Method of treating wool and product

By treating wool substrate with an aqueous oxidant after the reaction of alcohol and alkali, its structure is changed, the absorbency of wool is improved, the environmental pollution and insufficient absorbency of existing products are solved, and an environmentally friendly absorbent material is provided.

CN113494021BActive Publication Date: 2026-02-10ULCHEMY ENGINE LTD
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Patent Information

Application Number
CN202110787935.9
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Priority Date
2015-04-01
Filing Date
2015-06-01
Publication Date
2026-02-10
Estimated Expiration
2035-06-01

AI Technical Summary

Technical Problem

Existing disposable absorbent products such as diapers and pads contain chemicals that cause environmental pollution and are difficult to degrade. Furthermore, wool, as a natural material, is hydrophobic and has limited absorbency, failing to meet the requirements for environmental friendliness.

Method used

By treating wool substrate with an alcohol and alkali reaction mixture, followed by treatment with an aqueous oxidant mixture, the wool fiber structure is altered, giving it significant absorption properties.

Benefits of technology

The absorbency of wool products is increased to 800-2400% of that of untreated wool products. They can be used in a variety of absorbent products, including personal hygiene products, wound dressings and sportswear, and are biodegradable and free of chemicals.

✦ Generated by Eureka AI based on patent content.

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Abstract

The present invention relates to a wool treatment method and a wool product produced by the wool treatment method. In particular, the present invention relates to a wool treatment method for producing a wool product having enhanced absorbency and a wool product having enhanced absorbency.
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Description

TECHNICAL FIELD

[0001] The present invention relates to a wool treatment method and to a wool product produced by the wool treatment method. In particular, the present invention relates to a wool treatment method for producing a wool product having enhanced absorbency and to a wool product having enhanced absorbency. BACKGROUND

[0002] One aspect of concern to today's environmentally and health conscious consumers is the large amount of non-biodegradable waste generated by disposable products such as diapers, pads and incontinence pads. Disposable diapers contain chemical compounds such as superabsorbent polymers, polypropylene, adhesives, elastomers and pulp. Large amounts of these products end up in landfills and take a considerable amount of time to degrade, resulting in long-term harm to the environment.

[0003] Many consumers are seeking alternatives to currently available products of this type. Consumers are particularly seeking odorless, chemical free, biodegradable and environmentally friendly products that are reasonably priced and still provide the absorbency required of such products.

[0004] Absorbent products are also needed in other situations such as in household, commercial and industrial cleaning and when dealing with fluid spills, and for personal hygiene and healthcare products such as diapers, nappies, as breast pad and wound and surgical dressings. Also, there is a demand for absorbent clothing for sports, outdoor activities and general everyday fashion items.

[0005] Wool is a natural product that has many properties that make it a product or product component of choice for today's environmentally and health conscious consumers. Important properties of wool are that it is renewable, biodegradable, hypoallergenic, breathable, a natural insulator, durable, elastic and washable. However, wool as a natural product in its untreated form is hydrophobic and has very limited absorbency.

[0006] There is therefore a need to provide an absorbent material that is reasonably priced, derived from a naturally occurring and renewable source and acceptable to an increasing number of environmentally and health conscious consumers. There is a further need to provide at least a useful alternative to currently available absorbent materials. SUMMARY

[0007] In a first aspect, the present invention provides a method of treating a wool substrate comprising:

[0008] a first reaction step of treating the wool substrate with an alcohol and base reaction mixture and for a reaction time of about 5 minutes to 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.

[0009] In one embodiment, the wool substrate used in the first reaction step is a chemically untreated, nonwoven wool substrate.

[0010] In another embodiment, the wool substrate used in the first reaction step is a chemically untreated, knop-impregnated nonwoven substrate.

[0011] In another embodiment, the wool substrate used in the first reaction step is selected from (i) needle-punched or (ii) hydroentangled wool nonwovens comprising layered spunbonded or combed wool fibers.

[0012] In another embodiment, the wool substrate has a density of approximately 100 g / m² to 1000 g / m². In one embodiment, the wool substrate has a density of approximately 200 g / m² to 600 g / m².

[0013] In another embodiment, the wool substrate used for the first reaction step comprises loose wool fibers, preferably unprocessed but washed-out untreated wool fibers.

[0014] In one embodiment, the alcohol is selected from methanol, ethanol, propanol, butanol, or mixtures thereof.

[0015] In one embodiment, the base is selected from potassium hydroxide or sodium hydroxide or a mixture thereof.

[0016] In one embodiment, the base concentration in the alcohol mixture is about 0.5%-5%. Preferably, the base concentration in the alcohol mixture is about 1%-2%. More preferably, the base concentration in the alcohol mixture is about 1.5%.

[0017] In one embodiment, the oxidant is hydrogen peroxide.

[0018] In one embodiment, the concentration of the oxidant in the aqueous mixture is about 0.5-5%. Preferably, the concentration of the oxidant in the aqueous mixture is about 1-2%. More preferably, the concentration of the oxidant in the aqueous mixture is about 2.0%.

