CN115404700B - Preparation method of flame-retardant down fiber - Google Patents
Preparation method of flame-retardant down fiber Download PDFInfo
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- CN115404700B CN115404700B CN202211267519.7A CN202211267519A CN115404700B CN 115404700 B CN115404700 B CN 115404700B CN 202211267519 A CN202211267519 A CN 202211267519A CN 115404700 B CN115404700 B CN 115404700B
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- down fiber
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- 239000000835 fiber Substances 0.000 title claims abstract description 157
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 title claims abstract description 40
- 239000003063 flame retardant Substances 0.000 title claims abstract description 40
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 43
- 238000003756 stirring Methods 0.000 claims abstract description 30
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000004202 carbamide Substances 0.000 claims abstract description 19
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 18
- VHJLVAABSRFDPM-QWWZWVQMSA-N dithiothreitol Chemical compound SC[C@@H](O)[C@H](O)CS VHJLVAABSRFDPM-QWWZWVQMSA-N 0.000 claims abstract description 18
- 238000001914 filtration Methods 0.000 claims abstract description 15
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims abstract description 14
- 230000001105 regulatory effect Effects 0.000 claims abstract description 12
- 238000001035 drying Methods 0.000 claims abstract description 9
- 238000007599 discharging Methods 0.000 claims abstract description 6
- 150000007524 organic acids Chemical class 0.000 claims abstract description 6
- BJZIJOLEWHWTJO-UHFFFAOYSA-H dipotassium;hexafluorozirconium(2-) Chemical compound [F-].[F-].[F-].[F-].[F-].[F-].[K+].[K+].[Zr+4] BJZIJOLEWHWTJO-UHFFFAOYSA-H 0.000 claims abstract description 4
- 210000003746 feather Anatomy 0.000 claims description 39
- 238000000034 method Methods 0.000 claims description 17
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 14
- 238000005406 washing Methods 0.000 claims description 14
- 239000007788 liquid Substances 0.000 claims description 13
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 9
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 8
- 239000008367 deionised water Substances 0.000 claims description 7
- 229910021641 deionized water Inorganic materials 0.000 claims description 7
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 6
- 229910052708 sodium Inorganic materials 0.000 claims description 6
- 239000011734 sodium Substances 0.000 claims description 6
- 239000004094 surface-active agent Substances 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 5
- 235000014113 dietary fatty acids Nutrition 0.000 claims description 4
- 229930195729 fatty acid Natural products 0.000 claims description 4
- 239000000194 fatty acid Substances 0.000 claims description 4
- 150000004665 fatty acids Chemical class 0.000 claims description 4
- 150000002191 fatty alcohols Chemical class 0.000 claims description 4
- IMQLKJBTEOYOSI-GPIVLXJGSA-N Inositol-hexakisphosphate Chemical compound OP(O)(=O)O[C@H]1[C@H](OP(O)(O)=O)[C@@H](OP(O)(O)=O)[C@H](OP(O)(O)=O)[C@H](OP(O)(O)=O)[C@@H]1OP(O)(O)=O IMQLKJBTEOYOSI-GPIVLXJGSA-N 0.000 claims description 3
- IMQLKJBTEOYOSI-UHFFFAOYSA-N Phytic acid Natural products OP(O)(=O)OC1C(OP(O)(O)=O)C(OP(O)(O)=O)C(OP(O)(O)=O)C(OP(O)(O)=O)C1OP(O)(O)=O IMQLKJBTEOYOSI-UHFFFAOYSA-N 0.000 claims description 3
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 3
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 claims description 3
- 235000002949 phytic acid Nutrition 0.000 claims description 3
- 229940068041 phytic acid Drugs 0.000 claims description 3
- 239000000467 phytic acid Substances 0.000 claims description 3
- 235000002906 tartaric acid Nutrition 0.000 claims description 3
- 239000011975 tartaric acid Substances 0.000 claims description 3
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 claims description 2
- 238000000643 oven drying Methods 0.000 claims description 2
- AFVFQIVMOAPDHO-UHFFFAOYSA-M Methanesulfonate Chemical compound CS([O-])(=O)=O AFVFQIVMOAPDHO-UHFFFAOYSA-M 0.000 claims 1
- 238000002203 pretreatment Methods 0.000 claims 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 abstract description 10
- 229910052700 potassium Inorganic materials 0.000 abstract description 10
- 239000011591 potassium Substances 0.000 abstract description 10
- 125000002887 hydroxy group Chemical group [H]O* 0.000 abstract description 7
- 238000004132 cross linking Methods 0.000 abstract description 5
