US20240060230A1 - Launderable activated cotton garment - Google Patents
Launderable activated cotton garment Download PDFInfo
- Publication number
- US20240060230A1 US20240060230A1 US18/453,769 US202318453769A US2024060230A1 US 20240060230 A1 US20240060230 A1 US 20240060230A1 US 202318453769 A US202318453769 A US 202318453769A US 2024060230 A1 US2024060230 A1 US 2024060230A1
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- United States
- Prior art keywords
- garment
- cotton
- wax
- dye
- lock
- 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
Links
- 229920000742 Cotton Polymers 0.000 title claims abstract description 99
- 238000000034 method Methods 0.000 claims abstract description 98
- 239000004744 fabric Substances 0.000 claims abstract description 50
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 49
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims abstract description 45
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 27
- 229910000029 sodium carbonate Inorganic materials 0.000 claims abstract description 24
- 235000017550 sodium carbonate Nutrition 0.000 claims abstract description 18
- 238000004061 bleaching Methods 0.000 claims abstract description 11
- 150000007524 organic acids Chemical class 0.000 claims abstract description 9
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 24
- 239000000463 material Substances 0.000 claims description 16
- 150000001875 compounds Chemical class 0.000 claims description 13
- 102000028848 arylesterase Human genes 0.000 claims description 11
- 108010009043 arylesterase Proteins 0.000 claims description 11
- 239000003054 catalyst Substances 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 10
- 239000007844 bleaching agent Substances 0.000 claims description 9
- 229920001296 polysiloxane Polymers 0.000 claims description 9
- COHYTHOBJLSHDF-UHFFFAOYSA-N indigo powder Natural products N1C2=CC=CC=C2C(=O)C1=C1C(=O)C2=CC=CC=C2N1 COHYTHOBJLSHDF-UHFFFAOYSA-N 0.000 claims description 8
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 7
- 239000003638 chemical reducing agent Substances 0.000 claims description 7
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 6
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- 102000004190 Enzymes Human genes 0.000 claims description 5
- 108090000790 Enzymes Proteins 0.000 claims description 5
- 235000000177 Indigofera tinctoria Nutrition 0.000 claims description 5
- 239000003431 cross linking reagent Substances 0.000 claims description 5
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- 239000003352 sequestering agent Substances 0.000 claims description 5
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- 239000000243 solution Substances 0.000 description 16
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- 150000002978 peroxides Chemical class 0.000 description 11
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 9
- 102000016938 Catalase Human genes 0.000 description 9
- 108010053835 Catalase Proteins 0.000 description 9
- 239000003513 alkali Substances 0.000 description 9
- 239000011248 coating agent Substances 0.000 description 9
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- 238000004043 dyeing Methods 0.000 description 6
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- 238000007127 saponification reaction Methods 0.000 description 3
- 239000000984 vat dye Substances 0.000 description 3
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 description 2
- 239000004971 Cross linker Substances 0.000 description 2
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 description 2
- 229920000297 Rayon Polymers 0.000 description 2
- 238000002835 absorbance Methods 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical group [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 239000003518 caustics Substances 0.000 description 2
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- 238000004132 cross linking Methods 0.000 description 2
- 230000003247 decreasing effect Effects 0.000 description 2
- SZXQTJUDPRGNJN-UHFFFAOYSA-N dipropylene glycol Chemical compound OCCCOCCCO SZXQTJUDPRGNJN-UHFFFAOYSA-N 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- WQYVRQLZKVEZGA-UHFFFAOYSA-N hypochlorite Chemical compound Cl[O-] WQYVRQLZKVEZGA-UHFFFAOYSA-N 0.000 description 2
- COHYTHOBJLSHDF-BUHFOSPRSA-N indigo dye Chemical group N\1C2=CC=CC=C2C(=O)C/1=C1/C(=O)C2=CC=CC=C2N1 COHYTHOBJLSHDF-BUHFOSPRSA-N 0.000 description 2
- 229910021645 metal ion Inorganic materials 0.000 description 2
- 239000000178 monomer Substances 0.000 description 2
- 229930014626 natural product Natural products 0.000 description 2
- 229920000058 polyacrylate Polymers 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 230000000717 retained effect Effects 0.000 description 2
- 238000009991 scouring Methods 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 description 1
- 229920013646 Hycar Polymers 0.000 description 1
- QQILFGKZUJYXGS-UHFFFAOYSA-N Indigo dye Chemical compound C1=CC=C2C(=O)C(C3=C(C4=CC=CC=C4N3)O)=NC2=C1 QQILFGKZUJYXGS-UHFFFAOYSA-N 0.000 description 1
- JLVVSXFLKOJNIY-UHFFFAOYSA-N Magnesium ion Chemical compound [Mg+2] JLVVSXFLKOJNIY-UHFFFAOYSA-N 0.000 description 1
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000002250 absorbent Substances 0.000 description 1
- 230000002745 absorbent Effects 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 239000003570 air Substances 0.000 description 1
- 229910000329 aluminium sulfate Inorganic materials 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000000987 azo dye Substances 0.000 description 1
- 239000011324 bead Substances 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 239000004464 cereal grain Substances 0.000 description 1
- 231100000481 chemical toxicant Toxicity 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 description 1
- 229910000366 copper(II) sulfate Inorganic materials 0.000 description 1
- 230000002596 correlated effect Effects 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
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- 230000008030 elimination Effects 0.000 description 1
- 238000003379 elimination reaction Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000000834 fixative Substances 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 239000013505 freshwater Substances 0.000 description 1
- 231100001261 hazardous Toxicity 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- 229910000037 hydrogen sulfide Inorganic materials 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 239000008235 industrial water Substances 0.000 description 1
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 description 1
- 229910000359 iron(II) sulfate Inorganic materials 0.000 description 1
- 238000009940 knitting Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- SQQMAOCOWKFBNP-UHFFFAOYSA-L manganese(II) sulfate Chemical compound [Mn+2].[O-]S([O-])(=O)=O SQQMAOCOWKFBNP-UHFFFAOYSA-L 0.000 description 1
- 229910000357 manganese(II) sulfate Inorganic materials 0.000 description 1
- 239000000434 metal complex dye Substances 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000010908 plant waste Substances 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 229920002959 polymer blend Polymers 0.000 description 1
- 230000003334 potential effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 239000012279 sodium borohydride Substances 0.000 description 1
- 229910000033 sodium borohydride Inorganic materials 0.000 description 1
- JVBXVOWTABLYPX-UHFFFAOYSA-L sodium dithionite Chemical compound [Na+].[Na+].[O-]S(=O)S([O-])=O JVBXVOWTABLYPX-UHFFFAOYSA-L 0.000 description 1
- 238000005063 solubilization Methods 0.000 description 1
- 230000007928 solubilization Effects 0.000 description 1
- 238000010561 standard procedure Methods 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 239000003440 toxic substance Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 238000003911 water pollution Methods 0.000 description 1
- 238000009941 weaving Methods 0.000 description 1
- 210000002268 wool Anatomy 0.000 description 1
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 description 1
- 229910000368 zinc sulfate Inorganic materials 0.000 description 1
- 239000011686 zinc sulphate Substances 0.000 description 1
Images
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
- D06M11/73—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 carbon or compounds thereof
- D06M11/76—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 carbon or compounds thereof with carbon oxides or carbonates
-
- 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
- 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
- D06M2101/04—Vegetal fibres
-
- 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
- D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
- D06M2200/10—Repellency against liquids
- D06M2200/12—Hydrophobic properties
Definitions
- the present disclosure is directed to a process for increasing the strength and decreasing the wettability of cotton garments.