[0019] In one embodiment, the reaction time of the first reaction step is about 5-30 minutes. More preferably, the reaction time of the first reaction step is about 10-30 minutes. When the wool substrate is a nonwoven wool substrate, the preferred reaction time of the first reaction step is about 10 minutes. When the wool substrate contains loose wool fibers, the preferred reaction time of the first reaction step is about 12-14 minutes.

[0020] In one embodiment, the reaction time of the second reaction step is about 30-180 minutes. Preferably, the reaction time of the second reaction step is about 30-120 minutes. More preferably, the reaction time of the second reaction step is about 30-90 minutes. Most preferably, the reaction time of the second reaction step is about 60 minutes.

[0021] In one embodiment, the method of the present invention is carried out with a fiber-to-liquid ratio of 1:10 to 1:40.

[0022] In a second aspect, the present invention provides a wool product obtained by the above method, wherein the wool product has an absorption capacity that is at least 800% higher than that of an untreated wool substrate.

[0023] In one embodiment, the wool product has an absorption capacity at least 1000% higher than that of an untreated wool substrate. In another embodiment, the wool product has an absorption capacity at least greater than 1200% higher than that of an untreated wool substrate.

[0024] When the wool substrate contains loose wool fibers, the treated wool has an absorption capacity that is at least 1500% higher than that of untreated loose wool fibers, and up to 2400% higher than that of untreated loose wool fibers.

[0025] In one implementation, the wool product is further used in one or more products that require absorbent materials. Such products include personal hygiene products (e.g., diapers, pads, cloth diapers, etc.), wound dressings or surgical dressings, chemical spill or cleaning products, and sports, outdoor, and general everyday clothing.

[0026] This invention summary provides a general description of the features and advantages of certain embodiments of the invention. Further features and advantages will be described in the detailed description of the invention below.

[0027] The novel features considered to be inventive will be better understood through this detailed description when considered in conjunction with the accompanying drawings and embodiments. However, the drawings and examples are intended to help illustrate the invention or aid in understanding it, and are not intended to limit or restrict the scope of the invention. Brief description of the attached diagram

[0028] Figure 1 : A flowchart of a method for processing wool according to one aspect of the present invention.

[0029] Figure 2 This shows the results of an absorbency test evaluated by contact angle (θ) using goniometer measurement techniques. Absorbency was measured after the alkaline first reaction step and then after the oxidizing second reaction step.

[0030] Figure 3(a) and 3(b) Photographs showing the comparative absorbency results of untreated wool substrate 3(a) and treated wool substrate 3(b) in the presence of ink samples.

[0031] Figure 4 : This shows the absorption test established during the impregnation stage of the treatment of wool fiber substrate.

[0032] Figure 5 : This shows the absorption experiment set up during the drainage stage of the treatment of wool fiber substrate.

[0033] Figure 6 : Shows a combed wool fiber substrate compared to a control sample.

[0034] Figure 7 This shows the standard test data for absorbance of the treated wool fiber substrate.

[0035] Figure 8 : This shows the absorbency of a simulated hygiene product on a treated wool fiber substrate.

[0036] Figure 9 : Indicates the percentage of fiber loss in the wool fiber substrate treated during hand combing.

[0037] Figures 10-17 : Showing low- and high-magnification scanning electron micrographs of eight samples of treated wool fiber substrates. Invention Details

[0038] Before describing the invention in detail, it is helpful to provide definitions for certain terms used in this specification.

[0039] The term "about" used in relation to reference numerical values ​​means that the reference numerical value is plus or minus up to 10% of the reference numerical value. For example, the phrase "about 50" units covers a range of 45 to 55 units.

[0040] The term "wool substrate" as used includes unprocessed wool substrates, such as unprocessed sheep wool, loose wool fibers (including unprocessed, untreated wool fibers), cashmere, mohair, Angora goat wool, 100% hybrid wool; Merino wool; washed and dried unprocessed wool substrates; and washed, dried, and needle-punched unprocessed wool substrates into nonwoven webs or mats. Wool substrates preferably have a density of 100-1000 g / m², such as 100 g / m², 200 g / m², 400 g / m², 600 g / m², 800 g / m², or 1000 g / m².

[0041] The wool processing method of the present invention produces wool products with enhanced absorbency, making the wool produced by the processing method of the present invention a useful component of absorbent products or products requiring absorbency, such as diapers, incontinence pads, wound and surgical dressings, urinary incontinence pads, and sportswear for sports, outdoor activities and daily activities.

[0042] In a first aspect, the present invention provides a method for processing a wool substrate, comprising:

[0043] A first reaction step involves treating the wool substrate with an alcohol and alkali reaction mixture for approximately 5-60 minutes; and a second reaction step involves treating the wool substrate obtained from the first reaction step with an aqueous oxidizing agent mixture.