- 230000009920 chelation Effects 0.000 abstract 1
- 238000006068 polycondensation reaction Methods 0.000 abstract 1
- 102000011782 Keratins Human genes 0.000 description 16
- 108010076876 Keratins Proteins 0.000 description 16
- SCPYDCQAZCOKTP-UHFFFAOYSA-N silanol Chemical compound [SiH3]O SCPYDCQAZCOKTP-UHFFFAOYSA-N 0.000 description 10
- 125000003396 thiol group Chemical group [H]S* 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 7
- 230000002378 acidificating effect Effects 0.000 description 5
- 230000009286 beneficial effect Effects 0.000 description 5
- 238000005238 degreasing Methods 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- 230000003301 hydrolyzing effect Effects 0.000 description 4
- 235000018102 proteins Nutrition 0.000 description 4
- 102000004169 proteins and genes Human genes 0.000 description 4
- 108090000623 proteins and genes Proteins 0.000 description 4
- 235000001014 amino acid Nutrition 0.000 description 3
- 150000001413 amino acids Chemical class 0.000 description 3
- 230000018044 dehydration Effects 0.000 description 3
- 238000006297 dehydration reaction Methods 0.000 description 3
- 229920001184 polypeptide Polymers 0.000 description 3
- 102000004196 processed proteins & peptides Human genes 0.000 description 3
- 108090000765 processed proteins & peptides Proteins 0.000 description 3
- 230000033228 biological regulation Effects 0.000 description 2
- 235000019387 fatty acid methyl ester Nutrition 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 239000001226 triphosphate Substances 0.000 description 2
- 235000011178 triphosphate Nutrition 0.000 description 2
- UNXRWKVEANCORM-UHFFFAOYSA-N triphosphoric acid Chemical compound OP(O)(=O)OP(O)(=O)OP(O)(O)=O UNXRWKVEANCORM-UHFFFAOYSA-N 0.000 description 2
- QIIDATRCGITYRZ-UHFFFAOYSA-N Catalpol Natural products OCC1OC(OC2OC=CC3C(O)C(=C(CO)C23)O)C(O)C(O)C1O QIIDATRCGITYRZ-UHFFFAOYSA-N 0.000 description 1
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 1
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- LHDWRKICQLTVDL-PZYDOOQISA-N catalpol Chemical compound O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@H]1O[C@H]1[C@@H]2[C@@]3(CO)O[C@H]3[C@@H](O)[C@@H]2C=CO1 LHDWRKICQLTVDL-PZYDOOQISA-N 0.000 description 1
- UXSACQOOWZMGSE-UHFFFAOYSA-N catalposide Natural products OC1C(O)C(O)C(CO)OC1OC1C2C3(CO)OC3C(OC(=O)C=3C=CC(O)=CC=3)C2C=CO1 UXSACQOOWZMGSE-UHFFFAOYSA-N 0.000 description 1
- 210000000170 cell membrane Anatomy 0.000 description 1
- 239000003431 cross linking reagent Substances 0.000 description 1
- 235000018417 cysteine Nutrition 0.000 description 1
- 150000001945 cysteines Chemical class 0.000 description 1
- 238000004042 decolorization Methods 0.000 description 1
- 239000003599 detergent Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000012796 inorganic flame retardant Substances 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- LHDWRKICQLTVDL-UHFFFAOYSA-N methyl iridoid glycoside Natural products OC1C(O)C(O)C(CO)OC1OC1C2C3(CO)OC3C(O)C2C=CO1 LHDWRKICQLTVDL-UHFFFAOYSA-N 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000010355 oscillation Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 244000144977 poultry Species 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 229910052938 sodium sulfate Inorganic materials 0.000 description 1
- 235000011152 sodium sulphate Nutrition 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
- 150000003754 zirconium Chemical class 0.000 description 1
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
- D06M19/00—Treatment of feathers
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/32—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
- D06M11/36—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
- D06M11/46—Oxides or hydroxides of elements of Groups 4 or 14 of the Periodic System; Titanates; Zirconates; Stannates; Plumbates
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/244—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing sulfur or phosphorus
- D06M13/248—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing sulfur or phosphorus with compounds containing sulfur
- D06M13/252—Mercaptans, thiophenols, sulfides or polysulfides, e.g. mercapto acetic acid; Sulfonium compounds
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/322—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing nitrogen
- D06M13/402—Amides imides, sulfamic acids
- D06M13/432—Urea, thiourea or derivatives thereof, e.g. biurets; Urea-inclusion compounds; Dicyanamides; Carbodiimides; Guanidines, e.g. dicyandiamides
