • Fibres of this invention may have an advantageous smaller diameter. Fibres having a smaller diameter have a greater surface area which may be advantageous for air filtration, for example in face masks. Finer fibres may also be softer in texture. Furthermore, finer fibres may also have an increased rate of biodegradation after use.
  • a non-woven product comprising thermally processable homopolymeric polyvinyl alcohol fibres having a degree of hydrolysis of 88 wt% or greater made in accordance with the first aspect of the present invention.
  • a non-woven fibre product comprising homopolymeric polyvinyl alcohol fibres having a degree of hydrolysis of 88 wt% or greater.
  • a non-woven product is defined by ISO9092 as an engineered fibrous assembly, primarily planar, which has been given a designed level of structural integrity by physical and/or chemical means, excluding weaving, knitting or paper making.
  • Homopolymeric polyvinyl alcohol fibres of this invention provide many advantages in comparison to previously available polyvinyl alcohol containing fibres.
  • the fibres of this invention and products made from these fibres exhibit improved tensile strength, barrier properties, water solubility and biodegradability.
  • Homopolymeric polyvinyl alcohol fibres may unexpectedly exhibit all of these properties.
  • copolymers have only been able to compromise and provide one or more of these properties at the expense of other properties.
  • the fibres and products of the present invention have a desirable monomaterial structure which does not suffer from this disadvantage.
  • Non-woven products comprising polyvinyl alcohol fibres of this invention in combination with fibres of cellulose pulp, viscose and mixtures thereof have excellent flushability, for example in accordance with UK Water Fine to Flush WIZ 4-02-06.
  • Wet wipes manufactured from non-woven fibres of this invention exhibit excellent dry and wet tensile strength.
  • Fibres of this invention may be made by extrusion of filaments of the melted polyvinyl alcohol polymer through a spinneret having small holes, for example 0.25mm in diameter.
  • the extruded filaments may be drawn using godet rollers rotating at different speeds to form a multi filament tow.
  • the multifilament tow may be crimped by heating followed by shaping with toothed or fluted rollers and cutting with rotary blades to provide fibres of desired length. Use of specific fibre lengths may confer compatibility with various non-woven fibre processing techniques.
  • An extrusion temperature of 200°C to 250°C may be employed, preferably 210°C to 247°C.
  • the number of filaments in a fibre may be in the range 24 to 72, dependent on the equipment used. Use of fibre comprising a bundle of 50 to 72 filaments may be advantageous to improve cohesion of the bundle of filaments during drawing and may allow for a higher drawing ratio.
  • the larger number of filaments allows the tension applied during the drawing process to be distributed between the larger number of filaments.
  • the rotational speed of the first godet roller may be 200 to 310mpm (m/min). Use of a godet 1 speed greater than 300 mpm may increase the frequency of melt breaks. An optimum speed for godet 1 may be about 295mpm.
  • the rotational speed of the godet 5 roller may be 350 to 1665 mpm.
  • the rotational speeds of godets 2 to 4 may have intermediate values. A higher drawing ratio may be achieved using 72 filaments resulting a finer fibre of 3 dtex or greater at a godet 5 speed of 500 rpm or higher.
  • a metering pump speed may be employed. Use of a metering pump may improve stability of the process. A reduced residence time may reduce the risk of thermal degradation of the polymer.
  • a spin finish may be applied to the filaments before the fibre passes to the godet rollers.
  • a non-aqueous spin finish oil may be employed; for example, Tallopol DT, Tallopon Biocone or Vystat.
  • a spin finish content of 0.4 wt% to 4.7 wt% may be used at a spin finish pump speed of 4 to 15 rpm.
  • a minimum of 0.4 wt% of spin finish may be employed to provide sufficient cohesion between the filaments for drawing and winding.
  • Fibres in accordance with this invention may be laid to form non-woven layers or webs by various methods, including: carding, air laying or wet laying.
  • the fibres in a web may be bonded by a method selected from: hydroentanglement, needle punching, chemical or adhesive bonding and thermal bonding.
  • fibre bundles are separated and individualised using carding wires to produce an orientated fibre network structure.
  • Crimped polyvinyl alcohol fibres may be employed.
  • the opened polyvinyl alcohol fibres may be dried, for example at 130°C for 10 minutes prior to carding to improve uniformity of the resultant web. In exemplary embodiments, drying is not necessary.
  • thermally processable fibres of this invention allows manufacture on a commercial scale.
  • a blend of polyvinyl alcohol (PVOH) fibres with sustainable fibres may be employed, for example the sustainable fibres may be selected from: lyocell, polylactic acid (PLA), polyhydroxy alkanoates and mixtures thereof.