- Cotton is a natural fiber with a negative environmental impact when processed.
- the fiber is bleached, finished with strong alkali to prepare for a dying process, and dyed.
- the strong alkali has to be neutralized at each stage of production in particular to mitigate the damaging effluent that would otherwise be released into the worlds aqueous eco systems.
- Cotton is at the top end of this estimate, requiring more water to process than polyester, viscose rayon, and wool. Thus, it is likely that the production and dying of cotton fabric is a significant contributor.
- An embodiment described in examples herein provides a method for making water-resistant cotton garments.
- the method includes treating cotton fabric with soda ash at a temperature of less than about 150° F. (about 66° C.) and a pH of about 9.5 and bleaching the cotton fabric with hydrogen peroxide at a temperature of less than about 150° F. (about 66° C.).
- the hydrogen peroxide is neutralized, and the pH is lowered with an organic acid to between about 6 and about 7.
- a garment is made from the cotton fabric and a wax lock is applied to the garment.
- the garment is dyed at a temperature of less than about 150° F. (about 66° C.), and dried.
- Another embodiment described in examples herein provides a cotton garment formed from an activated cotton material, including a layer of natural wax locked to the surface of cotton fibers by a wax lock.
- FIG. 1 is a process flow diagram of a method for making a treated cotton garment.
- FIG. 2 is a process flow diagram of a dying process that uses a reduction dye (RD) to make the treated cotton garment.
- RD reduction dye
- Kiering The industry standard technique for treating cotton for dying is termed Kiering. Kiering is generally performed on cotton fabric or yarn to prepare it for dyeing. It uses a scouring process in which hot alkali (NaOH) solutions are used to saponify the natural wax coating on the cotton fibers, removing the wax. This increases the absorbancy (hydrophilicity) of the cotton fabric, making the fabric easier to dye.
- NaOH hot alkali
- the cotton is bleached to remove color bodies, forming a white material.
- the bleaching can be performed by the use of hydrogen peroxide or other bleaches, such as hypochlorite bleach, among others.
- the treated cotton can then be dyed, for example, as yarns, fabric, or garments, depending on the products.
- the cotton articles are passed through, or soaked in, baths that include chemicals that help the dye to adhere to the cotton, for example, by forming hydroxyl groups at the surface of the cotton.
- the cotton is then passed through, or soaked in, a bath containing the dye. This is often followed by multiple rinses to remove any excess dye that does not adhere to the cloth.
- the yarn is then formed into a fabric, for example, by knitting or weaving.
- the currently used techniques for treating cotton form an absorbent fabric with a color selected by the techniques used.
- the alkali treatment reduced the strength of the cotton fibers, for example, by as much as 50% or more, from the raw cotton.
- a process for producing a cotton product, termed an activated cotton, which leaves the natural wax in place on the cotton fibers, lowers water usage, and improves the properties of the cotton.
- the natural wax coating on the cotton fibers imparts high performance properties to yarns, fabrics, and garments, for example, increasing the cooling properties of the fabric by allowing water vapor to pass through the fabric without being adsorbed.
- the process includes the addition of a compound termed a wax lock.
- the wax coating on natural cotton is generally removed during Keiring. Further, even if left on by a milder process, home laundering will remove the natural wax in a few cycles. To overcome this, the activated cotton is treated with the wax lock to fix the wax in place on the fabric.
- the wax lock includes a silicone compound that interacts with the natural wax to prevent surfactants from removing the wax.
- the wax lock is a cross-linking agent, such as a synthetic acrylic oligomer, which is applied before the final drying process and activated during drying.
- a natural product that includes cross-linking material, along with a natural wax, can also be used.
- the cross-linking agent forms cross-links that hold the natural wax in place on the fibers. This retains the natural hydrophobicity of the cotton fabric and enables it to maintain the hydrophobicity during numerous home laundering cycles, for example, greater than 20 cycles, greater than 25 cycles, greater than 30 cycles, or longer.
- the bleaching is performed using hydrogen peroxide.
- a peroxide activator, triacetin is used along with a sequestering (or chelating) agent to protect the cotton fiber and the natural wax.
- the triacetin gradually lowers the pH, creating conditions for the peroxide to be a highly effective bleaching agent to prepare the cotton for dying. This allows the elimination of the strong caustic alkali used in used in traditional bleaching and dye preparation methods. This also creates conditions for an enzyme bleach catalyst to be effective.
- arylesterase is used as the oxidation catalyst.
- the arylesterase is effective at low concentrations (high dilutions), such as about 0.5 grams per liter (g/L) about 0.2 g/L, or less.
- high dilutions such as about 0.5 grams per liter (g/L) about 0.2 g/L, or less.
- the use of the arylesterase allows the hydrogen peroxide reaction to occur at lower temperatures and in a shorter time, which lowers both the time and energy for the reaction, increasing the economic yield.
- FIG. 1 is a process flow diagram of a method for making a treated cotton garment.
- An example of the treatment process used for the garment is described in the examples section below. It should be noted that the individual steps may be rearranged, eliminated, or modified. For example, in some embodiments, the soda ash pretreatment may be eliminated. It should also be noted that no surfactants or detergents are used in the process to avoid removing the natural wax coating, eliminating the potential negative environmental problems associated with surfactants or detergents.
- the method 100 includes five basic processes, a pretreatment process 102 used to clean the cotton fabric and bleach it to remove color bodies and prepare the fabric for dying.
- a garment production process 104 is used to prepare a garment from a pretreated fabric.
- a treatment process 106 is used to prepare the garment for dying and to apply the wax lock to the fabric.
- a dying process 108 is used to impart color to the garment.
- a drying process 110 is then used to fix the wax lock on the garment, protecting the natural wax coating on the cotton fibers, and allowing multiple home launderings without removing the wax coating.
- the pretreatment process 102 begins at block 112 with a soda ash pretreatment.
- soda ash Na 2 CO 3
- caustic soda NaOH
- the use of NaOH sets the pH at 12.5, which damages the cotton fibers and removes the natural wax by saponification.
- the soda ash sets the pH of the treatment, for example, to about 10, or about 9.5.
- the lower pH prevents, or decreases, the likelihood of saponification of the wax coating. Further, this is performed at a lower temperature than previous pretreatment procedures, for example, about 150° F. (66° C.).
- a bleach activator for example, glyceryl triacetate (triacetin)
- triacetin glyceryl triacetate
- the triacetin is available from Cekal Specialties of Mt. Holly, NC, USA, under the tradename CEKASSIST BIO.
- a sequestering agent such as ethylenediaminetetraacetic acid (EDTA)
- EDTA ethylenediaminetetraacetic acid
- the sequestering agent is CEKAQUEST PB from Cekal Specialties, which is also helping stabilize the hydrogen peroxide bleach. The decreasing concentration of the divalent metal ions will further stabilize the hydrogen peroxide during the bleaching procedure.
