Classifications

• • D—TEXTILES; PAPER
  • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
  • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
  • D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
  • D06M11/32—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
  • D06M11/36—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
  • D06M11/38—Oxides or hydroxides of elements of Groups 1 or 11 of the Periodic Table
• • D—TEXTILES; PAPER
  • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
  • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
  • D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
  • D06M11/32—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
  • D06M11/50—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with hydrogen peroxide or peroxides of metals; with persulfuric, permanganic, pernitric, percarbonic acids or their salts
• • D—TEXTILES; PAPER
  • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
  • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
  • D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
  • D06M13/10—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
  • D06M13/144—Alcohols; Metal alcoholates
• • A—HUMAN NECESSITIES
  • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
  • A61F—FILTERS IMPLANTABLE INTO BLOOD VESSELS; PROSTHESES; DEVICES PROVIDING PATENCY TO, OR PREVENTING COLLAPSING OF, TUBULAR STRUCTURES OF THE BODY, e.g. STENTS; ORTHOPAEDIC, NURSING OR CONTRACEPTIVE DEVICES; FOMENTATION; TREATMENT OR PROTECTION OF EYES OR EARS; BANDAGES, DRESSINGS OR ABSORBENT PADS; FIRST-AID KITS
  • A61F13/00—Bandages or dressings; Absorbent pads
  • A61F13/15—Absorbent pads, e.g. sanitary towels, swabs or tampons for external or internal application to the body; Supporting or fastening means therefor; Tampon applicators
  • A61F13/53—Absorbent pads, e.g. sanitary towels, swabs or tampons for external or internal application to the body; Supporting or fastening means therefor; Tampon applicators characterised by the absorbing medium
  • A61F2013/530131—Absorbent pads, e.g. sanitary towels, swabs or tampons for external or internal application to the body; Supporting or fastening means therefor; Tampon applicators characterised by the absorbing medium being made in fibre but being not pulp
  • A61F2013/530343—Absorbent pads, e.g. sanitary towels, swabs or tampons for external or internal application to the body; Supporting or fastening means therefor; Tampon applicators characterised by the absorbing medium being made in fibre but being not pulp being natural fibres
  • A61F2013/530357—Absorbent pads, e.g. sanitary towels, swabs or tampons for external or internal application to the body; Supporting or fastening means therefor; Tampon applicators characterised by the absorbing medium being made in fibre but being not pulp being natural fibres of wool
• • D—TEXTILES; PAPER
  • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
  • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
  • D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
  • D06M2101/02—Natural fibres, other than mineral fibres
  • D06M2101/10—Animal fibres
  • D06M2101/12—Keratin fibres or silk

Definitions

• the present invention relates to a wool treatment process and to a wool product produced by the wool treatment process.
• the invention relates to a wool treatment process that produces a wool product with increased absorbency properties and to a wool product that has increased absorbency properties.
• Disposable diapers contain chemical compounds such as super-absorbent polymers, polypropylene, adhesives, elastics and pulp. Large volumes of these products end up in landfills, and take long periods of time to degrade, causing long-term harm to the environment.
• biodegradable and environmentally friendly products that are reasonably priced and still provide the absorbency needed for such products.
• Absorbent products are needed in other situations such as in domestic, commercial and industry cleaning and when dealing with fluid spills, as well as for personal hygiene and health products, such as diapers, nappies, as nursing pads and wound and surgical dressings. Also, there is a need for absorbent clothing for sports, outdoor activities and general everyday fashion items.
• Wool is a natural product which has many characteristics that make it a product or product ingredient of choice for today's environmental and health conscious consumers. Important characteristics of wool are that it is renewable,
• the present invention provides a process for treating a wool substrate comprising: a first reaction step of treating the wool substrate with an alcohol and alkali reaction mixture for a reaction time of between about 5 - 60 minutes; and a second reaction step of treating the resulting wool substrate obtained from the first reaction step with an aqueous oxidizing agent mixture.
• the wool substrate used in the first reaction step is a chemically untreated nonwoven wool substrate.
• the wool substrate used in the first reaction step is a chemically untreated knop-infused nonwoven substrate.