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/50—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with organometallic compounds; with organic compounds containing boron, silicon, selenium or tellurium atoms
- D06M13/503—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with organometallic compounds; with organic compounds containing boron, silicon, selenium or tellurium atoms without bond between a carbon atom and a metal or a boron, silicon, selenium or tellurium atom
- D06M13/507—Organic silicon compounds without carbon-silicon bond
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/02—Natural fibres, other than mineral fibres
- D06M2101/10—Animal fibres
-
- 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
- D06M2200/30—Flame or heat resistance, fire retardancy properties
Abstract
The invention discloses a preparation method of flame-retardant down fiber, which belongs to the technical field of down fiber treatment, and is characterized in that down fiber is obtained after down pretreatment; adding down fibers and urea solution into a rotary drum, stirring for 5-10min, discharging urea solution, adding 1, 4-dithiothreitol solution, continuously stirring for 3-4h, filtering, taking down fibers out, rinsing, dehydrating, adding the down fibers and potassium fluorozirconate solution into the rotary drum, regulating pH value with organic acid, stirring for 5-6h, filtering, taking down fibers, rinsing, dehydrating, adding the down fibers and film forming solution into the rotary drum, regulating pH value with acetic acid, stirring, reacting for 30-40min, filtering, dehydrating, and drying to obtain flame-retardant down fibers; the 1, 4-dithiothreitol plays a role in chain extension, and the potassium fluozirconate can improve the flame retardant property of the down fiber after chelation, and the water resistance of the down fiber is improved by polycondensation and crosslinking of tetraethyl orthosilicate and hydroxyl groups to form a film.
Description
Technical Field
The invention belongs to the technical field of down fiber treatment, and particularly relates to a preparation method of flame-retardant down fibers.
Background
Eiderdown is typically taken from birds and is a mixture of feathers and down. The feather is a feather piece with harder poultry texture, plays a supporting role in the down feather, and is favorable for rebound of the down feather; the down is a three-dimensional spherical down, consists of a down core and a plurality of down filaments, has a fluffy structure, is light and soft, has excellent warmth retention property, and can be made into products such as down jackets, down quilts and the like.
The down fibre is a natural protein fibre, and the external surface of the down fibre is covered by a cell membrane formed by a bilayer of a catalpol and a triphosphate. Both the Zi-alcohol and the triphosphate are water insoluble matters, so the down feather fiber has better waterproof performance. The inner layer of the film is protein which is the main component of down fiber, commonly called down protein, and is formed by condensing various amino acids. The amino acids are combined into polypeptide chains in different forms, and the polypeptide chains are combined through hydrogen bonds and disulfide bonds among cysteines, so that the amino acid molecules are arranged according to a certain shape. The polypeptide chains are intertwined with each other and twisted into one strand, and the strands are further twisted together to form a rope structure. The kink forms more gaps and holes, which is also the reason for the light and warm-keeping of the down fiber.
As a natural protein fiber, the down fiber has higher limiting oxygen index, belongs to combustible fibers, and has important significance for increasing the flame retardant property. The prior patent with publication number of CN105780502B discloses a flame-retardant down fiber and a preparation method thereof, wherein the flame-retardant down fiber is obtained by grafting and modifying the down fiber with inorganic flame retardant zirconium salt by using organic acid as a cross-linking agent. After the flame-retardant down fiber is made into a product, consumers can dry and clean the product frequently in the using process, and finally the flame retardant property of the flame-retardant down fiber is reduced, so that the preparation method of the water-resistant flame-retardant down fiber is provided.
Disclosure of Invention
The invention aims to provide a preparation method of flame-retardant down fiber, which aims to solve the problems in the background technology.