- a bleaching procedure is performed using a 50% solution of hydrogen peroxide.
- an arylesterase catalyst is added to speed the reaction between the peroxide and the color bodies, as described herein.
- the arylesterase catalyst is produced by microorganisms, for example, in a commercial production process. Any number of arylesterase catalysts can be used in the current procedures.
- the arylesterase catalyst is obtained from Cekal Specialties under the tradename CEKAZYME BB.
- a catalase enzyme Any number of catalase enzymes may be used in the current procedures.
- the catalase is CEKAZYME EPK200 from Cekal Specialties.
- a test strip is used to confirm that the peroxide is eliminated. If not, in some embodiments, a water wash is used to rinse any remaining peroxide from the cotton. Generally, the peroxide is completely reacted, which allows a processor to go directly to the dyeing process. This avoids the washes that are needed to remove the peroxide, for example, saving around 10,000 liters of water per 1,000 kg of textile substrate.
- the pH is lowered to a pH of less than about 8, less than about 7, or between 6.5 and 7. In some embodiments, this is performed by the addition of an organic acid, such as citric acid, acetic acid, or others. In some embodiments, the pH is checked to confirm that it is between 6.5 and 7. If not, more acid may be added, and the pH retested.
- an organic acid such as citric acid, acetic acid, or others.
- a surface tension test may be used to confirm that the pretreatment process 102 did not damage or remove the natural wax coating.
- the surface tension test is performed by placing a drop of water on the surface of the fabric and noting if the water beads or is absorbed.
- a goniometer is used to determine the surface tension of the surface, which may be used to determine the efficacy of the treatment.
- the fabric from the pretreatment process 102 is then used to make a garment in the garment production process 104 .
- the fabric is cut into the appropriate shaped pieces, and sewn into the final garment.
- the pieces are generally larger than the final size expected for the garment, as the garment accounts for shrinkage during the dying, finishing, and drying stages.
- the treatment process 106 is used to prepare the garment for dying and to apply the wax lock if performance is desired.
- the treatment process 106 begins at block 120 , with the treatment of the garment with sodium sulfate.
- Na 2 CO 3 sodium sulfate
- Na 2 CO 3 sodium sulfate
- the pH may be checked, and more Na 2 CO 3 added if needed to adjust the pH to 9.5.
- the use of the weak alkali helps retain and protect the cotton wax and the cotton cellulose. It is used in place of the caustic soda (NaOH) used in the standard Kiering procedure, which would set the pH at 12.5, damaging the cotton and removing the natural wax via saponification.
- the wax lock is applied, for example, by adding the wax lock material to the solution containing the garment.
- the wax lock may include silicone compounds, acrylic oligomers, or combinations. Other materials may be used, such as other types of oligomers or monomers.
- the wax lock is hydrophobic, further protecting the natural was from being removed by laundering.
- the silicone wax lock compound used in some embodiments is available from Apexical Specialty Chemicals of Spartanburg, SC, USA, as Apexosil 2137.
- a small amount of acrylic monomers or oligomers may be included, such as about 1 wt. %, about 2 wt. %, about 5 wt. %, about 10 wt. %, about 20 wt. %, or higher.
- the wax lock is a blend that includes an acrylic oligomer, such as available from Cekal Specialties as CEKAPEL NFWR.
- the acrylic polymer blend includes 20-30 wt. % of a liquid, crosslinking acrylic polymer.
- the blend also includes 5-10 wt. % of dipropylene glycol. The dipropylene glycol lowers the viscosity of the polymer blend, improving the uptake into the cotton.
- the wax lock compound is a blend that includes natural plant material isolated from plant wastes, for example, the by-products that accumulate during the processing of cereal grains in the food industry.
- a crosslinker may be included in the blend to assist in locking the natural wax and the natural plant material to the fibers of the cotton.
- the natural plant material is available from Rudolf GmbH of Geresreid, DE, as RUCO®-DRY BIO CGR.
- the crosslinker is available from Rudolf as RUCO®-LINK XHC.
- Other products from Rudolf can be used as the wax lock in embodiments.
- RUCO®-DRY BIO NPE is a combined natural plant product and cross-linking agent that can be used as the wax lock.
- the dying process 108 is described with respect to blocks 126 to 132 . It can be noted that the generic procedure of FIG. 1 will work with all dyes. However, specific information on the use of pre-reduced dyes, such as reduction dyes, including indigo, sulfur dyes, pre-reduced indigo, and pre-reduced sulfur dyes, is described further with respect to FIG. 2 .
- reduction dyes including indigo, sulfur dyes, pre-reduced indigo, and pre-reduced sulfur dyes
- the dying compound is added to the solution containing the garment.
- the dye is a reactive dye, although any number of other types of dyes may be used, including direct dyes, sulfur dyes, azoic dyes, or vat dyes, among others described herein.
- the dye liquor is heated to a maximum temperature of about 140° F. (about 60° C.) at a rate of about 2° F./min (about 1.1° C./min.).
- the dye is allowed to stay in contact with the cotton for a sufficient period of time for absorbance, for example, 30 min., 45 min., 60 min., or longer.
- the dye and salts are rinsed from the garment.
- the pH is lowered to less than 8, or less than 7, or about 6.5. This is performed by the addition of an organic acid, such as citric acid, acetic acid, or the like.
- a water rinse is performed to remove the acid and any remaining dyes or salts from the garment.
- the pH of the rinse solution containing the garment is checked to confirm that it is between 6.5 and 7. If not, more acid may be added, and the pH retested.
- the garment is dried to fix the wax lock compound. In various embodiments, this is performed at a temperature of less than about 400° F. (about 204° C.), or less than about 390° F. (about 199° C.), or less than about 350° F. (about 177° C.), or less than about 310° F. (about 154° C.), or between about 300° F. (about 149°) and about 390° F. (about 199° C.), for example, in a tumble dryer or on a frame or moving line at a speed of about 25 to about 30 yds./min (or about 23 to about 27 meters/min).
- FIG. 2 is a process flow diagram of a dying process 200 that uses a reduction dye.
- a reduction dye is a dye that is insoluble in water until it is reduced.
- the RD is an indigo dye, a sulfur dye, a pre-reduced indigo dye, a pre-reduced sulfur dye, or other pre-reduced dye.
- the pre-reduced dye is not fully reduced, for example, only being reduced by about 60%.
- the dying process 200 begins with the treatment of the garment with sodium sulfate at block 118 , for example, using about 30 g/l to about 50 g/l.
- Na 2 CO 3 sodium sulfate
- the pH may be checked, and more Na 2 CO 3 added if needed to adjust the pH to 9.5.
- the garment is treated with the wax lock compound, as described herein.
- the RD is added to the solution.
- a reducing agent is added at block 204 to fully reduce the dye for solubilization.
- the reducing agent may be a catalase, such as CEKAZYME EPK200 from Cekal added at about 4 g/l to about 6 g/l, depending on whether the reduction dye is pre-reduced before use.
- the reducing agent is sodium borohydride, hydrogen sulfide, or sodium hydrosulfite, among others.
- a mordant or dye fixative agent, is added to assist in adhering the dye to the cloth.
- the mordant is Al 2 (SO 4 ) 3 , FeSO 4 , CuSO 4 , ZnSO 4 , or MnSO 4 , among others.