• the wool substrate used in the first reaction step is selected from (i) a needle punched or (ii) spunlaced (hydroentangled) wool nonwoven comprising layered spunbonded or carded wool fibres.
• the wool substrate has a density of between about 100 - 1000 grams per square meter. In one embodiment the wool substrate has a density of between about 200 - 600 grams per square meter.
• the wool substrate used in the first reaction step comprises loose wool fibres, preferably raw but scoured untreated wool fibres.
• the alcohol is selected from methanol, ethanol, propanol, butanol or mixtures thereof.
• the alkali is selected from potassium hydroxide or sodium hydroxide or mixtures thereof.
• the alkali concentration in the alcohol mixture is between about 0.5 - 5%.
• the alkali concentration in the alcohol mixture is between about 1 - 2%. More preferably the alkali concentration in the alcohol mixture is about 1 .5%.
• the oxidizing agent is hydrogen peroxide.
• the oxidizing agent concentration in the aqueous mixture is between about 0.5 - 5%.
• the oxidizing agent concentration in the aqueous mixture is about 1 - 2%. More preferably the oxidizing agent
• concentration in the aqueous mixture is about 2.0%.
• reaction time of the first reaction step is between about 5 - 30 minutes. More preferably the reaction time of the first reaction step is between about 10 - 30 minutes. Where the wool substrate is a nonwoven wool substrate, the preferred reaction time of the first reaction step is about 10 minutes. Where the wool substrate comprises loose wool fibres, the preferred reaction time of the first reaction step is about 12 to 14 minutes.
• reaction time of the second reaction step is between about 30 - 180 minutes.
• reaction time of the second reaction step is between about 30 - 120 minutes. More preferably the reaction time of the second reaction step is between about 30 - 90 minutes. Most preferably the reaction time of the second reaction step is about 60 minutes.
• the process of the invention is carried out with a fibre to liquor ratio of 1 :10 to 1 :40.
• the present invention provides a wool product obtained by the process defined above, wherein the wool product has absorbency properties at least 800% greater than an untreated wool substrate.
• the wool product has absorbency properties at least 1000% greater than the untreated wool substrate. In another embodiment the wool product has absorbency properties at least greater than 1200% greater than an untreated wool substrate.
• the treated wool has absorbency properties at least 1500% greater that the untreated loose wool fibres, and up to 2400% greater that the untreated loose wool fibres.
• the wool product is further used in one or more products requiring a material with absorbent properties.
• products include personal hygiene products such as diapers, diaper liners, nappies and the like, wound dressings or surgical dressings and the like, chemical spill or clean up products and the like, and sporting, outdoor and general everyday fashion garments.
• Figure 1 is a flow diagram of a process for treating wool according to one aspect of the present invention.
• Figure 2 shows the results of the absorbency testing evaluated by the contact angle ( ⁇ ) using a goniometer measurement technique. The absorbency was measured after the alkali first reaction step then after the oxidative second reaction step.
• Figures 3(a) and 3(b) show photos of the comparative absorbency results of an untreated wool substrate 3(a) compared to a treated wool substrate 3(b) in the presence of an ink sample.
• Figure 4 shows an absorption experimental set up for the immersion stage of wool fibre substrate treatment.
• Figure 5 shows an absorption experimental set up for the draining stage of wool fibre substrate treatment.
• Figure 6 shows the carded treated wool fibre substrate compared to a control sample.
• Figure 7 shows the standard test method absorbency data of the treated wool fibre substrate.
• Figure 8 shows the simulated sanitary absorbency of the treated wool fibre substrate.
• Figure 9 shows the percentage fibre loss during hand carding of the treated wool fibre substrate.
• Figures 10-17 show low and high magnification scanning electron micrographs of 8 samples of treated wool fibre substrate.
• wool substrate includes a raw wool substrate, such as raw sheep's wool, loose wool fibres, including raw untreated wool fibres, cashmere, mohair, angora, 100% crossbred wool; merino wool, a raw wool substrate that has been washed and dried; a raw wool substrate that has been washed, dried and has been needled into a nonwoven web or pad.