The aim of the invention can be achieved by the following technical scheme:
a preparation method of flame-retardant down feather fiber comprises the following steps:
step one: adding down into a rotary drum, adding water at 30-50 ℃ and surfactant, washing for 20-30min under the condition of 40-60r/min, and degreasing down; rinsing with running water for 5-10min, washing with hydrogen peroxide solution with concentration of 50-60mL/L at 70deg.C for 40-60min, rinsing down with running water for 5-10min, dehydrating, and oven drying to obtain down fiber;
step two: adding down feather fiber into a rotary drum, adding urea solution with the concentration of 8mol/L, stirring for 5-10min at 70-80 ℃ and 40-60r/min, discharging urea solution, adding 1, 4-dithiothreitol solution with the concentration of 4mmol/L into the rotary drum, and stirring for 3-4h at 70-80 ℃ and 40-60 r/min;
step three: filtering and taking out the chain-extended down fiber, rinsing the down fiber with running water for 5-10min, putting the down fiber into a clean rotary drum after dehydration, then adding a potassium fluozirconate solution with the concentration of 2-2.5g/L, regulating the pH value to 2-3 by using an organic acid, stirring for 5-6h under the conditions of 50-80 ℃ and 40-60r/min, filtering to remove the potassium fluozirconate solution, taking out the down fiber, rinsing the down fiber with running water for 5-10min, and dehydrating to obtain the grafted and modified down fiber;
step four: stirring and mixing tetraethyl orthosilicate, ethanol and deionized water to obtain a film forming liquid, putting the film forming liquid and the grafted and modified down feather fiber into a rotary drum, regulating the pH value to 5 by acetic acid, stirring and reacting for 30-40min at 100 ℃ under the condition of 40-60r/min, hydrolyzing the tetraethyl orthosilicate under the acidic condition to generate silanol, polycondensing and crosslinking hydroxyl groups in the silanol and the grafted and modified down feather fiber to form a film, rinsing the down feather fiber with running water for 5-10min after filtering, dehydrating and drying to obtain the flame-retardant down feather fiber.
Further, in the first step, the dosage ratio of the down feather, the water and the surfactant is 15g:500mL:1g.
Further, the surfactant in the first step is any one of fatty acid methyl ester sodium sulfonate and fatty alcohol ether sodium sulfate.
Further, in the second step, the dosage ratio of the down feather fiber, the urea solution and the 1, 4-dithiothreitol solution is 1g:100mL:150mL.
Further, the dosage ratio of the down feather fiber and the potassium fluozirconate solution after dehydration in the step three is 1g:120-150mL.
Further, in the third step, the organic acid is any one of tartaric acid, fatty acid and phytic acid.
Further, in the fourth step, the dosage ratio of tetraethyl orthosilicate, ethanol and deionized water is 10g:30g:80g.
Further, in the fourth step, the dosage ratio of the film forming liquid to the down fiber is 18-20g:1g.
The invention has the beneficial effects that:
the flame-retardant down fiber has good water resistance, and has excellent flame retardance after repeated washing. In the preparation process of the flame-retardant down fiber, firstly degreasing and decolorizing the down, then treating the down with urea, wherein the urea dissolves a small amount of keratin on the surface of the down fiber and damages the keratin structure on the surface of the down fiber, and the roughness of the surface of the down fiber is increased so as to increase the surface area of the down fiber; breaking disulfide bond on keratin by 1, 4-dithiothreitol to expose free sulfhydryl, and simultaneously, the 1, 4-dithiothreitol is recombined with free sulfhydryl on the surface of down fiber to play a role of chain extension, thereby being beneficial to restoring the conformation of keratin and keeping the original characteristics of the down fiber; the potassium fluorozirconate can effectively improve the carbon residue rate of the down fiber after being chelated, and improve the flame retardant property of the down fiber; the 1, 4-dithiothreitol provides a large amount of hydroxyl groups for the down feather fiber, the tetraethyl orthosilicate is hydrolyzed under the acidic condition to generate silanol, the silanol and the hydroxyl groups on the down feather fiber are condensed and crosslinked to form a film, the water resistance of the down feather fiber is improved, and the flame retardant property of the down feather fiber is further improved.