- the mordant is selected based on the efficacy and the potential effects on the color. Further, the mordant may increase the efficacy of the reducing agent, for example, if a catalase is used, by increasing the ORP of the catalase solution.
- the mordant can be added at about 10 g/l to about 20 g/l.
- the dye liquor and reducing agent are heated to a maximum temperature of about 140° F. (about 60° C.) at a rate of about 2° F./min (about 1.1° C./min.).
- the dye is allowed to stay in contact with the cotton for a sufficient period of time for absorbance, for example, 30 min., 45 min., 60 min., or longer.
- the dye, mordant, and salts are rinsed from the solution.
- an oxidizer is added to the water solution to oxidize the reduced dye.
- the oxidizer is hydrogen peroxide, air, oxygen, a water solution of ozone, and the like.
- hydrogen peroxide is added at between about 1 g/l and about 5 g/l.
- the dye is allowed to oxidize in air for about 20 to about 30 minutes. The amount of oxidation controls the color, with higher levels of oxidation correlated to darker colors.
- the pH is lowered to less than 8, or less than 7, or about 6.5. This is performed by the addition of an organic acid, such as citric acid, acetic acid, or the like.
- a water rinse is performed to remove the acid and any remaining dyes or salts. In some embodiments, the pH is checked to confirm that it is between 6.5 and 7. If not, more acid may be added, and the pH retested.
- any number of other dyes may be used in embodiments described herein, including, including vat dyes, sulfur dyes, pre-reduced versions of vat and sulfur dyes, and other dyes that are insoluble and are applied to substrates via redox methods.
- Other dyes include azo dyes, such as direct dyes, metal complex dyes, reactive dyes, substantive dyes, and aniline dyes, such as natural and synthetic indigo dye, among others.
- the treatment process described herein, for example, with respect to FIG. 1 was tested on cotton fabric using the parameters described in Table 1.
- the dye used in the process described in Table 1 can be used pre-reduced dyes, such as pre-reduced indigo and pre-reduced sulfur dyes, as shown in Table 2.
- cotton fabric can be made into garments, and the wax lock can be applied during the dying process, for example, before the dye is added.
- a cotton fabric prepared using this technique with a silicone softener as the wax lock compound retained the natural wax through greater than 25 laundering cycles using a cool wash cycle, 1 g/L Tide laundry detergent, and a cool dry cycle. This was tested by performed a surface tension test after each laundering cycle by applying a water droplet and determining that it beaded on the cotton fabric.
- the natural wax lock products from Rudolph, Ruco-Dry Bio CGR and Ruco-Dry Bio NPE are highly effective.
- the burst strength of the cotton fabric was compared to a sample of cotton fabric that was treated by the normal caustic wash.
- the test performed to determine the strength was the Mullen diaphragm burst test, following ASTM D3787.
- the strength retained by the cotton fibers depended on the initial lengths of the cotton fibers, e.g., the quality of the cotton.
- a sample of fabric made using a high-quality cotton and treated using the procedure described with respect to FIG. 1 provided an average burst strength of up to 210 psi (about 1448 kPa), versus a sample of the same fabric treated with the standard Kiering procedure, which had an average burst strength of about 110 psi (about 758 kPa).
- An embodiment described in examples herein provides a method for making water-resistant cotton garments.
- the method includes treating cotton fabric with soda ash at a temperature of less than about 150° F. (about 66° C.) and a pH of about 9.5 and bleaching the cotton fabric with hydrogen peroxide at a temperature of less than about 150° F. (about 66° C.).
- the hydrogen peroxide is neutralized, and the pH is lowered with an organic acid to between about 6 and about 7.
- a garment is made from the cotton fabric and a wax lock is applied to the garment.
- the garment is dyed at a temperature of less than about 150° F. (about 66° C.), and dried.
- making the garment includes cutting pieces from the cotton fabric and sewing the pieces together to form the garment.
- the method includes adding a bleach activator with the soda ash.
- the method includes adding a sequestering agent with the soda ash.
- the method includes adding an arylesterase catalyst with the hydrogen peroxide.
- neutralizing includes adding an enzyme to degrade the hydrogen peroxide.
- the organic acid includes citric acid.
- applying the wax lock to the garment includes treating the garment with sodium sulfate, treating the cotton with soda ash to raise the pH to about 9.5, and applying the wax lock to the garment.
- the dying includes treating the garment with a dye solution, rinsing the garment, neutralizing the dye solution to a pH of about 6.5, and rinsing the garment.
- the dye solution includes a pre-reduced dye.
- the method includes adding a reducing agent to the dye solution.
- the method includes adding a mordant to the dye solution.
- the method includes treating the garment with an oxidant.
- the method includes treating the garment with the wax lock.
- the method includes drying the garment at between about 300° F. (about 149° C.) and about 390° F. (about 199° C.).
- the wax lock includes a silicone compound.
- wax lock includes an acrylic compound.
- Another embodiment described in examples herein provides a cotton garment formed from an activated cotton material, including a layer of natural wax locked to a surface of cotton fibers by a wax lock.
- the cotton garment includes a dye.
- the cotton garment includes a pre-reduced dye.
- the pre-reduced dye includes indigo.
- the wax lock includes a silicone compound.
- the wax lock includes an acrylic oligomer.
- the wax lock includes a natural plant material.
- the wax lock includes a natural plant material combined with a cross-linking agent.
Abstract
A method for making water-resistant cotton garments and the water-resistant cotton garments are provided. An exemplary method includes treating cotton fabric with soda ash at a temperature of less than about 150° F. (about 66° C.) and a pH of about 9.5 and bleaching the cotton fabric with hydrogen peroxide at a temperature of less than about 150° F. (about 66° C.). The hydrogen peroxide is neutralized, and the pH is lowered with an organic acid to between about 6 and about 7. A garment is made from the cotton fabric and a wax lock is applied to the garment. The garment is dyed at a temperature of less than about 150° F. (about 66° C.), and dried.
Description
- This application claims the benefit of U.S. Provisional Application No. 63/373,101, filed Aug. 22, 2022, the contents of which are incorporated by reference herein.
- The present disclosure is directed to a process for increasing the strength and decreasing the wettability of cotton garments.
- Cotton is a natural fiber with a negative environmental impact when processed. Currently, the fiber is bleached, finished with strong alkali to prepare for a dying process, and dyed. The strong alkali has to be neutralized at each stage of production in particular to mitigate the damaging effluent that would otherwise be released into the worlds aqueous eco systems.
- A substantial amount of water waste is generated by repeatedly washing off the alkali involved in wet processing. For example, a report in the Planet Tracker, “Will Fashion Dye Another Day” (December 2020), notes “textile production requires an estimated 430 liters or 114 US gallons to produce 1 kg of textile fabric.” The report continues, stating that an estimated 8,000 toxic chemicals, used globally, are used to turn raw materials into textiles. Many of these chemicals are released into freshwater sources as waste streams. For example, “the dyeing and treatment of textiles is estimated to cause 20% of global industrial water pollution.”
- Cotton is at the top end of this estimate, requiring more water to process than polyester, viscose rayon, and wool. Thus, it is likely that the production and dying of cotton fabric is a significant contributor.