• the wool substrate preferably has a density of between 100-1000 grams per square metre, such as 100 gsm, 200 gsm, 400gsm, 600gsm, 800gsm or 1000 gsm.
• the wool treatment process of the present invention produces a wool product with increased absorbency properties, making the wool produced by the treatment process of the present invention a useful absorbent product or a useful ingredient for products that require absorbency, such as diapers, diaper liners, wound and surgical dressing, incontinence pads or the like, as well as for activewear garments used in sports, outdoor activities and everyday activities.
• the present invention provides a process for treating a wool substrate comprising: a first reaction step of treating the wool substrate with an alcohol and alkali reaction mixture for a reaction time of between about 5 - 60 minutes; and a second reaction step of treating the resulting wool substrate obtained from the first reaction step with an aqueous oxidizing agent mixture.
• the alkali concentration in the alcohol mixture is about 0.5 - 5%.
• the alkali concentration in the alcohol mixture is about 1 - 2%. More preferably the alkali concentration in the alcohol mixture is about 1 .5%.
• the alcohol and alkali reaction mixture comprises a mixture of ethanol and potassium hydroxide.
• the alcohol and alkali reaction mixture comprises about 1 .5% sodium hydroxide (for example, 2.8 kg of sodium hydroxide in 217 litres of ethanol). In another embodiment, the alcohol and alkali reaction mixture comprises about 1 .5% potassium hydroxide (for example 3.0 kg of potassium hydroxide in 200 litres of 96% ethanol).
• the oxidizing agent concentration in the aqueous mixture is about 0.5 - 5%.
• the oxidizing agent concentration in the aqueous mixture is about 1 - 2%. More preferably the oxidizing agent concentration in the aqueous mixture is about 2.0%.
• the oxidizing agent is hydrogen peroxide.
• the aqueous oxidizing agent mixture comprises 2% hydrogen peroxide (for example 9 litres 50% hydrogen peroxide in 224 litres of water).
• reaction time of the first reaction step is between about 5 - 30 minutes. More preferably the reaction time of the first reaction step is between about 10 - 30 minutes. Where the wool substrate is a nonwoven wool substrate, the preferred reaction time of the first reaction step is about 10 minutes. Where the wool substrate comprises loose wool fibres, the preferred reaction time of the first reaction step is about 12 - 14 minutes.
• reaction time of the second reaction step is between about 30 - 180 minutes.
• reaction time of the second reaction step is between about 30 - 120 minutes. More preferably the reaction time of the second reaction step is between about 30 - 90 minutes. Most preferably the reaction time of the second reaction step is about 60 minutes.
• the process of the invention is carried out with a fibre to liquor ratio of 1 :10 to 1 :40.
• the preferred ratio will depend on the nature and amount of the wool substrate being treated, the size of the reaction vessel and such like.
• the reagents in particular the alcohol
• the reagents are recovered and recycled where possible, reducing cost and harmful waste.
• the process includes the further step of rinsing the wool substrate with water between the first and second reaction steps.
• the process includes the further step of rinsing the wool product with water after the second reaction step.
• the process includes the further step of rinsing and then drying the wool product after the second reaction step.
• the wool substrate comprises 100% crossbred wool (approximately 35 - 42 micron).
• the process is preferably applied to a non-woven wool substrate.
• the non-woven wool substrate is 400 grams per square metre (gsm), although the non-woven wool substrate can also be of other densities such as 200 or 600 gsm.
• the non-woven wool substrate is produced in rolls of approximately 1 .5 metres by 30 metres, although it will be appreciated that any suitable width and/or length may be used.
• the process is applied to a loose wool fibre substrate.
• the process of the present invention is a wet treatment that impacts the entire wool fibre structure (the wool surfaces and also the wool matrix).
• the wool fibre undergoes relaxation through chemical changes (breaking and reforming the structure of the wool fibre bonds). More specifically, alkaline -OH ions break the disulfide bonds through the interaction of acidic hydrogen atoms next to the sulfur atoms and that allows the wool material to become significantly absorbent.
• the treatment process of the present invention produces a highly absorbent wool product, for example a treated wool substrate.