[0044] In one embodiment, the base concentration in the alcohol mixture is about 0.5-5%. Preferably, the base concentration in the alcohol mixture is about 1-2%. More preferably, the base concentration in the alcohol mixture is about 1.5%.

[0045] In one embodiment, the alcohol and base reaction mixture comprises a mixture of ethanol and potassium hydroxide.

[0046] In one embodiment, the alcohol and base reaction mixture contains about 1.5% sodium hydroxide (e.g., 2.8 kg of sodium hydroxide in 217 liters of ethanol). In another embodiment, the alcohol and base reaction mixture contains about 1.5% potassium hydroxide (e.g., 3.0 kg of potassium hydroxide in 200 liters of 96% ethanol).

[0047] In one embodiment, the concentration of the oxidant in the aqueous mixture is about 0.5-5%. Preferably, the concentration of the oxidant in the aqueous mixture is about 1-2%. More preferably, the concentration of the oxidant in the aqueous mixture is about 2.0%.

[0048] In one embodiment, the oxidant is hydrogen peroxide.

[0049] In one embodiment, the aqueous oxidant mixture contains 2% hydrogen peroxide (e.g., 9 liters of 50% hydrogen peroxide in 224 liters of water).

[0050] In one embodiment, the reaction time of the first reaction step is about 5-30 minutes. More preferably, the reaction time of the first reaction step is about 10-30 minutes. When the wool substrate is a nonwoven wool substrate, the preferred reaction time of the first reaction step is about 10 minutes. When the wool substrate contains loose wool fibers, the preferred reaction time of the first reaction step is about 12-14 minutes.

[0051] In one embodiment, the reaction time of the second reaction step is about 30-180 minutes. Preferably, the reaction time of the second reaction step is about 30-120 minutes. More preferably, the reaction time of the second reaction step is about 30-90 minutes. Most preferably, the reaction time of the second reaction step is about 60 minutes.

[0052] In one embodiment, the method of the present invention is carried out at a fiber-to-liquid ratio of 1:10 to 1:40. Preferred ratios will depend on the nature and amount of the wool substrate being treated, the size of the reaction vessel, etc.

[0053] In one implementation, reagents (especially alcohols) are recovered and reused, where possible, to reduce costs and hazardous waste.

[0054] In another embodiment, the method includes an additional step of rinsing the wool substrate with water between the first and second reaction steps.

[0055] In another embodiment, the method includes additional steps such as rinsing the wool product with water after the second reaction step.

[0056] In another embodiment, the method includes additional steps such as rinsing and subsequently drying the wool product after the second reaction step.

[0057] Preferably, the wool substrate comprises 100% hybrid wool (approximately 35-42 microns).

[0058] This method is preferably applied to nonwoven wool substrates.

[0059] In one embodiment of the invention, the nonwoven wool substrate has a density of 400 grams per square meter (gsm), however, the nonwoven wool substrate may also have other densities, such as 200 gsm or 600 gsm.

[0060] In one implementation, the nonwoven wool substrate is produced in rolls of approximately 1.5 meters by 30 meters; however, it should be understood that any suitable width and / or length may be used.

[0061] In another embodiment, the method is applied to a loose wool fiber substrate.

[0062] Not wishing to be limited by any particular theory, the method of this invention is considered a wet treatment that affects the overall wool fiber structure (wool surface and wool matrix). Wool fibers undergo relaxation (breaking and reorganizing the structure of wool fiber bonds) through chemical changes. More specifically, basic -OH ions break disulfide bonds by interacting with acidic hydrogen atoms adjacent to sulfur atoms, thus making the wool material significantly absorbent.

[0063] The processing method of the present invention produces highly absorbent wool products, such as treated wool substrates. In a preferred embodiment, the wool product is capable of absorbing up to 1200-1500% of its weight in moisture (compared to 30% for wool not treated by the method of the present invention). In another preferred embodiment, the wool product is capable of absorbing up to 2400% of its weight in moisture.

[0064] The useful properties of the wool products of the present invention may include: super absorbency, odor resistance, antimicrobial properties (through natural wicking of moisture and breathability of the material), chemical-free, non-synthetic and non-petroleum, rash-reducing, flame retardant, temperature-controlled, hypoallergenic, warm, comfortable, breathable, biodegradable and compostable, renewable and sustainable wool products that can be cut or shaped into any desired shape suitable for the desired purpose.

[0065] The wool products of this invention can be used in a variety of applications, including household, commercial and industrial cleaning products and cleaning accessories; beauty cleaning aids (e.g., face masks, exfoliating wipes / gauze, soap dispensers and scrubbing aids); diaper assemblies (e.g., soaking pads, catch layers and diaper pads); potty training base pads & booster pads; nursing pads for mothers; incontinence pads and pants; animal potty pads; pet bedding; oil and mechanical fluid spills; aids for absorbing any fluids exposed to electronic devices; medical devices (e.g., wound care dressings, surgical gowns, surgical gauze and body warmers); and fashionable sportswear for sports, outdoor activities and daily activities.