  • PVOH polyvinyl alcohol
  • a blending ratio of polyvinyl alcohol :lyocell of 70:30 wt% to 90:10 wt%, preferably 80:20 wt% or a ratio of polyvinyl alcohol:PLA of 70:30 wt% to 90: 10 wt%, preferably 80:20 wt% may be employed.
  • the carded web may have an areal density of 60 to 40gm -2 , for example about 50gm -2 .
  • 100% polyvinyl alcohol and 80:20 wt% polyvinyl alcohol:lyocell carded webs may be needlepunched at 9mm penetration depth, hydroentangled at 30 bar or chemically bonded using, for example, ethylene vinyl acetate (EVA) binder.
  • EVA ethylene vinyl acetate
  • Through air bonding in which hot air is forced through the web, for example by convection, may be employed to melt an adhesive to avoid producing excessive compression.
  • 80:20 wt% polyvinyl alcohol:PLA carded webs may be through air bonded at 120°C for 2 minutes.
  • Air laying methods may be employed, in which a turbulent air stream is used to produce an isotropic fibre network.
  • crimped polyvinyl alcohol fibres may be cut to a length of 5mm and blended with pulp fibres (approximately 2mm) Georgia Pacific (GP) cellulose.
  • pulp fibres approximately 2mm
  • GP Georgia Pacific
  • Ratios of polyvinyl alcohol: cellulose of 80:20 wt% to 20:80 wt% for example about 50:50 wt% may be employed.
  • the areal density may be about 50 gm -2 , dependent on the application, for example single or multiple use applications.
  • the polyvinyl alcohol fibres may be dried, for example at 130°C for 10 minutes, to improve separation. In exemplary embodiments, drying is not necessary.
  • the airlaid webs may be hydroentangled and then dried.
  • Fibres of this invention have the advantage that the polyvinyl alcohol fibrecontaining webs may be converted into hydroentangled airlaid non-woven fabrics having a high strength.
  • the fibres, particularly comprising warm water soluble polyvinyl alcohol, were found to partially dissolve during the hydroentanglement process resulting in strong but stiff fabrics.
  • a wetlaying process may be used to form non-woven fabrics with hot water-soluble polyvinyl alcohol fibres.
  • the polyvinyl alcohol fibres are dispersed in water and transferred onto a foraminous conveyor through which the water is removed to deposit a web of fibres.
  • the fibres may be cut to a suitable length, for example 5mm and blended with pulp fibres, for example Sodra Black, at ratios of polyvinyl alcohol:pulp of 50:50 wt% to 20:80 wt%.
  • Lyocell fibres (1.4 dtex/5mm) may be blended at ratios of polyvinyl alcohol:pulp of 50:50 wt% to 20:80 wt%.
  • the areal density may be about 60gm -2 . This density may be employed for manufacture of flushable wipes.
  • the wetlaid webs may be hydroentangled and dried at 100°C for 30 seconds.
  • the tensile strength was compared with commercial products.
  • a blend of polyvinyl alcohol:pulp:lyocell in a ratio of 40:40:20 wt% exhibited a relatively high tensile strength of 11 to 13N, typically about 12N.
  • Hydroentangled wetlaid fabrics of this invention incorporating pulp have relatively good tensile strength.
  • Pulp fibres have typically high liquid absorption capacity. After hydroentanglement, the wetlaid web remains saturated resulting in partial dissolution of the polyvinyl alcohol fibres during the drying stage.
  • the polyvinyl alcohol fibres act as a binder alongside formed hydrogen bonds between the pulp fibres.
  • the increase in specific energy during hydroentanglement may increase the dry tensile strength of the fabrics incorporating lyocell fibres.
  • Figure 1 is a diagrammatic view of fibre extruding apparatus in accordance with this invention.
  • polyvinyl alcohol homopolymer compositions may be employed.
  • FIG. 1 illustrates apparatus for extrusion of polyvinyl alcohol fibres in accordance with the present invention.
  • a feed hopper (1) supplies pellets of the polyvinyl alcohol composition to an extruder (2).
  • the molten polymer is delivered from the extruder to a melt pump (3) which meters the polymer to a spin pack (4).
  • the spin pack spins a fibre (10) through a quenching chamber (5) supplied with cooling air by a fan (11).
  • a spin finish applicator (6) applies a coating to the fibre (10).
  • the fibre is then delivered by roller (7) to a series of godet rollers (8) which produce drawn fibres.
  • the fibres are then collected on a winder (9).