- Further, the current processing techniques used for cotton are energy intensive, requiring multiple drying cycles. Reducing the heat used in dyeing and shortening the dye cycles will lower the energy demand.
- An embodiment described in examples herein provides a method for making water-resistant cotton garments. The method includes treating cotton fabric with soda ash at a temperature of less than about 150° F. (about 66° C.) and a pH of about 9.5 and bleaching the cotton fabric with hydrogen peroxide at a temperature of less than about 150° F. (about 66° C.). The hydrogen peroxide is neutralized, and the pH is lowered with an organic acid to between about 6 and about 7. A garment is made from the cotton fabric and a wax lock is applied to the garment. The garment is dyed at a temperature of less than about 150° F. (about 66° C.), and dried.
- Another embodiment described in examples herein provides a cotton garment formed from an activated cotton material, including a layer of natural wax locked to the surface of cotton fibers by a wax lock.
-
FIG. 1 is a process flow diagram of a method for making a treated cotton garment. -
FIG. 2 is a process flow diagram of a dying process that uses a reduction dye (RD) to make the treated cotton garment. - The industry standard technique for treating cotton for dying is termed Kiering. Kiering is generally performed on cotton fabric or yarn to prepare it for dyeing. It uses a scouring process in which hot alkali (NaOH) solutions are used to saponify the natural wax coating on the cotton fibers, removing the wax. This increases the absorbancy (hydrophilicity) of the cotton fabric, making the fabric easier to dye.
- However, multiple rinses of water are required to remove the alkali solutions. Further, the alkali softens the fabric by partially breaking down the fibers, leading to a lower strength product. The highly corrosive NaOH is also hazardous to operators if not properly handled in processing textiles. In addition, if the effluent created is not properly neutralized and disposed of it can be very damaging to water systems and the associated environment.
- After the scouring, the cotton is bleached to remove color bodies, forming a white material. The bleaching can be performed by the use of hydrogen peroxide or other bleaches, such as hypochlorite bleach, among others.
- The treated cotton can then be dyed, for example, as yarns, fabric, or garments, depending on the products. In the dying process, the cotton articles are passed through, or soaked in, baths that include chemicals that help the dye to adhere to the cotton, for example, by forming hydroxyl groups at the surface of the cotton. The cotton is then passed through, or soaked in, a bath containing the dye. This is often followed by multiple rinses to remove any excess dye that does not adhere to the cloth.
- If the treating and dying process is performed on a cotton yarn, the yarn is then formed into a fabric, for example, by knitting or weaving. The currently used techniques for treating cotton form an absorbent fabric with a color selected by the techniques used. However, the alkali treatment reduced the strength of the cotton fibers, for example, by as much as 50% or more, from the raw cotton.
- A process is provided herein for producing a cotton product, termed an activated cotton, which leaves the natural wax in place on the cotton fibers, lowers water usage, and improves the properties of the cotton. The natural wax coating on the cotton fibers imparts high performance properties to yarns, fabrics, and garments, for example, increasing the cooling properties of the fabric by allowing water vapor to pass through the fabric without being adsorbed. To implement this, the process includes the addition of a compound termed a wax lock.
- As described, the wax coating on natural cotton is generally removed during Keiring. Further, even if left on by a milder process, home laundering will remove the natural wax in a few cycles. To overcome this, the activated cotton is treated with the wax lock to fix the wax in place on the fabric. In some embodiments, the wax lock includes a silicone compound that interacts with the natural wax to prevent surfactants from removing the wax. In other embodiments, the wax lock is a cross-linking agent, such as a synthetic acrylic oligomer, which is applied before the final drying process and activated during drying. A natural product that includes cross-linking material, along with a natural wax, can also be used. The cross-linking agent forms cross-links that hold the natural wax in place on the fibers. This retains the natural hydrophobicity of the cotton fabric and enables it to maintain the hydrophobicity during numerous home laundering cycles, for example, greater than 20 cycles, greater than 25 cycles, greater than 30 cycles, or longer.
- In the process, the bleaching is performed using hydrogen peroxide. A peroxide activator, triacetin, is used along with a sequestering (or chelating) agent to protect the cotton fiber and the natural wax. The triacetin gradually lowers the pH, creating conditions for the peroxide to be a highly effective bleaching agent to prepare the cotton for dying. This allows the elimination of the strong caustic alkali used in used in traditional bleaching and dye preparation methods. This also creates conditions for an enzyme bleach catalyst to be effective.
- In various embodiments, arylesterase is used as the oxidation catalyst. The arylesterase is effective at low concentrations (high dilutions), such as about 0.5 grams per liter (g/L) about 0.2 g/L, or less. The use of the arylesterase allows the hydrogen peroxide reaction to occur at lower temperatures and in a shorter time, which lowers both the time and energy for the reaction, increasing the economic yield.
- The process changes and combinations described herein shorten the process further and increase water savings. This provides a more stable, repeatable, and ecologically favorable process. Further, the natural wax coating on the cotton will withstand 30 or more home laundering cycles with a surfactant, such as laundry detergent.
-
FIG. 1 is a process flow diagram of a method for making a treated cotton garment. An example of the treatment process used for the garment is described in the examples section below. It should be noted that the individual steps may be rearranged, eliminated, or modified. For example, in some embodiments, the soda ash pretreatment may be eliminated. It should also be noted that no surfactants or detergents are used in the process to avoid removing the natural wax coating, eliminating the potential negative environmental problems associated with surfactants or detergents. - The
method 100 includes five basic processes, apretreatment process 102 used to clean the cotton fabric and bleach it to remove color bodies and prepare the fabric for dying. Agarment production process 104 is used to prepare a garment from a pretreated fabric. Atreatment process 106 is used to prepare the garment for dying and to apply the wax lock to the fabric. A dyingprocess 108 is used to impart color to the garment. Adrying process 110 is then used to fix the wax lock on the garment, protecting the natural wax coating on the cotton fibers, and allowing multiple home launderings without removing the wax coating. - The
pretreatment process 102 begins atblock 112 with a soda ash pretreatment. The use of soda ash, Na2CO3, is in place of caustic soda (NaOH) used in the standard Kiering process. The use of NaOH sets the pH at 12.5, which damages the cotton fibers and removes the natural wax by saponification. The soda ash sets the pH of the treatment, for example, to about 10, or about 9.5. The lower pH prevents, or decreases, the likelihood of saponification of the wax coating. Further, this is performed at a lower temperature than previous pretreatment procedures, for example, about 150° F. (66° C.). - During the soda ash pretreatment at
block 112, a bleach activator, for example, glyceryl triacetate (triacetin), is added for activation of hydrogen peroxide in the subsequent bleaching procedure. The triacetin is available from Cekal Specialties of Mt. Holly, NC, USA, under the tradename CEKASSIST BIO. Further, a sequestering agent, such as ethylenediaminetetraacetic acid (EDTA), is used to lower the concentration of divalent metal ions, such as magnesium (II) and calcium (II). In an embodiment, the sequestering agent is CEKAQUEST PB from Cekal Specialties, which is also helping stabilize the hydrogen peroxide bleach. The decreasing concentration of the divalent metal ions will further stabilize the hydrogen peroxide during the bleaching procedure. - At
block 114, a bleaching procedure is performed using a 50% solution of hydrogen peroxide. During the bleaching procedure, an arylesterase catalyst is added to speed the reaction between the peroxide and the color bodies, as described herein. Generally, the arylesterase catalyst is produced by microorganisms, for example, in a commercial production process. Any number of arylesterase catalysts can be used in the current procedures. In an embodiment, the arylesterase catalyst is obtained from Cekal Specialties under the tradename CEKAZYME BB. - At