Detailed Description
The technical solutions of the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
Preparing flame-retardant down fiber, which comprises the following steps:
step one: putting 150g of down into a rotary drum, adding 5L of 30 ℃ water and 10g of fatty acid methyl ester sodium sulfonate, washing for 20min at 40r/min, and degreasing the down; and then rinsing with running water for 5min, washing with hydrogen peroxide with the concentration of 50mL/L at 70 ℃ for 40min, rinsing down with running water for 5min after decolorization, dehydrating, and drying to obtain the down fiber.
Step two: adding 100g of down fiber into a rotary drum, adding 10L of urea solution with the concentration of 8mol/L, stirring for 5min at 70 ℃ and 40r/min, dissolving a small amount of keratin on the surface of the down fiber by urea, destroying the keratin structure on the surface of the down fiber, and increasing the roughness of the surface of the down fiber so as to increase the surface area of the down fiber; discharging urea solution, adding 15L of 1, 4-dithiothreitol solution with the concentration of 4mmol/L into a rotary drum, stirring for 3h at 70 ℃ and 40r/min, breaking disulfide bonds on keratin by 1, 4-dithiothreitol to expose free sulfhydryl groups, and simultaneously, re-pairing the 1, 4-dithiothreitol with the free sulfhydryl groups on the surface of down fiber to play a role of chain extension, thereby being beneficial to restoring the conformation of the keratin and keeping the original characteristics of the down fiber.
Step three: rinsing the chain-extended down fiber with running water for 5min, putting 100g of the down fiber into a clean rotary drum after dehydration, then adding 12L of potassium fluozirconate solution with the concentration of 2g/L, regulating the pH value to 2 by using tartaric acid, stirring for 5h at 50 ℃ and 40r/min, filtering to remove the potassium fluozirconate solution, taking out the down fiber, rinsing with running water for 5min, and dehydrating to obtain the grafted modified down fiber.
Step four: stirring and mixing 1kg of tetraethyl orthosilicate, 3kg of ethanol and 8kg of deionized water to obtain a film forming liquid, putting 1.8kg of the film forming liquid and 100g of the grafted and modified down feather fiber into a rotary drum, regulating the pH value to 5 by acetic acid, stirring and reacting for 30min under the conditions of 100 ℃ and 40r/min, hydrolyzing the tetraethyl orthosilicate under the acidic condition to generate silanol, polycondensing and crosslinking the silanol and hydroxyl groups in the grafted and modified down feather fiber to form a film, rinsing the down feather fiber with running water for 5min after filtering, dehydrating and drying to obtain the flame-retardant down feather fiber.
Example 2
Preparing flame-retardant down fiber, which comprises the following steps:
step one: putting 150g of down into a rotary drum, adding 5L of water at 40 ℃ and 10g of sodium fatty alcohol ether sulfate, washing for 25min at 50r/min, and degreasing the down; and then rinsing with running water for 8min, washing with 55mL/L hydrogen peroxide at 70 ℃ for 50min, decolorizing, rinsing down with running water for 8min, dehydrating, and drying to obtain down fiber.
Step two: adding 100g of down fiber into a rotary drum, adding 10L of urea solution with the concentration of 8mol/L, stirring for 8min at the temperature of 75 ℃ and the speed of 50r/min, dissolving a small amount of keratin on the surface of the down fiber by urea, destroying the keratin structure on the surface of the down fiber, and increasing the roughness of the surface of the down fiber so as to increase the surface area of the down fiber; discharging urea solution, adding 15L of 1, 4-dithiothreitol solution with the concentration of 4mmol/L into a rotary drum, stirring for 3.5h at the temperature of 75 ℃ and the speed of 50r/min, breaking disulfide bonds on keratin by 1, 4-dithiothreitol to expose free sulfhydryl groups, and simultaneously, re-pairing the 1, 4-dithiothreitol with free sulfhydryl groups on the surface of down feather fibers to play a role of chain extension, thereby being beneficial to restoring the conformation of the keratin and keeping the original characteristics of the down feather fibers.
Step three: rinsing the chain-extended down fiber with running water for 8min, dewatering, taking 100g of down fiber, putting into a clean rotary drum, adding 13.5L of potassium fluozirconate solution with the concentration of 2.2g/L, regulating the pH value to 2.5 with fatty acid, stirring for 5.5h at 65 ℃ and 50r/min, filtering to remove the potassium fluozirconate solution, taking out the down fiber, rinsing with running water for 8min, and dewatering to obtain the grafted and modified down fiber.