  • Multifilament polyvinyl alcohol fibres were extruded using the following parameters. Parameters Drying time prior to extrusion (h) 8 Extrusion temperature (°C) 220 Metering pump speed (rpm) 9 Godet 1 speed (mpm) 295 Godet 2 speed (mpm) 297 Godet 3 speed (mpm) 500 Godet 4 speed (mpm) 515 Godet 5 speed (mpm) 530 Spin finish pump speed (rpm) 4 Spin finish content (%) 0.4 Yarn titre (dtex) 206-214 Filament count 72 Filament titre (dtex/fil) 2.9 Tenacity (cN/dtex) 3 Die hole diameter (mm) 0.25 Spin finish used Tallopol DT
  • the fibres were crimped using an IR heater temperature 220°C, speed 1.4 m/min, indented roller temperature 100°C and throughput rate 17 g/h.
  • Airlaid/Hydroentangled Composition 100% PVOH 80:20 PVOH: Lyocell 50:50 PVOH: Lyocell 20:80 PVOH: Lyocell 80:20 PVOH: hemp 50:50 PVOH: pulp Areal density (g/m 2 ) 49 47 47 36 50 50 Thickness (mm) 0.7 0.7 0.8 0.7 0.8 0.7 Dry tensile strength (N/25mm) 3.2 2.01 1.8 20.9 1.8 17.1 Wet tensile strength (N/25mm) 2.0 1.5 1.8 0.5 ⁇ 0.1 ⁇ 0.1 Dispersibility in the drainline (%) 99 99 98 95 98 100 Dispersibility in the sewer system (%) 73 69 64 19 75 100
  • the properties of wetlaid hydroentangled PVOH webs were as follows. Parameters Wetlaid/ Hydroentangled Composition 50:30:20% PVOH: Pulp: Viscose 40:40:20% PVOH: Pulp: Viscose 20:60:20% PVOH: Pulp: Viscose Areal density (g/m 2 ) 56 57 57 Thickness (mm) 0.83 0.92 1.10 Dry tensile strength (N/25mm) 13.93 12.35 13.05 Wet tensile strength (N/25mm) 6.38 4.36 2.56 Dispersibility in the drainline (%) 85 83 96 Dispersibility in the sewer system (%) 67 74 87
  • the tensile strength of webs comprising polyvinyl alcohol/pulp blends were compared with commercial flushable wipes.
  • the tensile strength was compared with lotion saturated wipes.
  • the commercial wipes were squeezed by hand to remove excess lotion.
  • the excess lotion was used to saturate the polyvinyl alcohol products of the present invention at a pick up of 200 wt% to 300 wt%.
  • the increase in the specific energy had a positive impact on the wet tensile strength of the wetlaid hydroentangled fabrics with an increase of approximately 100 to 170%.
  • the dispersibility of the wetlaid hydroentangled fabrics decreased with increased specific energy (30 bars x 2 / 50 bars x 4).
  • the fibres were more interlocked promoting fibre roping.
  • the wetlaid webs hydroentangled at high specific energy showed fragments size ⁇ 4cm which is one of the alternative requirements to pass the dispersibility in the sewer system.
  • the PVOH fibres were successfully converted into wetlaid hydroentangled fabrics.
  • the fabrics incorporating pulp fibres showed good dry and wet tensile strength and dispersibility, while the incorporation of lyocell fibres promoted the wet tensile strength but decreased the dispersibility of the hydroentangled wetlaid fabrics.
  • the commercial flushable wipes passed the dispersibility in the drainline test with more than 50 wt% passing through a 12.5mm screen.
  • the wetlaid hydroentangled polyvinyl alcohol-containing webs exhibited excellent results with more than 80 wt% passing through a 12.5 mm screen.
  • hydroentangled wetlaid non-woven polyvinyl alcohol/pulp fabrics were compared with commercial flushable wipes.
  • the commercial flushable wipes showed low dispersibility with less than 60 wt% passing through a 5.6mm sieve.
  • the hydroentangled wetlaid fabrics incorporating 20 wt% polyvinyl alcohol fibre and 80 wt% pulp exhibited excellent results with 90 wt% passing through a 5.6mm screen.
  • Webs comprising polyvinyl alcohol, pulp and viscose/lyocell exhibited better dispersibility performance in comparison to commercial flushable wipes.
  • PVOH fibres in hydroentangled wetlaid fabrics incorporating pulp fibres improved the dry tensile strength. Incorporation of viscose or lyocell fibres improved the wet strength of the fabrics. A superior combination of wet strength and dispersibility performance was achieved using 40 wt% polyvinyl alcohol, 40 wt% pulp and 20 wt% viscose fibres.