block 116, should there be any peroxide bleach remaining, it is neutralized by the addition of a catalase enzyme. Any number of catalase enzymes may be used in the current procedures. In an embodiment, the catalase is CEKAZYME EPK200 from Cekal Specialties. In some embodiments, a test strip is used to confirm that the peroxide is eliminated. If not, in some embodiments, a water wash is used to rinse any remaining peroxide from the cotton. Generally, the peroxide is completely reacted, which allows a processor to go directly to the dyeing process. This avoids the washes that are needed to remove the peroxide, for example, saving around 10,000 liters of water per 1,000 kg of textile substrate. - At
block 118, the pH is lowered to a pH of less than about 8, less than about 7, or between 6.5 and 7. In some embodiments, this is performed by the addition of an organic acid, such as citric acid, acetic acid, or others. In some embodiments, the pH is checked to confirm that it is between 6.5 and 7. If not, more acid may be added, and the pH retested. - A surface tension test may be used to confirm that the
pretreatment process 102 did not damage or remove the natural wax coating. In some embodiments, the surface tension test is performed by placing a drop of water on the surface of the fabric and noting if the water beads or is absorbed. In other embodiments, a goniometer is used to determine the surface tension of the surface, which may be used to determine the efficacy of the treatment. - The fabric from the
pretreatment process 102 is then used to make a garment in thegarment production process 104. For example, the fabric is cut into the appropriate shaped pieces, and sewn into the final garment. The pieces are generally larger than the final size expected for the garment, as the garment accounts for shrinkage during the dying, finishing, and drying stages. - After preparation of the garment, the
treatment process 106 is used to prepare the garment for dying and to apply the wax lock if performance is desired. Thetreatment process 106 begins atblock 120, with the treatment of the garment with sodium sulfate. Atblock 122, Na2CO3 (soda ash) is added to raise the pH to about 9.5, or about 10. The pH may be checked, and more Na2CO3 added if needed to adjust the pH to 9.5. The use of the weak alkali helps retain and protect the cotton wax and the cotton cellulose. It is used in place of the caustic soda (NaOH) used in the standard Kiering procedure, which would set the pH at 12.5, damaging the cotton and removing the natural wax via saponification. - At
block 124, the wax lock is applied, for example, by adding the wax lock material to the solution containing the garment. As described herein, the wax lock locks the natural wax to the cotton fibers, slowing its removal by laundering. The wax lock may include silicone compounds, acrylic oligomers, or combinations. Other materials may be used, such as other types of oligomers or monomers. Generally, the wax lock is hydrophobic, further protecting the natural was from being removed by laundering. The silicone wax lock compound used in some embodiments is available from Apexical Specialty Chemicals of Spartanburg, SC, USA, as Apexosil 2137. In some embodiments, a small amount of acrylic monomers or oligomers may be included, such as about 1 wt. %, about 2 wt. %, about 5 wt. %, about 10 wt. %, about 20 wt. %, or higher. - In some embodiments, the wax lock is a blend that includes an acrylic oligomer, such as available from Cekal Specialties as CEKAPEL NFWR. In this example, the acrylic polymer blend includes 20-30 wt. % of a liquid, crosslinking acrylic polymer. The blend also includes 5-10 wt. % of dipropylene glycol. The dipropylene glycol lowers the viscosity of the polymer blend, improving the uptake into the cotton.
- Similar materials are available from other suppliers. These include blends in the Hycar line from Lubrizol, Corp. of Wickliffe, OH, USA. Other materials are available from Apexical Specialty Chemicals, Huntsman Chemicals of Charlotte, NC, USA, and Chemours of Wilmington, DE, USA.
- In some embodiments, the wax lock compound is a blend that includes natural plant material isolated from plant wastes, for example, the by-products that accumulate during the processing of cereal grains in the food industry. A crosslinker may be included in the blend to assist in locking the natural wax and the natural plant material to the fibers of the cotton. The natural plant material is available from Rudolf GmbH of Geresreid, DE, as RUCO®-DRY BIO CGR. The crosslinker is available from Rudolf as RUCO®-LINK XHC. Other products from Rudolf can be used as the wax lock in embodiments. For example, RUCO®-DRY BIO NPE is a combined natural plant product and cross-linking agent that can be used as the wax lock.
- The dying
process 108 is described with respect toblocks 126 to 132. It can be noted that the generic procedure ofFIG. 1 will work with all dyes. However, specific information on the use of pre-reduced dyes, such as reduction dyes, including indigo, sulfur dyes, pre-reduced indigo, and pre-reduced sulfur dyes, is described further with respect toFIG. 2 . - At
block 126, the dying compound is added to the solution containing the garment. In some embodiments, the dye is a reactive dye, although any number of other types of dyes may be used, including direct dyes, sulfur dyes, azoic dyes, or vat dyes, among others described herein. The dye liquor is heated to a maximum temperature of about 140° F. (about 60° C.) at a rate of about 2° F./min (about 1.1° C./min.). The dye is allowed to stay in contact with the cotton for a sufficient period of time for absorbance, for example, 30 min., 45 min., 60 min., or longer. - At
block 128, the dye and salts are rinsed from the garment. Atblock 130, the pH is lowered to less than 8, or less than 7, or about 6.5. This is performed by the addition of an organic acid, such as citric acid, acetic acid, or the like. Atblock 132, a water rinse is performed to remove the acid and any remaining dyes or salts from the garment. In some embodiments, the pH of the rinse solution containing the garment is checked to confirm that it is between 6.5 and 7. If not, more acid may be added, and the pH retested. - In the
drying process 110, the garment is dried to fix the wax lock compound. In various embodiments, this is performed at a temperature of less than about 400° F. (about 204° C.), or less than about 390° F. (about 199° C.), or less than about 350° F. (about 177° C.), or less than about 310° F. (about 154° C.), or between about 300° F. (about 149°) and about 390° F. (about 199° C.), for example, in a tumble dryer or on a frame or moving line at a speed of about 25 to about 30 yds./min (or about 23 to about 27 meters/min). -
FIG. 2 is a process flow diagram of a dyingprocess 200 that uses a reduction dye. Like numbered items, including thepretreatment process 102,garment production process 104,treatment process 106, and dryingprocess 110, are as described with respect toFIG. 1 . As used herein, a reduction dye (RD) is a dye that is insoluble in water until it is reduced. In various embodiments, the RD is an indigo dye, a sulfur dye, a pre-reduced indigo dye, a pre-reduced sulfur dye, or other pre-reduced dye. The pre-reduced dye is not fully reduced, for example, only being reduced by about 60%. - As for the
treatment process 106 ofFIG. 1 , the dyingprocess 200 begins with the treatment of the garment with sodium sulfate atblock 118, for example, using about 30 g/l to about 50 g/l. Atblock 120, Na2CO3 (soda ash) is added to raise the pH to about 9.5, or about 10, for example, using about 6 g/l to about 10 g/l. The pH may be checked, and more Na2CO3 added if needed to adjust the pH to 9.5. Atblock 122, the garment is treated with the wax lock compound, as described herein. - At
block 202, the RD is added to the solution. As the dye is not soluble until it is reduced, a reducing agent is added atblock 204 to fully reduce the dye for solubilization. In some embodiments, the reducing agent may be a catalase, such as CEKAZYME EPK200 from Cekal added at about 4 g/l to about 6 g/l, depending on whether the reduction dye is pre-reduced before use. In other embodiments, the reducing agent is sodium borohydride, hydrogen sulfide, or sodium hydrosulfite, among others. - At
block 206, a mordant, or dye fixative agent, is added to assist in adhering the dye to the cloth. In some embodiments, the mordant is Al2(SO4)3, FeSO4, CuSO4, ZnSO4, or MnSO4, among others. The mordant is selected based on the efficacy and the potential effects on the color. Further, the mordant may increase the efficacy of the reducing agent, for example, if a catalase is used, by increasing the ORP of the catalase solution. The mordant can be added at about 10 g/l to about 20 g/l. - The dye liquor and reducing agent are heated to a maximum temperature of about 140° F. (about 60° C.) at a rate of about 2° F./min (about 1.1° C./min.). The dye is allowed to stay in contact with the cotton for a sufficient period of time for absorbance, for example, 30 min., 45 min., 60 min., or longer.