Step four: stirring and mixing 1kg of tetraethyl orthosilicate, 3kg of ethanol and 8kg of deionized water to obtain a film forming liquid, putting 1.9kg of the film forming liquid and 100g of the grafted and modified down feather fiber into a rotary drum, regulating the pH value to 5 by acetic acid, stirring and reacting for 35min under the conditions of 100 ℃ and 50r/min, hydrolyzing the tetraethyl orthosilicate under the acidic condition to generate silanol, polycondensing and crosslinking the silanol and hydroxyl groups in the grafted and modified down feather fiber to form a film, rinsing the down feather fiber with running water for 8min after filtering, dehydrating and drying to obtain the flame-retardant down feather fiber.
Example 3
Preparing flame-retardant down fiber, which comprises the following steps:
step one: putting 150g of down into a rotary drum, adding 5L of water at 50 ℃ and 10g of sodium fatty alcohol ether sulfate, washing for 30min under the condition of 60r/min, and degreasing the down; and then rinsing with running water for 10min, washing with 60mL/L hydrogen peroxide at 70 ℃ for 60min, decolorizing, rinsing with running water for 10min, dehydrating, and drying to obtain the down fiber.
Step two: adding 100g of down fiber into a rotary drum, adding 10L of urea solution with the concentration of 8mol/L, stirring for 10min at 80 ℃ and 60r/min, dissolving a small amount of keratin on the surface of the down fiber by urea, destroying the keratin structure on the surface of the down fiber, and increasing the roughness of the surface of the down fiber so as to increase the surface area of the down fiber; discharging urea solution, adding 15L of 1, 4-dithiothreitol solution with the concentration of 4mmol/L into a rotary drum, stirring for 4 hours at the temperature of 80 ℃ and under the condition of 60r/min, breaking disulfide bonds on keratin by 1, 4-dithiothreitol to expose free sulfhydryl groups, and simultaneously, re-pairing the 1, 4-dithiothreitol with the free sulfhydryl groups on the surface of down feather fibers to play a role of chain extension, thereby being beneficial to restoring the conformation of the keratin and keeping the original characteristics of the down feather fibers.
Step three: rinsing the chain-extended down fiber with running water for 10min, dewatering, taking 100g of down fiber, putting into a clean rotary drum, adding 15L of potassium fluozirconate solution with the concentration of 2.5g/L, regulating the pH value to 3 by using phytic acid, stirring for 6h at 80 ℃ and 60r/min, filtering to remove the potassium fluozirconate solution, taking out the down fiber, rinsing with running water for 10min, and dewatering to obtain the grafted modified down fiber.
Step four: stirring and mixing 1kg of tetraethyl orthosilicate, 3kg of ethanol and 8kg of deionized water to obtain a film forming liquid, putting 2kg of the film forming liquid and 100g of the down fiber subjected to grafting modification into a rotary drum, regulating the pH value to 5 by acetic acid, stirring and reacting for 40min under the conditions of 100 ℃ and 60r/min, hydrolyzing the tetraethyl orthosilicate under the acidic condition to generate silanol, polycondensing and crosslinking the silanol and hydroxyl groups in the grafted modified down fiber to form a film, filtering, rinsing the down fiber with running water for 10min, dehydrating and drying to obtain the flame-retardant down fiber.
Comparative example 1: on the basis of example 3, the down fiber was obtained by performing the treatment by the method of step one only.
Comparative example 2: on the basis of the embodiment 3, the down fiber is obtained by treating the down fiber by the method of the first step and then treating the down fiber by the method of the third step.
Comparative example 3: on the basis of the embodiment 3, the down fiber is obtained without the treatment of the method of the step three, and the rest steps are kept unchanged.
The performance test was performed on the finally prepared down fibers in examples 1 to 3 and comparative examples 1 to 3 (the principle of the method of comparative example 2 is the same as the prior art mentioned in the background art, and the flame retardant performance of the down fibers is improved by chelating and grafting the flame retardant), and the test method is as follows:
and (3) measuring the fluffiness, namely weighing 28.4g of different groups of down fibers respectively, transferring the down fibers into a cylinder of a fluffiness instrument, stirring the down fibers by using a glass rod to enable the down fibers to be tiled and to be in a completely fluffy state, covering the down fibers of different groups by using an aluminum plate with the same quality respectively, standing for 1min, recording scales on two sides of a cylinder wall, repeating the operation for three times, and taking an average value, wherein the average value is the fluffiness of the corresponding down fibers, and the fluffiness is more than 16cm and meets the standard.