[0066] In the attached diagram Figure 1 The present invention is illustrated in a preferred embodiment.

[0067] In this embodiment of the invention, the processing method includes a preliminary or pretreatment step for preparing a first reagent and a second reagent.

[0068] Once the reagent is prepared, the treatment method begins. Wool (e.g., a roll of nonwoven wool substrate) is immersed in a bath containing the first reaction mixture for treatment. The wool substrate remains in the bath with the first reaction mixture for a predetermined period of time, for example, about 5-60 minutes.

[0069] The wool substrate is removed from the bath and drained. The first reaction mixture is further processed to recover ethanol (which is reusable).

[0070] The treated wool substrate is then rinsed with water. Multiple rinsing cycles can be used.

[0071] In the second reaction step of the treatment method, the wool substrate obtained from the first reaction step is immersed in a bath containing a second reaction mixture for treatment. The wool substrate remains in the bath with the second reagent for a predetermined time period, for example, about 60-180 minutes.

[0072] Remove the wool substrate from the bath, drain it, and rinse it with water. Multiple rinsing cycles can also be used.

[0073] After rinsing, the wool substrate is dried to produce the treated wool product of the present invention.

[0074] Typically, the reagents used in the methods of the present invention are at a temperature of about 20°C (i.e., room temperature), and the methods are typically carried out at about 20°C (i.e., room temperature).

[0075] The invention will now be described with reference to embodiments.

[0076] experiment

[0077] Example 1 - Reaction Conditions

[0078] 1) Preparation of a 1.5% potassium hydroxide (KOH) ethanol (EtOH) solution:

[0079] 200 liters of EtOH containing 3.0 kg KOH particles or 400 liters of EtOH containing 6.0 kg KOH (preparing small amounts at higher concentrations is found to be most practical; for example, 3.0 kg in 20 liters, then appropriately diluted with EtOH to obtain a 1.5% KOH solution).

[0080] (1a) Add 20 liters of EtOH to a clean container (glass, stainless steel, or suitable plastic).

[0081] (1b) Slowly add 3.0 kg of KOH granules to (1a) and mix until all KOH granules are completely dissolved (Note: the mixture / container may generate some heat).

[0082] (1c) Then add an appropriate amount of EtOH to (1a) until a total KOH concentration of 1.5% in EtOH is obtained.

[0083] 2) Select a suitable wool substrate (e.g., 200gsm, 400gsm, or 600gsm wool substrate). Measure and determine the total dimensions and weight of the wool substrate.

[0084] 3) Treatment / processing scheme for EtOH containing 1.5% KOH:

[0085] (3a) Select a suitable dry and clean processing dish (preferably glass or stainless steel).

[0086] (3b) Add sufficient 1.5% KOH EtOH solution (prepared in advance) to the container (3a) and transport it carefully (using appropriate safety equipment and conditions).

[0087] (3c) Add wool substrate (e.g., 400 gsm wool substrate) and immerse it completely in a treatment solution containing 1.5% KOH in EtOH for 20 minutes at room temperature (20°C ± 2°C) (preferably without stirring).

[0088] (3d) If feasible, the treatment solution can be recycled for reuse or used to treat a second or third batch of wool substrate.

[0089] (3e) The treated wool substrate is then rinsed in reverse osmosis (RO) water at room temperature (preferably at least 5 times). The method may include drying the wool substrate prior to the application of hydrogen peroxide (H2O2) treatment.

[0090] 4) Preparation of a 2% aqueous solution of hydrogen peroxide (H2O2):

[0091] Option 1: Calculate the total amount of H2O2 required and add it to the reactor vessel, then fill with water until the desired concentration (i.e., 2%) is obtained.

[0092] Option 2:

[0093] (4.2a) Add 100 liters of RO water to a clean container (glass, stainless steel, or suitable plastic).

[0094] (4.2b) Add 1.5 kg of H2O2 (diluted to 30%) to (4.2a) and mix at room temperature to ensure uniform dissolution of H2O2. Add an appropriate amount of water to (4.2a) to obtain a 2% H2O2 concentration.

[0095] (4.2c) Processing conditions: A total exposure / treatment time of 60 minutes without agitation at room temperature (20°C ± 2°C) is preferred. This is followed by rinsing with water at least 5 times before drying (using hot air or other methods). Drying should not exceed 120°C, otherwise it may cause yellowing of the substrate.

[0096] Example 2 - Optimization of Reaction Conditions

[0097] 100% New Zealand sheep wool matrix (needle-punched wool nonwoven substrate) samples cut into circles with a diameter of 100 mm and a mass of 200 gsm or 400 gsm were used as substrates. Potassium hydroxide (KOH), 97.6% anhydrous ethanol (EtOH), hydrogen peroxide, and ammonium solution were used for pretreatment / posttreatment of the wool substrates.