- At
block 126, the dye, mordant, and salts are rinsed from the solution. Atblock 208, an oxidizer is added to the water solution to oxidize the reduced dye. In various embodiments, the oxidizer is hydrogen peroxide, air, oxygen, a water solution of ozone, and the like. In some embodiments, hydrogen peroxide is added at between about 1 g/l and about 5 g/l. In other embodiments, the dye is allowed to oxidize in air for about 20 to about 30 minutes. The amount of oxidation controls the color, with higher levels of oxidation correlated to darker colors. - At
block 128, the pH is lowered to less than 8, or less than 7, or about 6.5. This is performed by the addition of an organic acid, such as citric acid, acetic acid, or the like. Atblock 130, a water rinse is performed to remove the acid and any remaining dyes or salts. In some embodiments, the pH is checked to confirm that it is between 6.5 and 7. If not, more acid may be added, and the pH retested. - It can be noted that all of the enzymes described herein are available from other suppliers. For example, AB Enzymes of Darmstadt, DE, produces analogous arylesterase catalysts and catalase enzymes that may be used in the processes described herein.
- Further, any number of other dyes may be used in embodiments described herein, including, including vat dyes, sulfur dyes, pre-reduced versions of vat and sulfur dyes, and other dyes that are insoluble and are applied to substrates via redox methods. Other dyes than can be used include azo dyes, such as direct dyes, metal complex dyes, reactive dyes, substantive dyes, and aniline dyes, such as natural and synthetic indigo dye, among others.
- The treatment process described herein, for example, with respect to
FIG. 1 , was tested on cotton fabric using the parameters described in Table 1. The dye used in the process described in Table 1 can be used pre-reduced dyes, such as pre-reduced indigo and pre-reduced sulfur dyes, as shown in Table 2. -
TABLE 1 Parameters for treating process applied to cotton fabric DWELL TEMP. PRODUCT/ TIME in ° F. STAGE DOSE ACTION (MIN) (in ° C.) PROCESS NOTES PRETREATING 1 2 g/l Soda Ash 30 150 (66) Dwell (Na2CO3) 3 g/l Triacetin 0.5 g/l Sequestering agent 2 5.0 g/l Hydrogen 10 150 (66) Dwell Check pH 9.5-10 Peroxide (H2O2, 50 vol. %) 0.2 g/l 10 150 (66) Dwell Arylesterase catalyst 3 0.5 g/l Catalase Enzyme 15 120 (49) Dwell Check Peroxide Eliminated 4 0.32 g/l Citric Acid 12 Dwell Check pH 6.5-7 Water-Only Wash 120 (49) Optional, if peroxide is not eliminated Surface Tension Water beading Test for Wax on surface DYEING 1 30 g/l Sodium Sulfate 10 100 (38) Treat 10-15 Min 1A 6 g/l Soda Ash Dense 10 100 (38) Treat 1B Add Reactive Dye 10 100 (38) 2 Heat Dye Liquor 20 140 (60) Heat 3° F./min to 140° F. Max Temp. 3 Run 45 Mins 45 140 (60) Dwell 140° F. Max Temp. 4 Water Rinse 10 120 (49) Dwell 5 0.625 g/l Citric Acid 12 120 (49) Dwell 6 Water Rinse 8 120 (49)- Dwell 140° F. (60° C.) 140 (60) Max Temp. WAXLOCK 1 3-10% Wax lock Treat Wax lock OWB (silicone, acrylic, natural product) 2 Fixing wax lock 300 (149)- Dry 25-30 Yds/Min 390 (199) (23-27 m/min.) On Frame -
TABLE 2 Parameters for dying cotton fabric using a pre-reduced dye PRODUCT/ DWELL TEMP. in ° F. STAGE DOSE ACTION (MIN) (in ° C.) PROCESS NOTES DYEING 1 30 g/l Sodium Sulfate 10 100 (38) Treat 10-15 Min 1A 6 g/l Soda Ash 10 100 (38) Treat (Sodium Carbonate) 2 Pre-reduced Dye 10 100 (38) (Vat, sulfur, pre- reduced versions) 2A 4 g/l Catalase Enzyme 2B 10 g/l Aluminum Sulfate 10 100 (38) 2 Heat Dye Liquor 20 140 (60) Heat 2° F./min to 140° F. Max Temp. Check pH 3 Run 45 Mins 45 140 (60) Dwell 140° F. Max Temp. 4 Water Rinse 10 120 (49) Dwell 4A 1 g/l Hydrogen peroxide 10 120 (49) Dwell Oxidation 5 0.625 g/l Citric Acid 12 120 (49) Dwell Neutralize pH (to about 7.0) 6 Water Rinse 8 120 (49)- Dwell 140° F. (60° C.) 140 (60) Max Temp. - As described herein, after the pretreatment, cotton fabric can be made into garments, and the wax lock can be applied during the dying process, for example, before the dye is added. A cotton fabric prepared using this technique with a silicone softener as the wax lock compound retained the natural wax through greater than 25 laundering cycles using a cool wash cycle, 1 g/L Tide laundry detergent, and a cool dry cycle. This was tested by performed a surface tension test after each laundering cycle by applying a water droplet and determining that it beaded on the cotton fabric. As described herein, the natural wax lock products from Rudolph, Ruco-Dry Bio CGR and Ruco-Dry Bio NPE, are highly effective.