And (3) transparency test, namely, testing the transparency degree of oscillation filtered water for the washed down fiber according to the related regulations of FZ/T800001-2002 of the washed down feather test method, wherein the transparency is higher, the quality of the down fiber is better, and the transparency is more than 450mm and meets the regulations.
And (3) testing flame retardant property, namely respectively taking 50g of down fibers in different groups, putting the down fibers into corresponding crucibles, respectively moving the corresponding crucibles into a muffle furnace at 400 ℃, carrying out heat preservation and burning for 40min, and detecting the percentage of the mass of the residual substances in the crucibles in different groups to the mass of the original down fibers, namely the carbon residue rate. The higher the carbon residue rate of the down fiber is, the better the flame retardant property is.
And washing the down fibers in different groups with the same dosage of the blue moon down jacket liquid detergent under the same conditions, airing, repeating the washing operation for 20 times, respectively taking out 50g of washed down fibers, performing flame retardant property test, and recording the carbon residue rate.
The test results are shown in table 1:
TABLE 1
As can be seen from table 1, the bulk of the down fiber can be improved by both chelating high salt and by treating the down fiber with tetraethyl orthosilicate; the down fiber in comparative example 2 has a slightly lower transparency than the down fiber of comparative example 1, which is only defatted and decolorized, and the down fibers finally produced in examples 1 to 3 have a better transparency and a higher char yield after washing with water.
It should be noted that in this document, terms such as "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
Although embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made therein without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (8)
1. The preparation method of the flame-retardant down fiber is characterized by comprising the following steps:
step one: pretreating down to obtain down fiber;
step two: adding down feather fiber and urea solution into a rotary drum, stirring at 70-80deg.C and 40-60r/min for 5-10min, discharging urea solution, adding 1, 4-dithiothreitol solution, stirring for 3-4 hr, filtering to remove down feather fiber, rinsing, and dehydrating;
step three: adding the down feather fiber and potassium fluorozirconate solution treated in the previous step into a rotary drum, regulating the pH value to 2-3 by using organic acid, stirring for 5-6h at 50-80 ℃ and 40-60r/min, filtering, taking out the down feather fiber, rinsing, and dehydrating;
step four: stirring and mixing tetraethyl orthosilicate, ethanol and deionized water to obtain a film forming liquid, putting the film forming liquid and the down feather fiber treated in the previous step into a rotary drum, regulating the pH value to 5 by acetic acid, stirring and reacting for 30-40min at 100 ℃ under the condition of 40-60r/min, filtering, rinsing the down feather fiber, dehydrating and drying to obtain the flame-retardant down feather fiber;
the pretreatment method in the first step comprises the following steps: washing down with water and surfactant at 40-60r/min for 20-30min, rinsing with running water for 5-10min, washing with hydrogen peroxide at 70deg.C for 40-60min, rinsing with running water for 5-10min, dewatering, and oven drying.
2. The method for preparing flame retardant down fiber according to claim 1, wherein the dosage ratio of down, water and surfactant is 15g:500mL:1g.
3. The method for preparing flame-retardant down fiber according to claim 1, wherein the surfactant is any one of sodium fatty acid methyl sulfonate and sodium fatty alcohol ether sulfate.
4. The method for preparing flame-retardant down fiber according to claim 1, wherein the dosage ratio of the down fiber, the urea solution and the 1, 4-dithiothreitol solution in the second step is 1g:100mL:150mL.
5. The method for preparing flame retardant down fiber according to claim 1, wherein the dosage ratio of down fiber to potassium fluorozirconate solution in the third step is 1g:120-150mL.
6. The method for preparing flame-retardant down fiber according to claim 1, wherein the organic acid in the third step is any one of tartaric acid, fatty acid and phytic acid.
7. The method for preparing flame-retardant down fiber according to claim 1, wherein the dosage ratio of tetraethyl orthosilicate, ethanol and deionized water in the fourth step is 10g:30g:80g.
8. The method for preparing flame-retardant down fiber according to claim 1, wherein the dosage ratio of the film forming liquid to the down fiber in the fourth step is 18-20g:1g.
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