• the wool product is able to absorb up to 1200 - 1500% of its weight in moisture (compared with 30% for wool that has not treated by the process of the present invention).
• the wool product is able to absorb up to 2400% of its weight in moisture.
• Useful properties of the wool product of the present invention may include:
• the wool product of the present invention may be used in a variety of applications including domestic, commercial and industrial cleaning products and cleaning accessories, beauty cleaning aids (such as facial masks, exfoliating wipes/gauze, soap dispensers and scrubbing aids), diaper components (such as soaker pads, acquisition layer and nappy liners), toilet training bed pads & booster pads, nursing pads for mothers, incontinence pads and pants, animal toilet pads, pet beds, petroleum and mechanical fluid spills, aids to absorb any fluids exposed to electronic devices, medical devices (such as wound care dressings, surgical gowns, surgical gauze and body warmers), fashion activewear garments for sports, outdoor activities and everyday activities.
• a process according to one preferred embodiment of the present invention is shown in Figure 1 of the accompanying drawings.
• the treatment process involves preliminary or pre-treatment steps of preparing the first reagent and the second reagent.
• Wool for example a roll of non-woven wool substrate
• the wool substrate is retained in the bath of the first reaction mixture for a predetermined period of time, for example about 5 - 60 minutes.
• the wool substrate is removed from the bath and drained.
• the first reaction mixture is further processed, to recover ethanol (which may be re-used).
• the treated wool substrate is then rinsed using water. Several rinsing cycles can be employed.
• the wool substrate obtained from the first reaction step is treated by immersion into a bath containing the second reaction mixture.
• the wool substrate is retained in the bath of the first reagent for a predetermined period of time, for example about 60 - 180 minutes.
• the wool substrate is removed from the bath, drained and rinsed with water. Again, several rinsing cycles can be employed.
• the wool substrate is dried, to produce the treated wool product of the present invention.
• the reagents used in the process of the present invention will be at a temperature of about 20°C (ie room temperature), and typically the process will be carried out at about 20°C (ie room temperature).
• An appropriate wool substrate(s) was selected (such as 200 gsm, 400 gsm or 600 gsm wool substrate). The total size and weight of the wool substrate was measured and determined.
• a suitable dry and clean treatment vessel (preferably glass or stainless steel) was selected.
• the wool substrate for example, a 400 gsm wool substrate
• the treatment solution consisting of 1 .5% KOH in EtOH concentration for 20 minutes (preferably without agitation) at room
• the treatment solution was recovered for reuse, or used to treat a second batch or third batch of wool substrate, if practicable.
• the treated wool substrate was then rinsed (preferably, at least 5 times) in reverse osmosis (RO) water at room temperature.
• the process may include drying the wool substrate prior to applying the hydrogen peroxide (H2O2) treatment step.
• Option 1 The total requirement of H2O2 was calculated and added into the reaction vessel and filled with water until the desired concentration (i.e. 2%) was obtained.
• the wool sample was conditioned for 48 hours (20°C, 65% relative humidity) prior to treatment with a formulated treatment solution containing KOH/EtOH at various concentrations e.g. 1 %, 1 .5% and 2% over diverse time periods e.g. 10 minutes, 20 minutes and 30 minutes.
• a formulated treatment solution containing KOH/EtOH at various concentrations e.g. 1 %, 1 .5% and 2% over diverse time periods e.g. 10 minutes, 20 minutes and 30 minutes.
• KOH/EtOH was applied to treat 100mm circular diameter wool samples at room temperature over time periods of 10 minutes, 20 minutes and 30 minutes
• pre-treated sample were then individually treated (i.e. post-treated) with 2% H 2 O 2 at room temperature over time periods of 60 minutes, 90 minutes, and 120 minutes.
• pre-treatment experiments were conducted to treat wool samples using 1 .5%, 2% concentration of KOH/EtOH, followed by post-treatment using H 2 O 2 solution at the above mentioned conditions. The results are detailed in Table 1 below.
• Table 1 The variables tested, their concentration and conditions for the treatment of wool substrates (400gsm and 200gsm) were as follows.