- The burst strength of the cotton fabric was compared to a sample of cotton fabric that was treated by the normal caustic wash. The test performed to determine the strength was the Mullen diaphragm burst test, following ASTM D3787. The strength retained by the cotton fibers depended on the initial lengths of the cotton fibers, e.g., the quality of the cotton. A sample of fabric made using a high-quality cotton and treated using the procedure described with respect to
FIG. 1 provided an average burst strength of up to 210 psi (about 1448 kPa), versus a sample of the same fabric treated with the standard Kiering procedure, which had an average burst strength of about 110 psi (about 758 kPa). - A sample of fabric prepared from a lower quality cotton, e.g., with shorter fiber lengths, still maintained a significant strength advantage when treated with the procedure of
FIG. 1 versus the normal Kiering procedure. The fabric prepared from the lower quality cotton that was treated with the standard Kiering procedure had an average burst strength of about 93.9 psi (647 kPa). A sample of the same fabric treated with the procedure ofFIG. 1 had an average burst strength of about 109.8 psi (757 kPa). - An embodiment described in examples herein provides a method for making water-resistant cotton garments. The method includes treating cotton fabric with soda ash at a temperature of less than about 150° F. (about 66° C.) and a pH of about 9.5 and bleaching the cotton fabric with hydrogen peroxide at a temperature of less than about 150° F. (about 66° C.). The hydrogen peroxide is neutralized, and the pH is lowered with an organic acid to between about 6 and about 7. A garment is made from the cotton fabric and a wax lock is applied to the garment. The garment is dyed at a temperature of less than about 150° F. (about 66° C.), and dried.
- In an aspect, combinable with any other aspect, making the garment includes cutting pieces from the cotton fabric and sewing the pieces together to form the garment.
- In an aspect, combinable with any other aspect, the method includes adding a bleach activator with the soda ash.
- In an aspect, combinable with any other aspect, the method includes adding a sequestering agent with the soda ash.
- In an aspect, combinable with any other aspect, the method includes adding an arylesterase catalyst with the hydrogen peroxide.
- In an aspect, combinable with any other aspect, neutralizing includes adding an enzyme to degrade the hydrogen peroxide.
- In an aspect, combinable with any other aspect, the organic acid includes citric acid.
- In an aspect, combinable with any other aspect, applying the wax lock to the garment includes treating the garment with sodium sulfate, treating the cotton with soda ash to raise the pH to about 9.5, and applying the wax lock to the garment.
- In an aspect, combinable with any other aspect, the dying includes treating the garment with a dye solution, rinsing the garment, neutralizing the dye solution to a pH of about 6.5, and rinsing the garment.
- In an aspect, combinable with any other aspect, the dye solution includes a pre-reduced dye.
- In an aspect, combinable with any other aspect, the method includes adding a reducing agent to the dye solution.
- In an aspect, combinable with any other aspect, the method includes adding a mordant to the dye solution.
- In an aspect, combinable with any other aspect, the method includes treating the garment with an oxidant.
- In an aspect, combinable with any other aspect, the method includes treating the garment with the wax lock.
- In an aspect, combinable with any other aspect, the method includes drying the garment at between about 300° F. (about 149° C.) and about 390° F. (about 199° C.).
- In an aspect, combinable with any other aspect, the wax lock includes a silicone compound.
- In an aspect, combinable with any other aspect, wax lock includes an acrylic compound.
- Another embodiment described in examples herein provides a cotton garment formed from an activated cotton material, including a layer of natural wax locked to a surface of cotton fibers by a wax lock.
- In an aspect, combinable with any other aspect, the cotton garment includes a dye.
- In an aspect, combinable with any other aspect, the cotton garment includes a pre-reduced dye.
- In an aspect, combinable with any other aspect, the pre-reduced dye includes indigo.
- In an aspect, combinable with any other aspect, the wax lock includes a silicone compound.
- In an aspect, combinable with any other aspect, the wax lock includes an acrylic oligomer.
- In an aspect, combinable with any other aspect, the wax lock includes a natural plant material.
- In an aspect, combinable with any other aspect, the wax lock includes a natural plant material combined with a cross-linking agent.
- Other implementations are also within the scope of the following claims.
Claims (25)
1. A method for making water-resistant cotton garments, comprising:
treating cotton fabric with soda ash at a temperature of less than about 150° F. (about 66° C.) and a pH of about 9.5;
bleaching the cotton fabric with hydrogen peroxide at a temperature of less than about 150° F. (about 66° C.);
neutralizing the hydrogen peroxide;
lowering the pH with an organic acid to between about 6 and about 7;
making a garment from the cotton fabric;
applying a wax lock to the garment;
dying the garment at a temperature of less than about 150° F. (about 66° C.); and
drying the garment.
2. The method of claim 1 , wherein making the garment comprises:
cutting pieces from the cotton fabric; and
sewing the pieces together to form the garment.
3. The method of claim 1 , comprising adding a bleach activator with the soda ash.
4. The method of claim 1 , comprising adding a sequestering agent with the soda ash.
5. The method of claim 1 , comprising adding an arylesterase catalyst with the hydrogen peroxide.
6. The method of claim 1 , wherein neutralizing comprises adding an enzyme to degrade the hydrogen peroxide.
7. The method of claim 1 , wherein the organic acid comprises citric acid.
8. The method of claim 1 , wherein applying the wax lock to the garment, comprises:
treating the garment with sodium sulfate;
treating the cotton with soda ash to raise the pH to about 9.5; and
applying the wax lock to the garment.
9. The method of claim 1 , wherein the dying comprises:
treating the garment with a dye solution;
rinsing the garment;
neutralizing the dye solution to a pH of about 6.5; and
rinsing the garment.
10. The method of claim 9 , wherein the dye solution comprises a pre-reduced dye.
11. The method of claim 10 , comprising adding a reducing agent to the dye solution.
12. The method of claim 10 , comprising adding a mordant to the dye solution.
13. The method of claim 10 , comprising treating the garment with an oxidant.
14. The method of claim 1 , comprising treating the garment with the wax lock.
15. The method of claim 14 , comprising drying the garment at between about 300° F. (about 149° C.) and about 390° F. (about 199° C.).
16. The method of claim 14 , wherein the wax lock comprises a silicone compound.
17. The method of claim 14 , wherein the wax lock comprises an acrylic compound.
18. A cotton garment formed from an activated cotton material, comprising a layer of natural wax locked to a surface of cotton fibers by a wax lock.
19. The cotton garment of claim 18 , comprising a dye.
20. The cotton garment of claim 18 , comprising a pre-reduced dye.
21. The cotton garment of claim 20 , wherein the pre-reduced dye comprises indigo.
22. The cotton garment of claim 18 , wherein the wax lock comprises a silicone compound.
23. The cotton garment of claim 18 , wherein the wax lock comprises an acrylic oligomer.
24. The cotton garment of claim 18 , wherein the wax lock comprises a natural plant material.
25. The cotton garment of claim 18 , wherein the wax lock comprises a natural plant material combined with a cross-linking agent.
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US202263373101P | 2022-08-22 | 2022-08-22 | |
US18/453,769 US20240060230A1 (en) | 2022-08-22 | 2023-08-22 | Launderable activated cotton garment |
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KR101315368B1 (en) * | 2012-02-17 | 2013-10-08 | 조은효 | Synthetic textile Product having Moisture movement and Waterproof function and Method of manufacturing the Synthetic textile porduct |
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US20220389650A1 (en) * | 2021-01-25 | 2022-12-08 | Energy Ogre Llc | Launderable activated cotton |
US20220235518A1 (en) * | 2021-01-25 | 2022-07-28 | Energy Ogre Llc | Launderable activated cotton |
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