  • Process Variable Polymer G (3 dtex) Polymer G (2dtex) Extruder Zone 1 (°C) 230 232 Spin Pack (°C) 238 247 Throughput (kg/hr) 1.39 1.39 Die Head Pressure 25 20 Godet Speed 1 (rpm) 391 585 Godet Speed 5 (rpm) 1110 1665 Linear Density (dtex/ filament) 3.08 2.06 Tenacity (cN/dtex) 3.29-3.70 3.28-4.12 Extruder Zone Temperature (°C) Zone 1 225-232 Zone 2 233-237 Zone 3 235-242 Zone 4 240-247 Flange 240-247 Die Head 240-247 Metering Pump 240-247 Spin Pack 240-247

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Public Health (AREA)
  • Manufacturing & Machinery (AREA)
  • Epidemiology (AREA)
  • General Health & Medical Sciences (AREA)
  • Artificial Filaments (AREA)
  • Nonwoven Fabrics (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
EP23191132.2A 2022-08-13 2023-08-11 Fibres extrudées en alcool polyvinylique et produits fibreux Pending EP4321666A1 (fr)

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JP (1) JP2025526176A (fr)
KR (1) KR20250084915A (fr)
CN (1) CN120112686A (fr)
AU (1) AU2023327580A1 (fr)
CA (1) CA3264908A1 (fr)
MX (1) MX2025001785A (fr)
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Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB1199190A (en) * 1966-11-14 1970-07-15 Du Pont Absorbent Non-Woven Fabrics
US3997489A (en) * 1974-11-25 1976-12-14 E. I. Du Pont De Nemours And Company Melt extrudable polyvinyl alcohol compositions
WO2017046361A1 (fr) 2015-09-18 2017-03-23 Aquapak Polymers Limited Procédé et appareil pour la fabrication d'un alcool polyvinylique pouvant être traité
US20170369693A1 (en) * 2013-03-25 2017-12-28 Peter Morris Research And Development Limited Water-soluble polymer and polymer internal lubricant
WO2021067474A1 (fr) * 2019-09-30 2021-04-08 Monosol, Llc Structure composite non tissée soluble dans l'eau
WO2022008516A1 (fr) 2020-07-06 2022-01-13 Aquapak Polymers Limited Procédé de fabrication d'un mélange d'alcool polyvinylique plastifié
US20220228305A1 (en) * 2019-04-24 2022-07-21 Monosol, Llc Nonwoven water dispersible article for unit dose packaging

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CA2070589C (fr) * 1991-12-19 2000-11-28 Kimberly-Clark Corporation Methode de production de non-tisses en poly (alcool de vinyle)
JP2001123369A (ja) * 1999-10-20 2001-05-08 Kuraray Co Ltd 水解性不織布およびその製造方法
JP5767113B2 (ja) * 2008-12-23 2015-08-19 スリーエム イノベイティブ プロパティズ カンパニー パターン付きスパンボンド繊維ウェブ及びこれを作製する方法
TWI551739B (zh) * 2015-05-11 2016-10-01 Acelon Chem & Fiber Corp 製備奈米銀掺混天然纖維素紡黏不織布的方法
CN116133635A (zh) * 2020-06-27 2023-05-16 蒙诺苏尔有限公司 膜封闭的成形沐浴体验产品和其制造方法

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB1199190A (en) * 1966-11-14 1970-07-15 Du Pont Absorbent Non-Woven Fabrics
US3997489A (en) * 1974-11-25 1976-12-14 E. I. Du Pont De Nemours And Company Melt extrudable polyvinyl alcohol compositions
US20170369693A1 (en) * 2013-03-25 2017-12-28 Peter Morris Research And Development Limited Water-soluble polymer and polymer internal lubricant
WO2017046361A1 (fr) 2015-09-18 2017-03-23 Aquapak Polymers Limited Procédé et appareil pour la fabrication d'un alcool polyvinylique pouvant être traité
US20220228305A1 (en) * 2019-04-24 2022-07-21 Monosol, Llc Nonwoven water dispersible article for unit dose packaging
WO2021067474A1 (fr) * 2019-09-30 2021-04-08 Monosol, Llc Structure composite non tissée soluble dans l'eau
WO2022008516A1 (fr) 2020-07-06 2022-01-13 Aquapak Polymers Limited Procédé de fabrication d'un mélange d'alcool polyvinylique plastifié
WO2022008521A1 (fr) 2020-07-06 2022-01-13 Aquapak Polymers Limited Procédé de fabrication d'alcool polyvinylique homopolymérique plastifié et polymère d'alcool polyvinylique plastifié obtenu à partir de celui-ci

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EP4321665A1 (fr) 2024-02-14
WO2024037987A1 (fr) 2024-02-22
CA3264908A1 (fr) 2024-02-22
TWI892204B (zh) 2025-08-01
KR20250084915A (ko) 2025-06-11
TW202424296A (zh) 2024-06-16
MX2025001785A (es) 2025-03-07
AU2023327580A1 (en) 2025-03-27
CN120112686A (zh) 2025-06-06
JP2025526176A (ja) 2025-08-07

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