[0098] Wool samples were acclimatized for 48 hours (20°C, 65% relative humidity) and then treated for different time periods (e.g., 10 minutes, 20 minutes, and 30 minutes) with prepared treatment solutions containing different concentrations (e.g., 1%, 1.5%, and 2%) of KOH / EtOH. Using a pretreatment method with 1% KOH / EtOH, 100 mm diameter wool samples were treated at room temperature for 10, 20, and 30 minutes, respectively. The pretreated samples were then treated with 2% H₂O₂ at room temperature for 60, 90, and 120 minutes, respectively (i.e., post-treatment). Similarly, pretreatment experiments were conducted with 1.5% and 2% KOH / EtOH concentrations, followed by post-treatment with H₂O₂ solution under the same conditions. The results are detailed in Table 1 below.

[0099] Table 1: The following are the test variables, concentrations, and conditions for treating wool substrates (400 gsm and 200 gsm).

[0100] Reagents and treatment formulations Concentrations and conditions (e.g. time, temperature) Concentration of potassium hydroxide in ethanol (KOH / EtOH) 1%, 1.5%, 2%; room temperature (approximately 20°C) Exposure time to KOH / EtOH 10 min, 20 min, 30 min; room temperature (approximately 20°C) Exposure time to 2% hydrogen peroxide H2O2 60 min, 90 min, 120 min; room temperature (approximately 20°C)

[0101] For each treatment (pretreatment and posttreatment) associated with the specified treatment formulation and processing time, a set of test samples (n=5) was generated for absorbability testing. The water-salt water absorbency test method selected for evaluating untreated (control) and treated wool samples was based on ISO standard ISO 11948:1-1998: Total absorbability.

[0102] Prior to the absorbency test (mass change), all wool samples (treated and untreated) were acclimatized for 48 hours (20°C, 65% relative humidity) under the same environmental conditions required by ISO standard (ISO 11948:1-1998). The surface hydrophilicity of the wool products was investigated using a water contact angle meter (KSV CAM101). Absorbency was measured after the alkaline first reaction step and then after the oxidative second reaction step. Measurements were collected after 30 seconds of contact, and an average of five measurements was recorded. Figure 2 The results of absorbency tests, assessed by contact angle (θ), using goniometer measurement techniques are shown. The structure-functional properties of wool were investigated using FTIR (ATR) before, during, and after treatment. The surface morphology of the wool fibers was analyzed using scanning electron microscopy (SEM) image analysis. Water absorption was studied using the following standard method (ISO 11948:1-1998: Total Absorbency).

[0103] The hydrophilicity / absorbency results of the wool products obtained from 200gsm substrate are presented in Table 2 below.

[0104] Table 2: Descriptive statistics of water-salt water absorption percentage (200gsm wool substrate)

[0105]

[0106]

[0107] These results show that, compared to the control (untreated wool matrix), the treated wool samples exhibited a significantly greater water-salt water absorption capacity (approximately 1300% by weight). The treatment of the wool matrix did not alter the physical properties of the wool, such as its softness, brittleness, structural integrity, or odor. The treated wool products were slightly brighter (whiter) in color than those made with untreated wool matrix.

[0108] The hydrophilicity / absorbency results of the wool products obtained from the 400gsm substrate are presented in Table 3 below.

[0109] Table 3: Descriptive statistics of water-salt water absorption percentage (400gsm wool substrate)

[0110]

[0111] *Total percentage absorption capacity (weight after absorption / initial weight of sample × 100)

[0112] As shown in Table 3, the treated wool samples exhibited a significantly greater water-salt water absorption capacity (approximately 1300% by weight) compared to the control (untreated wool matrix). The treatment of the wool matrix did not alter the physical properties of the wool, such as its softness, brittleness, structural integrity, or odor. The treated wool products were slightly brighter (whiter) in color than those made with untreated wool matrix.

[0113] Figure 3(a) and 3(b) The comparison of absorbency between the untreated wool substrate in 3(a) and the treated wool substrate in 3(b) is clearly shown in the presence of ink samples. Figure 3(a) shows the hydrophobicity of the untreated wool pad and the ink forming beads on the surface of the wool substrate. In contrast, Figure 3(b) shows that the ink is easily absorbed into the wool substrate without forming any beads on the surface of the wool substrate at all.

[0114] Example 3 - Reusability of the reaction mixture

[0115] The reusability of the 1.5% KOH / EtOH reaction mixture was studied over four reaction / batch cycles. After the third cycle, the 1.5% KOH / EtOH reaction mixture turned a cloudy yellow / orange color and showed slight staining in the treated wool substrate, which appeared as a light yellow wool substrate.

[0116] Table 4 below shows the percentage of water-salt water absorbency. The results show that no significant difference in absorbency was observed between the wool substrate obtained from the treatment of the fresh KOH / EtOH reaction mixture and the wool substrate obtained from the KOH / EtOH reaction mixture reused in cycles 1-3. This strongly suggests that the first reaction mixture can be reused in multiple treatment cycles without compromising the absorbency results obtained. It should also be understood that EtOH can be recovered by distillation from the reaction mixture.