• Table 2 Grouped descriptive statistics for water-saline absorbency percentages (200gsm wool substrates).
• Table 3 Grouped descriptive statistics for water-saline absorbency percentages (400gsm wool substrates)
• Figures 3(a) and 3(b) clearly show the comparative absorbency of an untreated wool substrate in 3(a) compared to a treated wool substrate 3(b) in the presence of an ink sample.
• Figure 3(a) shows the hydrophobicity of an untreated wool pad and the ink beading on the surface of the wool substrate.
• Figure 3(b) shows the ink has been readily absorbed into the wool substrate without any beading at all on the surface of the wool substrate.
• the water-saline absorbency percentages are shown in Table 4 below. It can be seen from the results that there were no significant differences observed between the absorbency of the resulting wool substrate from the fresh treatment reaction mixture of KOH/EtOH and resulting wool substrate from the re-used reaction mixture of KOH/EtOH in cycles 1 -3. This strongly suggests that the first reaction mixture can be re-used over a number of treatment cycles without compromising the absorbency results obtained. It is also to be appreciated that the EtOH can be recovered by distillation from the reaction mixture.
• Table 4 Water-saline absorbency percentages and descriptive statistics results that illustrate the reusability of the KOH/EtOH reaction mixture (for an exposure duration of 10 mins) whilst still producing high absorbent wool products for a 400gsm wool substrate over 4 reaction cycles.
• Wool fibre was supplied from a Hawkes Bay wool scourer.
• the fibre was scoured strong wool (3/4 Romney breed, second shear) having good colour and low vegetable matter, with an estimated mean fibre diameter in the range 35 - 42 micron and estimated staple length of 100 - 120 mm.
• RO Reverse osmosis
• the Total Absorbency Capacity (ISO 1 1948:1 -1998) was tested for each of the treatment samples.
• the sample size was 10 cm x 10 cm (5 repeats for each variant).
• a simulated sanitary absorbency experiment was also carried out. For each treatment time one additional sample was run with 250 ml of solution being poured evenly onto the sample (covered by metal mesh and on top of plastic mesh). This was allowed to soak for 5 minutes and then drained for 5 minutes before weighing. This technique was trialled as it represented the mode of action for sanitary or nappy (diaper) type products, in terms of comparable liquid volume application from above, rather than below.
• a rectangle of conditioned, black, knitted wool fabric 25 cm x 20 cm was cut for each sample. This was then weighed before being spread out on a flat surface. A precisely weighed 5 g sample of each treatment duration was taken from the bulk material and then hand-carded in turn above a fabric piece.
• SEM Scanning electron microscopy
• Treated samples from 8 to 14 minutes inclusive do not have any significant signs of fibre damage in excess of what is normally found on scoured wool fibres (control sample). Once the treatment time reaches 16 minutes there are visible signs of damage to the surface of the fibres. In particular there is evidence of longitudinal 'wrinkles' forming on the fibres; these are more severe on the 18 and 20 minute samples.
• Figures 10-17 show the scanning electron microscopy images obtained from the different treatment samples.
• Table 6 Total Absorbancy, average and standard deviation
• Table 7 Simulated sanitary absorbancy
• the average total absorbency capacity of the treated samples ranged from 1884 - 2502%, with the untreated samples having an average of 473%.
• the treated sample with the lowest absorbency was the 20 minute sample (longest duration).
• the standard deviation was lowest for the 20 minute sample and highest for the 8 minute sample, with the remaining samples having similar standard deviations (including the control sample). This could be an indication of the levelness of the fibre treatment, with 8 minutes not allowing sufficient time for the liquor to penetrate and react evenly throughout the fibre bundles, meaning that samples taken from different regions of the treated material would behave differently.

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• Engineering & Computer Science (AREA)
• Textile Engineering (AREA)
• Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
• Chemical Or Physical Treatment Of Fibers (AREA)

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• 2015
  • 2015-04-01 JP JP2018502341A patent/JP6652629B2/ja active Active
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  • 2015-06-01 CN CN201510294002.0A patent/CN106167985A/zh active Pending
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