[0117] Table 4: Percentage of water-salt water absorbency and descriptive statistics, illustrating the reusability of the KOH / EtOH reaction mixture (exposure duration 10 minutes), while still producing a highly absorbent wool product with a wool substrate of 400 gsm over 4 reaction cycles.

[0118]

[0119] Example 4 - Treatment of wool fibers

[0120] Wool fiber supplied by Hawkes Bay Wool Brushers. This fiber is a strong wool (3 / 4 Romney variety, second shearing) with excellent color and low plant matter content, with an expected average fiber diameter of 35-42 microns and an expected fiber length of 100-120 mm.

[0121] The chemicals used for processing and testing (as noted by the supplier) are:

[0122] 1. Potassium hydroxide (analytical reagent), Fisher Chemical;

[0123] 2. Ethanol (96% v / v, food grade), Southern Grains;

[0124] 3. Hydrogen peroxide (25% v / v, derived from 50% v / v industrial grade), Jasol;

[0125] 4. Sodium chloride (AR, ACS), Pronalys; and

[0126] 5. Reverse osmosis (RO) water.

[0127] All treatments were performed under environmental conditions and all tests were conducted under standard textile testing conditions (20°C and 65% relative humidity).

[0128] All treatments were run at a fiber-to-liquid ratio of 1:40. A series of treatments were performed using 1.5% KOH / EtOH and 2% hydrogen peroxide, each with a different duration of ethanol hydroxide treatment but the same (60 minutes) hydrogen peroxide soaking period.

[0129] The following processing time was used for this process:

[0130] 1. Control group (untreated)

[0131] 2. 8 minutes

[0132] 3. 10 minutes

[0133] 4. 12 minutes

[0134] 5. 14 minutes

[0135] 6. 16 minutes

[0136] 7. 18 minutes

[0137] 8. 20 minutes

[0138] Each sample was then rinsed 5 times in RO water and then dried at 40°C for 30 minutes. Before testing, the dried samples were placed in labeled bags and then placed in an unsealed environment for at least 48 hours.

[0139] The "total absorbance" (ISO 11948:1-1998) was tested for each treated sample. The sample size was 10 cm × 10 cm (each variation was repeated 5 times).

[0140] Equipment: A plastic mesh with square openings (3mm wide, 20mm opening), a small sieve (pre-weighed), and a metal mesh to cover the sieve and keep the fibers in place.

[0141] The standard procedure is as follows:

[0142] 1) Weigh the dried, suitable product and place it in a sieve with a metal mesh on top (to hold the fibers). The sieve is placed on a plastic mesh.

[0143] 2) Lower the mesh and sieve it into a container of sodium chloride solution (9g / l, 1000ml) and soak for 5 minutes.

[0144] 3) Raise the grid to remove the sample from the reservoir and let it stand for 5 minutes to drain.

[0145] 4) Remove the sieve, remove the lid, and weigh.

[0146] 5) Calculate the difference between the dry weight and wet weight for the 5× sample.

[0147] 6) The mean and standard deviation of the calculation results.

[0148] exist Figure 4 and Figure 5 The experimental setup is shown in the figure.

[0149] Simulated absorbency tests of sanitary products were also conducted. For each treatment time, an additional sample was run by uniformly pouring 250 ml of solution onto the sample (covered by a metal mesh and placed on top of a plastic mesh). It was allowed to soak for 5 minutes, then drained for 5 minutes before weighing. This technique was tested based on comparable liquid volume applications from above (not below), as it represents how sanitary products or diaper (pad) type products function.

[0150] For each sample, a rectangular piece of black woven wool fabric (25cm x 20cm) suitable for the conditions was cut. It was then weighed and laid out on a flat surface. A precisely weighed 5g sample for each treatment duration was removed from the bulk material and then manually combed sequentially over the fabric sheet. Four sections of each sample were combed, each section combed 10 times. After combing, the fabric was weighed again, and fiber loss during manual combing was calculated. The combed fibers were bagged and labeled, and observations regarding combability, fiber hand feel, volume, and appearance were recorded. Figure 6 The images show un-carded fibers, carded fibers, and wool 'fiber catching' fabrics from the control samples.

[0151] Scanning electron microscopy (SEM) was used to obtain information related to the physical changes induced in the fibers during treatment. Samples were imaged by SEM by scanning them with a single beam of electrons in raster scan mode. This allowed for observation of the material at high magnification, and the fiber surface morphology, composition, and other properties were investigated. Samples were sputter-coated from a gold / palladium leaf source to impart conductivity to the sample surface. The samples were studied using a JEOL JSM 7000F field emission gun scanning electron microscope. The microscope was operated at 10 kV and the samples were observed over a working distance of 11.3 mm–13.7 mm. Samples treated for 8 to 14 minutes (inclusive) showed no significant signs of fiber damage, i.e., more fiber damage than is typically found on washed wool fibers (control samples). Once the treatment time reached 16 minutes, significant signs of damage were observed on the fiber surface. Specifically, there was evidence of longitudinal 'wrinkles' forming on the fibers; these longitudinal 'wrinkles' were more pronounced on samples treated for 18 and 20 minutes. Figures 10-17The images shown are scanning electron micrographs obtained from samples with different processing methods.

[0152] Each fiber sample was evaluated based on how it felt to the touch. There is a risk that this treatment could cause the samples to become brittle and stiff, which is easily felt when touching wool. Because this test is subjective, the samples were evaluated by three volunteers, who recorded general comments. Both combed and uncombed samples were evaluated.

[0153] result

[0154] Total absorption capacity

[0155] The complete set of results is provided in Lists 5-7 below.

[0156] Table 5: Total Absorption Capacity ISO 119848:1-1998

[0157]

[0158]

[0159] Table 6: Total Absorbance, Mean, and Standard Deviation

[0160]

[0161]

[0162] Table 7: Simulated Sanitary Material Absorbency

[0163] Treatment time Sample mass (g) Mass after immersion (g) Difference (g) % Absorbency Control 5.04 19.70 14.66 291.11 8 minutes 5.00 108.60 103.59 2070.02 10 minutes 5.04 110.46 105.42 2092.79 12 minutes 5.02 104.82 99.80 1988.34 14 minutes 5.06 117.78 112.72 2229.83 16 minutes 5.01 106.30 101.29 2022.45 18 minutes 5.06 101.72 96.66 1910.46 20 minutes 5.08 83.35 78.27 1542.24

[0164] Figure 7 The results of standard test methods are presented using charts and graphs. Figure 8 The diagram shows a simulated sanitary method.

[0165] Figure 7 Absorption data from standard test methods

[0166] The average total absorbance of the treated samples ranged from 1884 to 2502%, while that of the untreated samples averaged 473%. The treated samples with the lowest absorbance were those taken at 20 minutes (the longest duration). The standard deviation of the 20-minute samples (see Table 6 above) was the lowest, while the standard deviation of the 8-minute samples was the highest, with the remaining samples (including the control samples) having similar standard deviations. This can be seen as an indication of the level of fiber treatment; 8 minutes is not sufficient time for the liquid to penetrate and react uniformly throughout the fiber bundle, meaning that samples taken from different areas of the treated material will exhibit different performance.

[0167] Figure 8 Simulated sanitary absorbency

[0168] Individual tests simulating 'in use' conditions based on hygiene products yielded results similar to those of standard test methods. Figure 8 The lowest absorbability of the treated sample was observed with samples lasting 20 minutes.

[0169] Observations showed that for both testing methods, samples wetting was most rapid at 18 and 20 minutes, while samples wetting was slowest at 8 and 10 minutes. However, all seven treated samples did not require pressure to wetting, while the control samples tended to float on the surface of the solution until a mesh was placed on top of the sieve.

[0170] There is a risk that prolonged treatment duration can substantially damage the fibers and render them unsuitable for any subsequent machining required to produce yarn or fabric from these fibers. A simple comparison based on hand-carding tests considers the effect of treatment time on the fibers. Weakened fibers are more easily broken, and the resulting short fibers tend to be lost during carding. Figure 9 The figure shows the amount of fiber loss during hand combing. The results clearly show that for most of the treatment duration, the sample experienced a level of fiber loss comparable to the control sample. The 20-minute sample lost almost three times more mass than the other samples, indicating a higher level of fiber damage.

[0171] The aim of this work was to determine the potential of washed, loose wool fibers to be endowed with superhydrophilicity by the treatment method of this invention while still being able to withstand moderate processing. Results from absorbency, hand-carding, and SEM all demonstrated that damage to the fibers increased with increasing treatment duration. Although wetting with the test solution was the easiest method, a decrease in absorbency was observed at a duration of 20 minutes. Upon examination of the SEM images, it became apparent that multiple longitudinal 'wrinkles' appeared on the fibers, and internal collapse also occurred. It is possible that this condition affects absorbency by providing channels that promote absorption (through capillary action) but also make it easier for the solution to drain, and also by reducing the fiber's ability to retain moisture internally (due to partial collapse). The lower apparent elasticity of the fibers also reduces their ability to retain significant amounts of water between fibers. Similar effects were observed in the SEM images of samples at 18 minutes.

[0172] For combing, the 20-minute sample was the only treated sample that clearly showed significant fiber loss compared to the control sample. It also had the driest hand feel and the lowest observable volumetric and elastic properties. At the other end of the duration range, the 8-minute sample had the largest standard deviation of the overall absorbency data. This suggests that the treatment may be uneven throughout the sample. Considering all the data collected and the observations made, a treatment time of 12–14 minutes is recommended for loose fibers. At this level, fiber absorbability is in the 2400% range, SEM images show the lowest fiber damage (compared to the control sample), the sample contains no reinforced areas, and is easily hand-combed. The observed hand feel is drier than the control, but volumetric and elastic properties are not adversely affected, although this was assessed only through subjective testing.

[0173] The present invention and its embodiments have been described in detail. However, the scope of the invention is not intended to be limited to the embodiments described in the specification. Modifications and variations can be made to the disclosed embodiments without departing from the scope or essential characteristics of the invention.

Claims

1. A method for treating a wool substrate to increase the absorbency of the wool substrate, comprising: A first reaction step of treating the wool substrate with an alcohol and alkali reaction mixture, wherein the reaction time of the first reaction step is 8-14 minutes, wherein the alkali in the alcohol and alkali reaction mixture has a concentration of 0.5% w / v-5% w / v, and wherein the first reaction step is carried out at 20°C ± 2°C; and A second reaction step involves treating the wool substrate obtained from the first reaction step with an aqueous mixture of an oxidizing agent having a concentration of 0.5% v / v to 5% v / v. The reaction time of the second reaction step is 30-120 minutes, the second reaction step is carried out at 20°C ± 2°C, and a rinsing step is performed directly after the second reaction step to produce the treated wool substrate. Compared to an untreated wool substrate, the method enhances the absorption properties of the wool substrate, and the first and second reaction steps do not damage the wool substrate to the point that it is unsuitable for machining to produce wool yarn, wool fabric, or wool fabric products.

2. The method of claim 1, wherein the wool substrate used in the first reaction step is a chemically untreated nonwoven wool substrate.

3. The method of claim 1, wherein the wool substrate used in the first reaction step is selected from (i) a needle-punched wool nonwoven substrate comprising combed wool fibers or (ii) a hydroentangled wool nonwoven substrate comprising combed wool fibers.

4. The method of claim 1, wherein the wool substrate used in the first reaction step comprises loose wool fibers.

5. The method of claim 1, wherein the wool substrate is 100 grams per square meter to 1000 grams per square meter.

6. The method of claim 5, wherein the wool substrate is 200 grams per square meter to 600 grams per square meter.

7. The method of claim 1, wherein the alcohol is selected from methanol, ethanol, propanol, butanol or mixtures thereof.

8. The method of claim 7, wherein the base is selected from potassium hydroxide or sodium hydroxide or a mixture thereof.

9. The method of claim 8, wherein the base in the alcohol and base reaction mixture has a concentration of 1% w / v to 2% w / v.

10. The method of claim 8, wherein the base in the alcohol and base reaction mixture has a concentration of 1.5% w / v.

11. The method of claim 1, wherein the oxidant is hydrogen peroxide.

12. The method of claim 11, wherein the oxidant has a concentration of 1% v / v to 2% v / v.

13. The method of claim 11, wherein the oxidant has a concentration of 2.0% v / v.

14. The method of claim 8, wherein the reaction time of the first reaction step is 12-14 minutes.

15. The method of claim 8, wherein the reaction time of the first reaction step is 10 minutes.

16. The method of claim 8, wherein the reaction time of the first reaction step is 12 minutes.

17. The method of claim 11, wherein the reaction time of the second reaction step is 30-90 minutes.

18. The method of claim 11, wherein the reaction time of the second reaction step is 60 minutes.

19. The method according to any one of claims 1 to 18, wherein the fiber to liquid ratio is 1:10 to 1:

40.

20. A wool product obtained by the method of any one of claims 1 to 19, wherein the wool product has an absorption capacity at least 800% higher than that of an untreated wool substrate.

21. The wool product of claim 20, wherein the wool product has an absorption capacity at least 1000% higher than that of an untreated wool substrate.

22. The wool product of claim 20, wherein the wool product has an absorption capacity that is at least 1200% higher than that of an untreated wool substrate.

23. The wool product of claim 20, wherein the wool product has an absorption capacity at least 1500% higher than that of an untreated wool substrate.

24. The wool product of claim 20, wherein the wool product has an absorption capacity at least 2400% higher than that of an untreated wool substrate.

25. The wool product of any one of claims 20 to 24, wherein the wool product is further used in one or more products that require materials with absorbent properties.

26. The wool product of claim 25, wherein one or more products requiring absorbent properties include: Sportswear; Personal hygiene products; wound dressings or surgical dressings; And chemical spills or cleaning products.

27. The wool product of claim 26, wherein the sportswear includes clothing for sports, outdoor activities and everyday activities.

28. The wool product of claim 26, wherein the personal hygiene product includes diapers, diaper pads, and diaper cloths.

29. The wool product of claim 26, wherein the wool product is one or more of the following: odor-resistant, antimicrobial, moisture-wicking, breathable, chemical-free, non-synthetic, non-petroleum, rash-reducing, flame-retardant, temperature-controllable, hypoallergenic, warm, comfortable, biodegradable, and compostable wool products.

Citation Information

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